An Experimental Investigation of Creep and Viscoelastic Properties Using Depth - Sensing Identation Techniques

University of Tennessee, Knoxville
Trace: Tennessee Research and Creative

Exchange
Doctoral Dissertations
Graduate School
5-1997
An Experimental Investigation of Creep and

Viscoelastic Properties Using Depth-Sensing
Indentation Techniques
Barry Neal Lucas
University of Tennessee - Knoxville
Recommended Citation
Lucas, Barry Neal, "An Experimental Investigation of Creep and Viscoelastic Properties Using Depth-Sensing Indentation Techniques.
" PhD diss., University of Tennessee, 1997.
http://trace.tennessee.edu/utk_graddiss/1255
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To the Graduate Council:

I am submitting herewith a dissertation written by Barry Neal Lucas entitled "An Experimental
Investigation of Creep and Viscoelastic Properties Using Depth-Sensing Indentation Techniques." I have
examined the final electronic copy of this dissertation for form and content and recommend that it be
accepted in partial fulfillment of the requirements for the degree of Doctor of Philosophy, with a major in
Materials Science and Engineering.
Carl J. McHargue, Major Professor
We have read this dissertation and recommend its acceptance:
Warren C. Oliver, Ben F. Oliver, Thomas G. Carley
Accepted for the Council:
Carolyn R. Hodges
Vice Provost and Dean of the Graduate School
(Original signatures are on file with official student records.)
To the Graduate Council:
I am submitting herewith a dissertation written by Barry Neal Lucas entitled" An

Experimental Investigation of Creep and Viscoelastic Properties Using Depth
Sensing Indentation Techniques." I have examined the final copy of the dissertation
for fonn and content and recommend that it be accepted in partial fulfillment of the
requirements for the degree of Doctor of Philosophy, with a major in Metallurgical
Engineering.
. u
Carl J. McHargue, Chairperson

We have read this dissertation and
recommend its acceptan
Warren C. Oliver, Technical Advisor

:;7
,if.
ve
-=-
Thomas G. C
Accepted for the Council:
Associate Vice Chancellor and

Dean of the Graduate School
AN EXPERIMENTAL INVESTIGATION OF CREEP AND

VISCOELASTIC PROPERTIES USING DEPTH-SENSING
INDENTATION TECHNIQUES
A Dissertation
Presented for the
Doctor of Philosophy
Degree
The University of Tennessee, Knoxville
Barry Neal Lucas

May 1997
Dedication
This dissertation is lovingly dedicated to my wife and sons;
Becky, Noah, and Caleb Lucas
and to my parents;
Arvil and Jane Lucas
Thank you all.
11
Acknowledgments
There are many people to whom lowe a debt of gratitude for making this work
possible. First and foremost, my technical advisor throughout my graduate career, Dr.
Warren C. Oliver. It is from his creative imagination that the idea for the hardware built
for this study evolved. Not only has he acted as my advisor and mentor throughout the
entirety of this work, he has also been my friend. I will always consider him my greatest
teacher for it is from him that I have not only learned a great deal of materials science,
but also a great deal about what it takes to be a materials scientist.
I also wish to thank the other members of my committee, Dr. Carl J. McHargue,
Dr. Ben F. Oliver and Dr. Thomas G. Carley. In addition to these official members,
special thanks are owed to Dr. George M. Pharr of Rice University for his valuable
contributions to the indentation creep portion of this work, and to Dr. Jean-Luc Loubet
of the Ecole Centrale de Lyon for the opportunity to work with him on the measurement
of the viscoelastic properties of materials with indentation techniques.
There are many others who have helped in many ways during the course of this
work. Dr. Ting Y. Tsui and Dr. Alexeii Bolshakov, two fellow Ph. D. students who
have gone on to great things, are thanked for their assistance at various times during this
work. I would also like to thank all of the people at the Oak Ridge National Laboratory
with whom I have had the opportunity to work but are too numerous to name. These are
the people who have quite often given very unselfishly of both their time and resources
with no reason for doing so other than their willingness to help a friend. All of you are
graciously thanked and you will be sorely missed.
Saving the best for last, lowe everything that I have accomplished to my family
to whom this work is dedicated. My wife Rebecca has stood by me through all of the
iii
long days and nights and never wavered in her love and support. She is quite truly the
most remarkable woman that I know. Not only is she a wonderful wife, but also a
wonderful mother to my two sons Noah and Caleb. The three of them have been a
constant reminder that there are more important things in life than ones work. And
finally to my parents, thank you for giving me every imaginable opportunity, which is
all anyone can ever ask for.
Your never ending support for me throughout every
endeavor of my life will never be forgotten.

Financial support for this work from Nano Instr uments, Inc. and the division of
Materials Sciences, U.S. Department of Energy, under contract DE-AC05-840R2 1 400
with Lockheed-Martin Energy Systems, Inc. is gratefully acknowledged.
iv
Abstract
Broad band, quasi-static and frequency specific dynamic techniques adapted to

depth-sensing indentation testing have been utilized to measure both time dependent
plasticity (creep) at both room and elevated temperatures as well as time dependent
elasticity (viscoelasticity) at room temperature.
Indentation Creep
Using a variety of depth-sensing indentation techniques at both room and

elevated temperatures, the dependency of the indentation hardness on the variables of
indentation strain rate (stress exponent for creep, n) and temperature (apparent activation
energy for creep, Q), and the existence of a steady state behavior in an indentation creep
test with a Berkovich indenter were investigated. The indentation creep response of five
materials, Pb-65 at% In (at RT), high purity indium (from RT to 75C), high purity
aluminum (from RT to 250C), a vapor deposited amorphous alumina f ilm (at RT), and
single crystal alumina (sapphire) (at RT), was measured. It was shown for the first time
that the indentation strain rate, def ined as
it/h,
could be held constant during an
experiment using a Berkovich indenter by controlling the loading rate such that the
loading rate divided by the load,
Pip, remained constant.
This technique yields the
most unambiguous determination of the stress exponent for creep and seems to most
closely approximate the steady state results fr om uniaxial testing. The results from the
constant
P/p experiments were compared to the results from conventional indentation
creep experiments where the load is ramped on at a high rate and then held constant for a
period of time. It was shown that the transition from the loading segment to hold
segment shows a transient period with an apparent higher stress exponent for creep
which has previously been mistaken for power law breakdown type behavior. The
apparent activation energy for indentation creep in indium was found to be
approximately 78 kJ/mol, in excellent agreement with the activation energy for self
diffusion in the material. The temperature dependence of the indentation creep process
in aluminum was found to be best described by an effective diffusion coefficient as
described in the literature for bulk aluminum at intermediate temperatures.
performing
By
Pip change experiments it was shown that a steady state path independent
hardness could be reached in an indentation test with a geometrically similar indenter.

The arrival at a new steady state value of hardness seems to depend on t he accumulation
of strain rather than a relaxation time. The measurements on amorphous alumina and
sapphire demonstrate the technique' s ability to measure differences in the time
dependent response of materials that can not be tested with other techniques.
Viscoelasticity
Using a frequency specific dynamic indentation technique, a general method to

measure the linear viscoelastic properties of polymers was determined. The polymer
tested was an amorphou s unvu1canized natural rubber, poly-cis l,4-isoprene. By
imposing a small harmonic force excitation on the specimen during the indentation
process and measuring the displacement response at the same frequency, the complex
elastic modulus, G*=G'+ iG" , of the polymer was determined.
The portion of the
displacement signal which is "in phase" with the excitation represents the elastic
response of the contact and is related to the stiffness (S) of the contact and to the elastic
modulus, or storage modulus (G') , of the material. The "out of phase" portion of the
displacement signal represents the energy being absorbed by the material, i.e. the
VI
damping (Coo where 00=2

material.
1t
t) of the contact, and thus the loss modulus (G" ) of the
It was shown that the storage, S,
and loss, Coo, components of the
displacement response scale as the respective component of the complex modulus

multiplied by the square root of the contact area.
Vll
Table of Contents
Chapter 1 Introduction
1 . Introduction
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1 . 1 Time Dependent Plasticity - Creep

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3. 1 Description of Nano Indenter II .. . .

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3.2 Description of the High Temperature Mechanical Properties

Microprobe ................................................................ ...................... 46
3.2. 1 Introduction ....................................................................... 46
3.2.2 Loading System ................................................................. 48
3.2.3 Displacement Sensing System ....................... ................... 48
3 .2.4 Vacuum I Manipulation System ...................... .................. 50
3.2.5 Temperature Monitoring and Control ............................... 5 1
Chapter 4 Developing a Set of Indentation Creep Constitutive
Equations and Defining Indentation Creep Terminology .
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4. Introduction ........................................................................................ 52
4. 1 Differences Between Uniaxial and Indentation Creep ..................... 52
4. 1 . 1 Introduction ....................................................................... 52
4. 1 .2 Steady State versus Transient Behavior ............................ 53
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Homogeneous Stress Distribution versus Radial

Stress Distribution ........................................................... 54
4. 1 .4 Constant Volume versus Expanding Volume ................... 54

4. 1 .5 User defined Geometry versus Material Defined
Geometry ......................................................................... 55
4.2 Analogy Between Indentation and Uniaxial Geometries ................. 55
4.3 Definition of Hardness as Indentation Stress ................................... 57
4.3 "Steady State Indentation Strain Rate and Hardness" ...................... 58
Chapter 5 Indentation Creep. Materials/Sample Preparation . . .
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5 . 1 Lead-65 at% Indium............................ ............................ ................. 60

5.2 Indium
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5 . 3 Aluminum
5.4 A1203
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Chapter 6 Indentation Creep - Experimental Techniques and Details . . . . 63

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6. 1 .4. 1 Development of a Constant "Indentation

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6. 1 .4.2 Experimental
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pip Change
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6.3.2 HTMPM ............................................................................ 76

Chapter 7 Indentation Creep - Results and Discussion .
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Chapter 8 Indentation Creep. Conclusions and Suggestion for

Future Research
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Chapter 9 Developing Indentation Viscoelasticity Constitutive

Equations
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9. Introduction
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Chapter 10 Indentation Viscoelasticity - Materials/Sample

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1 2 . 1 Introduction
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Chapter 13 Indentation Viscoelasticity - Conclusions and Suggestions

for Future Research
1 3 . 1 Conclusions
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Bibliography
Appendices
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A. l Calibration and Characterization of Nano IndenterII

A.2 Modeling the Elastic Contact
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A.3 Calibration and Characterization of HTMPM

Appendix B. Area Verification .
Indium
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B .2 Aluminum
Vita
. 1 87
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Appendix A. Dynamic Modeling
B.l
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1 87
1 87
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List of Figures
Figure 1 . A comparison of activation energies for creep and self diffusion for a
wide range of materials. From Sherby[35].
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Figure 2 . A plot of stress change data for AI from Horiuchi and Otsuka[45]
replotted by Sherby et al[26]. .................................. . ...................................... 1 7
Figure 3 . A schematic o f the strain response to an applied stress for a purely
elastic material. ........................................................... . .
Figure 4. A schematic of the strain response to an applied stress for a
viscoelastic material. ................... .................................................................... 37
Figure 5. A schematic of the Nano Indenter II. .. ......................................................... .45
Figure 6. A schematic of the High Temperature Mechanical Properties
Microprobe. . . ........................................................ .......................................... 47
Figure 7. Geometric comparison of uniaxial compression specimen (a) and
indentation creep 'specimen' (b) and equations for describing each . .............. 56
Figure 8. A plot of the load time history for step load experiments conducted on
Pb-65 at% In, amorphous A1 2 0 3 , and sapphire . ..............................................65
Figure 9. A plot of the load time history for the study of step loading effects on
In
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Figure 1 0. A plot of load versus time for the constant rate of loading
experiments. .. ............................. . ....................................................... ... ........ 68
Figure 1 1 . A plot of load versus time for the experiments, conducted on In,
during which
Figure 1 2. A plot of
pip was held constant. ................................ .......................... 7 1
pip versus displacement for pip change experiments
conducted on In . ................................................................. ..... ...................... 73

xiii
Figure 1 3 . A typical plot of displacement versus time during 3600 second hold
period under constant load following an 80 mN step load for Pb-65
at% In
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Figure 14. A log-log plot of indentation strain rate versus hardness for step load
experiments conducted on Pb-65at% In . . ...................................................... 80
Figure 1 5 . A semi-log plot of displacement versus time for In showing the
response of the material to a variety of step loads . ....................................... 8 1
Figure 1 6. A plot of displacement versus time showing the oscillatory response
of the indenter during the 80 ms immediately following a step load of
9 mN on In
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Figure 1 7. A plot of indentation strain rate versus displacement for CRLlHold

experiments conducted on In. . . ........................................ ..... ........................ 86
Figure 1 8. A plot of hardness versus displacement for CRLlHold experiments
conducted on In . .
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Figure 1 9. A log-log plot of the average indentation strain rate versus the
average hardness for series of constant loading ratelhold experiments
on In
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Figure 20. A plot of displacement versus time during the hold period under
constant load following a 1 second ramp to 1 0 mN for In at
temperatures ranging from - 1 00C to 75C . ................................................. 90
Figure 2 1 . A log-log plot of indentation strain rate versus hardness for
indentation creep experiments on In at temperatures of 28, 50, and
75C . . . .. .................................................. ......................... .............................. 9 1
xiv
Figure 22. A plot of indentation strain rate versus displacement for three
different constant Pip experiments conducted on In showing
constant indentation strain rates equal to 0.5 Pip .
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.
....
. . .. . . 93
..
...
..
Figure 23. A plot of hardness versus displacement for five different constant
Pip experiments conducted on In showing indentation steady state

behavior in response to constant Pip load ramp . ........................................ 94
Figure 24. A log-log plot of average indentation strain rate versus average
hardness for constant Pip experiments conducted on In . ............................ 95
Figure 25 . A log-log plot of hardness versus time under load for In
. ...
..............
. . . 97
...
...
Figure 26. A log-log plot of hardness versus time for In for experiments
conducted using 1 0 second constant rate of loading ramp to 1 0 mN
followed by a hold period under constant load ............................................. 100
Figure 27. A log-log plot of indentation strain rate versus hardness for
experiments conducted using 1 0 second loading ramp to 1 0 mN
followed by a hold period under constant load. ............................................ 1 0 1
Figure 28. A plot of indentation strain rate versus time for 1 , 1 0, and 30 second
load ramps to 10 mN followed by hold period under constant load for
In
. ..................................................................................................................
1 02
Figure 29. A log-log plot of indentation strain rate versus hardness comparing
the results of the CRUHoid experiments to the results of the constant
Pip experiments. ......................................................... ................................ 1 03

Figure 30. A plot of displacement versus time during hold period under constant
load following 1 second ramp to 10 mN for Al at temperatures
ranging from 1 00C to 250C . ................................... ................................... 106
xv
Figure 3 1 . A log-log plot of indentation strain rate versus hardness for

indentation creep experiments on Al conducted at 2 1 e . .............. ............... 1 07
indentation creep experiments on AI conducted at 1 00e. ........................... 1 08
indentation creep experiments on
AI
conducted at l 50C. ........................... 1 09
indentation creep experiments on Al conducted at 200C. ........................... 1 1 0
indentation creep experiments on Al conducted at 250C. ........................... 1 1 1
indentation creep experiments on Al conducted at 2 1 , 1 00, 1 50, 200,
and 250C . .......... . .................. ............ . .................. . ................ ........................ 1 1 3
Figure 37. A plot of the displacement versus time response to 80 mN step load
for a 1 .9/lm amorphous alumina film on sapphire . .. . ................................... 1 15
Figure 38. A log-log plot of indentation strain rate versus hardness for 1 .9 /lm
amorphous alumina film on sapphire . .. . ........................................................ 1 16
Figure 39. A plot of displacement versus time response to 80 mN step load for
sapphire
. ........................................................................................................
1 17
Figure 40. A log-log plot of indentation strain rate versus hardness for sapphire . ........ 1 1 8
Figure 4 1 . A plot of hardness versus homologous temperature for In over the
homologous temperature range of 0.4 to 0.8 . ................. .............................. 1 20
Figure 42 . A plot of natural log of indentation strain rate at constant values of
hardness versus the reciprocal absolute temperature for In . ......................... 1 22
xvi
Figure 43 . A log-log plot of temperature compensated indentation strain rate

versus hardness for 28, 50 and 75C experiments on In. .............................. 123
Figure 44. A plot of the shear modulus and Young's modulus of In as a function
of temperature[66] . ................................................................ ........................ 125
Figure 45 . A plot of the natural log of the indentation strain rate at constant
values of HlG and HIE versus the reciprocal absolute temperature for
In
..................................................................................................................
126
Figure 46. A plot of natural log hardness at constant time under load versus the
reciprocal homologous temperature for In . ................................................... 128
Figure 47. A plot of average hardness versus homologous temperature for Al
over the homologous temperature range of 0.31 to 0.56. .......... ................... 129
Figure 48. A plot of Young's modulus versus temperature for A1[40] . ......................... 132
Figure 49. Plot of dislocation density calculated from the Taylor relation by
replacing the normalized stress dependence,
relation with (Hl3E)
. . . ...........
alE,
of the Taylor
. . . . . . .. . ...................................
..
. ...... ..................
133
Figure 50. A log-log plot of temperature compensated indentation strain rate

(indentation strain rate divided by the effective diffusion coefficient)
versus HIE for AI. . . .
.
..
....................
. .
...
................................ . . . .............
..
....
. 135
.
Figure 51. A plot of indentation strain rate versus displacement for Pip change
experiments on In
. ..............
..
......
. ...
..
....
....
....
..
. . ............. ............................
138
Figure 52. A plot of hardness versus displacement for Pip change tests on In . ...... .... 139
Figure 53. A plot of stress versus strain from uniaxial compression experiments
run on Pb-65 at% In alloy at a variety of crosshead speeds . ...... ................... 142
Figure 54. A log-log plot of stress versus strain rate as a function of strain for
uniaxial compression tests on Pb-65 at% In . .......................................... ...... 143
xvii
Figure 55. A log-log plot of indentation strain rate versus hardness and uniaxial
strain rate versus stress at 10 and 80% strain for Pb-65 at% In . ................ ... 144
Figure 56. A log-log plot of indentation strain rate versus hardnessl3 .3 and
uniaxial strain rate versus stress at 1 0 and 80% strain for Pb-65 at%
In
..................................................................................................................
145
Figure 57. A log-log plot of indentation strain rate versus hardness for constant
Pip experiments on In plotted with tensile strain rate versus stress

data from Weertman[39] . ....... ... ............... ..................................................... 147
versus hardness for constant Pip experiments on In plotted with
temperature compensated tensile strain rate versus stress data on In
from Weertman[39] . . . .................................................................................... 148
Figure 59. A log-log plot of indentation strain rate versus hardness/3 .3 for
constant Pip experiments on In plotted with tensile strain rate versus
stress data from Weertman[39] . .................................................................... 149
Figure 60. A plot of the Bower factor[76] for relating indentation strain rate to
uniaxial strain rate versus stress exponent for creep . .................................... 1 5 1
Figure 6 1 . Log-log plot of indentation strain ratelBower factor versus hardness
for constant Pip experiments on In plotted with tensile strain rate
versus stress data from Weertman[39]. .............................. ........................... 1 52
Figure 62. A log-log plot of indentation strain rate divided by the effective
diffusion coefficient versus HIE for Al plotted with bulk data
obtained in torsion and tension from Luthy et al[40] . ................................... 1 54
XVlll
Figure 63 . A log-log plot of indentation strain rate divided by the effective

diffusion coefficient versus Hl3 .3E for AI plotted with bulk: data
obtained in torsion and tension from Luthy et al[40] and Trozera et
al [77] . ... ............... .............................. ......... ....................................... ............ 1 55
Figure 64. A plot of a typical load time history for constant contact area/variable
frequency experiment conducted on polyisoprene. .. . ... .......... .................... ... 1 70
Figure 65. A typical plot of load versus displacement for polyisoprene during
constant contact area/variable frequency experiment. ......... ......................... 1 74
Figure 66. A log-log plot of dynamic compliance, h1F, versus radial frequency
showing response of free hanging indenter as well as the response of
the indenter in contact with polyisoprene under conditions of three
different constant contact areas . ....... ............................................................. 1 75
Figure 67. A semi-log plot of phase angle, $, versus radial frequency showing
response of free hanging indenter as well as the response of the
indenter in contact with polyisoprene under conditions of three
different constant contact areas. ....................... ............ ...... ............. .............. 177
Figure 68. A log-log plot of stiffness, S , and damping, COl, versus radial
frequency for polyisoprene under conditions of constant contact area . ........ 1 78
Figure 69. A plot of the storage modulus, G', and loss modulus, Gil, as a function
of radial frequency for polyisoprene under conditions of constant
contact area. ............ ............... .............................................................. ......... 1 79
Figure 70. A plot of dynamic compliance versus absolute displacement of
capacitive plate in gap for conditions of no contact between the
indenter and sample and conditions of increasing contact area
between indenter and polyisoprene . .................................... ................. ........ . 1 8 1
xix
Figure 7 1 . A plot of the phase angle versus absolute displacement of capacitive

plate in gap for conditions of no contact between the indenter and
sample and conditions of increasing contact area between indenter
and polyisoprene
. .....
. .. . . . . .. ..
...
. ..
..
..........
...
.
. .........
..
. ..
...... .
....
. . .. ..
... .
.......
Figure 72. A plot of contact stiffness, S , versus displacement for polyisoprene ...
. ..
. . 1 82
..
..
......
1 84
Figure 73. A plot of the contact damping coefficient, C, versus displacement for
polyisoprene . .
.
....
...............
....
. ....
.
....
.......
. . . .. .
..
...
..
.. .........
. . . .
..
..
..
.......
.. .
... .....
1 85
Figure 74. A log-log plot of the storage modulus, G', and loss modulus, Gil, of
polyisoprene as a function of radial frequency showing data from
constant contact area/variable frequency experiments and constant
frequency/variable contact area experiments
. .
. ... ...
.....
.....
. ..
...
........
. . . . . . 1 86
..
.. ..
Figure 75. Log-log plot of dynamic compliance versus radial frequency for the
Nano Indenter II free hanging indenter.
...
...........
. . ... . ..
...
......
.......
. ..
..
....
. .199
Figure 76. A plot of Nano Indenter II support spring stiffness as a function of

the absolute position of the indenter with respect to the capacitive
displacement gauge.
... .....
...... .. . ..
..
.. .
....
..
.....
. .. . ....
..
..
.......
.. .
...
.......
....
. . ..
..
..
....
20 1
Figure 77. A plot of Nano Indenter II damping coefficient as a function of the

absolute position of the indenter with respect to the capacitive
displacement gauge
. ....
.. . . .... .
.
..
..
..
.........
. . ..
.
..
..
...... .
...........
..........
. . .
..
..
........
...
202
Figure 78. A schematic of the components of the HTMPM for consideration in

the dynamic model.
. .. . .
............ ..
.. .
.....
. .. .
..
. . . . ... . .
.. ......... ..
..
. .
. . .
.... ..
..
.....
.........
205
Figure 79. A plot of displacement versus time showing free vibration of

HTMPM indenter in response to step load .
.....
. . .. . . .
...
..
..
....
. .. . . . ..
...
..
..
.. .
........
207
Figure 80. A plot of cycle number versus time yielding the damped natural
frequency of the HTMPM indenter mass, spring, dashpot system . . . . .
.
xx
..
. .....
208
Figure 8 1 . A plot of the absolute peak: displacement of the HTMPM indenter

versus time during free vibration showing exponential decay of the
vibrational amplitude
...................................................................................
209
Figure 82. A plot of displacement versus time showing free vibration of the
HTMPM specimen stage in response to a step load
.............
..
.....................
21 1
frequency of the HTMPM stage mass, spring, dashpot system
. ...........
..
.
.....
212
Figure 84. A plot of the absolute peak: displacement of the HTMPM stage versus
time during free vibration showing exponential decay of the
vibrational amplitude
............
.....
.................. ....................... ..... ......... . . .
.....
213
Figure 85. A plot of amplitude versus frequency for forced vibration of the
HTMPM specimen stage
. .............
....................................... . .....
..................
215
Figure 86. A plot of (Xindenter-Xstage)lXstage showing predicted response

calculated from dynamic model solution for contact conditions
determined from %Step Load Experiments
.................................
...............
22 1
Figure 87. A plot of the optically measured contact area divided by the contact
area calculated from total depth of the indent and the perfect
Berkovich indenter area function as a function of loading time for In .
.
.....
. 223
.
Figure 88. A plot of the optically measured contact area divided by the area
calculated from total depth of indent and perfect Berkovich indenter
geometry as a function of homologous temperature for AI. ... . .. . . . . .... . . . . . . . . . . . 224
xxi
List of Tables
Table ( 1 ). Summary of Stress Exponents Determined for Indium
....
............... ..........
Table (2). Range of temperatures for indentation creep of Aluminum . . .

.
Table (3). Summary of dynamic constants for the Nano Indenter
IT
..
..
............ ......
1 05
1 12
obtained
from fit of equation (64) to the dynamic compliance versus radial

frequency
....................................................................................................
1 99
Table (4). Coefficients of third order polynomial fit to the Nano Indenter IT
support spring stiffness as a function of absolute position within the
capacitive gap . ... ............................ .............................................................. 203
Table (5). Coefficients of fourth order polynomial fit to indenter damping
coefficient as a function of position within the capacitive gap . ..... ............. 203
Table (6). Summary of dynamic constants for HTMPM indentation head . .................. 206
Table (7). Summary of dynamic constants for HTMPM specimen stage
xxii
. .. . . .
.. . .
..
..
........
210
Chapter 1 Introduction
1. Introduction
The purpose of this study is to contribute to the understanding of how to use
depth-sensing indentation techniques to measure the time and temperature dependent
mechanical properties of materials. The basis for all studies of mechanical properties is
the response of a material to an applied force. This response can generally be thought of
as occurring by three different means: ( 1 ) elastic (recoverable) deformation where the
strains are nearly instantaneous ; (2) elastic deformation where the strains are not
instantaneous but rather depend on time and/or temperature, and; (3) plastic deformation
where the material undergoes non-recoverable strain the extent of which may depend on
time, temperature and the prior strain/time history the material has undergone. As the
problem of measuring time insensitive elastic and athermal plastic phenomena using
depth-sensing indentation techniques has been addressed by previous authors [ I -3], it is
the study of time and temperature dependent mechanical properties that will be the topic
of this work.
The techniques for the measurement of time dependent phenomena can be
conveniently divided into two classes: ( 1 ) broad-band, quasi-static or creep techniques
where the load, stress or strain-rate is held constant for a period of time ranging from
seconds to hours while the response of the material is monitored, and; (2) frequency
specific dynamic techniques where the load or stress is varied at a single frequency and
the response of the material is measured. While standard bulk testing techniques exist
for these types of measurements, in many instances the volumes of material of interest
may be on the scale that bulk techniques become impractical. Such is the case in the
thin film devices found in the microelectronics industry, the protective coatings and
aesthetic finishes found in the automotive industry, the adhesives and backing materials
found in the paper industry, the skin effects due to the solidification process in injection
molded thermoplastics, the surface layers formed by techniques such as ion implantation
or irradiation , the individual cell walls in trees or even the diseased arterial tissue found
within the human body, to name just a few. While in some of these cases specimens
may be prepared in a form that allows testing with standard uniaxial techniques, these
preparation processes may be very tedious or in some instances may very well alter
those properties that are of interest. It then becomes necessary to find an alternate
means for mechanical characterization. Depth-sensing indentation testing has proven to
be a reliable technique for measuring many of the important mechanical properties of
such small volumes of materials.
In this work, a variation of both the broad band, quasi-static and frequency
specific dynamic techniques described above will be utilized to measure both time
dependent plasticity or indentation creep at several temperatures and time dependent
elasticity or viscoelasticity at room temperature.
1.1 Time Dependent Plasticity - Creep
1.1.1 Introduction
The goal of this study of indentation creep is to explore the dependency of the
indentation stress, or hardness, as measured using depth-sensing indentation techniques,
on the variables of strain rate and temperature as well as to investigate the existence of a
steady state behavior in indentation creep.
These relationships have been very
thoroughly studied in bulk materials and are fairly well understood.
One equation used to describe the behavior of materials under creep conditions is
e = AcT'
where e and
CT
(1)
are the strain-rate and stress, respectively. The quantity n i s known as
the stress exponent for creep. When a material behavior is well described by this
equation using a constant value of n, the phenomenon is referred to as power law creep.
The stress exponent of the steady state creep rate in pure metals at elevated temperatures
(T
>
0.5Tm) in many cases has a value of about 5 [4] . The maj ority of indentation creep
work has centered around measuring the strain rate dependence of the hardness at room
temperature. Here, analogies are typically drawn between a uniaxial flow stress and the
hardness, and the uniaxial strain rate is related to the instantaneous displacement rate of
the indenter divided by the instantaneous displacement, a quantity known in the
literature as the indentation strain rate. Using these analogies, an attempt is made to
gain information into the stress dependence of deformation, i.e., the stress exponent for
creep.
Reasonably good agreement has been found between the stress exponents
measured with depth-sensing indentation and those measured using uniaxial techniques
although questions still exist about the appearance of deviation from power law behavior
at lower than expected strain rates.
1.1.3 Mechanisms of Creep

At temperatures above 0.5 Tm, creep in pure metals for which dislocation glide is
easy is thought to be controlled by the climbing of dislocations out of their glide planes
to overcome obstacles to motion. The climb velocities are limited by the rate at which
vacancies can diffuse in the material.
As such, creep at elevated temperatures is
expected to follow an Arrhenius type of behavior of the form
(2)
where Q is the apparent activation energy for creep, R is the gas constant and T is the
absolute temperature and the remaining variables are as previously defined. A semi-log
plot of strain-rate versus Iff will then yield the activation energy for the rate controlling
mechanism. The apparent activation energies for high temperature creep in pure metals
as determined by uniaxial techniques have been shown to be in general agreement with
the activation energy for self diffusion[5]. Using the same analogies for stress and strain
rate described above, the temperature dependence of indentation creep has received
limited attention, mainly being investigated through the use of impression creep
experiments at elevated temperatures using a flat-ended punch or hot hardness tests
where hardness as a function of dwell time under load has been measured[6- 1 3] .
Another concept developed to describe the creep process i s the idea of a steady
state microstructure. At a given temperature and stress, given enough time, there is
strong evidence that a steady state strain rate and microstructure can be reached in some
materials[ 1 4]. Any perturbations in these parameters will typically result in a transient
period of time during which the microstructure will evolve to a new state representative
of the new set of conditions. Following this transient period, steady state conditions can
again be reached. Experimental evidence has shown that the microstructure that is
developed in a given metal undergoing steady-state creep is independent of its previous
work-hardened or pre-crept condition and depends only on the value of the steady-state
stress[ I 5]. The notion of a steady-state stress or microstructure during indentation creep
tests incorporating a sharp indenter has not been investigated to date due to the lack of a
test technique capable of yielding a constant indentation strain-rate. A new technique
which allows the indentation strain rate not only to be controlled but varied
systematically is introduced in this work. This type of test makes possible, for the first
time, the investigation of a path independent steady state being reached in an indentation
test.
1.2 Time Dependent Elasticity . Viscoelasticity
1.2.1 Introduction
The goal of this study of viscoelasticity is to attempt the first quantitative

measurement of viscoelastic properties using dynamic depth-sensing indentation
techniques. The object of a phenomenological study such as this is not to discover the
relaxation properties in a complete fashion, but rather to be able to predict behavior
under certain circumstances having observed it under others.
According to McCrum et al or Nowick and Berry [ 1 6, 1 7], if the stress is

expressed in complex form,
(3)
where
0"0
is the stress amplitude and
strain is given by
is the angular frequency, then the complex
(4)
where
ro
is the strain amplitude. The stress-strain relationship for such a material may
be expressed as
..
Gr
'*
'*
=
(G '-iG ) r
..
(5)
"
where
G' (m) Gol

Irl
=
Gol cosl/J
Iro
(6)
is the storage modulus of the material and
Gil (m) Gol

In
=
Gol sin l/J

Iro
(7)
is the loss modulus of the material. More detailed information concerning this type of
material behavior may be found in the literature review section of this work.
A variety of bulk techniques incorporating either a quasi-static or a dynamic
mechanical testing technique exist for measurement of these properties. Recent efforts
to measure these properties using both Surface Force Apparatuses[ 1 8 , 1 9] and Atomic
Force Microscopy[20] have been made. While a limited amount of qualitative work has
been performed using dynamic contact techniques a quantitative model has not been
developed due to these systems inabilities to accurately determine the contact area
between the tip and the sample or the net applied strain amplitUde. This work represents
the first attempt at measuring the viscoelastic properties of materials using a depth-
sensing indentation system where a precise knowledge of both the contact area and the
applied force are known.
1.2.3 Mechanisms of Viscoelastic Behavior

Unlike phenomenological theories , molecular theories attempt to explain the
relaxation behavior of polymers in terms of proposed mechanisms for the motions of
polymer molecules [ 16]. The mechanisms of viscoelastic behavior differ greatly not only
from material system to material system, but within a specific material system as well
evidenced by the fact that most polymers exhibit more than one mechanical
relaxation [ 1 6] . There are three theories that are typically considered to be generally
applicable to a wide range of polymer systems: (I) the large scale motions of a polymer
chain in a viscous medium; (2) the interaction of a moving unit with a neighboring unit
by means of jumping across a potential energy barrier from one equilibrium position to
another; and, (3) local mode theories which consider relaxations resulting from damped
oscillations of molecular groups close to their equilibrium positions. While not a
specific topic of this work, a brief discussion of these phenomena is included in the
review of the literature.
Chapter 2 Review of Literature
2. Introduction
An important aspect of any scientific endeavor is to understand the work that has
been performed by other authors in the subject area and to use this knowledge as a
rational starting point for further work. As the goal of this work is to further the
understanding of how time and temperature dependent properties measured by means of
depth-sensing indentation can be compared and related to those same properties
measured using standard bulk techniques, this review of literature is intended to acquaint
the reader with the current base of knowledge in the areas of mechanical properties that
are pertinent to the work at hand and entails a review of the fundamentals of timedependent plastic and elastic behavior and the techniques and models that currently exist
for their measurement and understanding. This review is by no means meant to be a
complete review of the field of the study of mechanical properties, instead readers are
urged to consult the numerous excellent documents referenced herein for more detailed
information about any of the specific areas that may be of interest.
2.1 Time Dependent Plasticity - Creep
2.1.1 Introduction
The progressive deformation of a material at constant stress is called creep [2 1 ] .
Central t o the understanding of creep properties i s the dependence of the creep rate on
the variables of stress and temperature[22] or conversely the dependence of the creep
stress on the variables of strain-rate and temperature. These relationships have been
very thoroughly studied in bulk materials and
are
fairly well understood. A third idea
central to the understanding of the creep process is the development and role of the creep
microstructure. This review will focus on the fundamentals of these three parameters.
2.1.2 Review of Uniaxial Literature
2.1.2.1 Effect of Stress
Power-Law Creep
The central idea of power law creep is that the creep rate, e , at a given
temperature depends both upon the applied stress, cr, and at least one strength factor, 't':
(8 )
e = t(O', "C) .
Under constant stress, the creep rate depends on how the strength parameter changes in
the course of creep. B ailey[23] and Orowan[24] have suggested that strain hardening
and recovery serve to increase and decrease the strength respectively and that at steady
state the rate of hardening is equal to the rate of recovery [25] and propose an
evolutionary law for the strength parameter during creep of the form
(9)
By taking into account the appropriate expressions for hardening and recovery, it is
possible to arrive at the Dom equation that expresses the correlation of creep rates
among various metals as a function of stress and temperature[22] which can be

expressed as:
( 1 0)
where f(T) is the temperature dependence which will be considered in the following
section, G is the shear modulus , n is the stress exponent which is defined as dinEldlna at
a constant temperature and A is a parameter which accounts for any effects of structure
not explicitly included in the derivation of the Dom equation.
For certain pure metals under the appropriate conditions, n is generally found to
range from 4-6 with an average of about 5 . It is interesting to note that the actual
derivation of the natural creep law for diffusion controlled creep yields a power law 3
dependence rather than the power law 5 dependence as suggested from a large body of
experimental evidence[ 14] .
The appearance of the shear modulus in equation ( 1 0) is a factor that warrants
consideration. According to Sherby et al [26], the elastic modulus is the second of two
main principal factors (the first being the diffusion coefficient) influencing the creep rate
at a given level of stress. This factor is important because the speed of dislocation glide
and climb are strongly influenced by the elastic stress fields of dislocations obstructing
the path of moving dislocations. This hypothesis is demonstrated by a log-linear relation
between the steady state flow stress at a given value of e/ D , where D is the appropriate
diffusion coefficient, and the corresponding elastic modulus.
10
Power-Law Breakdown
Although high-temperature creep can often be described by a power-law creep

equation with a constant stress exponent of 4-6, this relationship is unable to
appropriately describe the creep response at low temperatures or high stresses. This
failure of the power-law creep equation is typically known as power law breakdown[27] .
According to Ashby and Frost[28], power law breakdown represents a transition
from a diffusion limited dislocation motion to an obstacle limited glide regime.
However, others have pointed out that this trend can perhaps be explained by
considering the effects of diffusion along dislocation cores[29]. It is possible to
empirically describe the phenomenon of power law breakdown using a hyperbolic sine
function of the form[30]
(1 1)
but this expression has not yet been derived from the consideration of mechanisms
involving dislocation motion.
2.1.2.2 Effect of Temperature
Creep is possible only because of thermal activation of deformation processes

and in the absence of thermal fluctuations, creep could not occur[3 1 ] .
It i s well
established that atom mobility, i.e., the diffusion coefficient, is of primary importance in
influencing the creep rate in metals above O.4T m.
This fact is convincingly
demonstrated by the equality of the activation energies for creep and lattice self
diffusion at temperatures above O.6Tm[32-34] and is supported by a large body of
experimental evidence as shown in Figure ( 1 ) which is a plot comparing the activation
11
tN,
GJ
0
,'
E
..,
::!:
mm3/mole
10
10
w/
>l!)
a:::
W
Z
2
aFt NI elFt
Mt 0
N ,Ct -:7t9Br
QC = QL
>
Zn
0.1
o - T I'-
.-
GJ
0
'"
1O f:
,'-Pb
e LI
..
<:J
Age,.
P
P.
N..
0.01
0 .01
")TI
N.
Z
0
C/)
:J
U.
U.
0
U.
...J
UJ
C/)
M,.,..,'At A9
.-
7'c.s" 6VC. .?
0
.-
.6A1203
Mo
Nb
Ta
...
uo ...."
/
'-AI
0.1
CRE E P ACT IVAT I ON ENERGY, Q c
,
10
M J/mole
Figure 1 . A comparison of activation energies for creep and self diffusion for a
wide range of materials. From Sherby[35].
Source:
O. D. Sherby and A. K. Miller, ASME Journal of Materials and
Technology, Vol. 1 0 1 , 1 979, 387.
12
energies for steady-state creep and l attice self diffusion for a l arge number of
materials[35] . The narrow temperature regime for which the correlation between power
law creep and diffusion holds for some metals led some authors such as Poirier[36] to
question the role of diffusion in power law creep and to suggest that nondiffusional
processes such as cross slip are more important. However, the evidence for diffusion
controlled creep remains strong for many metals and the description of high temperature
creep in terms of diffusion is far more complete and predictive than any other approach
yet devised.
Given that at temperatures above 0.5 Tm, creep in pure metals is thought to be
controlled by the climbing of dislocations out of their glide planes to overcome obstacles
to motion, the climb velocities are limited by the rate at which vacancies can diffuse in
the material. As such, creep at elevated temperatures is expected to follow an Arrhenius
type of behavior of the form
e. = eo
. exp(- Q)
( 1 2)
RT
absolute temperature. A semi-log plot of strain-rate at constant stress versus 1fT will
then yield the activation energy for the rate controlling mechanism. This temperature
dependence may conversely be presented in terms of the appropriate diffusion
coefficient, Le., the self-diffusion coefficient for pure metals, as
( 1 3)
13
where DL is the lattice self-diffusion coefficient, G is the shear modulus, b is the

B urger's vector and T is the absolute temperature.
In calculating the temperature compensated creep rate it is often necessary to
take into account the temperature dependence of the shear modulus in order to arrive at
an appropriate activation energy[37, 38]. It has been shown for a number of materials
that taking values at a constant stress rather than at a constant value of a/G(T) can lead
to overestimation of the activation energy for creep[39].
At lower temperatures, corresponding to higher stresses and strain rates, the
stress exponents for steady state creep become much greater than 5. In addition to
higher stress exponents, the activation energies for creep in this regime
are
lower than
those expected for lattice self diffusion. This observation has been explained by an
additional dislocation creep mechanism where transport occurs via dislocation core
diffusion[28] . This contribution can be accounted for by defining an effective diffusion
coefficient as
( 14)
where D c is the core diffusion coefficient and fc and fv are the fraction of atom sites
associated with each type of diffusion. The value of fv is essentially unity. The value of
fc is determined by the dislocation density, p, as fc
ac p where ac is the cross-sectional
area of the core. At high temperatures (>0.5 Tm ), the l attice diffusion contribution is
dominant (high temperature creep) while at intermediate temperatures (0.3-0.5 T m )the
core diffusion contribution becomes dominant (low temperature creep) .
This
mechanism has been observed as the dominant mechanism in high purity aluminum in
the temperature range 0.29 to 0.48 Tm by Luthy, Miller and Sherby[40].
14
One major limitation of the effective diffusivity concept is that it fails to provide
a natural explanation of the steadily increasing stress exponent in power-law
breakdown [27].
2.1.2.3 Formation of Steady State Microstructure

The final idea central to the understanding of the creep process is the
development and role of the creep microstructure.
The formation of subgrains
dominates the microstructural changes that occur during creep flow in most annealed
polycrystalline metals at temperatures above 0.4 Tm[32-34] . The first researchers to
observe the formation of subgrains were Jenkins and Mellor in 1 93 5 [4 1 ] .
An
explanation of subgrain development however was not proposed until the late 1 940's
when Wood and co-workers[42, 43] suggested that these cells were due to accumulation
of edge dislocations by climb (polygonization) leading to the development of low-angle
boundaries which are now universally called "subgrains."
The "cell" or subgrain structures that are associated with the creep process do not
form instantaneously, rather, they form gradually throughout the course of primary
creep[ 14]. During the initial stages of deformation, dislocations move through a well
annealed crystal at speeds approaching the speed of sound in the material[44] . During
this period of time, the dislocation density increases abruptly and the dislocations are
typically distributed in a homogeneous fashion[ 1 4] . This rapid deformation continues
until the interdislocation stresses approach the applied stress. If there were no thermal
activation, deformation would stop at this point. However, at elevated temperatures,
thermal activation allows continued dislocation motion past obstacles and deformation
can continue. Steady state creep coincides with the development of a steady state
substructure which is characterized by the condition that the average dislocation density
15
and the subgrain size remain constant with further creep strain [27].
These substructural changes that occur during the creep process are known to be
insensitive to temperature and to only depend on time and stress[22] according to the
relationship
( 1 5)
where A is the subgrain size, A is a constant equal to approximately 4 for a number of

materials but appearing to be a function of the stacking fault energy, b is the Burger's
vector,
cr
is the stress, and E is the temperature compensated Young's modulus. This
constancy of microstructure for a given level of stress has been shown by incorporating
stress-change tests where the applied stress is abruptly changed once the steady state has
been reached. The data of Horiuchi and Otsuka[45] as analyzed by Sherby, Klundt and
Miller[26] show that when the stress is suddenly decreased, an instantaneous drop in the
strain rate occurs where the rate of strain is below the steady-state value for the lower
stress. This significantly lower value of the creep rate is attributed to the finer subgrain
size developed at the higher stress. These data are shown in Figure (2). As further strain
is incurred, the creep rate is observed to increase. This increase in creep rate is
accompanied by an increase in subgrain size. Eventually a new steady state creep rate,
identical to the steady state creep rate at the lower stress, is obtained as the new subgrain
size for the low creep stress is attained. An increase in the creep stress is observed to
have the opposite effect as that observed in the stress-drop test.
Assuming the constancy of structure at a given level of stress, Sherby et al[26]
developed an equation which predicts the creep rate as a function of the subgrain size.
16
HiOh purity aluminum

683K
.....
'u
..
.08
CREE P
.16
.24
STRAIN
Figure 2. A plot of stress change data for Al from Horiuchi and Otsuka[45]
replotted by Sherby et al[26].
Source: O. D. Sherby, R. H. Klundt, and A. K. Miller, Met. Trans. A, 8A, 1 977,
843.
17
Based on the stress change tests as described above, Sherby et al arrive at a relationship
for the flow stress-instantaneous creep rate which pertains to a constant structure. They
find that the stress exponent, n, for constant structure creep tests is closer to 8 than to 5
as determined under conditions of constant stress. They summarize the instantaneous
constant structure creep rate for polycrystalline metals as
( 1 6)
where S is a constant equal to about 1 .5x 1 09 for high stacking fault energy metals and
all other quantities are as previously defined. Equation ( 1 6) is seen to reduce to the 5
power law equation normally given for describing the steady state creep rate of many
pure polycrystalline metals as the microstructural dependence is of reciprocal third order
dependence on stress.
2.1.3 Review of Indentation Creep Literature
2.1.3.1 Introduction
Since the flow stress of a material is a function of strain rate and temperature, the
hardness of a material should be expected to vary in an analogous way [ l O]. This fact
has led to numerous studies attempting to correlate the measured hardness or indentation
stress with the variables of time (or indentation strain rate) and temperature.
The techniques used to measure the time and temperature dependent properties
of materials with indentation testing may be divided into two classes: ( 1 ) conventional
microhardness and "hot hardness" experiments where an attempt to gain insight into the
time and temperature dependent properties was made by monitoring the optically
18
measured hardness as a function of dwell time under load and temperature, and; (2)
depth-sensing indentation techniques at both room and elevated temperatures where the
load on the indenter or the displacement of the indenter is controlled dynamically while
the other is monitored in such a way to define both an indentation strain rate and an
indentation stress or hardness.
2.1.3.2 Conventional Indentation Techniques

A s the techniques for measuring the time and temperature dependence of
materials using these techniques are quite often intermingled, this section of the review
will attempt to follow the chronological history of this technique rather than attempting
to separate the work into separate areas of time and temperature dependence. The
subject of microstructure will not explicitly be discussed in this section.
The earliest technique used in an attempt to gain information into the time and
temperature dependence of hardness was the hot hardness test. This type of test utilized
a standard micro indentation system modified to allow for elevated temperature
measurements. Experiments were typically conducted to study the effects of dwell time
and temperature on hardness.
One of the original works in this area was that of Mulhearn and Tabor in
1 960[9] . Starting with a power law equation for viscous creep they arrived at an
expression relating the measured hardness to time under load. For loading times
exceeding a few seconds they found, at any one temperature, a linear relationship
between log hardness and log time. This relationship was found to be independent of
temperature and the results were explained in terms of viscous creep.
Coincident to this work by Mulhearn and Tabor was an independent study by
Pomey and co-workers[46] that found evidence showing that the relationship between
19
log hardness and log time was in fact a function of temperature, the slope of a plot of log
hardness versus log time increasing with increasing temperature.
These conflicting results led to a study of the indentation hardness and the creep
of solids by Atkins et al in 1 966[ 1 0]. They began by reviewing the earlier study of
Mulhearn and Tabor[9] and stated that rather than use a steady-state creep equation, it is
more appropriate to use a transient equation of state due to the fact that the growth of the
indentation with loading time is determined by the rate at which the elastic plastic
boundary can diffuse into the specimen. Using an expression for transient creep from
Mott[47] developed for conditions of constant stress, Atkins et al arrive at an expression
relating the measured hardness to the time under load that is strikingly similar to that
obtained by Mulhearn and Tabor[9] . They assume that even though the expression of
Mott is explicitly for conditions of homogeneous deformation under conditions of
constant stress, it can be applied to an indentation test if the stress exponent is large and
the stress is not changing rapidly.
Atkins et al began by examining the creep response of indium using a variety of
indenter geometries.
An
important finding of their work is that the rate at which the
deformation proceeds, i.e., the rate of progression of the elastic/plastic boundary, does
not depend upon the geometry of the indenter unless the change in geometry i s
accompanied by a change i n the mode o f deformation. This leads them t o suggest that
the rate of deformation cannot be associated with the geometry of the indenter itself but
rather the rate at which the elastic/plastic boundary can diffuse into the material.
Atkins et al examined data from indium, lead, aluminum, MgO, and we
obtained by performing 1 second load ramps followed by holds under constant load at
P max for a variety of times. The load was then removed and the size of indentation
measured.
20
Atkins et al found a linear log hardness-log time relationship for longer loading
times but found that the slope of the line increases, i.e., there is a deviation from
linearity, for short loading times. In the linear region they find that the stress exponent
for creep, n, is approximately 1 0 for the stresses involved in hardness measurements.
Atkins et al also found, in accord with a number of other authors, that the slope of a plot
of log hardness versus log time increases with increasing temperature.
By analyzing the data according to their assumed equation of state, Atkins et al
c alculate an apparent activation energy for creep from the data at various temperatures.
They found values near that for self-diffusion for Sn (Trrm =O.54-0.78) and Al
(Trrm=O.64-0. 8 1 ). Atkins et al concluded that the observed hot hardness behavior
closely parallels the creep characteristics of the materiaL
A major problem associated with the technique of Atkins et al is that the result
depends on a measure of absolute time under load. An important question is how time
zero is appropriately defined, i.e., at the beginning of the loading segment or at the
beginning of the constant load segment as is done by Atkins et al. If the loading time is
short, the effects of the choice of time zero become less pronounced very quickly,
however, as Atkins et al point out, there seems to be a dependence of the result on the
rate at which the load was applied. This seems a logical result as the strain rate
experienced by the material will depend upon how the load was applied.
In another study of hot hardness data obtained under conditions of constant time
of loading, Larsen-Badse[ 1 1 ] determined "apparent activation energies for indentation
hardness" using a relationship of the form
( 17)
21
where H is the hardness, Q' is the apparent activation energy, and T is the absolute
temperature. From the values obtained for 23 pure metals, Larsen-Badse concluded that
the apparent activation energy for the hot hardness tests was proportional to but not
equal to the activation energy for self-diffusion or steady-state creep.
The data of Larsen-Badse were subsequently reanalyzed by Sherby and
Armstrong [ 12] who show that rather than an expression such as equation ( 1 7) as used by
Larsen-Badse[ l 1 ] , an expression of the form
( 1 8)
where QL is the activation energy for self-diffusion and n is the stress exponent for creep
is more appropriate. Comparison of this expression with that of Larsen-Badse reveals
that the apparent activation energy obtained by Larsen-Badse is equal to the activation
energy for self-diffusion divided by the quantity nR. Since n=5-7 for pure metals at
elevated temperatures and R
2 CalIK mol, QL is roughly 1 0- 14 times Q' which agrees
well with the experimental results.

Sherby and Armstrong go on to analyze the hot hardness data in terms of the
creep characteristics of pure metals. They begin by introducing an expression for the
temperature dependence of the hardness that incorporates the temperature dependence of
the elastic modulus, E. This equation is then used to examine the hot hardness behavior
of Al and Cu at temperatures ranging from 0.55 to 0.95 Tm. They show that a plot of
log (HIE) versus the reciprocal homologous temperature, T mIT, shows two linear
regions with a break at 0.75 Tm. At temperatures greater than 0.75 Tm, they find
activation energies nearly equal to those for self-diffusion in the two materials.
22
Sherby and Armstrong associate the break in the curve of log
(HIE) versus log
(TmlT) with the onset of power-law breakdown behavior based on an analysis of the
average strain rate occurring under the indenter and the high temperature diffusivity.
They premise this argument with an important statement, that the strain rate in a
hardness test is not constant. They assume that an average strain rate can be defined
by considering that a characteristic strain of about 1 0% for a Vickers indenter occurs

during the 30 seconds during which the load is applied. (The idea of defining a
characteristic strain rate based on the time under load and a characteristic strain will be
subsequently discussed further in light of this study.) B ased on this analysis and a
typical high temperature diffusivity, Sherby and Armstrong arrive at a value of e I D ,
where D is the diffusion coefficient, o f 109 , a value where they claim power-law
breakdown is observed to occur for most metals.
Two conclusions are drawn by Sherby and Armstrong from these results
regarding the hot hardness testing of pure metals . B etween 0.75 and 1 .0 Tm, the
deformation process is associated with lattice self-diffusion and creep flow in the power
law region. Between 0.5 and 0.75 Tm, the rate determining process is associated with
dislocation pipe diffusion and creep flow in the power law breakdown region. It is
important to bear in mind that implicit to their determination of activation energies is the
assumption of a constant value of 5-7 for the stress exponent for creep at elevated
temperature in pure metals.
In the most recent analysis of hot hardness testing by Sargent and Ashby [ 1 3 ] , a
variety of analysis techniques are outlined by which the stress exponent for creep and
the apparent activation energy for creep can be determined.
Sargent and Ashby begin by performing a dimensional analysis of creep
indentation from which several analysis techniques can be surmised. According to
23
Sargent and Ashby, when an indenter is pressed into a "hot" surface, it penetrates the
material first by yielding and subsequently by creep. The load on the indenter, P, is
carried by a projected contact area, A, such that the indentation pressure, H =PIA. The
stresses cause the material to creep and the indenter penetrates the material. As the
deformation proceeds, the pressure is reduced as the contact area grows. S argent and
Ashby derive a relationship for the hardness as a function of time of the form
( 1 9)
where
(20)
0'0
and C are constants, t is the time under load, and n is the stress exponent for creep.
The stress exponent for creep can be determined by one of a number of methods
from the S argent and Ashby analysis. From equation ( 1 9), the slope of a plot of log
(H/G) versus log time is - lin. If this equation is appropriate, the data should be a family
of straight lines with a change in slope being accounted for by the dependence of the
stress exponent on temperature.
Alternatively, differentiation of equation ( 1 9) gives the rate of indentation in
terms of the time rate of change of the hardness as
1 dH
=
H dt
1
nt
(2 1 )
24
such that a plot of log ( l1H dHldt) versus log time superimposes all of the data for one
material on a master curve having an intercept of lInt at the specific value of t.
The apparent activation energy of the creep process is determined either via a
plot of In(HlG) versus (TlTm) at constant time having a slope of Q/nRTm or conversely
by a plot of In time versus (TmIT) at constant (HlG) having a slope of QIRTm which
suggests a constant structure.
Sargent and Ashby apply their analysis to hot hardness data for Armco iron and
copper. Reasonably good agreement between the stress exponent for creep and the
activation energy obtained from their analysis and that obtained from uniaxial data for
the iron is obtained. The large scatter in the indentation data for the copper prevented
any conclusions from being drawn from that analysis.
One potential problem associated with the analysis of Sargent and Ashby is that
the stress and displacement fields beneath the indenter are assumed to be self-similar as
the deformation proceeds and to change only in scale and not in shape. This would not
seem to be entirely true as the basis for this analysis is that
as
the deformation proceeds
the stress and strain rate are changing in such a way that the relationship between the
two is related to the stress exponent of the material. The stress and displacement fields
might be expected to vary as the deformation proceeds due to these changes.
2.1.3.3 Depth Sensing Indentation Techniques
Introduction
The use of depth-sensing indentation techniques to study the time-dependent

properties of materials is an area of recent undertaking, having only seen a large amount
of work within the last l O years. The majority of this work has concentrated on
25
measuring the relationship between the hardness and an experimentally defined

indentation strain rate. While a limited amount of work has been performed at elevated
temperatures to investigate the temperature dependence of the indentation creep process,
the majority of the work has been at or below room temperature[48] or utilized a flat
ended punch[6] rather that a geometrically similar indenter.
Effect of Stress
There are four types of tests that have been employed using depth sensing
indentation systems to gain insight into the relationship between the indentation strain
rate and the indentation stress or hardness: indentation load relaxation (ILR) tests[49,
50] , constant rate of loading ( CRL) tests[5 1 , 52] , constant load hold indentation creep
tests[53-58] and impression creep tests[6, 8].
Indentation Load Relaxation (ILR)
The idea of using ILR techniques was first presented by Hannula et al[49] . In
this type of experiment, an indenter is pushed into a sample surface with the aid of a
crosshead. When the desired load or displacement is achieved, the position of the
indenter is fixed. Load relaxation occurs by conversion of the elastic strain in the
machine and the specimen into plastic strain in the specimen. This technique has been
used[50] to study time dependent deformation in small volumes. Using a Vickers
indenter with a 1 !lm2 flat area on the apex, an effective stress was defined as
(22)
where P is the load on the indenter and A is the projected area of contact. An effective
26
strain rate was defined as

.
E = Ch
where c is a constant,
(23)
it is the instantaneous descent rate of the indenter and h is the
indenter depth (total depth or plastic depth), The stress-exponent for creep is then
defined as d in e / d in H at constant temperature.
Constant Rate of Loading (CRL)
The constant rate of loading (CRL) test is a multi-indentation test that was
developed for determining stress exponents using depth sensing indentation systems[5 1 ,
52] . This type o f test utilized the ability of the Nano Indenter t o incrementally apply
the load on the indenter at rates specified by the experimenter. In a CRL test, the
indenter is loaded at a constant loading rate until the indenter has reached a prescribed
depth in the material. A complete series of experiments would involve this procedure
utilizing a different loading rate for each indentation made and calculating an effective
stress for that loading rate from the applied load and the achieved depth. The stress
exponent for creep is then defined in an analogous way as d In e / d in H ,
The significant problem associated with performing experiments in this fashion
is that the indentation strain rate is continually changing throughout the loading
segment. While the changes in the stress and strain rate may be small, this type of
experiment is nonetheless a far more dynamic test than the others.
27
Constant Load - Hold
The idea of measuring creep properties of materials with depth-sensing

indentation systems under conditions of constant load was first introduced by Pollock et
al[53] . Following the ideas of Atkins, Silverio and Tabor[ 1 0] , Pollock makes the
approximation that the strain rate, t. , as predicted by any physical model for creep,
should scale according to
h
8. = k2 -h
where
(24)
is the instantaneous descent rate of the indenter, h is the instantaneous
displacement and k is a geometric constant. Using this analysis Pollock investigated the
time dependent response of Ni films on Si at room temperature.
Mayo and Nix developed a similar technique for determining time dependent
properties with the Nano Indenter [54, 55]. Their experimental procedure involved
loading the indenter at a high loading rate and then holding the load on the indenter
constant and monitoring the displacement of the indenter as a function of time. Since
the contact area changes as the indenter penetrates the material while the load is held
constant, the hardness or effective stress changes as the test proceeds. This allows one
to obtain several effective stress-effective strain rate pairs from one indentation
experiment.
Raman and Berriche[56, 57] utilized this technique to investigate the creep
behavior of sputtered Sn and Al films on Si. They found that the stress exponents
obtained from the indentation tests were in reasonable agreement with those obtained
from conventional uniaxial tests.
28
This technique was also used by Poisl et al [59] to empirically determine the
relationship between the indentation strain rate and the uniaxial strain rate as measured
for amorphous Se.
They found that at temperatures above the glass transition
temperature Newtonian viscous or power law 1 flow was observed ( i.e., the slope of a
plot of log hardness versus log indentation strain rate yields a straight line with a slope
of unity). Assuming that the coefficient relating the hardness and the flow stress,
0',
of
Se was equal to 3, i.e., H=3cr, the relationship between the indentation strain rate and the
uniaxial strain rate was determined. Poisl et al found that the coefficient relating the
indentation strain rate to the effective strain rate is equal to 0.09, or = 0. 09/ where
/ is the indentation strain rate as previously defined in equation (24).
This type of experiment suffers from the same problem however that the CRL
experiment experiences in that the indentation strain rate is continually changing
throughout the loading segment and the subsequent hold segment.
Impression Creep
As discussed above, one of the problems associated with the current state of
indentation creep testing with sharp indenters is that when the hardness decreases with
time, the stress driving the creep process also decreases and no steady state can be
achieved. To avoid these difficulties, Chu and Li[6, 8] proposed a new type of test for
bulk materials in which the shape of the indenter is changed from a sphere or pyramid to
a circular cylinder with a flat end. As the contact area remains constant during the test,
the punching or indenting stress is thus constant at constant load.
By incorporating finite element analysis, Yu and Li[60] show in a concurrent
paper that the effective Von Mises stress available for creep at any distance relative to
the punch radius is proportional to the applied punching stress. As a result, the steady
29
state impressing velocity is proportional to the punch radius, and has the same stress
dependence as the steady state creep rate. Using a power law constitutive equation, Chu
and Li therefore arrive at an expression relating the punch velocity to the effective stress.
Following a short transient period, they observe a "steady-state" velocity during which
the descent rate of the indenter is found to have the same stress dependence as that
observed during conventional unidirectional creep tests using bulk specimens for LiF
single crystals[7], succinonitrile crystals[6], and 8-tin single crystals[8].
The only significant drawback of this technique is that the volume of material
being deformed is essentially defined by the radius of the punch[7 ] . To perform these
experiments in such a way as to constrain the plastically deformed volume to shallow
depths it becomes necessary to use punches of smaller and smaller diameters. As the
size of the punch is decreased, the errors associated with the contact area of the flat
punch become more pronounced eventually limiting the useful range of the technique.
These problems can be overcome by using geometrical similar indenters such as a
pyramid or cone if a technique can be developed that allows a similar "steady-state" to
be reached.
Comparison of Indentation Techniques for Determining Stress Exponent
The ability of the above mentioned approaches to obtain consistent and

technique independent data has been examined by Stone and Yoder[48] in investigating
the rate dependent and rate independent components of the hardness of Mo. Using
constant load-hold, indentation load relaxation, and indentation rate change experiments,
they found that the strain rate sensitivity, m (where m= l In), was independent of the
method of measurement and in general agreement with values obtained from uniaxial
techniques
30
Effect of Temperature. Q
The temperature dependence of indentation creep data is an area that has

received little attention in terms of depth-sensing techniques due mainly to the inherent
difficulties in measuring the small displacements associated with the technique at
elevated temperatures. The work that has been accomplished has typically been
conducted around room temperature or using techniques that incorporate large
displacements such that the thermal effects become small in comparison to the creep
displacements.
The earliest investigations into the temperature dependence of indentation creep
were carried out using the impression creep test described previously. Yu and Li and
Chu and Li investigated the temperature dependence of the impression creep process in
LiF single crystals[7], succinonitrile crystals[6] and -tin single crystals [8]. They
reported activation energies for high temperature impression creep that were in good
agreement with the activation energies reported for high temperature uniaxial creep as
well as the activation energies for self diffusion.
Poisl et al[59] investigated the temperature dependence of the indentation creep
process using a Berkovich indenter by changing the ambient temperature of the
laboratory near room temperature in their investigation into the relationship between
indentation creep and uniaxial creep in amorphous Se. From the Newtonian portions of
the curves of log hardness versus log indentation strain rate they were able to calculate
an activation energy for the indentation creep process. Using the indentation strain rates
at a constant hardness, they obtained an activation energy of 495 kJ/mol which compares
favorably with the activation energy for viscous flow of 535 kJ/moL
Stone and Yoder[48] used an indentation system capable of operating in the 1 60298K temperature range to investigate the rate dependent and rate independent
31
components of the hardness of Mo. They reported activation volumes , v*, defined as
v* = 9kT / mH
(25)
where m is the strain rate sensitivity of the hardness, H. Using this technique they found
activation volumes in agreement with those reported in the literature given 50% typical
scatter in the data.
Indentation Steady State
A final concept developed to describe the creep process is the idea of a steady
state stress or strain rate and microstructure. At a given temperature and stress (or strain
rate), given enough time, there is strong evidence that a steady state strain rate (or stress)
and microstructure can be reached in some materials [ 14]. The onset of steady state
creep is believed to occur when the rate of hardening in the material is balanced equally
by the rate of recovery.
In an indentation test, the dynamics of deformation are very different than that
occurring in the previously described uniaxial creep test. The deformed volume of
material under the indenter is continually expanding to encompass previously
undeformed materiaL As the material strains under the indenter, the material underneath
the indenter is very often likened to an expanding cavity with a hydrostatic core where
no deformation is occurring and an expanding elastic/plastic boundary. The creep
process is believed to depend upon the rate at which the elastic/plastic boundary can
proceed into the materiaL The question then becomes what steady state entails in an
indentation creep experiment.
32
One indentation technique which has been shown to be capable of reaching a

steady state is the impression creep test. Using a flat cylindrical punch, which yields a
constant value of stress or indentation pressure, Chu and Li and Yu and Li show that a
typical depth versus time curve under constant load resembles a conventional creep
curve with both transient and steady state stages for LiF single crystals [7], succinonitrile
crystals[6], and -tin single crystals[8]. They state that the cause for the transient stage
is believed to be due to the development of a steady state plastic zone under the punch,
for example a sub grain or cell structure not very different from that developed during
conventional steady state creep. This hypothesis is supported by the subgrain formation
beneath the cleaved surface of a LiF single crystal after high temperature impression
creep testing.
The notion of a steady-state stress or microstructure during indentation creep
tests incorporating a sharp indenter has not been investigated to date due to the lack of a
test technique capable of yielding a constant indentation strain-rate. While much of the
previously discussed work using geometrically similar indenters has been conducted
under the assumption that the fact that the stress is changing only marginally during the
experiment does not greatly effect the results, no experimental evidence has been
obtained that verifies this hypothesis.
2.2 Time Dependent Elasticity - Viscoelasticity
2.2.1 Definition and Terminology

Viscoelasticity refers to time-dependent elastic or recoverable deformation[6 1 ].
Consider for example the simple example give by McCrum[ 1 6] where a weight is
suspended from a polymeric filament. The strain incurred as a result will not be
33
constant but will slowly increase with time at temperatures above 0 K. This effect is due
to molecular rearrangements in the solid induced by and proportional to the stress. If the
strains are small, on release of the stress, the molecules slowly return to their former
spatial arrangement and the strain simultaneously returns to zero. The mechanisms of
viscoelastic behavior differ greatly depending upon the material system, but are typically
ascribed to a viscous flow process that results in the measured strain lagging behind the
applied stress. The mechanical parameters defined to describe such a solid under stress
must therefore depend on time (and/or temperature which will not be discussed here).
In the consideration of viscoelastic behavior, two types of mechanical responses
may be considered: a broad band quasi-static response function where the material
behavior is observed over periods of several seconds and longer under conditions of
constant applied stress or strain, or a frequency specific dynamic response function
where the behavior of the material is studied over much shorter periods of time when a
periodically varying stress or strain is imposed on the system. It is a variation of the
dynamic response function that will be utilized in this work and will therefore be the
focus of this review.
Before beginning it should be pointed out that the phenomenological description
of viscoelastic behavior is well known and accepted in the polymer community and is
the subject of many excellent texts. A large part of the phenomenological review
contained herein is from McCrum[ 1 6] , Nowick and Berry[ 1 7], or Zener[62], all of
whom have done an excellent job in outlining the measurement of the dynamic
mechanical response of materials .
34

If a sinusoidal stress is applied to a viscoelastic solid, then the strain response
generally lags behind the applied force by some phase angle. This phase lag results
from the time necessary for molecular rearrangements in the material [ 1 6] . The dynamic
response function of the material is most conveniently described in terms of complex
notation[ 17]. Let the stress be written as
(3)
where
0'0
is the stress amplitude and OJ is the radial frequency of vibration (OJ=21tf,
where f is the vibrational frequency). The resulting strain will also be periodic in nature
and can be expressed in the form
(4)
where Yo is the strain amplitude and <I> is the angle by which the strain l ags behind the
stress or conversely Y1 is the amplitude of the component of strain in phase with the
stress and Y2 is the amplitude of the component of strain 90 out of phase with the
applied stress.
Consider first a perfectly elastic solid. A situation similar to that shown in
Figure (3) will exist where the resulting strain is exactly in-phase with the applied stress,
i.e., there is no damping and <1>=0. The ratio O'/Y then gives the shear modulus of the
material G.
Now consider a linear viscoelastic solid. Here the strain is time-dependent and
lags behind the stress by a phase angle <I> as shown schematically in Figure (4). For this
35
Elastic Material
..0
'-
--
..
CJ)
CJ)
Q)
'
Stress
- - - - - Strain
+-'
en
Time
Figure 3 . A schematic o f the strain response to
an
applied stress for a purely
elastic material. The strain is exactly in phase with the applied stress.
36
Viscoelastic Material
...
,
,
I
,
,
,
,
,
,
,
,
,
,
.-
.......
(J)
--
Stress
en
en
(])
:to...
.......
(J)
- - - - - Strain
<I> =t ro
"
"
,
,
,
I
I
I
Ti me
Filjure 4.
A schematic of the strain response to an applied stress for a
viscoelastic material. The strain lags behind the applied stress by a phase angle <\>.
37
case the ratio a/y is a complex quantity. Nowick and Berry [ l 7] and McCrum[l 6] define
this complex modulus, G*(ro), as
*
(G I -iG
..
)r
(5)
where
G (m )
I
ao/
Ir1
ao/ cos l/J

Iro
(6)
ao/ sin l/J

Iro
(7)
and
G " (m )
ao /
Ir2
where G' and Gil are defined as the storage and loss modulus respectively and are related
to the relaxed modulus, Gr, and unrelaxed modulus, Gu, measured in a creep response
experiment according to
(26)
and
(27)
where 't is the relaxation time under conditions of constant strain. At sufficiently low
38
frequencies, the strain will be proportional to the stress with the relaxed modulus as the
*
proportionality constant such that G (0) = G I = Gr .
At very high frequencies,
G ( 00) = G ' = Gu . The function Gil is a Debye peak that resides at the frequency where
roT
= 1 holds, i.e., at the resonant frequency of the mechanism.

The importance of the phase angle <p can be realized by calculating the ratio of
the energy dissipated and the energy stored in a cycle of vibration. This is often called
the specific loss[1 6] and is related to the phase angle <p by the relationship
(28)
Several indirect methods have frequently been employed for specific loss
measurements. These methods have been described by Zener[62], McCrum[ 1 6] and
N owick and Berry [ 17] and typically involve methods employing resonant systems
vibrating at a natural frequency either in forced vibration or in free decay.
One indirect method of measurement involves measuring the amplitude of
vibration under conditions of forced oscillation, the frequency of the excitation force
being slowly varied while the amplitude is held constant. The amplitude of the resultant
vibration will be a maximum when the excitation frequency is equal to the resonant
frequency of a specific defect within the solid. In this type of experiment, if Llm is the
change in the excitation frequency to change the amplitude from half-maximum on side
of the resonant peak to half-maximum on the other side, then
(29)
39
where Q- l is analogous to the definition of Q found in resonant electrical circuits and

corresponds to the sharpness of the resonance peak,
COr
is the resonant frequency of the
defect and <l> is again the angle of the phase lag. It is therefore observed that high
specific loss values correspond to low Q values and broad resonance peaks.
A second, indirect, method of measuring mechanical losses involves the
measurement of the energy per unit volume, t:,.W, dissipated per cycle of vibration.
Here, the energy of vibration, W, is defined as the strain energy per unit volume when
the strain is at a maximum. At this point the energy is entirely potential in nature and is
directly proportional to the square of the amplitude of the oscillation. A measure of the
decay of the oscillation in free vibration therefore gives an indirect measure of the
internal losses and is given by the logarithmic decrement, 0, where
(30)
w here A is the amplitude of the free vibration of the system and n is the number of the
vibrational cycle. The log decrement is related to the internal friction through the
relation
0 = n tan l/J
(3 1)
where <l> is, again, the loss angle between the applied stress and the resulting strain.
To summarize the relationships between the previously defined quantities, the
following relationships may be written:
t:,.W
= Q- l = tan l/J
2n W
(32)
40
where <I> is the loss or phase angle, Q- l represents the sharpness of the resonant peak, and
is a measure of the energy lost per cycle of vibration as defined by equation (29).
AWIW
The relationships between the specific values of the damping coefficient, C, and
stiffness, k, that are normally referred to in mechanical models and the parameters
and
Gil
G'
as defined in the dynamic response function for the system can be better
understood by considering once again the energy losses that occur in the system during a
complete cycle of vibration. The power absorbed by a damper responding harmonically
at a given frequency is proportional to the square of the amplitude[63], i.e.,
(33)
where C is a damping coefficient of a dashpot element in standard units of N s / m. The

total energy of the system can be calculated from the potential energy at the maximum
amplitude, i.e.,
W = kX2
(34)
where k is the stiffness of a spring element in units of N / m. From comparison with

equation (28) it can be noted that
1C
G"
Y6
oc 1C
Cm X2
(35)
and
41
(36)
or simply stated, the loss modulus, Gil, is proportional to the damping coefficient of the
material multiplied by the radial frequency and the storage or elastic modulus, G', is
proportional to the stiffness of the materiaL
These relationships will be further
expanded in the following section on measuring time-dependent elasticity from

indentation experiments.
2.2.3 Mechanisms of Viscoelastic Relaxation

While not a specific topic of this study, the mechanisms of viscoelastic
relaxation in polymers are important in aiding the understanding of the
phenomenological measurement approach taken herein. A brief general survey of the
different types of relaxation regions and relaxation mechanisms observed for solid
polymers is therefore in order.
In order to identify and compare the locations of loss peaks for different
polymers, the peaks are often labeled with the Greek letters
to this nomenclature, the
a.
a.,
, 'Y, etc. [ 1 6] According
loss peak corresponds to the relaxation observed at the
highe st temperature (at a given frequency) or the lowest frequency (at a given
temperature) [64] .
The most pronounced mechanical relaxation region for polymers in the
amorphous state is associated with the glass transition and occurs at temperatures at or
around the glass transition temperature, a region where the effective viscosity increases
rapidly for non-crystalline materials[6 1 ] . This transition is usually labeled
a.
and is
referred to as the glass-rubber relaxation[ 1 6]. From a molecular point of view, it has
been widely accepted for many years that the glass-rubber relaxation results from the
42
large scale rearrangements of the polymer chains occurring by rotations around main
chain bonds [ 1 6] .
Long chain polymers in the vicinity of their glass transition
temperature are capable of marked viscoelastic behavior, the viscous component of their
flow being involved with stress-assisted interchain sliding[6 1 ] .
I n addition to the glass-rubber relaxation, amorphous polymers usually exhibit at
least one secondary relaxation region. These secondary loss regions result from motions
within the polymer in the glass-like state. In this state the main chains are effectively
"frozen-in" so that these relaxations cannot be due to large scale rearrangements of the
main polymer chain. Since the molecules of most amorphous polymers contain side
groups capable of undergoing hindered rotations independently of the chain backbone,
these secondary relaxations are often ascribed to such rotations.
43
Chapter 3 Experimental Equipment
3. Introduction
The use of depth-sensing indentation techniques to measure a variety of
mechanical properties of small volumes of materials has seen vast expansion during the
past decade.
This has been made possible in l arge part due to advances in
instrumentation and techniques capable of accentuating specific material properties by

precisely controlling the load-time or displacement-time history of the experiment. Two
distinct instruments were utilized in this study. The first a Nano Indenter n, is a state of
the art commercial depth-sensing indentation system that is widely used in both industry
and research. The second instrument is a prototype high temperature depth-sensing
indentation system developed at the Oak Ridge National Laboratory. A brief description
of the Nano Indenter II system is followed by a more complete description of the new
prototype high temperature instrument.
3.1 Description of Nano Indenterll

Figure (5) is a schematic of the Nano Indenter II (Nano Instruments, Inc., Oak
Ridge, TN, 37830) used for the majority of the room temperature experiments. The
intricacies of the system have been detailed elsewhere [ 1 ] and will not be discussed here.
The indenter is supported inside the indentation head by two leaf springs designed to
limit the motion of the indenter column to only the vertical direction. The load on the
indenter is generated through the use of a current carrying coil and permanent magnet
assembly . The resolution of the loading system is 50 nN. The displacement of the
indenter is measured with a three plate capacitive system with a resolution of 0.04 nm.
44
c
,------r-- CURRENT SOURCE
OSCILLATOR
. .... LOCK-IN AM PLIFIER
J===:i1rlii==:r-......
DISPLACEMENT
SENSOR
o
Figure 5 . A schematic o f the Nano Indenter II . A-Sample;
B-Indenter Column; C-Load Application Coil; D-Indenter Support Springs;
E-Capacitive Displacement Gauge; and F-Load Frame.
45
The operation of the system and the acquisition of data is controlled through a personal
computer. Data is typically acquired at a rate of 3 load, displacement and time data
points per second.
The Nano Indenter II is typically operated in one of two modes; a constant
loading rate mode achieved by direct control over the load ramp or a constant
displacement rate mode achieved by means of a feedback loop between the calculated
displacement rate and the loading rate. In addition to these two modes of operation, the
system has the ability to apply step loads by a direct set of the digital to analog converter
(DAC) controlling the current to the load application coil.
3.2
Description of the High Temperature Mechanical Properties
Microprobe
3.2.1 Introduction
The High Temperature Mechanical Properties Microprobe (HTMPM) is an ultra
low load, ultra-high vacuum (UHV), high temperature, depth sensing indentation
system. A schematic of the system is shown in Figure (6). It combines the well
developed technology found in the current ambient temperature mechanical properties
microprobes[3] with the ability to perform similar experiments at temperatures ranging
from - 1 00C to approximately 300C. All functions of the system with the exception of
the temperature control of the indenter and specimen are controlled from a personal
computer and a Hewlett Packard (HP) 3852 Data Acquisition and Control Unit.
46
Zygo System
---- CURRENT SOURCE
Power Supply
Power Supply
Laser Pattern
Figure 6.
Microprobe.
A schematic of the High Temperature Mechanical Properties
A-Sample; B-Indenter; C-Load Application Coil; D-Indenter Support
Springs; E-Indenter Thermocouple; F-Indenter Temperature Controller; G-Indenter

Heater; H-Sample Thermocouple; I-Sample Temperature Controller; J-Sample Heating
Stage; K-Measurement Mirror; and L-Reference Mirror.
47
3.2.2 Loading System
The load on the indenter is generated via a coil and permanent magnet assembly
as in the Nano Indenter II. The load coil is rigidly attached to the indenter column and
resides in the gap of a permanent magnet.
The load on the indenter is varied by
changing the current through the coil. The voltage (current) is supplied via a I 8-bit
digital to analog converter (DAC) and a I 6-bit offset DAC. Four independent load
ranges are available which differ in maximum loading capability and load resolution.
The load resolution of the system is 1 .0 JlN. The voltage output of the load card is
monitored continuously during experiments, thus giving a constant measure of the load
being applied to the indenter.
3.2.3 Displacement Sensing System
The displacement measurement for the HTMPM is achieved through the use of
an Axiom 2120 He-Ne laser interferometric displacement sensing system
manufactured by the Zygo Corporation.
The complete interferometric system is
mounted above the indentation head outside of the vacuum chamber. The beams are
passed into the vacuum chamber through a strain-free sapphire viewport that is coated
for zero reflectance. Two of the beams from the interferometer strike a mirror that is
clamped between the indenter column and the indenter while the other two beams strike
a mirror that is rigidly coupled to the specimen. This is shown schematically in Figure
(6 K&L). This configuration allows for a direct measure of the displacement of the
indenter into the specimen with very little possibility for other contributions to the
displacement measurement. Laser measurement techniques are extremely well suited
for this type of application due to the inherent accuracy provided by interferometry and
the very high data acquisition rate available from the system.
48
In a typical interferometer, a monochromatic light source is passed through a

beam-splitter which transmits half of the beam to a moveable mirror and reflects the
remainder 90 to a fixed mirror. The two beams are then recombined and their
interference is observed. When one of the mirror is displaced the intensity of the
recombined beams will vary as the light waves from the two beams interfere by adding
and canceling. The cycle of intensity change of the interference of the recombined
beams represents a half-wavelength displacement of travel of the measurement mirror.
If the wavelength of the light is known, the displacement of the measurement mirror can
be determined. The accuracy of such a system can be further enhanced by utilizing two
frequency laser interferometric techniques which are found in the Axiom 2/20 system.
In a two frequency heterodyne system, the laser beam contains two frequency
components which differ in frequency by a fixed amount. In the Axiom 2120 system,
this is achieved by first polarizing the beam so that only one frequency is present and
then passing this single frequency beam through an acousto-optic frequency shifter
which transmits one-half of the beam unaltered while the other is diffracted at a small
angle and shifted up 20 MHz. One of these frequency components is used as the
measurement beam and is reflected from the moving indenter while the other frequency
component is used as a reference signal and is reflected back from a stationary mirror
that is rigidly coupled to the front of the specimen. These two beams are then
recombined and the interference between the 20 MHz beat frequency and the unaltered
beam are used to determine the change in displacement. Utilizing a double pass
interferometer thus yields a displacement resolution of 1 .25 nm.
Since the measurement update rate of the laser interferometer is determined by
the frequency of the measurement signal (20 MHz), the Axiom 2120 system is capable of
producing an updated displacement reading 2 million times per second.
49
Due to
hardware limitations, the rate at which data can be acquired from the system is limited
and displacement data are normally acquired at a rate of approximately 3 points per
second. However, it is possible to conduct dedicated measurements from the laser
system for very short periods of time in order to obtain displacement data at exceedingly
high rates. By passing data directly into an integer array into the data acquisition control
unit's mainframe memory, displacement data can be acquired at rates up to 1 90,000 data
points per second. A similar type of displacement reading into a real array yields a data
acquisition rate of 3700 data points per second. These "bursts" of displacement readings
can be performed at any time during the experiment, for example following a step-load,
without interrupting normal experimental flow and the data retrieved on experiment
completion. This very exciting feature of the measurement system gives the HTMPM
very unique capabilities not found in other mechanical properties microprobes.
3.2.4 Vacuum / Manipulation System
The HTMPM indentation system is completely contained within a DHV

manipulation chamber. DHV conditions are achieved through the use of four liquid
nitrogen sorption pumps for rough pumping of the system from atmospheric pressure
and two ion pumps and one titanium sublimation pump for further pressure reduction.
Typical operating pressure is = 1 0-8 Torr.
The manipulation system of the chamber allows for five independent axes of
motion of the specimen stage for laser alignment and specimen positioning . Visual
imaging of the specimen is done by rotating the specimen 90 about the x-axis to a long
working distance Questar telescope located outside the vacuum chamber. Positioning
of the specimen is achieved by a calibrated move from the focal point of the telescope to
the indenter.
50
3.2.5 Temperature Monitoring and Control
Temperature monitoring in the HTMPM is achieved through the use of two type
K thermocouples, one placed directly on the tip and one on the backside of the specimen
as shown in Figure (6). These thermocouples are monitored by two Eurotherm type 801
temperature controllers that output a PID (ProportionallIntegrallDerivative) control
signal to two independent programmable power supplies which in tum supply power for
tip and specimen heating. Heating is achieved through the use of a tungsten resistance
heater located just above the indenter and tantalum resistance heater located in the
specimen stage. Temperatures of less than ambient are achieved by flowing liquid
nitrogen or another cooling medium through cooling channels in the copper shroud that
contains the indentation head and the copper stage which supports the specimen.
51
Chapter 4 Developing a Set of Indentation Creep

Constitutive Equations and Defining Indentation Creep
Terminology
4. Introduction
As previously discussed in the literature review, the phenomenological

description of uni axial creep at intermediate and elevated temperatures is quite
complete. While very distinct differences exist between uniaxial and indentation testing,
analogies can be made between the two types of tests in order to aid in describing the
phenomenon of indentation creep. It is also necessary to define the terminology that
will be used to describe the indentation creep process. These topics are discussed in the
following sections.
4.1 Differences Between Uniaxial and Indentation Creep
4.1.1 Introduction
In attempting to compare the mechanical properties of materials measured by

different techniques, it is important to realize that quite often the measurement technique
itself may have a bearing on the measured properties. A few of the important questions
are: " Is the test a measure of steady state or transient properties?" ; "What is the stress
distribution? " ; "What volume of material is determining the measured response?" ;
"What is the geometry of the 'specimen' ?" A brief look at the differences between
uniaxial testing and indentation testing in light of these questions is in order.
52
4.1.2 Steady State versus Transient Behavior

The majority of uniaxial creep data presented and analyzed in the literature deal
with steady state creep, i.e., the relationship between stress and strain rate under the
conditions where the control variable is held constant and the dependent variable has
arrived at a constant value indicative of the imposed state variables. Uniaxial testing
typically imposes a constant stress (creep test) or a constant strain rate and then looks for
the other to become constant at large strains, i.e., the onset of steady state creep.
In
most types of indentation creep tests, the indentation strain rate, and therefore
hardness, continuously change during the experiment. For instance, in a constant load
creep test the indenter is loaded at a specified rate and the load is then held constant for a
period of time while the displacement is monitored. The indentation strain rate changes
both during loading due to the imposed loading rate and also in the subsequent hold
segment under constant load due to the decreasing pressure (hardness) as the contact
area increases. While these changes in the indentation strain rate and hardness may be
small, the actual response is being governed by the material properties that are of
interest. As the strain rate and hardness are constantly changing, the microstructure is
continually evolving. While the deformation under a pyramid shaped indenter has
typically been viewed as being geometrically similar from a time-independent point of
view, this type of test does not yield geometrical similarity from a rate-dependent point
of view. That is to say, as the deformation proceeds under the indenter, the strain-rates
experienced by geometrically similar portions of material change as the deformation
proceeds. It is therefore desirable to perform an indentation experiment during which
the indentation strain rate and therefore hardness remain constant.
53
4.1.3
Homogeneous Stress Distribution versus
Radial S tress
Distribution
While the uniaxial test yields a uniform distribution of stress on a macroscopic

scale, the stress available for creep under the indenter is known to scale as some radial
function away from the surface[6] . The strain rate in any given volume of material will
therefore depend on the local state of stress. As continuity must be preserved, it
therefore seems likely that there is some volume of material beneath the indenter that is
responsible for controlling the rate of deformation.
4.1.4 Constant Volume versus Expanding Volume

During plastic deformation in a uniaxial test, volume is always conserved[65] .
As previously discussed, in a uniaxial test, the microstructure evolves to a steady state
during the course of primary creep due to the non-uniform stress distribution on a
microscopic scale[ 14] . The onset of steady state creep is believed to be associated with
the point at which the further hardening of the material is balanced by the rate of
recovery. Any perturbations in the control parameter will typically result in a transient
period during which the microstructure will evolve to a new state representative of the
new set of conditions. Given enough time, steady state conditions can again be reached.
The arrival at a new steady state is believed to be representative of a new microstructural
state in the deforming volume.
In an indentation test, the deformed volume of material is continually expanding
to encompass previously undeformed material. The material underneath the indenter is
very often likened to an expanding cavity with a hydrostatic core where no deformation
is occurring and an expanding elastic/plastic boundary. The creep process is believed to
depend upon the rate at which the elastic/plastic boundary can proceed into the material.
54
In
contrast to the uniaxial test, the indentation creep process is therefore seen to entail an
ever increasing volume of material as deformation proceeds.
4.1.5 User defined Geometry versus Material Defined Geometry
Another central difference between uniaxial testing and indentation testing lies in
the geometry of the two tests. In any mechanical tests, forces and displacements are
controlled and/or measured depending upon the type of apparatus being used. However,
the displacement response alone of a sample to an applied force tells nothing of the
properties of the material without incorporating the geometry of the specimen.
In uniaxial testing, the geometry of the test is defined by the user. Specimens are
typically geometrically simple, e.g., a cylindrical compression specimen or a dog-bone
tensile specimen.
In
an indentation test, the geometry of the test is actually being controlled by the
very properties of the material that are of interest, e.g., the hardness, Young's modulus,
or strain rate sensitivity. The test itself is typically designed to examine the properties
that are of interest.
4.2 Analogy Between Indentation and Uniaxial Geometries
Figure (7a) is a schematic of a simple compression specimen along with a short

list of previously discussed equations to describe the mechanical response. The uniaxial
strain rate is defined as some characteristic change in size of the specimen as a function
of time, e.g., the displacement rate, divided by a characteristic length scale, e.g., the
length of the specimen. The stress that the sample will support is defined as the applied
force divided by the cross-sectional area of the specimen. Finally, the uniaxial strain
rate can expressed as a function of the microstructure, fuCA), the activation energy for
55
p
p
1
I dl
e. = -
I dt
uf =
I dh
e'. = -
H=
P;A
h dt
P;A
Bi = h( J,. )e-%T(
H )n
(b)
(a)
Figure 7. Geometric comparison of uniaxial compression specimen (a) and

indentation creep 'specimen' (b) and equations for describing each.
56
creep, Q,
and the stress exponent for creep, n.
Figure (7b) is the corresponding
geometrical representation for an indentation creep 'specimen.' It is possible to define an

indentation strain rate as some characteristic change in size of the specimen as a function
of time, e.g., the displacement rate, divided by some characteristic length scale, e.g., the
depth of the indentation[50, 5 1 , 53]. The mean stress or pressure that the 'specimen' will
support can be defined as the load divided by the contact area between the indenter and
the specimen, a quantity typically defined as the hardness of the material. Finally, the
indentation strain rate can be expressed as a function of the microstructure, fiO,,) , the
activation energy for indentation creep, Qi, and the stress exponent for indentation
creep, ni.
4.3 Definition of Hardness as Indentation Stress

The most general definition of hardness is that it is the equivalent of the average
pressure under the indenter, calculated as the applied load divided by the projected area
of contact between the indenter and the sample[ I ]. In a conventional microhardness test,
hardness is calculated by dividing the applied load by the projected contact area
calculated by measuring the diagonals of the hardness impression once the load has been
removed. As the scale of indentation testing samples has become increasingly smaller,
the need for the ability to obtain hardness data without the need for imaging the
indentations has become more prevalent. Depth-sensing indentation techniques can be
used to measure the hardness of a material without the need for post-imaging of the
indentation[ l , 3]. The hardness can be calculated as
= Pmax
(37)
57
where H is the hardness defined as the mean pressure the material will support under the
peak load, Pmax, and A is the projected area of contact calculated from the depth of the
indent (either the total depth or more typically the plastic or contact depth, see [ 1 , 3])
and a precise knowledge of the shape function of the indenter (the function relating the
depth of penetration to the projected cross-sectional area of contact).
In its simplest definition, hardness is typically thought of as describing an
athermal strength of a material. However, as the flow stress of a material is a function of
strain rate and temperature, the hardness of a material should be expected to vary in an
analogous way [ l O] . For this work, hardness will be defined as the instantaneous mean
pressure that the surface will support as calculated from the load divided by the
projected contact area. The contact area is calculated from the total depth of the indent
and the area function for the perfect Berkovich indenter except for the case of the
amorphous alumina film and sapphire where the contact area was calculated based on an
elastically corrected contact depth. The accuracy of defining the hardness based on the
total depth of the indent rather than an elastically corrected depth is discussed in
Appendix B . The hardness will be considered to be a function of the indentation strain
rate and temperature in a manner analogous to the flow stress in a uniaxial creep test.
4 . 3 "Steady State Indentation Strain Rate and Hardnesstt

The term "steady-state" is seen to appear throughout the review of uniaxial creep
in Chapter 2. It was pointed out that steady-state implies that at a given temperature, a
balance has been reached between hardening and recovery effects such that for a given
applied stress or strain rate, the resulting strain rate or stress is constant. Steady-state is
also typically thought to imply a constant microstructural state in the material.
58
In the literature review of indentation creep using depth-sensing indentation

techniques it was pointed out that a possible problem associated with the current state of
indentation creep testing with sharp indenters is that in none of the currently used test
techniques is the indentation strain rate,
iz/h, or hardness constant.
While it has been
pointed out by a number of authors that phenomenological descriptions developed for

constant stress can be used since the hardness is changing very slowly, this fact has
never been born out experimentally due to the lack of a test technique with a
geometrically similar indenter capable of performing a constant strain rate or constant
stress experiment.
59
Chapter 5 Indentation Creep - Materials/Sample

Preparation
5.1 Lead-65 at % Indium
Pb-65 at% In has a melting point of 468 K ( 195C). Its most common use is as a
corrosion resistant plating material and solder for glass and silicate materials [66] . The
alloy was chosen for study due to its low melting point and well characterized creep
characteristics [66].
The Pb-65 at% In alloy used for both indentation and compression testing was
prepared from commercially obtained Pb and In of greater than 99.999% purity. The
indentation specimens were prepared by rolling the homogenized alloy to approximately
0.75 mm and then annealing for 1 .5 hours at 1 70 C. The resulting grain size was
approximately 1 mm. The compression specimens were prepared by swaging an as-cast
3/8 " rod to 1 /4", homogenizing for 24 hours at 1 700 C, swaging to 118 " and then
machining to approximately a 3 :2 height to diameter ratio. The machined specimens
were then annealed 40 minutes at 1 00 C; the resulting average grain size was 50 ).Lm.
The surface was prepared for indentation testing by microtome polishing at room
temperature with a diamond knife.
5.2 Indium
Pure In has a melting point of 429.8 K ( 1 56.6C). Because of its bright color,
light reflectance and corrosion resistance, it is a valued plating metal, especially for
reflectors [67] .
Its creep properties are also well known over a wide range of
homologous temperature[39].
60
The indium specimens used for all indentation tests were prepared from
commercially available In of greater than 99.999% purity. Specimens were cast using
standard techniques to a thickness of 0.3885 ". The as cast material was then rolled to a
final thickness of 0.0825" before being cut to the final dimensions and subsequently
annealed at l OOC for 1 hour.
The surface was prepared for indentation by
electropolishing in a 3: 1 solution of methanol and nitric acid maintained at 20C. This

process resulted in a mirror finish surface with a final grain size of approximately 2-3
rnrn.
5 .3 Aluminum
Pure AI has a melting point of 933.5 K (660.4C). It is perhaps the most widely
studied of all materials in terms of its creep properties having been investigated by
numerous authors. It was chosen for this study for this reason as well as its interesting
creep behavior in the intermediate temperature range accessible with the HTMPM.
The aluminum specimens used for all of the indentation experiments were
prepared from commercially available AI of greater than 99.999% purity. Specimens
were cast using standard vacuum-arc techniques to a thickness of 0.2885", The as cast
material was then rolled to a final thickness of 0.0905" before being cut to the final
dimensions and subsequently annealed at 350C for 1 hour. The surface was prepared
for indentation using the method outlined in Oliver and Pharr[3]. Specifically, the
specimen was ground with successively finer grits of SiC abrasive taking care to remove
the damage layer at each step. The specimen was then polished for 8- 1 2 hours on a
vibratory polisher using 3 J.lm diamond paste and water on a TEXMETTM cloth followed
by 8- 1 2 hours using 0.5J.lm diamond paste and water on a MASTERTEXTM cloth. Final
61
polishing was performed using colloidal silica and a MASTERTEXTM cloth for 1 5-20
minutes.
5.4 A1zD3
Single crystal Ah0 3 has a melting temperature of 2030C (2303K). Alumina
ceramics are the most widely used oxide-type ceramic, chiefly because alumina i s
plentiful, relatively low in cost, and equal to or better than most oxides in mechanical
properties[67 ] .
The amorphous alumina film and sapphire were both chosen a s
examples of materials whose time dependent properties could only be characterized

using indentation creep techniques.
The amorphous alumina used for the indentation study was a 1 .9 Jlm thick
electron beam evaporated film deposited on a single crystal Al2 0 3 (sapphire) substrate
having its c-axis normal to the surface. Indentations were made in both the film and the
bare substrate in order to compare the time dependent properties of the two materials.
62
Chapter 6 Indentation Creep - Experimental

Techniques and Details
6. Introduction
A variety of experimental load-time histories are used at various times

throughout this study in an attempt to determine the most appropriate method for
measuring indentation creep properties. The experiment types are presented essentially
in chronological order. The reasons for the transition from one experiment type to
another will become clear as the results obtained from each are presented.
The
presentation of the data for any given material on which a number of different types of
experiments have been performed will follow this chronological order unless for the
sake of continuity it becomes cumbersome to do so. All of the load-time histories used
in this work will be presented in this chapter and referred to according to the experiment
type located in parentheses after each section heading.
Two other topics important to the results are the indenter geometry and the
problem of thermal drift in the experiment. These issues are discussed subsequent to the
presentation of the load time histories.
6.1 Load Time Histories
6.1.1 Step LoadIHold (Step/Hold)
Step loads are achieved in the Nano Indenter by multiplying the magnitude of
the step load required, P, by the reciprocal of the load calibration (e.g., V/JlN) to
determine the magnitude of the current change required in the load coil. The appropriate
63
information is then written to the digital to analog converter controlling the actual load
current.
A load-time history of a typical step load experiment utilized in this study is
plotted in Figure (8). In this experiment, the indenter was step loaded from the point of
contact to the desired maximum load after which the load was held constant and the
displacement monitored as a function of time. This type of loading enabled very high
displacement rates to be achieved during the first portion of the constant load segment.
Data was initially acquired at a rate of 3 data points per second during the initial rapid
descent of the indenter. The data acquisition rate was slowed to approximately one data
point every five seconds after the first fifteen seconds of the experiment. The hold
segment was continued until a specified minimum displacement rate was reached. The
indenter was then step unloaded to a load of 20 JlN, held at constant load, and then ramp
reloaded and ramp unloaded to obtain the elastic and plastic properties of the material.
This experiment was carried out at room temperature on three materials: the Pb-65 at%
In alloy, the 1 .9 Jlm amorphous Al2 03 film and its sapphire substrate.
6.1.2 % Step/Hold
A variation of the step load experiment was utilized in the HTMPM to take
advantage of the high data acquisition rates in determining the effect of the percentage
of the maximum load that was applied in a step fashion. Figure (9) is a plot of the load
versus time history used for this experiment. All of the experiments were conducted to a
maximum load of 1 0 mN. As shown in Figure (9), the load was applied by first ramping
the load to a percentage of Pma x in 1 0 seconds and then immediately applying the
remainder of the load in a step fashion. The load was then held constant for a period of
time such that the displacement versus time response under constant load could be
64
Co nsta nt
Load
80
..-
z
E
60
Ramp
Load
"C
ca
0
..J
Step
U n load
40
20
Hold @
C o n stant
Load
O ULJ...L.L..L.L.u...JL...W.r.I.........
.
..
..
...L.L
...
...L.L.:LLJ
50
1 00 1 50
Time (8)
200
250
Fi&ure 8 . A plot of the load time history for step load experiments conducted on
Pb-65 at% In, amorphous Ab03, and sapphire.
65
10
8
Percent of
Ramped On
P
g
"'0
as
o
....J
max
1 0 0/0
--
- - - - - 20 0/0
4
-
70 %
2
=o
for Hold Seg ments

Followi ng Step Load
o ....
o
1 0 1 5 20 25 30
5
Time (8)
Figure 9 . A plot of the load time history for the study o f step loading effects on
In. Following a load ramp to 1 0, 20, 30, and 70% percent of the maximum load, the
remaining percentage of Pmax was applied in a step fashion.
66
monitored. Experiments were conducted in which 90, 80, 70, and 30% of the maximum
load was applied in a step fashion. Note the definition of t=O that will be used for the
displacement versus time response to this experiment type. These experiments were
carried out on pure In at room temperature in the HTMPM.
6.1.3 Constant Rate of LoadingIHold (CRLlHold)

The CRUHold type of experiment was first utilized by Mayo et al[55] in their
study of nanophase Ti0 2 . This type of experiment utilizes the ability of the Nano
Indenter and the HTMPM to incrementally apply the load on the indenter at a rate
specified by the user.
Figure ( 1 0) is a plot of the load time history for a variety of constant rate of
loading experiments. As shown in the figure, the load on the indenter was ramped to a
specified maximum at a constant loading rate and then held constant for a period of
time.
Elevated temperature experiments on In and Al were conducted using a 1 second
ramp to maximum load, 10 mN for In and 100 mN for Al respectively . The load ramp
was immediately followed by a hold period under constant load to monitor the
displacement versus time (indentation creep). Typical hold time under constant load
was 1 80 seconds.
Room temperature experiments were conducted on In at four different loading
rates; 0. 1 , 0.3, 1 , and 1 0 mN/s to a maximum load of 1 0 mN . This type of experiment
allowed the indentation strain rate and hardness to be determined during a segment when
both were expected to be changing.
67
15
P,(m N/s)
--0- 1 0
1
0.3
-f:r- O.1
10
-
z
E
"'0
ctS
0
--.J
---
20
40
60
80
1 00
Time (8)
Figure 10.
experiments.
A plot of load versus time for the constant rate of loading
A 1 second ramp ( 1 0 roNls) was used in the elevated temperature
experiments on In and AI. The remaining ramp rates were used in the study of the
effects of loading rate on the indentation strain rate and hardness of In at room
temperature. The maximum applied load for all experiments was 10 roN.
68
6.1.4 Constant
6 . 1 .4.1
pip
Development of a Constant "Indentation Strain Rate"
Experiment
The technique for conducting constant indentation strain rate experiments can be
developed from the equation for the hardness of a material. Recall from equation (37),
(38)
H=-=
A ch2
where H is the hardness, P is the load, A is the projected contact area, h is the contact
depth, and c is a constant that depends upon the geometry of the indenter (24.56 for the
perfect Berkovich geometry). Equation (38) can be rewritten as
(39)
Differentiating equation (39) with respect to time leads to

2
2chhH + ch iI
==
(40)
which can be simplified as follows:

2
2chhH = P ch iI
(4 1 )
h=
P - ch2 iI
(42)
--
2chH
2chH
69
ch 2 if
h = 2ch2 H - 2ch 2 H
P
(43)
Substituting in from equation (38) yields
h p if
-h = 2P - 2H
(44)
or
(45)
where ei is the indentation strain rate.
Equation (45) suggests an indentation
experiment perfonned with a pyramid shaped indenter during which the loading rate is
controlled so that the loading rate divided by the load is constant can result in a constant
value of the indentation strain rate if a steady state value of the hardness can be reached
and
if = O .
This type of test is very appealing as the loading rate i s a directly
controllable parameter in the Nano Indenterrr.
6.1.4.2 Experimental
To test the hypothesis that controlling the loading rate in such a manner as to
maintain Pip constant would result in a constant indentation strain rate, a series of
experiments at a variety of Pip values were conducted on pure In at room temperature.
Figure ( 1 1 ) is a plot of the load time histories used for these experiments. As shown in
the figure, the loading rate was controlled in such a way to maintain the instantaneous
70
15
i:.I. ....
...
..
..
....
...
....
...
...a...
""""""""'a.....&.. ""'"
O .Iriii....
a
200
400
600
Time (8)
800
1 000
Figure 1 1 . A plot of load versus time for the experiments, conducted on In,
during which
Pip
was held constant. Four constant
Pip
to a maximum load of 10 mN to determine if a constant

result in a constant indentation strain rate.
71
experiments were conducted
Pip
loading scheme would
value of Pip constant up to a maximum load of 1 0 mN. The load was then held
constant for a period of time and the displacement versus time was monitored. Values
of P'1P of 0.2, 0. 1 , 0.02, 0.0 1 and 0.005 s- 1 were used.
6.1.5 it/p Change

In order to investigate the response of pure In to an abrupt change in the
indentation strain rate, a series of experiments were conducted in which the value of
Pip was changed during the experiment at some specified depth. This type of
experiment allowed the investigation of the existence of a path independent indentation
steady state.
Figure ( 1 2) is a plot of the control variable, Pip , during these
experiments. Experiments were conducted in which Pip was abruptly changed from a
value of 0.02 to 0. 1 as well as from 0. 1 to 0.02 at a depth of 3000 nm.
6.2 Indenter Geometry

All of the experiments conducted in this work were performed using a Berkovich
indenter; a three sided pyramidal indenter with the same depth to area ratio as a Vickers
indenter. The projected area of contact for a perfect Berkovich geometry is given by
24. 56h;
(46)
where he is the contact depth of the indentation. The Berkovich geometry is typically
chosen over a Vickers indenter as it is much easier to produce near perfect tips due to the
natural intersection of three planes at a point. Unless otherwise specified, the area
function used for calculating the hardness will be that of equation (46).
72
I ndium
0. 1
, ( S- l )
.
, ( S- l )
0.01
2000
-0-
0.1
0.02
>
0 . 02
->
4000
3000
Displacement (nm)
0. 1
5000
Figure 12. A plot of Pip versus displacement for Pip change experiments
conducted on In. The initial value of Pip was maintained up to a displacement of 3000
nm at which time Pip was either increased or decreased according to the figure. The
new value of Pip was maintained up to a depth of 5000 nm.
73
Associated with a given geometry of indenter is the concept of a characteristic or

effective strain [68]. An empirical relation was found by Tabor[68] which suggested that
the hardness of a material as measured with a Vickers indenter was approximately equal
to the flow stress of the material at a strain of 8- 10%, i.e., the deformation due to the
indentation itself produces an additional strain of 8- 1 0% . Tabor proposed an effective
strain of 0.2 cot for a cone or pyramid with an included angle of 2. The concept of a
characteristic strain will be discussed further in comparing the indentation creep results
to the results for uniaxial testing of the same material.
6.3 Thermal Drift

Three types of displacements are measured by a depth-sensing indentation
system:
elastic displacements of the sample surface and the load frame , plastic
displacements into the sample, and displacements due to experimental (typically

thermal) drift[69].
In
order to interpret the data, it is necessary to accurately separate the
three components of displacement, or perform the experiments in such a way that certain
components of the displacement can be neglected. The elastic displacement of the
sample surface is an issue that will be dealt with subsequently, it is the issue of thermal
drift that will be addressed here. As the issue pertains differently to the Nano Indenter
II and the HTMPM, the two instruments will be dealt with separately.
6.3.1 Nano Indenter II

Experimental drift in the Nano Indenter II is caused by thermal expansions
which are detected by the capacitance gauge. Two sources of drift are typically
identified: ( I) thermal drift that occurs due to fluctuations in the temperature of the
laboratory, and (2) thermal drift that occurs due to Joule heating in the load application
74
coil(69]. Specific steps were taken to reduce the effects of these two possible sources of
error.
First, the Nano Indenter is i solated in a laboratory where the temperature is
controlled to within O.5C at all times. In addition to the tight temperature control of
the environment, the instrument is located within another isolation cabinet and has a
very large thermal mass preventing rapid changes in the temperature of the system.
Finally, the specimens were typically placed within the laboratory for at least 24 hours
before the experimental run to ensure thermal stability.
The effects of Joule heating were dealt with in two ways. In the step loadlhold
experiments conducted on Pb - 65 at% In, amorphous A12 03, and sapphire, which were
performed in an earlier version of the Nano Indenter , the magnitude of the step load
applied was such that the current through the load coil under load was exactly equal to
and opposite in sign of the current required to support the weight of the indenter (it
should be pointed out for clarity that the typical mass of the indenter is around 7 grams,
therefore the forces generated in the load application coil are typically supporting a large
fraction of the weight of the indenter rather than actually pushing on the indenter). This
minimized the effects of differential thermal expansion due to changes in the power
dissipated in the load coil.
The remaining room temperature experiments were
conducted in a version of the Nano Indenter with an Invar indenter tube. This material
which is known for its extremely low coefficient of thermal expansion around room
temperature is expected to minimize the effects of heating due to the load application
coil.
With these steps to minimize the effects of experimental drift taken, the effects
of thermal drift on the experimental results from the Nano Indenter II were assumed to
be
negligible and no correction for this contribution to the displacement was made.
75
6.3.2 HTMPM
As previously discussed, the design of the displacement sensing system of the
HTMPM is very different than that of the Nano Indenter . The interferometric
displacement measurement is made strictly on a differential basis with a measurement
mirror mounted directly above the indenter and a reference mirror rigidly coupled to the
upper surface of the sample. This configuration leaves little material to contribute to
experimental drift due to thermal expansion or contraction of components of the
indentation system.
As the temperature of the indenter tip and sample were directly controlled by
independent systems throughout the experiment, no effects due to changes in the
environment were expected. These two facts also led to the effects of thermal drift on
the displacement measurement in the HTMPM to be neglected.
One note, as will be pointed out in the results and discussion section, a long term
thermal stability problem was encountered at temperatures of less than RT in the
HTMPM. These problems did not stem from the heating system, rather the cooling
system. In order to achieve temperatures of less than RT, liquid nitrogen was passed
through cooling channels in the indentation head and specimen stage. Due to the violent
boiling of the liquid nitrogen in the cooling channels, the supply had to be valved off
during an experiment to reduce vibrational noise to an acceptable level. This resulted in
the thermal expansion of an elastic hinge that was responsible for one axis of alignment
of the laser measurement system. The problem was not directly one of a thermal
instability in the displacement measurement, rather one of system stability as the
temperature of vital components changed. This problem was avoided at temperatures
greater than room temperature by using nitrogen gas for cooling rather than liquid
nitrogen.
76
Chapter 7 Indentation Creep - Results and Discussion
7. 1 Effects of Stress
7.1.1 Introduction
The central theme of this section of the dissertation is to investigate fully the
relationship between indentation strain rate and hardness. Data from a variety of
experimental techniques as well as from a variety of materials will be presented. The
results obtained from the different experimental techniques will be compared and
evaluated.
7.1.2 Results and Discussion
7.1.2.1 Pb-65 at% In

Figure ( 1 3) is a typical plot of displacement versus time obtained for the Pb-65
at% In alloy during the hold segment under constant load using the Step LoadIHold load
time history. The displacement rate during the hold period was typically observed to
vary from approximately 70 nmls during the initial stages of the hold period under
constant load to approximately 0. 1 nmls at the end of the 1 hour hold under constant
load. By differentiating the displacement versus time data, the displacement rate of the
indenter,
it ,
can be obtained continuously during the constant load hold period. The
indentation strain rate can then be obtained by dividing the instantaneous descent rate of
the indenter by the displacement at that point in time,
it/h.
By defining hardness as the
load divided by the instantaneous contact area as previously outlined, plots of
77
(dh/dt)
5300
0.08
n m/s --"
5200
-
--
5 1 00
+-'
C
Q)
E
Q)
5000
()
Ctj
4900
4800
<II1II(----
4700
(dh/dt)
67
n m/s
Pb 65 at % I n
-
4600
1 000
2000 3000
Time (s)
4000
Figure 1 3 . A typical plot of displacement versus time during 3600 second hold
period under constant load following an 80 mN step load for Pb-65 at% In. The
displacement rate of the indenter was observed to vary nearly four orders of magnitude
during the hold period under constant load.
78
indentation strain rate versus hardness analogous to strain-rate versus stress curves
obtained using conventional bulk testing techniques can be obtained. Figure ( 14) shows
the results of the analysis of the indentation creep properties of the Pb-65 at% In alloy.
The importance of obtaining all of the data from a single indentation is evident from the
fact that indent-to-indent variations in the hardness of the material have little effect on
the overall shape of the curve, just its placement on the hardness axis. The slope of this
plot of log hardness versus log indentation strain rate yields the stress exponent for
indentation creep. A stress exponent of 90 was obtained at the high strain-rate portion of
the curve with the stress exponent approaching 6 as the strain rate decreased.
7.1.2.2 Indium
% Step/Hold Results
Figure ( 1 5) is a semi-log plot of the displacement versus time response of the
indenter obtained for indium for the %Step/Hold loading conditions to a maximum load
of 1 0 mN . The upper four curves show the displacement response to an applied step
load with varying amounts of the total load being applied during the ramp prior to the
step to maximum load. The percentage of Pmax stepped on at t=O is indicated for each
curve. There are several important features to note from these four curves.
First, note the wide range of descent rates experienced by the indenter as
indicated by the span of eight orders of magnitude on the time axis. This reveals one of
the useful aspects of the high data acquisition rates available with the interferometric
displacement sensing technique being used in the HTMPM.
Secondly, the depth achieved immediately following the step load is largest for
the largest percentage Pmax stepped on. This is believed to be due to the large inertial or
79
..I
en
CD
ctS
a::
c
ctS
10...
......
1 0. 3
.-
......
en
c
0
......
ctS
C
CD
"'C
C
......
1 0- 4
Pb 65 at % I n
-
1 0. 5
0. 1
0. 1 2 0. 1 4 0. 1 6 0 . 1 8 0.2
Hardness (G Pa)
Figure 14. A log-log plot of indentation strain rate versus hardness for step load
experiments conducted on Pb-65at% In. The slope of the line is the stress exponent for
creep. A stress exponent or approximately 6 was observed at the lower strain rates.
80
I ndium, P
0/0
4000
max
of P
=1 0mN
Ram ped
max
on During Pre-load
E
c
--
......
c
Q)
700/0
3000
+--;?""'7;?;
Q)
()
Cd
a.
en
2000
1 000
1 s Ramp to P
max
...
.a..-....-....
..
----.-....
...
----oI
...
Io-....
O Io..-..-
1 0-
1 0- 4
2
1 0Time (s)
10
10
Figure 1 5. A semi-log plot of displacement versus time for In showing the

response of the material to a variety of step loads. The oscillatory response to large step
loads is enclosed in "A" and is enlarged in Figure 1 6.
81
dynamic forces that are being experienced by the specimen as are evident from the
oscillatory response of the indenter following the applied step as shown in "A" in Figure
( 1 5) and enlarged in Figure ( 1 6).
Finally, immediately following the step load, an incubation period is observed
where the displacement rate of the indenter is observed to be smallest for the largest
step-fraction and the four curves are seen to reverse their order in terms of overall
displacement. Since under normal data acquisition conditions the first data point on
these curves is obtained at approximately 1 second, the region on the time axis where
these four curves intersect is not normally observed. This initial reduced creep rate i s
believed to b e due to ( 1 ) the stronger structure resulting from the higher strain rate
experienced by the material when a larger fraction of the maximum load is applied in a
step fashion, and; (2) the larger contact area and therefore the lower stress that results
from the dynamic overload. Finally, after the initial incubation period, the displacement
rates for the four curves become similar.
While not directly related to the creep properties of the material, the oscillatory
response to the dynamic overload warrants discussion. Figure ( 1 6) is an enlargement of
the area marked in flAil in Figure ( 1 5). It is a plot of displacement versus time showing
the oscillatory response of the indenter as it comes to rest during the 80 ms immediately
following an applied step load of 9 mN (90% of Pm ax ). Inertia calculations using the
maximum acceleration, d 2 xl dt2 , experienced by the indenter reveal that a dynamic
overload of as much as 40% of the applied load can be experienced by the specimen.
This phenomenon is seen to decrease as the step-fraction is reduced and is completely
absent when the step-fraction is reduced below 30% as shown in Figure ( 15).
A number of interesting observations can be made about the observed oscillation
following the step-load. The natural frequency of the oscillation, which is determined
82
3 1 70
1\
i ,
E
c
---
.......
,,
"
,"\
j \
; ! \ i \ / \ j
\'"
!
!
1('\'
,"
3 1 65
C
CD
CD
(.)
c..
en
.-
{\
: \
i i
I
I
; ;
V
\ t"
3 1 60
ro =21t{975c/s}=6 1 26. 1 /s
t :
3 1 55
j
\J
S=mro
2=2.82x1 05
N/m
3 1 50
0.01
0 . 002 0 . 004 0 .006 0 . 008
Time
(s)
Fiure 1 6 . A plot of displacement versus time showing the oscillatory response

of the indenter during the 80 ms immediately following a step load of 9 mN on In. The
frequency of the oscillation is directly related to the stiffness of the contact. The
exponential decay of the oscillation is representative of the losses in the material.
83
predominantly by the stiffness of the contact, S , and the mass of the indenter, m, is
observed to be 975 cyclesls
oscillator,
OJn
(6 1 26
rad/s) . Using an equation for a simple harmonic
..JSlm , together with the known mass of the indenter yields a contact
stiffness of 2.82x 1 05 N/m. If the contact area of the indentation is calculated from the
mean displacement of the oscillation, the storage modulus of the material can be
calculated from[70]
E=
-JH
(47)
2 {A
where S is the stiffness of the contact. This analysis results in a modulus of 1 3 .8 0 . 2

GPa, a bit higher than the literature value of 12.7 GPa. This slightly higher value of the
modulus is reasonable as the high frequency or unrelaxed modulus of a material is
expected to be somewhat higher than a low frequency or relaxed modulus. It is also
possible from the exponential decay of the oscillation to calculate an effective damping
coefficient of 7 N s 1m. After careful characterization of the dynamics of the indentation
system as very accurately detailed in Appendix A, it was determined that this number
most likely represents the damping or energy being absorbed by the sample material in
the vicinity of the indentation and is not energy absorbed elsewhere in the system.
Using the fact that the loss modulus is known to also scale as the square root of the
contact area (see Chapter
12), it is possible to calculate a loss modulus according to

(48 )
This calculation results in a loss modulus of 2.4 GPa. This value is seen to be roughly
20% of the storage modulus.
84
CRLlHold Results
Room Temperature
Figure ( 17) is a plot of the indentation strain rate versus displacement obtained
using the CRLlHold loading schemes. The strain rates were calculated by taking the
time derivative of the displacement during both the load ramp and during the subsequent
hold period under constant load and dividing the instantaneous rates by the displacement
at that point in time. The indentation strain rate is observed to decrease continuously
through the constant loading rate loading period and, even more rapidly, during the
constant load hold period.
Figure ( 1 8) is a plot of the calculated hardness versus displacement over the
same displacement range. (The accuracy of the calculated hardness is discussed in
Appendix B .) The hardness is observed to decrease as the experiment proceeds and the
indentation strain rate decreases. The change in the hardness is gradual during the
loading segment when the indentation strain rate is not changing rapidly and then
becomes much more pronounced once the loading stops and the strain rate drops rapidly.
Figure ( 1 9) is plot of the indentation strain rate versus the hardness from the
CRLlHold experiments. Each curve represents an average of five indentation performed
under each loading condition. It is observed that the data immediately following a
constant loading rate segment undergo a transient period immediately upon completion
of the load ramp. These data are then observed to converge to a common curve over a
period of time which is similar to the loading time. This transition region which appears
to have a higher stress exponent is believed to be due to the transient microstructural
evolution occurring immediately after the completion of the load ramp and is not
85
1 01
I nd i u m
P,(m N/s)
-0- 1 0
T"""
I
en
Q)
ct'S
......
-0- 1
-0-
1 0
0.3
-----fr- O. 1
II:
c
O ct'S
I-
......
CJ)
c
0
-:;:;
ct'S
......
1 0- 1
c
Q)
-c
c
2000
3000
4000
Displacement (nm)
5000
Fiure 17. A plot of indentation strain rate versus displacement for CRLfHold
experiments conducted on In. The indentation strain rate during a constant loading rate
segment is observed to decrease as a function of displacement.
86
0 . 04
P,(mN/s)
10
0 . 035
-<>-
as
0..
(!J
0.3
0 . 03
en
en
Q)
c
"'C
----fr-
0. 1
'-
0 . 025
0 . 02
I ndium
L..L.I.
..
...
........
.
&..L.L
.,j
L..L.&.
..
..&..&.
...
....
...
0 . 0 1 5 ........
5000
3000
4000
2000
Displacement (nm)
Figure 1 8. A plot of hardness versus displacement for CRLlHoid experiments
conducted on In. The hardness of a rate sensitive material is seen to decrease during a
constant loading rate segment due to the decreasing indentation strain rate.
87
10
--------p---
I ndi u m
,,
P,(m N/s)
en
'-'"
<>
o
6
10
1
0.3
0.01
6.1
1
4
1 0 - -----0 . 03 0 . 04
0 . 02
0.01
Average Hardness (G Pa)

Figure 1 9.
A log-log plot of the average indentation strain rate versus the
average hardness for series of constant loading ratelhold experiments on In. The
material is observed to undergo a transient response immediately following the
completion of the load ramp. The data are then seen to relax to single curve. A stress
exponent of 6 . 1 is obtained from the lower portion of the curve.
88
believed to be associated with power law breakdown.

discussed in light of the results from the constant
This point will be further
Pip analysis.
As previously pointed out, the indentation strain rate-hardness data during the
hold segment converge to a single curve after an initial transient period. A power law fit
to the linear portion of the data in this region yields an average slope of 6. 1 which is the
stress exponent for indentation creep in the material. This value is in good agreement
with the constant stress tensile data of Weertman[39].
Elevated Temperature
Figure (20) is a plot of the displacement versus time results for indium obtained
during the constant load hold period immediately following the load ramp as a function
of the test temperature. All of the data were acquired using the CRLlHold technique
with a 1 sec ramp to 1 0 mN . The data acquired for the temperatures less than room
temperature are terminated after 40 s due to longer term system stability problems at
these low temperatures.
Some important features to note from these curves are 1 .) the displacement
achieved by the indenter is less as the temperature is reduced indicating the material is
capable of supporting greater stresses and 2.) the sharpness of the break in the curves at
temperatures less than room temperature suggests a very high stress exponent, i.e., the
stress is becoming nearly constant very quickly.
Figure (2 1 ) is a log-log plot of indentation strain rate versus hardness for
experiments conducted at room temperature (28 C), 50 C and 75 C. The lower
temperature data is not included due to the previously mentioned experimental stability
problems.
89
I nd i u m
7000
6000
-
---
C 5000
Q)
Q)
4000
c.
CI)
.-
Cl
3000
2000
1 000
1 00
Time (5)
50
1 50
200
Fiiure 20. A plot of displacement versus time during the hold period under
constant load following a 1 second ramp to 1 0 mN for In at temperatures ranging from
90
1 02
28C ,
28C ,
50C ,
50 C ,
75 C ,
75 C ,
.
1 01
",-....
,...
I
(f)
---
Q)
+-'
CO
1 0
0:
s::::
CO
+-'
en
+-'
s::::
Q)
"'C
s::::
1 0- 2
Termi nation of
Load Ramp
1 0- 1
s::::
0
I n dent
I n dent
In dent
Ind ent
I n dent
I n dent
!:::.
1 0- 3
1 0- 4
Figure 2 1 .
I nd i u m
1 0- 2
H ardness (G Pa)
1 0- 1
A log-log plot of indentation strain rate versus hardness for
indentation creep experiments on In at temperatures of 28, 50, and 75C. The data are
observed to undergo a transient period immediately following the completion of the load
ramp yielding a higher apparent stress exponent for creep.
91
All of the data exhibit similar trends again showing a transient region in
progressing from the load ramp to the hold period under constant load. An interesting
note is that the length of the transient period seems to be reduced as the temperature is
raised perhaps due to the greater thermal energy available for microstructural
rearrangement. All of the data are seen to be linear near the end of the hold period with
a stress exponent of approximately 5 at the higher temperatures.
Constant P/p
Figure (22) is a plot of the indentation strain rates versus displacement obtained
using the constant Pip loading schemes as well as the data from the 1 mN/s CRLlHold
experiment for comparison. The strain rates were again calculated by taking the time
"-----------.,,.----..
----
derivative of the displacement, both during the loading segment and during the
"
_'''''_''''''i.. __.'_r_"rl'.t"",''-,1'__'''''_,,'h<
"",-"" '-"'--"''' -'''' '-- "'' .>'<-'''''-----", ,,., _,...,_,,,,,--r;-,..''''''''

'' '''''''''''',-.
subsequent hold segment, and dividing the instantaneous rates by the displacement at
..,'
.-"
that t:? int in ! ime. As suggested by equation (45), the indentation strain rates are
,-"." (,,, ,"
constant during the loading segment and equal to 0.5 Pip suggesting that an indentation
steady state has in fact been reached and
if
The indentation strain rate is again
o.
observed to decrease once the load ramp terminates.

Figure (23) is a plot of the calculated hardness versus displacement for the
constant Pip experiments as well as for the 1 mN/s CRLlHold experiment again for
comparative purposes. The calculated hardness is observed to remain constant during
the constant Pip loading segment and to systematically decrease as Pip , and thus
izlh,
is decreased.
Since for each Pip experiment a constant
izlh and H is achieved, it is possible
to tabulate "indentation steady state" strain rate-stress pairs analogous to uniaxial data.
Figure (24) is a log-log plot of indentation strain rate versus hardness for the data from
92
P,(mNI s)
1 .0
-
' 00
-
Q)
Cti
,(S- 1 )
0.2
....,,-- 0. 1
-0- 0.02
0.1
a:
c
ro
+-'
en
c
.o
I nd i u m
Cti
C 0 . 05
Q)
"C
C
o
200 0
3000
4000
Displacement (nm)
5000
Figure 22. A plot of indentation strain rate versus displacement for three
different constant Pip experiments conducted on In showing constant indentation strain
rates equal to 0.5 Pip . Data from the constant P = l mN/s experiment are included for
comparison.
93
0 .03
P,(mN/s)
1 .0
,(S-1)
0.2
--0-- 0. 1
0.02
0.0 1
0 .005
-0-
--0-
..-.
ctS
c..
---t:r-ill
0.025
{!J
en
en
(])
c
"C
ctS
I
I nd i u m
:I.-
0.02
3000
4000
Displacement (nm)
5000
Figure 23. A plot of hardness versus displacement for five different constant
Pip experiments conducted on In showing indentation steady state behavior in response
to constant Pip load ramp. Data from constant P = l mN/s experiment are included for
comparison.
94
,....
I
en
(])
ro
a:
c
ro
+-'
+-'
en
c
0
+-'
ro
c
(])
'"0
C
1 0- 2
+-'
(])
0')
ro
(])
>
I nd i u m , Constant
3
1 00.01
---------
0.03 0 . 04
0.02
Fiure 24. A log-log plot of average indentation strain rate versus average
hardness for constant Pip experiments conducted on In.
A constant power law
relationship is observed over the entire range of indentation strain rates investigated.
95
the constant Pip experiments. The data were generated by averaging the constant
hardness/constant
izlh
data between 2000 nm and the termination of the loading
segment. Each data point represents the average of five experiments at each Pip .
power law fit to the data yields a slope of 7.3 (R=0.995) which is the stress exponent for
creep in the material. Over the range of strain rates investigated the power law
relationship was observed to remain constant. The stress exponent for indentation creep
of 7.3 is very near the value of 7. 6 obtained for indium tested uniaxially by
Weertman[39] near room temperature.
Hardness versus Time (Sargent and Ashby Analysis)

As discussed in the literature review, one of the earliest techniques for gaining
information into the stress exponent for creep from an indentation test was to monitor
the optically measured hardness as a function of dwell time under load, the slope of a
plot of log hardness versus log time being equal to -(lIn) . This same analysis can be
performed with a depth-sensing indentation system. The centra! differencJs that rther
than removing the load to optically measure the size of the indentation, the hardness can
be calculated continuously as a function of time since the load on the indenter is known
and the contact area of the indentation can be obtained from the depth of the indentation
and the functional relationship between the contact area and the depth.
Figure (25) is a log-log plot of hardness versus time showing typical curves
obtained for In at room temperature for three different loading times that most closely
approximate the probable loading times used in a rnicrohardness system. These data are
plotted along with the data for In from Atkins et alL 10] obtained for a Vickers indenter
and conical indenters with apical angles of 1 05, 1 20, 1 3 6, and 1 50.
96
1 sec loading
1 0sec loading
30sec loading
--0- Atkins et. al. Cone
Atkins et. al. Vickers
I
I
\\
..
"\":\
-':rc..
I
"
.-....
co
c..
'I.
";.-.
I.
(!J
en
en
Q.)
c::
'"'C
"-
1 0- 2
CO
:c
I ndium
_
1 0- 3 1...1
10
1 0-
__"'-_...._
.. ......
1
2
3
4
10
10
10
10
Time (5)
...._
..
---1.
Figure 25. A log-log plot of hardness versus time under load for In. The data
shown are from Atkins et al[ l O] and from CRLlHold experiments to 1 0 mN from this
study. The slope of the line is - l in.
Source: A. G. Atkins, A. Silverio, and D. Tabor, J. lnst. Metals,
97
94,
369 ( 1 966).
According to Atkins et aI, this analysis should result in a linear relationship,

between log hardness and log time. The data from their work is seen to be linear with
slopes of -0.095 and -0.086 for the data from the conical indenters and the Vickers
indenter respectively. These slopes result in stress exponents of 1 0.5 for the conical
indenters and 1 1 .6 for the Vickers indenter as reported by Atkins et al in the cited work.
Note that due to some ambiguity in the paper by Atkins et al, some question as to the
absolute magnitude of the hardness values shown in this plot exists. This confusion
does not effect the stress exponents obtained from the data, rather the placement of the
data on the hardness axis.
Comparison of the data from the current study to that of Atkins et al raises three
points. First, as observed by Atkins et aI, the data for short loading times , e.g., 1
second, deviates significantly from linearity. This deviation is observed not only during
the initial portion o f. .!ht'? data where a transient state probably exists, but in the latter
.
stages of the data as well for reasons that are not completely understood. Second,
neglecting the data from the 1 second loading experiment, the slope of the log hardnesslog time data does seem to become constant once the initial transient period on going
from the load ramp to the hold period is surpassed. Finally, a lower stress exponent is
obtained for the data from this study than was obtained by Atkins et al. The average
slope of -0. 1 7 results in a stress exponent of 5 .9 as compared to values of roughly twice
that from the data of Atkins et al. The value of 5.9 obtained from this study agrees well
with both the stress exponent obtained from the log indentation strain rate-log hardness
data and the data from Weertman[39] .
One of the potential problems of the technique of Atkins et al is that it requires a
measure of an absolute variable, the time, rather than being based on a differential
variable such as the indentation strain rate. This is also a problem from a fundamental
98
standpoint in that the hardness as a function of time has no physical meaning, it is

simply a representation of the data based on the fact that the strain rate is decreasing as a
function of time under load. An excellent example where this can introduce problems is
observed in comparing the data from a number of experiments conducted with a 1 0
second loading time. Figure (26) is a log-log plot o f hardness versus time for five
experiments conducted with a 1 0 second loading ramp. The scatter in the initial portion
of these data is obvious. A log-log plot of indentation strain rate versus hardness for the
same data does not however show the same scatter as shown in Figure (27) . Rather, it is
seen that the data all lie very nicely on a single curve even during the initial portion of
the loading segment.
Strain Rate versus Time

One final issue that warrants discussion at this time is the analysis by Sherby[ 12]
suggesting that the average indentation strain rate scales with the characteristic strain of
the indenter divided by the time under load. Figure (28) is a plot of the indentation
strain rate,
hlh, versus time for the 1 , 1 0 and 30 second load ramp data on indium at
room temperature plotted along with the indentation strain rate predicted by dividing the
characteristic strain of a Berkovich indenter (0.08) by the time of the experiment. Once
the transient period on proceeding from the load ramp to the constant load hold period is
surpassed, good agreement is observed between the experimental indentation strain rate
and the indentation strain rate predicted by Sherby.
Comparison of Indentation Techniques for Obtaining Stress Exponent

Figure (29) is a log-log plot of indentation strain rate versus hardness for the data
from both the constant Pip experiments as well as the constant rate of loading/hold
99
I
I
\ . '"
I
,I
"
.
'
"
I
.
I
'
'
'
CJ)
CJ)
CD
c
\. .
,
,
... \ ..
\. t\ I
a.
a. \.
.
"
'
4
.
.
"E
J:
1
6.5
I nd i u m
10
1 01
Time (s)
10
Figure 26. A log-log plot of hardness versus time for In for experiments
conducted using 1 0 second constant rate of loading ramp to 1 0 mN followed by a hold
period under constant load. Note the scatter in the initial portion of the data due to
definition of absolute time. The slope of the line is equal to - lin and gives a reasonable
determination of the stress exponent at long times.
1 00
1 0 1 --------
I ndium
,I
en
Q)
+-'
ctS
a:
C
ctS
10+-'
1 0- 1
en
c
.0
-
+-'
ctS
+-'
C
Q)
"'C
C
6. 3
1
1 .01------0-.
0 .-04-0 2---0-.03--4
Hardness (G Pa)
Fiure 27.
experiments conducted using 1 0 second loading ramp to 1 0 mN followed by a hold

period under constant load. The indentation strain rate versus hardness relationship is
observed to follow a single curve throughout the entire experiment.
101
1 01
1 sec
load i n g
- - - - - - - - - 1 0sec loadin g
T"""
I
10
- 30sec loadin g
'.\
0. 08/Ti me, Sherby

P rediction
CIJ
---
Q)
ro
-\
',\
.
......
a:::
C
ro
'-
1
1 0-
......
ro
......
c
Q)
"'C
C
1;'.,-
'.
\/'\
:
......
en
C
0
,t
:,
':
0- 2
1 0-
" \,
"'\
I ndium
...I
....
..
L...
..
....
...I
.LI.III
..
L......&.
...I
.LI.IIIL...
.I.
...&.
...I
.&.I.I
.I.
III
1 0 -4 L.......
2
3
0
10
1 0- 1
10
1 01
10
Time (5)
Figure 28. A plot of indentation strain rate versus time for 1 , 10, and 30 second
load ramps to 10 mN followed by hold period under constant load for In. According to
the model of Sherby[ 1 2] , the indentation strain rate should scale as the characteristic
strain of the indenter (0.08 for Berkovich) divided by the time of the experiment.
1 02
10
--------
I nd i u m
,....
I
en
7.3
......
CO
c
a>
"'C
C
a>
C)
CO
l0a>
.....
P,(m N/s)
10
6.3
0.3
0. 1
-... ------........
...
...
.....&...
1 0-4 ....-0.01
0 . 03
0 . 02
--
----1
--
0 . 04

Figure 29. A log-log plot of indentation strain rate versus hardness comparing
the results of the CRLlHold experiments to the results of the constant
Pip experiments.
The stress exponent obtained from the two techniques is in reasonably good agreement.
1 03
experiments. Strain rate-stress pairs were calculated for both the loading segment and
hold segment from the CRLlHold experiments. Each set of data represents the average
of five separate indentation experiments performed for each loading rate.
Several
interesting observations can be made abouHhese data.

It was previously hypothesized that the transition region on going from a load
ramp to a c onstant load was due to transient microstructural evolution occurring
immediately after the completion of the load ramp and was not associated with power
law breakdown. This is supported by the fact that even at higher strain rates the constant
Pip data obey a constant power law relationship.
The similarity of the stress exponent
obtained from the two types of experiments and the offset in the hardness leads to two
conclusions. One, the dominant factor in both types of experiments seems to be the
stress exponent for creep. While the two sets of data were acquired under very different
conditions, the appropriate stress exponent seems to come out of both sets of data.
Secondly, the data from the CRL/Hold experiments appears to have a stronger
microstructure as indicated by the higher hardness determined at the same strain rate.
This is reasonable since the material has undergone a wide range of strain rates
beginning at very high values and decreasing throughout the experiment. The material
is therefore evolving from a strong microstructure to a weaker microstructure as the
experiment proceeds. This is in direct contrast to the constant
Pip experiments where
the indentation steady state is always expected to be approached from a hardening

direction.
Comparison of the stress exponents obtained from the hardness versus time data,
Figure (25), and the indentation strain rate versus hardness data, Figure (29), shows that
a similar value for the stress exponent is obtained from the two analyses, except at short
1 04
loading times. The values of the stress exponent obtained for each technique are
summarized in Table ( 1 ).
Table (1 ) Summary of Stress Exponents Determined for Indium.
.
Technique
Analysis
CRLIHold
versus H
6. 1
CRLIHold (High T)
versus H
Pip
versus H
7.3
CRL/Hold
H versus time
5 .9
Stress Exponent, n
7.1.2.3 Aluminum
CRLlHold Results
Room and Elevated Temperature
Figure (30) is a plot of the typical displacement versus time results for Al
obtained during the constant load hold period using the CRL/Hold loading technique as
a function of the test temperature. Again note the sharpness of the break in the curves at
lower temperatures suggesting a very high stress exponent at the low homologous
temperatures.
Figures (3 1 ) through (35) are log-log plots of indentation strain rate versus
hardness for experiments conducted at temperatures ranging from 2 1 C to 250C. (The
accuracy of the calculated hardness data is discussed in Appendix B .) The average
stress exponent or the range of stress exponents from each set of data is shown on each
plot. The stress exponent is observed to range from extremely high values near room
1 05
Al u m i n u m
4500
-...
c:
......
c:
Q)
Q)
4000
(.)
ctS
0CIJ
3500
3000
o
----
50 1 00 1 50 200 250 300 350

Time (5)
Figure 30. A plot of displacement versus time during hold period under constant
load following 1 second ramp to 1 0 mN for Al at temperatures ranging from 1 00C to
1 06
1 0- 1
________________________
Al umin u m , 2 1 C
.,.I
CIJ
Q)
as
a:
c:
as
1 0-
....,
,...
....,
CI)
c:
0
+=i
as
....,
c:
Q)
"0
c:
1 0- 3
77 - 1 30
1 0-
1 0- 5
0.4
........
..
....
...
....,I.
...
....
..,j
.L-I.
...
..L-..I...Ir...L.
.&..
&...L.
..L..
....
.:
..
Figure 3 1 .
0.5
Hardness (G Pa)
indentation creep experiments on Al conducted at 2 1 e.
1 07
1 0- 1
_____________
Al u m i n u m , 1 aaoe
0
.-..
.,I
f::,.
Cf)
--
Q)
S
.......
0
0
cr:
c
S
29
.-
.......
C/)
c
0
+=i
S
.......
C
Q)
"C
C
1 0- 5
0.3
""----'-...a.....II...I...IL..a..L.--&..IL..&...L..1..I
Fiure 32.
0.4
Hardness (GPa)
indentation creep experiments on Al conducted at 100C.
108
2
1 0- ...---___
---..__-_
,.I
en
---
Q)
ctS
.....
1 0- 3
36
a:::
"ffi
J....
.....
CJ)
c
0
+=i
ctS
.....
C
Q)
'"C
C
1 0 -4
Al u m i n u m , 1 50C
1 0 - 5 1..----_...&.-___'---_----'
0.4
0.2
0 .3
Hardness (GPa)
Fiure 3 3 .
indentation creep experiments on AI conducted at 1 50c'
1 09
Al u m i n u m , 200C
,.....
I
rn
1 0-
Q)
<a
a:
c
+""
CJ)
C
0
1 7-22
1 0- 3
+""
a:s
+""
c
Q)
-c
C
1 0-
1 0- 5
0.2
--------
Figure 34.
0.4
0.3
Hardness (G Pa)
1 10
Al u m i n u m , 250C
8
8- 1 0
1 0- 4 1.--_--'-_---'-_
0. 1
Hardness (G Pa)
....-'-....&-....
..
....
..
..
Fi/iure 35.
111
temperature to values of 8- 1 0 at 250C. Figure (36) is a log-log plot of indentation

strain rate versus hardness for the data obtained at all temperatures. A progression from
high stress exponents at high stresses to lower stress exponents at lower stresses i s
observed over the complete range of temperatures investigated, however, n o constant
power law region is observed. This range of stress exponents is not unexpected given
that at low homologous temperatures , see Table (2), and higher stresses the data are
expected to obey power law breakdown type behavior.
Several key issues must be kept in mind when considering these results. First, it
is important to remember that the indentation test is representative of a constant strain of
approximately 10%. At low homologous temperatures or high stresses, the dominant
feature of plastic flow in Al is work hardening.
It is
therefore more likely that these data
are representative of the transient creep properties of the material rather than large strain
steady state properties. Secondly, all of these data were acquired from a hold segment
following a 1 second ramp to maximum load. From the results on In, it is now known
that a transient period will exist at the beginning of these data that may effect the stress
exponent determination. At low homologous temperatures it is conceivable that this
transient period may persist well into the hold segment due to the absence of thermal
energy for microstructural rearrangement.
Table (2). Range of temperatures for indentation creep of Aluminum.
Temperature (Oe)
Temperature (K)
TfTm
21
294
0.32
1 00
373
0.4
1 50
423
0.45
200
473
0.5 1
250
523
0.56
1 12
.-
....
en
2 1 C
1 00 C
'\,
.7
1 50C
200C
250C
Q)
Cij
a::
c
ca
'
.-
+-'
CI)
C
o
1a
+-'
C
Q)
"'C
C
Al u m i n u m
0 .3
0.5
Hardness (G Pa)
Figure 36.
0.7
indentation creep experiments on Al conducted at 2 1 , 1 00, 1 50, 200, and 250C.
1 13
Figure (37) is a plot of the displacement versus time response from the hold
period under constant load for the amorphous alumina film obtained using the Step
LoadIHold loading technique. Note the wide range of descent rates experienced by the
indenter during the 60 s hold period under constant load.
Figure (38) is log-log plot of indentation strain rate versus hardness for the
amorphous alumina film. T.1lQtted here, haalculated from a
rather than the total depth of the indentation as was
elastically corrected contact
done for
_ the soft metals . A linear relationship between the indentation strain rate and
_.. _..____,_
""""-",,__n,,,,">4""'''''''-''''''"-'''_'''''''-_
-"""'V,'"
hardness on the log-log plot was observed over the range of strain rates obtained. A
stress exponent of 55.6O.72 was obtained from the slope of the log-log plot.
Figure (39) is a plot of the displacement versus time response from the hold
period under constant load for the single crystal Al2 0 3 substrate also obtained using the
Step LoadlHold loading technique. Again, note the wide range of descent rates
experienced by the indenter during the 60 second hold period under constant load as
well as the overall decrease in the absolute displacement as compared to the amorphous
"'"",.___c'eo_- -
alumina film denoting the ability of the sapphire sample of supporting higher stresses.
A linear relationship between the indentation strain rate and hardness on a log
log plot was also observed for the sapphire over the range of strain rates obtained as
shown in Figure (40). The hardness of the sapphire specimen was also calculated using
--- ----"""
,..--, *" ---'-'"""''""""""
"-> " "",,,,,,..

,, ....... -.,--,,.-,, -->"...-
'>" '""
.'
.-"... ,,.-..--------"'-.
an elastically corrected contact depth rather than the total depth of the indent. A stress
__
::*,Oi"
i"")('
'...-."-" '-;_..,,,""" ,,'

..
--."" ..,...,.1'1"""
.
--....
...
__ ....,w,.._"'., - .....-....
...
, .....,tT_>
.
,___,-------.-- ..' ...-......" _,_.........._"""
exponent of 1 1 34.7 was obtained from the slope of the log-lo elot.
---...__""'....
"
....."''''''.... _.''',''''...'''',,''< ''' --.,,_-,->,"w,'_>''_ _n.... -_"-
_S
".__, _ _
"
_"
"" _< .,
:.,"
....At
... ,.:."",/w,t--
11'-
"'"
The wide range of indentation strain rates shown in Figures (38) and (40)
demonstrates the utility of the indentation experiment.
l ! :-" , e
!
. _.
stress exponent are indicative of high strain rate tests performed on materials at small
____--..-'--"""'-" -."'..
",'
-,
"
1 14
, "
"-" '-- '
-,,.--,,-"'-' '.-'
..
_iI'
''',
'"
..-..
E
c:
......
c:
Q)
Q)
(.)
co
-
0..
(f)
.-
Amorphous AI
10
20
30
Time
on Sapphire
40
50
60
(8)
Figure 37. A plot of the displacement versus time response to 80 mN step load
for a 1 .9 Ilm amorphous alumina film on sapphire. Data shown are for the 60 second
hold period under constant load immediately following the step load.
1 15
10
-1
__----------__--------__
Slope
Stress Exponent, n
Standard Deviation
0ro
0.72
1 0- 2
en
Q)
ctS
.....
a:
c
ctS
10...
10
-3
55.6
.....
en
c
0
.....
ctS
c
Q)
"'C
C
.....
10
10
-4
-5
Amorphous AI
o n Sapphi re
----
Hardness (G Pa)
Figure 38. A log-log plot of indentation strain rate versus hardness for 1 .9 J.lm
amorphous alumina film on sapphire. The high stress exponent for creep is typical of
materials at low homologous temperatures.
1 16
350
-+-'
C
Q)
Q)
()
co
c..
en
345
Sapph i re
10
20
30
40
50
60
Time (s)
Figure 39. A plot of displacement versus time response to 80 mN step load for
sapphire.
The data shown are for the 60 second hold period under constant load
immediately following the step load.
1 17
1
1 0- ...----.-_____-------.
Sapphire
Slope = Stress Exponent, n

Standard Deviation = 4.7
..-
l en
--
Q)
ctl
a:
c:
ctl
"
1 0-
2
+
C/)
c:
o
Cii
c:
Q)
"'C
c:
1 0.
4 ____...._
...
___...._
..
__---1
18
19
Hardness (G Pa)
Figure 40. A log-log plot of indentation strain rate versus hardness for sapphire.
The stress exponent of the crystalline Al203 is observed to be nearly twice that of its
amorphous counterpart.
1 18
fractions of their melting temperature. The ability to obtain information into the time
dependence of flow from these materials alone attests to the value of the indentation
creep technique. No other test technique is known of that i s capable of yielding
comparative data for two materials such as these.
7.2 Effects of Temperature
7.2.1 Introduction
The central theme of this section of the dissertation is to investigate the effect of
temperature on the relationship between indentation strain rate and hardness. Data from
both In at high homologous temperatures and Al at intermediate homologous
temperatures will be presented and discussed.
7.2.2 Results and Discussion
7.2.2.1 Indium
Hardness versus Tffm

Figure (4 1 ) is a plot of the hardness versus homologous temperature calculated
from the applied load and the displacement at 1 5 s. It is observed that over the
homologous temperature range of 0.4 to 0.8 the hardness decreases by over an order of
magnitude. The change in hardness versus test temperature at a constant time under load
will be discussed again in an analysis for determining the apparent activation energy for
indentation creep.
1 19
o
A
p
P
=3 m N
= 1 0 mN
max
max
.-...
ct:S
0...
C!J
---
en
en
Q)
c
"C
'ct:S
I
1 0-
I ndium
2
1 00.3
0.4
0.5
0.6
0.7
0.8
0.9
Homologous Ternperatu re, T / T
Figure 4 1 . A plot of hardness versus homologous temperature for In over the

homologous temperature range of 0.4 to 0.8. The hardness was calculated from the load
divided by the contact area calculated from the total displacement 1 5 seconds into the
hold period.
1 20
Determination of Apparent Activation Energy for Indentation Creep

As previously discussed, at temperatures above 0.5 Tm, creep in pure metals in
which dislocation glide is easy is thought to be controlled by the climbing of
dislocations out of their glide planes to overcome obstacles to motion . The climb
velocities are limited by the rate at which vacancies can diffuse in the material. As such,
creep at elevated temperatures is expected to follow an Arrhenius type of behavior of the
form
s = so exp(-Q I RT)
( 1 2)
absolute temperature. The slope of a semi-log plot of strain-rate at constant values of
hardness versus lIT will then yield the activation energy for the rate controlling
mechanism.
Figure (42) is a plot of the natural log of the indentation strain rate at constant
hardness versus l IT for experiments conducted between 28C and 75C. The apparent
activation energy for indentation creep obtained by a linear fit to the data is 77.9 kJ/mol.
This is in excellent agreement with the . activation energy for self-diffusion in pure
indium which is reported to be in the range 75-78 kJ/mol[7 1 , 72] and in accord with the
observation that the activation energy for creep in pure metals is nearly equal to the
activation energy for self diffusion[5] .
B y compensating the indentation strain rate for the temperature of the
experiment, a normalized plot of indentation strain rate versus hardness can be obtained.
Figure (43) is a log-log plot of temperature compensated indentation strain rate versus
121
0
Slope -Q / Rx1 0
Q 77.9 kJ/mol
=
Q)
co
......,
-1
a:
c
co
'-
......,
en
c
0
+=i
co
c
Q)
"0
c
......,
..-
0
0>
0
....J
-2
-3
-4
-5
co
'-
::::J
ca
-6
-7
2.8
2.9
3. 1
3.2
3
( 1 / T)x1 0 (K1)
3.3
3.4
Fiiure 42. A plot of natural log of indentation strain rate at constant values of
hardness versus the reciprocal absolute temperature for In. The slope of the line is equal
to -QlRx 103 where Q is the apparent activation energy for creep. An activation energy
of 77.9 kllmol was determined for the high temperature indentation creep of In.
1 22
----
o
o
(J)
l"I"
II
c:
o
.....
c:
Q)
-0
c:
I nd i u m
8
--
1 0 -2
1 0- 1
1 0Hardness (GPa)
Fi&ure 43. A log-log plot of temperature compensated indentation strain rate

versus hardness for 28, 50 and 75C experiments on In. The indentation strain rates at
the three temperatures were normalized using an activation energy for creep of 77.9
kJ/mol.
1 23
hardness for the three sets of data shown in Figure (2 1). The fact that all three sets of
data, when compensated for the test temperature, lie on a single curve supports the
premise that the deformation is being controlled by a single thermally active process.
The slope of five agrees with observed values for stress exponents in pure metals
obtained from conventional means where the rate controlling process is dislocation
climb [4].
As previously discussed in Chapter 2, in calculating the temperature
compensated creep rate it is often necessary to take into account the temperature
dependence of the shear modulus, G, in order arrive at an appropriate activation
energy [37, 38] . It has been shown for a number of materials that taking values at a
constant stress rather than at a constant value of a/G(T) can lead to overestimation of the
activation energy for creep[39] .
Figure (44) is a plot of both the Young's modulus, E, and the shear modulus, G,
as a function of temperature[66] for pure In. By normalizing the hardness for the
temperature dependence of the modulus and determining indentation strain rates at
,
constant values of HJG and HiE the activation energy for the modulus compensated data
can be determined. Figure (45) is a plot of the natural log of the indentation strain rate at
constant values of HJG and HiE versus
Iff.
A linear fit to the two groups of data yields
values for the apparent activation energy for indentation creep of 59.3 kJ/mol and 58.0
kJ/mol respectively.
One possible explanation for the lower activation energy is that the mechanism is
not self diffusion but perhaps some coupled diffusion mechanism such as a combination
of lattice diffusion and dislocation core diffusion as has been observed in Al at
intermediate temperatures. However, at such high homologous temperatures, this
explanation seems suspect. A more likely explanation is that the differences in the
1 24
11
10
-o-
You ng's Modulus
ro
c..
1 1 .676 - O.0338T
(!J
"'-'"
C/)
::E
:::J
:::J
"'C
0
G
...
3
20
Shear
30
...
40
...
Mod u lus
4.67 - O.01 35T

...
50
do
...
60
70
80
Temperature (oC)
Fiure 44 . A plot of the shear modulus and Young's modulus of In as a function
of temperature [66].
Source: John C. Wei, "High Temperature Creep of Pb-In Alloys. "
Dissertation in Materials Science, Stanford University, December 1 980.
1 25
Ph. D.
-3
Q)
ca
a:
c
.ca
!o.,..
+-'
+-'
(j)
C
0
.+-'
ca
C
Q)
"'C
c
+-'
'+-
0
C>
0
--l
ca
!o.,..
::J
+-'
ca
- 3.5
-4
- 4.5
-5
-5 . 5
-6
H/E(T)
0=58.0 kJ/mol
- 6.5
2 .8 2 .9
3. 1 3.2
1 /Tx1 03 ( K- 1 )
3.3 3.4
Figure 45. A plot of the natural log of the indentation strain rate at constant
values of RIG and HIE versus the reciprocal absolute temperature for In. The slope of
the line is equal to -QlRx l03 where Q is the apparent activation energy for creep. This
analysis yields lower activation energies than were determined u sing values of
indentation strain rate at constant hardness.
1 26
activation energies determined from the two analyses, which are roughly 20% different,
are simply within the scatter of the data being used for determining the apparent
activation energy for creep.
A second technique for determining the activation energy for indentation creep is
that of S argent and Ashby [ 1 3] which involves plotting the natural log of the hardness
determined at a constant time under load versus the reciprocal homologous temperature,
the slope of such a line being equal to Q/nRTm . Figure (46) is a plot of In H versus
TmIT for In over the homologous temperature range of 0.7 to 0.8 1 . An activation energy
of 74 kJ/mol is found from the slope of this plot. This value i s also in good agreement
with the activation energy for self diffusion in the material.
7.2.2.2 Aluminum
Hardness versus Tffm

Figure (47) is a plot of hardness versus homologous temperature for Al
calculated from the applied load and the displacement at 15 s. It is observed that over
the homologous temperature range of 0.3 1 to 0.56 the hardness decreases from 0.43 GPa
to 0. 1 7 GPa.
Apparent Activation Energy for Indentation Creep

Due to the limited range of indentation strain rates and hardnesses covered at
each temperature and the fact that the activation energy exhibits a stress dependence due
to the dislocation core diffusion taking place in the intermediate temperature range
studied, an accurate determination of the apparent activation energy for indentation
creep of Al based on the results of this study was unattainable. It was therefore decided
1 27
-3.4
Slope
en
"C
C
o
(.) -3.6
4 . 1 634
Q/n RT
Q=74 kJ/mol
(])
en
LO
@)
en
en
(])
c
-3 .8
"E
co
I
-4
-4.2
I nd i u m
.. ...
... ..
-4.4 ......
1 .2 1 .25
.....
1 .35 1 .4
IT
..
...
....
...
....
.........
1 .3
T
..
....
..
.-...
...
......
1 .45
Figure 46. A plot of natural log hardness at constant time under load versus the
reciprocal homologous temperature for In. The slope of the line is equal to Q/nRTm
where Q is the apparent activation energy for creep. An activation energy of 74 kJl mol
was determined from the slope.
1 28
0.5
........
..
....
...
1""'1"
...
....
"1"'
....
..
....
...
1""'1"
...
....
"1"'
....
.-..
....
..
...
0.45
.-.
ctS
a...
CJ
--
en
en
Q)
c
"'0
ctS
I
Q)
C)
ctS
Q)
0.4
0 .35
0.3
0.25
0.2
0. 1 5
Al u m i n u m
0. 1
0.3 0 .35 0 .4 0.45 0.5 0.55 0.6
Homologous Tem peratu re, T / T
Figure 47. A plot of average hardness versus homologous temperature for Al

over the homologous temperature range of 0.3 1 to 0.56.
1 29
to apply the effective diffusion coefficient model of Luthy et al [40] to the indentation
data to determine qualitatively the accuracy of the method for indentation creep data in
the intermediate homologous temperature range.
The effective diffusion coefficient theory of Luthy et al is defined in equation
( 1 4) and is based on all published diffusion data for AI, namely two different lattice self
diffusion coefficients and one dislocation pipe diffusion coefficient and the fraction of
atoms participating in each type of diffusion.
Two different lattice diffusion coefficients exist in the literature; one for high
temperature diffusion as determined by tracer diffusion, and one for intermediate
temperature diffusion as determined by void shrinkage methods . Luthy et al use a
bilinear relation for the lattice diffusion coefficient of the form
DL
1. ?xl O
-4
exp
( - 142 ) + 6xl O- exp( - 1 1 5 ) (m2

7
RT
RT
I s)
(49)
and assume that the fraction of atoms participating in lattice diffusion is approximately
1.
Luthy et al[40] define the core diffusion contribution as
(50)
where the coefficient for dislocation pipe diffusion was previously determined by Volin
et al[?3].
The problem then becomes one of defining fe , the fraction of atoms
participating in dislocation core diffusion.

According to Luthy et al [40] , the value of fe is equal to nplN where n is the
number of atoms contributing to core diffusion, N is the density of atoms per m2 , and p
1 30
is the dislocation density. n is assumed to be 4 from the work of Volin et al[73] while
the atomic density of AI is approximately l x 1 0 19 m 2 . The density of dislocations is
found by Luthy et al from the Taylor relation[74] which is given by
(5 1 )
w here a is the steady state stress and E is the Young's modulus. Two major problems
are associated with this analysis concerning the indentation creep test. First, the stress in
a constant load indentation creep test is not constant but rather changes throughout the
course of the hold period under constant load. Secondly, at these low homologous
temperatures, the measured hardness is certainly not indicative of a steady state flow
stress considering the fact that a characteristic strain of roughly 1 0% is associated with
the indentation.
With these factors in mind, the most logical choice for replacing (alE) in the
Taylor relation seems to be the instantaneous value of (Hl3E). Using this parameter
allows for the dislocation density to change as the hardness decreases during the
experiment. It seems only logical that as the hardness and strain rate decrease during the
experiment, the dislocation density in a volume of material at a normalized distance rlh
from the indenter, where r is the radial distance from the tip of the indenter and h is the
depth of the indent, would decrease as well.
Figure (48) is a plot of the temperature dependence of the modulus used in normalizing
the hardness data and for calculating the dislocation density from the modified Taylor
relation. Figure (49) is a plot of the dislocation density obtained for the range of (HIE)
encountered in the experiments on Al obtained using equation (5 1 ) to c alculate the
dislocation density replacing (alE) by (HI3E). The soundness of this range
131
--
E = 68.691 -0.039904T
R= 0. 99996
66
-
Cd
Q..
C!J
---
en
::::J
::::J
"'C
o
64
en
C)
c
::::J
o
62
>-
60
Al u m i n u m
58
50
1 00 1 50 200 250 300

Temperatu re (OC)
Fiure 48. A plot of Young's modulus versus temperature for Al[40].

Source: H. Luthy, A. K. Miller, and O. D. Sherby, Acta Met., 28, 1 69 ( 1 980).
1 32
Modi'fied Taylor Relation
p=2x1 02DX(H/3E)2
.-.
(\J
I
"-"
C
en
c
Q)
c
o
+=i
as
(.)
o
en
--
,.
"
I'
o
0. 004
0 . 006
0 . 002
0 . 008
H I E
Figure 49. Plot of dislocation density calculated from the Taylor relation by
replacing the normalized stress dependence, crlE, of the Taylor relation with (H/3E).
'.
133
- . ",
'
of dislocation densities can be examined by considering a similar analysis put forward

by Taylor[75] for the work hardening of metal crystals such as
AI.
Taylor assumed that
the average distance a dislocation moved before it was stopped was L. If the density of
dislocations after a given deformation is p . then the strain is given by
e=px Lxb
(52)
where b is the burgers vector. Rearranging this equation and solving for the dislocation
density, p, using a value of L= l x 1 O-4 cm from Taylor[75], a burgers vector for Al of 1 0
nm, and the characteristic strain of the Berkovich indenter of 0. 1 , an average dislocation
density of 1 x 1 0 1 3 m- 2 is calculated. This value is in fair agreement with that obtained
using the modified Taylor relation above.
The contribution of the core diffusion term to the effective diffusion coefficient
can then be written as
(53)
where the fraction of atoms participating in core diffusion is represented by the second
bracketed term which depends on the ratio of Hl3E from equation (5 1 ).
Figure (50) is a plot of the indentation strain rate normalized by the effective
diffusion coefficient calculated from equations ( 1 4), (48), and (52) versus the hardness
normalized for the temperature dependence of the modulus. Examination of the plot
shows that the effective diffusion coefficient approach seems to bring the data together
on to a single curve in an acceptable manner. Attempts to fit these data using the
hyperbolic-sine function of Gara(al ere nsuccessful. '
1 34
1 02
0
0 0
Al u m i n u m
::e
Q)
......
(J)
as
a:
c
as
J.+"""
+"""
C/)
.-
c
0
C9
21 C
1 0 0C
1 50 C
200C
250C
+"""
.Fg

tit
f II

,"1t
I.
..
as
C
(J)
'"0
c
+"""
HIE
(indentation strain rate divided by the effective diffusion coefficient) versus HIE for AI.
The ratio of the hardness divided by three times the modulus (Hl3E) was used in the
effective diffusion coefficient equation in calculating the contribution from the
dislocation core diffusion term.
1 35
An examination of the indentation strain rate hardness data shows that no

constant power law region of behavior is observed to exist for Al over the temperature
range investigated. An examination of the values of
ifDeff
obtained using the effective
diffusion coefficient shows temperature compensated indentation strain rates ranging

from 1 0 1 3 to 1 02 1 . B ased on the observation from S herby and Armstrong[ 1 2] that
power law breakdown is observed to occur in most metals at values of
i I Deff greater
than 1 09 , the entire range of data covered in these experiments is expected to be in the
power law breakdown regime .
7.3 Steady State Path Independent Hardness
7.3.1 Introduction
The central theme of this section of this dissertation is to investigate the
existence of a path independent steady state hardness in an indentation test utilizing a
geometrically similar indenter. It has been shown in uniaxial creep tests that the
substructural changes that occur during the creep process are insensitive to temperature
and depend only on time and stress[22] according to equation ( 1 5). This constancy of
microstructure for a given level of stress has been shown by incorporating stress-change
tests where the applied stress is abruptly changed once the steady state has been reached
as discussed in Chapter 2 and shown in Figure (2). Analogous data from Pip change
experiments will be presented. The results will be analyzed and discussed based on
comparison to the stress change tests from bulk uniaxial creep testing.
1 36
7.3.2
pip change Tests on Indium

In order to test the hypothesis that a steady state value of hardness could be
reached that depends only on the imposed strain rate and temperature, a set of
experiments was conducted using the constant Pip loading technique that was
previously discussed. However, rather than maintaining the value of Pip constant
throughout the entire loading segment, Pip change experiments were conducted in
which the value of Pip was abruptly changed from an initial value to a new value at a
predetermined displacement. This type of experiment allowed the response of the
material to changes in the imposed indentation strain rate to be determined.
Figure (5 1 ) is a plot of the resulting indentation strain rate, calculated as the
instantaneous displacement rate divided by the instantaneous displacement, versus
displacement for the Pip change experiments. The initial indentation strain rate is
again observed to be constant and equal to 0.5 Pip . Upon a change in Pip , the
indentation strain rate is observed to go through a transient period and then approach a
new constant
izlh after a delta displacement of approximately 500 nm.
Figure (52) is the resulting hardness versus displacement for the Pip change
experiments. The measured hardness resulting from the Pip change is also observed to
undergo a transient period and then approach the indentation steady state value from the
constant Pip experiments. The displacement required seems to be somewhat a function
of whether Pip was increased or decreased. The delta displacement required to reach
the indentation steady state value at a Pip of 0. 1 is approximately 1 000 nm after the
Pip increase from 0.02 while the additional displacement required on going from a
Pip of 0. 1 to 0.02 requires nearly 2000 nm of displacement.
The requirement of additional strain rather than a characteristic time to reach a
new indentation steady state value of hardness can be understood by reexamining the
1 37
I nd i u m
(f)
,(S- l )
.
Q)
ro
a:
c
ro
'......
.-
-<>- 0 . 1
......
CJ)
c
0
'+=i
ro
c
Q)
'1J
C
-0-- 0 . 02
......
0.02->0. 1
0 . 1 ->0.02
1 0- 2
2000
4000
3000
Displacement (nm)
5000
Figure 5 1 . A plot of indentation strain rate versus displacement for Pip change
experiments on In. The indentation strain rate is observed to go through a transient
period and then reach a new indentation steady state value after the Pip change.
1 38
0.03
--e- 1 . 0
0.028
0.026
en
en
(])
c:
"C
ctS
I
-0- 0 . 1
-0-
0.02
0.02
->
0.1
ctS
c..
CJ
,(S-1)
0.024
0 . 022
0.02
0.01 8
I ndium
O. 0 1 6 1oooI..I..L.L..L.L.L
.I.
...I...&.
.I-I
.L.II...L.I.I..I.
.I
&.
.L.
.I..L.L
.&..L.
..L.L.L....
2000
4000
3000
Displacement (nm)
5000
Figure 52. A plot of hardness versus displacement for Pip change tests on In.
In a manner analogous to the indentation strain rate, the hardness is observed to go
through a transient period after the Pip change and then to reach a new steady state
value with further displacement.
1 39
indentation process. As previously discussed, the plastically deformed volume in the

indentation test is continually expanding into previously undeformed material. The
indentation steady state is therefore always being approached from a hardening direction
rather than a softening direction, even when pip has been decreased.
It is interesting to compare the pip change indentation experiments to the
uniaxial stress change experiments shown in Figure (2). While the transient response as
well as the progression to a new steady state is very different in the indentation and
uniaxial tests, comparison of the indentation pip change experiments to the uniaxial
stress change experiments reveals remarkably similar behavior between the two.
7.4 Comparison to Uniaxial Data
7.4.1 Introduction
While indentation creep testing is a viable technique for comparing the time
dependent properties of materials that cannot be characterized by standard bulk
techniques, how the indentation creep results can be compared to uniaxial creep data is a
subject of major importance. This section presents and discusses on an empirical level
how the indentation creep data and the uniaxial data compare. The specific ideas of
relating the indentation creep data to its uniaxial counterpart based on the ideas of ( 1 ) a
constraint factor relating the hardness and the uniaxial flow stress, (2) a characteristic
strain associated with the Berkovich indenter, and (3) a constant relating the indentation
strain rate to the uniaxial strain rate will be explored.
140
7.4.2 Pb-65 at % In
In order to directly compare the indentation creep data obtained for Pb-65 at% In
to uniaxial data, a series of compression tests were performed on the bulk alloy. Figure
(53) shows the stress-strain results for a series of uniaxial compression tests performed
at a variety of constant cross head speeds. Figure (54) shows the corresponding stress
strain rate results as a function of strain. Note that the stress exponent that one
determines from the compression data is highly dependent on the percent strain at which
the stress-strain rate pairs are tabulated.
Figure (55) is a plot of the indentation creep for Pb-65 at% In data along with the
uniaxial compression data at strains of 1 0 and 80%. According to Tabor[68], the
indentation hardness of a material should be approximately 3 . 3 times its strength at a
characteristic strain of 8- 1 0%. When the indentation hardness data for Pb-65 at% In are
divided by 3.3 and plotted versus the indentation strain rate along with the compression
stress-strain rate data at 1 0 and 80% strain, the plot shown in Figure (56) results. The
similarity of the indentation creep data to the uniaxial data at 10% strain implies that
indentation creep strength measured with this type of experiment can be represented by
the flow strength of the material when strained approximately 1 0%. This implies that
the indentation creep experiments as conducted on Pb-65 at% In, i.e., Step Load/Hold
experiments, are most likely measures of transient, and not steady state behavior. These
data suggest that the constraint factor and the concept of a characteristic strain seem to
be reasonably valid for Pb-65 at% In.
7.4.3 Indium
Since the constant Pip indentation experiments yield an indentation steady state
hardness, this type of experiment is believed to most closely approximate the results
141
50
-
co
c..
:E
40
en
en
(])
'-
......
30
co
'x
co
c
20
en
:::J
10
0.2
0.4 0.6
Strain
0.8
Figure 53. A plot of stress versus strain from uniaxial compression experiments
run on Pb-65 at% In alloy at a variety of crosshead speeds. The decrease in the stress
with increasing strain is believed to be due to dynamic recrystallization at the lower
strain rates due to the high homologous temperature.
142
1 0- 1
Pb - 65 at% I n
-0
......
I
1 0- 2
CJ)
----
-0-
%
80
0%
4
20 %
1 0%
Stra i n
Stra i n
Stra i n
Stra i n
Q)
+-'
CO
a:
c
ffi
s...
+-'
1 0- 3
CJ)
CO
X
CO
0-
::::>
1 0- 4
U niaxial Stress (G Pa)

Figure 54. A log-log plot of stress versus strain rate as a function of strain for
uniaxial compression tests on Pb-65 at% In. The stress exponent is seen to be highly
dependent upon the level of strain at which it is detennined.
143
Pb 65 atO/o I n
-
--0-
U niaxial Data @
-0-
Uniaxial Data @
1 0%
80%
Strain
Strain
I ndentation C reep Data
....
I
Q)
ca
a::
.c
+-'
(J)
1 0- 5
2
1 01 0- 1
U niaxial Stress or Hardness (G Pa)
___...-_____
______...-_
Figure 55. A log-log plot of indentation strain rate versus hardness and uniaxial
strain rate versus stress at 1 0 and 80% strain for Pb-65 at% In. The indentation creep
data are seen to display similar behavior to the uniaxial data at 1 0% strain.
144
Pb 65 at% I n
-
-0-
---0-
T""
en
'-'
U niaxial Data @ 1 0% Stra i n

Un iaxial Data @ 80% Strain
I ndentation C reep Data
1 0- 2
Q)
.......
a:s
a::
c:
.
-
a:s
.......
(/)
1 0- 3
0. 1
Un iaxial Stress or Hardness/3.3 (G Pa)
Fiure 56. A log-log plot of indentation strain rate versus hardness/3 .3 and
uniaxial strain rate versus stress at 10 and 80% strain for Pb-65 at% In. The constraint
factor of Tabor is seen to bring the two curves closer to coincidence but does not fully
account for the observed difference.
145
from the constant stress tensile experiments and will therefore be compared to the
steady-state uniaxial data.
Figure (57) is a log-log plot of both the indentation pip data and the constant
stress tensile data obtained by Weertman[39] at room temperature. Both the uniaxial
data and the indentation data are seen to exhibit constant power law behavior. As
previously discussed, the stress exponents obtained from the two types of data are for all
practical purposes identical, however, a finite offset is observed to exist between the
uniaxial and indentation data.
Figure (58) is a log-log plot of the temperature
compensated uni axial strain rate versus uniaxial stress plotted along with the
temperature compensated indentation strain rate versus the hardness. The data have
been compensated for temperature using the activation energy for self diffusion, 75
kJ/mol [39] .
A slightly lower value for the stress exponent is observed for the
indentation data as compared to the tensile data at room temperature when compared on
a temperature compensated strain rate basis.
Figure (59) is a log-log plot of the steady state uniaxial strain rate versus uniaxial
stress and indentation strain rate versus hardness/3 .3 according to the analysis of Tabor.
The constraint factor is again observed to bring the two sets of data closer together but
does not completely account for the observed difference.
The steady state like behavior of the constant pip data can be better understood
by considering the observations of Weertman who found that the creep rates of In were
typically found to be constant over a wide range of strain, typically 5 to 25%. Recalling
that the characteristic strain of a Berkovich indenter is approximately 8 to 1 0%, the
strains experienced in the indentation creep test were perhaps of sufficient magnitude to
reach steady state conditions in the material. This is in direct contrast to the Pb-65 at%
146
--GJ- Weertman , Constant Stress

--C- This Study, Constant
pip
..,....
I
7.3
en
--
(J)
ct:I
a:
c
"ct:I
So...
......
......
(f.)
I nd i u m
.1. ..
... ..
.. ..
.. ..
.. ..
... ..
.. ..
... ..
.. ..
1 0. 5 oo._--.....
1 0.3
1 0. 2
Stress or Hardness (G Pa)
......
Figure 57. A log-log plot of indentation strain rate versus hardness for constant
Pip experiments on In plotted with tensile strain rate versus stress data from
Weertman[39].
Source:
1.
Weertman, Trans. of AIME, 218, 207 ( 1960).
147
.,.....
I
1 01 5
CIJ
EEl
Wee rtma n , Constant Stress
<)
Th i s Study, Constant
Q)
ro
a::
OC
ro
....
......
EE
EEl
......
CJ)
"'C
Q)
......
ro
CIJ
c
Q)
a.
pip
<>
<>
<>
()
<)
JW
EEl EEl
Eil
EEl
EBEE
ffitJEEl
()
Q)
t!
....
::J
......
EE
EEl
ro
....
Q)
a.
EEl
I nd i u m
Q)
I-
3 EEl
1 Q -4
10
Stress or Hardness (G Pa)
Fiure 58. A log-log plot of temperature compensated indentation strain rate
versus hardness for constant Pip experiments on In plotted with temperature
compensated tensile strain rate versus stress data on In from Weertman[39] .
Source:
1.
Weertman, Trans. of AIME, 218, 207-2 1 8 ( 1 960).
148
--ITl-
Weertman , Constant Stress
This Study, Constant
pip
.-..
en
1 0- 2
(J.)
+oJ
ctS
a:
c:
.
ctS
"-
+oJ
C/)
1 0-
I nd i u m
1 0-5
1 0- 3
1 0- 1
1 0- 2
Stress or Hardness/3.3 (GPa)
_....i....i-........
i.---a..--a......&.r...
...O
....
.&.
..
..
....
..
.
Figure 59. A log-log plot of indentation strain rate versus hardness/3 .3 for
constant Pip experiments on In plotted with tensile strain rate versus stress data from
Weertman[39] .
Source: J. Weertman, Trans. of AIME, 218, 207-2 1 8 ( 1960).
149
In data where 1 0% strain is observed to be still in the transient region of the stress strain
curve.
Another method for relating the indentation data of a power law creeping solid to
its uniaxial counterpart is that of Bower et al[76] who used finite element modeling to
arrive at an expression for the 'effective stress' and 'effective strain rate' under the
indenter. Their effective stress is taken as the contact pressure or hardness, and the
effective strain rate is determined by the shape of the indenter and the displacement rate.
The effective stress is assumed to be related to the effective strain rate by the uniaxial
stress-strain response. Figure (60) is a plot of the Bower factor for relating indentation
and uniaxial strain rates
as
a function of the stress exponent. The data are observed to
follow an exponential increase as the stress exponent decreases. Assuming that the
hardness is equal to the uniaxial stress, the indentation strain rate divided by the Bower
factor should yield the uniaxial strain rate. Figure (6 1 ) is a plot of the indentation data
modified according to the appropriate Bower factor determined from an exponential fit
to the line in Figure (60). The Bower factor serves to shift the indentation strain rate
nearly four orders of magnitude on the strain rate axis. While this modification factor
also serves to bring the two sets of data closer together, it also fails to completely
reconcile the observed differences .
While the offset between the two sets o f data cannot be completely accounted for
by either constraint factors [68] or by predictions from time dependent finite element
calculations[76], the utility of the constant Pip indentation data is evident. The most
often sought after parameter in these types of experiments is how the rate of deformation
of the material changes in response to a change in the applied stress, Le., the stress
exponent for creep. From the comparison of the two sets of data it is obvious that the
stress exponent obtained from the two types of experiments is very similar.
1 50
6 .297 5 e
(- 1 .2093x)
'+
t)
ctJ
u..
Q)
o
al
Stress Exponent, n
Fiure 60. A plot of the Bower factor[76] for relating indentation strain rate to
uniaxial strain rate versus stress exponent for creep.
Source: A. F. Bower, N. A. Fleck, A. Needleman, and N. Ogbonna, Proc. R.
Soc. Lond. A,
441,
97 ( 1 993).
151
..
I
en
--10-
.....
--rn- Wee rt man , Constant Stress
()
ctS
LL
Mod ified by Bowe r Facto r
Q)
I nd i u m
0:
1 0 - 5 1-2
3
1 01 01 0- 1
Uniaxial Stress or Hardness (G Pa)
...&.....
.&
.._1---10
..
..
..
....
...
...
..
...
_"'-""'--......
Figure 6 1 . Log-log plot of indentation strain ratelBower factor versus hardness

for constant Pip experiments on In plotted with tensile strain rate versus stress data
from Weertman[39] .
Source: J. Weertman, Trans. of AIME,
1 52
218,
207-2 1 8 ( 1960).
7.4.4 Aluminum
Figure (62) is a log-log plot of temperature compensated indentation strain rate
versus hardness for Al plotted along with the steady state torsion and tension data of
Luthy et a1[40] . Figure (63) is a plot of the indentation creep data for Al where the
hardness has been modified by the constraint factor of Tabor[68] again plotted along
with the steady state data from Luthy et al as well as uniaxial stress strain rate data from
Trozera et al[77] tabulated at a strain of 1 0%. The constraint factor serves to bring the
two sets of data closer together, especially at the higher strain rates, but cannot account
completely for the offset. Two things must be kept in mind regarding this set of
indentation data.
First, it must again be kept in mind that the indentation data represent a constant
strain of approximately 1 0% . While at high homologous temperatures this level of
strain may be sufficient to reach steady-state conditions, this is not the case for AI.
From 0.2 to 0.6 Tff m, strain hardening is the dominant feature of plastic flow in AI.
This fact leads to experimental difficulties in obtaining steady state flow stresses since
extremely large strains are required to reach steady state[40]. The data from Luthy et al
were all obtained in torsion requiring large strains to reach steady-state, typically on the
order of 1 00 to 200%. It is therefore unrealistic to expect that the indentation data in the
same homologous temperature range should reflect the steady-state properties obtained
from the bulk testing at all, rather, the data should more likely represent the properties of
the material having undergone approximately 10% strain which is likely far from steady
state conditions. At small strains, such as 1 0%, the stress for a given strain rate is
expected to be significantly lower than the steady state flow stress. This would result in
apparently higher stress exponents for creep than would be obtained at higher strains as
exemplified by the data of Trozera et al[77] . As the temperature of the material is
153
.-....
C\I
I
--
Al uminum
.....,
.
<>
C
<D
-
()
This Study. C R UHold

Luthy, Torsion and Tension
!E
<D
o
()
c
o
CJ)
::J
"I
"l.
<D
>
t5
<D
"I
"I-
LU
;;<D
ct'S
a::
c
.....,
.....,
CJ)
1 0 1 3 __
1 0- 3
1 0- 4
1 0- 1
Stress/E or Hardness/E
Fiure 62. A log-log plot of indentation strain rate divided by the effective
diffusion coefficient versus
HIE
for Al plotted with bulk data obtained in torsion and
tension from Luthy et a1[40].

Source: H. Luthy, A. K. Miller, and O. D. Sherby, Acta MeL, 28, 1 69 ( 1 980).
1 54
<>
This Study, CRUHold, H/3 . 3

Luthy et ai, Steady State
Troze ra et ai , 1 0% Strain
1 01
____
1 0- 4
.-
3
1 01 0-2
Stress/E or Hardness/3.3E
__
Figure 63 . A log-log plot of indentation strain rate divided by the effective

diffusion coefficient versus Hl3 .3E for AI plotted with bulk data obtained in torsion and
tension from Luthy et al[40] and Trozera et a1[77].
Source: H. Luthy, A. K. Miller, and O. D. Sherby, Acta Met., 28, 1 69 ( 1 980).
T. A. Trozera, O. D. Sherby, and J. E. Dom, Trans ASM, 49, 1 73 ( 1 957).
1 55
raised, the required strain to reach steady state behavior is expected to decrease. This
would result in a stress closer to the steady state value being obtained at lower strains.
The comparison of the indentation creep data on Al seems to follow this
explanation. At low homologous temperatures, the stress exponent obtained from the
indentation data is observed to be similar to that obtained from the 1 0% data of Trozera
et al. As the temperature is raised, the stress exponents are observed to approach those
obtained from the steady state data of Luthy et al. Why the constraint factor of Tabor
does not appropriately account for the observed differences between the indentation and
uniaxial data at low temperatures can perhaps be explained by considering that the
surface of the Al was not in a well annealed state as was expected but had residual work
hardening due to the mechanical polishing. This could result in hardness values
corrected by the constraint factor being closer to the steady state values of stress as is
observed since the flow stress would not change nearly as dramatically as a function of
strain.
S econdly, these data were acquired using the CRLfHold technique.
This
technique has been seen to result in a transient period on completion of the load ramp
yielding higher apparent stress exponents during the initial stages of the hold period
under constant load. At smaller fractions of the melting temperature, these transients
could be expected to persist longer into the hold period resulting in abnormally high
stress exponents being observed well into the hold period, i.e., the hardened
microstructure due to the higher strain rates simply does not have sufficient thermal
energy to recover. Examination of the transient region for the elevated temperature data
on In does seem to suggest that
as
the temperature is increased, the harness-strain rate
behavior comes to a constant power law relation more quickly.
1 56
Chapter 8 Indentation Creep - Conclusions and

Suggestion for Future Research
8.1 Conclusions
U sing a variety of depth-sensing indentation techniques at both room and

elevated temperatures, the dependency of the indentation hardness on the variables of
indentation strain rate (stress exponent for creep, n) and temperature (apparent activation
energy for creep, Q), and the existence of a steady state behavior in an indentation creep
test with a Berkovich indenter were investigated. The indentation creep response of five
materials , Pb-65 at% In (at RT) , high purity indium (from RT to 75C), high purity
aluminum (from RT to 250C), a vapor deposited amorphous alumina film (at RT), and
single crystal alumina (sapphire) (at RT), was measured.
It was shown for the first time that the indentation strain rate, defined as
iz/h,
could be held constant during an indentation experiment using a Berkovich indenter by

controlling the loading rate such that the loading rate divided by the load,
remained constant.
The constant
Pip technique
Pip,
yields the most unambiguous
determination of the stress exponent for indentation creep and seems to most closely
approximate the steady state results from uniaxial testing.
Comparison of the results from the constant
Pip experiments
to the results from
conventional CRLlHold indentation creep experiments in Figure (30) shows that the
transition from the load ramp to the hold period under constant load shows a brief period
with an apparent higher stress exponent for creep. This feature is now believed to be
due a transient stage on going from the load ramp to the hold under constant load and
not to be associated with power law breakdown behavior. This is supported by the fact
1 57
that even at higher strain rates the Pip data obey a constant power law relationship.
The experiments conducted at different constant loading rates to the same maximum
load show that even though the indentation strain rates and hardnesses experienced
during the load ramps are very different, the indentation strain rate-stress data during the
subsequent hold period under constant load converge to a single curve after an initial
transient period.
The similarity of the stress exponent obtained from the constant Pip and
CRLlHold experiments and the offset in the hardness leads to two conclusions. One, the
dominant factor in both types of experiments seems to be the stress exponent for creep.
Secondly, the data from the CRL/Hold experiments appears to have a stronger
microstructure as indicated by the higher hardness determined at the same strain rate.
This result is expected due to the higher strain rates experienced by the material during
the experiment.
Comparison of the stress exponents obtained from the hardness versus time data,
Figure (26), and the indentation strain rate versus hardness data, Figure (30), for In
shows that a similar value for the stress exponent is obtained from the two analyses,
except at short loading times. While both techniques seem to yield similar results, the
relationship between the indentation strain rate and the hardness is based on a valid
material constitutive law.
The measurements of the stress exponents for creep on amorphous alumina and
sapphire demonstrate the indentation test's unique ability to measure differences in the
time dependent response of materials that cannot be tested with other techniques. The
ability to obtain information into the time dependence of flow from these materials alone
attests to the value of the indentation creep technique.
1 58
The indentation strain rate - hardness data for In at high homologous

temperatures obtained using the CRLlHold technique display a stress exponent of 5 in
excellent agreement with that obtained for high temperature uniaxial creep where
dislocation climb is the rate controlling mechanism[4].
The apparent activation energy for indentation creep in indium was found to be
approximately 78 kJ/mol, in excellent agreement with the activation energy for self
diffusion in the material. Temperature compensating the indentation strain rate using
the experimentally determined activation energy is seen to bring all of the data at the
various temperatures together onto single master curve supporting the hypothesis of a
single thermally activated rate controlling mechanism.
The technique for determining the activation energy for indentation creep of
S argent and Ashby [ 1 3] , which involves plotting the natural log of the hardness
determined at a constant time under load versus the reciprocal homologous temperature,
yields an activation energy for indentation creep of 74 kJ/mol for In. This value is also
in good agreement with the activation energy for self diffusion in the material. In light
of the transient period that exists on going from the load ramp to the hold period, caution
must be exercised to ensure that the hardness versus time data are obtained at times
greater than the relaxation time. As the relaxation time scales with the loading time, the
time required to apply the load would seem to be a logical lower limit on data obtained
using this technique.
The indentation strain rate - hardness data for Al show an appropriate decreasing
trend in the stress exponent for indentation creep as the test temperature is raised. The
temperature dependence of the indentation creep process was found to be reasonably
well described by an effective diffusion coefficient as described in the literature [40] for
bulk aluminum at intermediate temperatures.
1 59
By perfonning pip change experiments it was shown that a steady state path
independent hardness could be reached in an indentation test with a geometrically
similar indenter. The arrival at a new steady state value of hardness seems to depend on
the accumulation of strain rather than a relaxation time. Comparison of the pip change
indentation experiments to the uniaxial stress change experiments show that while the
transient response as well as the progression to a new steady state are very different, the
two types of experiments show remarkably similar behavior.
A final of discussion is how specifically the simple ideas of a characteristic
strain, constraint factor, and constant relating the indentation strain rate to the uniaxial
strain rates are either upheld or disputed. To begin, it is important to point out that no
clear cut method still exists for comparing indentation creep data to uniaxial creep data.
However, comparing the indentation data from this study to both the experimental and
literature data does reveal some important insights. Certainly in the case of the Pb - 65
at% In data at room temperature, a direct comparison with the uniaxial data at 1 0%
strain shows the most promising correlation suggesting that those data are representative
of small strain plasticity. If the hardness is divided by 3.3 and plotted along with the
uniaxial data, the two sets of data are observed to come remarkably close to one another.
The issue simply becomes with these two sets of data, "How close is close enough?"
The comparison of the indium data to the uniaxial data from the literature also shows
that the constraint factor serves to bring the two sets of data closer together, again
j ustifying the concept. The steady state like behavior of the constant pip data can be
better understood by considering the observations of Weertman who found that the creep
rates of In were found to
be
constant over a wide range of strain, typically 5 to 25%.
Recalling that the characteristic strain of a Berkovich indenter is approximately 8 to

1 0%, the strains experienced in the indentation creep test were perhaps of sufficient
1 60
magnitude to reach steady state conditions in the material. This is in direct contrast to
the Pb-65 at% In data where 1 0% strain is observed to be still in the transient region of
the stress strain curve. The correlation of the indentation creep Al data to the uniaxial
data can also be explained by considering the characteristic strain concept.
As
previously discussed, over the temperature range studied, the dominant feature o f the
stress-strain behavior of Al is work hardening[77]. Therefore, at small strains, such as
10% , the stress for a given strain rate is expected to be significantly lower than the
steady state flow stress. This would result in apparently higher stress exponents for
creep than would be obtained at higher strains. As the temperature of the material is
raised, the required strain to reach steady state behavior is expected to decrease. This
would result in a stress closer to the steady state value being obtained at lower strains.
The comparison of the indentation creep data on AI seems to follow this explanation. At
low homologous temperatures , the stress exponent obtained from the indentation data is
observed to yield higher stress exponents at similar strain rates similar to that of the
small strain data of Trozera et al[77]. As the temperature is raised, the stress exponents
are observed to approach those obtained from the steady state data of Luthy et al[40] .
Why the constraint factor does not serve to more appropriately account for the observed
differences is can perhaps be explained by the fact that the surface of the Al sample was
still in a work hardened state from the mechanical polishing. This would result in less
work hardening and hardnesses closer to the uniaxial steady state data. An interesting
note is that even though the indentation data appears to go from a transient like to steady
state like behavior over the range of temperatures studied, temperature compensating the
data based on the effective diffusion coefficient concept is observed to bring the data
together onto a single master curve suggesting that the mechanisms responsible for the
deformation are the same in the indentation test.
161

In light of the results from this work, several opportunities exist for extending the
study of indentation creep.
First, it would be most interesting to repeat the experiments at the elevated
temperatures using the constant
Pip
loading technique. This would allow a more
thorough study of the temperature dependence of indentation creep at these temperatures

without the ambiguities associated with the changing indentation strain rate and
hardness.
An important additional amount of work, now that the experimental details have
been worked out, would be to perform experiments that specifically test the ideas of
characteristic strain, constraint factor, and constant relating indentation strain rate to
uniaxial strain rate. An example would be a series of indentation experiments on
specimens that have been pre-strained various amounts, for instance, Al at room
temperature tested at a variety of strain rates. By performing tests out to 1 0% strain
increments, then performing indentation creep tests on the pre-strained samples, the
concept of a characteristic strain could perhaps be more fully investigated.
An even more challenging study would be to attempt to perform constant strain
rate indentation experiments with a spherical indenter where the strain is changing as a
function of depth rather than remaining constant as is the case for the geometrically
similar indenters.
Information on how the indentation data can then be related to
uniaxial stress-strain data could then perhaps be obtained.

While the indentation creep technique has been proven to yield appropriate stress
exponents for both viscous flow (n= l) and dislocation climb controlled creep (n=5), no
experiments have been performed on an alloy where dislocation glide (n=3) is expected
to be the rate controlling mechanism. An exciting extension of this would be to perform
1 62
experiments on a material that is known to undergo a glide to climb controlled transition

where the stress exponent is expected to change.
One aspect of the constant Pip experiment that was not addressed in this study
is the transient associated with reaching an " indentation steady state. " In a constant
strain rate uniaxial test, the stress gradually builds up with time until such a point when
the rate of hardening is balanced by the rate of recovery. How the dynamics of the
indentation experiment manifest themselves in the transient response of the material is
certainly a point of interest.
Another exciting aspect in the continuation of this work would be an upgrade of
the HTMPM to allow indentation creep properties to
be
investigated at higher absolute
temperatures. Certainly in the case of AI, the temperature regime accessible with the
current capabilities of the HTMPM is in the most complicated of all temperature regimes
for creep. The ability to achieve higher operating temperatures would allow a wider
range of relevant engineering materials to be investigated at high homologous
temperatures.
Obviously, these experimental techniques are aimed at the characterization of the
creep properties of thin films and small volumes of material that cannot be characterized
by existing bulk techniques. The creep properties of thin films may be very different
from their bulk counterparts due to the different diffusion paths and microstructures.
The understanding of the elevated temperature creep properties of these films would
yield vital information to the microelectronics industry that cannot perhaps be obtained
from any other technique.
1 63
Chapter 9 Developing Indentation Viscoelasticity

Constitutive Equations
9. Introduction
As discussed in Chapter 2, one phenomenological description for analyzing data

from bulk viscoelastic testing techniques is given by a set of equations describing the
dynamic response of the material as a function of frequency. In order to relate the
response measured in a frequency specific indentation test to that measured in the bulk,
an analogous set of equations for describing the response measured with the indentation
test is required.
9.1 Analysis of Indentation Data
The technique for measuring the viscoelastic properties of materials with depth
sensing indentation techniques involves an extension of the dynamic indentation
technique developed by Pethica and Oliver[78] for continuously monitoring the stiffness
of the contact between the indenter and the materiaL The technique involves applying
an oscillatory force to the indenter and measuring the amplitude and phase angle of the
displacement response at that frequency and is more completely described in Appendix
A dealing with dynamic modeling. However, in order to more completely describe the
properties of a viscoelastic material, it is desirable to appropriately account for the
mechanical losses that are occurring in the material as well. This is accomplished by
modeling the contact between the indenter and the specimen in terms of a frequency
dependent parallel spring and dashpot rather than a simple elastic element as was done
1 64
by Pethica and Oliver. This allows for the damping properties of the specimen to be
considered in the analysis.
The dynamic analysis of the indentation test can proceed in a manner similar to
that outlined in the formal theory of viscoelasticity. The difference in the analysis is that
in the indentation experiment the geometry of the test is dealt with according to contact
mechanics in order to arrive at values for moduli. The analysis begins by writing the
equation for Hooke's law in terms of complex notation, i.e.,
*
F = (S + iCm)h
(54)
where F* is the complex force, S is the storage or in-phase portion of the stiffness, Ceo is
the viscous or out-of-phase portion of the stiffness and h* is the complex form of the
displacement response. The result that is of interest is
II
G* = G ( m ) + iG ( m )
I
(55)
where G* is the complex modulus given by the sum of the storage part of the modulus
G' due to the stiffness S and the loss part of the modulus Gil due to the damping Ceo.
If an oscillatory force of the form F=Foe(icot) is applied to the system, a

displacement response of h=hoe(iol+q,) is obtained. A simple direct analysis can be
constructed by considering the response equations for the dynamic system as given by
Pethica and Oliver[78] but considering the more complex model for the material that
includes both spring and dashpot elements. The analysis begins by writing equations
(63) and (64) from Appendix A for the amplitude and phase angle as
1 65
(56)
and
tan
roCeq
Keq - mro2
(57)
where Keq is the equivalent stiffness of the spring elements in the model (contact,
indenter support springs, and load frame) and Ceq is the equivalent damping coefficient
of the viscous elements in the model (contact and air in capacitive gap). By combining
these two equations it is possible to solve explicitly for Keq and Ceq in terms of the
amplitude and phase response. This analysis results in the expressions
(58)
and
Fo S Ill At'f' Ce ro
q
flo
(59)
These two equations can be expanded if the equivalent stiffness and damping
coefficients are replaced by the appropriate quantities. Equations (58) and (59) then
become
1 66
(60)
and
Fo sin </> (Cro) - (C ro)

i
ho
(6 1)
Equations (60) and (6 1) can be solved independently for the stiffness of the contact, S ,
and the damping coefficient o f the contact, Coo, b y separating the displacement response
of the indenter to the oscillating force into the in-phase and out-of-phase components
respectively.
1 67
Chapter 10 Indentation Viscoelasticity

Materials/Sample Preparation
The material used in this study was an unvulcanized natural rubber or Hevea
Rubber. It is obtained from the latex (or milk) of the tree Hevea brasiliensis. It has the
chemical structure poly-cis l ,4-isoprene as shown below
Natural rubber is amorphous and rubbery at room temperature. It flows above 60C and
crystallizes on cooling below OC or upon stretching. It has a density of approximately
1 200 kglm3 and a glass transition temperature of -72 C. Polyisoprene was chosen for a
variety of reasons; 1 .) due to its tack, it was possible to have stable contact areas under
conditions of nearly zero load, and therefore zero creep; 2.) due to its relatively high loss
modulus, Gil, at room temperature, 0.029 MPa, as compared to a storage modulus, 0', of
0.4 1 MPa[79], and; 3.) its dynamic behavior has been well documented over a wide
range of frequencies [80].
The polyisoprene specimen was obtained in bulk form. The specimen was
prepared for indentation by mechanically shearing the surface in a manner similar to
microtome preparation. The actual rms roughness of the surface is not known but is not
expected to effect the results due to the large depths of indentation used for the study.
1 68
Chapter 1 1 Indentation Viscoelasticity - Experimental

Techniques
11.1 Introduction
Two distinct types of indentation experiments were conducted to investigate the
response of polyisoprene both as a function of the excitation frequency (Constant
Contact ArealVariable Frequency) and as a function of the size of the contact area
between the indenter and the material (Constant FrequencyNariable Contact Area). All
of the experiments were conducted at room temperature (T=23.9C) on a Nano
Indenter II operating in a frequency specific indentation mode. The fundamentals of
the operation of the instrument in this mode may be found in Appendix A, in Pethica
and Oliver[78], or in Oliver and Pharr[3].
11.2 Constant Contact Area/Variable Frequency

Figure (64) is a typical load versus time history for a constant contact
area/variable frequency experiment. This experiment was designed to investigate the
frequency response of polyisoprene at a constant contact area. The experiment consisted
of the following:
1 . The indenter approached the surface at a constant velocity of

10 nmls until contact was detected.
2. The load on the indenter was then increased at a constant
loading rate to a predetermined maximum loads of either 1 50,
300, lor 45 0
I..LN.
1 69
Constant Contact ArealVariable Frequency
z
E
---
"'C
<0
o
.....I
0.00 1
- 0.00 1
50
1 00 1 50 200
Tim e (s)
3600
Figure 64. A plot of a typical load time history for constant contact area/variable
frequency experiment conducted on polyisoprene.
1 70
3. The load on the indenter was then held constant for a 15 s

period during which the displacement versus time response
was monitored.
4. The load on the indenter was then decreased at a constant

unloading rate to a predetermined minimum load.
5. The load on the indenter was again held constant for a 1 5 s
period during which the displacement versus time response
was monitored.
6. The load on the indenter was then increased back to
approximately zero load, i.e., the initial load at the point of
contact.
7. The load on the indenter was then held constant for a period of
1 hr during which the dynamic scan through the spectrum of
frequencies was performed.
8. The indenter was unloaded at a constant unloading rate until the
contact between the indenter and the material was broken . .
The dynamic scan through the range of frequencies during Segment 7 of the experiment
was conducted in a single frequency mode using an EG&G 5302 digital signal
processing CDSP) lock-in amplifier. The range of frequencies investigated was from 50
mHz to 500 Hz. At the outset of the experiment, the phase angle between the output of
the oscillator of the lock-in amplifier and the measured force oscillation actually being
sent to the load application coil was set to zero degrees. All of the data were then
acquired by first measuring the actual force excitation at the excitation frequency and
maintaining the phase angle between the output of the oscillator and the measured force
171
at zero degrees In actuality, the stability of the oscillator never required the phase angle
between the output of the oscillator and the resulting force oscillation to be reset after an
initial set at the beginning of the experiment. The displacement response to the force
excitation was subsequently measured as well as the phase angle between the two.
While a measurement of the amplitude of both the in-phase and out-of-phase
components was available from the lock-in amplifier, the difference in magnitude of the
two components and the inability to set the sensitivity of the measurement
independently prevented this feature from being used. Measurements were made at a
frequency of 0.5 Hz at the beginning of the 1 hour hold period, at the 30 minute mark,
and at the end of the hold period to ensure that the size of the contact was in fact
remaining stable.
11.3 Constant FrequencyNariable Contact Area

In order to more clearly define the relationship between the damping coefficient,
Coo, and the area of contact between the indenter and the material, a second type of
experiment was performed in which the frequency of the excitation was held constant as
the indenter was loaded into the material. This experiment consisted of loading the
indenter at a rate of approximately 10 nmls while applying an oscillatory force at a fixed
frequency of 1 . 1 Hz and a fixed force excitation of 1 .5 J.!N. This type of experiment
allowed the dynamic response of the material to be characterized as a function of depth
at a constant frequency.
172
Chapter 12 Indentation Viscoelasticity - Results and

Discussion
12.1 Introduction
The central theme of this chapter of this dissertation is to present the results of
the frequency specific indentation measurements made on bulk poly isoprene.
Experiments from both constant contact area/variable frequency and constant
frequency/variable contact area experiments will be presented in an attempt to
quantitatively measure the viscoelastic properties of polyisoprene.
12.2 Constant Contact AreaIVariable Frequency

Figure (65) is a plot of load versus displacement for the load-time history shown
in Figure (64). Note that while significant amounts of both forward and reverse creep
were observed at the upper and lower holds under constant load during the 1 5 s periods,
only a very small amount of creep was observed during the 1 hr hold at nearly zero load
and the majority of this displacement was observed to occur during the first few seconds
of the hold. The fact that the area of contact remained nearly constant throughout this
entire period was confirmed by performing reference measurements at a frequency of
0.5 Hz at the beginning, halfway through, and at the end of the hold period.
Figure (66) is a plot of the dynamic compliance, the ratio of the displacement
response to the force excitation, as a function of frequency showing the response of the
free-hanging indenter as well as the composite response of the system with the indenter
in contact with the material under conditions of constant contact area for three different
peak loads. Note that not only has the compliance of the composite system decreased,
173
1 5s hold
.
.
.
Loadi ng
Seg m e n t
1 hr hold :
200
1 00
-
Z
::::1.
--
"'C
Cd
0
.....I
:,
:
.
:
:
F o rc e
.
.
:
- 1 00
,- :
- 200
- 300
o
..
.
1 5s
hold
20
10
5
15
Displacement (Jlm )
25
Figure 65 . A typical plot of load versus displacement for polyisoprene during

constant contact area/variable frequency experiment. Note the stability of the contact
during the 1 hour hold at near zero load.
1 74
Polyisoprene
...-
z
......
E
""-"
Ll.
......
..c::
Q)
()
c
ca
C.
1 0- 2
()
()
E
ca
c
>.
Free Hanging I ndenter
6.
- -0 -
450 IlN I ndent
- 300
JlN Indent
0 - 1 50 JlN Indent
-
3 --
1 0-
1
1
1 01 00
10
1 02
Radial Frequency, (0 (rad/s)
Fiiure 66. A log-log plot of dynamic compliance,
hIF,
versus radial frequency
showing response of free hanging indenter as well as the response of the indenter in
contact with polyisoprene under conditions of three different constant contact areas.
1 75
i.e., the dynamic stiffness has increased, the response of the system as a function of
frequency appears to have taken on a frequency dependence, i.e., dynamic compliance
is no longer approaching a constant value as was observed for the free hanging indenter
but is continuing to increase as the frequency is lowered. Figure (67) is a plot of the
phase angle, 4>, between the applied force oscillation and the resulting displacement
oscillation for the same set of experiments. By using these two sets of data and
equations (60) and (6 1 ) it is possible to calculate both the contact stiffness, S, and
contact damping coefficient, Ceo. The results of this analysis are shown in Figure (68)
which is a plot of both S and Ceo versus the radial frequency, eo. The storage part of the
stiffness is related to the storage modulus, 0', by equation (47) (G=E/2( 1+v), with v=0.5
for natural rubber) which is a well known result from classical contact mechanics.
It
is
proposed that the loss modulus could be related to the contact damping coefficient in the
same fashion, i.e.,
(62)
Figure (69) is a plot of both the storage and loss components of the modulus
calculated according to equations (47) and (62) as a function of the radial frequency. It
is seen that both expressions reasonably bring all three sets of data together onto a single
curve as a function of frequency. While the general trend of the data suggests that the
hypothesis in equation (62) was correct, a more definitive experiment to test the
conclusion was desired.
1 76
1 60
Polyisoprene
- -6 -
---
1 20
- 450 fl N I ndent
- 300
flN Indent
- - 1 50
flN Indent
-0 -
-e..
CD
C)
c:
<C
CD
en
ct'S
I,t:::>.B
"
80
"
"
"
I'
'
.c:
a..
1(;1
I,:
,''
I"I
40
J'
.. Q'
...
0 2
1 0-
10
Radial Frequency,
co
(rad/s)
Figure 67. A semi-log plot of phase angle, <\> , versus radial frequency showing
response of free hanging indenter as well as the response of the indenter in contact with
polyisoprene under conditions of three different constant contact areas.
1 77
E
.......
S 450 /IN Indent
S 300 /I N Indent
S 1 50 /IN Indent
1 02
---
..
1 02
CJ
$l)
-C
:::l
(Q
_.
...
::=
+=i
en
l:::.
l:::.
0
0
.....
(.)
CU
(J)
(J)
Q)
c:
c:
en
.....
0
0
()
l:::.
0
0
1 01
1 0- 1
0
0
l:::.
0
0
l:::.
C m 450 /I N Indent
C m 300 /I N Indent
C m 1 50 /I N Indent
Z
3
l:::.
0
0
.......
l:::.
0
0
1 01
---
2
10
1 01
10
Radial Frequency, OJ (rad/s)
Figure 68. A log-log plot of stiffness, S, and damping, Cm, versus radial
frequency for polyisoprene under conditions of constant contact area. The data have
been corrected for the contributions of the indentation system and represent only the
contributions from the material.
1 78
1
A
G ' (L=4 50 N )
G I (L =3
00 N )
G I (L=1 50 N )
CO
a..
'-'
0
en
en
(!)
s:
CJ)
::J
::J
-C
0
0
a.
c:
c:
Polyisoprene
en
...
Q)
C)
Ci)
<>
I::.
0.1
0
(j)
<>
I::.
.....
<>
I::.
I::.
0. 1
<>
"1J
Q)
I::.
'-'
l (
L= 45 0 N )
i l (L
I::.
Gi
<>
<>
Gi
=3 00 N )
l (L
= 1 50 JlN )
1 00
10
Radial Frequency,
ill
(rad/s)
Filjure 69. A plot of the storage modulus, 0', and loss modulus,
Gil,
as a function
of radial frequency for polyisoprene under conditions of constant contact area.
1 79
12.3 Constant Frequency/Variable Contact Area

In order to more clearly define the relationship between the damping coefficient,
Coo, and the area of contact between the indenter and the material, a second type of
experiment was performed in which the frequency of the excitation was held constant as
the indenter was loaded into the material. Each experiment consisted of loading the
indenter at a rate of approximately 10 mnls while applying an oscillatory force of 1 .5 JlN
at a fixed frequency of 1 . 1 Hz. If the hypothesis is correct that the damping coefficient
scales as the square root of the contact area then a plot of the measured damping
coefficient versus indenter displacement should yield a straight line with the loss
modulus then being given by
I I
= .J1i Slope
6 ...)24 . 56
OJ
(63)
where the slope of the line is dC/dh where h is the contact depth which can be related to
the area of contact for a perfect Berkovich indenter by A=24.5h2 .
Figures (70) and (7 1 ) show the measured dynamic compliance and phase angle
during the loading segment as a function of position within the capacitive plates as well
as the response of the indentation head with no contact over the same absolute voltage
range. While the voltage is linearly related to the displacement through a calibration
factor, a knowledge of the absolute position of the center plate in the gap was crucial for
appropriately correcting the measured response for the contributions of the indentation
system. By using the calibration data for both the damping coefficient of the indentation
head and the stiffness of the support springs as a function of position (as detailed in
Appendix A) it was possible to subtract out the contributions to the measured response
due to the machine leaving only the response due to the contact between the indenter
1 80
.-.
.......
E 0.01 5
u..
.......
..c:
Q)
()
c:
ctS
.-
0-
0.01
0
()
.-
ctS
c:
0.00 5
:)
--
I ndenter
--fr-- Free
Polyisoprene Response
Hanging Indenter
o --
4 -3 -2 - 1 0 1 2 3 4
I ndenter Position i n Capacitive Gap (V)
-
Figure 70. A plot of dynamic compliance versus absolute displacement of

capacitive plate in gap for conditions of no contact between the indenter and sample and
conditions of increasing contact area between indenter and polyisoprene.
The
contribution of the indentation system was removed based on the dynamic

characterization discussed in Appendix A.
181
--
Indenter + Polyisoprene Response
--!:r- Free H anging Indenter
60
-e-
Q)
en
c::
Q)
C/)
co
..c::
D-
30
.. ....
... ..
... ....
.. ....
.. ..
.. ....
... ..
... ....
.. ....
.. ....
... . ....
0 ......
1
-4 - 3 -2 - 1
2
3
4
0
I ndenter Position i n Capacitive Gap (V)

Figure 7 1 . A plot of the phase angle versus absolute displacement of capacitive
plate in gap for conditions of no contact between the indenter and sample and conditions
of increasing contact area between indenter and polyisoprene. The contribution of the
indentation system was removed based on the dynamic characterization discussed in
Appendix A.
1 82
and the material. Figure (72) is a plot of the calculated stiffness of the contact versus the
depth of the indenter. Note that the data are linear as is expected from theory. Figure
(73) is a similar plot for the calculated damping coefficient of the material versus the
depth of the indenter.
Note that these data are also linear supporting the earlier
hypothesis. A storage modulus of 0.37 MPa can be calculated from the slope of the plot
of stiffness versus indenter depth and a loss modulus of 0.054 MPa from the plot of the
damping coefficient versus the indenter depth. Both of these values agree well with the
data reported in the literature for polyisoprene[ 1 6] .
One final check as to the validity o f the results can b e made by adding the data
from the fixed frequency/variable contact area experiments to the plot obtained for the
variable frequency/constant contact area experiments. Figure (74) is the data from
Figure (69) replotted with the results of the fixed frequency experiments. Considering
the completely different dynamics of the experiments, good agreement is observed
between the two types of measurements.
) ,:
"
, ,
'"
1 83
AS
Slope = Mt
-Iii Slope . - 0 5
- E' G' 6 24.5 ' V 3
200
E
z
G ' = 0. 37 MPa
......
-
'"
en
en
OJ
c
::::
1 50
':.j:j
(j)
t5
1 00
Cd
c
o
.......
()
50
--
1 . 1097 + 6.2 1 0 1h;
R= 0.99957
1 0 1 5 20 25 30 35 40
Displacement (J.lm )
Figure 72. A plot of contact stiffness, S, versus displacement for polyisoprene.
The slope of the line is related to the storage modulus of the material. Good agreement
is found between these results and literature values for polyisoprene.
1 84
de
Slope =
M
5
-
G tf= 0. 054 MPa
""'-
en
Z
....,
c
Q)
.()
'+-
'+
Q)
o
0')
c
.-
0.
en
1
--
c = 0.37045 + 0. 14006h;
R= 0.99678
1 0 1 5 20 25
30 35 40
Displacment (Jim )
Figure 73 . A plot of the contact damping coefficient, C, versus displacement for
polyisoprene.
The data are observed to be reasonably linear over the range of
displacement measured. The slope of the line is related to the loss modulus of the
material.
1 85
...
ctS
c..
G'
G ' , L=450
G ' , L=300
G ' , L=1 50
----
Loading
r
0
CJ)
CJ)
(!J
s:
0
a.
c:
c:
CJ)
...
'"
en
:::J
:::J
"'0
0
G>
Q)
0>
0
0
0. 1
+-'
C/)
f::.
0. 1
l
G i Load ing
l
G i , L=450
l
G i , L=300
l
G i , L=1 50
&
0. 1 s:
f::.
0
0
""'0
0>
----
10
Radial Frequency,
ro
Figure 74. A log -log plot of the storage modulus,
1 00
(rad/s)
G',
and loss modulus,
G",
of
polyisoprene as a function of radial frequency showing data from constant contact

area/variable frequency experiments and constant frequency/variable contact area
experiments.
1 86
Chapter 13 Indentation Viscoelasticity - Conclusions

and Suggestions for Future Research
13.1 Conclusions
Using a depth-sensing indentation system operating in a frequency specific
measurement mode, it was possible to measure both the storage and loss modulus of
polyisoprene as a function of frequency.
The relationship between the measured
damping coefficient and the loss modulus was confirmed to scale as the square root of
the contact area between the indenter and the material as was previously known for the
relationship between the stiffness of the contact and the storage modulus . The results
obtained from the frequency specific indentation test agree well with the bulk values
reported in the literature.

The directions for future research in this area are virtually limitless as this work
presents the first such study of viscoelastic behavior using frequency specific depth
sensing indentation techniques. The application of the technique to other materials to
completely v alidate the results contained herein is therefore high on the priority list of
future work.
Obviously, the goal of this work is aimed specifically at the characterization of
the viscoelastic properties of thin films and small volumes of material that cannot be
characterized by existing bulk techniques. As such, specific instrumentation needs are
required due to the scaling down of the depth of the indentation as required for the
testing of these small volumes. While the dynamics of the indentation head are able to
1 87
be modeled quite accurately, the losses occurring in the indentation head itself due to the
capacitive displacement gauge are expected to be large compared to the response from
the material as the size of the indentation is reduced. Hardware is therefore needed to
reduce the losses in the system to a level such that the measured response is sensitive to
the damping coefficient of the contact. The characterization and utilization of this new
hardware is therefore of great interest.
1 88
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1 89
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Hill, Inc., New York, 199 1 ).
68.
D. S . Tabor,
69.
( 1 995).
Vibrations
12, 22 14 ( 1 977).
(McGraw-Hill Book
of Materials
of Metals
(The University of
(Addison-Wesley Publishing Co.,
Deutsch and W. R. E. A. W. Hoff, J. Polymer ScL, 40,
Hardness of Metals
2024
1 2 1 ( 1 954).
(Butler and
of Metals
1 980.
Materials Handbook 1 - 1056

(Clarendon Press, Oxford,
(McGraw
195 1 ).
S . P. Baker, T. W. Barbee, Jr., and W. D. Nix in Thin Films: Stresses and

eds. W. D. Nix, et al. (Mater. Res. Soc. Symp.
Mechanical Properties,
Proc. 239, 1992) 337.
70.
1. N. Sneddon, Int. 1. of Engng. Sci., 3,
71.
R. E. Eckert and H. G. Drickamer, J. Chern. Phys., 20,
72.
G. W. Powell and J . D. Braun, Trans.
73.
T. E. Volin,
74.
47 ( 1 965).
1 3 ( 1 952).
AIME , 230, 694 ( 1960).
K. H. Lie, and R. W. Baluffi,
Acta Met, 19,
263 ( 1 97 1) .
O. D. Sherby and C. M. Young. in Rate Processes in Plastic Deformation

, 497 (American Society for Metals, Metals Park, Ohio
of Materials
1 975).
145, 388 ( 1 934).
75.
G. 1. Taylor, Proc. R. Soc. A ,
76.
A. F. Bower, N. A. Fleck, A. Needleman, and N . Ogbonna, Proc. R. Soc.

Lond. A, 441, 97 ( 1 993).
77.
T. A. Trozera, O. D. Sherby, and 1. E. Doru, Trans AS, 49,

,
193
173 ( 1 957).
78.
1. B . Pethica and W. C. Oliver in Thin Films: Stresses and Mechanical

Properties, eds. 1. C. Bravman, et al. (Mater. Res. Soc . Symp. Proc . 130,
1 989) 1 3 .
79.
1. Brandrup and E. H. Immergut, Polymer Handbook (1. Wiley and Sons,

1 989).
80.
A. R. Payne. in Rheology of Elastomers , eds. P. Mason, N. Wookey 86
(Pergammon Press, London, 1 958).

81.
W. W. Seta, Schaum 's Outline of Theory and Problems of Mechanical

Vibrations (McGraw-Hill, Inc., New York, 1 964).
82.
N. A. Stilwell and D. Tabor, Proc. Phys. Soc. London, 78, 1 69 ( 1 96 1 ) .
1 94
Appendices
1 95
Appendix A. Dynamic Modeling
To determine mechanical properties with a depth-sensing indentation test it is

necessary to know four quantities: the displacement of the indenter into the material, the
load on the indenter, the time of the measurement, and the "stiffness" of the contact
between the indenter and the material. S tiffness has been enclosed in quotes here to
denote that there can be more than one component of the stiffness that is of interest. In a
standard depth-sensing indentation test, the load on the indenter is varied while the
displacement and time of the experiment are continuously monitored yielding three of
the four quantities. The stiffness of the contact can only be obtained during a partial
unload of the contact when the relationship between the load and the displacement is
being determined by the elasticity of the problem. A standard depth-sensing indentation
test must therefore involve at least a loading and unloading segment to completely
characterize both the elastic and plastic properties of a material.
A technique to avert the necessity of unloading the contact in order to measure
the stiffness has been developed. This technique involves treating the contact problem
dynamically and modeling the problem as a system of masses, springs and dashpots as
normally seen in vibrational analysis[78] . In the simplest sense, the contact between the
indenter and the material can be thought of as an elastic element or a spring with a
stiffness related to the Young's modulus of the material through a geometric factor. In a
more complex sense, the contact can be thought of as possessing both the capacity for
storing energy (stiffness) and the ability to dissipate energy (damping coefficient). By
appropriately modeling the dynamics of the system and the contact it is therefore
possible to completely model the indentation problem on a differential basis.
1 96
A.1 Calibration and Characterization of Nano IndenterII

Before delving into the properties of any material it is first necessary to
characterize the experimental apparatus such that the role that it plays in the measured
experimental response can be accurately accounted for. Any dynamic system in general
can
be
thought of as including a means for storing potential energy (springs or elastic
elements), a means for storing kinetic energy (mass or inertia elements), and a means for
dissipating energy (damper or dashpot)[63]. The first step in developing the dynamic
model for the indentation system is to examine the physical makeup of the system and
develop a model that represents all the important components of the system for the
purpose of deriving analytical equations governing the behavior of the system.
Figure (5) shows a schematic of the components of the Nanoindenter II
necessary for consideration of a dynamic model. The indentation column of mass m is
supported by two leaf springs of stiffness Ks which are designed to have very high
stiffness in the plane of the springs and to have relatively low stiffness in the vertical
direction, effectively limiting the motion of the indenter to a single degree of freedom.
The indenter is driven by a coil and permanent magnet assembly, the coil being rigidly
attached to the top of the indentation column. The displacement of the indenter column
is measured with a parallel plate capacitive displacement gauge. This introduces a
damping coefficient C i into the system which is expected to vary as the fourth order of
the position in the gap. When the indenter is not in contact with the specimen, the
system can be modeled as a single degree of freedom simple harmonic oscillator with
viscous damping.
As briefly described above, the force on the indenter is generated by a coil and
permanent magnet assembly. The magnitude of the force is controlled by varying the
current through the coil residing inside the magnetic field.
1 97
It
is also possible to add a
harmonic component to the current that is driving the coil. This achieved by using an
oscillator from a lock-in amplifier or similar device. By applying a harmonic force of
known amplitude at a specific frequency, and measuring the displacement response of
the system at that frequency and the phase angle between the two, it is possible to treat
the indentation system dynamically.
The system
as
previously described is quite easy to analyze as it is simply a
single-degree of freedom, damped system undergoing forced vibration.
The
displacement response of this system, h=hoe (i rot+$), is easily found for a driving force
of the form F=Foe(irot) to be
(64)
and the phase angle, $, between the applied force and the resulting displacement is
tan l/J
Cm
l --;:-
(65)
Ks - m m 2
One technique to investigate the dynamic response of the experimental

apparatus is to apply a harmonic force at different frequencies and measure the
displacement response at that frequency. Figure (75) shows a plot of the dynamic
compliance,
hIF,
as a function of the radial frequency for the Nano Indenter II for the
case when the indenter is not in contact with the sample. Note the absence of a resonant
peak in the curve suggesting that the system is over-critically damped. By fitting this
curve with equation (64) it is possible to determine the values for the dynamic constants
1 98
1 0. 1
.:------.--...---.----..--.......
""'!I
1 1K
1 /C co
i
---\.
1 0 6
0.01
________________
1 04
1
1 00
Radial Frequency, co (rad/s)
Figure 75. Log-log plot of dynamic compliance versus radial frequency for the
Nano Indenter II free hanging indenter. The data show no resonance peak: indicating
that the system is over-critically damped.
equation for a simple harmonic oscillator.
1 99
The data are fit extremely well by the
of the system. The results of such a fit are given in Table (3). Note the near perfect fit
of the data by the simple harmonic oscillator function.
Table (3), Summary of dynamic constants for the Nano Indenter II obtained from fit of
equation (64) to the dynamic compliance versus radial frequency.
Support spring stiffness, ks
27 N/m
Damping coefficient, Cj
6.4 Ns/m
Indenter mass, mj
0.006 kg
Correlation coefficient, R
0.999999
While this analysis precisely determines the mass of the indenter, the damping
coefficient and the stiffness of the leaf springs are known to vary over the range of travel
and must therefore be characterized as a function of position. This is accomplished by
stepping the indenter through its range of motion within the capacitive gap and
measuring the dynamic response at each position at a fixed frequency. These results can
be analyzed by simultaneously solving equations (64) and (65) for the stiffness and
damping coefficients.
By solving these two equations it is possible to obtain a
functional fit for both ks and Cj as a function of absolute position. Figures (76) and (77)
show the results of this analysis conducted at a frequency of 1 . 1 Hz. This specific
frequency was chosen as Ks and Cjffi are of nearly equal magnitude at this frequency. A
polynomial fit to these data was used to obtain a functional relationship for both Ks and
Cj as a function of position. The results of these curve fits are given in Tables (4) and
(5).
200
28
-
E
z
.......
"-"
(/J
""
26
+""
C
ctS
+""
en
c
o
()
24
C)
c
"
;::
en
22
o
--()-
K from Amplitude
s
and Phase Angle

20
-4 -3 -2 - 1 0 1 2 3 4
I ndenter Position in Capacitive Gap (V)
Fiure 76. A plot of Nano Indenter
II
support spring stiffness as a function of
the absolute position of the indenter with respect to the capacitive displacement gauge.
The data were fit by a third order polynomial to determine a functional relationship for
the data.
201
-o-
c. from Amplitude
I
12
and Phase Angle
E
en
z
11
o
...
.....
. Q)
(.)
10
......
Q)
o
C>
c
a..
ctS
-4
-3
-2
-1
I ndente r Position i n Capacitive Gap (V)
Fi&ure 77. A plot of Nano Indenter II damping coefficient as a function of the

absolute position of the indenter with respect to the capacitive displacement gauge. The
data were fit by a fourth order polynomial to determine a functional fit for the data.
202
Table (4). Coefficients of third order polynomial fit to the Nano Indenter II support
spring stiffness as a function of absolute position within the capacitive gap.
Co
27.3 1 2
ct
1 .2 1 73
C2
-0. 1 3229
C3
0.0034337
Correlation Coefficient, R
0.996
Table (5). Coefficients of fourth order polynomial fit to indenter damping coefficient as
a function of position within the capacitive gap.
Co
6.4435
ct
-0.01 5829
C2
0.39336
C3
0.0026807
C4
0.0 1 5 9 1 5
Correlation Coefficient, R
0.9999
A.2 Modeling the Elastic Contact

Once the indenter is brought into contact with the sample the analysis then
involves appropriately modeling the system and the contact between the indenter and the
sample. This has been done for the case of the simple elastic response of the material by
Pethica and Oliver[78]. The result is the introduction of two additional springs into the
dynamic model; one representing the contact (S). the other representing the finite
stiffness of the load frame (Kf). The amplitude response of the system is then found to
be
203
(66)
and the phase difference between the force and displacement signals is given by
(67)
The stiffness of the load frame can be determined from a method outlined by
Oliver and Pharr[3]. This model can be extended to include damping or energy losses in
the material as discussed in the section on viscoelastic measurements with the Nano
Indenter II.
A.3 Calibration and Characterization of HTMPM

Figure (78) shows a schematic of the components of the HTMPM necessary for
consideration in a dynamic modeL The indenter is supported inside the indentation head
by two leaf springs designed to have very low stiffness in the z direction (vertical
indentation direction) and to be very rigid in plane, thereby limiting motion of the
indenter to only the z-direction. The indenter can therefore be thought of as a mass, mi,
supported by a spring, Ks, and dashpot, Ci, in parallel as shown schematically in Figure
(78). The specimen stage shown schematically in Figure (78) is mounted to a long
cantilever tube that is rigidly mounted to a five axis manipulation system. In the
simplest sense, it can be modeled as a mass mst supported by a spring Kst (cantilever
tube) and dashpot Cst in parallel as shown in the lower portion of Figure (78). When the
two are not in contact they may each be considered as a single degree of freedom
204
tv
o
VI
Mass of Stage
mirror; and F -Specimen support stage with mass mst. Damping coefficient Cst> and Stiffness, Kst. .
B-Indenter column assembly with mass mi; C-Load application coil; D-Indenter support springs with stiffness Ks ; E-Reference
Figure 80. A schematic of the components of the HTMPM for consideration in the dynamic model. Shown are: A-Sample;
Ks
Dynamic Machine Res ponse, No Contact
system, i.e., the motion of each mass may be completely described by one coordinate
axis. The dynamic properties of the indenter and stage can be determined by analyzing
the vibratory response of the separate mass-spring-dashpot systems when excited by an
external force.
First, consider the free oscillation of the indenter when excited away from its
equilibrium position. Figure (79) is a plot of the indenter displacement as a function of
time in response to an impulse load. By analyzing this data it is possible to obtain all of
the dynamic properties of the indenter mass-spring-dashpot system. Figure (80) is a plot
of the cycle number of the oscillation versus the time of oscillation. The slope of this
line yields the damped natural frequency of the system. Figure (8 1 ) is a plot of the
absolute value of the peak indenter displacement as a function of time showing the
exponential decay of the free oscillation . The exponential term in the curve fit is
determined by the damping coefficient of the indentation head. The dynamic constants
determined for the HTMPM indentation head are s ummarized in Table (6).
Table (6). Summary of dynamic constants for HTMPM indentation head.
Measured Quantities
Applied Load, F
1 0.2 JlN
Resulting Displacement, X
Decay Constant, 'Y
1 6 1 nm
1 1 . 1 3 2 s- 1
14.48 Hz
Freguency of Free Oscillation, f

Calculated Quantities
63.2 N/m
9 1 .0 s- 1
9 1 .7 s- 1
Support Spring Stiffness, Ks

Damped Natural Frequency, rod
Natural Frequency, ron
7.5 1 8 g
Mass of Indenter, mj
0. 1 67 Ns/m
Damping Coefficient, Cj
206
Free Vibration of I ndenter

1 00
..-.
50
---
c:
+-'
c:
Q)
E
Q)
()
.
ctS
a.
en
-
- 50
- 1 00
- 1 50
0. 1
0.2
0.3
0.4
0.5
Time (s)
Figure 79. A plot of displacement versus time showing free vibration of
HTMPM indenter in response to step load. The frequency of the oscillation and the
exponential decay of the oscillation are representative of the dynamics of the indentation
head.
207
1
--
0.48771
1 4.483x R= 0.99997
----------
0.05 0. 1 0. 1 5 0.2 0.25 0.3

Ti me (5)
Fiiure 80. A plot of cycle number versus time yielding the damped natural
frequency of the HTMPM indenter mass, spring, dashpot system.
208
Decay of ampl itude of free

oscillation of i ndenter
c:
......
c:
Q)
Q)
(,)
ctj
a.
en
.-
1 50
.::s!.
ctj
Q)
CL
1 00
.....
o
Q)
:J
ctj
>
Q)
......
50
:J
o
en
..c
<C
0. 1
0.2
Ti me (s)
0.3
Fiure 8 1 . A plot of the absolute peak displacement of the HTMPM indenter

versus time during free vibration showing exponential decay of the vibrational
amplitude. The decay constant is representative of the damping coefficient of the
indentation head.
209
Next consider a similar analysis for the specimen stage. In order to study only
the motion of the stage, the two interferometer beams that normally strike the indenter
mirror were blocked off by a stationary mirror placed on the sapphire viewport. The
stage was then excited into vibration by first stepping the indenter onto the surface in
order to move the stage away from its eqUilibrium position, and then stepping the
indenter off of the surface to observe the free vibration of the specimen stage. Figure
(82) is a plot of the specimen stage displacement during free vibration as a function of
time. By analyzing these data it is possible to obtain all of the dynamic properties of the
stage mass-spring-dashpot system. Figure (83) is a plot of the cycle number of the
oscillation versus the time of oscillation. The slope of this line yields the damped
natural frequency of the stage system. Figure (84) is a plot of the absolute value of the
peak stage displacement as a function of time showing the exponential decay of the free
oscillation. The dynamic constants determined for the stage are summarized in Table
(7) .
Table (7). Summary of dynamic constants for HTMPM specimen stage.

Measured Quantities
Stage S tiffness, Kst
Decay Constant, 'Y
6.67x 1 05 N/m
5.76 s-l
23.05 Hz
Frequency of Free Oscillation, f

Calculated Quantities
Damped Natural Frequency, rod
144.8 1 s - l
Natural Frequency, COn
1 44.92 s- l
Mass of Stage, mst
3 1 .76 Kg
Damping Coefficient, C st
3 65.5 Ns/m
210
Free Vibration of
Speci men Stage
600
400
..-...
--
......
200
c
CD
CD
()
a:s
-200
o
-400
- 600
-800
0. 1
0.2
0.3
0.4
0.5
Time (s)
Figure 82. A plot of displacement versus time showing free vibration of the
HTMPM specimen stage in response to a step load. The frequency of the oscillation and
the exponential decay of the oscillation are representative of the dynamics of the
specimen stage.
211
14
--
--
--
y = 0.50791 + 23.047x R= 0. 99999
12
10
'-
Q)
..c
::J
Z
.::t::.
C\1
Q)
c..
6
4
2
o
Free Vibration of
Specimen Stage
0.1
0.2
0.3
0.4
0.5
0.6
Time (5)
frequency of the HTMPM stage mass, spring, dashpot system.
212
Decay of amplitude of free

osci llation of specimen stage
-...
E
c
--
+-'
C
Q)
600
Q)
(.)
as
C
en
o
.::s:.
m
c..
500
400
.....
o
Q)
300
>
.$
::J
o
en
.c
200
1 00
---
0. 1
0.2
0.3
0.4
0.5
Ti me (s)
Figure 84. A plot of the absolute peak displacement of the HTMPM stage versus
time during free vibration showing exponential decay of the vibrational amplitude. The
decay constant is representative of the damping coefficient of the specimen stage.
213
A second method for investigating the frequency dependence of a system is to

drive the system at a specific frequency and force and monitor the amplitude of the
resultant oscillation at the excitation frequency. This is extremely important for the
HTMPM since the specimen stage must be considered as a sink for vibrational energy
during dynamic experiments . By plotting the amplitude of the motion of the stage as a
function of the driven frequency it is possible to determine the frequency regime over
which the stage has little or no effect in the measured damping. Figure (85) is a plot of
the resultant amplitude of the stage as a function of the driven frequency. The resonant
peak for the system occurs at a frequency of approximately 22 Hz which corresponds
nicely with the natural frequency obtained from the free vibration experiments.
In order to measure material properties with the HTMPM it becomes necessary
to extend the dynamic model that was developed for the system in terms of its parts to
include the contact between the indenter and the material. In the simplest sense, the
contact c an be modeled as an additional spring and dashpot. The contact between the
indenter and the specimen couples the motion of the two single degree of freedom
systems. The analysis is no longer a simple one-degree of freedom system, but a more
complex two degree of freedom system requiring two independent axes to completely
describe the motion of the two masses.
For the dynamic analysis it is convenient to consider the indenter, of mass m I ,
damping coefficient C I and support spring stiffness k } , being driven by a force of the
form F=Foe(iwt) and being displaced in the x-direction about the X l axis (x is used rather
than z for the vertical axis to avoid ambiguity with the impedance matrix). The
specimen stage, of mass m2, damping coefficient C3, and stiffness k3, is then considered
as being driven by the motion of the indenter and is displaced in the x-direction about
214
2500
Forced Vibration
of Specimen Stage
-
---
Q)
'"C
:::J
.....
.-
c..
co
c
0
.....
.0
>
500
10
20
30
Frequency (Hz)
40
Fi!:ure 85. A plot of amplitude versus frequency for forced vibration of the
HTMPM specimen stage. The stage was excited using the indenter in contact with the
reference mirror of the stage.
A resonant peak was observed at a frequency of
approximately 22 Hz.
215
the
X2 axis.
The two masses are coupled by the stiffness of the contact, k2, and the
damping coefficient of the contact,
C2.
The solution to this mathematical model is a set of equations of the fonn
[m ].i + [ C ]i + [ k ]x F
(68)
where [m] is the mass matrix, [c] is the damping matrix and [k] is the stiffness matrix.
From the force balance, the equations of motion for the two coupled masses can be
written as
mIX] + {Cl + C2)XI - C2X2 + (k1 + k2 )xr - k2X2 Fo(t)

m2x2 + (C2 + C3)X2 - c2Xl + (k2 + k3)X2 - k2Xr 0
=
(69)
The general problem of a two degree of freedom system under external forces is
described in Rao[63] on page 245 as well as in Seto[8 1 ] Chapter 2.
Using the
Mechanical Impedance Method, by inspection from Rao, equation (69) can be rewritten
as
Defining the impedance matrix as
(7 1 )
216
where Zi = F . X is then given by Z-I F and by inspection from Rao, it is seen that
(72)
and
(73)
where
[
]
2
222 = [-m m2 + im( c2 + c3 ) + ( k2 + k3 ) ]
2
Zl 1 = -m ml + im (cl + c2 ) + (k1 + k2 )
Z1 2 = -im c2 - k2
(74a, b, c)
For simplicity, let ( k l+k2)=kA , (C l+C2)=CA, (k2+k3)=kB , and (C2+C3)=CB . Equations

(74a, b, c) then become
ZI I =
Z22
[kA - m2ml + imcA ]

[kB - m2m2 + imcB ]
ZI 2 = [-im
c2
(75a, b, c)
- Is ]
The denominator of the equations (72) and (73), Zl I Z22 - Z;2 ' can be simplified to the
form C+iD where
217
and
Therefore equation (72) for X 1 becomes
where A=(kB-mw2 ) and B=(<OcB), The magnitude of Xl is then
(79)
Similarly for X2 ,
x
-2 --
Z1 2FO
7 22
Z1 1 Z22 - "4
-
__
k2 + iOJC2
F
C + I'D
__
G + iH
C + I'D
(80)
where G=k 2 and H=C2W. The magnitude of X2 is then
(8 1 )
218
It is the ratio (X I-X21X2) that is of i mportance in this analysis as that ratio defines the
relative motion of the two masses, however, a complete description of this dynamic
problem involves completely defining the motion of the two masses in terms of the
amplitude and phase angle.
Recalling from equations (79) and (8 1) that X l and X2 can be written as the ratio
of two complex numbers, from complex number identities, X I and X2 can be rewritten
as
Xl =
A + iB
i
. Fo = Fo (K + zL) = IXl Ie I
C + ID
(82 )
where <l> 1=tan- I (KIL) and
X2 =
G + iH
Fo = Fo (M + iN) = I X2 Iei2
C + ID
.
(83)
where <l>2= tan- I (MIN).
K,
L, M, and N are easily found u sing complex number
identities. The complete solution is then given by
(84)
and
(85 )
The ratio (XI -X2)1X2 can easily be found from equations (82) and (83) to be
2 19
It is seen that the relative motion of the two masses is controlled by the elements that
couple the indenter and stage
plot of equation (86)
as
as
well as by the properties of the stage. Figure (86) is a
a function of frequency for the stiffness, 3.3x 1 05 N/m, and
damping coefficient, 7 N slm, calculated from the oscillatory response for In to the 9 mN
step load.
While the plot says nothing about the absolute magnitude of the
displacements of either the indenter or the specimen stage, it can lend valuable
information. It was previously determined that the resonant frequency of both the
indenter and the stage in the uncoupled mode were 14.5 and 23.0 Hz respectively. The
logical interpretation of the increase in the ratio for increasing frequency is that the
amplitude of the very massive stage is going to zero. This plot in conjunction with
Figure (85) showing the response of the stage to forced vibration lends strong support to
the hypothesis that the damping coefficient determined from the step load experiments is
representative of the losses in the sample.
220
1 04
5
Contact Stiffness=3. 3x 1 0 N/m
Damping Coefficie nt= 7 Ns/m
1 02
CD
0)
<a
(/J
-...
--.
X
I
CD
0)
<a
(/J
....
CD
c:
CD
"'C
c:
X
---
10
1 0-2
1 0- 4
1 0- 6
1 0- 1
1 0- 3 1 0. 2 1 0. 1 1 0 1 0 1 1 02 1 03 1 04
Frequency (Hz)
Io..o-...._
..
...._
..
...._
..
....-...
..
....I
...._
.
....
Figure 8 6 . A plot o f (Xindenter-Xstage)/Xstage showing predicted response

calculated from dynamic model solution for contact conditions determined from %Step
Load Experiments. The sharp decrease at approximately 20 Hz is at the resonant
frequency of the specimen stage. The response at higher frequencies is dominated by
the motion of the indenter.
22 1
Appendix B. Area Verification
B.t Indium
In order to verify the calculated hardnesses and the validity of neglecting the
elastic displacements, optical images were taken of indentations made under three
different loading conditions to measure the actual contact areas and to look for trends in
the error as a function of the loading time. Since for metals the lengths of the diagonals
of the indentation have been observed to remain relatively unchanged once the load is
removed[82], the residual contact area is expected to yield a good representation of the
contact area under load.
Figure (87) is a plot of the optically measured contact area divided by the
calculated contact area for indentations made in indium using 1 s, 1 0 s, and 1 00 s
loading ramps to a maximum load of 1 0 mN. While there is a trend in the scatter of the
data, the scatter decreasing with increasing loading time, all of the data are observed to
fall within an acceptable error window of 5%.
B.2 Aluminum
In order to verify the calculated hardnesses as a function of temperature and to
ensure that no trends were observed in the error as a function of temperature, optical
images were taken of the indentations to measure the actual contact areas.
Figure (88) is a plot of the measured contact area divided by the contact area
calculated from the total depth of the indent and the perfect area function for the
B erkovich indenter as a function of the homologous temperature. The error is seen to be
less than 1 0% over the entire range of temperatures investigated.
222
ca
1 .1
I nd i u m
t5
ca
+-"
+5 %
c:
1 .05
"0
Q)
co
::::s
(.)
as
t5
c:
0 . 95
0 . 9 -
1
10
....
1
...
1111
...
....
2....
...
1 ....
..
....
O
..
....oIaI.IoaoiI
10
10
10
10
Loading Time (s)

Figure 87. A plot of the optically measured contact area divided by the contact
area calculated from total depth of the indent and the perfect Berkovich indenter area
function as a function of loading time for In. The areas calculated from the total depth
are all seen to fall within 5% of the optically measured value.
223
ctS
Q)
+-'
(,)
ctS
C
o
+-'
Alu m i n u m
1 .1
()
'U
Q)
ca
::J
(,)
ctS
()
......
ctS
t5
c
o
()
'U
Q)
::J
(J)
ctS
Q)
0.9
a.....I-L-I.....I.
..&.....I..
....
..I...I
.r...
.I....I....
...L-I..
... ....I.....a.
..I...I
.L...
....L....I.
..I-'...t.
..I.-L
...L...I
o . 85
0.3 0.35 0.4 0.45 0.5 0.55 0.6
Homologous Tem peratu re, T / T
m
Fiure 88.
plot of the optically measured contact area divided by the area
c alculated from total depth of indent and perfect Berkovich indenter geometry as a
function of homologous temperature for AI. All of the data are observed to fall within a
1O% error window.
224
Vita
B arry Neal Lucas was born August 5, 1 966 in Louisville, Ky. He attended
elementary, intermediate and high school in the Grayson County Public School System
where he graduated from the Grayson County High School in May of 1 984. He attended
Brevard Junior College for three semesters on a track and cross-country scholarship
before transferring to Western Kentucky University in the fall of 1 985. There, he
studied Physics and Math and received his Bachelors of Science in Physics in May of
1 988. Upon graduation, he entered graduate school at Vanderbilt University in the
Materials Science and Engineering program. While enrolled at Vanderbilt, his research
was performed in the Metals and Ceramics Division at the Oak Ridge National
Laboratory through the Oak Ridge Associated Universities (ORAU) Program . He
received his Masters of Science in Materials Science and Engineering in May 1 990.
While continuing his work at the Oak Ridge National Laboratory, he entered the Ph. D .
program at the University o f Tennessee, Knoxville in September of 1 990. In November
of 1 995, after completing his research, he became gainfully employed at Nano
Instruments, Inc. His doctoral degree was conferred in May of 1 997.
He is presently the Head of the Analytical Sciences Division at N ano

Instruments, Inc. in Oak Ridge, TN.
225

An Experimental Investigation of Creep and Viscoelastic Properties Using Depth - Sensing Identation Techniques

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An Experimental Investigation of Creep and Viscoelastic Properties Using Depth - Sensing Identation Techniques

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University of Tennessee, Knoxville

Trace: Tennessee Research and Creative

An Experimental Investigation of Creep and

To the Graduate Council:

To the Graduate Council:

I am submitting herewith a dissertation written by Barry Neal Lucas entitled" An

Carl J. McHargue, Chairperson

Warren C. Oliver, Technical Advisor

Accepted for the Council:

Associate Vice Chancellor and

AN EXPERIMENTAL INVESTIGATION OF CREEP AND

Barry Neal Lucas

This dissertation is lovingly dedicated to my wife and sons;

Becky, Noah, and Caleb Lucas

Arvil and Jane Lucas

Thank you all.

Your never ending support for me throughout every

endeavor of my life will never be forgotten.

Broad band, quasi-static and frequency specific dynamic techniques adapted to

Using a variety of depth-sensing indentation techniques at both room and

could be held constant during an

Pip, remained constant.

This technique yields the

P/p experiments were compared to the results from conventional indentation

hardness could be reached in an indentation test with a geometrically similar indenter.

Using a frequency specific dynamic indentation technique, a general method to

The portion of the

damping (Coo where 00=2

t) of the contact, and thus the loss modulus (G" ) of the

It was shown that the storage, S,

and loss, Coo, components of the

displacement response scale as the respective component of the complex modulus

1 . 1 Time Dependent Plasticity - Creep

....... .... ......

1 .2.2 Phenomenological Description

2 . 1 Time Dependent Plasticity - Creep .

2.2 Time Dependent Elasticity - Viscoelasticity

2.2.2 Phenomenological Description

. ... ... ....

. ... ..... . . ....... ..

2.2.3 Mechanisms of Viscoelastic Relaxation

2. 1 .3 Review of Indentation Creep Literature ...

........ . .. ..... ....

2. 1 .2 Review of Uniaxial Literature . . . . . .

Chapter 3 Experimental Equipment

1 .2.3 Mechanisms of Viscoelastic Behavior . . .

1 .2 Time Dependent Elasticity - Viscoelasticity .

3. 1 Description of Nano Indenter II .. . .

3.2 Description of the High Temperature Mechanical Properties

Homogeneous Stress Distribution versus Radial

4. 1 .4 Constant Volume versus Expanding Volume ................... 54

5 . 1 Lead-65 at% Indium............................ ............................ ................. 60

Chapter 6 Indentation Creep - Experimental Techniques and Details . . . . 63

6. 1 Load Time Histories

... . .. ... . ....

6. 1 . 1 Step LoadIHold (Step/Hold) . .

...... .... . . ...

6. 1 .3 Constant Rate of Loading/Hold (CRLlHold) . . . .

..... .... ....

6. 1 .4. 1 Development of a Constant "Indentation

6.2 Indenter Geometry . . . . .

6.3 Thermal Drift . . . . .

6.3 . 1 Nano Indenter II . . .

..... ..... .. .. .. ... ...