by
YOHAN JANG
May, 2010
(signed)
Master of Science
degree *.
(date)
* We also certify that written approval have been obtained for any
proprietary material contained therein.
TABLE OF CONTENTS
Table of Contents ..............................................................................................................
List of Tables ....................................................................................................................
List of Figures ...................................................................................................................
Acknowledgement ...........................................................................................................
Abstract ...........................................................................................................................
1. Introduction ....................................................................................................................1
2. Background .....................................................................................................................4
2.1 Static Friction Theory ..............................................................................................4
2.1.1 Coulomb and Amontons Friction Theory ....................................................4
2.1.2 Bowden and Tabors Friction Theory ...........................................................5
2.1.3 Orowan and Shaws Friction Theory .............................................................7
2.2 Dynamic Friction Theory ........................................................................................8
2.2.1 Stribeck Friction Theory ..............................................................................10
2.2.2 Daltons Friction Theory ..............................................................................12
2.3 Fracture Mechanics of Coated Steel Sheet ............................................................15
2.3.1 Wedging Mechanism Causing Powdering ....................................................16
2.3.2 Buckling Mechanism Causing Powdering ....................................................17
3. Experimental Procedure ................................................................................................20
3.1 Material Properties .................................................................................................20
3.1.1 Special Treated Zinc Coated (STZC) Materials...........................................20
3.1.2 Hot- Dip Galvanized (GI) Material..............................................................23
iv
4. Results .........................................................................................................................44
4.1 Materials Characterization ...................................................................................44
4.1.1 Surface .......................................................................................................44
4.1.1.1 Surface Morphology ...................................................................44
4.1.1.2 Real Area of Contact ( Areal Fraction of Asperities ) ................51
4.1.1.3 Depth Profile of Alloying Elements ...........................................51
4.1.2 Microstructure ............................................................................................57
v
5. Discussion ...................................................................................................................88
5.1 Factors affecting Surface Friction .......................................................................88
5.1.1 Surface Morphology ..................................................................................88
5.1.2 Strain State .................................................................................................90
5.1.3 Microstructure ............................................................................................92
5.1.4 Galvanizing and Galvannealing Conditions ..............................................95
5.2 Factors affecting Coating Adhesion .....................................................................99
5.2.1 Microstructure ............................................................................................99
5.2.2 Strain State ...............................................................................................103
5.2.3 Galvannealing Conditions ........................................................................107
5.2.4 Steel Substrate ..........................................................................................108
5.2.5 Surface Friction ........................................................................................111
vi
vii
LIST OF TABLES
Table 3.1
Table 3.2
Table 3.3
Table 4.1
Table 4.2
Table 4.3
Table 4.4
Table 5.1
Table 5.2
Table A.1
Table A.2
Table A.3
viii
LIST OF FIGURES
Figure 2.1
Figure 2.2
Figure 2.3
Examples of static Friction (a) and dynamic Friction (b,c). Figure (a)
shows Coulomb friction which is independent of velocity. Figure (b)
shows there is a pre-sliding regime by microscopic motion before gross
sliding. Figure(c) shows both sliding velocity and frequency of velocity
oscillation lead a friction force. Figure (b) and (c) suggest that friction
is a function of either displacement or velocity........................................ 9
Figure 2.4
The Stribeck curve and the Stribeck effect by Stribeck model ...............11
Figure 2.5
Figure 2.6
Figure 2.7
Figure 2.8
Figure 2.9
Figure 3.1
Figure 3.2
Figure 3.3
Figure 3.4
Figure 3.5
ix
Figure 3.6
Punch with 101.6mm diameter and die set with 225mm diameter and
132.6mm diameter draw bead for hemispherical punch test (A) and
important parameters in equation (3.4) (B) .............................................37
Figure 3.7
Figure 3.8
Figure 4.1
SEM plan view images (200 ) of the STZC1 steel (a) and STZC2
steel (b) ....................................................................................................47
Figure 4.1
SEM plan view images (200 ) of the STZC3 steel (c) and GI steel
(d) ............................................................................................................48
Figure 4.1
Figure 4.2
SEM images of pattern (asperity) on the (a) STZC1, (b) STZC2, (c)
STZC3 (d) GI and (e) GA steels. Yellow arrow indicates surface
asperity ....................................................................................................50
Figure 4.3
Real area of contact of five coated steels at initial normal pressure=0 ...52
Figure 4.4
XPS (ESCA) Depth Profile of the (a) STZC1, (b) STZC2, (c) STZC3,
(d) GI and (e) GA steel coatings .............................................................55
Figure 4.5
Figure 4.6
Figure 4.7
Figure 4.8
Figure 4.9
Figure 4.10
Figure 4.11
Figure 4.12
Figure 4.13
Figure 4.14
Figure 4.15
Figure 4.16
Figure 4.17
LDH curves for the (a) STZC1, (b) STZC2, (c) STZC3, (d) GI and
(e) GA steels and (f) curves normalized by setting each plain strain
condition as an origin .............................................................................87
Figure 5.1
Figure 5.2
Figure 5.3
Figure 5.4
Figure 5.5
Figure 5.6
Figure 5.7
Figure 5.8
Figure 5.10
Figure 5.11
Figure 5.12
Figure 5.13
xii
ACKNOWLEDGEMENTS
The author would like to thank Professor Gary M. Michal for giving this research
opportunity and lending his insight and experience for long time to this project. His
guidance and support have always encouraged me to overcome various challenges. I am
proud to have the opportunity to work with him. Also, I would especially like to thank Dr.
Doojin Paik for all of his time and effort while being an invaluable help through the
length of this work. My thanks also to CMCM staff, Christopher J. Tuma, SCSAM staff,
Reza Sharghi and graduate colleague, Joshua Katz for all of their advice and help.
I would like to thank my wife, Yewon Lee and lovely son, Josiah Jang who kept on my
side and my parents who prayed for my ways.
Finally, I would like to glorify my god who guided my life and provided all supports for
my needs throughout this pursuit of a masters degree.
xiii
The Tribology and Formability of Zinc Coated Steel Sheets Subjected to Different Strain
States
Abstract
by
YOHAN JANG
Five types of zinc coated sheet steels were evaluated for their surface friction,
coating adhesion properties and formability under different strain states. The coefficient
of friction values found under biaxial tensile strain were significantly larger than those
associated with the drawing strain states. It was found that surface morphology, strain
state, and shear yield strength of the zinc coating were direct factors affecting surface
friction. The - phase based coatings exhibited the lowest coating adhesion either at the
plane strain condition or at the stretching condition whereas the - phase based coating
exhibited that at the drawing condition. It was found that coating adhesion depends
directly on the microstructure of the zinc coating and the strain state. It was also found
that surface friction and coating adhesion could affect the formability of a zinc coated
steel sheet by influencing its strain state and fracture mechanism, respectively.
xiv
1. Introduction
Zinc coated sheet steels such as galvanized or galvannealed are gaining
importance in the automotive industry due to their good drawability and corrosion
resistance. The steel with a thin zinc layer can be produced by passing the steel through a
molten bath of zinc at a temperature of around 460 C and various kinds of heat
treatments through a cascade of furnaces can be applied after this. The coated sheet steels
consist of a coating layer (~10m thick on each side of the substrate) and steel that is
nominally 0.7mm thick. In spite of its modest thickness compared to the substrate, the
coating layer has a critical role in the whole performance of the coated sheet steel. It is
well known that the zinc based coating layer increases corrosion resistance because zinc
is anodic with respect to iron, the zinc acts as a sacrificial anode to protect the substrate
from corrosion. Another important role of the zinc layer which is not as well known is its
ability to increase formability. The outer zinc coating layer serves as a thin film of soft
metal on the substrate and it avoids hard metal to hard metal contact which greatly
increases friction. Usually, the coating layer increases the formability of the steel sheet by
lowering its surface friction. Additionally, the coating layer can improve paintability and
weldability through post heat treatments [1,2].
Formability is a key characteristic in the application of zinc coated steel sheet for
processes which avoid machining such as automotive panels, the outer body of
appliances, and parts for aircraft. Two key properties that contribute to formability are
surface friction and coating adhesion. The lower the surface friction, the higher the
formability that is possible. Surface friction is a characteristic of a particular system, used
1
used to quantify the surface morphology of each material is described in section 3.2.
Several kinds of mechanical tests used for the measurement of friction, coating adhesion,
and formability are described in section 3.3. Several methods for microscopic surface
analysis and microstructural characterization are presented in section 3.4 and section 3.5,
respectively.
Chapter 4 includes the results of experiments described in chapter 3. The five zinc
coated materials are characterized in terms of both their surface and microstructural make
up in section 4.1. The surface frictional behavior of the five materials subjected to
different strain states is covered in section 4.2 and the coating adhesion behavior of the
materials subjected to different strain states is contained in section 4.3.
Chapter 5 discusses key issues uncovered through this study. Several factors
affecting surface friction and coating adhesion, empirical relationships among factors,
and fracture models for the five zinc coatings are discussed in section 5.1. The relevance
of surface friction and coating adhesion to formability, one of the biggest themes in this
study, is discussed in section 5.2.
Finally, chapter 6 presents the conclusions of this study about surface friction and
coating adhesion of zinc treated steel sheets subjected to different strain states and their
effects on formability.
2. Background
The friction between sheet metal and various tools is one of the most important
factors affecting the formability as well as the success of a sheet metal forming operation.
In this chapter, friction will be defined and categorized with models proposed from
various perspectives.
Friction is the tangential reaction force between two surfaces in contact. In other
words, if two bodies are placed in contact under a normal load, a finite force is required
to initiate or maintain sliding. This is the force of friction. This force is the result of many
different mechanisms, which depend on contact geometry and topography, properties of
the bulk, the material at the surfaces of the bodies, displacement, relative velocity of the
bodies, and the presence of lubrication. Many models have been developed to take into
account these various sources of friction. Important static friction models and dynamic
friction models that relate to sheet metal forming will be presented.
2.1 Static Friction Theory
2.1.1 Coulomb and Amontons Friction Theory
Static friction is the friction associated with sticking. It describes the friction force
at rest. The concept is opposed to dynamic friction. The early work concerning this form
of friction was done by Coulomb and Amontons. The main idea is that the frictional force
is independent of the area of contact of the sliding bodies and velocity (Coulombs law)
and proportional to the applied load (Amontons law). In general, contact occurred only
locally at the summit of the surface irregularities so that the real contact is very small and
the frictional force is almost independent of the apparent area of contact, but still
4
dependent on the real contact area. After Coulomb and Amontons had suggested the
postulates of frictional force, a conductivity measurement by Tabor proved their
postulates [3]. According to Tabors studies, the deformation of the surfaces is not elastic,
but mainly plastic and the metal flows under the applied load until the area of contact is
sufficient to support it. In the case of plastic flow, the area of contact, i.e. real contact
area, is directly proportional to the applied load, so that the frictional force is directly
proportional to the applied load. It is clear that the frictional resistance is determined
primarily by the real area of contact and that the load is important only insofar as it
affects this area from Coulomb, Amontons and Tabors friction theory. The Coulomb
friction can be described as
FC = FN
(2.1)
Fi
,
H
where H is the hardness of the weakest bulk material of the bodies in contact and the unit
for H is the Pascal. The total contact area ( Ar ) can thus be written=
Ar
F .
a
=
H
i
This relation holds even with elastic junction area growth, provided that H is adjusted
properly. For each asperity contact the tangential deformation is elastic until the applied
shear stress exceeds the shear strength y of the surface materials. The friction force, i.e.
plastic deformation forces of microscopical asperities in contact, is defined as FC = y Ar .
As a result, the friction coefficient can be expressed as =
FC y Ar y
. According
=
=
FN Ar H H
to this model, the friction coefficient is not dependent on the normal load or the velocity,
but on the properties of the surface material in the model.
The model implies that it is possible to manipulate frictional characteristics by
deploying surface films of suitable materials on the bodies in contact. As such a soft
coating layer on a coated sheet steel can be very important for decreasing the frictional
force. Figure 2.1 shows schematically how this is possible. (a) is hard/hard metal contact
and (b) is soft thin film layer/hard metal contact. For the case of (a), the high shear
strength of the hard metal makes the frictional force significant. However, in the case of
(b), the shearing takes place on the thin film which has a low shear strength. That is why
a coated steel sheet could have a low frictional force compared to non-coated steel sheet.
Even though the Bowden and Tabor model is close to understand the frictional
mechanism of coated steel sheets, it has still many limitations.
Figure 2.2: Various static friction models : (a) Coulomb and Amontons model ; (b) Bowden and
Tabors model ; (c) Orowans model ; (d) Shaws model
dependence of the frictional force in the early 19th century [9]. Hess et al. performed
experiments on the velocity dependence of friction with a periodic time-varying velocity
superimposed on a bias velocity and observed an unsteady sliding under high frequency
of velocity oscillation causes a multi-valued friction during acceleration and deceleration
[Fig.2.3 (c)] [10].
Figure 2.3: Examples of Static Friction (a) and Dynamic Friction (b,c). Figure (a) shows
Coulomb friction which is independent of velocity. Figure (b) shows there is a pre-sliding regime
by microscopic motion before gross sliding. Figure (c) shows both sliding velocity and frequency
of velocity oscillation lead a friction force. Figure (b) and (c) suggest that friction is a function of
either displacement or velocity.
boundary lubrication regime where the V / FN factor is very low, lubricant thickness is
at a minimum and surfaces are in contact at microasperities. The friction coefficient is at
its highest value in this state because lubricant is not effective. Figure 2.4 shows the
Stribeck curve and the Stribeck effect which corresponds to the dip in the frictional force
at low velocities.
Figure 2.4: The Stribeck curve and the Stribeck effect by Stribeck model
11
K =K 0 + K1PF + ......
PF 1
= (1 2 ) K1 1
K 0 K1
h0
12
(2.2)
where K is the bulk modulus of the lubricant, K 0 is the initial bulk modulus of the
lubricant, K1 is a unitless coefficient of pressure sensitivity , PF is the hydrostatic
compression applied, is the displacement of an asperity after deformation, and h0 is the
height of an asperity. As a result, the effect of trapped lubricant equals:
qtotal PF K 0 qdry
=
+
K 0 2k 2k
2k
(2.3)
where qtotal is the total pressure necessary to obtain a certain contact area, k is the bulk
modulus of the asperity, and qdry is the pressure necessary to obtain a certain contact area
without trapped lubricant. The first term corresponds to a contribution by lubricant
pressure and the second term corresponds to a contribution by applied pressure. Once
superimposed hydrostatic pressure is applied by trapped lubricant and the total normal
pressure required is constant, qdry decreases compared to the no lubricant trapped
condition. Because qdry is directly related to the real area of contact, a large reduction in
contact area could be achieved by trapped lubricant. It is evident that friction decreases as
real contact area decreases.
Daltons model and Bowden & Tabors model have directly contributed to the
understanding of the frictional behavior of coated sheet steel during forming operations.
Based on their fundamental model, extensive work has been done to modify the surface
coating layer and various lubricant have been used in order to obtain a low friction
coefficient, i.e. high formability. The frictional behavior of special treated zinc coated
13
material, one of the candidates to show high formability will be discussed in subsequent
chapters.
14
Figure 2.6: Trapped lubricant effect (a) no lubricant condition, (b) lubricant& trapped
condition ; y = the shear yield strength of surface material
15
Alpas et al. [12] stated that the driving force for interface crack propagation is an
inhomogeneous distribution of residual stress caused by the formation of the 1 phase
with a columnar morphology. Usually, the 1 phase is formed over the planar phase
and grows into the phase by forming a columnar morphology. The crystals cause
residual compressive stress and generate interfacial shear stresses along the -1 and -
phase boundaries. As a result, a crack can easily propagate through the interface when
subjected to lateral compression [Fig.2.8].
various sources that can initiate buckling. In the case of hot dip galvanizing or electro
galvanizing, the substrate can be exposed to an unclean environment just before the
coating layer is deposited. The deposited defects on the substrate can reduce adhesion
energy between the substrate and coating layer equivalent to roughly 150J/m2 in the case
of a zinc-steel interface. During the electro galvanizing process,
some amount of hydrogen can be injected between the substrate and the coating layer.
S.L. Amey et al. [13] showed that approximately 2 109 moles / cm 2 of hydrogen could
be absorbed into the steel in a commercial electro galvanizing line. A region debonded by
hydrogen could exhibit buckling when subjected to lateral compression.
Janavicius P. V. et al. [14] modeled the growth of an initially buckled area and
derived an expected critical pressure equation as follows.
1/2
EGa
Pcrit =
as a t
2
2a (1 )
18
(2.4)
1/2
32Ga
Pcrit
=
2
3(1
a 3
4 a
a +
t 1 t
1/2
as a = t
(2.5)
1/4
Pcrit
G 3 Et
= 4.8 a 4
a
as a t
(2.6)
19
3. Experimental Procedure
patterns were imprinted into STZC1, STZC2 and STZC3 via working rolls that were
patterned by an Electrical Discharge Texturing (EDT) method. Microstructure is one of
the key parameters that determines the powdering rate which in turn affects formability.
The main parameters that control the microstructure of a coating are galvannealing
temperature and time. Temperature controls diffusion length to a greater extent than time.
Thus, temperature was controlled to modify the thickness of the Fe-Zn alloyed layers.
STZC1,STZC2 and STZC3 were galvannealed in 452C, 465C and 516C , respectively
[Fig.3.1]. The Fe-Zn phases initially nucleate at the steel/coating interface and consume
the pure zinc phase, when the steel passes through the galvannealing furnace. The
initial Fe-Zn intermetallic compound grows rapidly. The phase grows at the expense of
the phase. Later, the phase can be consumed by the growing phase [15]. It is well
known that the brittle phase decreases the formability of galvannealed steel sheet. The
galvannealing time was controlled by the line speed of the rolling process and the short
time in the range of 1~5 seconds was designed to prevent transformation of phase to
phase. The galvannealing condition and mechanical properties for the STZC steels are
listed in Table 3.1. The substrates of the STZC materials are an interstitial free steel (IF
steel grade) and an interstitial free rephosphorized steel (IFP steel grade). Interstitial free
steels are a class of high formable steel with exceptionally low levels of interstitial
elements such as carbon and nitrogen (typically, total C 30ppm and total N 40ppm by
weight) and are mainly used for automotive application due to their high drawability [16].
Interstitial free rephosphorized steel provides a high yield and tensile strength. It has a
carbon content similar to an IF steel grade, but a much higher phosphate content
21
( 630ppm) leading to an increased yield strength and ultimate tensile strength due to
grain boundary hardening [17]. The rephosphorized steel grade was applied to only the
STZC3 material in order to evaluate how the substrate in a coated steel sheet affects its
total formability. The mechanical properties of a typical commercial IF-grade steel and a
IFP-grade are given in Table 3.2.
22
Table 3.1 Galvannealing condition and Mechanical properties for the STZC samples
Material
Grade
STZC1
STZC2
STZC3
IF
IF
IFP
Yield
GA heating
Strength
temperature(C)
(MPa)
452
465
516
160
152
264
Ultimate
Tensile
Strength
(MPa)
306
310
396
Elongation
(%)
Line
Speed
(mpm)
45
46
35
110
138
120
Table 3.2 Mechanical properties for commercial IF-grade and IFP- grade
Substrate
IF
IFP
Ultimate
Tensile
Strength
(MPa)
150~200 300~350
260~320 350~410
Yield
Strength
(MPa)
ef (%)
35
23
Material
Grade
GI
GA
IF
IF
Yield
GA heating
Strength
temperature(C)
(MPa)
505
156
146
Ultimate
Tensile Elongation
Strength
(%)
(MPa)
291
47
294
47
Al content
in the zinc
bath (%)
0.236
0.126
24
during a metal forming process, the initial real contact area, i.e. the sum of asperities was
calculated by a simple statistic method, called Systemic Manual Point Count [19].
3.2.1 Systemic Manual Point Count Method
The method is based upon the stereological principle that a grid with a number of
regularly arrayed points, when systematically placed over an image of a two dimensional
section through the microstructure, can provide, after a representative number of
placements on different fields, an unbiased statistical estimate of the volume fraction of
an identifiable constituent or phase. The method also can be used to measure the areal
fraction of asperities.
The systemic manual point count method requires a test grid and images obtained
from a scanning electron microscope. The test grid is in the form of a transparent sheet
where a specified number of equally spaced points formed by the intersection of very thin
lines is imprinted [Fig.3.2]. The scanning electron microscope provides excellent depth of
field and magnification high enough to adequately resolve the microstructure. It is
recommended to choose a magnification that gives an average constituent size that is
approximately one half of the grid spacing. The number of images or fields depends on
the desired degree of accuracy for the measurement. Table A.1 gives a guide to the
number of fields or images to be counted as a function of total number of points in the
test grid (PT), the relative accuracy which means a measure of the statistical precision,
i.e.=
% RA
95%CI
100 , and the magnitude of the areal fraction.
PP
The measurement procedure is as follows. The test grid which has a total of 100
25
PP =
1 n
PP (i)
n i =1
1/2
1 n
[ Pp (i ) Pp ]2
s
=
n 1 i =1
s
95% CI = t
n
(3.1)
26
27
subsequently determining the success or failure of sheet metal forming operations. The
friction depends strongly on what kind of forming conditions are operative. The friction
values need to be measured under different forming conditions. The cup test was
designed to determine surface friction values under conditions corresponding to drawing
strain states. The hemispherical punch test was designed to determine surface friction
values under conditions corresponding to biaxial stretching strain states.
3.3.1.1 Cup Test
In a deep drawing operation, friction exists in three regions. These regions are the
flange, the die radius, and the punch profile radius. The regions have different frictional
conditions. Throughout the flange region, in which the sheet is held with a normal force
exerted by a blankholder, sliding friction is predominant, and small amounts of strain are
present. In the die radius and punch profile regions, sliding is negligible, and stretching
due to the local plastic deformation of the sheet prevails [20]. The sliding friction in the
flange region is what needs to be measured in this test because the friction in the flange
region determines the ease of supply of material due to plastic flow and subsequently
drawability in a deep drawing operation [21].
Based upon modeling of the forming loads during drawing of a cup, the
relationship between maximum forming load, hold down load and sliding friction
coefficient has been developed. According to K. Langes Handbook of Metal Forming
[22], one of the relationships is that maximum forming load or drawing load is a linear
function of the hold down force and the coefficient of sliding friction is a simple multiple
of that slope. Swift et al. [23] found that the contact angle between the punch and the
28
drawn blank and the instantaneous blank radius are functions of the punch displacement
or forming load.
As a result, an equation (3.2) for the forming load, P , which takes into account
drawing stress (1), stress due to friction in the flange, stress due to friction over the die
radius (2) and stress due to bending and unbending (3) was obtained from the continuum
models by Swift et al.
X FN
t
P 2 Rmt 1.1 fm1 ln
=
+
exp( ) + fm 2
2r0
Rm Xt
(1)
(2)
(3.2)
(3)
In equation 3.2 is the coefficient of surface friction, is the contact angle, X is the
instantaneous blank radius, t is the blank thickness, Rm is equal to the punch radius plus
0.75t , FN is the hold down load, r0 is die radius, fm1 is the average flow stress in the
flange area of the blank, and fm 2 is the average flow stress when the blank undergoes
bending and unbending. The contribution to the forming load of fm1 and fm 2 , which
depend on the work hardening coefficient ( n ), is very small compared to that of the
coefficient of surface friction ( ). The coefficient of surface friction can be obtained by
taking the derivative of P with respect to FN resulting in equation (3.3). The value of
is determined through this transcendental equation by measuring the slope of the forming
load versus hold down load for particular values of the parameter X and .
dP 2 Rm
=
exp( )
dFN
X
29
(3.3)
The coefficient of surface friction, , for each of the five types of steel sheets
was determined through cup tests [Fig.3.3-A]. Initially about thirty blanks (74mm dia.)
were sheared from each type of steel using a shearing punch and hold down die set
mounted on a dual actuator hydraulic deformation press [Fig.3.4-B]. The punch and die
set was then replaced by a cup forming punch and male and female die set on the same
dual actuator hydraulic press [Fig.3.4-A]. Five of the thirty blanks for each steel were
used to determine the range of hold down loads where cups could be formed without
wrinkling their side walls or fracturing their bottoms. The acceptable range of hold down
loads ( FN ) for the STZC series steels and the GA steel was 2 to 11kN.The corresponding
range for the GI steel was 3 to 11kN. The remaining 25 blanks were used to measure the
punch load as a function of punch displacement for 5 different hold down loads and
subsequently to determine the slope,
dP
. The blanks were formed into cups employing
dFN
a punch speed of 20mm/sec after a mill oil was applied to the blanks using a soft brush.
Once the slope,
dP
was determined for a given punch displacement, the coefficient of
dFN
surface friction was calculated using equation (3.3) because the values for Rm is constant
(17.03mm) and and X are well established functions of punch displacement [24].
30
Figure 3.3: Schematic diagrams of cup test (A) and important parameters in equation (3.2) (B)
31
3cm
Figure 3.4: Preparations for cup test:(A-a) male die,(A-b) female die with 225mm diameter,
respectively, (A-c) punch with 33mm diameter, (B-a) 74mm blank, and (B-b) fully formed cup
32
the attainment of the maximum pressure. This means that the average pressure ( p )
exerted by the punch on the sheet surface reaches a maximum. Using these assumptions
and geometrical expressions for key parameters [Fig.3.6B] the following expression can
be derived to determine surface friction.
2 Xr0
(3.4)
In equation 3.4, is the surface friction coefficient, rc is the radius of the punch-sheet
interface boundary, r0 is the value of rc at the inflection point in a plot of loaddisplacement, is the punch radius, X is [ (dP / drc ) / P ]r , and P is the punch load.
0
34
The hemispherical punch test was used to obtain the coefficient of surface friction
under the condition of stretching based upon the work of Ghosh [25]. The hemispherical
punch employed had a standard diameter of 101.6mm, i.e. =50.8mm, and the blanks
were secured by a 132.6mm diameter draw bead [Fig. 3.6A]. The clearance between the
blank holder die set opening and the punch was 2.03mm. A hold down load of 170kN
was applied to completely eliminate metal flow into the die cavity. A constant punch
displacement rate of 25.4mm/min was maintained for all of the hemispherical punch
testing. The five different types of steels were sheared to form square shaped
(178mm 178mm) blanks.
The independent variables in Figure 3.6(B) are X and r0 . Two procedures were
required in order to determine X . Initially, punch load ( P ) versus punch displacement
( x ) plots were obtained from the hemispherical punch tests of the five different types of
steels. Punch displacements continued until the blanks fractured. The punch load data
obtained was used to convert to plots of punch load ( P ) versus radius of the punch-sheet
interface boundary ( rc ). According to Ghosh [25] [Fig. 3.7], the radius of the boundary of
the punch contact ( rc ) can be reliably determined as a function of punch displacement
( x ) regardless of the material or the test conditions. The punch load ( P ) versus the
radius of the boundary of the punch contact ( rc ) data were fitted with a fourth order
polynomial with an index of fit of 0.9999 using ORIGIN 8.0 software in order to get a
fourth order equation ( P = f (rc ) ) from which the derivative value, dP / drc could be
obtained. The next procedure was to determine an inflection point mathematically.
35
The punch load ( P ) versus punch displacement ( x ) plots were fitted with a fourth order
polynomial and fourth order equations were obtained from the fitting in a manner similar
to the first procedure. The specific punch loads and displacements at the inflection point
were determined after taking the second order derivative of the fourth order equations
( P = f ( x) ). The inflection point was found by solving for the value of X at which the
second derivative of plot was zero, i.e. d 2 P / dx 2 = 0 .
Once the punch load and displacement at the inflection point were determined, the
radius of the boundary of the punch contact at the inflection point ( r0 ) was obtained using
the first procedure. As a result, the coefficient of surface friction was calculated using
equation (3.4).
36
3cm
Figure 3.6: Punch with 101.6mm diameter and die set with 225mm diameter and 132.6mm
diameter draw bead for hemispherical punch test (A) and important parameters in equation (3.4)
(B)
37
Figure 3.7: Radius of the boundary of punch contact ( rc ) is plotted as a function of punch
displacement, for three test materials under different test conditions [25]
The test sequence began by cleaning each blank (77mm diameter) with methyl
alcohol followed by weighing each blank. A mill oil was then applied using a soft brush.
The blank was weighed again after application of the oil to monitor and control the
amount of oil applied. Approximately 0.1g oil equivalent to a 12m oil film thickness
was applied to each blank. The oiled blanks were then formed into cups employing a
punch speed of 20mm/sec and hold down loads in the range from 2kN to 11kN. Each
fully formed cup was rinsed in solvent and dried. After cleaning, Scotch 3710 tape was
applied to all of the cups inside and outside surfaces to pull off any loose coating.
Finally, the cup was weighed in gram once more. The difference in weigh between the
initial weighing of the blank and the final weighing of the formed cup established the
extent of powdering of the coated steel caused by the drawing operation.
A similar experimental procedure was applied after hemispherical punch testing
to measure the amount of exfoliation of a coating that occurred under a stretching strain
state. Blanks 178mm long with widths that varied from 125mm to 140mm were designed
to define the plane strain stretching condition. Before the blanks were subjected to
deformation they were cleaned with methyl alcohol and weighed. After the blanks were
deformed they were again cleaned with methyl alcohol and then Scotch 3710 tape was
applied to both their convex and concave surfaces to pull off any loose coating. The
deformed blanks were weighed again and the difference in weight between the initial
weighing and the final weighing was used to measure the extent of powdering of the
coating caused by the stretching operation.
39
Figure 3.8: Relationship between major engineering strain vs. minor engineering strain and
limiting dome height vs. blank geometry
the phases in the extreme outer surface of each of the zinc coatings. There were two
objectives to the analysis of the extreme outer surface. First, the frictional behavior of the
sheet is tied to its extreme outer surface at contact, i.e. tangent points. Knowledge of the
phases and composition at the extreme outer surface could be useful for friction control.
Second, it is known that the aluminum in the coating layer controls the formation of FeZn phases. However, the diffusion of aluminum to outer surface where it forms alumina
could affect weldability negatively [28]. Thus, the outer surface analysis with ESCA
provides some information about the weldability of the five coated steels.
41
edges. Epoxy resin was used as the mounting media. Grinding through 400, 600, and
1200 grit paper was carried out by hand making sure that back and forth motion over
each paper was performed with the interface between the mounting material and the zinc
coatings oriented parallel to the direction of motion. This procedure minimized smearing
of the coating. Polishing proceeded through 3m and 1m diamond slurries finishing
with a 0.05m alumina slurry. The polishing machine employed was adjusted to apply a
heavy, even pressure to each mount. After polishing the specimens were etched in a
solution consisting of 5% nitric acid and 95% methanol, i.e. Nital.
Cross sectional SEM images of the coating layer found on each of the five steels
were taken at 2000 using the back scattering electron (BSE) mode. Energy dispersive xray spectroscopy (EDS) analyses were conducted at several location throughout the
thickness of the zinc coatings in order to investigate the compositions of the Fe-Zn phases.
Elemental maps of the zinc coatings for the elements zinc, iron and aluminum were
obtained to investigate the distribution of those elements through the thickness of the
coatings.
43
4. Results
merged their surface patterns unlike the skin pass process and so formed a conglomerated
mesa-like surface morphology, i.e. hills with flat tops. The pattern on the GI steel has a
coarse mesa-like shape [Fig. 4.1(d)]. The pattern on the GA steel has a fine mesa-like
shape and the distance between pattern shapes is smaller than that found on the GI steel
[Fig. 4.1(e)].
A unit of pattern creates an asperity point, i.e. initial contact point with a die, and
its shape and distribution affect surface friction directly [29]. Figure 4.2 shows different
patterns formed via either the skin pass or the temper rolling process. An asperity point
on the STZC1 steel has a rounded droplet-like shape 20 m in diameter and it is
distributed very sparsely [Fig. 4.2(a)]. An asperity point on the STZC2 steel has a
truncated droplet -like shape with a 20m major axis and 10m minor axis [Fig. 4.2(b)].
The shape and distribution of its asperity points falls between those found on the STZC1
and STZC3 steels. An asperity point on the STZC3 steel has an elongated droplet- like
shape approximately 20m in size across its diagonal. Its asperity points are distributed
very densely [Fig. 4.2(c)]. An asperity point on the GI steel has a mesa-like shape with a
diagonal dimension of 50m and these form flat and large conglomerates that are
distributed sparsely [Fig. 4.2(d)]. An asperity point on the GA steel has a fine mesa-like
shape with a diameter of 6 to 7 m. These fine asperity points form flat and small
conglomerates densely distributed over the surface [Fig. 4.2(e)]. The matrix surrounding
these asperity points on the GA steel is comprised of rough valleys whereas those of the
STZC steels and the GI steel are fairly planar. These imply that the Fe-Zn intermetallic
crystals that comprise the GA steel affect the size of the asperity points, the size of
45
conglomerates, the spacing of conglomerates and the matrix structure surrounding the
asperity points.
46
Figure 4.1: SEM plan view images (200 ) of the STZC1 steel (a) and STZC2 steel (b)
47
Figure 4.1: SEM plan view images (200 ) of the STZC3 steel (c) and GI steel (d)
48
Figure 4.1: SEM plan view images (200 ) of the GA steel (e)
49
Figure 4.2: SEM images of pattern (asperity) on the (a) STZC1, (b) STZC2, (c) STZC3, (d) GI
and (e) GA steels. Yellow arrow indicates surface asperity
50
present in the outer 40nm of these four coating. The GA steel contains a signal from the
Fe2p peak profile in addition to the elements found on the STZC steels and the GI steel
profiles. The presence of iron proves that the outer surface of the GA contains an Fe-Zn
intermetallic phase.
Steel Type
STZC1
STZC2
STZC3
GI
GA
95%CI
2.7
4.1
4.5
3.8
4.1
21.7
38.5
39.5
34
39
50
STZC1
STZC2
STZC3
GI
GA
Steel type
Figure 4.3: Real area of contact of five coated steels at initial normal pressure=0
52
A significant concentration of oxygen was found for all five types of coatings at a
depth from 0 to 15nm below their surfaces. A mixture of zinc oxide (ZnO) and aluminum
oxide (Al2O3) must be present in the outer surface [30]. Under an assumption that the
total oxygen in the outer surface is consumed by the formation of the zinc oxide and the
aluminum oxide and the states of zinc in outer surface are a metal (Zn0) and an oxide
(Zn2+), it is possible to derive ratios of zinc oxide to zinc metal for the five types of
coatings. The results are given in Table 4.2. The higher galvannealing temperature and
the longer galvannealing time produced a higher percentage of oxidized zinc in outer
surface. The STZC3 steel and the GA steel have high percentages of oxidized zinc. The
conclusion is that the galvannealing process is one of the main factors that determines
what oxidation processes occurs on the outer surface.
The Al2p profiles reveal that a considerable amount of aluminum segregation to
the surface occurred. The aluminum added to the zinc bath for the formation of the
inhibition layer diffused to the outer surface and formed an aluminum oxide (Al2O3) layer.
The free energy of formation of Al2O3 is much lower than that for ZnO and provides a
driving force for the formation of Al2O3 on the surface of each coating. The profile of the
GI steel where the content of aluminum is two times higher than that of others is similar
to that of the others. The GI steel experienced no elevated temperature thermal exposure
after its coating layer solidified. The thermal exposure associated with the galvannealing
process affected the distribution of aluminum oxide. The GA steel which experienced
complete galvannealing processing developed the thickest Al2O3 layer. The STZC
samples had surface aluminum oxide levels that were lower than the GI and GA steels as
53
shown in Table 4.2. The high carbon content in the range from 0 to 5nm in the C1s
profiles resulted from either surface contamination due to residual oil or other
hydrocarbons.
54
Zn2p3/2
Zn2p3/2
O1s
O1s
Al2p
C1s
Al2p
C1s
Zn2p3/2
O1s
Zn2p3/2
O1s
C1s
Al2p
C1s
Al2p
e
Zn2p3/2
O1s
Fe2p
Al2p
C1s
Figure 4.4: XPS (ESCA) Depth Profile of (a) STZC1 (b) STZC2 (c) STZC3 (d) GI and (e) GA
steel coatings
55
Table 4.2 Atomic concentration, elemental ratio and zinc state ratio observed by XPS at 5nm
depth in the surfaces of five different coated steel sheets
Steel
Type
STZC1
STZC2
STZC3
GI
GA
Element
Atomic
Concentration
(at.%)
Zn
52
Al
11
28
Zn
52
Al
31
Zn
42
Al
45
Zn
47
Al
14
33
Zn
34
Al
13
47
Zn:Al:O
ZnO:Zn
Galvannealing
Temp.(C)
9:2:5
2:8
452
13:2:8
4:6
465
10:2:12
9:1
516
7:2:5
3:7
5:2:7
8:2
505
20
56
Galvannealing
Time(s)
1~5
4.1.2 Microstructure
The microstructural characterization of five coated steel sheets was carried out
using scanning electron microscopy (SEM) analysis combined with energy dispersive xray spectroscopy (EDS). Cross sectional specimens were used to evaluate morphological
changes across the coating thickness. Quantitative analysis of the chemical composition
of the coatings was performed at select points. Elemental maps were obtained to
qualitatively determine the distribution of phases in each coating.
4.1.2.1 Cross sectional Morphology
Cross sectional SEM images of the coating layer found on each of the five steels
are shown in Figure 4.5. The images were taken using the back scattered electron (BSE)
mode. In the BSE mode a region with a higher average atomic number will appear
brighter than an area with a lower average atomic number. Because the five coatings are
predominantly zinc with an atomic number of 30 and the substrates are predominantly
iron with an atomic number of 26, the zinc coatings are brighter than their substrate steels.
The GA steels coating had an average thickness of nominally 8 to 10m equivalent to
about 70g/m2. The GI steels coating had an average thickness of nominally of 17 to
19m equivalent to about 140g/m2. The average thickness of the zinc coatings on
STZC1,STZC2, and STZC3 steels fell between those of the GA and GI steels, i.e.
corresponding to a coating weight of 120g/m2. The variability in coating thickness
observed in the cross sectional images is consistent with the patterned surface structure of
the coatings that were found in the plan view images as shown in Figure 4.1 and Figure
4.2.
57
Fe-Zn intermetallic blocky crystals were identified in the STZC samples. The
yellow arrows indicate the crystals in Figure 4.5(a~c). The STZC3 steel [Fig.4.5(c)] with
its high annealing temperature and longer hold time has thick and long crystals whereas
the STZC1 steel [Fig.4.5(a)] with its low annealing temperature and short hold time has
slender and short crystals. The longer the hold time and the higher the annealing
temperature during galvannealing process resulted in more diffusional transformation
within the coating layer. Individual Fe-Zn crystals are not evident in the GI [Fig.4.5(d)]
and the GA [Fig.4.5(e)] samples because the GI steel did not experience the
galvannealing process and the GA steel was fully transformed to a single Fe-Zn
intermetallic phase.
Vertical and horizontal cracks in the coating and at the steel interface were found
in the GA steel [Fig.4.5(e), yellow circles] whereas they are not identified in the STZC or
GI samples. It means that the Fe-Zn intermetallic phase formed via the full galvannealing
process had more of a brittle character than the other four coatings. In Figure 4.5 coating
debris above the outer surface of several of the coatings appears to have formed during
sample preparation.
58
6m
4m
10m
0m
11m
Figure 4.5: Cross sectional images of five types of coating layer captured by back scattered
electron mode in SEM (2000 ) : (a) STZC1 (b) STZC2 (c) STZC3 (d) GI and (e) GA steels.
(Arrows from (a) to (e) indicate an Fe-Zn intermetallic phase formed through the thickness and its
average vertical height. Circles and ellipse in (e) indicate vertical cracks and horizontal crack,
respectively.)
59
the GI sample and essentially nonexistent for the GA sample. The inhibition layer
prevents the dissolution of iron into the molten zinc and in turn suppresses the formation
of Fe-Zn intermetallic phases.
Analyses of selected points in the five zinc coatings were conducted using energy
dispersive x-ray spectroscopy (EDS). Typical spectra obtained from the five types of
steels are displayed in Figure 4.6 (b), (c) through Figure 4.10 (b), (c). The phases
expected in the coatings are the Fe-Zn intermetallic phases delta () and zeta () and the
zinc solid solution phase eta (). The phase is nominally FeZn10 and its solubility range
for Zn is 85.6 to 91.8 at. % according to the Fe-Zn binary phase diagram [31]. The
phase is nominally FeZn13 and its solid solubility range for Zn is 92.8 to 95.0 at.%. The
phase has a solid solubility range for Zn of 98.5 to 100 at. %. According to all of the EDS
spectra [Fig. 4.6(b) ~ 4.10(b)], the main elements in all five coatings were zinc and iron.
Aluminum, silicon, phosphorous, carbon, and oxygen were detected as trace elements.
Aluminum is added to the zinc bath to form the inhibition layer. Silicon and phosphorous
are elements whose signal may have originated from the interstitial free (IF) steel and
rephosphorized steel substrates. The presence of carbon seems to be attributed to surface
contamination such as hydrocarbons from the chamber, vacuum pump, and the surface of
the sample [33]. The oxygen signal might be a result of surface oxidation. Quantification
of the EDS spectra revealed that the zinc content ranged from 91 to 94 at. % and the iron
content ranged from 6 to 9 at. % in the STZC samples. That result indicates the Fe-Zn
intermetallic phase found in the STZC samples is almost certainly phase. Their higher
than expected measured iron content seems to be attributed to extra iron signal being
61
detected by the EDS system because the phases are very close to their steel substrates.
The average zinc content away from the phase was 98 at. % . The zinc coatings for the
STZC samples were comprised of a matrix phase containing particles of the Fe-Zn
intermetallic phase. The zinc content ranged from 87.1 to 88.2 at. % and the iron
content ranged from 11.8 to 12.9 at. % in the GA sample. The GA sample with an
average concentration of 87.8 at. % zinc and 12.2 at. % iron was clearly comprised of
essentially pure phase. The zinc content ranged from 98.4 to 98.7 at. % and the iron
content ranged from 1.3 to 1.6 at. % in the GI sample. The GI sample with an average
concentration of 98.6 at. % zinc and 1.4 at. % iron was comprised of essentially pure
phase.
62
STZC1, (a)
(b)
(b)
(c)
Figure 4.6: EDS element mapping through the thickness of the STZC 1 steel (a) and energy
spectrum (b) and chemical composition (at.%) (c) from an Fe-Zn intermetallic phase (yellow
arrow) in the steel coating
63
STZC2, (a)
(b)
(b)
(c)
Figure 4.7: EDS element mapping through the thickness of the STZC 2 steel (a) and energy
spectrum (b) and chemical composition (at.%) (c) from an Fe-Zn intermetallic phase (yellow
arrow) in the steel coating
64
STZC3, (a)
(b)
(b)
(c)
Figure 4.8: EDS element mapping through the thickness of the STZC 3 steel (a) and energy
spectrum (b) and chemical composition (at.%) (c) from an Fe-Zn intermetallic phase (yellow
arrow) in the steel coating
65
GI, (a)
(b)
(b)
(c)
Figure 4.9: EDS element mapping through the thickness of the GI steel (a) and energy
spectrum (b) and chemical composition (at.%) (c) from a pure zinc coating (yellow arrow) on the
steel
66
GA, (a)
(b)
(b)
(c)
Figure 4.10: EDS element mapping through the thickness of the GA steel (a) and energy
spectrum (b) and chemical composition (at.%) (c) from a fully galvannealed zinc coating (yellow
arrow) on the steel
67
Fe2Al5
Figure 4.11: Fe-Zn-Al ternary phase diagram (isothermal section at 500C) [32]
68
material and the load loss due to a decrease of the area is much higher than the load
gained by strain hardening and sliding friction.
Maximum punch loads were applied at a punch displacement of 18mm in all five
zinc coated steels. This implies that the position at which the maximum loads are applied
is not a material factor, but a geometrical factor. The punch load was 32kN, 29kN and
37kN in the STZC1, STZC2 and STZC3 steels, respectively. The reason why the STZC3
steel exhibited the highest value for the punch load is that its substrate had the highest
tensile strength of the five steel types. The maximum punch load mainly depends on the
mechanical properties of the substrate because the thickness of the zinc coating is only 2
to 3 % of total thickness of a sample. The GI steel composed of a pure zinc coating
showed the lowest maximum pressure, 28kN whereas the GA steel and the STZC steels
with Fe-Zn intermetallic phases exhibited maximum punch loads in the range of 29kN to
37kN.
The slopes of forming load ( P ) vs. hold down load ( FN ) were obtained from
Figure 4.12 and used to calculate the coefficient of surface friction by applying Equation
3.2. The results are plotted in Figure 4.13. The coefficient of surface friction shifts as the
punch displacement increases in all five zinc coated steels. It implies that the forming of
the zinc coated steel sheet agrees with the dynamic friction theory described in Section
2.2.1 and 2.2.2. The traces of the coefficient of surface friction in Figure 4.13 are similar
to the prediction of the Daltons friction model (Fig.2.5). The asperities on the surface
start to deform plastically making the real contact area increase between punch
displacements of 10 to 20mm. This results in an increase in the coefficient of friction.
70
The constant value of the coefficient of friction then decrease for punch displacement
between 20 and 30mm is interpreted by Daltons model B and model C, respectively.
According to model B, the coefficient of friction is stable before it starts to increase or
decrease. According to model C, the coefficient of friction starts to drop as the forming
process continues. This can be explained by the trapped lubricant effect illustrated in
Figure 2.6. The effect means that the presence of trapped lubricant results in a
superimposed hydrostatic pressure acting in the valleys of the asperities which can reduce
friction in metal working processes.
The STZC1 samples and the STZC2 samples show a similar trace to that of the GI
samples whereas the STZC3 samples show a similar trace of that with the GA samples at
the pure drawing region. The coefficient of friction is significantly affected by the zinc
coating in that region. The STZC1 coating and the STZC2 coating are composed of
mostly the phase. As such they are similar to the zinc coating found on the GI samples.
The STZC3 coating contains a significant fraction of the Fe-Zn intermetallic phase
along with the phase. That coating microstructure is roughly similar to that found in the
GA samples. The variation in the coefficient of friction in the STZC1, STZC2 and the GI
samples is larger than that in the STZC3 and the GA samples. It implies that the shear
strength of the zinc coatings from the former are lower than that from the latter so that the
coatings in the former experience more severe plastic deformation, i.e.
( y ( Fe Zn ) y ( Zn ) ). The value of the coefficient of friction for the STZC1, STZC2 and
GI samples were between 0.09 and 0.11 and for STZC3 and the GA samples between
0.13 and 0.15. The latter group containing the Fe-Zn intermetallic and phases has a
71
higher range of coefficients of friction than the former group. The phenomenon can be
explained by Bowden and Tabors theory because the selected coefficients of friction
occur after a punch displacement that corresponds to considerable plastic deformation of
asperities and prior to a drop of friction by a lubricant effect, i.e. pseudo- dry condition .
According to their theory described in Section 2.1.2, the friction coefficient can be
expressed as =
FC y Ar y
when plastic deformation of surface asperities is
=
=
FN Ar H H
dominant and dry sliding contact occurs. As a result, the STZC3 and the GA samples
with a high shear strength ( y ( Fe Zn ) ) zinc coating develop higher surface friction under
drawing conditions than the STZC1, the STZC2 and the GI samples with their lower
shear strength ( y ( Zn ) ) zinc coating.
4.2.2 The Coefficient of Surface Friction under Stretching Conditions
The coefficient of surface friction under stretching conditions was calculated
following the procedure outlined in Section 3.3.1.2. Figure 4.14 shows the trace of the
punch load as a function of the punch displacement and the radius of the contact
boundary for the five zinc coated steel sheets. Because the relationship between the
punch displacement and the radius of the contact boundary ( rc ) does not depend on the
type of material, that relationship is the same for the five zinc coated steel sheets as
shown by the red dots in Fig.4.14. Using the data for the punch displacement vs. the
radius of the contact boundary and the data for the punch displacement vs. the punch load
obtained with the dual actuator hydraulic press as shown by the green dots in Fig.4.14,
the plots of the punch load vs. the radius of the contact boundary were obtained as shown
72
by the blue dots in Fig.4.14. Fourth order polynomial equations were fitted to the plots of
the punch load versus the radius of the contact boundary using the software ORIGIN. The
equations are given in Table 4.3. After the inflection points and values for X were defined
from punch load vs. punch displacement plots and the fourth order polynomial equations,
respectively, the coefficients of friction under stretching condition were determined. The
coefficient of friction are listed in Table 4.4
The coefficients of friction for the STZC1, the STZC2 and the STZC3 samples
were 0.21, 0.23 and 0.24, respectively. The coefficients of the GI and the GA samples
were 0.24 and 0.19, respectively. The values are higher than those obtained under the
drawing conditions. That result can be explained by the fact that the stretching forming
process produces a significant amount of new surface area which has intrinsically higher
frictional characteristics and also the much higher plastic deformation under stretching
conditions can lead to break out of the surface oil film [34]. Under stretching conditions,
it seems that the degree of plastic deformation of the surface asperities is very important.
The GA sample showed the lowest coefficient of friction under the stretching conditions.
It implies that the Fe-Zn intermetallic phase in the coating with its high shear strength
resists plastic deformation of asperities during the forming which suppress the breakdown
of the oil film and maintains low surface friction. As a result, in spite of the stretching
accompanying severe plastic deformation the GA sample maintains its oil pockets more
effectively compared to the other zinc coatings leading to its relatively low coefficient of
friction.
73
(b)
34
32
32
30
30
(a)
28
26
24
22
20
28
26
24
22
12
5
20
10
Pun 10 15
ch
Dis 20
pla
cem 25 30
ent
(mm
)
8
6
4
2
ld
Ho
35
wn
Do
ad
Lo
N)
(k
12
10
10
Pun
ch 15 20
Dis
pla
cem 25 30
net
(mm
)
(c)
8
6
4
35
ld
Ho
wn
Do
)
kN
d(
a
Lo
(d)
38
30
36
28
32
34
30
28
26
24
22
20
26
24
22
12
18
)
kN
8
d(
a
6
o
nL
4
ow
D
2
ld
Ho
10
10
Pun
ch 15 20
Dis
pla
cem 25 30
ent
(mm
)
35
20
5
12
Pun
ch 15 20
Dis
pla
cem 25 30
ent
(mm
)
)
kN
d(
a
Lo
10
10
8
6
4
35
ld
Ho
wn
Do
(e)
32
30
28
26
24
22
20
12
Pun 10 15
ch
Dis 20
pla
cem 25 30
ent
(mm
)
)
kN
d(
a
Lo
10
8
6
4
35
ld
Ho
wn
Do
Figure 4.12: Punch load as a function of hold down load and punch displacement of the (a)
STZC1, (b) STZC2, (c) STZC3, (d) GI and (e) GA steels
74
0.24
0.24
STZC1
STZC2
0.22
0.20
0.20
0.18
0.18
Coefficient of Friction
Coefficient of Friction
0.22
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
0.00
0.00
8
10
12
14
16
18
20
22
24
26
28
10
12
0.24
16
18
20
22
24
26
28
26
28
GI
0.22
0.20
0.20
0.18
0.18
Coefficient of Friction
Coefficient of Friction
0.24
STZC 3
0.22
14
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
0.00
0.00
8
10
12
14
16
18
20
22
24
26
28
10
0.24
12
14
16
18
20
22
24
GA
0.22
Coefficient of Friction
0.20
0.18
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
0.00
8
10
12
14
16
18
20
22
24
26
28
Figure 4.13: Coefficient of surface friction calculated as a function of punch displacement for
cups drawn from the STZC1, STZC2, STZC3, GI and GA steels
75
60
55
50
45
40
35
30
25
20
15
10
5
0
(b)
(a)
45 ry
40
35 da
30 oun
25 b
10
60
55
50
45
40
35
30
25
20
15
10
5
0
Pun 15
b
20
ch 20 25
15 act
Dis
pla 30 35
10 ont
)
5
(mm cem
f c (mm
ent 40 45 0
.o
)
d
Ra
Pun 15 20
20 ct
ch
ta
15
Dis 25 30
10 con m)
pla
35
f
5
c
(m
o
40
(mm em
d.
ent
45 0
)
Ra
(d)
(c)
60
55
50
45
40
35
30
25
20
15
10
5
0
45 y
40 ar
35 d
30 oun
25 t b
45
40 y
35 ar
30 und
25 o
10
Pun10 15
20 c
ch 20 25
15 nta )
Dis
10 co
pla 30 35
m
5
(m
of
(mm cem
ent 40 45 0 ad.
)
R
60
55
50
45
40
35
30
25
20
15
10
5
0
45 y
40 ar
35 d
30 oun
25 t b
Pun10 15
20 c
ch 20 25
15 nta )
Dis
10 co
pla 30 35
m
5
(m
of
(mm cem
ent 40 45 0 ad.
)
R
(e)
60
55
50
45
40
35
30
25
20
15
10
5
0
10
45 y
40 ar
35 d
30 oun
25 t b
Pun 15
20 c
ch 20 25
15 nta )
Dis
10 co
pla 30 35
m
f
5
(m
o
(mm cem
ent 40 45 0 ad.
)
R
Figure 4.14: Punch load as a function of punch displacement and radius of contact boundary of
the (a) STZC1, (b) STZC2, (c) STZC3, (d) GI and (e) GA steels
76
Table 4.3: Polynomial fits for punch load, P , as a function of contact radius, rc in mm
Steel Type
Condition
STZC1
Oil
STZC2
Oil
STZC3
Oil
0.16612-0.3501rc+0.0709rc2-0.0011rc3 +0.0000154rc4
GI
Oil
GA
Oil
Condition
Test Rate
STZC1
Oil
25.4mm/min
0.21
STZC2
Oil
25.4mm/min
0.23
STZC3
Oil
25.4mm/min
0.24
GI
Oil
25.4mm/min
0.24
GA
Oil
25.4mm/min
0.19
77
crack nucleation site causing a decrease in the fracture stress of the coating [35]. As a
result, anti-powdering characteristics might be deteriorated by an increase in the ratio of
phase to phase in the coating layer among short duration galvannealed steel sheets
containing a discontinuous phase. However, the GI composed of 100% phase
exhibited a higher powdering rate value of 0.006 0.003 g/m2 compared to the STZC
samples containing phase. This result implies that the powdering tendency is affected
by not only microstructure, but also other factors such as interfacial shear strength.
The powdering weight of the GA showed the highest value of 0.1 0.025 g/m2 for
the five zinc coated steels as expected. The result agrees with that from Inagaki et al. [36]
and Nakamori et al. [37]. According to their results, an increase in the volume fraction of
phase with an Fe concentration from 8 to 15 wt.% is responsible for the deterioration of
the powdering resistance. It suggests that the increase of hardness with increasing iron
content prevents the lateral tension and compression stresses from being relaxed and as
such facilitates the propagation of cracks. As a result, the phase with its relatively high
iron content causes increased levels of powdering.
4.3.2 Powdering under Plane Strain and Stretching Conditions
After the Limiting Dome Height (LDH) tests, a series of powdering tests was
conducted with the five coated steel sheets. One of advantages of the LDH test is that the
biaxial strain condition can be varied by modifying the blank width [Fig.3.8] so that the
powdering rate under different biaxial strain conditions can be easily compared. The
results are given in Figure 4.16. Generally the powdering values were similar to the ones
found under drawing conditions. The STZC samples had lower powdering values than
79
the GI sample. The STZC3 sample had a higher powdering value than the STZC1 and
STZC2 samples. The GA sample had the highest powdering values for both stretching
and drawing strain conditions.
The biaxial strain condition was modified by varying the blank width from
124mm to 139mm. That range of blank width produced conditions of drawing, plane
strain and stretching. The STZC1 sample developed a plane strain condition with a blank
width of 130mm. Its powder weight had the highest value at the plane strain condition.
The powder weights under stretching conditions were higher than that at a drawing
condition. The STZC2 sample achieved the plane strain condition at a 124mm blank
width. The powder weight under the plane strain condition for the STZC2 sample was
higher than the STZC1 sample. The STZC3 achieved the plane strain condition at a
127mm blank width. The powdering value at the plane strain condition for the STZC3
sample was higher than the values for the STZC1 and the STZC2 samples. This could be
explained by Smiths theory that addresses a brittle second phase as a crack source as
discussed in section 4.3.1. The GI sample achieved the plane strain condition at a 130mm
blank width. The powdering values were higher than the ones from the STZC samples
regardless of the strain condition. It seems that the low interfacial shear strength of the GI
steels coating resulted in a higher powdering rate. The GI showed the highest powdering
value at the plane strain condition like the STZC samples. The GA sample achieved a
plane strain condition at a 139mm blank. Its powdering values were much higher than the
ones from the STZC samples and the GI sample regardless of the strain condition. The
presence of the phase is the most important factor affecting the powdering rate
80
regardless of the strain condition. Unlike the STZC samples and the GI sample, the GA
sample exhibited the highest powdering rate at the drawing condition rather than the
plane strain condition. Knowledge of the fracture modes for a phase based - zinc
coating and the phase based zinc coating is needed to understand the difference. in
powdering behavior between the STZC samples and the GA sample. According to Parisot
R. et al. [38], intergranular cracking occurs very early during the deformation of an
phase based coating, leading to a relaxation of stresses. That crack type does not reach
the substrate whereas cleavage cracking that occurs under highly tensile conditions such
as plane strain and stretching condition reaches the coating/substrate interface. It implies
that the dominant facture mode for powdering in an phase based coating would be a
cleavage mode rather than an intergranular mode when the coating is fractured by a
wedging mechanism. It makes sense that an phase based coating showed the higher
powering rate at either plane strain or stretching conditions rather than drawing condition
because the cleavage cracks occur only in plane strain and stretching conditions.
However, the phase based zinc coating found in the GA sample shows a different
fracture mode. The phase based zinc coating seems to be much more sensitive to
whether a strain condition keeps a component of compression or not. It makes sense that
the powdering rate in the GA sample was higher under a drawing condition than under a
plane strain condition because the lateral contraction inducing compression is much
larger for a drawing condition as opposed to a plane strain condition. As a result, the
powdering in the phase based coating was due to crack propagation in a direction
parallel to the lateral compression rather than the crack propagation in the normal
81
82
(b)
0.010
0.009
0.009
0.008
0.008
(a)
0.010
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0.000
0.000
0
10
12
(c)
10
12
(d)
0.010
0.010
0.009
0.009
0.008
0.008
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0.007
0.006
0.005
0.004
0.003
0.002
0.001
0.000
0.000
0
10
12
10
12
(e)
(f)
0.20
0.12
STZC1
STZC2
STZC3
GI
GA
0.18
0.16
0.14
0.12
0.10
0.08
0.06
0.04
0.02
0.00
0.10
0.08
0.06
0.04
0.02
0.00
0
10
12
10
12
14
Figure 4.15: Powdering weight under the condition of drawing of the (a) STZC1, (b) STZC2,
(c) STZC3, (d) GI and (e) GA steels and (f) a comparison of the powdering rate in the five zinc
coatings
83
(b)
0.020
0.018
0.018
0.016
0.016
(a)
0.020
0.014
0.012
0.010
0.008
0.006
0.004
0.002
0.014
0.012
0.010
0.008
0.006
0.004
0.002
0.000
0.000
126
129
132
135
138
123
126
(c)
132
135
(d)
0.020
0.020
0.018
0.018
0.016
0.016
129
0.014
0.012
0.010
0.008
0.006
0.004
0.014
0.012
0.010
0.008
0.006
0.004
0.002
0.002
0.000
0.000
126
129
132
135
126
138
129
132
135
138
(e)
(f)
0.10
0.12
STZC1
STZC2
STZC3
GI
GA
0.09
0.10
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.08
0.06
0.04
0.02
0.01
0.00
0.00
126
129
132
135
126
138
129
132
135
138
Figure 4.16: Powdering weight calculated as a function of blank width from LDH tests of the
(a) STZC1, (b) STZC2, (c) STZC3, (d) GI and (e) GA steels and (f) a comparison of the
powdering rate in the five zinc coatings
84
4.4 Formability
The limiting dome height value, an effective predictor of formability was
measured using the limiting dome height test procedure described in section 3.3.3.1.
4.4.1. Limiting Dome Height Value
Limiting dome height (LDH) values of the zinc coated steel sheets were measured
using a LDH testing procedure. The results are given in terms of limiting dome height as
a function of blank width in Figure 4.17. The blank width with the lowest LDH value
(LDH0) corresponds to the plane strain condition and that width was set as the origin in
the Figure 4.17(f). The lower width and higher width correspond to a drawing condition
and a biaxial stretching condition, respectively. As a result, Figure 4.17(f) shows how
major strain varies as the strain states changes drawing (negative minor strain) to biaxial
stretching (positive minor strain). In other words, the LDH curves reveal a portion of a
forming limit diagram. However, the LDH curves in Figure 4.17 (f) are not quantitative
with regard to values for minor and major strains.
The LDH curves for the STZC samples [Fig.4.17 (a)~(c)] have a sharp V shape.
It implies that the strain state strongly affects the LDH values, i.e. the formability of the
zinc coated steel sheets. The slopes of LDH data depend on not only upon the strain state,
but also the characteristics of the zinc coating. It implies that the properties of the zinc
coating layer should be taken into account when considering overall formability. The
average LDH0 values for STZC1, STZC2 and STZC3 samples were 40.91.4mm,
37.61.0mm, 54.21.0mm, respectively.
The LDH curves for the GI and GA steels [Fig.4.17 (d),(e)] have a U shape and
85
the differences in the LDH values among the various strain states are lower than that of
the STZC steels. It implies that the sensitivity to strain state for the forming limit of the
GI and the GA steels is lower than that of the STZC steels. This result seems to be due to
the inhomogeneity of the steel sheet through its thickness. The STZC steels have an
phase layer, phase layer and the steel substrate layer whereas the GI and GA samples
have either a pure phase layer or a full Fe-Zn intermetallic phase layer and the steel
substrate. As a result, the GI and GA samples with a more homogeneously layered
structure respond less to a variation of strain state. The average LDH0 values of the GI
and the GA samples were 53.71.0mm and 35.21.0mm, respectively.
The LDH curves were normalized by setting each plane strain condition at the
origin for comparison purposes as shown in Figure 4.17 (f). The STZC 3 and the GI
steels showed the maximum formability and the GA steel showed the minimum
formability regardless of strain state. The formability of the STZC1 and STZC2 steel was
between those of the GI and the GA samples. It should be noted that the formability is a
mechanical property related to many parameters such as strain hardening component (nvalue), normal anisotropy (r-value) and the surface friction coefficient. A comparison of
the formability of five zinc coated steel sheets will be addressed in more detail in the next
chapter.
86
(a)
(b)
46
47
46
45
45
44
44
43
43
42
42
41
41
120
122
124
126
128
40
130
132
134
136
138
140
104
108
112
(c)
116
120
124
128
132
136
140
144
138
140
(d)
61
60
56
59
58
55
57
56
54
55
54
118
120
122
124
126
128
130
132
134
136
138
120
122
124
128
130
132
134
136
(f)
(e)
126
38.0
63
STZC1
STZC2
STZC3
GI
GA
37.5
60
57
54
37.0
51
36.5
48
45
36.0
42
39
35.5
36
128
130
132
134
136
138
140
142
144
146
148
150
-6
-4
-2
10 12 14
Figure 4.17: LDH curves for the (a) STZC1, (b) STZC2, (c) STZC3, (d) GI and (e) GA steels
and (f) curves normalized by setting each plane strain condition as an origin
87
5. Discussion
The surface friction, adhesion properties and formability of five zinc coated steel
sheets were analyzed. The next step is to clarify what factors affected surface friction
and coating adhesion and how the formability is correlated with surface friction and
coating adhesion. First, the factors affecting surface friction and adhesion propensities
will be discussed so that they can be controlled properly in zinc coated sheet steels. Next,
the formability will be correlated with surface friction and coating adhesion. Finally, how
the formability can be optimized via control of surface friction and coating adhesion will
be discussed.
5.1 Factors Affecting Surface Friction
There are many factors affecting surface friction either directly or indirectly.
Surface morphology and strain state affect directly surface friction because the former is
related to real contact area and the latter is related to modification of surface morphology,
i.e. roughness and creation of new surface. The microstructure of a zinc coating affects
indirectly surface friction because the combination of the type of phase and the geometry
of a phase affects mechanical properties such as the yield strength in shear. A galvanizing
condition like the aluminum content in the zinc bath and galvannealing conditions like
temperature and time affect indirectly the surface friction through their influence on the
microstructure.
5.1.1 Surface Morphology
The five zinc coated steel sheets experienced a modification to their surface
morphology via a skin pass process that imprinted their surface using a working roller
88
0.25
Coefficient of friction
0.24
GI
STZC3
0.23
STZC2
0.22
0.21
STZC1
0.20
0.19
GA
0.18
20
25
30
35
40
45
their phase asperities and that trend does not hold for the GA specimen. It implies that
surface friction could depend on not only the real area of contact as discussed by Bowden
and Tabor, but also other parameters such as the lubricant effect. The surface frictional
characteristics of the GA specimens coating with its higher hardness and yield strength
in shear and a surface morphology apparently composed of valleys and mesas, i.e. high
roughness, could be more strongly influenced by other parameters like the lubricant
effect rather than the real area of contact at a specific displacement. The frictional
characteristics of the zinc coatings with a low hardness and yield strength in shear and
low roughness including the STZC samples and the GI sample were more strongly
influenced by surface morphology at a specific displacement, showing a direct
relationship between coefficient of friction and the real area of contact.
5.1.2 Strain State
The surface friction was measured under different strain states like drawing and
stretching. Generally, the drawing condition and the stretching condition should be
considered differently. In a drawing operation as described in Fig.3.3, the regions
experiencing a frictional force are the flange, the die radius and the punch profile radius.
Throughout the flange region, in which the sheet is held with a normal force exerted by a
blank holder, sliding friction is predominant, and a pure drawing strain is present. In the
biaxial stretching condition as described in Fig. 3.5, metal sliding does not occur due to
constraints imposed by the draw beads. Plastic deformation continues until metal thinning
and ultimately failure take place. Due to stretching a large new area which has
intrinsically higher frictional characteristics is created during the deformation. That is one
90
of the reasons why the biaxial case has much higher surface friction than the drawing
case. According to several studies from Fox et al., Siegert et al., and Hira et al.
[39,40,41], surface friction under uniaxial deformation is higher than that under a
drawing strain. However, the increase of surface friction under uniaxial deformation is
lower than that from biaxial stretching because the new surface area created under the
uniaxial deformation is smaller than that under biaxial stretching. Surface friction as a
function of strain state is displayed in Figure 5.2 based upon values in the literature and
the present study.
0.26
0.24
GI[39]
GA[40]
P-GA[24,41]
Bare[25,40]
0.22
0.20
0.18
GI
GA
0.16
0.14
0.12
0.10
0.08
Drawing
Uniaxial
Biaxial
Strain State
Figure 5.2: Effect of different strain state on surface friction. Note GI: galvanized ,GA:
galvannealed, P-GA: galvannealed and phosphate treated, Bare: non-coated and open symbols:
present study (Source:Paik [24], Ghosh [25], Fox et al.[39], Siegert et al. [40], Hira et al. [41] )
Figure 5.2 shows that the coefficient of surface friction increases in going from a drawing
strain condition to a biaxial stretching condition for GI, GA, P-GA and bare steel surfaces.
91
The STZC steels which are not included in Figure 5.2 also exhibited a much higher
surface coefficient under biaxial stretching than under a drawing strain condition.
5.1.3 Microstructure
The microstructure of a zinc coating affects its surface friction in two ways. First,
it modifies the surface roughness and real area of contact for example when an Fe-Zn
intermetallic phases grow to the outer surface. A modification in the phase found at the
surface gives rise to a change of surface friction because the accompanying alteration to
the surface roughness and real area of contact are related directly to surface friction. L.G.
Garza et al. [42] showed that the surface friction of a galvannealed coated steel composed
of all phase is lower than that of a galvannealed coated steel with some amount of
phase on the surface.
Secondly, a change in the phase found at the surface modifies surface friction by
altering the yield strength in shear of the zinc coating. This factor applied to all five types
of steel coatings that were evaluated. The results of depth profiles of the five zinc
coatings [Fig. 4.4] and cross sectional analysis by SEM [Fig. 4.5] showed that the Fe-Zn
intermetallic phases such as the phase did not grow to the outer surface. According to
Bowden and Tabors friction theory, the surface friction is proportional to the yield
strength in shear of the surface layer. Thus, once the microstructure causes a
modification to the yield strength in shear of the coating, the surface friction changes.
The relationship between microstructure and yield strength in shear can be expressed
using a rule of mixture for composites and the Tresca yield criterion as follows.
92
=
y (T )
=
y (T )
y (T )
=
2
y (T )
=
2
(5.1)
(5.2)
where y (T ) = overall yield strength in shear in MPa, y (T ) = overall tensile yield strength
in MPa, y = tensile yield strength of phase i , Vi = volume fraction of phase i , = a
proportional factor, and H = Vickers hardness number of phase i . Equation (5.1) shows
that the greater the volume of a phase with a higher tensile yield strength that is contained
in a coating layer, the higher the overall yield strength in shear of the coating layer will
be. Because the tensile yield strength is proportional to hardness [43], equation 5.1 can be
expressed in the form of equation (5.2).
As a result, assumed the phase grows uniformly and continuously like Figure.5.3, the
magnitude of the yield strength in shear of the zinc coatings can be approximated as
follows.
=
y (T )
y (T )
=
2
t
tc
t2
ti
+ + Hi
tc
tc
2
H1 1 + H 2
(5.3)
where ti = thickness of phase i and tc = thickness of the overall coating layer. The yield
strength in shear of the five zinc coatings can be easily compared using equation 5.3 and
measured values for the hardness and thickness terms. The GI steel has the lowest yield
strength in shear because the zinc rich phase has the lowest hardness. The yield strength
in shear of the STZC steels depends on the volume fraction of phase with its higher
hardness than the phase. The yield strength in shear increases from the STZC1 steel to
93
the STZC3 steel because the thickness of the phase increases from the STZC1 steel to
the STZC3 steel. The GA steel has the highest yield strength in shear because the coating
is composed of the phase which is harder than the phase.
Figure 5.4 displays the coefficients of surface friction measured under a drawing
strain condition as a function of the average vertical height of the Fe-Zn intermetallic
phase present in each coating. The correlation between higher yield strength in shear (or
hardness) and increased coefficient of surface friction complies with the Bowden and
Tabors theory. The nonlinearity seems to be attributed to an imperfect match between
the average vertical height of the Fe-Zn intermetallic phase and the yield strength in shear.
Figure 5.4 implies that at a specific displacement, the predominant factor affecting
surface friction under a drawing condition could be due to the microstructure rather than
the lubricant or the surface morphology. Increasing surface friction is observed as the
average vertical height of the Fe-Zn intermetallic phase increases. Table 5.1 summarizes
the predominant factors affecting surface friction under specific conditions of biaxial
stretching and drawing strains.
Figure 5.3: A microstructure of zinc coating where an Fe-Zn intermetallic phase was grown
ideally
94
Q
Q
D0 exp
tc D0 exp
t
t
RT
RT
+ H2
H1
tc
tc
y (total )
=
=
y ( total )
2
2
(5.4)
produced using equation 5.4. Figure 5.5 lists the parameters used and the variation of the
yield strength in shear for galvannealing temperatures ranging from 700 to 800K,
corresponding to phase growth. The yield strength in shear of a zinc coating increases
as the galvannealing temperature increases. Figure 5.5 indicates that the surface friction
should increase as the galvannealing temperature increases. The galvannealing
temperature can modify indirectly the surface friction of a coating by increasing the
coatings yield strength in shear through increasing the amount of phase in the coating.
96
0.18
0.17
Coefficient of Friction
0.16
0.15
STZC3
0.14
0.13
GA
0.12
0.11
STZC1
0.10
GI
0.09
STZC2
0.08
0
10
11
12
Table 5.1 Predominant factors affecting surface friction under specific conditions
Steel Type
GI
Very Low
STZCs
STZC1
STZC2
STZC3
GA
Low
Intermediate
High
Very High
Strain Condition
Biaxial Stretching*
Drawing**
Microstructure
Surface Morphology
(Shear Yield
(Real Area of Contact)
Strength)
Microstructure
Surface Morphology
(Shear Yield
(Real Area of Contact)
Strength)
Forming
Condition
Forming Condition
(Lubricant)
(Lubricant)
Microstructure
(Shear Yield
Strength)
* punch displacement=25mm
** punch displacement=18mm
97
98
Figure 5.5: Effect of galvannealing temperature on shear yield strength of zinc coating [43,
44, 45]
F =
=
G
2 E ( S + P )
t1
(5.5)
Y 2 2 t1
GIC
E
(5.6)
decreases as the thickness of its brittle phase containing through thickness cracks
increases. Equation (5.6) presents this in terms of an energy release rate. Once the energy
release rate decreases due to the brittle phase and in turn exceeds the critical energy, the
system will fracture. Figure 5.6(a) shows powdering weight as a function of average
vertical height of phase in the STZC samples. The amount of powdering increases as
the average vertical height of phase, a brittle phase in + system increases. Figure
5.6(b) shows a comparison among the five zinc coatings. One can see that the powdering
weight of the GA is much larger than that of the other four steels. The coating of GA is
composed of only phase known as one of the most brittle phase in Fe-Zn intermetallic
phases and the coating itself acts as a crack initiation site. Figure 4.5 has already
represented that the GA involves many initial cracks of coating thickness. The effects of
Fe-Zn intermetallic phase on coating adhesion are illustrated schematically in Figure 5.7.
As a result, the coating adhesion depends on both the average vertical height and type of
Fe-Zn intermetallic phases and it is deteriorated as the average vertical height increases
and the brittleness of phase increases, i.e. K ICFeZn , GICFeZn .
100
(a)
0.0044
0.0040
0.0036
STZC3
0.0032
0.0028
0.0024
STZC1
0.0020
STZC2
0.0016
0.0012
0.0008
3
10
11
0.10
GA
0.08
0.06
0.04
0.02
GI
STZC1
STZC2
STZC3
0.00
0
10
12
101
GI steel
STZC steels
GA steel
Figure 5.7: The Fe-Zn intermetallic phases and surface oxides acting as initial crack sites
102
drawing condition meets the fracture requirement for the phase based coating. In fact,
the drawing condition involves lateral contraction that induces a strong compressive
strain so that crack propagation parallel to the direction of the coating /substrate interface
occurs more easily. Coating adhesion of the phase based coating appears to decrease
under a drawing condition. Figure 5.9 summarizes the effects of strain state on crack
propagation for the phase based and phase based coatings.
104
0.012
STZC1
STZC2
STZC3
GI
0.010
0.008
0.006
0.004
0.002
0.000
Pure Drawing
Plane Strain
Slightly Stretching
Strain State
0.12
b
0.10
0.08
0.06
0.04
0.02
0.00
Pure Drawing
Plane Strain
Slightly Stretching
Strain State
Figure 5.8: Effect of strain state on coating adhesion in phase based (a) and phase based
coating (b) based upon strain states generated during cup testing and LDH testing
105
Figure 5.9: Schematic illustration of crack propagation of phase based- and phase based
coating as fracture driving strains are subjected (Red line: crack initiation sites, blue line: crack
propagation)
106
107
variety of Fe-Zn intermetallic phases and the coating is deposited on an IF grade steel
substrate, microhardness values for a region with Fe-Zn intermetallic phases located
between the phase and the soft steel substrate will be relatively high. The high hardness
of the , and 1 Fe-Zn intermetallic phases and their concave downward distribution
allow cracks to easily initiate and propagate. The STZC1 and the STZC2 steels are
examples of this effect. If a zinc coating is deposited on an IFP grade steel substrate, the
shape of the distribution of the hardness of Fe-Zn intermetallic phases is transformed
from concave downward to roughly linear. The embrittling effect by Fe-Zn intermetallic
phases can be reduced by a modification of the steel substrate. The STZC3 steel
corresponds to this situation. One of the reasons why the STZC3 steel shows relatively
good coating adhesion in spite of having a relatively large amount of phase is that its
IFP steel substrate reduces the stress raising effect of that Fe-Zn intermetallic phase.
Figure 5.10 illustrates the effect of the steel substrates on crack formation in the STZC
steels.
Finally, the steel substrate can affect coating adhesion through the influence of
interdiffusion of Fe and Zn between a zinc coating and its steel substrate. W. Zhong et al.
[49] reported that Zn diffusion along ferrite grain boundaries can occur during
galvannealing and these Zn atoms can lead grain boundary embrittlement in IF grade
steel substrates. The P solute segregated to ferrite grain boundaries in IFP grade steels
can retard Zn diffusion and reduce the potential for embrittlement of IFP grade steels by
Zn. Zn embrittlement can give rise to a flaking coating failure mode. A flaking coating
failure involves both the coating layer and a part of the steel substrate unlike powdering
109
where only a failure of the coating layer occurs. Zn embrittlement of an IF steel substrate
can reduce coating adhesion and the overall formability of the steel sheet.
Table 5.2 Calculated lattice misfit of interfacial layers [33, 47, 48]
Steel
Substrate
Interfacial
Layer
Interfacial
Shear
Strength
(MPa)
IF
14.7~15.2
IFP
/1
20
f* =
Lattice Misfit
( f *)
Lattice Parameter
( a , nm)
1.282
0.893
1.282
1.796
0.435
0.286
| as a f |
as
STZC1, STZC2
STZC3
Figure 5.10: Effect of steel substrate on coating adhesion in the STZC steels
110
111
5.3 Formability
It has been known that factors such as anisotropy and strain rate sensitivity
interact in a complex way to establish the formability of zinc coated steel sheets.
However, surface friction and coating adhesion also are very important parameters that
need to be taken into account. In this section, how surface friction and coating adhesion
affect formability in the various zinc coatings will be discussed.
5.3.1 Surface Friction
Surface friction can affect formability by modifying the strain distribution and the
strain state. When the relationship between surface friction and formability is considered,
it is important to consider only a constant strain state because surface friction is very
sensitive to strain state as discussed previously. A specific LDH value under a stretching
condition corresponding to the positive X- direction in Fig. 4.17(f) was matched with a
surface friction coefficient under the same condition in all five zinc coated steel sheets.
The result shown in Figure 5.11 indicates two different relationships between surface
friction and formability. The formability is inversely proportional to the surface friction
for the STZC1 and STZC2 steels whereas the formability is proportional to the surface
friction for the GI and GA steels. The conflicting result implies that the formability of
zinc coated steel sheets is not only a function of surface friction. Other factors like
coating adhesion must be taken into account. The steel types showing proportionality
between surface friction and LDH value (dashed circles in Figure 5.11) have either
different coating adhesion properties or a different fracture mechanism associated with
their coating. The GA steel has a much higher powdering value than the GI steel.
112
LDH
Surface Friction Coefficient
0.24
50
0.23
LDH(mm)
a
0.22
40
0.21
30
0.20
60
0.19
20
STZC1
STZC2
STZC3
GI
GA
Figure 5.11: Effect of surface friction on formability in various zinc coated steel sheets
The STZC2 steel with an IF grade steel substrate can exhibit damage to its steel substrate
by zincembrittlement whereas the STZC3 steel with an IFP grade steel substrate should
resist such damage. The steel types will not show a consistent relationship between
surface friction and formability if other factors are variable. R. Stevenson [50] also noted
in his work that changes in the punch-sheet coefficient of friction cannot account for the
changes in formability of galvanized steel sheet when the sheets have different levels of
coating adhesion. The STZC3 and GI steels (solid circle b in Figure 5.11) also do not
show an inverse proportionality between surface friction and formability. Even though
the coating adhesion properties and the fracture mechanism of these two types of steel are
very similar, the difference in surface friction between the two steels is too slight to show
113
an effect. The STZC1 and STZC2 steels (solid circle a in Figure 5.11) show an
inversely proportional relationship between surface friction and formability. These two
steels have not only a very similar coating adhesion and fracture mechanism due to
similar Fe-Zn intermetallic phase thicknesses and the same type of steel substrates so that
the effect of surface friction on formability is isolated, but also a significant difference in
surface friction. It can be concluded that high surface friction reduces the formability of
zinc coated steel sheets. Amit K. Ghosh [25] also showed that a reduction of friction
gives rise to an improvement in dome height at failure and that result holds universally
for a variety of materials.
The negative effects of surface friction on formability can be explained in two
ways. First, surface friction can modify the strain distribution during the forming of a
zinc coated steel sheet by acting as an additional constraint. The modification to the strain
distribution is defined in the following equation by Ghosh and Hecker [51].
ln
(2 z0 ) sin 2 ( s / ) r
= r + + f
P
(5.7)
where = punch radius, z0 = initial material thickness, s = arc distance between any
material point and the pole of the punch semi-arc length of contact, r = radial stress,
P = punch load which is the sum of components of pressure and friction, r = major
STZC1
STZC2
STZC3
GI
GA
60
57
54
51
48
45
42
39
36
-8
-6
-4
-2
10
12
14
C (sin c cos c c )
sin c {sin 2 c + ( c sin c cos c )}
2
(Appendix 3)
where LDH0 = Limiting dome height value at plane strain, = coefficient of surface
friction, c = the value of at the interface boundary defined in Fig.3.6 and C =
proportionality factor
115
steel gives rise to premature fracture lowering the steels formability. However, if crack
propagation is prevented at the steel substrate like an IFP grade which has no zinc
embrittlement, this can give rise to a huge improvement in formability regardless of the
average vertical height of the Fe-Zn intermetallic phases [Fig. 5.13 (b)]. A loss of coating
adhesion by a combination of fracturing of the coating layer and the steel substrate
(flaking) can be a much better indicator of formability than simple powdering weight.
Finally, a relationship between the LDH value and coating adhesion is presented in
equation 5.8.
LDH0
1
(FW)C
(5.8)
where FW= a loss of coating by a combination of fracturing of the coating layer and the
steel substrate, i.e. flaking weight, and C= frequency factor of flaking 1/{the at.%
phosphorus at steel substrate}.
55
55
50
LDH0
LDH0
50
45
45
40
40
35
35
0
10
12
10
12
Figure 5.13: Effects of coating layer and steel substrate on formability; a) effect of average
vertical height of Fe-Zn intermetallic phase, b) effect of steel substrate (IF and IFP *)
117
6. Conclusions
There were three objectives to this study : 1.) to evaluate surface friction 2.) to
assess coating adhesion of differently treated zinc coated steel sheet subjected to different
strain states and 3.) to analyze factors correlated with surface friction and coating
adhesion. The conclusions of this study are listed below:
(I)
Five types of zinc coated sheet steels were evaluated for their surface friction and
coating adhesion properties. Three of the steels (STZC1, STZC2, STZC3) were designed
to have zinc coatings with iron and phase contents intermediate to those of -phase
galvanneal (GA) and - phase galvanized (GI) coatings. The STZC steels experienced an
intermediate galvannealing process and had microstructure containing + phases. The
phase with 6~9 at% iron grew at the expense of the phase. The STZC1 steel that
experienced a galvannealing process at the lowest temperature had a thin phase whereas
the STZC3 steel that experienced a galvannealing process at the highest temperature had
a thick phase. The GI and GA steels used for comparison purpose had pure phase and
pure phase microstructures, respectively. The aluminum used for suppressing Fe-Zn
intermetallic phases concentrated in two specific areas, the extreme outer surface and the
interface between a zinc coating and its steel substrate. The GI and STZC1 steels with a
thin Fe-Zn intermetallic phase exhibited a high aluminum deposition toward their
extreme outer surface whereas the STZC3 and GA steels with thick Fe-Zn intermetallic
phases exhibited lower concentration of aluminum both at their extreme outer surface and
the interface between their zinc coatings and their substrates. After being subjected to an
electric discharge texturing process, the surface of five zinc coatings showed specific
118
morphologies, affecting the shape of the asperities and real area of contact of their zinc
coatings.
( II )
The surface friction coefficient was measured under different strain conditions
such as drawing and stretching. The coefficient of friction of the five types of zinc
coated steel sheets observed during drawing strain state cup tests exhibited a dynamic
characteristic where surface friction varied as a function of punch displacement due to
deformation of surface asperities and lubrication effects. The measured coefficient of
friction from the STZC1, STZC2, and GI steels with a small amounts of Fe-Zn
intermetallic phase ranged from 0.09 to 0.11 whereas that from the STZC3 and GA steels
with larger volume fractions of Fe-Zn intermetallic phase ranged from 0.13 to 0.14.
These values were obtained at a punch displacement of 18mm. This result indicates that
modification of the mechanical properties of a zinc coating by a change of microstructure,
especially the shear yield strength affects surface friction, agreeing with Bowden &
Tabors adhesion theory. Under a stretching condition, the coefficient of frictions ranged
from 0.19 to 0.24, higher values than those obtained under a drawing condition.
Stretching produces a significant amount of new surface which has intrinsically higher
frictional characteristics. Under stretching condition, the coefficients from the GI and
STZC steels were proportional to the real area of contact whereas the GA steel had a
coefficient of surface friction that depended inversely upon real contact area. The
predominant frictional factor was the real area of contact for the GI and STZC steels with
their low shear yield strength whereas a lubrication effect was the primary frictional
factor for the GA steel with its high shear yield strength coating.
119
( III )
The powdering weight was measured under different strain states such as
drawing, modest drawing, plane strain, and modest stretching. Under a drawing strain
condition, the values of the powder weight of the STZC, GI and GA steels were
0.002~0.0035g/m2, 0.006g/m2, 0.1g/m2, respectively. The powdering weight increased as
the volume fraction of phase increased in the coating layer among STZC steel sheets. A
high iron content in a zinc coating ( 12.2 at% ) increases the level of powdering based
upon the results from the GA steels. The GA steel showed the highest powdering weight
among the five steel types regardless of the strain state. The iron content in the zinc
coating appears to be the strongest factor affecting coating adhesion. The STZC steels
and the GI steel exhibited higher powdering weights under plane strain and stretching
conditions than under a drawing condition whereas the GA steel exhibited higher
powdering weight under a drawing condition than under the plane strain and stretching
conditions. The fracture mechanism could depend on microstructure so that the soft
phase based coatings fractured by a tension-controlled mode whereas the less ductile
phase base coatings fractured by a compression- controlled mode.
( IV )
The surface morphology, strain state, and shear yield strength of a zinc coating
are direct factors affecting surface friction whereas the microstructure of a zinc coating
and galvannealing condition are indirect factors affecting surface friction. Stretching
deformation was associated with increased surface friction regardless of the displacement
and type of zinc coating due to the continuous creation of new surface. An increase of
real area of contact and volume fraction of an Fe-Zn intermetallic phase increased surface
friction at a specific displacement where lubrication effects were negligible.
120
(V)
Coating adhesion depends directly on the microstructure of the zinc coating and
the strain state. It depends indirectly on the galvannealing condition, the steel substrate
and surface friction. The effect of each factor on coating adhesion can be summarized as
follows. The coating adhesion deteriorated as the average vertical height and brittleness
of the Fe-Zn intermetallic phase increased. phase based coating adhesion deteriorated
under a drawing condition. phase based coating adhesion deteriorated under plane
strain or stretching conditions. Coating adhesion deteriorated due to excessive
galvannealing processing which increased the volume fraction of the Fe-Zn intermetallic
phases and thickened the brittle oxide layers on the extreme outer surface of the coatings.
Coating adhesion to the IFP grade steel substrate could be improved by forming a /1
semicoherent interface so that a much higher interfacial shear strength is achieved and
zinc embrittlement in steel substrate is suppressed.
( VI )
Surface friction could affect the formability of zinc coated steel sheet by
affecting the strain state. Strain modification by a frictional stress affects either the major
strain or minor strain producing an increasingly non-uniform strain distribution, i.e. strain
localization. Localized necking by frictional constraint contributes to premature fracture
and reduced formability. Even though a zinc coated steel is formed under a stretching
condition, the redistribution of strain by frictional constraint can give rise to a plane strain
condition resulting in reduced formability.
( VII )
of the sheet steel. An Fe-Zn intermetallic phase that degrades coating adhesion can assist
crack initiation in a steel substrate due to a zinc embrittlement phenomenon that
121
decreases the fracture strength of the zinc coated steel sheet. It was suggested that a
flaking weight, i.e. an evaluation of the significance of crack initiation in the steel
substrate, should be taken into account to establish a relationship between coating
adhesion and the formability of zinc coated steels.
122
7. Appendix 1
Table A.1 Prediction of the number of fields (n) to be observed as a function of the desired
relative accuracy and of the estimated magnitude of the areal fraction of the constituent
Amount of
areal
fraction, Af
(%)
2
5
10
20
16
310
125
65
30
25
200
80
40
20
49
105
40
20
10
100
50
20
10
5
16
1250
500
250
125
25
800
320
160
80
49
410
165
85
40
t
2.776
2.571
2.447
2.365
2.306
2.262
2.228
2.201
2.179
No. of Fields n
19
20
21
22
23
24
25
26
27
123
t
2.101
2.093
2.086
2.080
2.074
2.069
2.064
2.060
2.056
100
200
80
40
20
7. Appendix 2
Table A.3 Data used for calculation of ratio of a shear stress due to friction to a shear yield
strength of pure zinc coating and an interfacial shear strength of pure zinc coating
Tensile yield
strength[44,45]
( y )
Shear yield
strength
Coefficient of
friction () at
drawing strain
0.10
10kN
74mm
214MPa
107MPa
Interfacial
shear strength
( i )
Area of blank
Shear stress
applied due to
friction
( f = p )
Ratio
D
(A= )
2
Normal stress
applied
F
(p= N )
A
14MPa
4.3 10-3m2
2.3MPa
0.233MPa
Diameter of
blank ( D )
124
( y =
f
y
y
2
f
i
0.002 0.017
7. Appendix 3
P
{sin c + ( c sin c cos c )}
2
where P = punch load, = punch radius, c = the value of at the interface boundary
defined in Fig.3.6 and = coefficient of surface friction
Now represent both the normal pressure under free friction, i.e. p ( =0), and the normal
pressure under friction, i.e. p ( 0). Then
P
{sin c + ( c sin c cos c )}
p ( 0) = 2
and
p ( = 0)
=
P
(sin 2 c )
2
p= p ( 0) p ( = 0)
=
where C is
C (sin c cos c c )
sin 2 c {(sin 2 c + ( c sin c cos c )}
Assuming then this pressure difference ( p ) is proportional to the change in LDH, one
obtains
LDH0( = 0 ) =LDH0( 0 ) +
C (sin c cos c c )
sin 2 c {sin 2 c + ( c sin c cos c )}
where LDH0= Limiting dome height at plane strain and C= Proportionality factor
125
8. References
[1] Burghardt, A.J. et al. , Galvatech 92 Conference Proceedings, 189, 1992.
[2] Irie, T, Zinc Based Steel Coating Systems: Metallurgy and Performance, TMS, 143,
1990
[3] Bowden, F. P. and Tabor, D. , Proceedings of the Royal Society A, 169 , 391 , 1939.
[4] Tabor, D. , Surface and Colloid Science, 5, 245-312, 1972.
[5] Orowan, E., Proceedings of the Institution of Mechanical Engineers, 150, 140, 1943.
[6] Shaw, M. C. and Mamin, P. A., Journal of Basic Engineering, 82, 342, 1960.
[7] Rabinowicz, E., Journal of Applied Physics, 22, 1373-48, 1951.
[8] Dalton, G. , SAE Technical Paper No. 2001-01-0081, Warrendale, PA, USA. ,pp.1-6,
2001.
[9] Stribeck, H. , Zeitschrift Des Vereines Seutscher Ingenieure, 46, 1342-48, 1902.
[10] Hess, D. and Soom, A., Journal of Tribology, 112, 147-152, 1990.
[11] Bay and Wanheim, T. , Wear, 43, 45, 1977.
[12] Alpas, A. T. and Inagaki, J. , ISIJ International, 40, 172-181, 2000.
[13] Amey, S. L. , Metallurgical and Materials Transactions A, 25A, 723-731, 1994.
[14] Janavicius, P. V., Galvatech 95 Conference Proceedings, Sept. ,17-21, 1995.
[15] Jordan, C.E. , Metallurgical and Material Transactions A, 25A, 2101-2110, 1994.
[16] Takechi, H. , ISIJ International, 34(1), 1-8, 1994.
[17] Rege, J. et al. , IF steels 2000 Proceedings, Pittsburgh, PA, 327-338, 2000.
126
127
[36] Inagaki, J. et al. , SAE Technical Paper Series 890349, Warrendale, 1989.
[37] Nakamori, T. et al. , In Corrosion Resistant Automotive Sheet Steels, ASM, Metals
Park, 139, 1988.
[38] Parisot, R. et al., Metallurgical and Materials Transactions A : Physical Metallurgy
and Materials Science, 35A, 813-823, 2003.
[39] Fox, R. T. et al., Metallurgical Transactions A: Physical Metallurgy and Materials
Science, 20A, 2179-82, 1989.
[40] Siegert, K., et al., Society of Automotive Engineers [Special Publication]SP, SP1132,1996.
[41] Hira, T. et al., Sosei to Kako, 34, 1141-6,1993.
[42] Garza, L. G. and Van Tyne C. J., Journal of Materials Processing Technology, 187,
164-168, 2007.
[43] Busby, T. J. et al., Journal of Nuclear Materials, 336, 267-278, 2005.
[44] Wakamatsu, Y. et al., J. Jap. Inst. Met., 39, 903, 1975.
[45] Foct, J., Scripta Metall. Mater. 28, 127,1993.
[46] Lin, C. S. and Meshii, M., Mechanical Working and Steel Processing Conference
Proceedings, 31, 99-105, 1994.
[47] Wen, B. et al., Physical Review Letters, 101, 2008.
[48] Tu, King-Ning et al., Electronic Thin Film Science, Macmillan Publishing Company,
1992.
[49] Zhong, W. et al., Zinc-Based Steel Coating Systems: Production and Performance
Conference Proceedings, 185-194, 1998.
[50] Stevenson, R., Research Publication, GMR-4283, 1983.
128
[51] Ghosh, A. and Hecker, S., Metallurgical Transactions A, 6A, 1065, 1975.
[52] Stevenson, R., Journal of Applied Metal Working, 3, 1984.
129