METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 34A, APRIL 2003967

Effects of Test Temperature and Grain Size on the Charpy

Impact Toughness and Dynamic Toughness (K
ID
) of
Polycrystalline Niobium
D. PADHI and J.J. LEWANDOWSKI
The effects of changes in test temperature (196 C to 25 C) and grain size (40 to 165 mm) on
the dynamic cleavage fracture toughness (K
ID
) and Charpy impact toughness of polycrystalline
niobium (Nb) have been investigated. The ductile-to-brittle transition was found to be affected by
both changes in grain size and the severity of stress concentration (i.e., notch vs fatigue-precrack).
In addition to conducting impact tests on notched and fatigue-precracked Charpy specimens, ex-
tensive fracture surface analyses have been performed in order to determine the location of ap-
parent cleavage nucleation sites and to rationalize the effects of changes in microstructure and ex-
perimental variables on fracture toughness. Existing finite element analyses and the stress field
distributions ahead of stress concentrators are used to compare the experimental observations with
the predictions of various fracture models. The dynamic cleavage fracture toughness, K
ID
, was
shown to be 37 4 MPa and relatively independent of grain size (i.e., 40 to 105 mm) and
test temperature over the range 196 C to 25 C.
1m
D. PADHI, Process Engineer-III, is with Applied Materials Inc., Santa
Clara, CA 95054. J.J. LEWANDOWSKI, Leonard Case Jr. Professor of
Engineering, is with the Department of Materials Science and Engi-
neering, Case Western Reserve University, Cleveland, OH 44106. Con-
tact e-mail: JJL3@pop.cwru.edu and deenesh_padhi@amat.com
Manuscript submitted June 19, 2002.
I. INTRODUCTION
THE continuing desire for increasing the efficiency of
turbine engines via operating at elevated temperatures has
led to exploration into various materials systems. Niobium
(Nb) is a refractory metal with the distinction of pos-
sessing excellent ductility at low temperature, high-
temperature strength, and liquid metal corrosion resis-
tance. These properties have encouraged researchers to
investigate a variety of Nb-base systems for potential
aerospace applications. Recently, a number of research
groups
[16]
have investigated the fracture and fatigue be-
havior of Nb-Si systems, which combine a refractory metal
intermetallic, Nb
5
Si
3
, with the terminal refractory metal
phase (i.e., Nb with Si in solid solution).
Recent research studies
[16]
have demonstrated that Nb
can be used as a tough reinforcement in ductile-phase-
toughened Nb
5
Si
3
composites. The success of such a sys-
tem is significantly affected by the mechanical behavior
of the toughening phase (Nb) as well as the interfacial
strength between the brittle constituent (Nb
5
Si
3
) and the
toughening phase. Considerable efforts have been directed
in the past toward understanding the effects of changes in
grain size, test temperature, and strain rate on the tensile
flow behavior, cleavage fracture stress, and static plane
strain fracture toughness of Nb.
[712]
However, the ductile-
to-brittle transition and fracture toughness of Nb under
dynamic testing conditions, key considerations for struc-
tural applications, have not been investigated to the same
extent. The present investigation examines the effects of
changes in test temperature and grain size on the Charpy
impact and dynamic impact toughness (K
ID
) of polycrys-
talline Nb. The studies reported have been conducted on
materials identical to those reported previously,
[7,8]
en-
abling direct comparison.
II. EXPERIMENTAL PROCEDURES
A. Materials Tested, Heat Treatments, and Specimen
Details
Commercial purity Nb (i.e., Nb
cp
) was obtained from
Cabot Corporation (Bethlehem, PA) in the form of hot-
rolled square plates having a nominal thickness of 10.5
mm. The composition, determined via wet chemical analy-
sis, was identical to that tested previously
[7,8]
(i.e., oxy-
gen 165 ppm, nitrogen 63 ppm, silicon 0.03 at. pct, bal.
Nb). Unnotched bend bar specimens (dimensions: 55
10.5 10.5 mm
3
) were machined from the plates so that
the long axis of the bend bar was along the rolling direc-
tion. Each bend bar was wrapped in tantalum foil and heat
treated in a vacuum of 10
5
torr to minimize oxidation.
The temperature and time of annealing were varied in
order to obtain a range of grain sizes, measured via the
linear intercept method, and are reported in Table I. The
specimens were furnace cooled to 500 C under high vac-
uum followed by cooling in N
2
atmosphere to room tem-
perature. The heat-treated specimens were cut in three mu-
tually perpendicular directions, ground, polished, and
etched using a solution of 62.5 vol pct distilled water,
31.25 vol pct nitric acid, and 6.25 vol pct hydrofluoric
acid for approximately 200 seconds. Representative mi-
crographs of the specimens are shown in Figure 1. Mea-
surements of grain size on the three mutually perpendic-
ular directions revealed homogeneity in grain structure
indicating complete recrystallization.
Subsized tension specimens (i.e., gage diameter
3 mm, and gage length 12 mm) were machined along
the original rolling direction following ASTM E8M-94.
[13]
Standard Charpy specimens were machined from the heat-
treated bars in the L-S
[13]
orientation such that the notch
968VOLUME 34A, APRIL 2003 METALLURGICAL AND MATERIALS TRANSACTIONS A
Table I. Summary of the Heat Treatments and Grain
Sizes of Nb
cp
Heat Treatment
Temperature Time Grain Size
Material (C) (Min) (mm)
Nb
cp
1200 45 57 7
1200 60 39 3
1300 90 104 16
1300 120 165 28
Fig. 1Microstructures of recrystallized Nb
cp
specimens.
was along the long transverse direction, in accordance with
ASTM E23.
[13]
The dynamic fracture toughness test spec-
imens (i.e., fatigue-precracked Charpy specimens) were
obtained by introducing a starter notch of approximately
3-mm depth using a diamond-impregnated wire saw. This
was followed by fatigue precracking at 125 C in a three-
point bend (3PB) configuration, in accordance with ASTM
E399.
[13]
The fatigue precracking was conducted on a
20 Kip MTS (Minneapolis, MN) servohydraulic machine
using an MTS 442 controller and a DEC (Maynard, MA)
PDP-11 computer at a frequency of 20 Hz and a stress
ratio (R) of 0.1. Based on previous results for this mater-
ial,
[8]
fatigue precracking was conducted to achieve a total
crack length between 0.45 and 0.55 W at 125 C. This
ensured a small plastic zone size ahead of the fatigue crack
tip due to the significantly higher yield stress at 125 C
(e.g., 426 MPa) compared to 25 C (e.g., 160 MPa).
[8,16]
B. Mechanical Testing
Individual tension tests were conducted at a strain rate
of 6(10
4
) s
1
at temperatures ranging from 196 C to
25 C on the Nb
cp
specimens using an Instron 1142 screw-
driven machine and an MTS servohydraulic machine fit-
ted with an ATS low-/high-temperature cabinet. The low
temperatures were obtained by injecting liquid N
2
vapor
into the cabinet at intervals controlled by a thermocouple.
Temperature variation during the tests was 1 C. The
load-load point displacement traces were used to calcu-
late the 0.2 pct offset yield strength (s
y
).
The notched Charpy and fatigue precracked impact
specimens were tested in a Wiedemann Baldwin (Summit,
NJ) instrumented impact tester. Load, deflection, absorbed
energy, and velocity of the tup were acquired as a func-
tion of time via the DYNATUP* instrumentation pack-
*DYNATUP is a trademark of INSTRON Company, Canton, MA.
age. The impact tests were conducted in the temperature
range of 196 C to 25 C by using a mixture of 2-methyl
METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 34A, APRIL 2003969
(a)
(b)
Fig. 2Schematic of the fracture surface analyses for (a) fatigue-precracked impact test specimen and (b) Charpy impact test specimen.
Fig. 3Effect of changes in grain size on 0.2 pct offset yield stress of
Nb
cp
.
butane and liquid nitrogen in varying proportions. A non-
instrumented Charpy impact tester with a tup of higher ca-
pacity (325.4 J) was used for tests at temperatures where
the absorbed impact energy was greater than 81.4 J. The
peak load, initial crack length measured from fractured
specimens, and specimen geometry were used to compute
the dynamic fracture toughness (K
ID
) according to ac-
cepted procedures
[14]
and K calibrations.
[13]
C. Fracture Surface Analyses
The fracture surfaces of the notched Charpy specimens
and the fatigue-precracked Charpy test specimens were
analyzed using a Hitachi (San Jose, CA) 4500 S high-
resolution field emission gun scanning electron micro-
scope. For each sample, a montage consisting of several
micrographs was taken in the central 7 mm (thickness di-
rection) of the specimen in order to exclude the area under
plane stress condition, as shown in Figure 2. Each mon-
tage was examined to identify the potential nucleation sites
of cleavage fracture. This was achieved by tracing the
cleavage river lines back to a region from where all the
river lines appeared to emanate, as conducted previ-
ously.
[7,8,15]
In some cases, multiple sites of apparent frac-
ture nucleation were identified. The distances of these po-
tential cleavage fracture nucleation sites from the notch
tip/precrack front were measured. The relative amounts of
brittle (i.e., cleavage) and ductile (i.e., dimpled) fracture
were also quantified for the entire specimen cross sections.
III. EXPERIMENTAL RESULTS
A. Mechanical Tests
The 0.2 pct offset yield strength of Nb
cp
for different
grain size/test temperature combinations are plotted as a
function of average grain radius
1/2
(d
1/2
) in Figure 3.
No yield points were observed in any of the tension tests.
At a given test temperature and strain rate, the yield
strength of Nb
cp
is found to be essentially independent of
grain size in the range of current investigation (i.e., 40 to
165 mm) and a strong function of test temperature. From
the current investigation, the calculated values for the
HallPetch slope (k
y
) for Nb
cp
were found to be very
low, i.e., 5.6(10
4
) N/m
3/2
, 2.65(10
4
) N/m
3/2
, and 4.35(10
4
)
N/m
3/2
at 196 C, 75 C, and 25 C, respectively.
Adams et al.
[9]
reported a k
y
value of 2.76(10
4
) N/m
3/2
at
20 C under a strain rate of 2(10
4
) s
1
. Johnson
[10]
in-
vestigated the effects of grain size (37 to 138 mm) and test
temperature (196 C to 20 C) on the tensile proper-
ties of commercially pure sintered niobium at a strain rate
of 10
4
s
1
. No effect of variation in grain size on yield
strength was observed. Churchman
[11]
conducted tension
tests on high-purity Nb over the temperature range of
180 C to 80 C. His results showed that the yield
strength was unaffected by the change in grain size from
approximately 13 to 395 mm. The lack of yield points in
the present and previous tests
[9,10,11]
suggests that the lack
of impurity-induced pinning of dislocations is one poten-
tial reason for the low value of k
y
obtained presently and
reported previously. The yield strength increased with in-
creasing strain rate,
[16]
in agreement with results reported
elsewhere.
[12,18]
970VOLUME 34A, APRIL 2003 METALLURGICAL AND MATERIALS TRANSACTIONS A
Fig. 4Ductile-to-brittle transition behavior of Nb
cp
(Charpy impact
test). Arrows indicate specimens did not fail.
Fig. 5Absorbed impact energy normalized by initial uncracked liga-
ment area.
Fig. 6Effect of strain rate and test temperature on the yield stress of
Nb
cp
. *Using empirical constitutive equation.
[18]
The impact energy (C
v
) obtained from the dial reading
on the Charpy impact machine is plotted as a function of
test temperature in Figure 4. Two specimens (for each
grain size) were tested at each test temperature for re-
peatability. The lower shelf regime is associated with a
low value of absorbed impact energy (6.5 J), while the
upper shelf energy values for the 40 and 105 mm Nb
cp
are
found to be nearly equal (258 J). At 25 C test tem-
perature, the impact energy decreases with an increase in
grain size. The other test temperatures did not produce as
large a change as that obtained at 25 C.
The impact energy normalized by the area of initial un-
cracked ligament is plotted as a function of temperature
in Figure 5 for both the notched and fatigue-precracked
specimens. It appears from this plot that the complete tran-
sition to the upper shelf regime has not occurred at 25 C
in the fatigue-precracked specimens. Alternatively, the
ductile-to-brittle transition temperature of fatigue-
precracked specimens is found to be higher than that of
the notched specimens regardless of grain size.
The dynamic fracture toughness (K
ID
) was computed
according to accepted procedures.
[13,14]
The validity of lin-
ear elastic fracture mechanics (LEFM) conditions was
verified using standard ASTM procedures
[13,14]
adopted
for dynamic testing conditions
[17]
:
[1]
where
calculated fracture toughness, and
dynamic yield strength at a strain rate

j.
The strain rate achieved during the impact test (

j) can be
estimated as
[18,19]
[2]
where
W specimen width;
S span of loading points (40 mm for Charpy test);
Q 1.94 and 2.57 for V-notch and fatigue-pre-
cracked Charpy specimens, respectively; and
load point displacement rate.
Equation [2] yields

j values of approximately 380 and

505 s
1
, respectively, for notched and fatigue-precracked
Charpy impact tests. Considering the dearth of data on
yield stress of Nb
cp
at these strain rates, the empirical de-
pendence of flow stress of Nb
cp
on strain rate and test tem-
perature, determined recently by Nemat-Nasser and
Guo,
[18]
was used for computations. Work conducted at
Case Western Reserve University over a more limited
range of strain rates is in agreement with the results of
d
t

#
j c
3WQ
2(S>2)
2
d B
d
t
R
s
#
j
yd

K
O

LEFM:
4
p
a
K
Q
s
#
j
yd
b
2
B, a
0
, (W a
0
)
Table II. Dynamic Fracture Toughness and Corresponding Plastic Zone Size Calculations for Fatigue-Precracked
Impact Tests
Impact Plane
Energy Strain Validity
Grain Thickness Width (J)

K
ID
Plastic Criteria
Size Temperature a
avg
(B) (W) P
max
(Dial (MP a Zone Size (L)
(mm) (C) (mm) (mm) (mm) (kg)* Reading) **) (mm)

(mm)

L B L a
avg
L (W a
avg
)
40 195 5.9 10.4 10.1 314.1 3.1 41.4 91 2.2 Y Y Y
40 150 5.5 9.3 10.1 299.3 3.1 39.1 119 2.9 Y Y Y
40 125 5.6 10.4 10.2 329.8 4.4 38.2 142 3.4 Y Y Y
40 75 5.0 10.4 10.2 288.2 12.2 27.5 102 2.5 Y Y Y
40 75 5.7 10.3 10.1 297.9 5.3 36.7 182 4.4 Y Y Y
40 50 6.0 10.3 10.1 309.5 8.1 43.1 291 7.0 Y N N
40 50 5.1 10.3 10.1 337.1 16.4 33.7 178 4.3 Y Y Y
40 25 5.6 10.4 10.1 315.4 13.9 37.6 260 6.2 Y N N
40 25 5.4 10.3 10.1 373.4 18.6 41.8 321 7.7 Y N N
40 0 3.8 10.3 10.1 540.3 35.6 37.2 297 7.1 Y N N
40 25 4.4 10.4 10.1 423.1 77.6 34.8 302 7.2 Y N N
105 195 5.6 10.5 10.2 351.2 3.4 40.6 88 2.1 Y Y Y
105 125 5.4 10.4 10.2 354.3 4.4 38.1 113 2.7 Y Y Y
105 75 5.3 10.3 10.1 316.9 9.8 34.0 156 3.7 Y Y Y
105 75 4.8 10.3 10.1 351.4 4.6 32.6 144 3.4 Y Y Y
105 50 5.3 10.4 10.2 322.7 13.7 33.9 180 4.3 Y Y Y
105 25 4.6 10.4 10.2 358.4 14.6 30.9 149 3.6 Y Y Y
105 25 5.0 10.3 10.1 368.2 22.4 35.9 237 5.7 Y N N
105 0 4.7 10.3 10.0 378.6 37.8 34.7 258 6.2 Y N N
105 25 4.4 10.4 10.2 396.2 41.0 31.8 253 6.1 Y N N
*Instrumented tup reading.
**Using P
max

Using dynamic yield strength at a strain rate of 500 s

1
.
[18]

Using Eq. [1].

1m
METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 34A, APRIL 2003971
Fig. 7Effect of test temperature and grain size on dynamic precracked
fracture toughness (K
ID
).
Validity Criteria Satised
Nemat-Nasser and Guos work
[18]
[Figure 6]. The K
ID
and
the corresponding plastic zone size data are presented in
Table II. The LEFM criteria are violated at the highest
temperatures tested (e.g., 25 C to 25 C), and the K
ID
values provide a lower bound estimate for dynamic frac-
ture toughness of the material in this regime. However, it
is important to note that both crack length and specimen
thickness satisfied the LEFM criteria at the highest tem-
peratures, as shown in Table II. The LEFM criteria at the
highest temperatures were only violated in some of the
cases by L a
avg
and (W a
avg
), as shown in Table II.
In the lower shelf regime, the K
ID
is found to be relatively
unaffected by changes in test temperature and grain size
over the range tested, as shown in Figure 7.
B. Fracture Surface Analyses
Scanning electron microscopy (SEM) fracture analy-
ses at low magnification revealed that all the fatigue-
precracked Charpy impact specimens exhibited a pre-
dominance of cleavage fracture up to test temperatures
of 25 C. However, above approximately 50 C, the
fine- and coarse-grained specimens exhibited small
stretch zones (e.g., 100 mm) along some portions of
the fracture surface adjacent to the fatigue precrack.
Representative SEM fracture surface montages for the
40-mm grain size Nb
cp
precracked specimens tested at
196 C and 25 C are presented in Figures 8(a) and
(b), respectively. For the Charpy V-notch specimens, the
fracture surface was predominantly cleavage in the
lower shelf regime, as shown in Figure 9. Tables III(a)
and (b) present the distances of the apparent cleavage
fracture nucleation sites from the stress concentrator
(i.e., notch and precrack, respectively), while Figures
10(a) and (b) plot these data. Quantification of the
amount of cleavage vs ductile fracture present on the
notched Charpy impact fracture surfaces
[16]
indicated
972VOLUME 34A, APRIL 2003 METALLURGICAL AND MATERIALS TRANSACTIONS A
(a)
Fig. 8Fracture surface montage of an Nb
cp
40-mm fatigue-precracked Charpy specimen. (a) test temperature 196 C and (b) test temperature
25 C. Apparent cleavage fracture nucleation sites are shown inside the boxes.
that the transition from predominantly cleavage fracture
to ductile fracture occurred between 50 C (i.e.,
80 pct cleavage) and 25 C (i.e., 100 pct ductile
did not fail) for the 40-mm grain size Nb
cp
. In contrast,
the 105-mm grain size Nb
cp
Charpy specimens revealed
this transition to occur between 25 C (i.e., 75 pct
cleavage) and 0 C (i.e., 100 pct ductiledid not
fail).
[16]
The specimens tested on the upper shelf did not
fracture into two pieces; the extensive plasticity in these
cases permitted the intact specimen to exit the impact
machine (Figure 4).
IV. DISCUSSION
The present work has investigated the effects of changes
in microstructure, specimen geometry, and stress state on
the ductile-to-brittle transition, as well as the energy ab-
sorbed/toughness under such testing conditions. The ini-
tial discussion will focus on observations related to the
ductile-to-brittle transition, followed by a discussion of
the magnitude of fracture toughness possible in the lower
shelf regime for such materials, despite the appearance of
cleavage fracture.
(b)
METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 34A, APRIL 2003973
Fig. 9Fracture surface montage of a Nb
cp
40-mm notched Charpy specimen tested at 75 C. Apparent cleavage fracture nucleation site is shown
inside the box.
A. Ductile-to-Brittle Transition
Early concepts of the ductile-to-brittle transition behav-
ior of a material consider the competition between flow and
fracture.
[2027]
As originally proposed by Ludwik,
[20]
brittle
fracture occurs when the local stresses exceed the brittle
fracture stress. Considerable work has investigated the ef-
fects of changes in various microstructural features on the
magnitude of the cleavage fracture stress in ferrous-based
systems.
[15,2328]
Work on Nb
[7,8]
reveals a strong effect of
grain size on the cleavage fracture stress, with an increase
in the cleavage fracture stress arising through the decrease
in grain size. Temperature-independent cleavage fracture
stresses in the range 1150 to 1500 MPa were reported by
Samant and Lewandowski
[7,8]
on material of nearly identi-
cal chemistry and grain size as that tested presently.
1. Smooth tensile specimens
Figure 11 illustrates the effect of changes in test tem-
perature on reduction in area for the smooth tension spec-
imens and reveals significant ductility (i.e., RA 50 pct)
at 196 C, despite the appearance of 100 pct cleavage
fracture at 50 C in the notched/precracked specimens.
This is consistent with Ludwiks concept,
[20]
because the
Table III(a). Summary of Locations of Apparent Cleavage Fracture Nucleation Sites: Charpy Impact Test
Distance of Apparent Sites of Average Location of Peak
Grain Test Cleavage Fracture Nucleation from Measured Tensile Stress
Size Temperature Notch Distance from Ahead of Notch
(mm) (C) (mm) Notch (mm) (mm)
[30]
40 195 182 173 77 93 208 221 230 169 61 170
40 125 514 216 192 336 384 168 302 134 250
40 75 239 231 239 296 251 30 340
105 195 215 239 92 110 110 153 68 62
105 125 240 275 178 384 240 309 271 70 212
105 75 374 392 383 13 320
105 25 637 263 519 473 191 310
Table III(b). Summary of Locations of Apparent Cleavage Fracture Nucleation Sites: Fatigue Precracked Impact Test
Distance of Apparent Sites of Average Location of Peak
Grain Test Cleavage Fracture Nucleation from Measured Tensile Stress
Size Temperature Fatigue Precrack Distance from Ahead of Crack
(mm) (C) (mm) Precrack (mm) (mm)
[39]
40 195 115 18 100 61 61 79 79 73 31 76
40 75 154 134 189 64 135 53 101
40 25 269 96 198 243 192 200 66
40 25 239 155 183 192 43
105 195 183 163 127 258 139 136 150 165 45 148
105 75 489 367 165 49 267 198 183
105 25 377 377
974VOLUME 34A, APRIL 2003 METALLURGICAL AND MATERIALS TRANSACTIONS A
(a) (b)
Fig. 10Effect of test temperature on the location of apparent cleavage fracture nucleation sites: (a) Charpy impact test and (b) precracked impact test.
Fig. 11Effect of test temperature on RA at fracture (

j 6(10
4
) s
1
).
yield stress at 196 C (approximately 730 MPa) is well
below the cleavage fracture stress (i.e., 1150 to
1500 MPa), as determined elsewhere.
[7,8]
2. Notched charpy specimens
The two important considerations in analyzing the tran-
sition behavior of Charpy impact specimens are (a) the
distribution of stress ahead of the notch and (b) the criti-
cal cleavage fracture stress as a function of test tempera-
ture. Prior to general yield, the strain rate (

j) experienced
by the specimen can be estimated using Eq. [2] and the
measured velocity of the impacting tup (i.e., 5.24 m/s),
producing

j value of 380 s
1
, several orders of magnitude
higher than that experienced during a static test. There-
fore, the effect of changes in strain rate on the stress dis-
tribution ahead of the notch and s
F
is required. Green and
Hundy
[29]
have studied the profile of the stress field ahead
of a Charpy notch under static and impact conditions and
showed that the stress field ahead of the notch is unaf-
fected by the impacting conditions, provided the mode of
deformation was unaltered. However, the increase in the
yield stress due to the increased strain rate experienced by
the material in the vicinity of the notch increases the mag-
nitude of stresses ahead of the notch tip.
More recent finite element model work
[30]
has charac-
terized the magnitude and distribution of stresses in a
notched Charpy bar loaded in 3PB to various fractions of
general yield, analogous to work by Griffith and Owen
[31]
on notched four-point bend bars. The maximum stress in-
tensification for a notched Charpy bar at general yield was
shown to be 2.57 for the slip line field solution,
[32]
while
an analysis of a notched four-point bend specimen tested
to general yield for a material with moderate linear work
hardening revealed the maximum stress intensification to
be 2.6.
[31]
Other work
[33,34]
on notched four-point bend
bars has shown that higher rates of linear or power-law
work hardening, beyond those exhibited presently, in-
crease these values. The maximum stress intensification
at general yield in a notched Charpy bar calculated using
three-dimensional FEM
[30]
for a material with power-law
hardening (i.e., n 0.15) was 2.5. This information is
used subsequently to estimate the Nil Ductility Tempera-
ture (NDT) and is then compared to the present results.
At the NDT, the conditions for general yield and brit-
tle fracture are satisfied
[28]
:
[3]
[4]
where
maximum stress intensification ratio ahead of
a Charpy notch,
maximum principal stress along the direction
of loading,
dynamic yield strength, and
cleavage fracture stress. s
F

s
yd

s
max
11

R
R
s
max
ll
s
yd
Rs
yd
s
F
METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 34A, APRIL 2003975
Fig. 12SEM photograph of the fracture surface of a Nb
cp
105-mm
Charpy impact test specimen tested at 25 C. The presence of a stretch
zone prior to cleavage fracture nucleation is clearly evident.
Considering that Cottrells model for grain size control
of the brittle fracture stress is obeyed for Nb as shown
earlier,
[7]
it is estimated that the s
F
values for 40- and
105-mm grain size Nb
cp
specimens are approximately 1800
and 1300 MPa, respectively. Using the values for s
F
(i.e.,
1800 MPa and 1300 MPa) and the values for R (i.e.,
approximately 2.6) in Eq. [3], calculated values for s
yd
at
the NDT are 690 and 500 MPa for Nb
cp
Charpy specimens
having 40- and 105-mm grain size, respectively. From
Nemat-Nasser and Guos work,
[18]
the yield strengths of
Nb
cp
at 100 C and 25 C are approximately 675 and
525 MPa, respectively, at a strain rate of 380 s
1
(Figure 6).
Similarly, from Briggs and Campbells experimental
data,
[12]
the yield strengths of Nb at 75 C and 25 C
are found to be 706 and 517 MPa, respectively, at a strain
rate of 100 s
1
. This estimates that the NDT of a 40-mm
grain size Nb
cp
should lie in the vicinity of 75 C, whereas
the NDT of 105-mm grain size Nb should be near 25 C.
The data reported in Figure 4 are qualitatively consistent
with the preceding arguments. The NDT, defined as the
temperature at which the Charpy impact energy first be-
gins to rise, appears to be near 50 C for the 40-mm grain
size Nb
cp
and is near 25 C for the 105-mm grain size
Nb
cp
. Quantification of the amount of cleavage vs ductile
fracture present on fracture surfaces
[16]
indicated that the
transition from predominantly cleavage fracture to ductile
fracture occurred between 50 C (i.e., 80 pct cleav-
age) and 25 C (i.e., 100 pct ductiledid not fail) for
the 40-mm grain size Nb
cp
. In contrast, the 105-mm grain
size Nb
cp
Charpy specimens revealed this fracture mode
transition occurred between 25 C (i.e., 75 pct cleav-
age) and 0 C (i.e., 100 pct ductiledid not fail).
[16]
In
the present studies, the transition from lower shelf to upper
shelf for Nb
cp
40-mm grain size occurs at approximately
50 C to 25 C and takes place between 25 C and
0 C for 105-mm grain size material. Fracture surface
analyses revealed that all the Charpy specimens fractured
via cleavage mode at test temperatures below the NDT.
However, as the test temperature increased beyond the
NDT, specimens of both grain sizes showed appreciable
amounts of stretch zones immediate to the notch tip
(Figure 12). In addition, increasing amounts of local
plasticity were observed at the apparent cleavage fracture
nucleation sites (Figure 13), where evidence of limited
amounts of ductile fracture was present both at the ap-
parent nucleation site (Figure 13(a)) and along one of the
cleavage river lines (Figure 13(b)). Such features were
nonexistent at the lower temperatures. In the upper shelf
region, impact specimens exited the machine intact due to
the extensive plasticity exhibited (Figure 4).
The profiles of load vs time obtained from the
instrumentation package for tests conducted at temper-
atures up to the NDT were linear to maximum load. In
these cases, the maximum load (L
max
) recorded during
the impact tests conducted below the NDT can be con-
sidered as the load at which cleavage fracture started to
initiate/propagate. Using L
max
, the nominal applied stress
at fracture for each of the test conditions can be calcu-
lated as
[35]
[5] s
nom

6M
b(W a)
2
[6]
where
M bending moment experienced by the bar (N.m),
B specimen thickness (m),
W specimen width (m),
a notch depth (m),
L
max
load to failure (N), and
S span of loading in Charpy impact test (m).
Using this approach, it is possible to qualitatively
compare the location of apparent sites of cleavage frac-
ture nucleation with that of the peak stress in a manner
described elsewhere
[7]
for specimens loaded under sta-
tic conditions. Recent work on Nb
[18]
is combined with
presently reported effects of changes in strain rate on
yield stress in Figure 7, showing reasonable justifica-
tion in using an empirical prediction of yield stress of
Nb
cp
as a function of strain rate and test temperature.
[18]
Using Eq. [5] and [6] and the yield stress of Nb
cp
at 380
s
1
(during the Charpy test), the s
nom
/s
y
values are com-
puted for Nb
cp
specimens having 40- and 105-mm grain
size for test temperatures near and below the NDT. Com-
bining this information with the stress field analyses of
Wang et al.,
[30]
the distances of the potential nucleation
sites are calculated and summarized in Table III(a); the
experimentally observed distances of fracture nucleation
sites are found to be close to the location of the peak
tensile stress, providing evidence of a tensile stress con-
trolled brittle fracture process, in agreement with sev-
eral investigators.
[7,15,23,31]
As the test temperature is in-
creased above 196 C, the yield stress decreases and
a higher nominal bending stress needs to be applied in
order to achieve the temperature-independent critical
brittle fracture stress (s
F
) for Nb.
[7]
Thus, s
nom
/s
y
in-
creases and the location of the peak tensile stress moves
farther away from the notch tip, consistent with the data
presented in Figure 10(a).
M
L
max
S
4
976VOLUME 34A, APRIL 2003 METALLURGICAL AND MATERIALS TRANSACTIONS A
(a) (b)
Fig. 13Higher magnification view of a cleavage fracture nucleation site in a Nb
cp
105-mm Charpy impact specimen tested at 25 C, illustrating
local plasticity (inside the boxes): (a) nucleation site and (b) cleavage river line.
3. Fatigue-precracked charpy specimens
From the plot of absorbed impact energy (normalized
by initial uncracked ligament area) vs test temperature
(Figure 5), it appears that complete transition into the duc-
tile regime is not achieved even at room temperature for
the fatigue precracked specimens. Furthermore, when
compared with the absorbed energy values from the V-
notch Charpy tests normalized by initial uncracked liga-
ment area, it is clear that for a given grain size, the tran-
sition temperature of Nb
cp
specimen is higher for the
precracked specimens tested in impact. This is consistent
with the higher stress intensification (R) achieved in a
precracked impact test due to the very small root radius
(r V 1 mm) of the fatigue precrack in contrast to that of
a Charpy notch (r 250 mm). The location of apparent
cleavage sites ahead of the fatigue precrack (Table III(b))
is discussed in Section B.
B. Dynamic Plane Strain Fracture Toughness (K
ID
)
It appears from Table II that the LEFM criteria (calcu-
lated using the s
y
values at a strain rate of 500 s
1[18]
are
only violated for specimens tested at temperatures above
50 C and 25 C for Nb
cp
specimens having 40- and
105-mm grain size, respectively. In addition, the load-time
history of the specimens tested at 50 C for the 40-mm
grain size Nb
cp
specimen did not exhibit any nonlinearity
prior to fracture. In contrast, the instrumented load-time
trace for specimens tested at 25 C revealed some evi-
dence of nonlinearity, indicative of plasticity or stable
crack growth. Similar observations were made for the 105-
mm grain size Nb
cp
specimens tested at 25 C or higher
temperatures. Beyond the LEFM validity regime, the K
ID
values probably underestimate the actual dynamic tough-
ness of the material due to the increased plasticity or sta-
ble crack growth.
Over the range of LEFM validity (i.e., 196 C to
50 C for 40-mm Nb
cp
and 196 C to 25 C for
105-mm Nb
cp
), Figure 7 revealed that K
ID
is virtually in-
dependent of test temperature and grain size. Over that
range, Figure 10(b) further revealed that the location of
the apparent cleavage fracture nucleation sites were not
as affected by changes in test temperature as demon-
strated in the notched Charpy specimens shown in Fig-
ure 10(a). This observation can be rationalized following
arguments used in the cleavage fracture of steels
[23,3638]
and for polycrystalline Nb,
[7,8]
where a specimen having
a sharp crack, as in the case of a fatigue precrack, would
fail via cleavage when the maximum principal tensile
stress (s
max
yy
) ahead of the crack exceeded the critical
cleavage fracture stress (s
F
) over a microscopically sig-
nificant (characteristic) distance. The severity of stress
state provided by a sharp crack results in high stress in-
tensification ahead of the crack tip. Finite element analy-
ses of the stress field ahead of a sharp crack
[39,41,42]
show
that the maximum stress intensification achieved in a
specimen having a sharp crack is higher than in a blunt-
notched specimen, and depends on the work-hardening
behavior of the material. Thus, the issue of exceeding the
s
F
becomes secondary, while extending the s
max
yy
above
the s
F
over the characteristic distance becomes the con-
trolling event.
To rationalize the results of the present investigation
in light of the preceding arguments, it is important to con-
sider the distance of apparent cleavage fracture nucleation
sites from the crack tip (x). From fracture surface analy-
ses of fatigue-precracked specimens (Figure 10(b) and
Table III(b), it appears that x is slightly dependent on test
temperature in the range 196C to 25C for speci-
mens having 40- and 105-mm grain size. At the highest
test temperatures, this probably arises due to crack tip
blunting and the appearance of stretch zones at the crack
tip (Figure 12). In precracked specimens, the cleavage
fracture can nucleate, stochastically, anywhere in the re-
gion where s
max
yy
exceeds the s
F
. Thus, it is reasonable to
argue that x is indicative of the characteristic distance.
Previous work has shown that s
F
is independent of tem-
perature for Nb.
[7]
The present work indicates that the
METALLURGICAL AND MATERIALS TRANSACTIONS A VOLUME 34A, APRIL 2003977
Fig. 14Comparison of the experimentally obtained dynamic fracture
toughness (K
ID
) data with the predicted values using Traceys stress field
analyses.
[39]
global stress (i.e., applied dynamically) required to prop-
agate a crack in a brittle manner is unaffected by changes
in test temperature (in the range-196 C to 25 C), pro-
ducing a nominally temperature-independent value for the
dynamic fracture toughness over the range of tempera-
tures tested.
Early work
[37]
has suggested that the plane strain frac-
ture toughness (K
IC
) of metals that fail via slip-induced
cleavage can be predicted using s
F
, x, and the distribu-
tion of stress field ahead of the crack. The stress analysis
due to Tracey
[39]
is used for the present estimation in the
manner used previously by Samant and Lewandowski:
[7,8]
for static fracture toughness measurements made on es-
sentially identical Nb materials. It should be noted that
the work-hardening exponent (n) has a strong effect on
the stress field profile. From the tensile tests in the pre-
sent investigation, n was found to be between 0.05 and
0.08 in the temperature range of 196 C to 125 C and
between 0.15 to 0.2 in 75 C from room temperature.
Based on this, n is assumed to be zero for the test
temperature range of 196 C to 125 C and 0.2 for
higher test temperatures. The yield stress (at 500 s
1
) val-
ues used in the estimation are calculated using the em-
pirical equation from Nemat-Nasser and Guos work.
[18]
The temperature-independent s
F
values for the 40 and
105-mm grain size specimens are estimated from data
from Samant and Lewandowski
[7]
as discussed earlier in
this article.
Figure 14 compares the effect of changes in test tem-
perature and grain size on the predicted plane strain dy-
namic fracture toughness (K
ID
) and the experimentally ob-
tained data shown earlier in Figure 7. It is evident that
Traceys model predicts reasonably well for the low-
temperature (196C to 75 C) tests. This is consistent
with the observations of catastrophic crack propagation,
without any stable crack growth at these temperatures.
However, at higher temperatures (i.e. T 25 C), the
models prediction of fracture toughness is significantly
higher than that obtained experimentally. At these temper-
atures, the criteria for linear elastic fracture mechanics are
violated, as shown in Table III, and the experimentally ob-
tained K
ID
values underestimate the predicted toughness in
the manner demonstrated by Samant and Lewandowski
[7,8]
for static tests on similar materials. Attempts at using crack
gages to document/record any stable crack growth during
the instrumented impact tests at 75 C were unsuccess-
ful due to the difficulty and space limitations provided by
the impacting tup and specimen holder.
[16]
However, crack
gages were successfully used to record stable cracking of
these materials at high testing velocities and low tempera-
tures on a servohydraulic testing machine. These tests were
not conducted under the impact conditions used presently
and are reported elsewhere.
[16,40]
V. CONCLUSIONS
1. Smooth Nb
cp
tension specimens having grain sizes
ranging from 40 to 165 mm exhibited ductile fracture
when tested at a strain rate of 6(10
4
) s
1
over the test
temperature range of 25 C to 196 C. Over this
range, the HallPetch slope (k
y
) was found to vary be-
tween 2.65(10
4
) and 5.6(10
4
) N m
3/2
.
2. The ductile-to-brittle transition temperature of notched
Nb
cp
Charpy specimens was grain size dependent. The
NDT of 40-mm grain size Nb
cp
Charpy specimens was
near 50 C, while that of 105-mm grain size Nb
cp
Charpy specimens was near 25 C. The NDT of the
fatigue-precracked impact specimens was much higher
than that of notched Charpy specimens, consistent with
the differences in stress state between the specimens
tested.
3. All specimens tested at temperatures below the NDT
exhibited cleavage fracture with multiple sites of ap-
parent cleavage fracture nucleation located ahead of
the notch tip, consistent with tensile-stress-controlled
cleavage fracture. Increases in test temperature pro-
duced large increases in the distance ahead of the
notch where the apparent cleavage nucleation sites
were located, in rough agreement with the location
of peak tensile stress available from FEM analyses.
At temperatures above the NDT, local plasticity at
the notch and at the apparent cleavage fracture nu-
cleation sites was clearly evident. Extensive plastic-
ity was exhibited on the upper shelf without cata-
strophic fracture.
4. The plane strain dynamic cleavage fracture toughness
(K
ID
) was essentially independent of test temperature
(over the range 196 C to 50 C for 40-mm grain
size Nb
cp
and 196 C to 25C for 105-mm grain
size Nb
cp
) and grain size (40 to 105 mm). Despite the
predominance of cleavage fracture, the dynamic
cleavage fracture toughness was approximately 37
4 MPam.
5. The average distances of apparent cleavage fracture nu-
cleation sites from the fatigue precrack exhibited a
slight dependence on test temperature and grain size
over the range tested. At the highest test temperatures,
this likely results from crack-tip blunting and the
changes in stress distribution that are produced. Com-
parisons to available models of cleavage fracture
toughness revealed reasonable agreement for temper-
atures below the NDT.
978VOLUME 34A, APRIL 2003 METALLURGICAL AND MATERIALS TRANSACTIONS A
ACKNOWLEDGMENTS
The authors thank AFOSR (Grant No. F49620-96-1-
0164 and F49620-00-1-0067) for partial support of this
work. Partial support by Reference Metals Company
and supply of materials by Cabot Corporation are also
appreciated.
REFERENCES
1. M.G. Mendiratta and D. Dimiduk: Scripta Metall. Mater., 1991,
vol. 25, pp. 237-45.
2. M. Mendiratta, D. Dimiduk, and J.J. Lewandowski: Metall. Trans.,
A1991, vol. 22A, pp. 1573-84.
3. J.D. Rigney and J.J. Lewandowski: Metall. Mater. Trans., 1996,
vol. 27A, pp. 3292-306.
4. J. Kajuch, J. Short, and J.J. Lewandowski: Acta Metall., A, 1995,
vol. 43, pp. 1955-67.
5. W.A. Zinsser, Jr. and J.J. Lewandowski: Metall. Mater. Trans.,
A1998, vol. 29A, pp. 1749-57.
6. B.P. Bewlay, J.J. Lewandowski, and M.R. Jackson: JOM, 1997,
vol. 49, pp. 44-45.
7. A.V. Samant and J.J. Lewandowski: Metall. Mater. Trans. A, 1997,
vol. 28A, pp. 389-99.
8. A.V. Samant and J.J. Lewandowski: Metall. Mater. Trans. A, 1997,
vol. 28A, pp. 2297-307.
9. M.A. Adams, A.C. Roberts, and R.E. Smallman: Acta Metall., 1960,
vol. 8, pp. 328-37.
10. A.A. Johnson: Acta Metall., 1960, vol. 8, pp. 737-40.
11. A.T. Churchman: J. Inst. Met., 1960, vol. 88, pp. 221-22.
12. T.L. Briggs and J.D. Campbell: Acta Metall., 1972, vol. 20, pp.
711-24.
13. Annual Book of ASTM Standards, ASTM, Philadelphia, PA, 1994,
vol. 03.01.
14. J. Srawley and W. Brown: ASTM Special Technical Publication 410,
ASTM, Philadelphia, PA, 1966.
15. J.J. Lewandowski and A.W. Thompson: Metall Trans. A, 1986, vol.
17A, pp. 1769-86.
16. D. Padhi: Case Western Reserve University, Cleveland, OH, un-
published research, 2000.
17. T.L. Anderson: Fracture MechanicsFundamentals and Applica-
tions, 2nd ed., CRC Press, Boca Raton, FL, 1995.
18. S. Nemat-Nasser and W. Guo: Mater. Sci. Eng. A, 1999, vol. 284,
pp. 202-10.
19. R. Sandstrom and Y. Bergstrom: Met. Sci., 1984, vol. 18, pp. 177-86.
20. P. Ludwik: Z. Ver. Deut. Ing., 1927, vol. 71, pp. 1532-36.
21. A.H. Cottrell: Trans. TMS-AIME, 1958, vol. 212, pp. 192-203.
22. J.W. Taylor: J. Inst. Met., 1958, vol. 86, pp. 456-63.
23. J.F. Knott: J. Iron Steel Inst., 1966, vol. 204, pp. 104-11.
24. R.W. Armstrong, G.R. Irwin, and X.J. Zhang: George R. Irwin
Symp. Cleavage Fracture, K. Chan, ed., TMS, Warrendale, PA,
1997, pp. 51-58.
25. R.W. Armstrong: Phil. Mag., 1964, vol. 9, pp. 1063-70.
26. R.W. Armstrong: Metall. Trans., 1970, vol. 1, pp. 1169-76.
27. N.J. Petch: Acta Metall., 1986, vol. 34, pp. 1387-95.
28. J.F. Knott: Fundamentals of Fracture Mechanics, Butterworths,
Boston, MA, 1979.
29. A.P. Green and B.B. Hundy: J. Mech. Phys. Solids, 1956, vol. 4,
pp. 128-44.
30. G.Z. Wang, J.H. Chen, and J.G. Wang: Int. J. Fracture, 2003, in press.
31. J.R. Griffiths and D.R.J. Owen: J. Mech. Phys. Solids, 1971, vol.
19, pp. 419-31.
32. R. Hill: Mathematical Theory of Plasticity, Oxford University Press,
London, 1950.
33. D.R.J. Owen, G.C. Nayak, A.P. Kfouri, and J.R. Griffiths: Int. J.
Num. Meth. Eng., 1973, vol. 6, pp. 63-73.
34. D.J. Alexander, J.J. Lewandowski, and A.W. Thompson: J. Mech.
Phys. Solids, 1986, vol. 34, pp. 433-54.
35. J.M. Alexander and T.J. Komoly: J. Mech. Phys. Solids, 1962, vol.
10, pp. 265-75.
36. T.R. Wilshaw and P.L. Pratt: J. Mech. Phys. Solids, 1966, vol. 14,
pp. 7-19.
37. R.O. Ritchie, J.F. Knott, and J.R. Rice: J. Mech. Phys. Solids, 1973,
vol. 21, pp. 395-410.
38. R.O. Ritchie, B. Francis, and W.L. Server: Metall. Trans. A, 1976,
vol. 7A, pp. 831-38.
39. D.M. Tracey: ASME J. Eng. Mater. Technol., 1976, vol. 98, pp.
146-51.
40. D. Padhi and J.J. Lewandowski: Case Western Reserve University,
Cleveland, OH, unpublished research, 2002.
41. J.W. Hutchinson: J. Mech. Phys. Solids, 1968, vol. 16, pp. 13-31.
42. J.R. Rice and G.R. Rosengren: J. Mech. Phys. Solids, 1968, vol. 16,
pp. 1-12.
COPYRIGHT INFORMATION
TITLE: Effects of Test Temperature and Grain Size on the
Charpy Impact Toughness and Dynamic Toughness (KID)
of Polycrystalline Niobium
SOURCE: Metall Mater Trans Part A 34A no40 Ap 20032000
The magazine publisher is the copyright holder of this article and it
is reproduced with permission. Further reproduction of this article in
violation of the copyright is prohibited. To contact the publisher:
http://www.springerlink.com/content/1073-5623/