Int. J.

of Refractory Metals & Hard Materials 15(1997) 301-309

0 1997 Elsevier Science Limited
Printed in Great Britain. All rights reserved
0263-4368/97/$17.OO

PII: SO263-4368(96)00002-4

Temperature-Dependent Deformation and

Fracture Characteristics of a Tungsten Heavy
Metal

Erwin Pink,” Subodh &mar” & Robert Grillb

“Erich-Schmid-Institut fiir Festkiirperphysik, osterreichische Akademie der Wissenschaften,
A-8700 Leoben, Austria
‘Technologie-Zentrum, Plansee Aktiengesellschaft, A-6600 Reutte, Austria

(Received 23 October 1996; accepted 28 January 1997)

Abstract: The mechanical properties of a heavy metal with 925 wt.% tungsten
were investigated in tension. Three regions of distinct deformation characteristics
exist. The low-temperature behaviour (<4OO”C)resembles that of b.c.c. metals as
far as a steep strength-temperature curve and embrittlement are concerned, yet,
in detail, it deviates from that which would be predicted by the double-kink
theory. Between 450 and 650°C a strength peak appears, which is caused by
dynamic strain aging accompanied by negative strain-rate sensitivities and
serrated flow. This effect offers the possibility of a thermo-mechanical treatment
for improving the mechanical properties. Above 650°C strength and elongation
deteriorate rapidly. Fractography supports and explains these results. 0 1997
Elsevier Science Ltd. All rights reserved

INTRODUCTION occupies only a small volume fraction. The max-

imum size of the tungsten spheroids was about
Tungsten heavy metal is an alloy with b.c.c. 20-30 pm and it remained constant during the
tungsten spheroids embedded in a mostly f.c.c. elevated-temperature tests.
binder.’ While the theoretical understanding of
the plasticity of alloys with two equally-sized
phases is well-advanced,* it has not been tested EXPERIMENTAL RESULTS
against the actual behaviour of such tungsten
alloys. It is not known whether the two struc- Mechanical properties
tural components deform simultaneously or
consecutively at the various temperatures. The alloy was liquid-phase sintered and swaged
Therefore, it is of primary interest to clarify to to rods of 13 mm diameter. Tensile samples of
what extent the properties appear compatible 4 mm gauge diameter and 20 mm gauge length
with single-phase behaviour. Also, temperature- were prepared. Strength experiments were
dependent deformation mechanisms have, in carried out on two different tensile test
the past, not been determined in much detail. machines at nominal strain rates
The knowledge of deformation processes oper- i = 8.3 x 10-‘/s, at temperatures ranging from
ating at elevated temperature can be useful for - 147 to 800°C. The plastic strains were mea-
improving the properties by thermo-mechanical sured from the load-time curves, taking into
treatments. For the tests, a heavy metal with account the paper speed of the mechanically
925 wt.% tungsten was selected, in which the driven plotter. The high-temperature tests were
binder phase of 5 wt.% nickel and 2.5 wt.% iron conducted under a vacuum of 5.3 x lo-” Pa
301
302 E. Pink et al.

(4 x lo-” torr), The strain-rate sensitivities 40,

SRS = Ao/Alne were measured in tests at low - 35

0
0
temperatures by increasing the strain rate by a & t
- 30 00
factor of 5 and decreasing it again. In the high- 8 I 0 00

temperature tests, conducted on the other test 7 25

00
0 0
0
-
machine, the factor was mostly chosen to be
100, because the recording system only allowed
the observation of strain-rate changes in the
least sensitive load range, due to the lack of a
suppression device.
The load-elongation curves are ‘parabolic’ at
all temperatures. Figure 1 shows the tempera- -200 0 200 400 600 800

ture dependence of yielding in terms of the pro- Test temperature ( “C )

portional limits (T,,., at 0.1% strain, of the Fig. 3. The temperature dependence of necking as cal-
ultimate tensile stresses UTS and of the true culated from the diameter d, of the uniformly deformed
flow stresses G,,, at 10% strain. Figure 2 demon- shaft and the diameter d, of the neck.

1600 I I /
strates the elongation characteristics at the
point of the highest load where the uniform
deformation ends, E,, and at the point of frac-
ture, Ed; E, is the strain during necking. Below
about 3OO”C, the elongation values decrease
slowly, but complete brittleness is not even
reached at - 147°C. Thus, this ‘ductile-brittle
transition’ is, in agreement with other work,”
different from the sharp transition of tungsten
and other b.c.c. metals and alloys. The necking
200 I I
behaviour (given in Fig. 3 in terms of the reduc-
-200 0 200 400 600 800
tion of diameters) exhibits the same tendencies
Test temperature ( ‘C )
as the elongation characteristics. How the SRSs
Fig. 1. The temperature dependence of the O.l%-proof vary with strain and temperature is plotted in
stress, the ultimate tensile stress and the true stress at
10% strain, for a nominal strain rate = 8.3 x 10P’/s. the Fig. 4(a-c). The temperature dependence
of the SRSs at 10% strain is plotted in Fig. 5 for
the low-temperature mechanism.

Fractographic observations

The fracture surfaces of specimens which had

been tested at the different temperatures were
studied in the scanning electron microscope. At
$ 25
F
. the lowest test temperatures, from - 147°C
upward, the fracture surfaces consist mainly of
intact tungsten spheroids which are surrounded
by the brighter binder phase (Fig. 6). The
‘spheroids’ (the term derives from the appear-
ance of the tungsten grains in light-microscopy)
are in fact ‘polyhedrons’, since the grains are
400 600 800 prevented from further growing into a sphere as
Test temperature ( ‘C ) soon as two grains touch each other. Very few
Fig. 2. The temperature dependence of elongation charac- cleaved spheroids are seen. Above -30°C the
teristics. amount of cleavage increases, but intact tung-
 Temperature-dependent deformation and fracture of W-Ni-Fe 303

sten grains still dominate and tungsten-tung- 30

sten interfaces are, thus, seen in great numbers

25 .
(Fig. 7). On increasing the test temperature to 0000

above the transition temperature (roughly 2 20 . 0 0

42o”C), again, more and more tungsten

i!z
spheroids remain unfractured, contrasting with - 15 -
6Q”
0

previous reports,4 so that almost only tungsten-

2 0
(I) lo- 0

0
5 . 0
30 . . . . I.....,.. - 000
- 5092 1
0 ”
25. l z$.o. .
l ok
(A) _ -200 -100 0 100 200 300 400 500

O0 0 0 Test temperature ( *C )
‘;;; 20 - oQ 0 D vv -
AAA Fig. 5. The temperature dependence of the SRS at 10%
,3 - 112% 90% v plastic strain for the low-temperature mechanism.
4
- 15 -

0 2 4 6 8 10 12 14 16 18 20

Plastic strain (%)

1
6-

Fig. 6. Electron-scanning micrograph of a fracture surface

obtained at -70°C showing intact tungsten grains
-6' '.' ' '.I I embedded in a binder phase.
0 2 4 6 6 10 12 14 16 16 20

Plastic strain (%)

25

0 2 4 6 6 10 12 14 16 16

Plastic strain (%)

Fig. 4. The strain dependence of the strain-rate sensitiv-
ities for: (a) the low-temperature mechanism (&, = 5);
(b) the temperature range of DSA (E&,.= 100); and (c)
of the high-temperature region (EJE~ = 100).
304 E. Pink et al.

taminations which apparently had not been

loosened, since glide steps did not develop.
The existence of three different types of frac-
ture (cleavage of tungsten and along interfaces
of tungsten-tungsten and tungsten-binder) is
the reason why the ductile-brittle transition in
the heavy metal extends over a much wider

Fig. 8. Fracture surface of a sample tested at 325°C under

conditions of maximum ductility at low magnification.

tungsten interfaces dominate up to the highest

temperatures.
Between approximately 19 and 500°C the
fracture surface appears different, especially
when viewed under low magnification (Fig. 8). (4
Due to the good elongation (Fig. 2) and
specifically due to extensive necking (Fig. 3),
the diameters of the spheroids protruding from
the fracture surface are much smaller. The
binder has deformed further after having lost its
cohesion with the tungsten grains, so that these
become hidden to such an extent that even
holes seem to exist.
On the surface of the tungsten spheroids, and
especially on tungsten-tungsten interfaces, glide
traces can be recognized very easily (Fig. 9)
after testing between 160 and 625°C when the
(b)
spheroids do not break by cleavage. In the
Fig. 9. Tungsten grains with glide traces at high magnifica-
transition range to a rather brittle behaviour no tion (a) T = 48O”C, wavy slip lines, (b) T = 575”C, straight
glide steps are seen. Whether this is due to a slip lines.
complete lack of defomation of tungsten or
simply because of the small amount of deforma-
tion is difficult to decide. It appears plausible
that these glide steps destroy the cohesion
between binder and spheroids, and between
adjacent spheroids, causing fracture paths along
such interfaces. Indeed, the extent of cleavage
decreases as more and more glide traces appear
above 420°C as mentioned before. At the tem-
peratures of maximum elongation even the
binder, which appears deformed to a large
extent (Fig. S), exhibits glide traces (Fig. 10).
At the highest test temperatures, between 650
and SOO”C, cleavage is completely absent. Also,
in contrast to lower temperatures, no glide
traces exist (Fig. 11). Instead, the tungsten- Fig. 10. Glide traces on the binder phase from a test at
tungsten interfaces are often covered with con- 230°C.
 Temperature-dependent deformation and fracture of W-Ni-Fe 305

0 10% strain

*
P

0
-AaMe 0
0.0
Fig. 11. Fracture surface of a sample tested at 800°C. 0.0 0.2 0.4 0.6 0.8 1.0

u* I uo*

Fig. 12. Comparison of experimental data with the

temperature span than it does for the single- double-kink theory in terms of the activation volumes.
phase b.c.c. metals and their common b.c.c.
alloys. The reason why the embrittlement was,
at least at the lowest temperatures used in this mechanism which is not influenced by the
work, not complete may be due to the f.c.c. deformation structure (i.e. by the degree of
binder serving as a last intact structural link deformation). Figure 12 is a further check for
before the final fracture. the validity of the DK-mechanism. Assumptions
had to be made:

DEFORMATION MECHANISMS (1) For the stresses crOat zero Kelvin. They
are obtained from extrapolating the
curves in Fig. 1 (e.g. oo10 = 2000 MPa)
The following considerations are restricted
which is admittedly difficult.
mostly to the behaviour at medium degrees of
deformation. The testing procedures did not (2) For the athermal component cr, which
arises from long-range barriers to disloca-
allow a precise investigation of yielding and at
tion motion. The stress difference
strains immediately beyond it.
a(T) -6, corresponds to the thermally
activated applied stress o*(T). For tung-
The temperature range below 400°C
sten, tested at strain rates as applied in
this investigation, cfl remains the only
The deformation of b.c.c. metals at low tem-
applied-stress contribution (because the
peratures is characterized by strength values
DK-mechanism is completely thermally
increasing drastically with decreasing tempera-
activated) at about To = 600 K.’ There-
ture. The double-kink (DK) mechanism oper-
fore, the stresses at 350°C at yield or at
ates.5.6 In f.c.c. metals, the strength increase is
10% strain are approximated as the
moderate, due to the mechanism of glide dis-
respective athermal contributions.
locations cutting through a barrier of forest dis-
Another estimate is based on the plot of
locations. A determination of other specific
V* vs true stress: the stress where the
properties can add more information on which
curve becomes vertical is c~. Both esti-
of the two constituents of the heavy metal
mates yield CJ~~,~ = 750 MPa.
deforms predominantly. One first diagnosis
comes from the strain dependence of the SRS (3) For the activation volume v,* at zero
thermally-activated stress; 35 x 10V2’ cm”
or the stress activation volume
was chosen, slightly higher than the
v* = kT { alnd&* JT= 2kTISRS highest v* obtained in the tests.
with the thermally-activated shear stress z* These data were used to plot the normalized
approximated as 0*/2 (see below). The strain v*/v,* - 8/G0*- relation for true stresses at 10%
independence of the SRS (at least at the higher strain in Fig. 12. The diagram also contains the
temperatures, see Fig. 4(a)) and thus of v*, as theoretical relation as it was calculated from the
previously reported,7 could be a sign for a DK- DK-model.’ While the agreement with the
306 E. Pink et al.

theory is almost perfect for molybdenum” (a may operate, but due to high strain hardening
metal similar in many respects to tungsten), the in the vicinity of yielding it is difficult to
experimental data from the tungsten heavy measure exactly the load change which arises
metal deviate considerably at higher thermal- due to rate changes. It was shown by metal-
stress levels. Plausible and even excessive varia- lographic means that it is the binder which
tions of the parameters v<,*, co and op do not deforms initially,12 and a micromechanical
bring the experimental data points closer to the investigation limited the contribution of the
theoretical line. binder at room temperature to strains below
An activation enthalpy 2%,” thus to strains at which it is difficult to
analyze the rate-dependent characteristics with
AH = -v”T(~WI~T)~
the presently applied method.
can be calculated from v” and the temperature Taking into account this initial binder activity,
dependence of r*. The enthalpy AH,, which one could interpret the negative slopes of some
depends on the rate-controlling mechanism and of the SRS-strain curves in Fig. 4(a) as the
is obtained at about 4 eV (385 kJ/mol) from an binder contribution extending to higher strains
extrapolation to zero stress in Fig. 13, has a as the temperature decreases. This may be a
value which is very high in comparison to those clue for explaining the lack of agreement with
typical for the low-temperature mechanism of the DK-model at the low temperatures. Still
pure b.c.c. metals (for tungsten, AH, should further support comes from the lack of slip lines
amount to 0.8 eV (77 kJ/mol).’ While an addi- on the surfaces of the tungsten spheroids,
tional increase of 30% at most is to be expected reported earlier.
due to periodic internal stress fields’, lo in not When slip lines appear on tungsten grains
purified metals, both the present experimental between 90 and 350°C (i.e. close to the tem-
AH, and that of commercial molybdenum” are perature T,, of zero thermal stress), the v*-
similar. These Via-group metals appear to be values might stand after all for the
affected by their extremely low solubilities for DK-mechanism (see Fig. 12). The activation
interstitials. enthalpy AH0 (which derives from enthalpies
In Fig. 12, results from yield-stress data are obtained at these temperatures), though too
included, assuming that the activation volumes high to comply with the DK-theory, at least
measured at 10% strain are equally valid for resembles that of a commercial ‘single-phase’
yielding, since the temperature dependencies of refractory metal’ ’ and, thus, asserts the partici-
the thermal components of both CT,.,and glo are pation of the tungsten spheroids in the defor-
equal (Fig. 1; this differs from the behaviour of mation process at these higher temperatures.
a heavy metal with only 85 wt.% tungsten7). The old understanding was that the deforma-
However, it is not clear whether this assumption tion properties of a heavy alloy are determined
is realistic. There are indications of higher SRS- by the stronger tungsten phase and that the
values close to the yield point (not included in strength of the binder is raised during deforma-
Fig. 4(a)). Another deformation mechanism tion through a hydrostatic stress component to
the strength level of the tungsten.’ This view
does not address the question of why the two
constituents of the alloy participate to varying
5
extents when the test temperature is changed.

The temperature range SOO-700°C

% 3-
v .
. 10% strain In dilute alloys, dynamic strain aging (DSA)
2’ . . operates at temperatures where the diffusion of
the alloying or foreign element is fast enough to
interfere with the movement of the disloca-
0 ” ‘.’ a 3 “’
0 100 200 300 400 500 600 700 600 tions.14 The foreign element may be dissolved
Thermal stress O* ( MPa ) in the matrix on substitutional or interstitial
Fig. 13. The stress dependence of the activation enthalpies lattice sites in b.c.c. alloys, or on substitutional
of deformation. sites in f.c.c. alloys. Consequences of DSA are a
 Temperature-dependent deformation and fracture of W-Ni-Fe 307

Table 1. The effect of a 10% pre-deformation at temperatures of dynamic strain aging on the room temperature properties
Material Pre-deformation Tensile test at room tenperature
Temperature True stress at max. Fracture
mode (“C) load (Mpa) elongation
(So)
W-Ni-Fe 5;: tension 1266f8 13.3 * 1.1
tension 1365 +7 12.1* 0.9
Mild steel 20 rolling 538+38 13.4 f 1.4
400 rolling 592 + 38 12*0-&0*7

strength increase or a delayed strength decrease tungsten being strengthened and the binder
with increasing temperature, a negative SRS in being recrystallized is not clear. There is no
part of the affected temperature region, and conclusive evidence of recrystallization when
discontinuities along the stress-strain curves the micro hardnesses of the binder are com-
indicating an inhomogeneous deformation (i.e. pared after deformation at room temperature
a severely localized deformation mode, and a and at the temperature of DSA.15
Portevin-LeChatelier effect, i.e. a ‘jerky’ propa- DSA offers, in addition to mechanical work-
gation of the deformation front). ing or dispersion hardening,” a way to
The deformation characteristics of the heavy strengthen the heavy metal by a thermo-mech-
alloy observed around 600°C in particular the anical treatment. It has been reported20’21 that
strength peak (Fig. l), the negative SRS (Fig. pre-deforming an alloy at the temperature of
4(b)), the Portevin-Le Chatelier effect and the DSA improves the room-temperature proper-
pronounced straight glide traces in Fig. 9(b) ties. Not only are the ultimate tensile-strength
arising from severe strain localization all testify values raised, but the fracture elongations are
to the occurrence of such DSA.15 A negative not notably affected. Such results are listed in
SRS at 200°C’” could not be found. Contrary to Table 1 for the heavy alloy and for mild steel.
expectations, because the solubility of carbon in A larger increase in strength could possibly
pure tungsten is too small to initiate DSA,“*18 be achieved when rolling, which allows higher
it was proven that it is most probably the diffu- degrees of pre-deformation, is applied at the
sion of carbon which is responsible.” Although temperatures of DSA. The rolling temperature
pure tungsten cannot dissolve sufficient carbon will have to be higher than the peak tempera-
to initiate DSA, the tungsten in the liquid-phase ture in the tensile tests since, due to the higher
sintered alloy has a larger solubility for it, due deformation rates during rolling (estimated to
to its higher concentrations of substitutional be of the order of l-2 s-l), the temperature
iron and nickel. range of DSA will be raised. Since carbon
Of interest is the correspondent behaviour of within the tungsten lattice was identified to be
strength and elongation at 600°C - the tem- the cause of DSA in the heavy alloy,15 it is
perature of maximum DSA. The elongation possible to calculate the necessary deformation
data show the expected tendency, confirming rate with the help of the appropriate data.
the embrittlement due to DSA (c.f. the ‘blue A strengthening by means of static aging in a
brittleness’ of steels): they drop above 400°C similar temperature range which can be rein-
(Fig. 2) where the strength-temperature curve forced by pre-deformation has been described
in Fig. 1 begins to level off. However, once this before. ‘9,22 It was believed to be due to nano-
lower level is reached, further increasing the meter-sized particles within the tungsten grains
strength (Fig. 1) does not result in a further which are too small to be identified; it was
decrease of the elongation. Comparison with speculated that they are precipitates of nickel or
Fig 2 shows that also the elongation increases iron.19 The improvement was also traced back
upon approaching the temperature of the DSA- to dissolved and precipitated carbon.22 This is
strength peak. This exceptional behaviour is more plausible since both static and dynamic
contrary to the common understanding that the aging often coincide in the same material,
elongation deteriorates when the strength is caused by the action of the same type of dis-
improved. Whether it is a combined effect of solved element.
308 E. Pink et al.

(as, for instance, the result for yt at 700°C indi-

cates).

CONCLUSIONS

-200 300 400 500 600 700 800

Deforming the tungsten heavy alloy in a wide
temperature range dicloses the following
True stress o ( MPa )
Fig. 14. The strain-rate sensitivities of Fig. 4c, plotted
effects:
against the true stress.
(1) Below 4Oo”C, the steep increase of the
strength characteristics with decreasing
temperature and the resulting embrittle-
The temperature range above 700°C ment seem to comply with the low-tem-
perature behaviour of b.c.c. metals. Upon
A rapid loss of strength, as seen above 700°C in closer examination, however, the activa-
the present results, occurs in metals generally tion volumes deviate at the lowest tem-
above a ‘plateau’ region at more than 0.5 of the peratures from those demanded by the
melting temperature T,. Tungsten should double-kink theory. It appears possible
weaken at more than 1000°C. Therefore, the that the f.c.c. binder phase partakes in
tungsten spheroids are not involved in the the initial stages of deformation. That
decrease of the strength (indeed no slip traces this contribution is enhanced at the low-
can be seen on their surfaces, see Fig. 11). The est temperatures is presently only a
strain dependence of the SRS (Fig. 4(c)) also speculation. One would expect different
indicates that neither DSA nor a strain-inde- temperature dependences of the stresses
pendent mechanism (typical of a b.c.c. metal) in initial and later strain regions if dif-
operates. It should be a high-temperature pro- ferent crystal structures were involved in
cess which controls the deformation in the the deformation, however, no such effect
binder phase from 700°C (i.e. -0.57 T,,, for the was observed. Therefore, some coupled
Ni-Fe-binder) upwards. In Fig. 14 the SRSs effect may take place. It would be
are plotted against their respective true stresses interesting to see whether experiments
on the stress-strain curves. Their intercepts with materials with less binder phase
with the stress axis can be taken as athermal resemble the double-kink behaviour
stress contributions.23,24 Then the slopes of the more closely.
lines in Fig. 14 equal the stress sensitivity of the (2) Around 6OO”C, the heavy metal exhibits
strain rate DSA and all the accompanying features
like negative SRSs and (weak) serrated
12= {~ln~/~lno}, = c/ {&r/alne}, z AalASRS
flow. It is the carbon in the tungsten
which is also the stress exponent in the high- spheroids which is responsible.” Within
temperature rate equation the range of DSA, the gain in strength is
accompanied by an increase of the frac-
e = CJ”exp { - AHJkT >
ture elongation. This effect provides the
We obtain n ~223 for 700°C and about 5 for potential for strengthening the alloy by a
800°C. The high value for 700°C may be con- thermo-mechanical treatment without a
sidered as a meaningless transitional value. The simultaneous loss of ductility. It has to be
n for 800°C complies with the theoretical it = 3- explored whether this type of strengthen-
5 for diffusion-assisted dislocation creep. An ing could be combined with static aging
estimate of the activation enthalpy which also improves the strength.‘“,”
The results from the strain-rate changes
at elevated temperatures which provided
did not lead to a reliable result, probably since the information on the SRSs are quanti-
the temperature dependence of the stress in the tatively not correct because of the large
observed high-temperature range is still influ- applied ratio of 100. This can lead to two
enced by the preceding secondary mechanism types of errors in the low-strain portions
 Temperature-dependent
of the stress-strain curves. Effects which
again could arise from the binder will be
obscured and the onset strain for serra-
tions (i.e. the change-over from positive
to negative SRS-values) will be measured
falsely. When the rate is increased by a
high ratio, the new rate has to be main-
tained over a long strain range; mean-
while the mechanism could have been
modified without being noticed. Further-
more, applying a too large ratio may lead
to testing conditions outside the range of
DSA. It will be necessary to repeat these
tests on a more sensitive tensile test
machine which allows the observation of
stress increases and decreases in the most
sensitive load range so that small rate
ratios within a short strain distance can
be applied.
(3) Above 7OO”C, the binder phase is likely
to dominate the deformation. For con-
firmation, more experiments at higher
temperatures will be necessary so that an
activation enthalpy can be determined.
Fractographic studies revealed, besides
already known features like cleavage or inter-
face fractures, the existence of glide traces on
the surface of the tungsten spheroids. This fur-
nished the means to differentiate between
degrees of the contribution of tungsten to the
deformation in certain temperature ranges and
helped to explain some results from strength
tests.
ACKNOWLEDGEMENTS
This work was partly supported as Project P
9361-TEC by the Fonds zur Forderung der wis-
senschaftlichen Forschung in Vienna.
deformation and fracture of W-Ni-Fe 309
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