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with the tensile axes parallel to the rolling direc- peratures, and this led to a microstructure con-
tion. The specimens were annealed in air at sisting of uniform fine grains with dimensions
773 K for 11 h to allow for static recrystallization similar to that in the fine-grained core [21, 23].
and the stabilization of microstructure. Tensile Prior to tensile testing, the fine-grained core had
tests were carried out in an Instron machine an initial spatial grain size d = 5.4 pro, where
modified to operate at constant true strain rates. d = 1.74L with /~ the average linear intercept
The specimens were tested at a temperature of grain size.
723 K and at strain rates between about 10 -5
and 10-l s-~ to determine the variation with
3. Experimental results
strain rate in both the flow stresses and the elon-
gations to failure. A few additional experiments 3.1. The variation in flow stress with strain rate
were performed in which tensile tests were inter- Figure 2 illustrates the variation in flow stress
rupted prior to specimen failure. a with strain rate g for the experimental condi-
The cross-sectional areas of fractured speci- tions used in this study. It is clear that the A1-Li
mens were measured along the gauge length. As alloy exhibits a sigmoidal relationship between
illustrated in the schematic Fig. 1, the cross- the flow stress and the strain rate, which is typical
sectional areas were measured from one end of of superplastic alloys. The data shown in Fig. 2
the gauge length, /, and these data were normal- may be divided into three regions: a region I at
ized with the total gauge length at fracture, Lf, to f < 10 -4 s-l, a superplastic region II at strain
facilitate a direct comparison of data from speci- rates between about 10 -4 and 3 x 10 -3 s -1 and a
mens with varying gauge lengths at fracture. region III at g > 3 x 10 -3 s -J. The strain rate
The deformed specimens were sectioned sensitivity m, given by the slope of the curve in
parallel to the tensile axis and polished metallo- Fig. 2, is about 0.45 at strain rates between about
graphically. The final stage of polishing was con- 10 -4 and 10 -3 s-l, and the value of m decreases
ducted with MgO powder using very light both at g< 10 -4 s- 1 and at g> 3 × 10 -3 s- ~. The
pressure. The development of internal cavitation vertical arrows in Fig. 2 show the strain rates used
during deformation was studied by examining the in the following study on flow localization and
polished specimens by both optical and scanning cavitation.
electron microscopy (SEM). The cavity nuclea-
tion sites were identified qualitatively using 3.Z The variation in elongation to failure with
energy-dispersive X-ray analysis in an SEM. The strain rate
polished sections were then etched for about 20 s Figure 3 illustrates the variation in elongation
in a solution of 1.5 ml HC1, 2.5 ml HNO3, 2 g to failure with strain rate. The maximum elonga-
NaF and 195 ml H 2 0 to determine the variation tion to failure of 560% is obtained at a strain rate
in grain size with experimental conditions. The of 3× 10 -4 S-l. A comparison of Figs. 2 and 3
fracture surfaces of selected specimens were also
characterized by SEM. 60
Inspection of the alloy after annealing revealed I I ' ' ' ' ~'"1
the presence of a bimodal grain size distribution T=7~K
at the surfaces and a fine-grained core. Prelimi-
nary experiments indicated that the coarse grains
at the surfaces recrystallized dynamically during 10 ~ s ~ , , j " ~ l 0.45
the initial stages of deformation at elevated tern-
800
I I ........ I
AI - 2.6% Cu - 2.4% Li - 0 . 2 0 Zr IL
T = 723 K
600
400
!1
200
¢
o I 1 , , ...... I
10-5 10-4 10-3 10-2 10-1
(s -1) II
Fig. 3. The variation in elongation to failure with initial
strain rate, where AL is the change in gauge length and L , is
the initial gauge length.
100
80
/
6o/
<co
40
10
0.2
I
~:(S-1)
• . 5 x 10"5
0 3 x 10`4
I
0.4
T-723 K
n l . 3 x 10-2
t~L / LO (%)
I
0.6
360
560
180
I
0.8
l\
1.0
m,-
50 p m
t-----q
.Q/Lf
Fig. 7. Optical micrograph of a region near the fracture tip of
Fig. 5. The variation in the reduction in area with the the specimen pulled to failure at g= 1.3x 10 -2 s-L The
normalized gauge length at failure for the specimens tested at tensile axis is horizontal.
the highest, optimum and lowest strain rates used in this
study; A~ and AA are the original cross-sectional area and
the changes in cross-sectional areas respectively. The vertical
arrows indicate the locations of the fracture tips.
1150 Pm I
~_30 p m I
Fig. 9. Optical micrograph of a region near the fracture tip Fig. 10. A higher magnification optical micrograph of the
of the specimen tested at g = 3 x 10 a s - ~.The tensile axis is specimen pulled to failure at g=3 x 10 -4 S I. The tensile
horizontal. axis is horizontal.
There is a possibility that the value of m typically equal to about unity in region II. The
changes during a tensile test so that m determined experimental measurements indicate that the
from the initial stages of deformation (Fig. 2) may grain growth per unit strain, Ad/Ae, is equal to
not reflect the true resistance to necking during 6.4, 5.1 and 2.2/~m for the specimens pulled to
an entire tensile test. Following the earlier sugges- failure at strain rates of 5 x 10-5, 3 x 10 -4 and
tion of Ghosh and Ayres [39], Lian and Baudelet 1.3x 10 -' s -I respectively. These results are
[40] have shown analytically that ductility is consistent with previous detailed analyses of data
governed largely by the value of m just prior to on other superplastic alloys [47] and they imply
failure. However, a recent detailed study by that the rate of strain hardening increases with a
Caceres and Wilkinson [41] revealed that the decrease in strain rate, since the flow stress
value of m remains essentially constant during increases with grain growth.
superplastic deformation. Therefore it is sug- Based on the above discussion, it is concluded
gested that while the value of rn may change that the optimum elongations are obtained at the
during a tensile test, the occurrence of maximum lower end of region II, because under such condi-
ductility at strain rates towards the lower end of tions an appropriate combination of strain rate
region II is not caused by a change in m during sensitivity and strain hardening provides the
tensile tests. maximum resistance to flow localization. At
It is now recognized that most superplastic strain rates in the middle of region II the strain
materials cavitate during deformation and that rate sensitivity is high but the contribution of
failure is caused frequently by the process of cavi- strain hardening to necking resistance is low; in a
tation [42-44]. Therefore a difference in levels of similar manner, at lower strain rates in region I,
cavitation with strain rate may lead to a lack of a although the contribution of strain hardening is
correlation between maximum ductility and high, the strain rate sensitivity is low.
maximum m. However, a detailed inspection of
micrographs such as Figs. 9 and 12 suggests that 4.3. The nucleation of cavities
in the present study there is very little difference The nucleation of cavities is an important first
in the levels of cavitation in regions I and II. An step in the process leading to cavitation failure in
essentially identical observation was reported many superplastic alloys. In the present study,
recently by Caceres and Wilkinson [45]. It is metallographic inspection of deformed speci-
therefore concluded that the occurrence of maxi- mens reveals that cavities nucleate preferentially
mum ductility at the lower end of region II is not at coarse AI-Fe-Cu particles. In addition, both
caused by a difference in levels of cavitation. the increase in the number density of cavities and
As shown by Hart [31], the resistance to flow the distribution of cavity sizes observed at any
localization is generally provided by a combina- given strain, as noted from Figs. 8 and 9, suggest
tion of two factors: (a) a high value of m and (b) a that cavities nucleate continuously during super-
high value of the strain-hardening coefficient 7 plastic deformation. This observation is similar to
(= 6l~0/6e). In early work it was assumed that a recent report on cavitation in a superplastic
superplastic materials exhibit negligible strain commercial copper alloy [48].
hardening and therefore the resistance to flow Stowell [42] has suggested that, because of the
localization and ductility were correlated directly extensive thermomechanical treatment applied to
with rn [37]. Hamilton [46] has recently examined induce a fine grain size, cavities may exist prior to
the combined effect of m and 7 on flow localiza- elevated temperature deformation in many super-
tion during superplastic flow. In the present study plastic alloys. There is some experimental evi-
it is anticipated that the considerable grain dence indicating that coarse particles may crack
growth observed during deformation will lead to during ambient temperature deformation in
strain hardening* because, in superplastic A1-Li alloys [49, 50]. However, a detailed inspec-
materials tested at a constant strain rate, o oc d', tion of the alloy used in the present study failed to
where d is the grain size and the exponent c is reveal the existence of cavities prior to super-
plastic deformation. In addition, there was no
evidence of particle cracking in specimens either
*As noted previously [21], the occurrence of strain hard- before or after superplastic deformation, Fig. 11,
ening may not be apparent in stress-strain curves, because
the flow stresses may be underestimated in the presence of
and cavities appeared to nucleate during super-
diffuse necking. plastic deformation. In this context it is important
56
to note that, because of the low flow stresses increased considerably, the rate of grain growth
associated with superplastic flow, only cavities decreases and this reduces the level of accommo-
with fairly large dimensions may remain stable dation to grain boundary sliding [52]. However,
against surface tension forces, and cavities with recent careful studies of concurrent grain growth
radii less than r 0 (= 2v/a, where v is the surface in several superplastic alloys [47], including a
energy) will tend to be sintered at elevated tem- Zn-A1 alloy, indicate that the rate of grain growth
peratures. For the present study, using typical remains constant throughout a tensile test.* Con-
values of o = 10 MPa and v = 1 J m-2, the value sequently, a decrease in the rate of grain growth
of r 0 is determined to be about 0.5/~m. Cavities does not appear to be a plausible explanation for
with these dimensions should be clearly resolved the nucleation of cavities during the later stages of
by SEM, so that the failure to observe any pre- deformation. The present experimental results
existing cavities is not related to the lack of reso- from a specimen pulled to an elongation of 300%
lution. under optimum conditions appear to indicate that
Bampton and Edington [51] and Pandey et al. a critical grain size exceeding about 12 /~m is
[17] have shown that hydrogen gas bubbles may necessary to nucleate cavities. However, an
form in aluminum-based alloys during exposure inspection of the specimen pulled to failure at
to elevated temperatures. In the present study, 1.3 x 10 -2 s- ~ reveals that near the fracture tip
microstructural examination of annealed speci- where cavitation occurs, the grain size is about
mens prior to tensile testing did not reveal the 8.4 ,um. These results indicate therefore that the
presence of hydrogen gas bubbles. However, it is critical grain size to nucleate cavities depends
important to note that in the presence of gas pres- upon the experimental conditions. It is suggested
sure, cavities with dimensions less than r 0 may that the occurrence of grain growth is not related
remain stable, so that it is not possible to rule out directly to the nucleation of cavities, but that con-
completely the existence of very small gas current grain growth assists indirectly in nucleat-
bubbles. ing cavities by increasing the flow stress during
An interesting aspect of this study is the obser- deformation. A similar suggestion was incorpor-
vation that cavitation does not occur during the ated by Ghosh [53] in a theoretical model for con-
initial stages of deformation. Thus, for example, tinuous cavity nucleation in a superplastic
cavitation was not observed under optimum con- aluminum-based alloy.
ditions in a specimen pulled to an elongation of
100%, and even in a specimen pulled to an elon-
gation of 300%, cavitation was observed only in
4.4. The rate-controlling cavity growth
the highly deformed central region of the gauge
mechanisms
It is now recognized that in superplastic
length. Microstructural inspection also revealed
materials cavities, upon nucleation, may grow
the occurrence of concurrent grain growth during
predominantly by one of three independent
deformation, such that in the specimen deformed
mechanisms [54-56]: (a) diffusion, (b) super-
under optimum conditions to an elongation of
plastic diffusion and (c) power-law. The cavity
300%, the grain size had increased from an initial
value of 5.4/~m to values of 15 and 12 ~m in the growth rates per unit strain, dr/de, for these three
highly deformed region with cavities and in a mechanisms are given by the following expres-
region with no cavities about 1 mm away from the sions:
highly deformed region respectively. In the speci- (a) diffusion cavity growth in superplasticity
men tested at a strain rate of 1.3 x 1 0 - 2 S-1 in [55, 57]
region III, cavitation was observed near the frac-
ture tip, and the grain size in the cavitated region d__[r= ffa6D~b( O-- 2 v/r)
of the specimen was measured as 8.4/~m. de 5r2kTg (1)
Livesey and Ridley [52] studied cavitation in
superplastic Zn-22% A1 eutectoid alloys and con- where ff2 is the atomic volume, 6 is the grain
cluded that cavities are nucleated only after the boundary width, Dg b is the grain boundary diffu-
initial fine grain size has increased by concurrent
grain growth to a critical value of about 8 /.tm.
*It is important to note that in most of these studies, con-
These results were rationalized by noting that current gram growth was correlated with the true local strain
after high strains, when the grain size has along the gauge length.
57
10"2
I
I
I
I
' i between cavity shapes and the dominant cavity
growth mechanism was reported earlier by Ridley
et al. [65]. A possible cause for this discrepancy is
the effect of surface diffusion at elevated temper-
atures.
I Hancock [58] developed the power-law growth
mechanism for high temperature creep by modi-
10.3 [ l , , ,,,,,,I
10-1 1.0 10 10-2
fying the low temperature plasticity-induced
cavity growth model of McClintock [66]. Plastic-
r (lain)
ity-controlled cavity growth at low temperatures
Fig. 13. The variation in cavity growth rate with cavity leads to cavities that are elongated along the ten-
radius for a specimen tested at ~ 5 × 10 -5 s t. The theoreti-
cal curves are shown for the diffusion, superplastic diffusion
sile axis. Figure 14 is a schematic illustration for
and power-law growth mechanisms. the development of rounded cavities from
58
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