Materials Science and Engineering, A l l 9 (1989) 145-151
Effects of Parent Phase Aging on the Martensitic Transformation in a
CuZnA! Alloy
Z.-G. WEI* and D. YANG
Department of Materials Engineering, Dalian University of Technology, Dalian (China)
(Received December 13, 1988)
Abstract
The kinetics of aging in the temperature range
from room temperature to 320 °C and the effects of
aging on the martensitic transformation tempera-
tures in a ternary CuZnAl alloy have been studied
in detail. The reversible variation in M s tempera-
ture--that is, the depression of M s after aging at
higher temperatures near Too, and the recovery of
M s with aging time at lower temperatures--is
ascribed to DQ~ ordering and reordering in which
the long-range order and short-range disorder
change with temperature and time. The activation
energies associated with the processes have been
determined and it has been found that quenched-
in vacancies influence the kinetics of the reordering
processes at lower temperatures in a significant
way, whereas the ordering at higher temperatures
shows little dependence on the concentration of
vacancies. From the Landau theory, the tempera-
ture dependence of the order parameter ~1has been
calculated and a good correlation has been found
between ~l and M~.
1. Introduction
Since the stabilities of the metastable parent/3
phase and the martensite phase are directly
related to the shape memory performance and
other properties of copper-based shape memory
alloys, considerable efforts have recently been
devoted to the study of the complex aging effects
in these alloys [1-6[. Among the previous studies,
the stabilization phenomena of the martensites
have received much more attention, whereas the
literature on the aging of the/3 phase is relatively
smaller. As a matter of fact, the aging of the
*Present address: Department of Mechanical Engineering,
China University of Mining and Technology, Xuzhou.
Jiangsu, China.
0921-5093/89/$3.50
145
parent phase is particularly interesting because
the process involves ordering, which plays a very
important role in the subsequent martensitic
transformations. Generally speaking, in copper-
based memory alloys the metastable low temper-
ature /3 phase possesses either a B2 or D03
superlattice [3, 4, 7, 8]. The long-period stack-
ing order martensites (9R, 18R and others) are
derived from the ordered parent phase on
quenching. Many experimental results and theo-
retical analyses have demonstrated that the
characteristics of martensitic transformations and
other related properties are very sensitive to the
state of atomic order in the parent phase [3, 6,
9-18].
The as-quenched alloy with a subambient M~
temperature is in the fl phase state after solution
treatment and quenching. It has been widely
observed that aging at around room temperature
in the alloys results in an increase in M r tempera-
ture [2, 4, 5, 7]. The isothermal transformation
phenomena observed in CuA1Ni and CuZnAl
alloys are believed to be due to the increase in M~
temperature [19- 21 ]. Several investigations have
shown that the post-quench thermal history,
particularly short-time aging at intermediate
temperatures, can influence the martensitic trans-
ition temperatures [22-25]. Rapacioli et al. [23]
reported that in a CuZnAl alloy the martensitic
transformation temperatures were depressed by
about 25 °C after a flash anneal and quench from
300 °C; however, the transition temperatures
subsequently returned to their original values
after prolonged aging at room temperature. Using
a Cu-25.0at.%Zn-8.8at.%Al alloy, Schofield and
Miodownik [24] investigated the aging effects in
the range 39-67 °C. By careful control of the
post-quench thermal history they found that M~
shifted upwards for about 20 °C after prolonged
aging, while M s was depressed up to 30 °C when
© Elsevier Sequoia/Printed in The Netherlands
146
the Ms-stabilized samples were heat treated in the
temperature range 100-200 °C. The variation in
M S during aging at these temperatures was con-
firmed to be reversible. In an early study in a
C u - 2 6 Z n - 4 A I alloy, Cook and Brown [25]
obtained similar conclusions.
The decay of the excess quenched-in vacancies
during aging and the reversible variation of M S
suggest that it is impossible for a clustering reac-
tion, either of vacancies or of some atom species,
to act as the origin for the Ms changes. Most
investigators believe that the aging process is in
essence an ordering reaction. Changes of long-
range order [2, 4, 6, 25] and short-range disorder
in an ordered matrix [22, 24] and transitions
between different ordered structures, e.g. the
B 2 # D 0 3 transition [2, 7, 24], have been tenta-
tively suggested as possible factors which may
result in the reversible variation of M S tempera-
ture.
In this paper the effects of parent aging on the
M Stemperature and the influence of quenched-in
vacancies have been investigated in more detail.
The experimental results are examined and the
mechanism of the aging effects is discussed
in terms of long-range order and short-range
disorder.
2. Experimental details
The alloy used was prepared by melting
99.99% metals in a graphite crucible in an induc-
tion furnace. The ingot was hot rolled to wires
1.0 mm in diameter. The composition of the
alloy was 24.3 at.% Zn, 9.0 at.% A1 with copper
making up the balance. The electron concentra-
tion of the alloy was estimated to be about 1.42.
For the as-quenched samples after solution treat-
ment, the start temperature of martensitic trans-
formation M~ was determined to be 5 °C. All of
the samples used were held at 850 °C for 5 min
and then oil quenched. The as-received samples
were subjected to different thermal treatments,
followed immediately by measurement of the
electrical resistivity and determination of the
transformation temperatures.
3. Results
Figure 1 shows the variation of M S as a
function of temperature when the as-quenched
samples were held isothermally at temperatures
ranging from room temperature to 100 °C. In this
temperature range, M S shifts upwards at different
rates by up to about 18 °C. This is in very good
agreement with results obtained previously [23-
25]. It is seen that with prolonged aging duration
M~ increases gradually and then reaches a stable
value. The initial rate of increase becomes faster
while the stable M~ value reached is lowered
as the aging temperature increases. The aging
process at around 85 °C is interesting. M s is seen
to increase to a peak value, then to decrease
and finally to attain its stable value. This peculiar
behaviour of the M S temperature becomes more
visible at 100 °C. In Fig. 2 the variation in M s vs.
aging temperature at different times is shown.
Apparently the stabilized M S value obtained
during aging at a lower temperature is higher than
that at a higher temperature, though the rate of
change of the former process is a few orders of
magnitude lower than that of the latter. Accord-
ing to an Arrhenius-type equation, the thermal
activation energy associated with the process
of M S increasing is estimated to be 0.54 eV
(51.8 kJ mol- 1).
Figure 3 shows the aging at temperatures from
100 to 300 °C. An initial steep decrease in M s
22
~o / ~ - . . . . " ~oo~-
6
2 I I I L I I I
20 4O 60
Ageing Time (rain.)
Fig. 1. Variation of M s in as-quenched samples during aging
at temperatures below 100 °C.
22
18
10
2 I I I- 1
0 25 50 75 100
Ageing Temperature ('C)
Fig. 2. Variation of M~ vs. aging temperature (below 100 °C)
at different aging times.
 147

10
21 45t
140°C c
o -,,~,,,,,~
. JOf'C ,
u15
v
-20 , .. 8\ ~o'c
2C0~ 9
-35 l ~l
8°C
240"C
-50 / •" 1 " I - too'c
J I I I I I I -3 ,~'q"- i t r I I J
0 30 60 9O 0 30 60 90 120 150 180 210
Ageing Time (see.) Ageing Time (rain,)
Fig. 3. Depression of M s vs. aging time at various tempera- Fig. 4. Variation of M, at lower temperatures for alloy
tures above 100 °C. samples reheated to 160 °C for 30 s and then requenched.

occurs after aging at a particular temperature and

quenching. It can be seen that with increasing
temperature the initial rate of decrease becomes
larger and a greater M~ depression is reached.
The activation energy for the depression process
is calculated as 0.32 eV (30.5 kJ mol-1). This is
also in good accordance with the result (0.30 eV)
obtained from calorimetric data by Planes
et al. [26].
The depression of M s temperature can be
recovered by subsequent aging at lower tem-
peratures. As shown in Fig. 4, M Sis depressed to
about - 5 °C after aging at 160 °C for 30 s; how-
ever, the recovery of the original stable M Svalues
at temperatures below 100 °C occurs during this
period. The activation energy for the M~ recovery
is estimated to be 0.80 eV (76.6 kJ mol- ~), which
is a little larger than that for the as-quenched
samples (0.54 eV). The difference between the
processes for the two kinds of samples as shown
in Fig. 1 and Fig. 4 respectively is attributed to
the larger concentration of frozen-in vacancies
and residual stress in the as-quenched samples. It
is well known that the thermal diffusion process
during aging is assisted or governed by the
quenched-in vacancies. Whenever a defect is
introduced into the crystal lattice, the atoms in its
near neighbourhood rearrange themselves into a
configuration of minimum energy.
In order to examine the influence of quenched-
in vacancies on the aging process, the as-quench-
ed samples were held in boiling water for 30 min
to anneal out the frozen-in vacancies. Subse-
quently the samples were reheated to tempera-
tures between 100 and 320 °C and then quenched
and held isothermally at temperatures below
100 °C. It is found that the kinetics of aging at the
higher temperatures is affected by the vacancies
to a lesser extent. However, the M s recovery pro-
21
025__
9 _.-"~'7"--- 80'c
,'~$7,~'---• • ~oo°c
3 o// 18°C
-3 -- l I i I I ,. e
0 30 60 90 120 150 180 210
Ageing Time (rain.)
Fig. 5. Variation of M~ at lower temperatures for alloy
samples annealed at 100 °C for 30 min and then reheated to
160 °C and quenched.
cesses at the lower aging temperatures are found
to be influenced pronouncedly by the vacancies,
as shown in Fig. 5. It is seen that the recovery
rates in the samples annealed out of quenched-in
vacancies are much smaller and the stable M s
values attained at the various temperatures are
also a little lower by comparing Fig. 5 with Fig. 4.
In this case the activation energy for the recovery
process is determined to be 1.58 eV (151.6 kJ
mol-l), which is double that of the as-quenched
samples. The preceding results clearly indicate
that although the quenched-in vacancies do have
an effect on the aging process, particularly in the
lower temperature range, they are not by any
means the predominant factor responsible for the
changes of Ms temperature. As we will discuss
later, the aging in the temperature range of inter-
est is mainly due to ordering and reordering of
the parent phase, though the diffusion and the
rate of change in atomic order do depend par-
tially on the vacancy concentration and vacancy
mobility.
The overall variation tendency of M~ tempera-
ture during aging in the temperature range
studied is illustrated schematically in Fig. 6.
i48
Figure 7 shows the stable M s value as a function
of aging temperature. In the present work the
variation of M s temperature in the temperature
range studied is also confirmed to be reversible;
in other words, the depression in M s during aging
at higher temperatures and the recovery of stable
Ms at lower temperatures can be repeated. It is
noteworthy that besides Ms, other martensitic
transformation temperatures such as A s, A f and
Mf behave in a similar way as M s does during the
aging processes described above.
4. Discussion
The complicated changes of M s temperature
during aging at some temperatures--that is, the
initial increase and then slight decrease in M s at
temperatures in the range 70-120 °C--imply that
the aging is not a simple process but may involve
several phenomena. Measurements of the elastic
properties during short-time aging in the fl phase
revealed that there exist at least two components
[27, 28]. One is the process in which M s increases
(while the shear elastic constant C' decreases)
~ - - -
tem~~ - increasincj
~ ' ~ - -
1 I I I I I
1 2
Ageing Time (,~btt~-~ u~,)
Fig. 6. Schematic diagram illustrating the overal! variation
tendency of M~ during aging in th.e temperature range of
interest.
30
10
.w
v
-10
-3°
-50
I
20
I I
60 100 1/,0 180 220
1 I
Ageing Temperature ('C)
Fig. 7. The stable M~ attained during aging at temperatures
ranging from room temperature to 320 °C.
and the other is the process in which M s de-
creases (while C' increases). A resistivity study
made in fl-CuZn alloys also concluded that the
residual resistivity after quenching and aging
consists of two components [29]. It can be tenta-
tively suggested that the aging process mainly
involves changes in long-range order and short-
range disorder, which are temperature depen-
dent. As we will see in the following, whenever
the alloy samples are held at a higher temperature
near the critical temperature for order-disorder
transition, a lower long-range order and a greater
concentration of wrong atom pairs are produced
and retained after quenching. At lower tempera-
tures the corresponding order values (degrees)
are greater and the decay of the retained dis-
ordered atom pairs proceeds during the aging.
The aging processes at transient temperatures
can be thought of as a combination of the two
components.
It is useful to separate the B2 and D 0 3 ordering
in the alloy. Within the composition range of the
alloy used in the present work, both the B2 and
D 0 3 superlattice may be contained in the parent
phase. Transmission electron microscopy (TEM)
observations [7, 8, 30] have confirmed this point.
__ --
The CuZnA1 alloy exhibits two ordering pro-
cesses, i.e.b.c.c.--'B2 and B2--,D03, prior to the
martensitic transformation. It is widely accepted
that the former cannot be depressed by rapid
quenching while the latter can be partially sup-
pressed. In the low temperature range, D 0 3
ordering must take some time to accomplish and
reach its equilibrium state. It is very difficult to
exclude the possibility that the B2 ~ D 0 3 transi-
I I
3 tion occurs during aging in the as-quenched
samples. However, when the alloy samples are
kept at lower temperatures for enough long times
so that the B2 superstructure transforms com-
pletely into the D 0 3 structure, it is proved in the
present study that the reversible variation in M s
temperature can still be observed during the sub-
sequent aging at temperatures from M s to To%
(the critical transition temperature). This fact
strongly suggests that the reversible variation of
M~ cannot be ascribed to the B2 ordering or the
B2 ~ D 0 3 transition.
o o o The critical temperature for B2~D03, say
Too,, can be calculated by Inden's method [31]
I I
260
I
300
and a few investigators have determined the criti-
cal temperatures for CuZnAI alloys [8, 24, 32].
TD% for the CuZnAI alloy used in this work is
estimated to be 260 °C (533 K) and its b.c.c.-B2
 149

transition temperature TB2 is about 500°C If this condition is not satisfied, a relaxation
(773 K) [32]. Electrical resistivity and differential process occurs in which ~ varies with time and
scanning calorimetry (DSC) experimental results tends to the equilibrium value of the order
suggest that TD0~for alloys of similar composition parameter
to that used in this work is about 240-280 °C [8,
33]. In addition, for the different effects of B2 and
D 0 3 ordering on the phase stability, such as mar-
tensitic transformation temperatures [14-16, 22,
0 =
io 1 (3)

28], it is expected that the aging temperature which can be rewritten as

dependence of M~ should show some noticeable
T c - T=fl~l 2 (4)
change in tendency around TD0~.This is verified
in Fig. 7 where the peculiar behaviour of the where r = 2b/a. For the alloy used, Tc= 533 K.
stable M~ above 250 °C does not arise from the Assume r~= 0 at T = T c and that r~ has its maxi-
formation of bainite or from the thermal decom- mum value/Tmaxat T= 273 K. The calculated r/as
position of the parent phase for the very short a function of temperature (T/Tc) is shown in Fig.
holding time (a few seconds only). Thus the aging 8. The temperature dependence of the corre-
at temperatures below 250 °C is mainly related to sponding stable Ms (AMs/AM, max) is shown in
the D03 ordering and reordering. Fig. 9. From Figs. 8 and 9 it is easy to see the
Minute changes in the order are believed to
produce substantial changes in the martensitic 1.o
transformation temperatures [4]. In the tempera-
ture range below Tr~0~the long-range order varies
-- C
continuously from zero to unity with decreasing
temperature. On the other hand, the changes in
order require thermally activated atomic re-
~ 0.5
arrangement and hence take a finite time. This r~
means that a change within the ordered phase
may produce a metastable situation. Conse-
quently, the transformation temperature varies
with the long-range order until the equilibrium
state is attained. It is established that the ternary o I I i 1
006 0.7 0.8 0.9 1.0
CuZnA1 alloy, in contrast to binary CuZn, FePt
T/T¢
and Some other fl phase alloys, shows an increase
in M s with increasing degree of D03 order [10, Fig. 8. Variation of calculated 0 as a function of aging
temperature (T/Tc), where T is absolute temperature. Calcu-
15, 22]. lation results for two CuZnAl alloys used in refs. 24 and 25
It is well known that the change in state of a are also presented. (A) Cu-24.3at.%Zn-9.0at.%Al alloy; (B)
body in a second-order phase transition is Cu-26Zn-4A1 alloy [25]; (C) Cu-25.0at.%Zn-8.8at.%Al
alloy [24].
described by the order parameter r/, which is zero
above the critical order-disorder transition tem- 1.o
perature 7~ and non-zero below Tc. In the Landau
theory the thermodynamic potential f2 near the
transition point can be expressed as [34]
\
if2 = ff20(T,/.t) + ( T - To)at/2 + b r / 4 + ... (1) iri-

where a and b are positive coefficients which are '0.5

temperature dependent and p is the chemical ,ca

\
potential. In a spatially homogeneous body the &

value of if2 is determined by the minimum of

the thermodynamic potential per unit volume
f2( T,/.t, r/) as a function of r/with given tempera-
ture T and chemical potential p: 0.6 0.7 0.8 0.9 1.0
T/Te
0f2
--=0 (2) Fig. 9. Variation of AMJAM~ maxwith aging temperature (T/Tc),
Or/ where AM~= M~( T) - M~(Tc) and AM~max=M,(RT ) - M~( T~).
150
good correlation between r/ and M s. From a
modified phenomenological model and by
comparison with experimental results, Vinals
and coworkers [14, 15] found that the ternary
CuZnA1 alloys have
Ms(S2) = -AS22 + BS 2 - C (5)
where A, B and C are positive constants which
depend on the material; the parameter $2 and
another one S 1 are defined by Murakami et al.
[35] to describe the state of long-range order.
Although the order parameters are defined in a
different way, their results are consistent with
ours as shown in Figs. 8 and 9.
Owing to the difficulty in directly measuring
the long-range order, there are few experimental
data on order for copper-based memory alloys.
Several investigations made on martensite have
shown that a few per cent change in the degree of
order occurs during aging [36, 37]. Transmission
electron microscopy (TEM) observations have
indicated that the change in size of antiphase
domains depends on the quenching rate and tem-
perature [8, 17, 23]. The growth of antiphase
domains during aging after flash heating [23]
suggests an increase in the degree of D 0 3 order.
The main mechanism of ordering at these tem-
peratures is the growth of antiphase domains. As
the temperature is lowered, the degree of order
within the antiphase domains increases.
In the aforegoing discussion the contribution
of the short-range disorder is neglected. How-
ever, since the aging process, particularly the
complex changes of M s in the range 70-120 °C as
mentioned above, cannot be interpreted in a
satisfactory way by the change in long-range
order, it is necessary to take into account the
short-range disordered atom pairs which were
suggested to have significant effects on the mar-
tensitic transformations, especially in CuZnA1
alloys [22, 29].
It is well established that below the critical
temperature of the order-disorder transition
there exists a small amount of disorder in the
long-range-ordered matrix. The disordered atom
pairs which are obtained by interchanging the
corresponding right atom pairs are also tem-
perature dependent. The formation energy for
the wrong atom pairs decreases when the temper-
ature approaches the critical transition tem-
perature, and the decrease leads to a strong
increase in the number of disordered pairs. The
disordered atom pairs are produced in thermal
equilibrium and are retained after the subsequent
quenching to lower temperatures. In binary CuZn
alloys only the nearest-neighbour (n.n.) atom
pairs have to be considered, while in ternary
CuZnA1 alloys mainly next-nearest-neighbour
(n.n.n.) disordered C u - Z n pairs contribute to the
change in M s [22]. The concentration of the dis-
ordered atom pairs is given by
~1AB
(i) = r/(Ai~(0)exp { -Ef~A'B)} (6)
KBT
where r/~(0) is the concentration of possible
pair sites for n.n. (i=1) or n.n.n. (i=2) inter-
changes of atoms A and B. Eft(A, B) is the corre-
sponding formation energy in the fl phase. In the
CuZnAI alloy the formation energy of CuZn
wrong atom pairs was estimated to be 0.15 eV
(18x103k) and the concentration at around
200 °C is of the order of 10 -3 [22]. The presence
of the disordered atom pairs increases the energy
of the martensite with respect to the/3 phase and
thus lowers M s, while the decay of the retained
pairs would increase M s.
5. Conclusions
A reversible variation in M s has been observed
during aging in the temperature range from M s
(as-quenched) to TD% in as-quenched samples
and in samples heat treated at moderate tempera-
tures. The thermal activation energy associated
with the ordering at higher temperature is deter-
mined to be 0.32 eV and the ordering is found to
be less dependent on the quenched-in vacancies.
The ordering causes M s to be lowered by up to
about 50 °C. The recovery of M s during the re-
ordering at lower temperatures is affected by the
vacancies in a significant way. The activation
energy for the recovery process in as-quenched
samples is 0.54 eV whereas the energy is more
than doubled in the annealed samples without
quenched-in vacancies. The reordering increases
Ms by up to about 18 °C.
Experimental results and theoretical analyses
suggest that the reversible variation in M s can be
mainly attributed to changes in the temperature-
dependent long-range order and short-range dis-
order in the D 0 3 ordered matrix. The contri-
bution of the disordered atom pairs is interpreted
following Rapacioli and Ahlers [22]. On the basis
of the Landau theory, the equilibrium order par-

ameter r/has been calculated and a good correla-
tion has been found between ~/and M s.
Acknowledgments
The authors wish to acknowledge Professor
N. F. Kennon and Professor L. Delaey for their
provision of some valuable references. The
authors have discussed the experimental results
with Professor T. Y. Hsu, Shanghai Jiao Tong
University; his kind advice and stimulation are
appreciated.
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