Acta Materialia 51 (2003) 4487–4495

www.actamat-journals.com

Enhanced growth of intermetallic phases in the Ni–Ti

system by current effects
J.E. Garay, U. Anselmi-Tamburini 1, Z.A. Munir ∗
Department of Chemical Engineering and Materials Science, University of California, One Shields Avenue, Davis,
CA 95616, USA

Received 13 December 2002; received in revised form 13 December 2002; accepted 9 May 2003

Abstract

The effect of direct current upon interfacial reactions in the Ni–Ti system was investigated. Isothermal diffusion
couple experiments were conducted under varying current densities to de-couple Joule heating from intrinsic effects
of the current flux. Current densities of up to 2546 A cm⫺2 were used in the temperature range of 625–850 °C. All
of the intermetallic compounds (NiTi, Ni3Ti and NiTi2) present in the equilibrium phase diagram were identified in
the product layer. In addition, β-Ti solid solutions formed in samples annealed above the α→β temperature, 765 °C.
The growth of all product layers was found to be parabolic and the applied current was found to significantly increase
the growth rate of the intermetallic layers. Using Wagner’s analysis the present results were compared to published
results on current-free diffusion couples. The intrinsic growth rate constant of the NiTi2 intermetallic was found to be
43 times higher under the influence of 2546 A cm⫺2 than that obtained without a current at 650 °C. The effective
activation energy for the formation of all phases was found to decrease with increasing current density. The effect was
strong for all phases but the decrease was most marked for Ni3Ti. In this case, the activation energy decreased from
292 kJ mol⫺1 under the influence of a current density of 1527 A cm⫺2 to 86 kJ mol⫺1 when the current density was
2036 A cm⫺2. The results are explained in terms of current induced changes in the growth mechanism arising from
changes in the concentration of point defects or their mobility.
 2003 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Electric current effects; Intermetallics; Growth rates; Titanium–nickel; Reactive diffusion

1. Introduction and consequently their synthesis by self-sustaining

With a few exceptions, the enthalpy of forma-
tion of most intermetallic phases is relatively low
∗
Corresponding author. Tel.: +1-530-7520554; fax: +1-
530-7528058.
E-mail address: zamunir@ucdavis.edu (Z.A. Munir).
1
Permanent address: Dipartimento di Chimica Fisica, Univ-
ersità di Pavia, V.le Taramelli, 16, 27100 Pavia, Italy.
combustion has been limited [1]. Activation by
thermal means (e.g., the preheating of the elemen-
tal reactants) and by electrical means (the impo-
sition of a field) has been utilized to overcome the
thermodynamic limitation [2]. In the former case,
the product is often multi-phase, containing sig-
nificant amounts of phases not intended by the
starting stoichiometry. The use of an electric field
(in reality a current) has been shown not only to

1359-6454/03/$30.00  2003 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/S1359-6454(03)00284-2
4488 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495

have a significant role in activating the process, but
also in influencing the nature of the product. In an
investigation on the synthesis of Ti3Al, it was
found that the rate of the reaction increased with
an increase in the applied field and that the nature
of the product changed with this increase. Ulti-
mately at a relatively high field, only the desired
Ti3Al phase was present [3]. Similar results were
obtained in the case of another intermetallic,
FeAl [4].
In these and other similar observations, the role
of the current was initially assumed to be thermal,
providing Joule heat to the reactants and product.
Modeling studies based on this assumption have
been made and the results show qualitative agree-
ments with the experimental observations [5–7].
However, non-thermal current effects on mass
transport through electromigration have been
known for decades and experimental observations
demonstrating such effects have been provided
[8,9]. In a recent investigation, we have shown that
the imposition of a DC current across interfaces
between Al and Au metal layers has a significant
effect on the growth rate of the intermetallic layers
and on the incubation time for the nucleation of
these product phases [10,11]. In these results, no
effect of the direction of the DC current on the
growth of the products was observed, implying that
electromigration is not the dominant effect of the
current.
In this paper, we investigate the effect of the
current on the phase formation kinetics of products
resulting from the interaction of Ti and Ni and we
compare our results with those reported earlier on
diffusion couples without a current [12].
The Ni–Ti system has received much attention
primarily for its commercially important intermet-
allic phase, NiTi. This material has relatively high
ductility and corrosion resistance in addition to dis-
playing the shape memory effect. Other alloys in
the system have received attention, including a
quasi-crystalline phase which can be formed near
the NiTi2 compound, and also because Ti-rich Ni–
Ti alloys can form metallic glasses [13]. Also of
interest is replacing Al with Ti in Ni-based superal-
loys, because Ti is believed to enhance the high
temperature strength [14].
There are three equilibrium intermetallic phases
in the Ni–Ti system (Fig. 1) Ni3Ti, NiTi and NiTi2.
Ni3Ti is a hexagonal close-packed superlattice and
NiTi2 has a complex face-centered cubic structure
with 96 atoms per unit cell (space group Fd3m)
[15,16]. The structure of the third equilibrium
phase NiTi is interesting in that it has a high and
low temperature crystal structures due to a mar-
tensitic-type transformation. This transformation
leads to a shape memory effect. The high tempera-
ture “austenitic” phase has a B2 (CsCl) structure
(space group Pm3m), while the low temperature
“martensite” has a more complex monoclinic
B19⬘-type structure (space group P21/m) [17].
2. Experimental procedure
A schematic of the apparatus we used in our
experimental investigation is shown in Fig. 2. It
consists of a vertical cylindrical vacuum chamber
housing two electrodes surrounded by a furnace.
The electrodes carry current to the sample and pro-
vide a small mechanical load to ensure good con-
tact between the reactants. The electrodes are mol-
ybdenum rods 28 mm in diameter with a terminal
part reduced to 5 mm diameter, allowing the exter-
nal DC power supply to produce a current density
up to 3310 A cm⫺2 through the sample. The fur-
nace consists of a cylindrical tungsten mesh 16.5
cm in diameter and 6.5 cm long powered by an
AC power supply. A 0.5-mm diameter type K
Fig. 1. Ni–Ti phase diagram.
 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495
Fig. 2. Schematic of experimental apparatus.
(chromel–alumel) thermocouple placed in contact
with both the sample and one electrode was used
to monitor temperature and provide feedback to the
PID furnace controller. The experiments were per-
formed under high vacuum (ⱕ5 × 10⫺7 Torr).
The samples consisted of three metallic layers
with an Ni foil sandwiched between two Ti foils.
The foils were circular in shape, 5 mm in diameter
and of 127 µm thick. All foils were reported to be
99.99% pure (ACI Alloys, San Jose, CA). The
three-layer assembly provides both a Ti–Ni and
Ni–Ti interface with respect to the direction of the
DC current, thus providing the opportunity to
investigate the influence of current direction on
interfacial reactions. In addition, molybdenum foils
were used as protection layers between the elec-
trodes and the sample ensemble. Prior to each
experiment, the foils were polished using 600 and
1200 grit SiC metallographic paper and cleaned
with acetone.
Experiments were conducted under varying time
(0.5–30 h), current density (0–2546 A cm⫺2), and
temperature (625–850 °C). At the end of each
experiment, the cooled samples were mounted in
conductive epoxy resin (Buehler Konductomet),
sectioned perpendicularly to the metal interfaces,
and prepared metallographically. The thickness of
each of the intermetallic layers was measured using
scanning electron microscopy (SEM). The compo-
4489
sition of the products in the reaction layer was
determined through electron microprobe analyses
(EPMA).
3. Results
In the experimental conditions we have investi-
gated, the interaction between Ni and Ti always
produced well-defined product layers that grew
parabolically. The composition of these layers cor-
responded to all the intermetallic phases present in
the phase diagram (Fig. 1). Samples which reacted
above 765 °C also contained a β-Ti solid solution
layer. An example of a product layer morphology
is shown by the SEM micrograph in Fig. 3. An
important observation concerning the formation of
these layers was that it was independent of the
direction of the current, i.e., identical layer growth
was observed on both interfaces. Fig. 4 shows a
typical trend in the growth of the individual phase
layers (NiTi2, NiTi, and Ni3Ti) and the total pro-
duct at 700 °C when the reaction was carried out
without an electric current. These results show a
parabolic growth for all three phases. Furthermore,
there is a clear indication that an incubation time
is required for the nucleation of these phases. With
two exceptions, these observations are in partial
agreement with the results of the only reported dif-
fusion couple study on Ti–Ni system [12]. The
exceptions relate to the incubation time and to the
kinetics of the growth of one of the phases. In the
Fig. 3. Back-scattered electron micrograph showing typical
product layers. Sample reacted at 650 °C for 8 h with current
density of 1527 A cm⫺2.
4490 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495
Fig. 4. Product layer thickness squared (⌬x)2 vs. time for
samples reacted at 700 °C with no current (0 A cm⫺2).
previous work by Bastin and Rieck [12], no incu-
bation period was observed and the growth of the
Ni3Ti phase was not parabolic as was the case for
the other two phases. With regards to the incu-
bation period, the difference between our work and
that reported by Bastin and Rieck [12] may be the
consequence of the sample preparation method
employed by these authors. They prepared their
diffusion couples by initially welding the reacting
layers, a circumstance that could produce some
degree of intermixing of the reactants at the inter-
face prior to the initiation of the diffusion experi-
ments.
With the application of a current, significant
changes in the reactivity between Ti and Ni were
observed. Fig. 5 shows the growth behavior of the
layers in the presence of a current density of 2036
Fig. 5. Product layer thickness squared (⌬x)2 vs. time for
samples reacted at 650 °C with current density of 2036 A cm⫺2.
A cm⫺2 at 650 °C. In contrast to the case where
the growth took place in the absence of a current,
Fig. 4, here no induction time in layer growth is
apparent. A more significant difference, however,
is the marked increase in growth rate. In the
absence of a current and at a higher temperature
(700 °C) no product was observed after 5 h of
annealing, within the limits of resolution of our
measurements (0.1 µm). In contrast, at 650 °C, the
total product layer was about 9.5 µm thick after 5
h of annealing. The dramatic effect of the current
is shown more explicitly in Fig. 6. This shows the
effect of the current density on the thickness of the
NiTi layer resulting from reacting the system for
4 h at 650 °C. As the current density is increased
from 1018 to 2546 A cm⫺2 the thickness of the
NiTi layer increased by nearly a factor of seven
under the same conditions. Qualitatively similar
results were obtained for the other intermetallic
phases at this and other temperatures. However,
although the current had an effect on the growth
of the layers in all conditions, the effect was more
pronounced at lower temperatures.
In the work of Bastin and Rieck [12,18],
incremental product formation was investigated by
using two compounds as reactants to obtain kinetic
data on the formation of an intermediate phase.
Although we used Ti and Ni as starting reactants,
our results can provide similar kinetic information
using the recent analysis of Buscaglia and
Anselmi-Tamburini [19] based on the derivations
of Wagner [20]. This analysis is based on the
Fig. 6. NiTi layer thickness (⌬x) vs. current density for
samples reacted at 650 °C for 4 h.
 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495
assumptions that: the growth of all phases is para-
bolic, local equilibrium is established at each inter-
face, the phases have narrow homogeneity ranges,
and the extent of solubility in the terminal phases,
i.e., Ti and Ni, in this case, is limited. These
assumptions can be reasonably applied to the Ni–
Ti system in the temperature range of this investi-
gation. The homogeneity range of the phases NiTi
and NiTi2 below 750 °C is relatively small and the
fairly large solubility of Ti in Ni can be ignored
since the diffusivity of Ti in Ni is extremely slow
even at fairly high temperatures [18].
Using the nomenclature of Wagner, we calculate
the rate constant of the first kind, kI, from the
slopes of lines such as those shown in Fig. 7 which
is for the growth of the NiTi layer at 750 °C under
different current densities. Thus
(⌬x)2 ⫽ kIi t
where ⌬x is the thickness of the layer of the inter-
metallic and t is time. When only one phase forms,
then the constant is the true rate constant and is
referred to as the rate constant of the second kind,
kiII. The relationship between kiI and kiII has been
provided by Buscaglia and Anselmi-Tamburini as
冋冘
(ni⫺1⫺ni+1)Vi
i⫺1
Cj ni
kIIi ⫽ C2 n ⫹ (2)
(ni⫺1⫺ni)(ni⫺ni+1) i ij ⫽ 1VjCi Vi
冘 册
n
njCj
⫹ i ⫽ 1,…,n
V C
j ⫽ i⫹1 j i
Fig. 7. NiTi layer thickness squared (⌬x)2 vs. time for experi-
ments reacted at 650 °C for different current densities.
4491
where Ci = √kIi, Vi the molar volumes, and ni the
stoichiometric coefficients of each phase nor-
malized to 1 mol of component B, AniB. Values of
kiII represent the intrinsic property of each phase,
depending only on the interdiffusion coefficient
and the free energy of formation of that phase.
The intrinsic rate constants obtained through this
method for all the experiments performed at tem-
peratures (650–750 °C) below the α→β transition
temperature for Ti are reported together with the
first kind constants in Table 1. It should be noted
that no data are reported in this table for the highest
current density, 2456 A cm⫺2, at 750 °C. Under
these conditions, the growth rate is so high that the
middle, Ni, layer of the starting material will be
completely consumed after a relatively short time.
When this occurs, the equilibrium conditions will
be different. Table 2 reports the first kind rate con-
(1)
stants for experiments performed at temperatures
(800–850 °C) above the α→β transition tempera-
ture for Ti. Intrinsic (second kind) rate constants
cannot be calculated for the higher temperatures,
since above 765 °C, the extensive solubility of Ni
in Ti to form β-Ti violates the assumption in the
derivation of this kinetic parameter, as indicated
above.
4. Discussion
From the calculations described above, we are
able to compare our results with those of Bastin
and Rieck [12,18]. The rate constant, kII, determ-
ined by these authors for the growth of the NiTi
phase at 700 °C (grown from the couple Ni3Ti and
NiTi2) is reported as 1.5 × 10⫺11 cm·s⫺1. Under
the same conditions (i.e., at 700 °C and without
using a current) but starting with the couple Ni and
Ti, we calculate a value for the intrinsic constant
of 2.43 × 10⫺11 cm·s⫺1. The agreement between
the two values is reasonable.
However, the imposition of a current during the
reaction shows a significant change in this con-
stant. Table 3 shows the ratios of the kII values
calculated in this work under various current den-
sities to those calculated by Bastin and Rieck (with
no current) at the temperatures indicated for the
phases NiTi and NiTi2. No comparison is made for
4492 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495

Table 1
Calculated growth rate constants for intermetallic phases in the Ni–Ti system. T below α→β transition of Ti

T (°C) Current density (A cm⫺2) Phase kI × 1012 (cm2 s⫺1) kII × 1012 (cm2 s⫺1)

650 1527 NiTi 1.89 8.02

NiTi2 0.25 2.21
Ni3Ti 1.32 3.64
2036 NiTi 6.98 34.0
NiTi2 0.62 7.48
Ni3Ti 12.90 28.90
2456 NiTi 27.80 117.00
NiTi2 2.60 26.70
Ni3Ti 21.10 56.40
700 1527 NiTi 9.02 38.80
NiTi2 0.63 7.52
Ni3Ti 8.59 21.70
2036 NiTi 14.50 62.00
NiTi2 1.28 13.80
Ni3Ti 14.00 36.40
2456 NiTi 58.10 208.00
NiTi2 4.61 44.90
Ni3Ti 21.42 58.00
750 1527 NiTi 23.00 90.90
NiTi2 1.75 18.60
Ni3Ti 12.00 34.80
2036 NiTi 34.30 140.00
NiTi2 3.42 33.10
Ni3Ti 19.90 56.70

Table 2
Table 3
Calculated growth rate constants for intermetallic phases in the
Ratios of intrinsic rate constant of this work (kII) with current
system Ni–Ti. T above α→β transition of Ti; current density
to values calculated from Bastin and Rieck, kIIBR, without cur-
= 1527 A cm⫺2
rent [12]

T (°C) Phase kI × 1012 (cm2 s⫺1)

Phase T (°C) Current density kII/kIIBR
(A cm⫺2)
800 NiTi 34.40
NiTi2 4.36
NiTi 650 1527 2.7
Ni3Ti 19.50
2036 11.3
850 NiTi 121.00
2546 39.0
NiTi2 21.70
700 1527 2.6
Ni3Ti 23.50
2036 4.1
2546 14.2
750 1527 1.8
the Ni3Ti since in the work of Bastin and Rieck, 2036 2.8
NiTi2 650 1527 3.6
the growth of this phase was not parabolic. Table 2036 12.2
1 shows a considerable increase in the rate constant 2546 43.7
as a result of the application of a current. The 700 1527 2.2
increase depends on the magnitude of the current 2036 4.0
density in all cases, but is most pronounced at the 2546 13.2
750 1527 2.1
lowest temperature, 650 °C. At this temperature, 2036 3.7
the ratio of the rate constant for NiTi increases
 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495 4493

from 2.675 to 39.028 as the current density is

increased from 1527 to 2546 A cm⫺2. An approxi-
mately similar increase was observed for the NiTi2
phase at this temperature. Due to the high reac-
tivity at higher temperatures, no data were obtained
for the highest current density, 2546 A cm⫺2 for
both intermetallics. The effect of current density
on the rate constant, kII, for all three intermetallic
phases at 650 °C is shown in Fig. 8.
The observed effect of the current on the rate of
growth is now examined in terms of its effect on
the activation energy. Fig. 9(a)–(c) is Arrhenius
plots of the intrinsic constants for the intermetallic
phases NiTi, Ni3Ti, and NiTi2, respectively. In
each case plots for different current densities are
shown. For the cases of NiTi and NiTi2, the cur-
rent-free data of Bastin and Rieck [12] are also
plotted. The figures show a significant reduction in
the activation energy with an increase in current
density for all phases, although the dependence on
current density appears to be different for each
phase, with the largest decrease being observed in
the Ni3Ti case. The calculated values of the acti-
vation energy for different current densities and
temperature ranges are also reported in Table 4. It
should be noted that in the investigation on the
Au–Al system, the current had no apparent effect
on the activation energy.
As indicated above, the degree of influence of
the current on the activation energy depends on the
phase produced. Examining the ratio of the acti-
vation energy at the lowest and intermediate cur-

Fig. 9. (a) Temperature dependence of NiTi intrinsic growth

rate constant for samples reacted with current densities of 1527
and 2036 A cm⫺2. The results of Bastin and Rieck [12] with
no applied current (0 A cm⫺2) are plotted for comparison. (b)
Temperature dependence of Ni3Ti intrinsic growth rate constant
for samples reacted with current densities of 1527 and 2036 A
cm⫺2. (c) Temperature dependence of NiTi2 intrinsic growth
rate constant for samples reacted with current densities of 1527
and 2036 A cm⫺2. The results of Bastin and Rieck [12] with
no applied current (0 A cm⫺2) are plotted for comparison.
Fig. 8. Intrinsic growth rate constants (kII) vs. current density
for sample reacted at 650 °C.
4494 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495
Table 4
Effect of current density on activation energy for phase growth
in the system Ni–Ti. values for zero current density from Bastin
and Rieck [12]
Phase Current Activation energy (kJ mol⫺1)
density
(A cm⫺2)
NiTi 0 363.1 [12]
1527 313.9
2036 181.4
NiTi2 0 346.4 [12]
1527 275.1
2036 190.9
Ni3Ti 0 n/a
1527 292.7
2036 86.4
rent densities (with those with no current) provides
the values 0.30, 0.58, and 0.69 for the phases
Ni3Ti, NiTi, and NiTi2, respectively. The obvious
correlation is with the nickel content of the phase:
the current being more effective in the formation
of the phase with the highest Ni content. In view
of the fact that the diffusivity of Ni in Ti is higher
than that of Ti in Ni [18], we would propose that
the current has a greater effect on the diffusion of
Ni in the intermetallic. However, the absence of
diffusion data of Ni in these intermetallics makes
it impossible to ascertain the validity of this pro-
posal.
As indicated above with reference to Fig. 3, the
growth of all layers was symmetric with respect to
the direction of the DC current. This observation
is taken as an indication that electromigration is
not the dominant effect of the current. Similar
results were reported for the Au–Al system
[10,11]. In addition to electromigration (electron
wind effect), the current can possibly play other
roles and other explanations have also been offered
for the observation of current direction indepen-
dence. It was proposed in one study that the current
enhances the nucleation rate of the new phases [8].
In our previous work, we observed a significant
effect on nucleation time in the system Au–Al [11]
in which layer growth was also independent of cur-
rent direction. In the previous study, however, a
nucleation time was observed even under the high-
est current density employed. In contrast, in this
study, the imposition of a current reduced the incu-
bation time to zero (compare Fig. 4 with Fig. 5).
However, since the growth of the layers is consist-
ent with bulk diffusion, the effect of the current on
nucleation is likely governed by diffusion also as
has been pointed out by Thompson [21].
Thus in the absence of a clear electromigration
effect, the role of the current in enhancing dif-
fusion may relate to changes in defect concen-
tration or their mobility. In a recent positron
annihilation spectroscopy investigation by Asoka-
Kumar et al. [22], it was found that the imposition
of a current increased the concentration of vacanc-
ies in metals. The observed enhancement of the
growth of the intermetallics by the current may,
therefore, relate to an increase in the defect con-
centration in these phases or on their mobility. No
information on the effect of the current on defect
mobility is at hand, but on-going investigations are
aimed at determining this possible effect.
Another important aspect of the diffusion study
in the Ni–Ti system is the role of the Ti phase
transformation on the observed reactivity. Bastin
and Rieck [12] reported that the transition of Ti
from α to β produces a considerable decrease in
intermetallic layer growth rate due to the higher
solubility of Ni in β-Ti. The transition between the
two forms occurs at 765 °C, a temperature corre-
sponding to the Ti-rich eutectoid shown in Fig. 1.
Fig. 10 shows the temperature dependence of the
Fig. 10. Temperature dependence of NiTi growth rate con-
stant showing effect of β-Ti phase transformation, for samples
reacted with a current density of 1527 A cm⫺2. The results of
Bastin and Rieck [12] with no applied current (0 A cm⫺2) are
plotted for comparison.
 J.E. Garay et al. / Acta Materialia 51 (2003) 4487–4495
experimental growth constant for the NiTi phase
from the results of Bastin and Rieck and from
those obtained in this study when a current density
of 1527 A cm⫺2 was employed. In both cases, a
discontinuity is observed in a temperature range
very close to the transformation temperature (1 / T
= 9.63 × 10⫺4). In addition to confirming the effect
of phase transformation on the kinetics, this obser-
vation is also a validation of the temperature
measurements in our system.
5. Conclusion
The imposition of a DC current was found to
increase the reactivity of the Ni–Ti system. In iso-
thermal diffusion couple experiments, the current
pronouncedly increased the growth rate and
decreased the effective activation energy for
growth of all three intermetallic phases (Ni3Ti,
NiTi and NiTi2). The effect increases with an
increase in the magnitude of the current density in
all cases at all temperatures in the study, but is
most marked at the lowest temperature, 650 °C.
The effect on growth rate was strongest for the
NiTi2 compound, whose intrinsic growth rate con-
stant was 43 times higher under the influence of
2546 A cm⫺2 compared with no current diffusion
couple experiments at the same temperature of 650
°C. The effect was nearly as strong (39 times
higher) for the NiTi phase. By contrast, the applied
current decreased the effective activation energy
most dramatically in the Ni3Ti case falling from
292 kJ mol⫺1 under the influence of 1527 A cm⫺2
to 86 kJ mol⫺1 for 2036 A cm⫺2. It is suggested
that the application of the current increases the
mobility of defects or increases their concentration
over the thermal equilibrium value, thereby
increasing the product growth rate. Studies are
underway to determine the validity of these
proposed explanations using electrical resistivity
4495
measurements and positron annihilation
spectroscopy.
Acknowledgments
The financial support of this work by the
National Science Foundation is gratefully
acknowledged.
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