JMEPEG (2014) 23:255–261 ASM International

DOI: 10.1007/s11665-013-0759-9 1059-9495/$19.00

Structure-Property Relationship of Cu-Al-Ni-Fe Shape

Memory Alloys in Different Quenching Media
Safaa N. Saud, E. Hamzah, T. Abubakar, and S. Farahany

(Submitted July 21, 2013; in revised form September 3, 2013; published online October 25, 2013)

This paper presents the effects of heat treatments using various quenching media on the phase transfor-
mation parameters and microstructure parameters. The effects of different quenching methods, step-
quenched and up-quenched, in various media were evaluated by using differential scanning calorimetry,
field emission electron microscopy, energy-dispersive spectrometry, atomic force microscopy, x-ray dif-
fraction, and Vickers hardness. The variations of the structure and properties of Cu-Al-Ni-Fe shape
memory alloys were linked to the variations of morphology, type, and stabilization of the obtained phase.
From the DSC results, the use of ice water as a quenching medium produced the highest transformation
temperatures, while a brine solution-quenching medium resulted in the highest change of the entropy and
enthalpy. Additionally, it was found that the best grain refinement was observed through the use of an oil-
quenching medium, due to its high cooling rate.

on the MT characteristics (Ref 9). For instance, at a high

Keywords Cu-Al-Ni-Fe, quenching media, shape memory alloys,
thermal treatment, transformation temperature
1. Introduction
Shape memory alloys (SMAs) are an intelligent group of
shape memory materials, which are often capable of recovering
their original shape by increasing the applied temperature (Ref
1). These kinds of alloys are being used for various engineering
applications attributable to their unique thermo-mechanical
response. SMAs are able to transform between a high
temperature phase typically called austenite and a low temper-
ature phase typically called martensite, a phenomenon which is
termed reversible martensitic transformation (MT) (Ref 2, 3).
The most significant aspect of the difference of the unique
thermo-mechanical properties such as the superelastic (SE),
pseudoelastic, one-way, and two-way shape memory effect is
the martensite phase transformation (Ref 4, 5). Among the
different types of alloys which are able to possess shape
memory properties, Cu-based SMAs have given effective
consideration because of their large superelastic window, their
wide range of transformation temperatures, their high damping
properties, and their low cost. Furthermore, it was declared that
the Cu-Al-Ni SMAs have the ability to transform into several
types of phase transformation (b, b01 ; c01 ; and a), depending on
the alloying composition, applied stress, and thermal treatment
(Ref 2, 6-8). The b phase of Cu-Al-Ni SMAs has less stability
at room temperature and is able to retain a metastable phase
when thermal treatments are applied. Moreover, it has been
observed that thermal treatments can obtain a significant effect
temperature, the b phase has a bcc disorder structure and the
corresponding stability decreases with an increasing application
of temperature, while at a low temperature, the b phase can be
retained in a metastable phase by choosing the lowest cooling
rate medium such as air cooling (Ref 10-12). From another
point of view, the thermodynamic parameters are very sensitive
to the thermo-mechanical system of the MT in the Cu-Al-Ni
SMAs. Usually, an improvement of the transformation temper-
ature can lead to the type of quenching media (Ref 13, 14). In
this study, for the optimization of Cu-Al-Ni-Fe SMAs and the
improvement of their hardness, heat treatment was applied with
different quenching media, which is known as the most
effective way for improvement. This paper focuses on the
effects of thermal treatment and quenching media on the
structure and properties of the Cu-Al-Ni-Fe SMA.
2. Experimental Details
The Cu-Al-Ni-Fe SMAs were prepared by melting the pure
elements in an induction furnace and then pouring into a mild steel
mold with a rectangular ingot shape. The composition of this alloy
was Cu-11.5 wt.% Al-4 wt.% Ni-0.25 wt.% Fe SMA, which has
been investigated via inductively coupled plasma mass spectrom-
etry (ICP-MS). The samples were cut from the ingot to their final
dimensions (10 mm 9 10 mm 9 2 mm) by using EDM wire
cutting. Before applying the heat treatment conditions and
quenching media, the samples were homogenized at 900 C for
30 min, and then quenched in water. The cut samples were divided
into six groups, as shown in Fig. 1. The samples were given the
following heat treatment and quenching media:

Safaa N. Saud, E. Hamzah, T. Abubakar, and S. Farahany, Faculty

a. Heated up to 900 C for 30 min, then step-quenched in a
of Mechanical Engineering, Universiti Teknologi Malaysia, 81310 solution of water and 10% NaOH (5 C);
UTM Johor Bahru, Johor, Malaysia. Contact e-mails: safaaengineer@ b. heated up to 900 C for 30 min, then step-quenched in
gmail.com and esah@mail.fkm.utm.my. ice water at 0 C;

Journal of Materials Engineering and Performance Volume 23(1) January 2014—255

Fig. 1 Schematic diagram of various heat treatments and quenching media for different Cu-Al-Ni-Fe SMAs: (a) solution of 10% NaOH and
water bath, (b) ice water bath, (c) brine solution bath, (d) oil bath, (e) water up-quenched bath, and (f) oil up-quenched bath

c. heated up to 900 C for 30 min, then step-quenched in

brine solution (salt and water) at 20 C;
d. heated up to 900 C for 30 min, then step-quenched in
an oil bath at room temperature;
e. heated up to 900 C for 30 min, then quenched in ice
water after being up-quenched in a water bath at 100 C
for 10 min, (900 fi 100 fi 0 C);
f. heated up to 900 C for 30 min, then quenched in ice
water after being up-quenched in an oil bath at 200 C
for 10 min, (900 fi 200 fi 0 C).

In order to measure the cooling rate of each quenching

medium, thermal analysis was carried out by joining a K-type
thermocouple with each sample and inserting it into the
furnace; all the samples were heated up to 900 C and
afterward cooled in different quenching media. The tempera-
ture-time data were recorded using the EPAD-TH8-K high-
speed data acquisition system connected to a computer with
DEWESoft 7.0.5 at a dynamic rate of 100 Hz/ch. For the Fig. 2 The cooling rate curves of different quenching media
purpose of plotting and smoothing the cooling curve of the
obtained data, FlexPro8.0.31 data analysis software was used
with the type of quenching media as shown in Fig. 2. It was
for determining the characteristic data.
subsequently revealed that the slowest cooling rate was
In order to examine the effects of quenching media on the
obtained with the solution of 10% NaOH and the water bath,
microstructures in terms of grain size and morphology, optical
even as the maximum cooling rate was acquired with the oil
microscopy and field emission electron microscopy were used.
bath. The curve values of the cooling rate were calculated either
The phase and crystal structure determinations were carried out
by dividing the variations of the quenching temperature by the
by x-ray diffraction using Cu Ka radiation with a locked couple
variations of the quenching time or by the slope of proportional
mode, a 2h range between 30 to 60, and a 0.05/s scanning
straight line, which is often more appropriate to reveal the
step. The initial and final transformation temperatures were
transformation rate of each quenching media, in other words,
determined using a differential scanning calorimeter (DSC).
which could refer to the elucidation of the diffusivity of the
The scanning was carried out at rate of 10 C/min in between
combined metal straight into their interfaces during the cooling
50 and 300 C. The quenched samples were ground and
process.
polished, then etched in solution containing 2.5 g ferric
The transformation characteristics of the Cu-Al-Ni-Fe SMA
chloride acid (FeCl3Æ6H2O) and 48 mL methanol in 10 mL
with various quenching media were investigated. The transfor-
HCl for 4 min (Ref 15-17). Vickers hardness test set with
mation start and finish temperatures were As (austenite start), Af
10 kg for 25 s was performed to measure the hardness of these
(austenite finish), Ms (martensite start), and Mf (martensite
alloys.
finish) during the heating and cooling processes. The martens-
itic phase inherited the atomic order of the b phase as a
displaced character of the MT. The endothermic peaks which
were observed during the heating process and the exothermic
3. Results and Discussion peak which was observed during the cooling process are
illustrated in Fig. 3.
The cooling rate was measured for the different quenching From the obtained results of DSC, it was observed that the
media. It was found that the cooling rates varied in accordance curves of the martensite austenite transformation changed

256—Volume 23(1) January 2014 Journal of Materials Engineering and Performance

Fig. 3 DSC curves of Cu-Al-Ni-Fe SMA with various quenching media: (a) heating and (b) cooling

Table 1 The transformation temperature parameters of Cu-Al-Ni-Fe SMA with different quenching media
Quenching media As, K Af, K Ms, K Mf, K Af-As, K Ms-Mf, K To, K

Oil bath 508.41 515.38 503.94 498.71 279.97 278.23 509.66

Brine bath 507.71 515.22 504 498.28 280.51 278.72 509.61
Solution of 10% NaOH and water 507.55 515.24 504.1 498.43 280.69 278.67 509.67
Ice water 509 515.76 504.30 491.5 278.76 285.75 509.485
Oil up-quenched bath 507.14 515.11 503.86 498.5 280.97 278.36 509.485
Water up-quenched bath 507.46 514.82 504.27 498.6 280.36 278.67 509.545

either in location or shape, depending on the values of the

transformation temperature and the value of the heat flow. All
these variations were mainly attributed to the type, morphology,
and stability of the obtained phase and were closely related to
the changes of the thermodynamic parameters, such as entropy
and enthalpy. The data of both transformations are tabulated in
Table 1. The transformation temperatures varied according to
the varying quenching media. It was found that the maximum
values of the transformation temperature were obtained during
the ice water bath. The range of the phase change temperature
varied with the different quenching media, and the tendency to
decrease or increase depended on the cooling rate of each
treatment.
As seen from the DSC results, the thermodynamic param-
eters were determined for the austenite and martensite trans-
formation, as tabulated in Table 2. It was found that the
enthalpy values of the forward transformation were greater than
the reverse transformation, which revealed that the required
heat for the forward transformation should be more than for the
reverse transformation. From the same point of view, the values
of enthalpy and entropy of the direct and reverse transforma-
tions were given the highest changes through the brine
solution-quenching bath for both transformations. The recorded
curves of the heating and cooling processes were integrated as a
function of temperature. The total area under the curve was
expressed as a value of enthalpy (DH), where the value of
entropy was equal to dividing the value of enthalpy changes by
the equilibrium temperature. The argumentation of Salzbnenner
and Cohen (Ref 18) was used to determine the value of the
equilibrium temperature To. The following equation was used to
express the equilibrium temperature (To) between the martens-
itic and austenitic phases:
1
To ¼ ðMs þ Af Þ ðEq 1Þ
2
In addition, To for the alloy, when the DGM!A ðTo Þ and
DGA!M ðTo Þ ¼ 0 at T = To, is expressed as (Ref 19)
DH M !A DH A!M
To ¼ or To ¼ ðEq 2Þ
DS M !A DS A!M
Figure 4 shows the field electron scanning electron micro-
graphs and energy-dispersive spectroscopy of the quenched
samples. These samples were heat treated at 900 C, followed
by quenching in oil, brine, NaOH solution, ice water, oil up-
quenched, and water up-quenched. These samples showed
plate- and needle-shaped martensite microstructures, but varied
in terms of orientation and size. However, the Energy-
Dispersive Spectroscopy results confirmed the exact composi-
tion of each phase of the XRD curves by confirming the
availability of iron content in the microstructures and its
participation in the obtained phases.
Figure 4(a) shows the self-accommodation of the martensite
formed in the oil-quenched sample. It was noticed that the
microstructure of martensite was of a self-accommodation
group (Ref 15) and the exhibited phase was b01 phase, where
these groups had nucleated and grown at several sites in a grain
(Ref 20). The boundaries of b01 grew in the matrix of the a
phase, and small needles were observed, which belonged to b¢
phase. Figure 4(b) also shows a similar phase transformation in
oil quenching, but the martensite needles were indistinct.
Moreover, the martensite plate groups were obtained in very
thin and sharp shapes. Figure 4(c) shows the presence of very

Journal of Materials Engineering and Performance Volume 23(1) January 2014—257

Table 2 Quenching media effect on the thermodynamic parameters of Cu-Al-Ni-Fe SMA
Quenching media DHM fi A, (J/g) DSM fi A, (J/kg k) DHA fi M, (J/g) DSA fi M, (J/kg k)

Oil bath 3.917 7.68552 5.917 11.6097

Brine bath 3.959 7.76869 5.244 10.29022
Solution of 10% NaOH and water bath 3.293 6.46104 4.275 8.38778
Ice water 3.022 5.93125 7.701 15.11467
Oil up-quenched bath 2.513 4.93243 3.049 5.98447
Water up-quenched bath 3.36 6.59412 4.094 8.03462

Fig. 4 Field emission scanning electron microscopy and energy-dispersive spectrometry of Cu-Al-Ni-Fe SMA homogenized samples after being
heat treated and quenched in (a) oil bath, (b) brine solution bath, (c) solution of 10% NaOH and water bath, (d) ice water bath, (e) oil up-quen-
ched bath, and (f) water up-quenched bath

thin martensite, which was identified as b¢ phase. The
morphology of the grain was very smooth, due to the type of
cooling rate. However, when the sample was quenched in ice
water, structures were produced of other quenching media, b¢
and b01 , with a monoclinic 18R structure accumulated in the a
matrix, as shown in Fig. 4(d). Furthermore, the b01 formed
regularly with uniform orientations, which the transformation
was completed. From the same point of view, the expected
phases for both oil up-quenched and water up-quenched
showed similar phase transformations as the other media, but
the shape of the b01 phase was thicker and longitudinally
oriented, as shown in Fig. 4(e) and (f).
Figure 5 shows the XRD patterns of Cu-Al-Ni-Fe SMA,
which were heat treated to 900 C and then quenched in different

258—Volume 23(1) January 2014 Journal of Materials Engineering and Performance

types of quenching media. The XRD patterns confirmed the initial
microstructural observation that the austenite transformed into b01 ,
b¢, and a phases after they had undergone various heat treatment
processes. Figure 5(a) shows the XRD pattern of sample (a),
which exhibited peaks corresponding to b01 and a phases, where
the a phase was indicated on two peaks (200) and (220), b01 was
indicated on two peaks (0018) and (311), and b¢ was indicated on
one peak (202). The XRD patterns of sample (b) showed similar
peaks to sample (a), as shown in Fig. 5(b). However, there was a
high increase in the intensity value for (220)a. Meanwhile, the
XRD patterns of the solution of 10% NaOH and the water sample
showed peaks corresponding to a and b01 phases with a
monoclinic 18R structure, where the indication had taken the
same peaks of other alloys, as shown in Fig. 5(c). The XRD
patterns of sample (d) showed two phases that indicated ( b01 , b¢)
in sample (d), as shown in the Fig. 5(d). The XRD patterns of
both oil up-quenched and water up-quenched showed almost
similar results with two phases of a and b01 indicated on the same
peaks. The difference between the two alloys was the peaks of the
oil up-quenched, which had more intensity than the water up-
quenched, as shown in the Fig. 5(e) and (f).
The indexed diffraction peaks showed that the Cu-Al-Ni-Fe
SMA under different thermal treatments had a monoclinic
structure in its martensite condition and the diffraction patterns
were indexed on the basis of the monoclinic structure (Ref 21,
22). So, according to the monoclinic unit cell roles, we calculated
the lattice parameters as given in Table 3 by using the following
equation (Ref 23):

Fig. 5 XRD patterns of Cu-Al-Ni-Fe SMA homogenized and heat treated followed by quenching in (a) oil bath, (b) brine solution bath, (c)
solution of 10% NaOH and water bath, (d) ice water bath, (e) oil up-quenched bath, and (f) water up-quenched bath

Journal of Materials Engineering and Performance Volume 23(1) January 2014—259

Table.3 Lattice parameters and the crystalline size of Cu-Al-N-Fe SMA with different quenching media
Lattice parameters

Quenching type a, Å b, Å c, Å Crystalline size, Å

Oil bath 4.5112 6.2232 37.9435 271

Brine solution bath 4.3538 6.2407 37.8498 300
Solution of 10% NaOH and water bath 4.0543 8.3796 37.9081 191
Ice water bath 4.1968 6.7646 37.8837 151
Oil up-quenched bath 4.0521 6.3613 37.8637 233
Water up-quenched bath 4.3525 6.2567 37.8566 215

Fig. 6 AFM 3D surface morphology of Cu-Al-Ni-Fe SMA with different quenching media: (a) oil bath, (b) brine solution bath, (c) solution of
10% NaOH and water bath, (d) ice water bath, (e) oil up-quenched bath, and (f) water up-quenched bath

   2  size produced the maximum value with a brine solution-

1 1 h2 k2 1 l 2hl cos b quenching bath, and then decreased to the minimum value
¼ þ 2þ 2þ  ; ðEq 3Þ
d 2 a2 sin2 b b c sin2 b acsin2 b with the ice water bath. All these changes were due to the
variation of phase transformation characteristics.
Using AFM, the grain refinement and surface morphology
where d is the space between the planes, (hkl) are Miller variations under the effect of different quenching media were
indexes, (a, b, and c) are the axis lengths, and b is an interaxial observed and tabulated, as shown in Fig. 6 and Table 4,
angle. To confirm the obtained structure, the a/b ratio pffiffiffi was respectively. It has been declared that the surface morphologies
calculated. It was found that this ratio was less than 3=2in of the Cu-Al-Ni-Fe SMAs are mainly dependent on the type
value of the order case, due to the variation of atomic sizes for and concept of the thermal treatment. The cooling rate is the
the 18R martensite. The changes in the peak characteristics of most effective parameter that can control grain refinement;
the XRD results were determined, as well as the observed therefore, grain size and roughness can be controlled. It was
variations of the peak locations of each treatment. As can be found that the 10% NaOH and a water solution bath obtained
seen from the XRD results, the crystalline sizes were measured, the largest grain size, which is attributed to the effect of the
as shown in Table 3. The crystalline sizes, which were formed cooling that had the slowest rate and allowed the grain growth
in the structure of Cu-Al-Ni-Fe SMAs via different thermal enough time; therefore, the grain size and roughness indicated
treatments, were determined using the following relation: the highest values, as can be seen in Table 4. From same point
0:9  ðkÞ of view, the grain size decreased along with the oil bath to
Crystalline size ðd Þ ¼ ; ðEq 4Þ 900 lm, due to the high cooling rate, which restricted the grain
B  cos h
growth. However, with increasing the cooling rate, the
where k is the wavelength, B is the full width at half maxi- nucleation under cooling increased. The phenomenon of an
mum, and h is the Braggs angle. It was found that crystalline increase in the nucleation temperature with an increase in the

260—Volume 23(1) January 2014 Journal of Materials Engineering and Performance

Table 4 The values of grain size, roughness, and hard-
ness corresponding to the types of quenching
Grain size, Roughness, Hardness,
Quenching media lm mm MPa
Oil bath 900 2.889 178
Brine solution bath 1200 4.76 160
Solution of water and 1700 7.987 165
10% NaOH bath
Ice water bath 1450 3.248 149
Oil up-quenched bath 1300 6.725 152
Water up-quenched bath 1350 3.225 154.5
solidification rate is mainly dependent on the mobility of the
clusters of atoms in the melt. The fluctuation clusters and
fluctuation embryos are attributed to the production of frozen
atoms, which are the nucleation primers. It has been declared
that with an increase in the cooling rate, the number of
nucleation primers increased, and the recalescence temperature
decreased. This effect has a significant effect on grain size. On
the other hand, the roughness reached a maximum value after
10% NaOH with a water bath, due to the presence of the b01
phase with a very high intensity. Therefore, it has been clarified
that when the density of the b01 phase increases, the surface
roughness of the obtained material increases as well.
The hardness values of the Cu-Al-Ni-Fe SMAs, heat treated
and quenched in different media, are shown in Table 4. It was
observed that different heat treatments had significant effects on
the hardness property. The oil-quenched sample exhibited greater
hardness compared with samples quenched in other quenching
media. This was due to the complete transformation of the initial
structure of the b01 and the higher grain growth. The ice water-
quenched sample had lesser hardness than the others.
4. Conclusions
The influence of quenching media on the structure and
properties of Cu-Al-Ni-Fe SMA was investigated. The changes
of the transformation temperatures and thermodynamic param-
eters were observed with regard to the variation of the
quenching media mechanisms, which led to the various
morphologies and structures of the obtained phases. Further-
more, through analyzing the XRD results, it was found that the
crystalline size had significant control on the transformation
temperatures. The hardness showed the greatest values with the
use of an oil bath, due to the high stability, distribution, low
grain size, and the regular orientation of the b01 phase, as well as
excellent structure homogeneity.
Acknowledgments
The author(s) would like to thank the Malaysian Ministry of
Higher Education (MOHE) and Universiti Teknologi Malaysia for
providing the financial support and facilities for this research,
under Grant No. R.J130000.7824.4F150.
Journal of Materials Engineering and Performance
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