Applied Surface Science 318 (2014) 100–104

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Applied Surface Science

journal homepage: www.elsevier.com/locate/apsusc

Effect of Cu concentration on the formation of Cu1−x Znx shape

memory alloy thin films
İsmail Hakkı Karahan a , Rasim Özdemir a,b,∗
a
Department of Physics, Mustafa Kemal University, Hatay 31000, Turkey
b
Kilis Vocational High School, Kilis 7 Aralık University, 79000 Kilis, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: The Cux Zn1−x (x = 0.06, 0.08, 0.1) deposits were fabricated by a electrodeposition method. The structural
Received 12 November 2013 and electrical properties of the films were investigated by cyclic voltammetry (CV), X-ray diffraction
Received in revised form 17 January 2014 (XRD), Scanning electron micrograph (SEM), and DC resistivity measurements. Phase identification of
Accepted 20 January 2014
the samples was studied by the XRD patterns. XRD patterns shows the characteristics XRD peaks cor-
Available online 27 January 2014
responding to the, ˇ, and  phases. The grain sizes of the samples were decreased whereas microstrain
increased with the increase in Cu2+ substitution. The SEM study reveals the fine particle nature of the
Keywords:
samples with increasing Cu content. DC resistivity indicates the metallic nature of the prepared sam-
Electrodeposition
Cu–Zn alloy ples. It has been found that the Cu ions have a critical influence on the resultant structure and resistivity
Electrical property properties of the Cu–Zn samples.
Shape memory alloys © 2014 Elsevier B.V. All rights reserved.

1. Introduction of rubber to steel, good mechanical resistance and conformability,

Electrodeposited metallic layers is generally practiced to modify
the substrate surface in order to produce a wide range of use-
ful materials with improved mechanical, chemical and physical
properties. This technique has demonstrated to be very conve-
nient because of its simplicity and low cost in comparison with the
other method such as sputtering and vapor deposition. Thus, eco-
nomical materials can be used as substrates, making this process
economically attractive. Compared to pure metal coatings, elec-
trochemically deposited alloys show better properties, since their
chemical composition can be varied to the required function. Since
the physicochemical properties of alloys are seriously affected by
their compositions as well as structures [1–8], a reliable control of
the composition and structure for these engineering alloys is an
important issue for their wide applications.
Properties of an electrodeposited film can be affected by many
parameters, such as the bath type, pH, deposition potential, and
metal ion contents. In particular, the metal ion concentration has
been observed to significantly affect the microstructure and mag-
neto transport properties of electrodeposited films.
Cu–Zn alloys have been widely used in industry, owing to their
attractive features such as protection against corrosion, adhesion
hardness and decorative value [9–15].
Commercial electrodeposition of Cu–Zn alloys in cyanide baths
produces high-quality deposit but environmental problems arise in
the use and disposal of cyanide. Thus an extensive search has been
made for satisfactory alternative electrolytes [12].
Cu–Zn electrodeposits can be produced from electrolytes other
than cyanide baths, namely, from electrolytic solutions based on
sorbitol [12], mannitol [14], sorbitol based alkaline [16], nitrilo-
triacetic acid (NTA) [17], pyrophosphate [18–21], citrate [13,22],
citrate based cysteine and benzotriazole [23], tartrate [24], glycerol
[25–27], and sulphate [28].
The plating of Cu–Zn alloys from citrate bath has not been exten-
sively studied. However, for baths containing more than 0.02 Molar
copper ions have not been clarified.
In this study, we decided to study these alloy deposits pre-
pared from a citrate bath with various Cu/Zn ratios to explore how
copper content would influence the deposition process and the
morphology, composition and electrical resistivity of the Cu–Zn
electrodeposits. The aim of this study was reduce the toxicity and
the cost of the electroplating process while maintaining the quality
of the coatings.
2. Experimental details

∗ Corresponding author at: Mustafa Kemal University, Faculty of Art and Science,
Department of Physics, 31000-Hatay, Turkey. Tel.: +90 326 245 58 66;
fax: +90 326 245 58 67.
E-mail address: ihkarahan@gmail.com (R. Özdemir).
Electrodeposition was realized in a conventional glassy cell in
non stirred and non aerated conditions. The bath composition
and deposition parameters for the Cu–Zn deposits are reported in
Table 1. All the chemicals used were of analytical grade. Double

0169-4332/$ – see front matter © 2014 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.apsusc.2014.01.119
 İ.H. Karahan, R. Özdemir / Applied Surface Science 318 (2014) 100–104 101

Table 1
Electrolyte composition and deposition conditions for Zn1−x Cux films electrodeposited on aluminum substrate at pH 5.8 and 20 ◦ C for the duration of 1 h.

Sample CuSO4 .5H2 O (mol L−1 ) ZnSO4 .7H2 O (mol L−1 ) Na3 C6 H5 O7 (mol L−1 ) Current (mA)

Zn74 Cu26 0.06 0.2 0.5 60

Zn63 Cu37 0.08 0.2 0.5 60
Zn48 Cu52 0.10 0.2 0.5 60

distilled water was used for preparation of the electrolyte solu-

tion. Pure aluminum foil with a surface area 3.8 cm2 was used
as substrate and before each experiment; the samples were pol-
ished, degreased, and activated by dipping in a 1 M NaOH with
surfactant at 70 ◦ C during 5 min and finally rinsed with the twice
distilled water (18 M cm) and dried with fresh air. The CV exper-
iments were conducted in a freshly prepared electrolyte given as
Table 1, without purging. A scan rate of 10 mV s−1 was selected
based on preliminary experiments. The scan began from 0.5 V in
the positive direction, up to −1.6 V, and finally reversed to 0.5 V.
The potentials were measured versus a saturated calomel refer-
ence electrode (SCE). Characterization of the coatings was done
by a variety of analytical facilities. The surface morphology of
the deposits was observed by means of a JEOL scanning electron
microscope (SEM). The attached energy dispersive spectroscopy Fig. 1. Influence of the copper concentration on the cyclic voltammograms for the
(EDS) detector was used to determine atomic composition of the electrodeposition from zinc solution (0.2 M ZnSO4 .7H2 O) in 0.5 M Na3 C6 H5 O7 , pH
alloy. Each sample was analyzed at three locations, to confirm 5.8, v = 10 mV s−1 .
uniformity.
A Rigaku diffractometer was used to analyze the crystallo- in the temperature range of 100–350 K were carried out by using
graphic structure of alloys. The X-ray diffractometer was operated a Keithley 2400 source measure unit. The samples were placed
at 30 kV and 30 mA with CuK˛ radiation. The film composition was onto cold finger of a Janis liquid nitrogen cryostat and the tempera-
determined via an Energy Dispersive X-ray Spectrometer (EDX). ture was accurately monitored with a Lake–Shore 320 temperature
The grain size (D) was calculated using Scherer’s formula [29]. controller.
0.9
D= (1) 3. Results and discussion
ˇ × cos 

The microstrain was obtained by using the relations [30]
ˇ × cos q
ε=
4
where ˇ is the full-width at half maximum,  is the wavelength of
X-ray used (1.5400 Å), and  is the diffraction angle.
The resistivity measurements were carried out using the four
point probe method. For this purpose; the electrodes were attached
to the contact regions with silver paint. The ohmic behavior of
the contacts in the studied temperature region was confirmed by
the linear variations of the I–V characteristics which is indepen-
dent from the reversal of the applied currents. The thermal voltage
effect was eliminated by taking the average of voltage readings
with two reverse currents at each temperature. Each sample was
measured several times to make sure that the obtained data was
reliable. The temperature-dependent conductivity measurements
3.1. Electrodeposition and properties of Zn, Cu, and Zn1−x Cux thin
films
(2)
To define the effect of electrolyte concentration on the Cu–Zn
alloy deposition process cyclic voltammetry technique was used.
Fig. 1 shows voltammograms for the aluminum electrode in the
Cu–Zn baths. From this figure, the influence of copper content
on the potentiodynamic cathodic and anodic polarization parts
of cyclic voltammograms curves can be seen. The potential was
scanned from 0.5 V to the cathodic direction up to −1.6 V and
ended at 0.5 V. It is apparent from Fig. 1 that the anodic part
in the cyclic voltammograms consisted of one anodic current
peak for all the films. This shows that the alloy dissolution takes
place under one potential values. The anodic process, in general,
shows an anodic dissolution peak A (A1 for 0.10 M, A2 for 0.08 M
and A3 for 0.06 M CuSO4 solutions) at 0.1 V vs SCE. In solutions,

Fig. 2. XRD analysis of Cu–Zn thin films.

102 İ.H. Karahan, R. Özdemir / Applied Surface Science 318 (2014) 100–104

Fig. 3. (a) SEM images of Zn74 Cu26 alloy (0.06 M CuSO4 .7H2 O). (b) SEM images of Zn63 Cu37 alloy (0.08 M CuSO4 .7H2 O). (c) SEM images of Zn48 Cu52 alloy (0.10 M CuSO4 .7H2 O).

during the forward scan towards the negative direction, the
cathodic current increased sharply when the deposition begins.
In addition, the increase in the current density at potentials more
negative than ∼−1.20 V can be attributed to a significant hydrogen
evolution reaction (HER) in parallel to Cu–Zn electrodeposition. It
was observed that in presence of more copper ion the cathodic
current was increased. Cu–Zn electrodeposition in the presence
of 0.06 M copper presents a reduction peak at −1.05 V versus
SCE. Upon reversal of the potential-sweep direction, a dissolution
peak was observed at 0.15 V. When the copper concentration was
increased to 0.08 M, the electroreduction peak shifted to −1.2 V
and the dissolution peak of the deposit showed an increase. When
the copper concentration was increased to 0.1 M, the reduction
peak was practically unaffected, but the dissolution peak increased
again.
It may be noted, in Fig. 1, that the deposition rate is affected in
cathodic region by the concentration of copper, since the cathodic
current density in this region increased when the concentration
 İ.H. Karahan, R. Özdemir / Applied Surface Science 318 (2014) 100–104 103

of this complex in the bath increased (20 mA cm−2 , 0.06 M CuSO4 105
in the bath; 30 mA cm−2 , 0.08 M CuSO4 in the bath; 34 mA cm−2 , 100
0.08 M CuSO4 in the bath). In this region a primary bulk nucleation
95
and growth of copper occurred.

The cathodic current starts to increase and forms the cathodic
peak at a potential that depends on bath condition.
The reaction responsible for the cathodic peak is reaction (1):
2+ − 0
(1)Cu + 2e = Cu
Upon the sweep reversal, the cathodic current density gradually
decreases, until it crosses 0 and turns into anodic current. Further
sweep in the positive direction results in the anodic peak, which
corresponds to the reaction (1) in the reverse direction. The current
density past the peak is 0, indicating the completion of oxidative
dissolution of metallic copper at the electrode surface. In the anodic
direction, however, the oxidation of copper starts from the surface
that already has copper deposited, resulting in a potential close to
the Cu/Cu2 equilibrium potential. Due to the difference in depo-
sition and dissolution potentials, a crossover occurs between the
cathodic and anodic current traces [31] at the crossover poten-
tial Ex. The presence of the crossover is diagnostic for the nuclei
formation on the electrode [32].
The preferential crystal orientation of zinc electrodeposits
depends on the experimental conditions [33,34], such as current
density, bath composition, pH and temperature. Fig. 2 shows the
X-ray diffraction patterns obtained for several Cu–Zn coatings elec-
trodeposited at gradually increasing copper concentration. From
the XRD measurements in the electrodeposited samples ˛, ˇ, and
 phases were detected. When the deposit was formed in the pres-
ence of 0.06 M Cu (Zn74 Cu26 ), a considerable decrease of the (1 1 0)
peak was observed, as well as of the peaks associated with planes
(2 1 1), due to the change in orientation of the Cu–Zn crystallo-
graphic planes by the incorporation of copper. When the copper
content in solution was increased to 0.08 M (Zn63 Cu37 ) and 0.1 M,
the peaks associated with plane (1 1 0) and (2 1 1) diminished fur-
ther and (1 1 1) peak was appeared. When the copper content in
solution was increased to 0.1 M (Zn48 Cu52 ), a peak (3 1 1) then
appeared at a value of 2 = 88◦ .
When Zn electrodeposited with other metals the morphol-
ogy of the deposits modifies because of their influence on the
growth of the initial nuclei [33]. Fig. 3 shows SEM micrographs of
deposits formed from the Zn74 Cu26 (Fig. 3(a) 0.06 M CuSO4 .7H2 O);
Zn63 Cu37 (Fig. 3(b) 0.08 M CuSO4 .7H2 O) and Zn48 Cu52 (Fig. 3(c)
0.10 M CuSO4 .7H2 O) the acidic citrate–sulfate Zn–Cu solutions at
various copper concentrations. It is observed that the deposits
are generally composed of fine grains. The metallic luster and the
brightness of the deposit increased with increasing of the copper.
In the presence of 0.06 M copper in the bath, the deposit being
compact and formed by small cubical crystallites. With a copper
concentration of 0.08 M, a deposit with even smaller grain size was
observed with slim rods (Fig. 3b), and at the 0.1 M copper grain size
was began to bigger non-coalesced globular crystallites and the film
Grainsize (nm)
90
85
80
75
70
65
60
20 30 40 50 60
Copper in Deposited CuZn (%)
Fig. 4. Grain size (D) with Cu content.
Fig. 4 shows that the crystallite diameter decreased from
100 to 66 nm with increase in Cu2+ substitutions, which is in
agreement with the results observed in the literature [35,36]. Fur-
ther, the substitution of Cu2+ in place of Zn2+ ion increased the
crystalline size, due to the large size mismatch between Cu2+
and Zn2+ ions. Hence, in order to relax the volume strain the
crystallite size decreases with the increase in Cu2+ concentra-
tion. Other possible explanation to decrease of crystallite size is
that the ionic radius of Cu is smaller than the ionic radius of
Zn.
The temperature dependent electrical resistivity measurements
for all samples were carried out in the temperature range of
100–350 K and the variations of normalized resistivity of five sam-
ples were plotted as a function of temperature in Fig. 5. There is a
gradual linear drop in resistivity as the temperature is lowered from
320 K. The resistivity increased with the increase in Cu substitu-
tion. The resistivity increased with the Cu substitution as it should
since increasing disorder, brought about by rising Zn concentra-
tion, contributes to the increasing electron scattering and hence to
increasing resistivity.
Electrical resistivity increases with increasing Cu content and
more increase in these elements in the sample decreases the resis-
tivity [37,38]. Fig. 6 illustrates increase in electrical resistivity
values for the alloys with increasing Cu concentrations in film. Fig. 6
shows the strong dependence of the resistivity on the composition
of thin films. This strong dependence on the composition can be
understood qualitively by considering the densities of states. The
density of states splits up into contributions from the components
(Zn, Cu) of the alloy. The two contributions are well separated in
energy.
Zn63Cu37 Zn48Cu52 Zn74Cu26
1.00
Normalized Resisvity

was compact. Naturally, morphologies of Cu–Zn deposits were con-

0.90
nected with the discharge mechanism of the complex agent adding
to the bath. 0.80
The average crystallite size of the samples was calculated
from the peak width at the half maximum of the peak (ˇ), 0.70
using Eq. (1).The microstrain (ε) for preferential orientation were
calculated using the Eq. (2). Table 2 shows the calculated aver- 0.60
age crystallite size of the samples obtained at different bath
compositions. The grain sizes were found to be within the 0.50
range of approximately 66–100 nm as seen from Fig. 4. The 50 100 150 200 250 300 350
average crystallite size of the Cu–Zn alloys decreased and micros- Temperature (K)
train increased when the increase in Cu concentration in the
bath. Fig. 5. Normalized electrical resistivity against temperature for the Cu–Zn alloys.
104 İ.H. Karahan, R. Özdemir / Applied Surface Science 318 (2014) 100–104

Table 2
Grain size, micro strain values for Zn74 Cu26 , Zn63 Cu37 and Zn48 Cu52 alloys.

Samples ␪ (◦ ) d(Å) FWHM Grain size (nm) Micro strain

Zn74 Cu26 43.201 2.0924 0.382 100.1 0.1183

Zn63 Cu37 43.240 2.0906 0.579 66.1 0.1862
Zn48 Cu52 42.306 2.1346 0.541 69.7 0.1622

0.25 [7] E. Beltowska-Lenman, A. Riesenkampf, An investigation of the electrodepo-

sition kinetics of permalloy thin films using a rotating disc electrode, Surf.
Technol. 11 (5) (1980) 349–355.
Electrical resisvity (μΩcm)

0.22
0.19
0.16
0.13
0.1
20 30 40 50 60
Copper in thin film (%)
Fig. 6. Effect of Cu ratio in the film and electrolyte in different temperature on the
electrical resistivity.
4. Conclusions
Zn74 Cu26 , Zn63 Cu37 and Zn48 Cu52 alloy films were synthesized
via electrodeposition method. X-ray diffractograms assured the
cubic spinel structure for all the investigated samples with the
appearance of small peaks represented a secondary phase due to
the presence of rare earth La3+ ions. XRD patterns confirmed that
the electrodeposited samples have ˛, ˇ, and  phases. The average
crystallite size of the samples varied from 67 to 100 nm. Micros-
train have been calculated Scherrer’s formula The strain of the films
increased firstly linearly with the increase of Cu substitution. But,
the crystallite size was reduced with the increase of Cu2+ ions. The
structural characterization of the powders using XRD confirmed the
formation of nanosized films. Bright, compact and good adherent
alloy coatings were obtained with galvanostatic conditions. Elec-
trical resistivity measurements showed the strong dependence of
the resistivity on the Cu content in the electrolyte and in the Cu–Zn
films. This strong dependence on the composition can be under-
stood qualitively by considering the densities of states.
Acknowledgement
Financial support of this research by the Mustafa Kemal Uni-
versity Scientific Research Projects is gratefully acknowledged
(MKU-BAP- 1005M 0118 and 1204 D 0110).
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