Journal of Alloys and Compounds 714 (2017) 530e536

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Journal of Alloys and Compounds

journal homepage: http://www.elsevier.com/locate/jalcom

Microstructure and corrosion behavior of electrodeposited Ni-based

nanocomposite coatings reinforced with Ni60Cr10Ta10P16B4 metallic
glass particles
Farzaneh Bahrami, Rasool Amini*, Amir Hossein Taghvaei**
Department of Materials Science and Engineering, Shiraz University of Technology, 71555-313, Shiraz, Iran

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

Article history: Ni-based nanocomposite coatings reinforced with Ni60Cr10Ta10P16B4 metallic glass powders have been
Received 12 January 2017 successfully deposited by a direct current electrodeposition method in a typical Watt's bath. The effect of
Received in revised form the glassy particles content on the microstructure, micro-hardness and corrosion behavior of the coat-
1 April 2017
ings have been evaluated. The structural investigations have been conducted by X-ray diffraction (XRD)
Accepted 7 April 2017
and scanning electron microscopy (SEM). The corrosion behavior of the coatings has been investigated in
Available online 8 April 2017
a 3.5 wt % NaCl solution by a potentiostat-galvanostat device in the potentiodynamic polarization mode.
The composite coatings with the negligible amounts of porosity and crack, homogeneous distribution of
Keywords:
Ni-based composite coatings
the glassy particles, and appropriate bonding at the matrix/reinforcement interface are obtained. The
Metallic glass results demonstrate that the crystallographic texture and surface morphology of the coatings are
Electrodeposition significantly changed by the addition of the glassy particles into the bath. A minimum matrix crystallite
Microstructure size of 31 nm and maximum glassy particles incorporation of about 6.4 vol% are obtained for the particles
Corrosion behavior concentration of 10 g/L in the deposition bath. The microhardness of the coating is enhanced with
increasing the content of the reinforcing particles in the bath and reaches a maximum value of 475 HV
for the particles concentration of 10 g/L. Moreover, the corrosion current density and corrosion rate are
significantly reduced from 2.25 mA/cm2 and 0.958 MPY for the pure Ni coating to 0.05 mA/cm2 and 0.021
MPY for the nanocomposite coating.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction hardness, enhanced corrosion and abrasion resistance, improved

self-lubrication, and good fracture and tensile strength, compared
Electroplating is employed to deposit a film of a metal or an to pure metal and alloy coatings [6]. The co-deposition process
alloy, or their composite films reinforced by micron/nano-sized includes diverse types of reinforcing particles, such as metallic,
metallic or nonmetallic particles. This process is a method to pro- nonmetallic or polymers in the electrolytic or electroless bath [7]. A
duce a dense, uniform and adherent coating, which provides wear great variety of ceramic particles have been employed in electro-
and corrosion resistance, good mechanical properties, and can plating of Ni-based composite coatings, such as TiO2 [7], Al2O3 [8,9],
change thermal, magnetic and optical characteristics [1e3]. ZrO2 [10,11], SnO2 [12], WC [13], SiC [14,15], TiN [16], and Al2O3þSiC
Among the wide range of accessible materials used as the matrix [17,18].
in the electrodeposition process, Ni is a multipurpose metal in steel The increase of strength without sacrificing ductility is a pri-
plating, due to its excellent corrosion resistance and industrial mary purpose in the production of metal-matrix composites
characteristics [4,5]. Nowadays, composite coatings produced by (MMCs). It is well-known that the overall properties of MMCs, in
the electroplating process are developed due to their high the form of bulk or coatings, are greatly correlated with the matrix/
reinforcement interface [19]. Hence, a large difference between the
matrix and reinforcing particles' characteristics can have detri-
mental effects on the deposit properties [20]. For instance, the
* Corresponding author.
interface between ceramic particles and metallic matrix is not
** Corresponding author.
E-mail addresses: [email protected] (R. Amini), [email protected]
generally strong, resulting in an insufficient load transfer from the
(A.H. Taghvaei). matrix to the reinforcement upon mechanical loading [21]. In

http://dx.doi.org/10.1016/j.jallcom.2017.04.069
0925-8388/© 2017 Elsevier B.V. All rights reserved.
 F. Bahrami et al. / Journal of Alloys and Compounds 714 (2017) 530e536 531

addition, the weak particles/matrix interface and the tendency of in distilled water before electroplating. The electrolyte composition
the ceramic particles to agglomeration could produce voids at the and electrodeposition parameters are listed in Table 1.
reinforcement/matrix interface or inside the particle clusters Prior to electrodeposition, Ni60Cr10Ta10P16B4 glassy powders
[22,23]. Such voids adversely affect the corrosion behavior of the were produced by mechanical alloying of the elemental powders in
substrate and provide cracking upon loading, which can deteriorate a high-energy planetary ball mill for 150 h under an argon atmo-
the mechanical properties of the composite film. Moreover, a sig- sphere. The milling speed and ball-to-powder weight ratio were
nificant difference between the thermal expansion coefficient of selected 450 rpm and 20, respectively. The above composition was
the metallic matrix and ceramic reinforcement can produce inter- designed according to the rapidly-solidified Ni65þxCr10-xTa5P16B4
nal strain in the coating upon subsequent heat treatment, which (x ¼ 0, 5) MGs exhibiting an outstanding corrosion resistance [36],
can affect its overall properties [24]. where the increase of the Ta content from 5% in the original
The above problems can be addressed by different strategies, composition to 10% can produce amorphous powders by mechan-
including coating of ceramic reinforcements [25] or using other ical alloying. Fig. 1 shows the X-ray diffraction pattern and scanning
types of reinforcements with a notably better compatibility and electron microscopy image of the prepared powders. The observed
wetting with the matrix. Metallic glasses, MGs, have been recently halo pattern and the absence of any Bragg peak clearly reveal the
used as the reinforcement in MMCs owing to their high strength, amorphous structure of the powders. According to the inset of
excellent corrosion behavior and, more importantly, very good Fig. 1, the powder particles have a semi-spherical morphology with
interfacial bonding and a similar coefficient of thermal expansion an average particle size of about 6 mm. More details about the
with metallic matrices [19,26]. It should be emphasized that most characterization of the produced powders will be published
of the researches in this area are limited to the production of Al- elsewhere.
based MMCs in the bulk form, reinforced with Al- [27e29], Mg- In order to minimize the particle agglomeration and to provide a
[30], Fe- [31,32], Ni- [33] and Zr- [34] based MGs. To the best of our uniform distribution of the glassy particles in the composite coat-
knowledge, no research has been reported on the preparation and ings during electrodeposition, 0.1 g/L sodium dodecyl sulfate, SDS
characterization of electrodeposited Ni-based nanocomposite as the surfactant was added to the electrolyte bath. Moreover, 3 g/L
coatings reinforced with MGs. saccharin was used as a surface modifier to decrease the crystallite
Toward addressing the challenges of developing desirable size of the Ni matrix.
coatings, including a suitable interfacial bonding between con- Structural studies were performed by X-ray diffraction (XRD,
ventional ceramic reinforcements and Ni matrices and their ho- Bruker Advanced 2) with Cu Ka radiation (l ¼ 1.154 Å) in an angular
mogeneous distribution, the present work focused on Ni-based range of 30e105 at a step size of 0.02 and a counting time of 2 s.
nanocomposite coatings reinforced with MG particles for the first The crystallite size of the electrodeposited coatings was calculated
time. The influence of the MG powder concentrations in the by Double-Voigt method, using the MAUD software. Moreover, the
deposition bath on the crystallite size, textural properties, morphology and microstructure of the deposited coatings were
morphological evolution, microhardness, and corrosion behavior of evaluated by scanning electron microscopy (SEM, FEI, Nova Nano-
the composite coatings was systematically investigated. To enhance sem430). The microhardness of the coatings was also measured on
the compatibility of the reinforcement and matrix, a Ni-based MG
of the well-known Ni-Cr-Ta-P-B alloy system prepared by me-
chanical alloying. It has been shown that the selected MG exhibit
high strength and superior corrosion resistance due to the forma-
tion of a stable passive film enriched with Cr-Ta double oxy-
hydroxides ((Cr,Ta)xOy(OH)z) [35,36].

2. Experimental procedure

Ni/MG composite coatings were electrodeposited on steel sub-

strates in a typical Watt's bath. A pure Ni plate of 25  20 mm2 and
a CK45 steel plate of 10  15 mm2 were used as the anode and
cathode, respectively. CK45 steel was used because of its low price
and accessibility, where its relatively low corrosion and wear
resistance can be significantly improved by using a coating process.
The surface preparation was conducted on the steel substrates in
several steps. Initially, they were mechanically polished up to 800-
grit finish, and then ultrasonically cleaned by distilled water and
acetone to eliminate surface contaminations. Subsequently, the
samples were activated in 10 vol% H2SO4 bath for 2 min and washed Fig. 1. XRD pattern and SEM image of the synthesized metallic glass powders.

Table 1
Electrolyte composition and electrodeposition parameters.

Electrolyte composition Electrodeposition parameters

Component Concentration (gr/L) Current density (A/dm2) 1

Nickel sulfate, NiSO4$7H2O 240 Deposition time (min)/Temperature ( C) 90/45

Nickel chloride, NiCl2$H2O 36 PH 4
Boric acid, H3BO3 40 Magnetic stirring speed (rpm) 450
Sodium dodecyl sulfate, C12H25NaO4S 0.1 Anode/cathode material Pure Ni plate/steel plate
Saccharin 3 Anode to cathode surface area 3
Metallic glass particles, Ni60Cr10Ta10P16B4 0, 5, 10, 20, 40 Distance between the electrodes (cm) 3
532 F. Bahrami et al. / Journal of Alloys and Compounds 714 (2017) 530e536

the cross-sections by a Vickers microhardness indenter under a

load of 50 g and holding time of 10 s. The average value of ten
measurements was selected as the final microhardness values.
The corrosion behavior of the deposits was investigated by a
potentiostat-galvanostat device (Ivium, Vertex) using a three-
electrode cell in a 3.5 wt % NaCl solution at room temperature.
The samples were isolated with epoxy resin and an area of 1 cm2
was exposed as a working electrode. Pt and Ag/AgCl electrodes
were used as counter and reference electrodes, respectively. The
experiments were performed at a constant scan rate of 5 mV/s. The
corrosion potential (Ecorr) and corrosion current density (icorr) were
evaluated by the Tafel extrapolation method [37]; then, the corro-
sion rate of the coatings was calculated by the Faraday equation
[38].

3. Results and discussion

3.1. Structural and microstructural studies

Fig. 2 shows the cross-sectional SEM images of the Ni-based

composite coating obtained at 10 g/L concentration of the glassy
particles in the Watt's bath. As can be seen, a coating with an Fig. 3. Volume fractions of the incorporated glassy particles as a function of their
average thickness of 60 mm is uniformly deposited on the steel concentration in the electrolyte bath.

substrate, with no detectable porosity and cracks in the coating and

coating/substrate interface. In addition, a homogeneous distribu-
morphology is considerably changed with the addition of the
tion of the glassy particles (ranging from 4 mm to 8 mm) throughout
reinforcing particles to the Watt's bath. With the incorporation of
the Ni matrix is confirmed.
the particles, the surface heterogeneity notably increases and the
The volume fractions of the glassy particles estimated from the
surface morphology of the coatings is changed from smooth for the
cross-section images by an image analyzer software (Material Plus,
pure Ni coating to a protruding crystallite morphology originating
4.2) are illustrated in Fig. 3. It is inferred that by increasing the
from the a heterogeneous nucleation and growth of Ni crystals on
particle concentration in the bath, the fraction of the MG in the
the reinforcing particles [42,43].
deposits increases and finally reaches its maximum amount (6.4 vol
According to Fig. 4 (b), the coating prepared from 5 g/L MG in the
%) at 10 g/L. More concentrations of the glassy particles in the bath
Watt's bath contains a few numbers of reinforcement colonies with
result in a less incorporation of the particles in the electrodeposited
a relatively non-uniform distribution, caused by a low concentra-
coatings. Indeed, at a sufficiently high concentration of the particles
tion of the glassy particles in bath. The further increase in the
in the bath, not only the tendency of the particles to stick together
concentration to 10 g/L and 20 g/L enhances the number of the
and agglomerate in the electrolyte are considerably increased [39],
colonies and improves their distribution in the matrix, while
but also elastic collisions between the particles is enhanced [40].
simultaneously reduces their size (see Fig. 4(c) and (d)). However,
Moreover, at the large concentrations of the reinforcing particles,
at the sufficiently high concentrations of the MG in the bath (e.g.
the elimination of Hþ ions from the cathode surface is reduced,
40 g/L), particles agglomeration occurs, which causes the formation
leading to an increase in the number of evoluted H2 bubbles on the
of a small amount of large colonies at the coating surface (Fig. 4(e)).
cathode surface. This thereby impedes the movement of the rein-
According to Figs. 2 and 4, no detectable voids and cracks appear
forcing particles toward the cathode surface [41]. These phenom-
in the electrodeposited Ni coatings. It can originate from the for-
ena prevent the effective absorbance of the glassy particles to the
mation of an excellent metallurgical bonding between Ni matrix
cathode surface during electrodeposition.
and Ni-based MG, as a result of compatibility between their com-
Fig. 4 illustrates the effects of the reinforcing particles concen-
positions. It is well-established that a proper wetting between the
tration on the topography and surface morphology of the electro-
filler and matrix improves the particles distribution and declines
deposited coatings. It is clearly observed that the surface

Fig. 2. Cross-sectional SEM images of the nanocomposite coating deposited in the bath containing 10 g/L of the glassy particles at different magnifications.
 F. Bahrami et al. / Journal of Alloys and Compounds 714 (2017) 530e536 533

Fig. 4. SEM images of the Ni-based coatings deposited in the baths containing the different concentrations of the glassy particles; (a) 0 g/L, (b) 5 g/L, (c) 10 g/L, (d), 20 g/L, and (e)
40 g/L.

the composites' defects as a result of strong interfacial bonding diffraction plane, thereby indicating a random texture in the de-
[24,44]. posits. Because of a lower planar atomic density of (2 0 0) plane
The XRD patterns of the produced pure Ni and Ni/MG composite than the (1 1 1) plane in the face-centered cubic (FCC) structure, the
coatings are shown in Fig. 5. Significant texture changes can be seen surface energy of (2 0 0) plane is higher than (1 1 1) in Ni. Hence, the
by the addition of the glassy particles to the electrolyte bath. addition of the glassy particles leads to the transition of Ni atoms
Although the (1 1 1) and (2 0 0) peaks are obviously observed in all from a higher-energy level to a lower one; consequently, (1 1 1)
of the patterns, the other peaks especially (2 2 0) and (3 1 1) show becomes the main diffraction plane [45]. This textural trans-
remarkably low intensities. It can be inferred that the monolithic Ni formation can result from the heterogeneous nucleation and
coating exhibits mainly a preferred orientation of (2 0 0). According growth of Ni crystals on the glassy particles [3]. It has been found
to Fig. 5, by the incorporation of the glassy particles into the Ni that the growth orientation of Ni crystals is changed from a pyra-
matrix during electrodeposition, the intensity of the (2 0 0) peak is midal mode to a colony-like structure in the presence of reinforcing
meaningfully reduced and the (1 1 1) diffraction acts as the main particles [46].
In order to compare the preferred growth orientations of the
produced composite coatings, the texture coefficients (TC) of the
different planes are calculated according to the following equation
[47]:

IðhklÞ=I0 ðhklÞ
TCðhklÞ ¼ P (1)
I¼1 IðhklÞ=I0 ðhklÞ

where I and I0 are intensity of the (hkl) plane for the coating and Ni,
respectively. Table 2 lists the TC values for (1 1 1), (2 0 0), (2 2 0) and
(3 1 1) planes of the produced coatings. By increasing the particles
concentration in the bath, TC of (1 1 1) to (2 0 0) reflections is
initially increased from 0.3 (for pure Ni) to 0.96 (for 10 g/L); then,
due to the reduction of the reinforcement content in the deposits, it
is reduced gradually to 0.6 (for 40 g/L). At the moderate concen-
tration of the reinforcement in the electrolyte bath (10 g/L),
wherein the sufficient amount of the glassy particles is incorpo-
rated into the Ni matrix, the texture modification from the soft [1
0 0] mode to the preferred [2 1 1] one occurs, which is in good
agreement with the effect of other reinforcing particles reported in
the literature [48].
Fig. 6 represents the Ni-matrix crystallite size of the electro-
deposited coatings as a function of the particle concentration in the
bath. Owing to the enhancement of Ni nucleation sites by the
particle incorporation [20,49], the Ni crystallite size initially de-
creases from z47 nm at 0 g/L, to z 31 nm at 10 g/L. However, at the
higher concentrations of the glassy particles in the electrolyte, the
Fig. 5. XRD patterns of the coatings electrodeposited in the bath consisting the various
crystallite size gradually increases and reaches z40 nm at 40 g/L.
quantity of the glassy particles. The peaks belong to the FCC Ni matrix with no evi- Compared to monolithic deposit, the structural refinement for a
dence of reinforcement peaks according to its amorphous nature. composite coating can be attributed to the nucleation of small
534 F. Bahrami et al. / Journal of Alloys and Compounds 714 (2017) 530e536

Table 2
Texture coefficient (TC) values calculated for the pure Ni and Ni/metallic glass nano-
composite coatings.

Metallic glass particles concentration Texture Coefficient (TC)

in the Bath (g/L)
(1 1 1) (2 0 0) (2 2 0) (3 11)

0 0.81 2.73 0.027 0.186

5 1.1 2.22 0.18 0.48
10 1.38 1.43 0.36 0.82
20 1.31 2.13 0.14 0.45
40 1.3 2.15 0.09 0.44

Fig. 7. Microhardness variations of the coatings as a function of the glassy particle

concentrations in the Watt's bath.

mechanisms, including (1) grain boundary strengthening (Hall-

Petch), (2) Orowan strengthening, (3) particle strengthening, (4)
texture modifications, can contribute to the microhardness
enhancement by the particle incorporation in the deposited com-
posite coatings [55]. Due to appropriate bonding at the interface of
the glassy particles and Ni matrix, the load can be efficiently
transferred from the matrix to the hard glassy particles; conse-
Fig. 6. Ni-matrix crystallite size of the produced coatings as a function of the particle quently, the hardness of the composite coating increases [56]. In
concentration in the bath. addition, the texture modification from soft [1 0 0] mode to the
preferred [2 1 1] one can also contribute to the hardness
improvement occurring in the deposits after the glassy particles
grains on the surface of the incorporated particles [50]. The incor-
incorporation (see Table 2) [45]. According to Fig. 6, the crystallite
poration of the reinforcing particles enhances the cathode area, and
size of the Ni matrix is reduced upon the glassy particle incorpo-
consequently increases the available sites for nucleation, resulting
ration. Hence, the grain boundary strengthening mechanism can
in grain size refinement [51]. According to Fig. 6, the increase of
also contribute to the microhardness enhancement, based on the
crystallite size for the high concentration of MG demonstrates that
Hall-Petch equation [57]. However, no remarkable strengthening is
content of the incorporated particles is decreased, due to the
expected to obtain through the interaction of dislocations with the
agglomeration and suspension effect, as mentioned above. It is
glassy particles. According to the Orowan mechanism, the rein-
worth to note that the effect of the reinforcement content on the
forcing particles cannot noticeably impede the movement of dis-
crystallite size reduction is significantly less than that reported by
locations and increase the microhardness when their particles size
some researchers in Ni-based composite coatings [20,50,52]. This
is larger than 1 mm [58]. It should be noticed that the glassy par-
effect is attributed to the coexistence of the saccharin modifier and
ticles size varies from 4 mm to 8 mm, according to Fig. 2.
glassy particles in the Watt's bath. It is well-understood that the
saccharin species plays a crucial role in the Ni crystallite size
refinement [53,54]. 3.3. Corrosion studies

To determine the corrosion and passivation behavior of the

3.2. Microhardness evaluation coatings, polarization tests were conducted in the 3.5 wt % NaCl
solution. Prior to the potentiodynamic tests, the samples were
Fig. 7 depicts the evolution of microhardness in the cross- immersed for an hour in the NaCl solution and then the open circuit
section of the nanocomposite coatings as a function of the MG potentials (Eocp) are measured. Fig. 8 exhibits the polarization
concentrations in the Watt's bath. As can be observed, by increasing curves of the samples. The electrochemical data extracted from the
the particles concentration in the bath, the microhardness is curves are listed in Table 3. As can be seen, by the glassy particle
enhanced form 438 HV (in pure Ni) to 575 HV (in 10 g/L); then, due incorporation into the Ni-based deposits, not only the corrosion
to the decrease in the volume fraction of the MG incorporated in current densities and consequently the corrosion rates of the
the coating, it is gradually reduced to 449 HV (in 40 g/L). Several coatings are significantly reduced, but also the corrosion potentials
 F. Bahrami et al. / Journal of Alloys and Compounds 714 (2017) 530e536 535

electrodeposition bath, the corrosion current density is initially

reduced from 0.958 MPY (in 0 g/L) to 0.021 MPY (in 10 g/L) and then
gradually increases. The lowest corrosion rate is obtained at the
moderate concentrations of the reinforcement (e.g. 10 g/L), since
the coating is dense, uniform, and almost defect-free in comparison
to the other coatings. At 20 g/L and 40 g/L concentrations, the
colony size becomes larger and the particle agglomeration starts
gradually. This effect results in the production of defects, surface
morphology deterioration, and the particles content reduction in
the deposited layer, reducing the corrosion resistance of the de-
posits in the NaCl solution.

4. Conclusions

In this study, a novel Ni-based nanocomposite coating rein-

forced with Ni60Cr10Ta10P16B4 metallic glass (MG) particles was
prepared by electrodeposition and the effect of the MG particles
concentration in the Watt's bath on the structure, microhardness
and electrochemical corrosion properties was investigated. It was
indicated that a coating with an average thickness of 60 mm and a
homogeneous distribution of the MG particles was uniformly
deposited on the steel substrate with negligible porosity and cracks
in the coating and coating/substrate interface. The results demon-
strated that the incorporation of the MG reinforcement notably
affected the surface topography, crystallite size and textural prop-
erties of the coating. A maximum content of the glassy particles in
the coating was obtained to be 6.4 vol% for the particle concen-
tration of 10 g/L in the bath. In addition, at this concentration, the
Fig. 8. Potentiodynamic polarization curves of the produced pure Ni and nano-
maximum amount of the coating's microhardness was achieved,
composite coatings in the 3.5 wt % NaCl solution.
where its quantity was about 1.3 times (137 HV) higher than pure
Ni coating. Also, the electrochemical studies revealed that by
move toward noble directions. The coating corrosion resistance is increasing the particle concentration in the electrolyte bath, the
influenced by chemical composition, microstructural characteristic, corrosion rate was initially reduced from 0.958 MPY (for pure Ni) to
preferred orientation, and crystallite size [47]. Since the MG rein- 0.021 MPY (at 10 g/L) and then it increased to 0.562 MPY (at 40 g/L).
forcement can modify the microstructure of the Ni layer and act as This corrosion improvement (up to 45 times compared to the non-
an inert physical barrier to diffuse the corrosive species in the reinforced Ni-based coating) was incredible and, to our knowledge,
coating thickness [52], the corrosion resistance of the coating can was not reported in the literature for any Ni-based nanocomposite
be improved considerably by the glassy particle incorporation. In coatings.
addition, from the electrochemical view point, the enhanced
corrosion resistance can be correlated with the formation of Acknowledgements
abundant micro-galvanic cells, where the glassy particles and Ni
matrix act as cathode and anode, respectively. It should be noted The authors would like to thank the Shiraz University of Tech-
that a uniform distribution of the MG particles and their superior nology (Department of Materials Science and Engineering) due to
interfacial bonding with the Ni matrix notably decrease the local- the support of this study.
ized corrosion and encourage the occurrence of homogeneous
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