Review Article: Composite and Nanocomposite Coatings

Journal of Metallurgical Engineering (ME) Volume 3 Issue 1, January 2014
doi: 10.14355/me.2014.0301.04
www.me-journal.org
Review Article: Composite and

Nanocomposite Coatings
Z. Abdel Hamid
Corrosion Control and Surface Protection Lab. Central Metallurgical R & D Institute, Cairo, Egypt
forzeinab@yahoo.com
Abstract
Composite or nanocomposite coatings, a new branch of
deposition that possess unique physical and mechanical
properties are formed by mixing two or more dissimilar
materials at the micron or nanoscale. Composites are used
when a combination of properties is required that cannot be
found in a single material. The properties of composite
depend upon not only the individual components used but
also the morphology and the interfacial characteristics. The
nancomposites can exhibit enhanced mechanical, electrical,
magnetic, and/or optical properties compared with their
conventional micron-scale (or larger) counterparts. Nanocomposite materials and coatings therefore offer enormous
potential for new applications including: aerospace,
automotive, electronics, biomedical implants, non-linear
optics, mechanically reinforced lightweight materials,
sensors, nano-wires, batteries, bioceramics, energy
conversion and many others.
This review presents the scientific framework for the
advances in the composite and nanocomposite coatings
research, including fundamental composition/property
relationships, fabricating techniques, and applications of
nanocomposite coatings. Additionally, the co-deposition of
various metallic matrices with a great variety of nano-sized
powders from hard carbides, oxides, and ceramics are
discussed.
Keywords
Composite; Nano Composite; Nanomaterials; Nanoparticles,
Ceramic powder; Reinforcement; Deposition Processes
Introduction
The composite and nanocomposite coatings represent
a new class of materials, whose mechanical and
tribological properties are not subjected to volume
mixture rules, but depend on grain boundary effects,
and synergetic interactions of the composite
constituents owing to the size effect (Catledge A. etal.
2002, Roy R etal. 1986). These materials can be
classied as hard, superhard or ultrahard for hardness
materials over 20, 40 or 80 GPa, respectively (Veprek S
etal. 1999). Hard coatings are used in many
applications, for example, cutting and polishing tools,
molds, dies, hard disk and other wear-resistant

applications. However, for engineering applications,
hardness must be complimented with high toughness,
which is a property of equal importance as hardness
(Zhang S., etal. 2005, Musil J etal., 2005 and. Voevodin
A. A. etal., 2005). The production of nanocomposite
coatings can be achieved through the co-deposition of
the matrix material containing disturbed particles of
powders, fiber or whiskers. There are many techniques can be used for nanocomposite fabrication such
as electrodeposition (Sautter F.K., 1963), electroless
(Gui Y. L. etal., 1993 ), magnetron sputtering (Musil J.
etal., 2001) and sol-gel (Lakshmi R. V., etal., 2011). The
electroplating and electroless co-deposition techniques
are the most common for preparing nanocomposite
coatings. Detailed description of applied deposition
techniques, mechanisms and influencing factors will
be presented in this text.
Electrodeposition Technique
Firstly, electrodeposition technique has been evolved
into a mature subject of research and development
today due to its wide range of applications. Composite
electrodeposition has been identified to be a
technologically feasible and economically superior
technique for the preparation of such kind of
composites. It is well known that insoluble particles or
bers can be co-deposited with metal or alloy to form
composite coatings by electrodeposition method.
During this process, the powder particles are
suspended in a conventional plating electrolyte and
captured in the growing metal film.
The electrodeposition of small particles with metals
had resulted over the past two decades in a number of
attractive industrial applications: large-scale composite
plating of systems like Ni-SiC, Co- TiO2 and Zn- NiSiO2 (Changgeng X. etal. 1988, Chan R.W, etal. 1996).
In 1997, our laboratory group at CMRDI has
introduced first contribution to composite coating
development through the deposition of high wear
resistance composite coatings by Saher group (Shawki
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S. etal., 1997). On the other hand, Abdel Hamid, has

studied thermodynamic parameters of composite
coatings and suggested the deposition mechanism
(Abdel Hamid Z., 2001). Following, Abdel Hamid
group has investigated the deposition of different
composite coatings containing polymers and ceramics
such as PTFE, SiC, WC and TiC-Al2O3 powders (Abdel
Hamid Z. etal., 2002, Abdel Hamid Z., etal. 1999 and
Abdel Aal A. etal., 2006). Shawky et al. (Shawki S. etal.,
1997) proved that the electrodeposited Ni-P composite
coatings incorporating a variety of inorganic particles
can be obtained from Watts nickel bath containing
sodium hypophosphite. The mechanism of codeposition of various particles (SiC, Al2O3, quartz and
sand) was studied in view of the electro-kinetic charge
characterizing the solid particles. Surface active agent
such as sodium oleate has been used to improve the
mobility of the particles in the plating solution. The
purpose was to increase particle content in the coating
to attain high hardness values. Special attention was
given to the deposition process using SiC particles.
The surface morphology, hardness and wear
resistance of the composite coatings were determined.
Hardness and wear resistance values were maximized
by simple heat treatment in air atmosphere which led
to the precipitation of the hard Ni3P phase. Sound,
coherent and high wear resistance coatings could be
produced. Borkar T., et al. deposited nickel composite
coatings (Ni Al2O3, NiSiC, and NiZrO2) from Watts
bath using direct current (DC), pulsed current (PC),
and pulsed reverse current (PRC) (Borkar T., etal.
2011). This study proved that all the coatings exhibited
significant improvement in microhardness and wear
resistance due to enhanced reinforcement of nanoparticles in the coatings as shown in Figs. 1&2.
examined and compared with polyethylene-free nickel

deposits. An optimum value of polyethylene (30 vol.%)
was obtained at 30 gl-1 polyethylene particles in the
electrolyte, at 7.59 Adm-2 at pH 4 and temperature 50
C. The microhardness wear resistance and corrosion
resistance of the composite were found to be greater
than that of free nickel deposits. The surface
morphology and distribution of PE particles in the Nicomposite is shown in Fig. 3.
FIG. 2 THE VARIATION OF WEIGHT LOSS FOR PURE NICKEL

AND NICKEL COMPOSITE COATINGS DEPOSITED BY DC, PC
AND PRC ELECTRODEPOSITION METHODS (Borkar T., etal. 2011)
FIG. 3 THE SURFACE MORPHOLOGY AND DISTRIBUTION OF

PE PARTICLES IN THE NI-COMPOSITE (ABDEL HAMID Z. etal.,
2002).
FIG. 1 MICROHARDNESS OF PURE NICKEL AND NICKEL

COMPOSITE COATINGS DEPOSITED BY DC, PC AND PRC
ELECTRODEPOSITION METHODS (Borkar T., etal. 2011)
Abdel Hamid et al. proved that Nickel-polyethylene

composites can be produced by electrodeposition
technique using Watts nickel bath (Abdel Hamid Z.
etal., 2002). The properties of the composites such as
microhardness, wear and corrosion resistance were
30
Recent literature on the electrodeposition of metallic

coatings containing nanosized particles was surveyed
(Liu Y etal.,2008 and Xue J., etal., 2004). The nanosized
particles, suspended in the electrolyte by agitation or
use surfactants, can be codeposited with the metal
matrix. The incorporated of nanosized particles can
improve microhardness and corrosion resistance,
modify growth to form a nanocrystalline metal deposit
and a shift in the reduction potential of a metal ion.
Many operating parameters influence the quantity of
incorporated particles, including current density, bath
agitation (or movement of work piece) and electrolyte
composition. High incorporation rates of the dispersed
Recently, Ni nanocomposite coatings have gained a

significant interest as anodes for fuel cell applications
(Abdel Aal A., etal. 2008, Abdel Aal A., etal. 2009,
Zhang L., 2010, and Lu B., etal. 2010). They were
prepared by incorporating of nano-sized metal oxide
particles such as TiO2, ZnO or Al2O3 into the Ni matrix
by electroless or electrodeposition technique. Ni or its
composite as a catalyst was used for electrooxidation
of small organic molecules (Abdel Aal A.,etal. 2009,
Zhang L., 2010). It was found that the electrooxidation
process at the Ni-based catalyst involved the
formation of a higher valence Ni oxide which acted as
a chemical oxidizing agent. The -Ni(OH)2/-NiOOH
redox couple acted as an effective electron transfer
mediator for the oxidation process (Kim J.W., etal.,
2005). Abdel Aal A. etal. demonstrated that the
presence of TiO2 nanoparticles deposited with Ni as
nanocomposite
electrodes
improves
the
electrocatalytic activity and the stability of Ni catalyst
towards electrooxidation of methanol, formaldehyde
and glucose in alkaline solutions (Abdel Aal A., etal.
2008, Abdel Aal A., etal. 2009). So far, little work has
been reported in the literatures concerning the role of
nano-sized metal oxides in enhancing the catalytic
activity of Ni catalysts. Instead, there are some articles
that address the role of some metal oxides in
stimulating non- nickel catalysts. For example, Xu C.,
etal. reported that the addition of oxides like CeO2,
NiO, Co3O4 and Mn3O4 promoted the Pd/C for alcohol
electrooxidation in alkaline media (Xu C., etal. 2005).
Additionally, Wang etal. reported that NiO
significantly improves the electrode performance for
methanol oxidation in terms of the reaction activity
and poisoning resistance (Wang M., etal. 2009).
Moreover, the deposition of CoO on a Pt electrode
represented prominent electrocatalytic activity
towards the mediated electrooxidation of ascorbic acid,
glucose and methanol (Helia H., etal. 2010). Oxides of
Ni-Cu exhibit low overvoltage for methanol oxidation
and act as effective anode materials (Shobha T. etal.
2003). Other metal oxides granted the catalyst
antipoisoning ability and improve the kinetic
processes, such as MgO (Liu B., etal. 2007, Samant P.V.
etal., 1999). Based on the literature survey, it was
found that the role of nano-sized metal oxides in
enhancing the electrocatalytic activity of Ni as a
nanocomposite catalyst has not been studied enough,
this scope needs more investigation.

a
FIG. 4 SEM OF A) Ni FREE Cr2O3/C, AND Ni-NANO

Cr2O3/C ELECTRODES PREPARED AT DIFFERENT
CONTENT OF Cr2O3 IN THE BATH: B) 2, C) 5 AND D) 20
g l-1 (Hassan H. B., etal. 2011).
1 Vf %
400
II - 3 Vf %
III - 7 Vf %
I / mA cm-2
particles have been achieved using a high nanoparticle

concentration in the electrolyte solution, smaller sized
nanoparticles; a low concentration of electroactive
species, ultrasonication during deposition and pulsed
current techniques.
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IV - 10 Vf %
300
Ni-free Cr2O3 /C
200
100
0
0
300
600
900
1200
E / mV (MMO)
FIG. 5 CYCLIC VOLTAMMOGRAMS OF THE
ELECTROCHEMICAL OXIDATION OF 2.0 M ETHANOL AT
NI-FREE Cr2O3/C AND NI-NANO Cr2O3/C (I, II, III & IV
ELECTRTODES CONTAINING DIFFERENT VF % OF Cr2O3 IN
THE DEPOSITS) IN 1.0 M NAOH AT A SCAN RATE OF 50 mV
S-1 (Hassan H. B., etal. 2011).
Z. Abdel Hamid group successfully prepared nanocomposite coatings consisting of nickel matrix and
Cr2O3 nanoparticles by means of electrodeposition
technique onto commercial carbon substrates (Hassan
H. B., etal. 2011). The co-deposition of nano-sized
Cr2O3 particles in a metal deposit modified the surface
morphology of nickel matrix (see Fig. 4). In comparison
with Ni/C electrode, the nanocomposite of NieCr2O3/C (7Vf %) showed a higher surface area, catalytic
activity and stability towards the electrochemical
oxidation of ethanol in 1.0 M NaOH solution. Higher
kinetic parameters such as the charge transfer
31
coefficient and charge transfer rate constant in the

redox species of Ni were recorded at Ni-Cr2O3/C
(7Vf %) electrode compared with Ni/C electrode. A
higher diffusion coefficient of ethanol as well as
catalytic rate constant k is obtained at Ni-Cr2O3/C
(7Vf %) electrode compared with that obtained at Ni/C
electrode. Fig. 5 shows the behavior of the electrochemical oxidation of different electrodes containing
different Cr2O3 contents in 1.0 M NaOH and 2.0 M.
Notably, as the amount of Cr2O3 in the prepared
electrode increases the oxidation peak current density
of ethanol increases up to 7Vf % and then it decreases
at 10Vf % Cr2O3 as the Ni particles may aggregate at
high content of Cr2O3. So, the best result regarding the
highest catalytic activity and the highest oxidation
peak current density is obtained with Ni-Cr2O3/C
(7Vf %) [327 mA cm-2 at 775 mV] compared with Ni/C
[179mAcm-2 at 738 mV] or the other Ni-Cr2O3/C
electrodes.
containing 0.05 M glucose (Fig. 7). Also, its stability

with time is better than that of Cu/C electrode. The
proposed composite electrode has reasonable
sensitivity and selectivity towards glucose electrooxidation. Owing to its safe and simple fabrication
technique, it is recommended to be used for the
development of enzyme-free glucose sensors.
1 g L-1 CuO
3 g L-1
5 g L-1
10 g L-1
60
I / mA cm-2
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30
-30
-600
-300
300
600
900
1200
E / mV (MMO)
120
1 g L-1 CuO
3 g L-1
5 g L-1
10 g L-1
I / mA cm-2
90
60
30
0
-30
d
-600
-300
300
600
900
1200
E / m V (MMO)
FIG. 7 CYCLIC VOLTAMMOGRAMS OF ELECTRODEPOSITED
CUCUO/C CONTAINING DIFFERENT AMOUNT OF CUO IN
THE DEPOSITION ELECTROLYTE AT A SCAN RATE OF 50
MV S-1 IN: A) 0.25 M NAOH AND B) 0.25 M NAOH + 0.05 M
GLUCOSE ( HASSAN H. B., etal. 2011) .
FIG. 6 SEM IMAGES OF Cu AND CuCuO FILMS
DEPOSITED FROM A NONCYANIDE ALKALINE
ELECTROLYTE AT 25 C, 4 A dm2, 35 g L1 MANNITOL
CONCENTRATION AND CONTAINING DIFFERENT CuO
CONTENTS ( HASSAN H. B., etal. 2011).
Additionally, Z. Abdel Hamid group have been

successfully fabricated CuCuO composite films on
carbon electrodes via an electrodeposition route from
an environmentally safe alkaline electrolyte containing
manntiol as a complexing agent (Hassan H. B., etal.
2011). The study proved that the presence of CuO
reduces the Cu grain from 24.3 to 11.2 nm as shown in
Fig. 6. The electrochemical studies revealed that the
performance of CuCuO/C composite electrode
towards glucose electrooxidation is superior to that of
electrodeposited Cu/C electrode in alkaline solution
32
FIG. 8. SEM IMAGES OF A NI-MWCNT COMPOSITE FILM

UNDER: (A) LOW MAGNIFICATION AND (B) HIGH
MAGNIFICATION (Susumu A., etal. 2008).
The Japanese team has fabricated multiwalled carbon

nanotube (MWCNT) composite films by an electrodeposition technique (Susumu A., etal. 2008), and
proved that MWCNTs distributed homogeneously
across the surface of the film and tightly incorporated
within the deposited Ni (Fig. 8a & b).

Electroless Technique
Due to the success of composite electrodeposits
fabrication, similar technology was applied to
electroless deposits in the late 1960s in Germany, and
the Netherlands and the USA in the early 1970s. Then,
successful co-deposition of ultra-fine particles such as
metallic powder, carbides, oxides, diamond and
polymers with metal or alloy matrix have been
reported by (Gui Y. L., etal. 1993) who used an
intermediate layer containing nely divided Al 2O3 and
PVC particles distributed within a metallic matrix.
This intermediate layer was deposited using the
electroless coating technique. Electroless coating
technology is credited mainly to Brenner & Riddell
(Brenner A., etal. 1946). By the controlled chemical
reduction reaction, the electroless coating chemistry
has emerged as one of the leading growth areas in
surface engineering and metal
nishing etc. In this
technique, the composite coatings are produced by codeposition of fine inert particles into a metal matrix
from an electroless bath. The excellent wear resistance
of electroless nickel can be further enhanced by
codepositing hard particulate matter with the nickelphosphorus alloy.
In the recent years, electronics and electrical
engineering have faced the problem how to coat
dielectrics (glasses, ceramics, polymers), semiconductors and metals difficult to be coated (aluminum and
magnesium alloys, titanium, tungsten, molybdenum,
etc.). Electroless plating on aluminum and many of its
alloys is applied with a view to improve the surface
hardness, corrosion protection as well to provide
possible welding. Many authors have dealt with the
electroless nickel on aluminum due to the relatively
low price of aluminum and its alloys. Abdel Hamid
Z.etal. have been investigated electroless nickel
phosphorous composite containing, ZrO2, TiO2, and
Al2O3 on 6061 Al alloy from acidic bath as seen in Fig.
9 (Abdel Hamid Z. et al. 2002). Fig.9 shows the
microstructure of as-cast 6061 Al alloy and the
distribution of the different particles on the surface of
composite coatings. It reveals a very high volume
percent of Al2O3 particles in the deposit if compared
with another two reinforced particles. The mechanism
of incorporation of reinforced particles was suggested
and confirmed in view of zeta potential and the
calculated free energy of adsorption of the particles
( Gads) of the composites. The effect of different
composites on the mechanical properties of the deposit
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such as hardness and wear resistance illustrated that

the reinforced particles as well as the heat treatment
provide satisfactory improvement in hardness (Fig. 10)
and wear resistance of the deposits.
FIG. 9. THE MICROSTRUCTURE OF 6061 Al ALLOY AND THE

DISTRIBUTION OF THE DIFFERENT REINFORCEMENT
PARTICLES ON THE SURFACE OF COMPOSITE COATINGS.
(A) Al 6061, (B) Ni P, (C) NiPTiO2, (D) NiPZrO2, (E) NiP
Al2O3 (Abdel Hamid Z. et al. 2002)
FIG. 10 THE RELATION BETWEEN THE DIFFERENT TYPES OF

COMPOSITE COATING AND MICROHARDNESS (ABDEL
HAMID Z. et al. 2002).
Additionally, the incorporation of WC with Ni-P

alloys has been investigated by Z. Abdel Hamid et al.
(Abdel Hamid Z., etal. 2007). The influence of plating
parameters such as WC content, pH, temperature and
stirring rate on the content of WC codeposited with
NiP alloys were investigated. The maximum value of
WC (5055 Vf%) codeposited can be achieved at a
particle content of 20 gL1 in the electrolyte, at pH 5.5
6, temperature 8590C and stirring rate of 150 rpm as
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shown in Fig. 11. SEM and X-ray diffraction revealed

that the phase structure of the solid solution cannot be
varied by codeposition of WC particles in NiPalloys,
and it only influences the growth of the crystal planes.
such as tips for earth moving equipments, molds,

cutting tools and engine parts (Guo Z., etal. 2003).
The applications of electroless Ni-P alloy coating in
engineering could be especially promising; if one
notices that the coating can be deposited on any
irregularly shaped surfaces and on many substrates
including nonconductors. The Ni-P-CB (carbon black)
nanocomposite coatings have been successfully deposited
on an ABS plastic matrix via electroless plating process
for the development of infrared detecting technologies
and low infrared-emissivity materials (Xiangxuan L.,
etal. 2010 ). Fig. 13 shows surface morphology of the
NiP and NiPCB composite coatings. It reveals the
presence of the CB in the NiP layer affects the
heterogeneity of the surface and increases the number
of boundaries between Ni and other particles in the
matrix. The incroporated CB grains into the
amorphous matrix distinctly enlarge the surface
development of the composite NiPCB layer.
FIG. 11 SURFACE MORPHOLOGY OF NIP WITH, A)

WC FREE, B) +5 gl1 WC, C) +10 gl1 WC, D) +15 gl1 WC,
AND E) +20 gl1 WC (ABDEL HAMID Z., etal. 2007).
Abdel Aal et al. prepared novel NiP composite

coatings containing (TiCAl2O3) powder synthesized
by self-propagation high temperature synthesis (SHS)
(Fig. 12) on steel substrate using electroless plating
technique (Abdel Aal A.,etal. 2007). Incorporation of
(TiCAl2O3) particles in deposited coating significantly
improves the corrosion resistance, wear resistance and
increases the hardness of deposited layer.
FIG. 13 SURFACE MICROGRAPHS OF THE (A) NiP AND (B) Ni

PCB COMPOSITE COATINGS (XIANGXUAN L., etal. 2010 ).
Mechanism of Nanocomposite Coating
FIG. 12 SEM MORPHOLOGY OF THE PREPARED (TiC

Al2O3) POWDER (Abdel Aal A.,etal. 2007).
The precise nature of the process of codeposition and

the arrival to the cathode of the solid particle was
subject to controversy. Within the last 50 years, many
theoretical models have been proposed to explain the
mechanism used to produce nanocomposite coatings
where nano-sized particles are suspended in the
electrolyte and co-deposited with the metal. Three
main mechanisms were previously suggested (Celis
J.P., etal. 1991 ) to explain the difference in the ability
to deposit various types of solid particles:
electrophoresis, mechanical entrapment and physical
adsorption.
The incorporation of nano sized particles within Ni-P

autocatalytic coatings greatly enhanced mechanical
properties and corrosion resistance relative to the pure
metal. In some cases, embedding particles in
electroless deposited metals added entirely new
features to the coatings performance, which widened
their use in different industries from high technology,
The first theoretical model was suggested by

Guglielmi where the co-deposition has usually been
explained based on adsorption of metal ions on the
particles (Guglielmi N., 1972). He reported that
electrophoretic attraction is the driving force behind
the entrapment of particulates in the growing film and
proposed a mechanism of two adsorption steps, a) a
34
loose adsorption, which is physical in nature and b) A

strong adsorption step that takes into account the
electrochemical nature of the process. The physical
adsorption step (a) was described by a Langmuir
isotherm similar to the approach of adsorption ions.
Accordingly, the surface coverage of the particles is a
function of their concentration in solution. The strong
adsorption step (b) is similar to a Tafel kinetic
expression and also includes a term for the loose
adsorption. In this step, the particles are irreversibly
adsorbed where Faradays law and a kinetic expression
for the current described the volume fraction of the
deposited metal. Celis et al. (Celis J., etal. 1977 and
Celis J., etal. 1987) verified the validity of the model
for the deposition of Cu-Al2O3 coating and proposed
an improvement over the Guglelmi model based on a
statistical approach. They postulated a five-step
adsorption process (Fig. 14). a) An adsorbed double
layer of cations forms around each particle in the bulk
of the solution. b) The particles are transferred by bulk
convection to the boundary layer. c) The particles
diffuse through the boundary layer to reach the
surface of the cathode. d) At the cathode, the adsorbed
electroactive cations are reduced. e) When a fraction of
the ions originally adsorbed on a particle are reduced,
the particle is captured by the growing film.
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An improvement of Guglielmi's model was postulated

by Saher Shawki et al. (Shawki S. etal. 1997). They
thought that the inclusion of solid particles depends
largely on their mobility and electrokinetic nature in
the plating solution. The described mechanism has
been designed to elucidate the aspect of the deposition
process on the basis of the electrokinetic mechanism.
Solid particles in solutions are electrolytically charged
by adsorbing ions on their surfaces. The sign and
magnitude of the electrolytic charge is known as zeta
potential (). The values of zeta potential for different
particles were determined in dilute solution at pH of
the plating solution containing all the plating species.
The mechanism of solid particle electrodeposition
could be suggested as follows: positively charged Ni
ions in solution are adsorbed on negatively charged
solid particles. The particle with adsorbed ions
migrates to the cathode where metal ions are reduced
to Ni atoms forming the coating with the entrapped
solid particle occupying a place in the metal (or alloy)
matrix. A schematic diagram illustrating the
mechanism is shown in Figure 15.
FIG. 15 SCHEMATIC DIAGRAM OF THE MECHANISM OF SOLID

PARTICLE MOBILITY IN THE PLATING ELECTROLYTE (Shawki
S. etal. 1997).
The higher magnitude of the charge on the particle

lead to decreasing the amount deposited in the coating.
This can be explained on the basis of the following
assumptions: - Particle/ion mobility: with high
potential, a greater number of Ni ions are adsorbed on
the surface of the solid particle. The aggregates of Ni
ions surrounding a particle behave as one large
charged body suspended in the electrolyte. The
mobility of the later formation is, therefore, expected
to decrease under the heavy weight of the coupled
formation. The result will be a smaller number of solid
particles reaching the cathode.
FIG. 14 THE MODEL FOR THE DEPOSITION OF Cu-Al2O3
COATING DESCRIED BY CELIS ET AL(Celis J., etal. 1977 and Celis
J., etal. 1987).
- Relative amount occluded: since Ni ions:

surrounding each particle are immediately reduced to
Ni atoms at the cathode surface, the relative amount of
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particles of high potential (quartz, sand)

incorporated in the coating will be less than the
amount of particles of lower potential (SiC, Al2O3). In
solution, the later type of particles is surrounded by
fewer Ni ions; the result is high content of particles in
the coating (Shawki S. etal. 1997). Kuo et al. explained
the co-deposition process basssed on that a particle
group could be embedded into the metal matrix when
the attraction force between the particle group and
electrode is stronger than the removing force (due to
agitation) on the electrode (Kuo S., etal. 2004).
Factors Influencing Nanocomposite Coatings
Several factors influence the incorporation of hard and
soft particles in a matrix including, particle size and
shape, particle charge (zeta potential), the
concentration of the particles in the plating solution,
the method and degree of agitation beside operating
conditions of plating process (such as temperature,
current density, pH,etc). The below topics discuss in
details the influence of these parameters on the
incorporation rate and hence the structure, the
morphology and the properties of the coatings.
Effect of Particles Size and Shape
The size of the particles has a definite impact on their
incorporation in the matrix. In general, it is
recommended that particles size have enough size to
settle in the solution yet not so large as to make the
deposit rough or make it difficult for them to be held
in suspension. Also, the size of the particles should be
selected with reference to the thickness of the
electrodeposition, as attempts made to incorporate 10
m size particles in a 7 m thickness deposit resulted
in unsatisfactory deposit and incorporation of 10 m
size particles even in 25 m thickness deposit
physically weakened the deposit (Shreir L.L., 1955). It
is suggested that particles in the size range of 2-7 m
might be suitable for codeposition in a matrix.
Particle shape also plays a vital role in determining
their incorporation level. It is generally believed that
angular shaped particles will have a greater tendency
to hold on to the surface upon impingement than
round one. However, Apachilei etal. showed that
spherical shaped alumina particles resulted in better
incorporation than irregular ones (Apachilei I., et.al.,
1998). The difference in particle shape also has a
bearing on the type of finish of the deposit. Very
smooth and rough surface were obtained from small
rounded particles and large angular particles,
respectively.
36
Our group at CMRDI studied the effect of particle

shape (spherical or rods) (Abdel Aal A., etal. 2009).
The study proved that the shape of particle affects not
only the co-deposited powder fraction, but also the
morphology of coatings. Figure 16 exhibits the SEM
morphology of the Ni-W-P-SiC nanocomposite coating
electrodeposited from the plating bath containing 5 g/l
of rod and spherical shaped SiC powder. It can be seen
that SiC nano-rods disperse uniformly and
homogeneously and the content of particles is at high
level compared with the spherical shaped (Abdel Aal
A., etal. 2009).
FIG. 16 SEM IMAGES OF NI-W-P COATING CONTAINING:

(A) ROD SiC AND (B) SPHERICAL SiC (Abdel Aal A., etal.
2009).
Effect of Concentration of the Dispersed Particles

Concentration of the dispersed particles in the
electrolyte bath also plays a major role in influencing
the incorporation level. Incorporation of Al2O3, TiO2
etc particles in nickel electroplating or electroless
matrix was studied by many authors (Susumu A.,elal.
2008, Ik-Hyun O. etal. 2005, Chen W., etal. 2010,
Zieliska K., etal. 2012, Dong D., etal. 2009, Vaezi M.R.,
etal. 2008, and Mohajeri S., etal. 2011). They found
that the incorporation of particles increase with
increase in their concentration in the bath up to critical
concentration. With further additions, the particles
incorporation decreased, as the particles appeared to
agglomerate in the bath and decreasing trend was
observed as shown in Fig. 17,18 and 19. This is in a
good agreement with the Guglielmi's model, where
the concentration of powder (C) and its embedded
fraction () are related mathematically by following
quation:
C
=
e
Mi0
1
exp( A B) + C
nF m v0
k
where M is the atomic weight of the electrodeposited

metal, i0 the exchanging current density, n the valence
of the electrodeposited metal, F the Faraday constant,
m the density of electrodeposited metal, the
overpotential of electrode reaction, i= i0 exp (A) and k
the Langmuir isotherm constant, mainly determined
by the intensity of interaction between particles and
cathode. The parameters 0 and B are related to

particle deposition, and both play a symmetrical role
with the parameters i0 and A related to metal
deposition. The constants A and B can be seen as the
total charge passing through the electrode interface
and carried by Ni2+ ions and charged particles during
the reaction.
FIG. 17 THE VARIATION OF EMBEDDED WC IN THE MATRIX

WITH DIFFERENT WC CONTENTS IN THE ELECTROLYTES
(Susumu A., elal. 2008).
FIG. 18 DEPENDENCE OF Cr2O3 VF% IN THE DEPOSIT ON ITS

CONTENT IN THE PLATING SOLUTION OPERATED AT 50 mA
Cm-2, 150 rpm, pH 5 AND 55 C (Hassan H. B.,etal. 2011).
Powder content in deposit, wt.%
40
AlN
30
20
TiO2
10
-10
10
20
30
40
50
60
70
80
Powder content in plating bath, g/l
FIG. 19 THE VARIATION OF EMBEDDED FRACTION WITH

NANO POWDER CONTENT FOR AlN (Abdel Aal A., etal. 2006)
AND TiO2 (Abdel Aal A. , 2008)
Effect Agitation
Agitation of the plating solution is also a key factor in
determining particle incorporation. Various methods
of agitation employed include circulation by pumping,
purging, of air, ultrasonic agitation, and the plate-
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pumper technique. In general, if the agitation is too

slow (laminar flow), the particles in the bath may not
disperse completely, except when their density is low.
On the other hand, if the agitation is too high
(turbulent), particles will not have sufficient time to
get attached to the surface, and this results in poor
particles incorporation. Kalantary et.al. have
suggested that the laminar-turbulent transition region
is the most effective agitation condition to maximize
incorporation of particles in electroless composite
coatings (Kalantary M. R., et.al. 1993). Mechanical
agitation resulted in lesser incorporation due to the
directional flow in the bath. Although agitation by
nitrogen avoids the directional flow, it does not help
decrease the extent of aggregation of nano-sized
diamond particles in the bath.
Effect of Additives
Besides the above factors, some special additives such
as surfactants, play a major role in deciding the
incorporation of second phase particles. These
additives are especially important in the incorporation
of hard and soft particles like polytertra
fluoroethylene
(PTFE),
graphite,
molybdenum
disulphite (MoS2) and SiC. Kunugi Y. et.al. have
suggested that though surfactant additives enable a
higher level of incorporation of PTFE particles
(Kunugi Y. et.al. 1990). Abdel Hamid et. al. have used
a Zwitterionic Surfactant to increase the incorporation
of PTFE with nickel matrix (Abdel Hamid Z. etal. 2003
and Shawki S. etal. 1997), and sodium silicate to
increase the incorporation of SiC and Al2O3 in nickel
matrix deposited by electroplating process. Wu Y. et.al.
have suggested that an electroplating additive
Na3Co(NO2)6 can promote the codeposition of the SiC
particles, but the Al2O3 and ZrO2 particles can form
composite layers without the assistance of the additive
(Wu Y, et.al., 2003).
Rudnik E., et.al. studied electrodeposition of SiC
particles with nickel matrix in the presence of cationic
surfactant cetyltrimethylammonium bromide (CTAB)
(Rudnik E., et.al. 2010), and proved that SiC
incorporation into the composite coating increased
with increasing surfactant concentration in the bath.
Cationic surfactant inhibited adsorption of cations
(Ni2+) and enhanced adsorption of anions (Br) on the
positive charged carbide surface, but Br/Ni2+ molar
ratios for adsorbed ions were higher than in the bath.
It was attributed to the CTAB adsorption realized
predominantly by hydrophobic interactions between
aliphatic chain of the molecule and SiC surface with
37
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the positive head group of CTA+ pointed toward the

bulk solution. Amadeh A. etal. studied the effect of
sodium saccharin and sodium dodecyl sulfate
additives on the amount of incorporated WC with Cr
electrodeposition (Amadeh A., etal. 2012).
Effect of Electrolyte pH and Particle Charge
The pH value of the electrolyte plays an important role
in the co-deposition process. pH is counted as the
most effective parameters on zeta potential () of the
powders. Many chemically simple surfaces, such as a
SiC dispersed in a dilute salt solution, showed a
common pattern when the pH is varied. For the
deposition of Ni-Cr2O3 composite coating at different
pH values, Hassan H. B., Z. et al. (Hassan H. B., Z. et
al. 2011) found that the Vf % of Cr2O3 increases as
increasing pH values and attains the greatest value at
pH 5-6 (Fig. 20). With further increasing pH larger
than 6, the Vf % of Cr2O3 in the deposited layer
decreases due to the formation of nickel hydroxide in
alkaline medium, which leads to decreasing the
deposition rate and consequently decreasing the Vf %
of Cr2O3. The deposition behavior of Cr2O3 with pH
can be explained by an electrophoresis phenomenon
due to the formation of an ionic cloud around the
Cr2O3 particles. Electrophoresis is the induced motion
of colloidal particles or molecules suspended in ionic
solutions that result from the application of an electric
field. The electrophoretic velocity is a function of the
etectrostatic forces on the surface charge, the
electrostatic forces on their electric double layers, and
the viscous drag associated with both the motion of
the colloidal particles as well as the motion of the ionic
cloud the colloidal particles. The sign and magnitude
of the electrolytic charge is known as zeta potential ().
60
10
the amount of embedded reinforcements. Direct

current (DC) electrodeposition methods are commonly
used for fabrication of metallic as well as composite
coatings. The DC electrodeposition methods are often
associated with slower deposition rates and coating
defects such as surface roughness, porosity, poor
adhesion, undesirable microstructure, etc. Recently,
pulse current (PC) and pulse reverse current (PRC)
electrodeposition methods have attracted significant
attention to improve deposition rates and microstructure of the coatings for better mechanical and
corrosion properties (Aperador Chaparro W.A., etal.
2007 and Balasubramanian A., etal. 2009). The effect of
current density on the volume percent of the PE
(polyethylene) in the Ni matrix has been studied by
Abdel Hamid Z. et al. (Abdel Hamid Z., etal. 2002).
The data indicated that the volume percent of the PE
increased with increasing current density up to 7.5
Adm-2 as shown in Fig. 21. With further increase in the
current density, the extent of codeposition of PE
decreases.
FIG. 21 EFFECT OF CURRENT DENSITY ON THE VOLUME

PERCENT OF PE IN THE DEPOSITS, THE DEPOSITION AT
PH 4, 50 C AND AT 10 gl-1 PE PARTICLES IN THE BATH.
(Abdel Hamid Z., etal. 2002).
50
Zeta potential, mV
Vf of Cr2O3
40
30
20
-10
-20
-30
10
0
2
pH
-40
2
10
pH
FIG.20. RELATIONSHIP BETWEEN PH OF THE

ELECTROLYTE AND A) VF% OF Cr2O3 IN THE DEPOSITED
LAYERS, B) ZETA-POTENTIAL OF Cr2O3 PARTICLES (THE
COATING PROCESS OPERATED AT 50 C, 150 rpm, 7Adm-2
AND 20 gl-1 Cr2O3) (Hassan H. B., Z. et al. 2011).
Effect of Current Density

Current density of the plating solution plays an
important role in the electrodeposition process beside
38
FIG. 22 EFFECT OF CURRENT DENSITY ON WT.% OF Co

DEPOSITED Si3N4 (Abdel Aal A., etal. 2006).
Additionally, Krishnaveni et al. found that content of
nano Si3N4 particles increases into Ni-B matrix with

increase in current density and reaches a maximum at
1 A/dm2 (Fig. 22), beyond which it decreases
(Krishnaveni K., etal. 2008). The observed trend is in
agreement with our results in the deposition of ZnZnO-TiO2 (Fig. 23) and Ni-SiC nanocomposite (Abdel
Aal A., etal. 2006) (Fig. 24).
FIG. 23. EFFECT OF CURRENT DENSITY ON WT.% OF CoDEPOSITED TiO2 (Abdel Aal A., etal. 2006).
www.me-journal.org
incorporation (Guglielmi N., 1972). At high current

densities, Ni ions are transported faster than the
second phase particles which are transported by the
mechanical agitation. Hence, the co-deposition of
second phase particles becomes particle-transfer
controlled.
In recent years, many researchers have applied pulse
current (PC) instead of direct current (DC) electrodeposition methods for the preparation of composite
coatings. Gyftou group proved that specific selection
of the pulse current parameters results in the
production of composite Ni-SiC electrodeposits with
better and predefined properties, higher incorporation
percentages and more uniform distribution of the
particles in the metallic matrix than those attained by
direct current techniques (Gyftou P., etal. 2005).
Similar findings were obtained by Steinbach and
Ferkel during the preparation of Ni-Al2O3 by PC and
DC electrodeposition methods (Steinbach J., etal. 2001).
They reported that nanocrystalline Ni-Al2O3 composite
coatings can be produced by PC electrodeposition. In
contrast to Ni-Al2O3 composite coatings prepared by
DC electrodeposition, Al2O3 nano-particles embedded
in the nanocrystalline Ni-Al2O3 composite coatings are
less agglomerated and a particle size selection of the
co-deposited nanoparticles during PC plating takes
place.
Characterization and Application of Nanocomposite Coatings
FIG. 24. EFFECT OF CURRENT

DENSITY ON VOLUME FRACTION
OF SiC CONTENT IN THE
DEPOSITED LAYER (Abdel Aal A.,
etal. 2006).
The explanations of this behavior based on adsorption

of ions on the particles, activation and diffusion
control of metal deposition, point of zero charge of the
particle and fluid flow resistance of the particles have
been suggested. Hwang and Hwang have suggested
that at low current densities, the particle co-deposition
rates are determined mainly by the reduction of
adsorbed H+ ion on the particle whereas at high
current densities, reduction of both the metal ions as
well as the H+ ions becomes important in determining
the co-deposition rate of the particle (Hwang B., etal.
1993). Yeh and Wan (Yeh H., etal. 1997) have reported
that at low current densities co-deposition of second
phase particles in Ni matrix follows Guglielmis twostep adsorption model and results in a higher level of
Due to their enhanced hardness, wear resistance and

corrosion resistance when compared to pure metal or
alloy, nanocomposites generally exhibited wide
engineering applications in different fields. The
amount of incorporated particles is the key parameter
for the success of metal matrix composite applications,
since it largely determines the composite properties
such as wear resistance, corrosion resistance, and
hardness when compared with the corresponding
values for pure metal or alloys deposits (LozanoMorales A., etal. 2004). Furthermore, the co-deposition
of a sufficient amount of non-agglomerated particles
should lead to production of harder and more
resistant coatings (Zanella C., etal. 2009). Particlereinforced composite coatings based on nickel and
alumina are applied in different technological fields
with high demands on friction and corrosion
resistance (Jung A., etal. 2009). Lekka et al. showed
that the co-deposition of SiC nanoparticles leads to a
more noticeable grain refinement and, as a
consequence, the nanocomposite deposits present a
39
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very high microhardness, 61% higher than pure

copper deposits, and an increase of 58% of the
abrasion resistance (Lekka M., etal. 2009). Future
applications of these materials depend on the ability to
produce them with controlled composition and
properties, using inexpensive and reliable techniques.
Ali Eltoum M.S.et al. proved that the incorporation of
titania nanoparticles with Ni matrix obviously affects
the surface morphology of the coatings, as shown in
Fig. 25 (Ali Eltoum M.S., etal.). The titania particles
appear as light spots in the darker nickel
matrix. Because of the addition of TiO2 nanoparticles
to the bath, the microstructure of the nickel matrix
changed from spherical (Fig. 25a) to granular (Fig. 25b).
FIG. 25. SEM OF ELECTRODEPOSITED NI-TiO2

COMPOSITE WHERE, A) PURE NI, AND B) NI-NANO
TIO2 DEPOSITED FROM BATH CONTAINING 0.2 M
NiSO4, 0.2 M C6H11NaO7, 0.4 M BORIC ACID OPERATED
AT 25 C , 2.5 Adm-2,AND pH 8 25 (Ali Eltoum M.S., etal.)
L. Yan et al. fabricated Ni-SiO2 nano-composite

coatings by electrodeposition technique on the
AZ91HP magnesium alloy surface (Yan L., etal. 2011).
They proved that the Ni-SiO2 nano-composite coatings
with uniform crystalline, dense structure can be
obtained on AZ91HP magnesium alloy with high wear
resistance compared to magnesium alloys and pure
nickel coatings.
Wang et al. proved the remarkable increase in the
hardness of Ni-ZrO2 composite coatings compared to
pure Ni which was attributed to the combination of
Hall-Petch strengthening and Orowan strengthening
(Wang W., etal. 2005). While Xu R. et al. attributed the
higher hardness of Ni-W-P-SiO2, Ni-W-P-CeO2 and NiW-P- SiO2-CeO2 nanocomposite coatings to the
formation of hard Ni3P phase ( Xu R., etal. 2008). Qu et
al. reported that the existence of nano-sized CeO2
particles, as the second phase, reduces the grain size of
Ni matrix. Accordingly, the higher microhardness
value of the nanocomposites may be due to the
incorporation of reinforcement particles and the
decrease of the grain size of Ni matrix of the
composites (Qu N. et al., 2004). Yang Y. et al. have
40
been successfully synthesized NiPZrO2 using

electroless method (Yang Y. et al. 2011). They proved
that the microhardness of nano-composite coating was
improved to1,045 HV200 compared to 619 of the NiP
coating.
Consequently,
the
coating
obtains
significantly improved wear resistance. Additionally,
our group in CMRDI proved that the nano composite
coatings are characterized by lower corrosion rate and
corrosion current density compared to the conversion
coating by electroless or electroplating technique.
Recently, Ni nanocomposite coatings have gained a
significant interest as anodes for fuel cell applications
(Abdel Aal A., etal. 2009, Abdel Aal A., etal. 2008, and
Sattarahmady N., etal. 2010). Fuel cells are an
important technology for a potentially wide variety of
applications including micro power, auxiliary power,
transportation power, stationary power for buildings
and other distributed generation applications, and
central power. They were prepared by incorporating
of nano-sized metal oxide particles such as TiO2, ZnO
or Al2O3 into the Ni matrix by electroless or electrodeposition technique. photocatalytic applications
using oxides as TiO2 and ZnO have received much
attention to solve some environmental problems due
to the highest photocatalytic activity, being non-toxic,
stable in aqueous solution and relatively inexpensive
(Calza P., etal. 1997). Ni or its composite as a catalyst
was used for electrooxidation of small organic
molecules (Hassan H. B., etal. 2011, Hassan H. B., etal.
2011).
Conclusions
The results of this investigation suggest some general
conclusions, which can be summarized as follows:
- The plating parameters such as temperature, pH of
the plating solutions, stirring rate, concentration of the
reinforcement, and current density have effect on the
deposition.
- The inclusion of solid particles depends on their
electrokinetic nature (zeta potential, ) of the
reinforcementsin the plating solution.
- The incorporation of reinforcements in the deposit
improves the microhardness, the wear as well as the
corrosion resistance of the deposit.
- The hardness of nanocomposite coating depends
directly on the Vf% of nano reinforcement.
-Nanocomposite coatings have gained a signi
cant
interest as anodes for fuel cell applications.
- Composite and nanocomposite electrodes have

catalytic activity towards electrooxidation of glucose
in alkaline medium.
- Composite and nanocomposite electrodes enhance
catalytic activity and stability towards electrooxidation
of the alcohol compared with conventional electrodes
used.
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Journal of Metallurgical Engineering (ME) Volume 3 Issue 1, January 2014