Surface & Coatings Technology 200 (2006) 3933 – 3941

www.elsevier.com/locate/surfcoat

Influence of particle size on the microstructure, hardness and corrosion

resistance of electroless Ni–P–Al2O3 composite coatings
J.N. Balarajua,*, Kalavatib, K.S. Rajama
a
Surface Engineering Division, National Aerospace Laboratories, Post Bag No. 1779, Bangalore 560 017, India
b
Materials Science Division, National Aerospace Laboratories, Post Bag No. 1779, Bangalore 560 017, India

Received 24 September 2004; accepted in revised form 5 March 2005

Available online 26 April 2005

Abstract

High phosphorus electroless nickel bath has been used to prepare composite coatings containing alumina powders (50 nm, 0.3 Am and 1.0
Am). Deposits were characterized for its structure, morphology and hardness. Incorporation of particle has a marginal influence on the
composition. More amount of particle incorporation and uniform distribution was found in composite coatings obtained with 1.0-Am (C3)
alumina particles compared to 50-nm (C1) and 0.3-Am (C2) alumina particles. XRD results showed a broad peak of nickel and low intensity
alumina peaks present in C3 composite coating in as-plated condition. A marginal improvement in hardness was noticed in as-plated
composite coatings. A 15% increase in microhardness was observed in the heat-treated (400 -C for 1 h) composite coatings. Potentiodynamic
polarization measurements made on these deposits in 3.5% sodium chloride solution showed that uniform corrosion occurred in C1 and C2
composite coatings whereas localized corrosion was observed in C3 composite coating.
D 2005 Elsevier B.V. All rights reserved.

Keywords: Electroless Ni – P; Composite; Alumina; Hardness; Corrosion resistance

1. Introduction CeO2, TiO2 [5], Al2O3 [6] and PTFE [7] and the particles
used are of the micron size. Codeposition of the particles
Autocatalytically deposited Ni – P amorphous alloys depends on the size, shape, density, concentration and
have many industrial applications because of their para- method of suspension in the bath. In addition, it is very
magnetic properties, excellent resistance to wear and much dependent on the charge present on the particle.
corrosion, and high hardness. Codepositing another metal- Electroless plating of NiP on TiO2 powders with the size
lic or non-metallic elements or abrasive/lubricative par- about 10 nm has been reported [8]. Nanodispersed SiO2,
ticles or combination of them in binary Ni –P matrix can CeO2 [9] and Zn3(PO4)2, ZnSnO3, and ZnSiO3 [10]
further enhance these properties. Recently, electroless particles were codeposited in nickel phosphorus matrix
nickel composite coatings have gained more attention in and corrosion and tarnish resistance properties were
research community due to their ability to produce discussed. Electroless Ni – P with nanometer diamond
coatings that posses improved wear, abrasion and lubrica- particle composite coatings was prepared and the codepo-
tion properties than Ni – P deposits. Several particles have sition mechanism was explained [11]. Recently carbon
been incorporated in the nickel matrix, and among them, nanotubes (CNT) were codeposited in Ni– P matrix and
the combinations that have received considerable attention their tribological properties were evaluated [12]. Nano-
are electroless nickel with SiC [1], B4C [2], Si3N4 [3,4], meter-size Al2O3 particle-reinforced Ni – P matrix compo-
sites were prepared and were characterized [13]. Aim of
the present investigation is to study the particle size effect
* Corresponding author. Tel.: +91 80 2508 6247; fax: +91 80 2521 0113. on the deposit properties. Hence, in this study, using
E-mail address: [email protected] (J.N. Balaraju). alumina powders of sizes 50 nm, 0.3 Am and 1.0 Am, Ni –
0257-8972/$ - see front matter D 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2005.03.007
3934 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941

Table 1 Magnetic stirrer (Remi make) was used to get uniform

Composition of as-plated electroless Ni – P and composite coatings suspension of particles in the solution. About 400 mL of
determined by EDX analysisa
solution containing alumina particles taken in a 500 ml
Type of coating Ni (wt.%) P (wt.%)
glass beaker were stirred for more than 12 h on a magnetic
Ni – P 90.1 9.9 stirrer using a PTFE coated magnetic paddle to get better
Ni – P – Al2O3 (50 nm) 91.8 8.2
wettability of the particles. Using a band heater electroless
Ni – P – Al2O3 (0.3 Am) 91.9 8.1
Ni – P – Al2O3 (1.0 Am) 92.2 7.8 solution was heated up to 85 T 2 -C. The obtained
a
Only Ni and P (100%) were considered.
deposition rate was in the order of 11 – 13 Am/h. All the
specimens were plated for 2 h except the specimens used
for corrosion studies, which were plated for 1-h duration
P composites were prepared and their surface morphology, only. After plating, the specimens were taken out then
structure and hardness properties were investigated. thoroughly rinsed with deionized water and air dried at
room temperature. Then these specimens were used for
further characterization.
2. Experimental For studying the surfaces and cross-sections of deposits,
scanning electron microscope (Leo make, Model 440I) and
Mild steel specimens (2.5 cm  2.5 cm  0.08 cm) were optical microscope (Leica make, Model DMIRM) was used,
used for plating electroless NiP and nanocomposite coatings and the deposit composition was analyzed by EDX analysis.
containing alumina particles. Specimens were ultrasonically Alumina content (percent of area incorporation) in compo-
cleaned in acetone, cathodically cleaned in 10% sodium site coatings was evaluated by using two-dimensional image
hydroxide solution at 1 A/sq. inch for 5 min. Then analysis system (Leading Edge, Australia) and the thickness
specimens were thoroughly rinsed with deionized water of deposits was measured by weight gain basis method and
and immersed in 50 vol.% sulphuric acid solution for also further confirmed by metallographic cross-sections of
deoxidization for 30 s. After deionized water rinse, speci- the deposits by optical microscope. Alumina content (wt.%)
mens were transferred immediately to the plating solution. present in the composite coatings was determined by
Electroless nickel bath was used for preparing the Ni – P dissolving the films in 1:1 nitric acid solution. Since
and composite coatings. Bath contains nickel sulphate 21 alumina particles were resistant to acid, it remains as such
g/L, sodium hypophosphite 24 g/L, lactic acid 25 g/L, and hence, particles were centrifuged at 2000 rpm (Remi
propionic acid 3 g/L and small amounts of lead nitrate and make). Acid solution was decanted and centrifuging was
operated at pH 4.7 – 4.9 and temperature 90 T 2 -C. repeated thrice with deionized water so that particles were
Alumina powders used were of the sizes 50 nm, 0.3 Am free from any metallic ions. Finally, wet particles were dried
(Buehler make) and 1.0 Am (Baikalox make). About 50 ml in an oven at 100 -C for more than 12 h. By knowing the
of electroless nickel solution containing 6 g/L of alumina weights of the composite films and alumina particles,
powder was thoroughly mixed using mortar and pestle. percentage incorporation of alumina was calculated. From

Fig. 1. SEM morphology of as-plated electroless composite coatings. (a) Ni – P, (b) C1 coating, (c) C2 coating, (d) C3 coating.
 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941 3935

Fig. 2. SEM morphology of as-plated electroless composite coatings. (a) Ni – P, (b) C1 coating, (c) C2 coating, (d) C3 coating.

the decanted solution, phosphorus and nickel content were heat-treated specimens under a 50-gf load. Average of five
estimated. X-ray diffraction (XRD) analysis was performed measurements was reported as a hardness value.
with a Rigaku D/max 2200 powder diffractometer using Cu Potentiodynamic polarization studies were made using an
Ka radiation to study structural changes in Ni –P – Al2O3 electrochemical system (Auto Lab PG Stat 30). This
composite coatings. instrument has T1 Amp as the current range at T30 V as
The isothermal heat treatment at 400 -C was used for 1 h the out put voltage. A three-electrode corrosion cell was
to improve the mechanical properties of Ni – P – Al2O3 used. The specimen to be tested was used as a working
deposits. The hardness of Ni –P and Ni – P– Al2O3 compo- electrode. A platinum rod was used as the counter electrode;
site coatings (C1, C2 and C3) was measured using Buehler the reference electrode was an Ag/AgCl (3M KCl) was
make microhardness tester with a Vickers diamond indenter. used. The electrolyte used was 3.5% sodium chloride
Hardness test was carried out on surface of as-plated and solution in nondeaerated conditions. The coated specimens

1 µm

Fig. 3. X-ray images of as-plated C1 composite coating.

3936 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941

were masked with lacquer so that only 1-cm2 area was phosphorus content was noticed for C1, C2 and C3
exposed to the electrolyte. Samples were degreased with composite coatings, i.e., 8.2, 8.1 and 7.8 wt.% respectively.
acetone, rinsed in deionized water before corrosion testing. Thus the chemical composition of the Ni– P matrix has not
Potentiodynamic polarization studies (Tafel plots) were been influenced much with the incorporation of alumina
carried out by polarizing the working electrode from the particles.
OCP to the extent of T200 mV at a scan rate of 1 mV/s. Alumina particles incorporated in the Ni –P matrix for
Current response was recorded and analyzed as Tafel plots. the C1, C2 and C3 composite coatings were found to be 2.4,
From the analysis of the result, i corr and E corr are obtained 3.7 and 8 wt.% respectively. In general, the incorporation of
from the software installed in the instrument. second phase particles in electroless Ni – P composite
coatings depends on two factors [14]. Particle impingement
on the electrode surface and holding time of the particle on
3. Results and discussion the electrode surface. Lower incorporation of 50-nm and
0.3-Am particles in C1 and C2 composite coatings can be
In general, electroless Ni – P coating structure and ascribed to the smaller size of the particles, which are
properties mainly depends on the amount of phosphorus (believed to be) swept away from the electrode surface
present in the deposit. Hence, EDX analysis has been compare to 1.0-Am size particles (C3). In literature, it has
carried out to see the effect of codeposition of alumina been reported that 12wt.% incorporation of nanoalumina
particles on the chemical composition of the coating. The particles was obtained after using a surfactant in Ni – P bath
chemical content of as-plated Ni– P and all composite with air agitation and also after the addition of 10 g/L
coatings is given in Table 1. A marginal variation in particles in the bath [13]. In the present work, we have

Fig. 4. Optical micrographs of cross-sections of as-plated electroless composite coatings. (a) Ni – P, (b) C1 coating, (c) C2 coating, (d) C3 coating, (e) SEM
micrograph of cross-section of C1 coating.
 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941 3937

obtained 8 wt.% incorporation of 1.0-Am particles without

using a surfactant and also only 6 g/L of particles in Ni –P
bath.
Fig. 1(a –d) exhibit the scanning electron micrographs of
the surface of the electroless Ni– P and C1, C2 and C3
coatings. It can be seen that surface of Ni – P coating is very
smooth, but the surfaces of the composite coatings are
coarser. There are many nodular protrusions over the
surfaces. These nodules are spherical in shape and composi-
tional analysis carried out on nodules showed that presence
of alumina particles apart from nickel and phosphorus. And
also it is evident from the micrographs that the alumina
particles are distributed throughout the surface although
agglomeration is seen in some places. More amount of
particle incorporation is seen in the case of C3 composite
coating. And also it has been observed that from micro-
graphs taken at higher magnification (Fig. 2), increasing the
particle size from 50 nm to 0.3 Am has reduced nodularity.
In the case of 1.0-Am composite coating no nodules are
seen. Fig. 3 gives the X-ray mapping of as deposited C1 Fig. 6. EDX spectra of as-plated C3 composite coating.
composite coating. From the X-ray images, it can be seen
that nickel and phosphorus are uniformly distributed in the in C1and C2 nanocomposite coatings even though presence
deposit whereas image of aluminium shows wherever the of alumina particles evident from the SEM, optical micro-
particle present in the deposit. graphs and gravimetric analysis. Fig. 5(b) gives the
However, to further analyze the distribution of these diffraction pattern for C3 composite coating. Apart from
particles through the thickness of the deposit, optical single broad peak, there are low intensity peaks present in
micrographs of the cross-section of these coatings [Fig. the diffraction pattern. Single broad peak corresponds to Ni
4(a – d)] were taken. It is obvious from the micrographs (111) plane at 45.3-. Low intensity peaks correspond to
that more uniform distribution and higher incorporation of alumina. Since the weight percent incorporation of alumina
particles throughout the thickness is seen in the case of present in C3 composite coating is about 8 wt.% hence, the
C3 coating compared to C1 and C2 composite coatings. peaks corresponding to alumina are detectable. Y.C. Wu et
More agglomeration of 50-nm particles can be seen from al. had also shown the presence of SiC peak in XRD pattern
the SEM image of cross-section of C1 composite coating of as deposited Ni –P-SiC composite coating [15]. The SiC
[Fig. 4(e)]. particle they have used is of 3 –5 Am and incorporation
XRD patterns of the C1and C3 coatings in as-plated obtained is about 6.8% and 11.6% in two different
condition are shown in Fig. 5. There is a single broad peak composite coatings. It can be concluded that incorporation
seen for as-plated C1 composite coating [Fig. 5(a)]. This of alumina particles in Ni – P matrix has not affected the
corresponds to Ni (111) plane at 44.66-. Grain size structure of the composite coatings. This is because that the
calculated using Debye– Scherrer formula is about 1.6 nm. structure of Ni – P alloys varies strongly from crystalline to
Diffraction peak correspond to alumina could not be traced
1400
Microhardness (Hv50gf )

1200
Ni 1000
(b) Al2O3
800
Intensity (a.u.)

600

400

200
(a)
0
Ni-P Ni-P C1 C1 C2 C2 C3 C3
20.000 40.000 60.000 Type of coating
2θ (deg) As-plated Heat-treated

Fig. 5. XRD pattern of as-plated composite coating. (a) C1 coating, (b) C3 Fig. 7. Effect of incorporation of alumina particles size on the microhard-
coating. ness of electroless Ni – P and composite coatings.
3938 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941

1.0x10-0 composite coatings. However, the increment in microhard-

1.0x10-1 1. Ni-P ness is only marginal from C1 to C3 composite coatings. In
2. C3
1.0x10-2 3. C2 the present investigation, we have shown that hardness can
1.0x10-3 4. C1
be improved by increasing the level of incorporation of
I \A.cm-2

1.0x10-4 particle in the deposit and annealing temperature.

1.0x10-5
Fig. 8 shows the electrochemical results obtained from
1.0x10-6
polarization studies for electroless Ni –P and composite
1.0x10-7
3 4 coatings in nondeaerated 3.5% sodium chloride solution.
1.0x10-8 2
1 Corrosion characteristics of electroless Ni – P and nano-
1.0x10-9
-0.600 -0.529 -0.457 -0.386 -0.314 -0.243 -0.171 -0.100 composite coatings are given in Table 2. All the deposits
E/Ag/AgCl (3M KCl) were around 11 Am in thickness.
Corrosion current density (i corrr) for electroless Ni – P
Fig. 8. Potentiodynamic polarization curves of electroless Ni – P and coating is 0.64 AA/cm2. Whereas i corr values for C1, C2 and
composite coatings.
C3 coatings are 0.96, 0.67 and 0.59 AA/cm2, respectively.
Even though corrosion current densities are within 1 AA/
amorphous phases with the content of phosphorus present in cm2 for all the coatings, but there is a large variation in R p
the deposit [16]. Fig. 6 gives EDX spectra for C3 composite values as seen from Table 2. It can be recalled from EDX
coating. From the spectra, the presence of alumina in the analysis of the coatings that the amount of phosphorus
composite coating is evident. Similar observation is also present in Ni –P and C1, C2 and C3 coatings are about 9.9,
noticed for C1 and C2 composite coatings. 8.2, 8.1 and 7.8 wt.%, respectively. However, all the
Microhardness values of electroless Ni – P and C1, C2 coatings showed relatively good resistance to corrosion in
and C3 composite coatings in as-plated condition are 551, sodium chloride solution. XRD patterns for all the coatings
595, 611 and 601 Hv respectively [Fig. 7]. It is clear from showed these coatings are amorphous in nature. In general,
the figure that a marginal increase in hardness has been corrosion resistance of any alloy depends on the speed of
observed in as-plated composite coatings compared to Ni – formation of a surface protective film apart from the amount
P coating. However, the increase in hardness was found to of phosphorus present in the deposit [17].
be more in the annealed coatings. Microhardness values in Within composite coatings, C1 composite shows lower
annealed (400 -C/1 h) condition are 926, 1155, 1173 and corrosion resistance compare to other two coatings. This can
1228 Hv for electroless Ni –P, C1, C2 and C3 coatings be attributed to the effective metallic area available for the
respectively. This increment in hardness is about 250 Hv corrosive medium to attack. However, there is not much
in the case of composite coatings. A marginal difference in difference in corrosion current densities is seen between C3
hardness is seen within composite coatings in both as- and C2 composite coatings even though the particle
plated and heat-treated conditions. The higher hardness incorporation is much higher in C3 coating. Hence, to
obtained for composite coatings is due to double strength- further analyze this aspect, all sample surfaces, after
ening effect from the dispersion strengthening of hard corrosion, were examined by SEM [Fig. 9(a – d)]. From
phase and precipitation strengthening of Ni– P alloy. It Fig. 9(a), it can be seen that bright white spots visible at the
shows that microhardness of annealed composite coatings center. EDX analysis of the white spot showed that it
depends on three factors namely level of incorporation, contains Ni, P, Fe, O and their element percentages are
annealing temperature and uniform distribution with less 65.14, 4.88, 10.84 and 19.14 respectively. Corroded surface
agglomeration. of C1 composite coating is shown in Fig. 9(b). Presence of
In fact, the percentage area incorporation, calculated alumina was found from EDX analysis of bright region
from image analysis, of 50-nm alumina particles in C1 whereas in the nodular region showed the presence of Ni, P,
composite coating is around 7% compared to 13% and 40% and alumina. However, in dark region, iron oxide is found
for 0.3- and 1.0-Am alumina particles in C2 and C3 along with other constituents. Iron oxide content in dark
composite coatings respectively. From this, it is evident region is less than 1 wt.%. Similar observations were made
that even though the level of incorporation is less in C1 in corroded surface of C2 composite coating. Corroded
coating, the higher hardness is in par with C2 and C3 surface of C3 composite coating showed the presence of

Table 2
Corrosion characteristics of as-plated electroless nickel and composite coatings in 3.5% sodium chloride solution
Type of coating Coating i corr E corr ba bc Rp
thickness (Am) (AA/cm2) (mV) (V/dec) (V/dec) (V cm2104)
Ni – P 11 0.640 325 0.079 0.103 2.387
Ni – P – Al2O3 (50 nm) 11 0.964 367 0.095 0.108 1.529
Ni – P – Al2O3 (0.3 Am) 11 0.670 369 0.100 0.087 2.538
Ni – P – Al2O3 (1.0 Am) 11 0.595 354 0.109 0.077 3.292
 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941 3939

Fig. 9. SEM morphology of corrosion tested electroless composite coatings in 3.5% NaCl solution. (a) Ni – P, (b) C1 coating, (c) C2 coating, (d) C3 coating.

Fig. 10. X-ray images of corroded C3 composite coating.

3940 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941

bright white region, cracked pattern and surrounded by gray polycrystalline materials because of the freedom from grain
region with bright spots [Fig. 9(d)]. Based on the or grain boundaries and because of the glassy film, which
observations made with corroded surfaces of C1 and C2 form on and passivate their surfaces. Hence, electroless Ni–
composite coatings, the bright region of C3 was expected to P coatings show better corrosion resistance compared to
correspond to alumina. However, the EDX analysis showed composite coatings [18]. When the particles are codepos-
that it contains iron content about 45 wt.%, oxygen 43 wt.%, ited, it is believed that the formation of passive layer might
nickel 9.4 wt.% and negligible amounts of phosphorus and be disturbed and this could be the reason for slight decrease
alumina. Whereas cracked regions showed the presence of in corrosion resistance for composite coatings. However,
about 10 wt.% of iron. Fig. 10 shows the X-ray images of Shoeib et al. [19] concluded that incorporation of polymer
corroded surface of C3 composite coating at 3000 X. particles, such as poly vinyl alcohol and poly vinyl chloride,
Images of Fe and O clearly show the presence of iron oxide. improves the corrosion resistance of electroless Ni – P
Whereas spot densities of nickel and phosphorus are deposits. It has also been reported that the corrosion
uniform except the bright region where the iron oxide is resistance of electroless nickel composite coatings in neutral
present. Iron and oxygen images taken from adjacent area of salts spray tests confirmed that the degree of corrosion
corroded surface are given in Fig. 11. From the images, it is protection offered by them is the same as that provided by
evident that spot density of iron is very less (0.8 wt.% Fe). the electroless Ni – P coatings having a similar thickness
From the above, it can be concluded that uniform corrosion [20]. Our results showed a marginal variation in corrosion
would have occurred in C1 and C2 composite coatings and current density in all the coatings studied. However, further
localized corrosion in C3 composite coating. studies are to be carried out to elucidate the corrosion
In general, electroless Ni – P is a barrier coating, mechanism.
protecting the substrate by sealing it off from the corrosive The above studies on the influence of particle size on
environments, rather than by sacrificial action. The high structure and morphology of Ni –P – Al2O3 composite coat-
resistance is a result of the amorphous nature and passivity ings show that the addition of alumina particles influences
of the Ni – P deposits. Amorphous alloys offer better the morphology and properties of the composite coatings.
corrosion resistance to corrosion attack than equivalent The coating surface appears more uniform with less

50 µm

Fig. 11. X-ray images of adjacent to corroded surface of C3 composite coating.

 J.N. Balaraju et al. / Surface & Coatings Technology 200 (2006) 3933 – 3941 3941

agglomerated particles, increase in particle size and its Grips, Ms. V. Ezhil Selvi and Dr. Anjana Jain in collecting
amount in the deposit. Separate alumina peak is visible in the data.
XRD pattern with the higher particle incorporation in the
deposit, which is evident in 1.0-Am composite coating.
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