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EFFECT OF PLATING PARAMETERS ON NiP-SiC ELECTRODEPOSITION

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NiP-SiC composite coatings were produced under both direct and pulse current conditions, from an additive-free modified Watts type bath. The influence of current parameters and hydrodynamic conditions of plating bath in the structure, morphol- ogy and mechanical properties of the composite coatings were examined. Addition- ally, micro-structural and hardness modifications induced by specific heat treatment of the coatings were investigated. Structural analysis revealed the production of an amorphous NiP matrix for the majority of coatings. However, the phase N12P5 was detected for the first time in the NiP matrix for the deposits containing phosphorus up to 12% wt, prepared under specified experimental conditions. Furthermore, the percentage of the embedded SiC micro-particles was found to be strongly depended on the duty cycle of the imposed pulses.
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EFFECT OF PLATING PARAMETERS ON NiP-SiC ELECTRODEPOSITION


P. Papavasilopoulou1, A. Zoikis-Karathanasis1, E.A. Pavlatou1, N. Spyrellis1
1. General Chemistry Laboratory, School of Chemical Engineering,
National Technical University of Athens, 9 Heroon Polytechniou Str., Zografos Campus,
Athens 15780, GREECE


ABSTRACT
NiP-SiC composite coatings were produced under both direct and pulse current
conditions, from an additive-free modified Watts type bath. The influence of current
parameters and hydrodynamic conditions of plating bath in the structure, morphol-
ogy and mechanical properties of the composite coatings were examined. Addition-
ally, micro-structural and hardness modifications induced by specific heat treatment
of the coatings were investigated. Structural analysis revealed the production of an
amorphous NiP matrix for the majority of coatings. However, the phase N12P5 was
detected for the first time in the NiP matrix for the deposits containing phosphorus
up to 12% wt, prepared under specified experimental conditions. Furthermore, the
percentage of the embedded SiC micro-particles was found to be strongly depended
on the duty cycle of the imposed pulses.

KEYWORDS:
Composite coatings, NiP matrix, SiC particles, Pulse plating


1. INTRODUCTION

Co-deposition of fine particles of ceramic or polymer compounds in the electroplated layer is a
well established method for producing composite coatings with enhanced mechanical properties
such as hardness, wear resistance and corrosion resistance. During the co-deposition process
the reinforcing particles, which are in suspension in the electrolyte, are entrapped in the growing
matrix either by electrophoresis, mechanical entrapment or adsorption phenomena /1/. The
presence of the second phase in the matrix improves the mechanical durability of the coatings
and hence, the industrial applications of the materials giving them a longer time life.
The matrix of a composite deposit could consist of a metal or an alloy. Such an alloy that endur-
ingly accretes the interest of scientists the last few decades is nickel phosphorous (NiP), which
presents better mechanical properties than those of pure nickel. Indeed, NiP surpass nickel in
hardness as well as, in wear and corrosion resistance /2-4/. The characteristic of NiP alloy is
that the incorporation of phosphorous as alloying element in the nickel lattice affects the struc-
ture of the as deposited alloy. Thus, depending on the phosphorous content the alloy could be
crystalline, amorphous or a mixture of crystalline and amorphous phase. In general NiP alloys
with phosphorous content over 9 wt% are considered as amorphous /5-6/. After thermal treat-
ment at about 400 oC the amorphous phase is crystallized at steady phases of Ni and Ni3P /7-8/.
This crystallization is accompanied by an important increase in hardness /3, 8/.
Regarding the second phase of the composite coatings, among a plethora of reinforcing parti-
cles, ceramic powders have attracted the interest of research as they combine high wear resis-
tance with low cost /9/. Consequently, SiC, TiO2, Al2O3, Si3N4 and WC have been used as rein-
forcing means in composite deposits /10-14/. However, the ceramic powder that have been
most examined is SiC in various grain size /15-20/. Apachitei et al. /21/ suggests that the com-
bination between NiP and SiC particles has proved to be the most cost effective and best per-
forming combination in applications areas where abrasive wear resistance is the main require-
Proceedings of the 7th International Conference Coatings in Manufacturing Engineering, 1-3 October 2008, Chalkidiki, Greece
Edited by: K.-D. Bouzakis, Fr.-W. Bach, B. Denkena, M. Geiger,
Published by: Laboratory for Machine Tools and Manufacturing Engineering (????),
Aristoteles University of Thessaloniki and of the Fraunhofer Project Center Coatings in Manufacturing (PCCM),
a joint initiative by Fraunhofer-Gesellschaft and Centre for Research and Technology Hellas
417


ment. Also, Chen et al /22/ refers that SiC particles can increase the hardness of a composite
coating and improve the resistance to abrasion when a hard and stable matrix supports them.
Most of the researches regarding NiP-SiC composite coatings refer to electroless deposition or
direct current electrodeposition. Berkh et al. /15, 23/ using various grain sizes (1.1 – 3.3 ?m) of
SiC and saccharin as an additive managed to produce coatings with 6.5 wt%, while Shawki /16/
proved that the load of particles in the electrolyte as well as the applied current density are im-
portant factors for the inclusion of the particles in the deposit. More recently Chou et al. /18/
came to the conclusions that the presence of SiC particles in the bath reduces the phosphorous
content in the deposit, affecting its microstructure and that submicron SiC particles aggregates
into large clusters in the NiP-SiC coating. Aslanyan et al. /20, 24/ studied the effect of SiC parti-
cles in the wear behavior of the composite coatings and supported that it depends on presence
of SiC particles as well as on the precipitation of Ni3P which in turn depends on the phosphorous
incorporation during electroplating as well as on the heat treatment process. Very recently /25/
Hou et al. using pulse current electrodeposition for producing NiP-SiC deposits from a sulfmate
bath, found that at the same average current density, SiC content in deposits is higher than that
producing in direct plating. Furthermore, the phosphorous content in the deposit decreased with
rising SiC content in the bath.
In our work for the first time a systematic study on the effect of pulse plating electrodeposition
parameters, such as it is duty cycle and frequency of pulses, on the structure, morphology and
mechanical properties of the NiP-SiC composite coating was studied. Moreover, the impact of
the hydrodynamic conditions realized through the variation of the rotating disc electrode velocity
was examined.


2. EXPERIMENTAL

The electrolytic co deposition of NiP alloy with SiC particles of mean diameter of 1 ?m was
achieved by a modified Watt’s type bath of 1 L volume. The composition of the electrolytic bath
is shown in table 1.

Table 1: Composition of electrolytic bath.
Solution composition

NiSO4·6H2O
330 g L-1
NiCl2·6H2O
35 g L-1
H3BO3
40 g L-1
NaH2PO2·H2O
10,8 g L-1
SiC powder
20 g L-1
(mean diameter of 1 ?m)



All the electrodeposition experiments were performed on a rotating disc electrode (RDE) with a
rotating velocity that varied from 200 up to 1200 rpm. Brass discs of 25 mm diameter that firstly
were mechanically polished and chemically cleaned in an ultrasonic agitated bath were used as
a substrate. The anode was a nickel foil of 99.9% purity. The temperature of the solution was
kept constant at 65±1 ?C and the pH of the bath was set at 2.5. Furthermore, in order to main-
tain the SiC particles in suspension a magnetic stirrer was implied at the bottom of the electro-
lytic cell for at least 24 hours before plating.
Two types of current were used in the electroplating process: direct (DC) and pulse (PC) cur-
rent. In the DC plating the current density was 7 A/dm2, while in the case of PC deposition the
pulse current peak was 7 A/dm2. The duty cycle values were set at 10, 30, 50, 70 and 90% and
the frequency of the imposed pulses was varied from 0.01 up to 100Hz.
418
7th
Coatings – 2008


After electrodeposition experiment ultrasonic cleaning was imposed for 10 minutes in distilled
water, in order to remove loosely adsorbed SiC particles from the surface. The thickness of the
deposits was above 50?m in order to avoid any possible influence of the substrate in the follow-
ing measurements. Furthermore all deposits were thermally treated at 400 ?C for 1 h in atmos-
phere. The heating rate step was 5?C/min, whereas the deposits were cooled calmly at room
temperature.
The structure of the composite coatings before and after thermal treating was investigated using
X-ray diffraction (XRD). The surface microstructure as well as cross sections of the coatings
were observed by scanning electron microscopy (SEM). Compositional analysis of P content in
the alloy matrix and SiC particles in the coating was made either by X-ray Fluoresce (XRF) or by
energy dispersion spectroscopy (EDS). Measurements of the Vickers microhardness (HV in
GPa) composite deposits were performed on the surface by using a Reichert microhardness
tester under 50 g load for 15 s and the corresponding final values were determined as the aver-
age of 10 measurements. Finally, the surface roughness of the deposits was determined using
an electronic pin profilometer.


3.
RESULTS AND DISCUSSION
3.1. Structure and morphology
Compositional analysis made by using XRF technique showed a diversification of phosphorous
content in the alloy matrix of composite coatings. So, the phosphorous content is oscillating be-
tween 4-12 wt%. Recent research on NiP composite coatings reinforced by nano-WC particles
(200 nm), produced under the same experimental conditions, revealed minor alteration of phos-
phorous content (13-15% wt) in NiP matrix with codeposition percentage of WC particles ex-
ceeding 20% wt /14/.
X-ray diffraction analysis showed an amorphous structure of NiP matrix in the majority of the
produced composite coatings (Figure 1a, 2a). Characteristic of the amorphous phase of the al-
loy is the wide broadening of [111] diffraction peak of nickel that is observed at 2??45º. It should
be noticed that the widening of the diffraction peak (FWHM measurement) depends on the
amount of phosphorous content in the alloy. So, low phosphorous content is associated with
thinner diffraction peaks, implying that the matrix could be in the transition limit from the crystal-
line to the amorphous phase (Figure 1a).

Amorphous
Ni
phase
Ni3P
Ni
Amorphous
phase
SiC
Ni3P
(
a
.
u
.
)
Ni2P
n
s
ir
y
(
a
.
u
.
)
n
s
ity
SiC
te
te
In
In
(a)
(a)
(b)
(b)
20
40
60
80
100
20
40
60
80
100
2 theta
2 theta


Figure 1: XRD patterns of NiP-SiC deposit
Figure 2: XRD patterns of NiP-SiC deposit
with low phosphorous content (P wt%
with high phosphorous content (P wt%
4.35) produced under pulse plating
11.6) produced under pulse plating
(dc=10%, v=0.1Hz) a. before and b. after
(dc=10%, v=10Hz) a. before and b. after
thermal treatment.
thermal treatment.

After thermal treatment at 400 oC the amorphous phase of NiP matrix has been fully crystallized
to the steady phases of Ni and Ni3P. Deposits with low phosphorous content (4-7.5 wt%) exhibit
XRD patterns with main diffraction peaks those of Ni (Figure 1b), while deposits with high phos-
Coatings Deposition, Proccesses and Properties
419


phorous content (7.5-12 wt%) reveal main diffraction peaks of Ni3P (Figure 2b). Moreover, coat-
ings with a matrix containing phosphorous higher than 11.5 wt% demonstrated diffraction peaks
of Ni2P.
An exception was observed for the coating produced under pulse plating conditions (d.c. = 10%
and v = 100Hz) at a rotating velocity of RDE of 700 rpm, as a crystalline form was revealed. In-
deed, as it is shown at the XRD pattern of Figure 3a, the crystalline phase of Ni12P5 was de-
tected accompanied by an amorphous phase. The amount of phosphorous content was 11.5
wt%, while a high percentage of SiC particles was also codeposited (22% wt). After thermal
treatment at 400oC the amorphous phase was crystallized at the steady phase of Ni3P, while the
Ni12P5 phase was not affected. It should be noticed that it is the first time that the crystalline
phase of Ni12P5 is observed at NiP coatings produced by electrodeposition in the as plated form.
Furthermore, there is no reference in literature for crystalline NiP in the as plated form contain-
ing so high percentage of phosphorous.

Ni
Ni12P5
12P5
Ni3P
.)
.)
(
a
.u
SiC
t
e
n
s
i
ty
SiC
In
I
n
t
e
n
s
it
y
(
a
.u
20
40
60
80
100
120
20
40
60
80
100
120
2 theta
2 theta


Figure 3a: XRD pattern of as plated NiP-SiC
Figure 3b: XRD pattern of heat treated NiP-
composite coating produced at d.c.=10%
SiC composite coating produced at
and v=100Hz and ?=700rpm of RDE.
d.c.=10% and v=100Hz and ?=700rpm of
RDE.

Regarding the codeposition of SiC particles it is evident that the imposition of pulse plating led to
higher percentage of particles incorporation (Figure 4). Additionally, it seems that the codeposi-
tion of SiC particles is favored at velocities of RDE in the range of 450 – 950 rpm. In general, as
the rotation velocity is increased, a beneficial effect on the particle incorporation is revealed,
which might be attributed to an increased convective flow towards the disc electrode. On the
other hand, the codeposition percentage tends to decrease at very high rotation velocities. In
this case, intense radial flow tends to remove the attached particles before they become en-
gulfed in the metal matrix /26/.

DC PC 50%-1Hz
4,00
3,00
t
%
w 2,00
C
Si 1,00
0,00
200
450
700
950
1200
RDE velocity (rpm)

Figure 4: Dependence of SiC particles embedment on type of current (DC or PC with d.c. 50%
and v=100Hz) and on RDE velocity.
420
7th
Coatings – 2008


As far as concerning the influence of pulse current parameters (duty cycle, and frequency) on
SiC incorporation in the matrix, low duty cycle, e.g. 10%, favors the embedment of SiC particles
in the matrix, while the opposite occurs when high duty cycles are imposed, as it is shown in
Figure 5. Furthermore, the practice of high frequency pulses (e.g. 100 Hz) led to composite
coating with higher percentage of embedded reinforcing particles. Therefore, it seems that there
is a proper combination of Ton and Toff determined by the imposed frequency and duty cycle,
which permits a sufficient replenishment of the catholyte enriched in SiC particles during Toff and
a adequate deposition time Ton that allows the total engulfment of particles in the NiP matrix.


10%
50%
90%
25
20
t
% 15
w
C 10
Si
5
0
0,01
0,1
1
10
100
Frequency (Hz)

Figure 5: Dependence of SiC particles incorporation on duty cycle and frequency of the impose
pulses for RDE velocity of 700 rpm.


DC plating has as a result poor dispersion in the NiP matrix. On the other hand, the application
of pulse current deposition led to coatings with better distribution of SiC particles on the surface
as long as, across the depth of the deposits, than those produced under direct current regime
(Figure 6).

(a)

(b)

Figure 6: SEM images of (a) surface and (b) cross section of NiP-SiC coating produced under
DC regime with RDE velocity of 700 rpm.


Additionally, the coatings produced by PC plating presented an increase of incorporated SiC
particles in the matrix with fine distribution across the surface and the depth of the coatings
(Figure 7).
Coatings Deposition, Proccesses and Properties
421


Compared to pure NiP coatings, the surface morphology of the composites is characterized by
sheroidal formation. It seems that SiC particles prefer to be embedded on the borders of these
formations (Figure 6a and 7a).

(a)

(b)

Figure 7: SEM images of (a) surface and (b) cross section of NiP-SiC coating produced under
PC regime (v=1Hz, d.c.=50%) with RDE velocity of 700 rpm.

The composite coating that exhibited the crystalline phase of Ni12P5 presented also a peculiar
surface morphology (Figure 8). The surface consists of two discrete areas A and B (Figure 8a),
where the amorphous phase (A) of the alloy-matrix alternates with the crystallites of Ni12P5 (B)
(Figure 8b). Thermal treatment at 400oC had no effect on the morphology of the composite de-
posits. However, EDX analysis on the surface of the coatings revealed an amount of oxygen
probably due to surface oxidation.

(a)

(b)

Figure 8: (a) SEM image of NiP-SiC coating produced under PC regime (v=100Hz, d.c.=10%)
with RDE velocity of 700 rpm. (b) Detail of the highlighted area of Figure 8a.


3.2. Mechanical properties

Concerning the as plated form of NiP-SiC composite coatings, a slight alteration of the hardness
values was revealed depending on the incorporation percentage of SiC particles in the matrix.
Figure 9 shows the dependence of Vickers microharndess on the velocity of RDE. In all cases it
is clear that the imposition of pulse plating conditions (e.g. d.c.=50% and v = 100 Hz) led to
coatings with higher values of microhardness than those produced under direct current regime.
Moreover, the coatings that have been produced by pulse current plating at d.c. = 10%, that
presented the highest embedding percentage of SiC particles, exhibited also the highest values
422
7th
Coatings – 2008


of microhardness reaching the value of 7.19 ± 0.7 GPa for the coating produced at v=100Hz
(Figure 9). It should be noticed that this coating presented also the crystalline structure. The ef-
fect of frequency on hardness values of the deposits at a given duty cycle seems to be incon-
siderable, except of the case of coatings produced at duty cycle 10%, where microhardness is
increased with increasing values of frequencies. The hardness values of NiP-SiC composite
coatings are higher than those of pure NiP coatings produced under similar conditions /14/.

(a)
(b)
10%
50%
90%
DC
PC 50%-1Hz
8,00
8,00
)
a) 7,50
a
P
P
G 7,00
G 7,00
6,50
ss (
e
ss (
e
n
n
d 6,00
6,00
r
d
ar
a
5,50
s H
s H
5,00
5,00
i
cker 4,50
V
i
cker
V
4,00
4,00
0,01
0,1
1
10
100
200
450
700
950
1200
Frequency (Hz)
RDE velocity (rpm)


Figure 9: Hardness values of as plated NiP-SiC coatings vs. a: Frequency and d.c. for velocity
of RDE 700 rpm and b: RDE velocity and type of current (DC or PC).


After thermal treatment at 400 oC the hardness values of the coatings were almost duplicated in
all cases (Figure 10). That hardening effect is caused due to the crystallization of the amor-
phous NiP matrix to the steady phases of Ni and Ni3P, as it has been observed at the XRD pat-
terns (Figures 1, 2).

(a)
(b)
10
50
90
DC
PC 50%-1Hz
14,00
14,00
)
)
a
a
p
p 13,00
G 13,00
G 12,00
ess (
ess (
n
11,00
n
12,00
r
d
r
d
a
a 10,00
H
H
s
s
11,00
9,00
i
cker
8,00
i
cker
V
V
10,00
7,00
0,01
0,1
1
10
100
200
450
700
950
1200
Frequency (Hz)
RDE velocity (Hz)


Figure 10: Hardness values of heat treated NiP-SiC coatings vs. a: Frequency and d.c. for ve-
locity of RDE 700 rpm and b: RDE velocity and type of current (DC or PC).


Although some researches support that there is a correlation between phosphorous content and
hardness of NiP deposits, no such dependence was observed in this work. However, it seems
that microhardness values depends on the incorporation percentage of SiC particles in the NiP
matrix in the as plated form as well as, after the thermal treatment of the deposits.

4. CONCLUSIONS
Coatings Deposition, Proccesses and Properties
423



NiP-SiC composite coatings have been produced under both direct and pulse plating conditions.
The imposition of PC plating led to deposits with higher incorporation of SiC particles and more
uniform distribution in the matrix than in the case of DC plating. Under specific PC conditions
(d.c. = 10%, v=100Hz and RDE velocity 700rpm), a deposit presenting a mixture of amorphous
and crystalline (Ni12P5 phase) NiP matrix has been produced. It should be noticed that it is the
first time that a crystalline phase is achieved for NiP deposits in the as plated form with a high
phosphorous content (11.5 % wt.) produced by electrodeposition. After thermal treatment at 400
oC the amorphous phase of NiP matrix has been fully crystallized in the steady phases of Ni3P,
Ni and Ni2P. This crystallization was accompanied by a remarkable increase of hardness values.
In detail, as plated coatings presented hardness in the range of 5.30 – 7,2 GPa, while after
thermall treatment the values were about 10 – 14 GPa.


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Coatings Deposition, Proccesses and Properties
425





426
7th
Coatings – 2008


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