Mat.-wiss. u. Werkstofftech. 2017, 48, 785–791 DOI 10.1002/mawe.

201700017 785

Abrasion and erosion wear of electrodeposited nickel -

silicon carbide nanocomposite coatings
Abrasiv- und Erosionsverschleiß von galvanisch Nickel -
Siliciumkarbid Nanokomposit-Beschichtungen

V. Alar1, I. Žmak1, I. Stojanović1, V. Šimunović1, Z. Čeralinac2

A nickel matrix with silicon carbide nanoparticles composite coating is prepared by

electrodeposition on non-alloyed steel, assisted with an ultrasonic treatment of the
galvanic bath. The abrasion and erosion wear resistance of the coating is de-
termined, as well as its micro-hardness. The structure and the composition of the
nickel nanocomposite coating is defined using scanning electron microscopy and
energy-dispersive X-ray spectroscopy. The corrosion behavior is investigated by
the potentiodynamic polarization methods in the 3.5 wt% sodium chloride solution.
The results show improved mechanical properties, wear and corrosion resistance
as compared to the nickel metallic coating.

Keywords: Nickel nanocomposite coating / silicon carbide nanoparticles /

electrodeposition / wear resistance / ultrasound treatment

Eine Nickelmatrix mit Siliciumkarbid-Nanopartikel Komposit-Beschichtung wurde

durch galvanische Abscheidung auf unlegiertem Stahl hergestellt. Die galvanische
Abscheidung ist durch eine Ultraschallbehandlung des galvanischen Bades unter-
stützt. Abrasiv- und Erosionsverschleißfestigkeit sowie Mikrohärte der Beschich-
tung wurden bestimmt. Struktur und Zusammensetzung der Nickel-Nanokomposit-
Beschichtung wurden unter Verwendung von Rasterelektronenmikroskopie und
energiedispersiver Röntgenspektroskopie untersucht. Das Korrosionsverhalten
wurde durch potenziodynamische Polarisationsverfahren in 3,5 Gew% Natrium-
chlorid-Lösung untersucht. Die Ergebnisse zeigen verbesserte mechanische Ei-
genschaften, Verschleiß- und Korrosionsbeständigkeit im Vergleich zur Nickel-Me-
tallbeschichtung.

Schlüsselwörter: Nickel-Nanokomposit-Beschichtung / Siliciumkarbid-Nanopartikel /

elektrochemische Abscheidung / Verschleißfestigkeit / Ultraschall-Behandlung

1 Introduction One of the most dangerous consequences of such

impacts is the corrosion, which initially causes the
Steel constructions and products are exposed to var- deterioration on the outer surfaces, subsequently
ious impacts from the surrounding environment. reaches the interior and can permanently damage a

1 University of Zagreb, Faculty of Mechanical Engi-

neering and Naval Architecture, I. Lučića 5, HR- Corresponding author: I. Žmak, University of Zagreb,
10000 Zagreb, Croatia Faculty of Mechanical Engineering and Naval Architec-
2 Končar Electrical Engineering Institute, Fallerovo ture, I. Lučića 5, HR-10000 Zagreb, Croatia,
šetalište 22, HR-10000 Zagreb, Croatia E-Mail: irena.zmak@fsb.hr

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certain product or a construction. The abrasion and
erosion wear from the mechanical interaction be-
tween the components or fluids also contributes to
the deterioration of various steel products. The need
for the corrosion protection systems with an in-
creased wear resistance is therefore very important
from the aspect of prolonging the durability of
many steel applications.
The development of the nanotechnology has
opened new possibilities to produce coatings which
offer much better surface protection and increase
the durability of the steel products. One of the mate-
rials with improved properties is the nanocomposite
coating based on the metal matrix with embedded
nanoparticles of various dimensions and forms. The
embedded nanoparticles change the microstructure
of the metallic coating through the electrodeposition
process, which results in nanostructured coatings.
Such nanostructured coatings are more compact,
and thus more resistant to negative environmental
impacts. The most prevailing metal coating in the
industry is certainly the nickel coating. Nickel coat-
ing was also used in this paper as the metal matrix
for the embedding of the silicon carbide nano-
particles, as well as in other recently published re-
search work [1-3]. This paper investigates the im-
pact of the various concentrations of the silicon
carbide nanoparticles onto the wear and corrosion
resistance. As a novelty, the ultrasonic treatment of
the galvanic bath was applied during both the sus-
pension preparation and the deposition process.
2 Preparation of the nickel nanocomposite
coating
The nickel nanocomposite coating was prepared by
the electrodeposition process or electroplating. A
non-alloyed cold-bent steel plate was used as a base
for the coating. The dimensions of the steel plate
were 60 mm length, 20 mm width and 8 mm thick-
ness, with a total surface area of 1200 mm2 to be
coated. Before the application of the nanocomposite
coating, the sample surface was sanded with 600-,
800- and 1000-grit sandpaper and polished with the
suspension of 1 mm aluminium oxide particles. The
sample surface was degreased in an ultrasonic bath
of ethyl alcohol for five minutes. The electrolyte
solution was defined according to Watts bath type,
as: nickel sulphate (240 g L-1), nickel chloride
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(45 g L-1), boric acid (30 g L-1) and sodium dodecyl
sulphate (2 g L-1) [4]. The process parameters for
the application of the nanocomposite coating were
as follows: current density (j = 2 A dm-2), temper-
ature (T = 45 8C), pH value (pH = 4.5) and deposi-
tion time (t = 30 min).
Nanoparticles of the silicon carbide, provided by
NaBond Technologies, Shenzhen, China were used
during the nickel electrodeposition process. Three
different samples were prepared with 20 g L-1,
30 g L-1 and 40 g L-1 concentrations of the nano-
particles in the electrolyte solution. The silicon car-
bide particles had a spherical shape with the average
particle size of 50 nm, according to the manu-
facturer’s specifications. Before the nanocomposite
electrodeposition process was started, the silicon
carbide nanoparticles were dissolved in the electro-
lyte solution with an ultrasonic probe. The ultra-
sound was used in order to prevent the agglomer-
ation and improve the dispersion of the silicon
carbide nanoparticles, which as a result should lead
to improved mechanical and protective properties of
the nanocomposite coating. It is expected that the
ultrasonic treatment should eliminate the pores and
voids produced on the substrate surface by the hy-
drogen evolution during the electrodeposition proc-
ess.
During the electrodeposition process the silicon
carbide nanoparticles are deposited on the cathode
together with the nickel ions. Thus, silicon carbide
nanoparticles are embedded in the crystal structure
of the nickel coating which results in a nano-
composite coating [5].
3 Methods for determining the nickel
nanocomposite coating properties
The structural analysis of the prepared nano-
composite coating was conducted with the surface
analysis techniques, such as the scanning electron
microscopy and the energy-dispersive X-ray spec-
troscopy on the electronic microscope VEGA TES-
CAN TS 5136 MM equipped with the INCA soft-
ware from Oxford Instruments.
The mechanical properties of the nickel nano-
composite coating were determined with the Knoop
micro-hardness test and by measuring the abrasion
and erosion resistance. The Knoop micro-hardness
test was conducted according to the EN ISO
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4516:2003 international standard with the micro- 4 Results and discussion

hardness tester TUKON TESTER Model FB WIL-
SON. The structural classification of the nickel nano-
The abrasion resistance was measured by the composite coating, conducted with the physical-sur-
standard dry sand/rubber wheel method, according face instrumental methods (the scanning electron
to the ASTM G65-94 international standard. The microscopy and the energy-dispersive X-ray spec-
OTAWA AFS 50/70 quartz sand of 300 mm and troscopy), provided the information on the quantity
1200 HV0.03 was used as the abrasive. The sam- and the allocation of the nanoparticles, as well as on
ples were loaded with 45 N force, and 500 wheel the structure and composition of the nanocomposite
turns in 100-turn steps were applied. The nano- coating. Scanning electron microscopy images of
composite coating mass loss due to the abrasive the nickel coating and nanocomposite coatings
wear was determined by weighing the sample be- show that the embedding of solid silicon carbide
fore and after the testing using the METTLER B5C nanoparticles in the nickel metal matrix has caused
1000 balance. The mass loss of the nanocomposite a change in the microstructure of the nanocomposite
coating was used as a measure of the abrasion wear coating in comparison to the nickel coating, Figure
resistance. 1. With the increase of the weight content of the sil-
The particle erosion resistance was tested by icon carbide particles, the microstructure of the
high speed rotation of the samples, which collide nanocomposite coating becomes more granular. The
with the abrasive particles of dry sand. Dry 300 mm silicon carbide particles act as the nucleation sites
OTAWA AFS 50/70 quartz sand of 1200 HV0.03 for the nickel deposition which results in a sig-
flowed freely from a tank through the nozzle. The nificant change in the size of the nickel crystal de-
sand entry angle was 908, which exposed the coat- posited on the nanocomposite coating [6].
ings to the highest erosion level. The erosion resist-
ance was determined with 20,000 pivot turns. The
impact of the sand onto the specimens leads to the
erosion wear on the surface hit by the sand par-
ticles. The nanocomposite coating mass loss was
determined by weighing the sample before and after
the testing, i. e. the mass loss of the nanocomposite
coating was used as a measure for the erosion wear
resistance.
The electrochemical measurements were also
performed. The polarization measurements were
conducted using the EG&G Model 273 Potentiostat/
Galvanostat with the SoftCorr III application, ac-
cording to the ASTM G61 standard test method.
Three electrode cells contained 600 mL of 3.5 wt%
sodium chloride solutions at room temperature. The
coated specimens were used as the working elec-
trode. Two graphite electrodes and one saturated
calomel electrode (SCE) were used as the counter
and the reference electrodes, respectively. The cor-
rosion potential (Ecorr), corrosion current density
(jcorr) and polarization resistance (Rp) were de- Figure 1. Scanning electron microscopy images of the nickel
termined from the polarization curves. coating (a); nickel nanocomposite coatings with 20 g L-1 (b);
30 g L-1 (c); and 40 g L-1 (d) silicon carbide particles in the elec-
trolyte solution.
Bild 1. Rasterelektronenmikroskopie-Bilder der Nickel-
schicht (a); Nickel Nanokomposit-Beschichtungen mit
20 g L-1 (b); 30 g L-1 (c); und 40 g L-1 (d) Siliciumkarbid-Teil-
chen in der Elektrolytlösung.

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The energy-dispersive X-ray spectroscopy mi-
cro-images of the nickel nanocomposite coatings
were taken by mapping 20 mm 3 20 mm sample sur-
face, in order to determine the composition of the
nanocomposite coatings, Figure 2. Based on these
results, it can be concluded that the increase in the
concentration of the silicon carbide nanoparticles in
the electrolyte solution leads to an increase in the
weight content of the silicon carbide nanoparticles
in the nanocomposite coating. The weight content
Figure 2. Energy-dispersive X-ray spectroscopy analysis
and mapping of micro-images of the nickel nanocomposite
coating with: 20 g L-1 (a), 30 g L-1 (b) and 40 g L-1 (c) concen-
trations of the silicon carbide particles in the electrolyte solu-
tion.
Bild 2. Energiedispersive Röntgenspektroskopie-Analyse
und Kartierung von Mikrobildern der Nickel Nanokomposit-
Beschichtung mit: 20 g L-1 (a), 30 g L-1 (b) und 40 g L-1 (c)
Konzentrationen der Siliciumkarbid-Partikel in die Elektrolyt-
lösung.
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of the silicon carbide nanoparticles had a maximum
value of 1 wt% in the nanocomposite coating pre-
pared from the electrolyte solution with a 40 g L-1
concentration of the silicon carbide nanoparticles. In
addition, the energy-dispersive X-ray spectroscopy
micro-images clearly show that the silicon carbide
nanoparticles are well distributed over the entire
surface of the nanocomposite coating, and there
isn’t any agglomeration of the nanoparticles.
The Knoop micro-hardness test of the nickel
coating and silicon carbide nanocomposite coatings
was conducted under the load of 0.1 3 9.81 N for 15
seconds, Table 1. The results show that the nano-
composite coatings have higher micro-hardness val-
ues than the nickel coatings. The nanocomposite
coating prepared from the electrolyte solution with
the 40 g L-1 concentration of the silicon carbide
nanoparticles had the highest micro-hardness value
(HK0.1 = 832). The increase in the micro-hardness
of the nanocomposite coating can be ascribed to the
presence of the intrinsic hardness of the co-de-
posited ceramic phase, i.e. nano-sized silicon car-
bide, and to the fact that the ceramic phase is well
dissolved in the nickel metal matrix, which leads to
the enhancement of the nanocomposite coating mi-
crostructure [7]. Therefore, the increase in the con-
tent of the extremely hard silicon carbide nano-
particles contributes to the increase of the
nanocomposite coating hardness.
The increase of the silicon carbide nanoparticles
concentration in the electrolyte solution resulted
also in an increase of the nanocomposite coating
abrasion resistance, Figure 3. The greatest weight
loss (Dm = 60.6 mg) was observed on the nickel
coating, and the smallest (Dm = 29.7 mg) on the
nanocomposite coating prepared from the electro-
lyte solution with 40 g L-1 silicon carbide.
The increase of the silicon carbide nanoparticles
concentration in the electrolyte solution resulted in
an increase of the nanocomposite coating erosion
resistance as well, Figure 4. The worst erosion re-
sistance (Dm = 17.3 mg) was observed on the nickel
coating and the best erosion resistance (Dm = 5.6
mg) on the nanocomposite coating prepared from
the electrolyte solution with 40 g L-1 silicon carbide.
Homogenously allocated nano-sized silicon carbide
in the nickel matrix, with the microstructural mod-
ifications of the nanocomposite coating formed dur-
ing the co-deposition of the silicon carbide nano-
particles with the nickel ions contribute to an
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Table 1. Knoop micro-hardness of the nickel- and nanocomposite coatings.

Tabelle 1. Knoop-Mikrohärte von Nickel- und Nanokomposit-Beschichtungen.

Coating type Concentration of the silicon carbide nanoparticles in the elec- Knoop micro-hard-
trolyte solution [g L-1] ness, HK0.1
Nickel coating - 562
Nanocomposite 20 649
coating
Nanocomposite 30 721
coating
Nanocomposite 40 832
coating

The pure presence of the silicon carbide nano-

Figure 3. Abrasion resistance of the nickel- and nano-
composite coatings.
Bild 3. Abriebbeständigkeit der Nickel- und Nanokomposit-
Beschichtungen.
particles is not enough to improve the corrosion re-
sistance, but a uniform particle dispersion is also es-
sential. The potentiodynamic polarization curves
were recorded for pure nickel and the nickel – sili-
con carbide nanocomposite coatings in 3.5 wt% so-
dium chloride solution, Figure 5. For each speci-
men following corrosion parameters were
determined: corrosion potential (Ecorr), polarization
resistance (Rp) and corrosion current density (jcorr),
Table 2. The increase in the amount of the co-de-
posited silicon carbide nanoparticles in the nickel
matrix improves the steel corrosion resistance in salt
solutions. The silicon carbide nanoparticles play a
major role in improving the corrosion protection by
two mechanisms. Firstly, the silicon carbide nano-
particles act as an inert physical barrier to the ini-
tiation and development of the defects, modifying
the microstructure of the nickel layer, and hence im-

Figure 4. Erosion resistance of the nickel- and nanocompo-

site coatings.
Bild 4. Erosionbeständigkeit der Nickel- und Nanokomposit-
Beschichtungen.
Figure 5. Potentiodynamic polarization curves of nickel- and
nanocomposite coatings.
increase in the abrasion and erosion resistance of Bild 5. Potenziodynamische Polarisationskurven von Nickel-
the nickel nanocomposite coating [8]. und Nanokomposit-Beschichtungen.

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Table 2. Potentiodynamic polarization corrosion parameters for nickel coating and nickel - silicon carbide nanocompo-
site coatings in 3.5 wt% sodium chloride solution.
Tabelle 2. Potenziodynamische Polarisationsmessungen von Nickel-Beschichtung und Ni-SiC-Nanokomposit-Be-
schichtungen in 3,5 Gew.% Natriumchlorid-Lösung.
Coating type Corrosion potential, Ecorr
[mV (SCE)]
Pure nickel -459
Nickel + 20 g L-1 sili- -375
concarbide
Nickel + 30 g L-1 sili- -372
concarbide
Nickel + 40 g L-1 sili- -312
concarbide
proving the corrosion resistance of the coating. Sec-
ondly, the dispersion of the silicon carbide nano-
particles in the nickel layer results in the formation
of many corrosion microcells in which the silicon
carbide nanoparticles act as a cathode and the nickel
as an anode, since the standard potential of the sili-
con carbide is more positive than that of the nickel.
Such corrosion microcells could facilitate the anodic
polarization [9, 10]. Therefore, the presence of the
silicon carbide inhibits the localized corrosion, and
mainly the homogeneous uniform corrosion occurs.
5 Conclusion
The use of the physical-surface methods (the scan-
ning electron microscopy and the energy-dispersive
X-ray spectroscopy) and tribological methods (mi-
cro-hardness, abrasion and erosion resistance) de-
termined the composition, structure, mechanical and
tribological properties of the electrodeposited nickel
– silicon carbide nanocomposite coatings. The re-
sults indicate enhanced wear resistance of the nickel
nanocomposite coatings with reference to the nickel
metallic coating. The use of the ultrasound during
electroplating of the nanocomposite nickel coating
improved the film properties by refining the micro-
structure and thus leading to a harder and more
compact coating layer. Ultrasonic treatment im-
proved also the quality of the deposit layer through
its enhanced wear resistance and homogeneous
morphology.
The best abrasion and erosion resistance and
highest hardness were observed in the nickel nano-
composite coating prepared from the electrolyte sol-
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Polarization resistance, Corrosion current density,
Rp [kW cm2] jcorr [mA cm-2]
1.53 65.19
15.07 45.29
45.73 8.67
50.51 1.38
ution with 40 g L-1 silicon carbide. Also, by increas-
ing silicon carbide content in the coating, the
corrosion current density decreased and the corro-
sion potential shifted towards more positive poten-
tials, which was determined through the potentiody-
namic polarization method in 3.5 wt% sodium
chloride solutions.
The increase in hardness and wear resistance
of the nanocomposite coating with reference to
the nickel coating can be ascribed firstly to the
presence of the co-deposited ceramic phase, i.e.
hard silicon carbide nanoparticles. Secondly,
nano-sized silicon carbide is well dissolved in the
nickel metal matrix, which leads to the enhance-
ment of the microstructure through the formation
of the nanocrystalline nickel, and thus a more
compact coating structure. The refined micro-
structure of the composite coatings correspond-
ingly increased the wear resistance. In order to
enhance wear and corrosion resistance of a nano-
composite coating it is very important to deposit
it pore-free. This paper has demonstrated that the
ultrasound treatment allows a successful applica-
tion of high-quality and highly protective nano-
composite coatings.
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Received in final form: February 27th 2017
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