JMEPEG (2017) 26:2118–2128 ÓThe Author(s).

This article is an open access publication

DOI: 10.1007/s11665-017-2662-2 1059-9495/$19.00

Effect of Surface Roughness and Structure Features on

Tribological Properties of Electrodeposited
Nanocrystalline Ni and Ni/Al2O3 Coatings
Anna Góral, Lidia Lityńska-Dobrzyńska, and Marcin Kot

(Submitted January 30, 2017; in revised form March 28, 2017; published online April 13, 2017)

Metal matrix composite coatings obtained by electrodeposition are one of the ways of improving the
surfaces of materials to enhance their durability and properties required in different applications. This
paper presents an analysis of the surface topography, microstructure and properties (residual stresses,
microhardness, wear resistance) of Ni/Al2O3 nanocomposite coatings electrodeposited on steel substrates
from modified Watts-type baths containing various concentrations of Al2O3 nanoparticles and a saccharin
additive. The residual stresses measured in the Ni/Al2O3 coatings decreased with an increasing amount of
the co-deposited ceramics. It was established that the addition of Al2O3 powder significantly improved the
coatings microhardness. The wear mechanism changed from adhesive-abrasive to abrasive with a rising
amount of Al2O3 particles and coating microhardness. Nanocomposite coatings also exhibited a lower
coefficient of friction than that of a pure Ni-electrodeposited coating. The friction was found to depend on
the surface roughness, and the smoother surfaces gave lower friction coefficients.

7-14). Moreover, increasingly popular are functionally graded

Keywords friction coefficient, metal matrix composite, Ni/nano-
Al2O3, residual stresses, surface topography, wear nanocomposite coatings (e.g., Ni/Ni-Al2O3, Ni-W-Al2O3) into
which alumina content increases from the substrate toward the
surface of the coating possessing improved wear and corrosion
resistance properties (Ref 15, 16). The incorporation of hard
ceramic particles into the metallic matrix enables the manufac-
1. Introduction turing of composite coatings with enhanced mechanical and
tribological properties as compared to pure metal coatings (Ref
9-12, 17, 18). Therefore, they are applied as the coatings
Metal matrix composite (MMC) coatings reveal improved
reducing friction and wear in friction nodes (Ref 19, 20).
properties (compared to pure metal), derived from the co-
Ni/Al2O3 coatings are considered as potential candidates to
deposition of dispersed hard particles in the metallic matrix.
replace electrodeposited hard chromium coatings, the produc-
They are produced by different technologies, depending on the
tion of which is limited by restrictive environmental laws (Ref
application and economic reasons. Several metals, e.g., nickel,
21-23). Ni/Al2O3 nanocomposite coatings are used primarily to
copper or chromium, are mainly used as the metal matrix,
increase the wear resistance of metal surfaces in microdevices.
whereas metal oxides, carbides, borides and polymers are the
Due to their good tribological and anticorrosion properties, they
co-depositing particles (Ref 1-4). Electrochemical deposition is
find application as coatings of engine cylinders, high-pressure
a method of covering conductive surfaces with metals or alloys
valves, and dies and in the production of car accessories and
as well as composite coatings aimed at obtaining the required
small aircraft and electrotechnical parts (Ref 24-26). Elec-
surface characteristics. It enables control of the deposit
trolytic nickel coatings exhibit specific properties, such as good
microstructure and thickness as well manufacture of nanocrys-
corrosion resistance and catalytic activity in many electro-
talline coatings in a single step without secondary treatment
chemical processes (Ref 27). Incorporating ceramic nanopar-
(Ref 5). During the electrodeposition process of composite
ticles into the nickel matrix allows one to obtain higher
coatings, dispersed hard particles are kept in suspension in an
microhardness and good wear properties (Ref 11, 28). Ni/Al2O3
electrolyte and then incorporated into the metal matrix.
have been extensively studied; however, considerable research
Through the application of different plating baths and different
has been focused on the impact of the electrodeposition
types of particles (oxides, carbides, graphite, sulfides and
parameters, especially the value and kind (direct, pulse) of the
PTFE), the production of a large range of composite coatings
current density (Ref 11, 13, 29-31) as well as the type and
exhibiting excellent properties, such as wear resistance, corro-
concentration of the applied additives (Ref 5, 6), on the
sion resistance and lubrication, depending on the type, amount
manufacture process and the volume fraction of the particles
and distribution of the co-deposited particles was possible (Ref
built in the nickel matrix. It is known that an addition of
saccharin to the electrolytic bath causes grain size refinement of
Anna Góral and Lidia Lityńska-Dobrzyńska, Institute of Metallurgy the materials (Ref 32-38). The microstructure refinement, in
and Materials Science of the Polish Academy of Sciences, 25 turn, has a significant impact on the mechanical wear properties
Reymonta St., 30-059 Kraków, Poland; and Marcin Kot, Faculty of
Mechanical Engineering and Robotics, AGH University of Science and of the coatings. Additionally, decreasing the ceramic particle
Technology, av. Mickiewicza 30, 30-059 Kraków, Poland. Contact size can also affect the properties in a positive way, mainly
e-mail: [email protected]. through the hardening of the metal matrix coatings by finely

2118—Volume 26(5) May 2017 Journal of Materials Engineering and Performance

dispersed particles (Ref 31). To enhance the tribological ically dispersed in the bath for 2 h and mechanically agitated
properties of electrodeposited nanocomposite coatings, the (800 rpm) using a magnetic stirrer. During the electrodeposi-
interface between the nanoparticles and the metal matrix must tion, the bath was stirred using a magnetic stirrer with a stirring
have enough strength to ensure that the embedded particles are rate of 500 rpm and circulated with a peristaltic pump (50 rpm).
not torn out during tribological contact. Aruna et al. (Ref 12) The obtained coatings were ultrasonically cleaned to remove
have shown that the wear resistance of Ni/Al2O3 containing particles loosely adherent to their surface. The thickness of the
alpha alumina is higher than that of the composites containing analyzed coatings was in the range of 9.7-12 lm. The coatings
gamma alumina and mixtures of alpha, gamma and delta were completely characterized with the use of XRD techniques
alumina. Gul et al. (Ref 11) have compared the tribological (Bruker D8 diffractometer with Co Ka filtered radiation) as well
properties of Ni/Al2O3 coatings produced by the way of as scanning and transmission electron microscopes (SEM—FEI
applying both the direct (DC) and pulse (PC) current densities. QUANTA 3D FEG, and TEM—FEI TECNAI G2). The thin
They showed that the coating obtained with PC did not reveal a foils were prepared by the focused ion beam (FIB) technique
significant increase in hardness; it had a larger grain size and with the use of an FEI Quanta 3D dual beam. The amount of
more plastic deformation compared with the DC-coated mate- Al2O3 nanoparticles incorporated into the Ni matrix was
rials. Improving the abrasive resistance of the components is determined with the use of Locos Shire dedicated to image
becoming a research subject of top priority and a great industrial analysis. The particles percentage by volume (vol.%) was
importance. It is known that the friction coefficient and the wear determined based on ten areas of the SEM coating microstruc-
resistance of a material are related to its surface topography and, tures (8.9 lm 9 14.7 lm) of the cross sections of the coatings.
usually, smoother surfaces give a lower friction coefficient (Ref The residual stresses were measured based on the 311 Ni
39-41). However, this relationship depends on the environmen- reflection (2h = 114.9°)—with the use of the sin2w method. The
tal conditions and on the material types of the two friction indentation technique (Ref 44, 45) was used to evaluate the
surfaces, as well as on the type of motion. hardness and the elasticity modulus. The tests were performed at
This paper presents the effect of the surface roughness of the the 50 mN maximum load and the 100 mN/min loading and
thin nanocrystalline Ni and Ni/Al2O3 coatings electrodeposited unloading rate with the use of the CSEM-MCT equipment. On
from the Watts bath containing various amounts of Al2O3 each coating, at least nine indentations were made, and for
nanoparticles on their friction and wear resistance, which has not further analysis, the average values were taken. The tests of the
been investigated, yet. A novelty of this paper is also the linking wear and friction coefficient of Ni/Al2O3 coatings were
the mechanical and tribological properties of the Ni/Al2O3 performed under dry conditions with the use of a ball-on-disk
nanocomposite coatings with the structure features observed in tribometer [according to the ISO standard (Ref 46)] with 6-mm-
nanoscale, especially growth-type nanotwins existing in the diameter sintered a-Al2O3 spheres. The tests were performed at
nickel matrix. Furthermore, the influence of a saccharin additive the temperature of 22 ± 2 °C with the relative humidity of
in the electrolytic bath on the microstructural features of Ni/ 50 ± 2%. The normal load was 10 N, the linear sliding speed of
Al2O3 coatings, depth-sensing indentation response, residual the ball was 0.05 m/s, the radius was 7 mm, and the number of
stresses and wear behavior has been investigated and compared cycles was 20,000. Only for the Ni/Al2O3-80 + S wear, the
with that of pure Ni and Ni/Al2O3 coatings obtained from the bath index wear was calculated after 80,000 cycles. After the tests,
without an additive. The selection of saccharin was dictated by the wear track profiles were measured, and then, the specific
earlier examinations, which revealed higher microhardness and wear index WV was calculated from the formula:
good anticorrosive properties of the resulting coatings (Ref 42).
V
WV ¼
Fn  s

2. Experimental Details where V—volume of the removed material calculated on the

basis of the average cross-sectional area of the grooves,
Fn—normal load, s—sliding distance. The worn surfaces
Nickel/alumina nanocomposite coatings were deposited were subjected to SEM observations for the analysis of the
electrochemically from a modified Watts bath containing wear mechanism. The topography of the coatings after polish-
120 g/L NiSO4Æ6H2O, 70 g/L NiCl2Æ6H2O and 50 g/L H3BO3 ing was analyzed by means of a Talysurf CCI Lite non-con-
into which various amounts (20, 40, 60, 80 g/L) of a-Al2O3 tact 3D profiler (Ref 47).
nanopowder were added. These samples were denoted as: Ni,
Ni/Al2O3-20, Ni/Al2O3-40, Ni/Al2O3-60 and Ni/Al2O3-80.
Additionally, nanocomposite coatings produced from the bath,
which, beside the 80 g/L of a-Al2O3, contained 1 g/L of 3. Results and Discussion
saccharin, were also examined and denoted as Ni/Al2O3-80 + S.
The size of the alumina particles ranged from 80 to 150 nm. The 3.1 Microstructure of Ni and Ni/Al2O3 Coatings
details regarding the electrodeposition of nickel/alumina coat-
ings on low carbon steel substrates have already been published The SEM BSE surface morphologies of pure Ni and Ni/
(Ref 13, 43). In order to identify the effect of the ceramic Al2O3-20, Ni/Al2O3-40, Ni/Al2O3-60, Ni/Al2O3-80, Ni/Al2O3-
particles on the Ni/Al2O3 deposit properties, all the coatings 80 + S composite coatings are presented in Fig. 1. The pure Ni
were deposited using a potentiostat/galvanostat AUTOLAB deposits exhibited a pyramidal microstructure on the surface, as
model PGSTAT 302 under the same conditions: current density shown in Fig. 1(a). The microstructure of the composite Ni/
of 5 A/dm2, pH 4, temperature of 40 °C, anode—a vertically Al2O3 coatings was finer, with visible Al2O3 particles (fine dark
placed nickel (99.9% purity) plate, and cathode—a vertically areas), as shown in Fig. 1(b), (c), (d), (e), and (f). The
mounted low carbon steel disk with a diameter of 20 mm. composite coatings produced a flatter surface when compared
Before the co-deposition, the alumina particles were ultrason- to the nickel deposits. The coatings did not reveal any pores or

Journal of Materials Engineering and Performance Volume 26(5) May 2017—2119

Fig. 1 SEM BSE microstructures of the surfaces of coatings: Ni (a), Ni/Al2O3-20 (b), Ni/Al2O3-40 (c), Ni/Al2O3-60 (d), Ni/Al2O3-80 (e), Ni/
Al2O3-80 + S (f)

Fig. 2 SEM BSE microstructures of the cross sections of coatings: Ni (a), Ni/Al2O3-20 (b), Ni/Al2O3-40 (c), Ni/Al2O3-60 (d), Ni/Al2O3-80 (e),
Ni/Al2O3-80 + S (f)

fissures on the surfaces. As can be seen from the cross sections with the alumina and saccharin additive (Fig. 3a, b, and c) and
presented in Fig. 2, all the produced coatings were compact. led to a fine-grained microstructure as shown in Fig. 3(c). The
The nanoparticles present in the Ni matrix were usually Ni and Ni/Al2O3 coatings revealed the presence of numerous
concentrated in agglomerates, as shown in Fig. 2(b), (c), (d), nanotwins in the Ni matrix, which influence the mechanical
(e), and (f). The distribution of agglomerates in the coating properties of the coatings. The smallest matrix grains contain-
became more uniform with an increasing amount of Al2O3 ing nanotwins were observed in the Ni/Al2O3-80 + S compos-
nanoparticles added to the electrolyte. Furthermore, it is worth ite coating produced from the bath including saccharin. A
emphasizing that although these coatings were thin (9.7- detailed description of the Ni and Ni/Al2O3 coating microstruc-
12 lm), they revealed a uniform particle agglomerate distribu- tures containing nanotwins formed during electrodeposition
tion from the substrate to the coating surface. The Al2O3 was recorded in Ref 43. An increasing (from 20 to 80 g/L)
nanoparticles had an influence on the crystallization behavior of amount of the ceramic phase in the electrolyte caused a rise of
the composite coatings. The surfaces of the Al2O3 nanoparticles the amount of the ceramic particles from 7.9 to 9.9 vol.%
provided new sites for the nucleation of nickel grains, so the embedded in the Ni matrix (Fig. 4), as was estimated on the
amount of nucleation sites for the Ni grains was higher than for basis of the SEM microstructures. These percentages by
pure Ni. It was found that the Ni matrix grew in the form of volume of the incorporated Al2O3 nanoparticles were compa-
columnar grains in all the coatings, which decreased in size rable to those determined in Ref 11.

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Fig. 3 Bright-field TEM image of the cross sections of coatings: Ni (a), Ni/Al2O3-80 (b), Ni/Al2O3-80 + S (c) with nanotwins marked with
arrows

Fig. 4 Volume fraction of Al2O3 nanoparticles incorporated into

coatings at various Al2O3 concentrations in the electrolyte

3.2 Surface Topography of Coatings

Four coating surface structures (Ni, Ni/Al2O3-20, Ni/Al2O3-
80 Ni/Al2O3-80 + S) as regards their tribological behavior were
characterized. The surface topography, depth histogram and
bearing curve for the Ni and Ni/Al2O3 coatings are presented in
Fig. 5. According to ISO 25178, the height parameters were
calculated based on all the measurement data from the optically Fig. 5 Surface topography (a, c, e, g) and depth histogram with
scanned surface area and are presented in Table 1. The bearing curve (b, d, f, h) for coatings Ni (a, b) Ni/Al2O3-20 (c, d),
parameters were derived from the Abboit-Firestone curve, Ni/Al2O3-80 (e, f) and Ni/Al2O3-80 + S (g, h)
which characterizes the functional behavior of the measured
surface. As shown in Table 1, the arithmetic mean height Sa,
surface. Additionally, higher values of kurtosis Sku for both
giving a very good overall description of the height variations,
coatings were the result of larger grains in the profile of the
was the highest (0.4147 lm) for the pure Ni coating and the
surface. The other topography parameters, such as the maxi-
lowest (0.228 lm) for Ni/Al2O3-80 + S. As shown in Table 1,
mum valley height Sv and the maximum height Sz, were
the differences in the values of Sa for the examined Ni/Al2O3
significantly lower for the composite coatings compared to the
coatings were insignificant. A similar trend was observed for
pure Ni ones. A difference was only seen for the parameter of
the root mean square deviation (Sq).
the maximum peak height Sp, which was the highest for Ni/
The skewness (Ssk) and kurtosis (Sku) were also measured,
Al2O3-80. It can be concluded that the deposited Ni/Al2O3
which are the two key parameters characterizing the asymmetry
coatings revealed up to 45% lower roughness of their surfaces
and the flatness of the surface distribution. The skewness
than the pure Ni coatings.
parameter Ssk was close to zero, which was reflected in the
symmetrical height distribution for the Ni/Al2O3-20 and Ni/
3.3 Residual Stresses of Coatings
Al2O3-80 + S coatings. The pure Ni showed negative skew-
ness—0.867, indicating a surface with more deep and sharp The values of residual stresses are presented in Fig. 6. All
valleys, while Ni/Al2O3-80 exhibited a positive value 0.879, the examined coatings revealed tensile residual stresses.
describing a surface with peaks protruding from a mostly planar Increasing the amount of incorporated Al2O3 nanopowder

Journal of Materials Engineering and Performance Volume 26(5) May 2017—2121

Table 1 Surface topography parameters according to ISO 25178
Height parameters

Coating Sa, lm Sq, lm Ssk Sku Sp, lm Sv, lm Sz, lm

Ni 0.4147 0.5538 0.8673 5.9688 1.8499 4.5523 6.4021

Ni/Al2O3-20 0.2582 0.3272 0.3024 3.3296 1.2502 1.1130 2.3632
Ni/Al2O3-80 0.3019 0.4030 0.8790 6.4893 3.0223 1.3749 4.3972
Ni/Al2O3 + S 0.2280 0.2892 0.1038 3.2715 1.4196 1.0369 2.4565

Sa, arithmetic mean height; Sq, root mean squared height; Ssk, skewness; Sku, kurtosis; Sp, maximum peak height; Sv, maximum valley depth; Sz,
maximum height

microhardness due to the increased Al2O3 content in the

deposited layer was highly correlated with the volume fraction
of alumina. The microhardness in the coatings increased by
about 30% with the increasing amount (up to 80 g/L) of Al2O3
in the bath. The Ni/Al2O3-80 composite coating containing
9.9 vol.% of incorporated Al2O3 had the microhardness of
4.4 GPa, whereas the pure Ni coating has 3.42 GPa. The
obtained microhardness values were in the same range as the
values for the Ni/Al2O3 nanocomposites containing nanopar-
ticles reported by Corni et al. (Ref 50). With the increase in the
ceramic phase content in the coatings, the grain size of the Ni
matrix was decreased (Ref 17). Therefore, the increase in the
microhardness values of the Ni/Al2O3 nanocomposites might
be due to a smaller grain size of the Ni matrix favored by the
nanosized Al2O3 particles. The increase in the microhardness
values in the composite coatings was the result of a dispersion-
Fig. 6 Residual stresses determined in Ni and Ni/Al2O3 nanocom- strengthening effect by the Al2O3 nanoparticles, which impede
posite coatings obtained from the bath containing various amounts of the motion of dislocations in the metallic matrix, or the Orowan
Al2O3 and saccharin hardening mechanism (Ref 51). Nano-a-Al2O3 particles local-
ized at the Ni grain boundaries inhibited the dislocation motion,
restrained the growth of columnar grains of nickel and
resulted in a decrease in their values. The highest value of provoked the nucleation of new sites. Similar results were
252 MPa was revealed for the pure Ni coating and the reported in other metal matrix nanocomposites, such as Ni-
lowest—193 MPa—for the Ni/Al2O3-80 + S sample obtained Al2O3 (Ref 11, 13, 28), Ni-CeO2 (Ref 17) and Ni-SiC (Ref 18).
from the electrolyte with saccharin. The low residual stresses However, the highest microhardness was revealed by the
are connected with the considerable grain refinement of the Ni coatings obtained from the electrolyte with a saccharin additive.
matrix. The grain size of nickel was smaller with a high Al2O3 Taking into consideration the fact that, in this case, the amount
nanoparticle content in the electrolyte, so that residual stresses of incorporated ceramic particles was smaller than in the
could not accumulate as much as with larger grains (Ref 48). composite coatings without saccharin (Fig. 4 and 7a), the
Taking into account the above considerations, it can be deduced higher hardness in this case is more strongly correlated with the
that the saccharin additive is an effective residual stress reducer refinement of the Ni matrix grains than with the embedding of
in the Ni/Al2O3 coatings. The character of the determined Al2O3. The mechanism of saccharin acting as a grain refiner
residual stresses agreed with those recorded by Erler et al. (Ref during the electrodeposition of Ni is due to: (i) blocking of the
48) for Ni/Al2O3 by means of in situ measurements of the strip surface by the formation of complex deposits, which increases
contraction. They estimated lower values of stresses (less than the frequency of nucleation and decreases the diffusion of the
170 MPa), which was probably related to the content of sodium adsorbed Ni ions on the cathode, thus retarding the crystal
dodecyl sulfate in the electrolyte and a different method used to growth (Ref 32-37), (ii) hydrogen evolution on the cathode, (iii)
measure them. However, the estimated tensile stresses were in changing of the cathodic overpotential (Ref 32, 38). As
contradiction with the compressive stresses (841.9 MPa) in presented in Ref 43 the effect of the saccharin on the Ni
Ni coatings produced with the use of pulse plating from a bath crystallite size refinement was much larger than that of Al2O3
containing saccharin and sodium lauryl sulfonate, presented by nanoparticles. The Ni/Al2O3-80 + S coating possessed the
El-Sherik et al. (Ref 49). crystallite size two times smaller than the Ni/Al2O3 coatings
obtained from the bath without saccharin. The coatings with
3.4 Mechanical Properties of Ni and Ni/Al2O3 smaller grains had a larger grain boundary area and, conse-
Nanocomposite Coatings quently, higher microhardness. The presence of saccharin in the
bath significantly enhanced the formation of growth-type
The indentation microhardness (H) of the deposited Ni/
nanotwins in the deposit. An increasing number of nanotwins
Al2O3 nanocomposite coatings revealed the opposite tendency
in the matrix caused an increase in the coating microhardness
to that of the residual stresses (Fig. 7a). The improved

2122—Volume 26(5) May 2017 Journal of Materials Engineering and Performance

Fig. 7 Mechanical properties of the coatings: indentation microhardness (a), load-penetration depth behavior of Ni and Ni/Al2O3-40, Ni/Al2O3-
80, Ni/Al2O3-80 + S (b), SEM BSE microstructures of indentation imprints on the surface of Ni/Al2O3-80 (c), Youngs modulus of coatings (d)

Table 2 Results of microhardness and Youngs modulus measured for Ni and Ni/Al2O3 coatings
Coating Indentation microhardness H, GPa Youngs modulus E, GPa H/E

Ni 3.42 ± 0.35 210 ± 8 0.0163

Ni/Al2O3-20 3.54 ± 0.32 208 ± 4 0.0170
Ni/Al2O3-40 3.69 ± 0.27 201 ± 10 0.0184
Ni/Al2O3-60 4.29 ± 0.35 232 ± 12 0.0185
Ni/Al2O3-80 4.40 ± 0.53 221 ± 18 0.0199
Ni/Al2O3 + S 5.30 ± 0.44 229 ± 14 0.0231

because the nanotwin boundaries blocked the motion of The results of Youngs modulus measured for the coatings
dislocations in the matrix to obtain higher mechanical strength. produced from the bath containing various amounts of a
Figure 7(b) presents an exemplary indentation load versus ceramic phase and saccharin are presented in Fig. 7(d). Youngs
penetration depth hysteresis for Ni and three Ni/Al2O3 modulus remained on the level of 210-232 GPa. The highest
nanocomposite coatings. The lowest penetration depth at 50 values were revealed by the coatings Ni/Al2O3-60 (232 GPa)
mN load was obtained for the Ni/Al2O3-80 + S coatings and Ni/Al2O3-80 + S (229 GPa). Interestingly, these values of
obtained from the electrolyte with the saccharin additive and E corresponded to the lowest values of residual stresses in these
the highest penetration depth for the pure Ni deposit, which coatings, 219 and 193 MPa, respectively. Moreover, the ratio
correlates inversely with the results of microhardness presented between the microhardness (H) and the elastic modulus (E) was
in Fig. 7(a). The SEM images (Fig. 7c) of the indents after the calculated, because, as presented by Leyland et al. (Ref 52), it
Vickers indentation showed an elasto-plastic character of the might be a suitable parameter for the foreseeing of the wear
deformation. No circumferential or corner cracks were found behavior of a coating. It was so-called elastic strain to failure
for the nanocomposite coatings. Additionally, the indentation (H/E), and it is considered as a reliable indicator of a good wear
imprint observed in the area containing more of the ceramic resistance in a coating. According to Ref 52, the most durable
phase was approximately the same as that in the area with fewer coatings can be obtained if H/E has a high value, i.e.,
particles, which indicates that the amount of the ceramic phase sufficiently high hardness (to resist plastic deformation), but
could be higher under the indent. This testifies the coatings with a low elastic modulus (similar to, or slightly below that of
homogeneity, which was confirmed by only a 10% scatter of the substrate material). The values of H/E calculated for the Ni,
the indentation results. Ni/Al2O3-20, Ni/Al2O3-40, Ni/Al2O3-60 Ni/Al2O3-80 and Ni/

Journal of Materials Engineering and Performance Volume 26(5) May 2017—2123

Al2O3-80 + S coatings are presented in Table 2. They show the wear index. The volume of the waste material was the
that the best wear resistance should be exhibited by the Ni/ volume of the grooves reduced by the uplifted volume. The
Al2O3-80 + S coating. In the case of the other Ni/Al2O3 wear resistances of the Ni/Al2O3 nanocomposite coatings were
nanocomposite coatings, the wear resistance should increase strongly related to the Al2O3 nanoparticles content in the Ni
with the increasing amount of the ceramic particles incorpo- matrix. Figure 8 shows the relationship between the particles
rated into the coating. concentration in the electrolyte and the wear index. The results
indicated that the wear resistance increased with the Al2O3
particles content in the electrolyte and later the volume
3.5 Tribological Properties of Ni and Ni/Al2O3 Coatings
fraction of nanoalumina in the deposited layer. It is evident
The wear behavior of the Ni and Ni/Al2O3-20, Ni/Al2O3-40, from Fig. 8-10 that the Ni/Al2O3 nanocomposite coatings
Ni/Al2O3-60, Ni/Al2O3-80, Ni/Al2O3-80 + S coatings was exhibited a better wear resistance than the pure Ni coating in a
examined under dry sliding conditions. The measurements of sliding contact with the alumina ball. The Ni/Al2O3-80 coating
the friction track profiles of the samples showed the presence of exhibited a three times lower wear than the Ni coating and the
high volumes of uplifted material located at both sides of the specific wear rate reached the value of 0.9 9 106 and
groove. As the size of these uplifted materials was 15-20% of 2.9 9 106 mm3/Nm, respectively. This wear index was in the
the grooves, they were taken into account in the calculation of same range as the value reported by Aruna et al. (Ref 12)
(9.419 107 for a Ni/Al2O3 coating with a-Al2O3 nanoparti-
cles). This can be attributed to the hard nature of the
reinforcements and the dispersion-strengthening effect with
the incorporation of the ceramic nanoparticles. As shown in
Fig. 3, the coatings structure contained numerous nanotwins.
There were the growth-type (111) nanotwins observed along
the [011] zone axis and their size decreased with the increasing
amount of built Al2O3 nanoparticles and decreasing size of Ni
grains (Ref 43). The higher nucleation, due to the nanoparticle
incorporation, disturbed the growth of the nickel matrix and
resulted in its smaller grain size. The nanocrystalline matrix
besides nanotwins revealed other structure defects, such as
stacking faults and dislocations. The most number of these
defects was observed in the structure of the Ni/Al2O3-80 + S
coatings. These coatings with the smallest the grain size
revealed the smallest twin lamellae, and the highest mechanical
and tribological properties. This is related to the fact that
dislocation motion in the matrix is blocked by the nanotwin
boundaries, and therefore, they required the higher external
Fig. 8 Wear index determined for pure Ni and Ni/Al2O3 nanocom- stress to cross the twin boundary. Such morphology was
posite coatings produced from the electrolyte containing various beneficial for the improvement in the wear resistance, since it
amounts Al2O3 nanoparticles and saccharin additive could increase the load-carrying capacity of the coatings. In this

Fig. 9 SEM BSE microstructures of wear tracks after wear tests of coatings: Ni (a), Ni/Al2O3-20 (b), Ni/Al2O3-40 (c), Ni/Al2O3-60 (d), Ni/
Al2O3-80 (e), Ni/Al2O3-80 + S (f)

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Fig. 10 High magnification SEM BSE microstructures of wear tracks after wear tests of the coatings: Ni (a), Ni/Al2O3-20 (b), Ni/Al2O3-40 (c),
Ni/Al2O3-60 (d), Ni/Al2O3-80 (e), Ni/Al2O3-80 + S (f)

case, the matrix carried the load and the fine particles impeded deformation with microcracks of worn layers transferred
the motion of dislocations (Ref 53). With the grain refinement between the counter body ball and the composite interfaces.
of the Ni matrix, the load-carrying capacity and the resistance The higher amount of Al2O3 nanoparticles in the coatings
to plastic deformation increased (Ref 18). It was especially reduced plastic deformation zones and changed the wear type
visible in the case of the Ni/Al2O3-80 + S coating, where it was to abrasion. Some delamination was the result of debris
impossible to calculate the wear index after 20,000 cycles. A smearing on the composite surfaces, and fatigue crack growth
destruction of this coating was constituted by a plurality of mechanisms subsequently caused material removal from the
scratches which were observed in the area of the friction track. composite surfaces. An addition of the saccharin to the
However, an apparent deep wiping was not visible. That is why electrolyte produced less amount of wear debris smeared on
additional tests in an extended time (80,000 cycles) of the the surface. The higher vol.% of the Al2O3 nanoparticles
samples collaboration with the ball surface were performed. incorporated into the coating enhanced the coatings degree
The wear of this coating was abrasive. The volume of the of wear resistance, which may be attributed to the higher
uplifted material on both sides of the grooves comprised 7% of microhardness corresponding to the higher load bearing
the total volume of the furrow, so it was negligible and did not capability and lower ductility (Ref 54). The better wear
take a significant part in the fissuring. The coating revealed the coating resistance indicated the high strength of the particles
highest wear resistance of all the examined Ni/Al2O3 coatings. to the metal matrix bonds.
The incorporated nanoparticles reduced the direct contact It was shown that, after a short running-in stage at the
between the metal matrix and the Al2O3 ball during the beginning of the test, the friction coefficient (COF) of
tribological test, which reduced the adhesive wear between the nanocomposites entered a steady-state period. However, for
metal and the ball. The wear mechanism of pure nickel and the Ni/Al2O3-80 + S, similarly as for the Ni coating, it exhibited a
composite coatings was analyzed by SEM observations of the change during 18,000 cycles, maintaining an upward trend by
wear tracks, as shown in Fig. 9 and 10. From the low keeping a stable value during the test of 0.31 and 0.45,
magnification SEM micrographs (Fig. 9), it can be seen that the respectively. The same character of the curves suggested the
lowest wear appeared in the coating produced from the bath friction coefficient in this composite depending to a large extent
containing 80 g/L Al2O3 and 1 g/L saccharin. The Ni/Al2O3 on the matrix characteristics. The other Ni/Al2O3 nanocom-
coatings obtained from the bath containing more than 40 g/L posites showed a much more stable friction coefficient with a
Al2O3 particles exhibited a better wear resistance than the pure similar value (0.31-0.34), as shown in Fig. 11, and its value did
Ni coating when sliding against the alumina ball. Compared not change significantly with the increasing ceramic particle
with the pure Ni coating, the worn surface of the Ni/Al2O3 content in the electrolyte. Figure 11 shows that the Ni/Al2O3
composite coatings decreased with the increasing amount of the nanocomposites exhibited a lower friction coefficient (more
ceramic particles. Wear track of pure Ni coating exhibited than 30%) than the Ni deposit under identical wear test
dominant adhesive wear mechanism, whereas Ni/Al2O3 conditions. The coatings Ni/Al2O3-20 and Ni/Al2O3-40 showed
composites showed a preferably abrasive type of wear, practically the same values 0.31, the coatings Ni/Al2O3-
whose predominance increased with the increasing alumina 80—0.34, and the smallest value was achieved for Ni/Al2O3-
content. Some rows of grooves, smearing and plastic 60. The lower friction coefficient can be explained in terms of
deformation were seen in wear tracks at higher magnification good interfacial bonding between Ni and the ceramic particles.
SEM images, as shown in Fig. 10. The plastic deformation The fine surface morphology of the nanocomposite coating
occurred by smearing of the wear debris on the alumina ball probably increased the load-carrying area and reduced the stress
was also observed. The surfaces of Ni/Al2O3 showed plastic between the friction couples. The lower friction coefficient of

Journal of Materials Engineering and Performance Volume 26(5) May 2017—2125

 case of the friction coefficient. Instead, the wear resistance of
the coatings corresponded very well with the predictions
resulting from the determined values of H/E. The best wear
resistance was revealed by the Ni/Al2O3-80 + S coating, which
was related to a significant grain refinement of the Ni matrix.

4. Conclusions

This paper presents a characterization of the surface

topography, as well as the mechanical and tribological prop-
erties of thin nanocomposite Ni/Al2O3 coatings electrode-
posited from the Watts bath containing various amounts (20,
Fig. 11 Variation of the friction coefficient of nickel and Ni/Al2O3 40, 60, 80 g/L) of Al2O3 nanoparticles. The obtained results are
nanocomposite coatings with sliding cycles shown below.
the composite coating could be explained by the ‘‘microball 1. The co-deposition of a-Al2O3 particles into the nickel
bearing’’ effect of the nanoparticles during sliding (Ref 28). matrix provided a refinement of the nickel grain sizes
The presented values of COF are much lower than those and a significant improvement in the coating properties,
obtained by Aruna et al. (0.819) and Saha et al. (0.5) (Ref 12, such as microhardness, wear resistance and friction coef-
31). Gul et al. (Ref 11) have shown changes of the coefficient of ficient, compared with the pure nickel coatings.
friction depending on the kind and values of the current density 2. The Ni/Al2O3 nanocomposite coatings showed an evident
as well as the sliding speed determined for the coatings relationship between their composition and microhard-
obtained from the bath containing HPB surfactant. They ness, which increased (30%) with the increase in the
demonstrated that the coefficient of friction decreased with amounts of incorporated particles (up to 9.9 vol.%). This
the increasing sliding speed and it achieved the value below 0.2 was because the composite coating was strengthened by
for the sliding speed of 150 mm/s. the fine crystal and the hard particle dispersion intensifi-
cation. The coatings hardening corresponded to the rise
3.6 Correlation Between Surface Topography and Friction in the wear resistance.
Coefficient as Well as Wear Resistance 3. The incorporation of Al2O3 into the Ni matrix improved
The friction coefficient was found to depend on the surface the wear resistance of the Ni deposits. The wear index
roughness, and it was higher for rougher surfaces. The decreased with the rise in the amount of alumina
performed examinations showed that the pure Ni coatings nanoparticles. The Ni/Al2O3-80 coatings deposited from
revealed the highest friction coefficient (Fig. 11). In general, we the solution containing 80 g/L of Al2O3 exhibited a three
can ascertain that this coating exhibited the values of all the times lower wear index than the pure Ni coatings.
surface topography parameters being significantly higher than 4. The friction coefficient was found to depend on the sur-
those of the composite Ni/Al2O3 coatings. The Ni coating face roughness, and it was lower for smoother surfaces
revealed a deviation from the Gaussian distribution with the of the coatings. The wear resistance of the coatings did
surfaces of negative asymmetry (Ssk = 0.867) and great not show a distinct dependence on the surface topogra-
sharpness of the profile (Sku = 5.9688). Of all the Ni/Al2O3 phy. It affected only the initial process of wear.
composite coatings, that obtained from the bath containing 5. All the coatings revealed tensile residual stresses, which
80 g/L a-Al2O3 showed the highest COF, which was, however, were insignificantly (20%) reduced as the amount of
significantly lower than that of the Ni coating. It can also be incorporated Al2O3 nanoparticles increased.
noticed that the friction tends to be lower for the coatings Ni/ 6. The addition of 1 g/L of saccharin into the electrolyte
Al2O3-20, Ni/Al2O3-40, Ni/Al2O3-80 + S—its value was al- did not enhance the incorporation of ceramic particles
most the same after 20,000 cycles (Fig. 11). This agreed with into the coating. However, it had a positive impact on
the surface topography parameters determined for the Ni/ the microstructure refinement of the matrix, the micro-
Al2O3-20, Ni/Al2O3-80 + S coatings, which were very similar hardness increase and the residual stress reduction in the
(Table 1). Moreover, the skewness parameter Ssk was close to coatings.
zero and the kurtosis Sku was close to 3, which proves the 7. Compared to the electrodeposited pure nickel, the Ni/
Gaussian-type distribution (Ssk = 0, Sku = 3). The Ni/Al2O3-80 Al2O3 composite with nanoparticles exhibited a higher
coating revealed significantly higher values of each measured microhardness and a better wear resistance. The best
parameter, which was reflected in a slightly higher friction mechanical and tribological properties were revealed by
coefficient (Fig. 11). Interestingly, although Ni/Al2O3-80 dis- the Ni/Al2O3-80 + S coating.
closed a similar kurtosis as the Ni coating, the skewness 8. The studies have shown that the friction coefficient and
parameter (Ssk = 0.879) was positive, contrary to Ni. The the wear resistance of the Ni/Al2O3 coatings can be pre-
obtained results stayed in agreement with (Ref 39), who dicted in advance on the basis of the surface roughness
showed that a positive skewness reduced the coefficient of measurements and the elastic strain to failure calculations
friction, while in the case of a negative skewness, the friction is (H/E). The Ni/Al2O3 nanocomposite coatings were char-
more intense than the Gaussian distribution. acterized by a low wear index and friction coefficient,
Regarding the wear resistance of the coatings, it did not which is very promising in the perspective of their use as
show a distinct dependence on the surface topography, as is the a replacement for hard chromium coatings.

2126—Volume 26(5) May 2017 Journal of Materials Engineering and Performance

Acknowledgments 17. N.S. Qu, D. Zhu, and K.C. Chan, Fabrication of Ni-CeO2 Nanocom-
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to the original author(s) and the source, provide a link to the 23. Directive 2000/53/EC—the ELV Directive
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2128—Volume 26(5) May 2017 Journal of Materials Engineering and Performance