Tribology International 98 (2016) 253–260

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

Tribological performance of PEO-WC nanocomposite coating on Mg

Alloys deposited by Plasma Electrolytic Oxidation
Hadi NasiriVatan, Reza Ebrahimi-Kahrizsangi n, Masoud Kasiri Asgarani
Advanced Materials Research Center, Materials Engineering Department, Najafabad Branch, Islamic Azad University, Najafabad, Isfahan, Iran.

art ic l e i nf o a b s t r a c t

Article history: AZ31B Mg alloy specimens were coated by PEO technique in WC nano-powder containing phosphate
Received 18 July 2015 based electrolyte under constant current densities. Wear rate and COF diagrams were plotted in order to
Received in revised form investigation of WC nano-particles presence and it was found that nano-particle presence can decrease
6 February 2016
wear rate and COF significantly down to 77% and 55%, respectively. Cross sectional imaging showed that
Accepted 22 February 2016
Available online 3 March 2016
coating thickness increase with coating time and in case of nano-particle containing coatings become
more compact but thickness decreases slightly. Investigation of surface morphology indicated that in
Keywords: presence of nano-powder, porosity as well as mean diameter of pores decreased, but prolonging coating
PEO time even in presence of nano-powder, led to mean diameter of pores reached up to 8.34 mm. Presence of
Wear
nano-powders, also increased hardness of coatings considerably.
Nano-composite coating
& 2016 Elsevier Ltd. All rights reserved.
AZ31B Mg Alloys

1. Introduction of surface composition by Radio-frequency plasma chemical vapor

Tungsten in carbide form has broad and important applications
in industries as a refractory metal. According to proper hardness
and high wear resistance of Tungsten Carbide (WC), it has vast
applications as a hard material in metal working and drilling
industries and also mining industries under high pressure and
temperature [1–3].
Magnesium and Aluminum are usually used in weight-critical
structural applications, for example vehicles and aerospace. Mg is
about 35% lighter than Al, and both have similar melting point and
strength. Mg has the drawback of limited formability, duo to its HCP
structure, while Al has high formability as it is in FCC structure [4,5].
Mg alloys also has lower elastic module than Al, 40–45 GPa for Mg
alloys in comparison to 69.6 for Al alloys. Mg alloys have promising
applications in some number of areas in industries including
automotive, aerospace, computer and IT through their low density
and high specific strength and hardness. However their applications
are strictly limited through their low thermal resistance. Up to now
various techniques have been used to overcome these limitations of
Mg alloys including anodizing [6], deposition of metallic resistant
coatings [7], surface melting by laser beam [8], purification of cast
leading to better wear and corrosion resistance [9] and modification
n
Corresponding author at: Advanced Materials Research Center, Materials
Engineering Department, Najafabad Branch, Islamic Azad University, Najafabad,
Isfahan, Iran.
E-mail addresses: hadinasirivattan@gmail.com (H. NasiriVatan),
rezaebrahimi@iaun.ac.ir (R. Ebrahimi-Kahrizsangi).
deposition (RF-CVD) [10]. Performing a surface protective process is
suitable for Mg alloys [11].
Appling coatings in order to eliminate limitations of metal
applications and to achieve maximum performance in them, is a
way to simultaneously achieve protection against wear and keep
mechanical behavior of base metal. Composite coatings duo to vast
practical applications have significant industrial importance. Pre-
sence of nano-particles in composite coatings as hard and wear
resistance materials are in high interests. Generally hard ceramic
particles such as alumina, tungsten carbide and silicon carbide are
used in order to increase composite coatings hardness [12].
Plasma Electrolytic Oxidation is a process similar to anodizing
performed at high voltages, applied on light metals above dielec-
tric breakdown of coating, in which a high crystallinity thick
coating with desired properties is formed. This process leads to
formation of plasma as micro discharges on metal surface and gas
liberation. Short lifetime (about hundred ms to a few ms) micro
discharges define chemical and thermal situations and play a
significant role in phase formation, composition and morphology
of oxide coatings [13]. These sparks lead to forming plasma
channels which in chemical reactions occur and cause to fabricate
products (coating). Xin et al. [14] showed that type of current-AC
or DC- applied for PEO coating process can alter the phase com-
position and consequently density, hardness and corrosion resis-
tance of formed coating on Al alloy. Guangliang et al. [15] found
that high and low current density lead to fabricate mainly γ-Al2O3
and α-Al2O3 respectively on Al alloy substrate. PEO is an envir-
onmentally friendly and commodious process drawing attentions

http://dx.doi.org/10.1016/j.triboint.2016.02.029
0301-679X/& 2016 Elsevier Ltd. All rights reserved.
254 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260

to itself since it is a new method of producing ceramic coatings Table 1

with unique properties on valve metals, such as Al, Mg and Ti and Composition of AZ31B alloy used in this study as substrate of coating.
their alloys [16]. Wear resistance, mechanical strength and elec-
element Mg Zn Si Mn Fe Cu Al
trical insulation of these metals and their alloys could be improved
by PEO process [17]. Generally PEO is accepted as a prospective Wt% Balance 1.00–1.15 Max 0.2–0.4 Max 0.00– 2.5–3.5
surface treatment for Mg alloys. Ceramic coatings could be formed 0.022 0.003 0.030
in-situ in silicate based electrolytes, consisted of mostly MgO,
Mg2SiO4 and MgAl2O4 [18]. These coatings have high hardness
values and wear resistance comparing to uncoated substrate under
proper conditions of coating process, and perform good electro-
magnetic performance. Wheeler et al. [19] compared mechanical
properties of coatings fabricated by hard anodizing and PEO pro-
cess on 5056 AA indicating very better behavior of PEO coating.
Unfortunately they crack easily and fall of which leads to loosing
protection of Mg alloys, since these oxide ceramic composite
coatings show high illuminations and their expansion coefficient
differ significantly from Mg alloys. It has reported that PEO coat-
ings are porous in outer layers which is a drawback in tribological
and wear performances. PEO is a complex process which reacts
components of electrolyte after diffusion and electrophoresis
through discharge channels and electrochemical oxidation on the
metal surface. It has reported that electrolyte components parti-
cipate in PEO process. Tong et al. introduced silicon oxide [20] and
iron [21] particles into electrolyte and realized that they can
embed in ceramic matrix and produce denser coatings.
Present research attempts to study effects of process para-
meters on nano-composite coating properties, thickness and type.
It mainly focuses on study of wear properties surface morphology
and composition of WC nano-composite coatings produced by PEO
process. Wear resistance is studied through coefficient of friction
and wear rate.

2. Materials and methods

Samples used in this study were AZ31B prepared in square

shape with thickness of 2 mm acquired from Bohler with com-
Fig. 1. TEM image of WC nanoparticles embedded into some coatings.
position presented in Table 1. Sample preparation included
grinding with abrasive SiC papers in 5 meshes including 200, 800,
1200, 2500 and 4000. Deionized water and hot air flow were used
to wash and dry samples, respectively. In order to connect anode Table 2
to samples, they were drilled and screwed from smallest surface to Condition of PEO coating process in terms of coating time and presence of nano-
attach the anode electrode. In order to obtain more reliable results powder in the electrolyte. Specification of coatings fabricated by PEO process. Pore
diameter, cross thickness and porosity percentage are evaluated by analyzing
statistically, according to repeatability of each process, for each
SEM image.
series of experiment at least three samples were used.
Electrolyte composition used in PEO process was based on 4 g/lit Sample code Nanopowder Time of coating deposition (min)
sodium phosphate (Na3PO4) with 1.5 g/lit KOH and in 4 cases WC
NP5 WC 5
nanoparticles with diameter less than 80 nm (Fig. 1) were added in
NP10 WC 10
5 g/lit concentration. Philips-CM120 TEM was used to determine NP15 WC 15
nanoparticle size. A&D-GR202 balance with 50 mg accuracy was NP20 WC 20
used for weighing the samples. To achieve a uniform distribution of SS5 – 5
SS10
10
nanoparticles in fabricated coatings, suspension was stirred for 6 h
SS15
15
on magnetic stirrer before coating process as well as during coating SS20
20
process.
PEO station consists of a 20 KW power supply, a rectifier with
maximum output voltage of 600 V and electrolyte container with process, samples were rinsed with distilled water and dried in
water cooling system which maintained temperatures below warm air flow (Table 2).
30 °C. The current and potential difference between anode (sam- To investigate the morphology of free surface of coatings, cross
ple) and cathode was measured by two separated avometers section and composition of coatings, WEGA TESCAN SEM with
APPA-series 500 connected to a computer to plot potential-time RONTEC EDS analyzer and ZEISS SIGMA/VP SEM were used. ImageJ
diagram during coating process. During coating process, applied software was used to analyze SEM micrographs to calculate per-
current density was maintained constant equal to 55.02 A/cm2. centage of porosity, pore dimension and coating thickness; the
Coating times were 300, 600, 900 and 1200 s. After coating error of this method is quietly related to statistical techniques so
 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260
that according to calibration of the gauge of software, for example
for each measurement in term of unit ‘mm’, the value of error
would be 0.5 mm. Furthermore QnIX8500 instrument was used to
measure coating thickness so that for each sample, 18 measure-
ment were performed. Surface roughness (Ra) of coatings was
evaluated using Taylor Hobson Sutronic25-Stylus type surface
Fig. 2. Potential variations between anode (sample) and cathode (water cooling
stainless steel) in term of time during coating process for two samples coated for
1200 s.
Fig. 3. SEM images captured from free surface of coatings (a) NP5, (b) NP10, (c) NP15, (d) NP20, (e) SS5, (f) SS10, (g) SS15, (h) SS20.
255
profilometer with 710 nm accuracy. This analysis was carried out
3 times for each sample and mean values were reported. In order
to investigate wear resistance and coefficient of friction of sam-
ples, pin on disk wear test was performed according to ASTM G-99
standard, applying 1.2 kgf and 0.5 kgf on pin for measuring COF
and wear rate respectively with 5 mm round head pin made of
WC-Co cermet in room temperature and ambience humidity.
Mean coefficient of friction is obtained by averaging from all data
of COF throughout the sliding pin on surface of coating after
1500 cm distance with 5 cm/s linear speed. Hardness of coatings
was evaluated by SCTMC-MHV1000 with 0.5 HVN equipped by
prismatic indenter according to E-384 ASTM standard.
3. Results and discussion
Fig. 2 Presents potential variations versus time for samples
coated for 1200 s. Samples coated in shorter times showed very
good sameness with these curves, so duo to high resemblance, only
curves for samples coated for longest times with and without pre-
sence of nano-powder are presented here. Results are in agreement
with previous studies [22] and show that samples coated in elec-
trolyte containing nano-powder have 10 to 15 V lower sparking
voltages in comparison to samples coated in electrolyte without
nano-powder. In initial stages of sparking, the size of sparks is
256 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260

Fig. 4. EDS maps illustrating distribution of considered elements in free surface of coatings NP5. This image were obtained by EDS probe connected to SEM microscope.

Fig. 5. SEM images captured from cross section of coatings. (a) NP5, (b) NP10, (c) NP15, (d) NP20, (e) SS5, (f) SS10, (g) SS15, (h) SS20. Both types of close and open pores can
be observed in these images.

smaller leading to create less porous coating with higher electrical
resistance; therefore to maintain current density constant, more
rate of voltage increase is demanded. But after about 100 s of
coating process as growth of coatings takes place, sparks become
larger leading to create more porous coating layers having less
electrical resistance, hence less rate of voltage increase is required
[23]. Nano-composite coating containing nano-powder has lower
resistances in comparison to coating without nano-powder. This
can be attributed to some reasons such as less porosity of nano-
composite coatings, lower energy required for formation of coating
in presence of nano-particles, etc. which will be discussed later. In
addition, voltage-time diagrams of sample containing nano-powder
are much more uniform and with less fluctuations, showing more
uniform formation of coating during PEO process.
Fig. 3 shows SEM images captured from free surface of coatings
and Fig. 4 illustrates typically distribution of elements on surface of
coating NP5 containing nano-powder. To study morphology of coat-
ings with more details, SEM images from cross section of coatings are
presented in Fig. 5. Table 2 represents weight, thickness, porosity and
mean pore diameter of coatings. It can be observed that the structure
of coatings become coarser by increasing coating time for both types
of ordinary and nano-composite coatings. Addition of nano-powder
decreases mean pore diameter from 8.42 mm for samples without
nano-powder to 7.19 mm for samples with nano-powder and also
decreases mean surface porosity from 10.59% for samples without
nano-powder to 9.81% for samples with nano-powder. Introduction of
nano-powders leads to more decrease of pore diameter (about 15%)
than porosity percentage (less than 1%). If porosity percentage can be
 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260 257

Fig. 6. EDS maps illustrating distribution of considered elements in cross section of coating NP5.

Fig. 7. EDS map obtained from SEM image with high magnification from a single pore at free surface of sample NP15: (a) outside and (b) bottom of pore.

estimated as Eq. (1): d¼ mean pore diameter;

A¼unit area.
P ¼ ðnπ d^2Þ=4A  100 ð1Þ According to proportional of P to square of d and less decrease of P
where in: than value should be decreased corresponding to decrease of d, one
P ¼porosity percentage; can conclude that introduction of nano-powders leads to increase of
n ¼number of circular pores per unit area; number of pores in unit area. In presence of nano-powder, the outfalls
258 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260

Fig. 8. Variations of coefficient of friction during sliding the pin on free surface of coating for (a) samples with nano-powder and (b) samples without nano-powder.

of pores become more closed, therefore porosity and mean pore

diameter are decreased with addition of nano-powder, implying good
agreement with similar works on nano-composite PEO coatings [24].
Additionally, all weight changes between before and after coating
process, are positive for both coatings with and without nano-parti-
cles, indicating that coating formation rate is more than substrate
dissolution rate [25]. As it can be realized from data presented in
Table 2 and as expected, increase of coating time leads to increase of
weight change. In addition, investigation of coating thickness with
probe shows that thickness increases with coating time.
As presented in Fig. 4, all considered elements, even W, dis-
tribute uniformly in coating, showing uniform distribution of
nano-particles in coating and indicates no agglomeration has
taken place during coating process [26]. Mean thicknesses mea-
sured by Image-J software from Fig. 5 are listed in Table 2, again
show that increase of coating time results in increase of thickness.
Fragments of coating dispatched from samples during metallo-
graphy, in mount region implies ceramic nature of coatings. It
seems that addition of nano-powder increases compactness of Fig. 9. SEM micrographs of worn surface for sample NP5.
coatings and, in turn, decreases thickness of them. These results
are in accordance with other findings in nano-composite PEO
coatings [27]. Although increasing trend of thicknesses obtained thickness leading to completely elimination of coating in early
from analyzing SEM images is almost same as that resulted from
stages of wear test. Addition of nano-particles to coatings led to
measurement by probe, there is considerable difference between
increase in hardness, 442 Hv0.1 for coating fabricated in the most
thicknesses measured by probe and those obtained from analyzing
coating time. Surface composition of coatings with and without
cross section SEM images. This 1.8–2.7 times larger values of
nano-powder does not differ much; however presence of nano-
thicknesses measured by probe might be due to high porosity and
unevenness of free surface of coatings which can affect on mea- powder decreases wear rate and wear track width significantly. On
sured value of thickness. the other hand presence of nano-powder, does not affect hardness
Fig. 6 shows typically map of element distribution in cross considerably which can be attributed to unchanging the compo-
section of coating NP5, and as it can be obviously observed all sition of coating, which consists of mainly MgSiO4, MgO and Mg
elements, including W, are uniformly distributed across coating. (OH)2 and insufficient content of nano-powder for filling pores to
Fig. 7 demonstrates a single pore from sample NP15 containing the desired level that can enhance the hardness of porous coating.
WC nano-powder, and apparently nano-particles are absorbed and Presence of nano-powder in coatings decreases wear rate from
trapped inside of pores, particularly in bottom of them so that 28.65  10
4 to 6.67  10
4 mg m
1 N
1 and wear track width
walls of pores contain less nano-particles [28,29]. Somewhat open from 1801 mm to 491 mm for coating created in the most coating
pores with links together can be seen in this figure. time (Table 4).
Fig. 8 shows variation of COF during wear test, and Fig. 9 shows Fig. 10 shows images and element distribution in coatings after
typically SEM image of worn surface of coating NP5. Table 3 pre-
wear test. According to good wear behavior of NP20 sample, EDS
sents extracted data from wear test including wear rate, wear track
analysis confirms that owing to uniform distribution of W over the
width and COF as well as hardness and roughness of coatings.
cross of coating, even after removing portion of coating because of
Almost all samples without nano-powder reveal similar behavior
and have close mean COF values. By embedding nano-powder into wear, still distribution of W is uniform leading to good wear
coatings, mean COF values begin to decrease [30–32]. As it is resistance of nano-composite coatings. Also continuous tracks of
evident from Fig. 8, samples containing nano-powder show similar wear and occurring no layer breakdown in worn samples, indi-
trend, except for sample NP5, which might be due to its very low cates very good cohesion and adhesion of coating to the substrate.
 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260 259

Table 3
Results extracted from wear and hardness test. Wear track width was measured from SEM image of worn samples. Much higher values of wear track width for ordinary
coatings can be attributed to less strength of them.

Sample Weight before Weight after Weight difference Average of hole dia- Probe thick- Surface Porosity Cross thick- Probe thickness
Cross thickness
code PEO (g) PEO (g) (mg) meter(lm) ness(lm) percent ness(lm)

NP5 4.26116 4.27405 12.89 5.34 16.94 8.94 6.34 2.67

NP10 4.44741 4.46789 20.48 7.32 23.09 9.11 10.15 2.27
NP15 4.97646 5.00452 28.06 7.76 28.37 10.47 12.06 2.35
NP20 4.16794 4.20017 32.23 8.34 28.42 10.71 14.76 1.93
SS5 4.89875 4.91424 15.49 7.01 17.50 11.78 9.67 1.81
SS10 2.73822 2.75956 21.34 8.35 25.37 10.47 11.49 2.21
SS15 5.19725 5.22893 31.68 9.04 30.27 10.48 12.58 2.41
SS20 4.80496 4.84384 38.88 9.29 34.47 9.62 18.30 1.88

Table 4

Sample Average of friction Wear track width (lm) Wear Rate (mg/(m N)) Hardness (Hv0.1) Rughness (Ra)(lm)
code coefficient 7 0.005 7 0.5 mm  10
4 70.005 7 0.5 HVN 7 10 nm

NP5 0.23 1165 9.71 232 0.99

NP10 0.19 1114 9.14 244 1.36
NP15 0.15 495 6.86 231 1.68
NP20 0.14 491 6.67 442 2.46
SS5 0.34 1318 22.94 220 1.14
SS10 0.31 1474 22.54 320 1.52
SS15 0.33 1534 24.29 231 1.95
SS20 0.31 1801 28.65 408 2.13

Fig. 10. EDS map obtained from SEM image of coatings after wear test illustrate element distribution in and around wear track: (d) NP20, (e) SS5, (f) SS10, (g) SS15, (h) SS20.
260 H. NasiriVatan et al. / Tribology International 98 (2016) 253–260
4. Conclusions
In this article, effect of coating time and presence of WC nano-
powder in PEO nano-composite coatings was studied. Samples
coated in suspension including nano-powder had 10–15 V less
sparking voltage in comparison to samples without nano-powder.
Addition of nano-powder decreases mean pore diameter averagely
15% for samples with nano-powder comparing to to samples
without nano-powder and also decreases averagely 6% mean
surface porosity. Samples containing nano-powder were more
compact comparing to ones without nano-powder. Distribution of
elements over structure of coating was uniform and nano-particle
absorbance was occurred inside pores, mainly at the bottom of
them and walls of pores absorbed less nano-particles. No layer
breakdown phenomena or non-uniform abrasion was observed in
samples during wear test. By addition of nano-powder, mean value
of COF was decreased averagely 45%. Agglomeration of nano-
powders did not occur inside wear track. With introducing
nano-particles into coating roughness did not change considerably
but hardness increased with coating time up to 442 Hv0.1.
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