J. Cent. South Univ.

(2014) 21: 4415−4423

DOI: 10.1007/s11771-014-2443-0

Microstructure and abrasive wear behaviour of anodizing composite films

containing SiC nanoparticles on Ti6Al4V alloy

LI Song-mei(李松梅), YU Xiu-mei(郁秀梅), LIU Jian-hua(刘建华), YU Mei(于美),

WU Liang(吴量), YANG Kang(杨康)

School of Materials Science and Engineering, Beihang University, Beijing 100191, China
© Central South University Press and Springer-Verlag Berlin Heidelberg 2014

Abstract: Anodized composite films containing SiC nanoparticles were synthesized on Ti6Al4V alloy by anodic oxidation procedure
in C4O6H4Na2 electrolyte. Scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray photoelectron
spectroscopy (XPS) were employed to characterize the morphology and composition of the films fabricated in the electrolytes with
and without addition of SiC nanoparticles. Results show that SiC particles can be successfully incorporated into the oxide film during
the anodizing process and preferentially concentrate within internal cavities and micro-cracks. The ball-on-disk sliding tests indicate
that SiC-containing oxide films register much lower wear rate than the oxide films without SiC under dry sliding condition. SiC
particles are likely to melt and then are oxidized by frictional heat during sliding tests. Potentiodynamic polarization behavior reveals
that the anodized alloy with SiC nanoparticles results in a reduction in passive current density to about 1.54×10-8 A/cm2, which is
more than two times lower than that of the TiO2 film (3.73×10-8 A/cm2). The synthesized composite film has good anti-wear and
anti-corrosion properties and the growth mechanism of nanocomposite film is also discussed.

Key words: Ti6Al4V alloy; anodic oxidation; SiC nanoparticle; composite film

improved through preparing proper hard films on their

1 Introduction
Titanium and its alloys have been extensively used
in aerospace industry, warship, and biomedical materials,
due to their high specific strength, good corrosion
resistance and excellent biocompatibility [1−2]. However,
titanium and its alloys constantly perform unstable
friction coefficient, severe abrasive and adhesive wear
which greatly limit their applications [3−4]. Therefore, it
seems necessary to find an appropriate way to improve
their wear resistance and mechanical characteristics.
Anodic oxidation is a traditional surface
modification method, by which a compound oxide film is
grown in-situ on valve-metals directly [5]. On one hand,
this technology is a more advantageous method because
of its low cost and easy operation; on the other hand, it
can greatly improve their resistance to wear, adhesion
and corrosion [1, 6−7]. YETIM [8] has reported that the
wear rate of CP-Ti significantly decreased with anodic
oxidation treatment in all wear conditions since oxide
film acted like a solid lubricant. Nevertheless, in some
severe friction conditions, anodizing films are unable to
meet the need of mechanical friction parts. It is believed
that the wear resistance of titanium and its alloys will be
surface [9]. One solution is to add appropriate
nanopowders in electrolyte during anodization process
for fabricating composite films [10]. Some nanoparticles
will deposit in the oxide layers through mechanical and
physical effect (or electrochemical action). This method
not only increases mechanical properties of the anodic
films, but also enhances their corrosion resistance and
thermal conductivity [10−12]. A number of
investigations of fabricating composite films on
aluminum alloys have been taken foremost [10−17].
CHEN et al [10] successfully prepared a composite film
containing superfine Al2O3 and PTFE particles on 2024
Al alloy using an anodizing method and the synthesized
films have good anti-wear and self-lubricating properties.
MATYKINA et al [16] investigated the incorporation of
zirconia into alumina-based films formed on aluminum.
They discovered that the nanoparticles were incorporated
mainly near the film surface and within cavities inside
the film.
During recent years, there is an increasing tendency
of studying composite films on titanium and its alloys [9,
18−20]. ALIOFKHAZRAEI et al [9] fabricated
Si 3 N 4 /TiO 2 composite films on commercially pure

Foundation item: Project(51271012) supported by the National Natural Science Foundation of China
Received date: 2013−09−02; Accepted date: 2013−12−25
Corresponding author: LI Song-mei, Professor, PhD; Tel/Fax: +86−10−82317103; E-mail: songmei_li@buaa.edu.cn
4416
titanium by plasma electrolytic oxidation (PEO). MU
et al [19] studied the preparation and tribological
properties of self-lubricating TiO2/graphite composite
film on Ti6Al4V alloy through PEO process. They
concluded that the graphite-containing oxide composite
film registered much lower friction coefficient and wear
rate than the oxide film without graphite under dry
sliding condition, exhibiting excellent self-lubricating
property.
However, the second phase incorporated to the base
alloy likely makes the material more sensitive to
corrosion in various environments. For example, metal
matrix composites (MMCs) consisting of Al-alloy 8090
reinforced with SiC particles have been proved to be
sensitive to corrosion in chloride-containing
environments [21]. Generally, the composite materials
are sensitive to corrosion in hostile environments, due to
either selective corrosion at the interface, galvanic
reactions between the reinforcements and the matrix, or
the defects at the interface, causing fissures which create
pathways for corrosion [22]. Moreover, few studies have
been done on composite films on titanium alloys through
anodic oxidation process. Therefore, we conducted this
study to fabricate a SiC reinforced composite film on
Ti6Al4V alloy through anodic oxidation in neutral
sodium tartrate solution for possible anti-wear and anti-
corrosion properties of the achieved films. The surface
characteristics, as well as the tribological properties and
electrochemical properties of SiC-containing anodic
oxide films, were analyzed.
2 Experimental
2.1 Preparation of oxide films
A forged block of Ti6Al4V alloy was cut into slices
with the dimensions of 1 mm×1 mm×0.5 mm. The
nominal components of Ti6Al4V alloy are given in
Table 1. Samples were abraded with silicon carbide
paper with continuous grades from 200 to 2000 grit
before anodizing treatment. Then, they were
ultrasonically cleaned in acetone solution, then rinsed in
de-ionized water and air dried, finally.
The anodizing process was conducted using a
direct-current (DC) pulse power source (WMY-V) in a
cell with a thermostat water bath and a magnetic stirring
apparatus. This cell consisted of Ti6Al4V sample as the
anode, 1Cr18Ni9Ti stainless steel plate as the cathode,
and 40 g/L C4O6H4Na2 solution as anodizing electrolyte.
Before being added into the electrolyte, 0.1 g/L SiC
powders (particle size of 40 nm) and 0.02 g/L additive
C12H25-OSO3Na (SDS) were ultrasonically dispersed for
1 h. The additive, SDS, a kind of anionic surfactant, was
added to make the SiC particles suspended and
negatively charged in the electrolyte. The parameters of
J. Cent. South Univ. (2014) 21: 4415−4423
anodizing process are given in Table 2. After the
treatment, the coated samples were rinsed with water and
then dried in the air.
Table 1 Nominal composition of Ti6Al4V alloy (mass
fraction, %)
Al V Fe C N O Ti
6.32 4.10 0.30 0.10 0.05 0.13 Bal.
Table 2 Parameters of fabrication process
Parameter Value
−2
Current density/(A·dm ) 7
Loading time/min 5
Anodizing time/min 60
Temperature/°C 20±2
Duty ratio/% 20
Frequency/Hz 2
2.2 Morphology and composition analyses
The micro-morphologies of surface and cross-
section of the anodizing films were examined using
scanning electron microscopy (SEM, Hitachi S-4800).
The nanocomposite film fabricated with the addition of
reinforced SiC particles was further examined by energy
dispersive spectroscopy (EDS) to determine the
distribution of Si and C elements in the film. In addition,
the chemical status of SiC in the film was examined by
X-ray photoelectron spectroscopy (XPS, Kratos-Axis
Ultra, using Al Kα radiation energy of 1486.8 eV).
2.3 Tribological and electrochemistry tests
The tribological tests were carried out with a ball-
on-flat contact configuration using a reciprocating
friction and wear test-rig of UMT-2MT (CETR, USA)
under dry conditions at room temperature with a load of
4 N and an oscillating amplitude of 6 mm for 30 min. A
Si3N4 ceramic ball with a diameter of 2 mm and surface
roughness Ra of about 0.01 µm was used as the
counter-face material. After the tests, a Phase Shift
Micro-XAM 3D surface profile was used to measure the
morphologies and depth profiles of wear tracks. Then,
making the area of wear track multiplied by the
oscillating amplitude could gain the wear volumes. Wear
rates of the samples could be calculated as
ω=V/(L×N) (1)
where ω is wear rate, V is wear volume, L is sliding
distance and N is load. Morphologies of the wear tracks
after the abrasion tests were examined by scanning
electron microscopy (SEM, Camscan CS3400) equipped
with EDS analysis.
Electrochemical tests were performed in a
J. Cent. South Univ. (2014) 21: 4415−4423
traditional three-electrode cell (with the oxide sample as
working electrode, a platinum electrode as counter
electrode and a Hg2Cl2/Hg electrode as reference
electrode) using a potentiostat/galvanostat (Parstat 2273,
USA) in a 3.5% NaCl solution. The scanning rate of the
potentiodynamic polarization curve was 0.5 mV/s, with a
scanning range from −0.25 V to +0.25 V vs the open
circuit potential. All experiments were carried out at
room temperature.
3 Results and discussion
3.1 Morphology and composition of films
The surface SEM morphologies of the oxide films
formed in the C4O6H4Na2 electrolyte without and with
SiC particles are shown in Fig. 1(a) and Fig. 1(b),
respectively. It is obvious that the surfaces of both films
are characterized by irregular petaloid drums and
micro-cracks, which is a normal morphology of samples
after anodic oxidation in the C4O6H4Na2 electrolyte [23].
On the basis of our former work, the occurrence of
petaloid drums and micro-cracks is attributable to the
explosion of oxygen bubbles which are emitted from the
electron transport channels at the beginning of dielectric
breakdown [23−24]. Irrespective of the addition of SiC
particles, there are no significant differences on the
surface between the oxide film and nanocomposite film.
It can be seen from Fig. 1(b) that SiC-rich particles are
non-uniformly distributed on the surface and many of
them appear to concentrate within internal cavities and
micro-cracks. The higher magnification SEM micrograph
Fig. 1 Surface SEM morphologies of oxide films formed in C4O6H4Na2 electrolyte: (a) Without SiC particles; (b) With SiC particles;
(c) High magnification of (b); (d) SiC particles
4417
of Fig. 1(b) is shown in Fig. 1(c). The particles with the
size of 40−60 nm are similar with the original particles
added into the electrolyte (Fig. 1(d)). EDS analysis of
local point A of the film surface reveals that titanium and
oxygen are the primary film constituents (Table 3), with
a Si molar fraction of 7.93%. The results clearly
demonstrate the incorporation of SiC particles into the
oxide film during the DC anodic oxidation procedure.
Figures 2(a) and 2(b) show the cross-sectional SEM
micrographs of the oxide films formed in the C4O6H4Na2
electrolyte without and with SiC particles, respectively. It
is revealed that the thickness of nanocomposite film
(35 µm) is slightly thicker than the particle-free film
(30 µm). Both films are well bonded with the substrate
and some micro-cracks can be observed in the films.
According to the EDS analysis, both the top of the
composite film (e.g. Point B in Fig. 2(b)) and the inner
regions (e.g. Point C in Fig. 2(b)) contain Si element
(Table 3). This infers that the SiC particles distribute
throughout most region of the coating. It can also be seen
that there are some white regions in the cross-section of
the film (Fig. 2(b)) and one region is examined more
closely (Figs. 2(c) and 2(d)). The size of the particles in
Fig. 2(d) is also similar to the added particles (Fig. 1(d)).
But one distinctive discovery is that the SiC particles are
embedded into the composite layer, forming an integral
part of it (Fig. 2(d)).
The X-ray photoelectron spectroscopy (XPS) is
introduced to examine the chemical status of SiC in the
nanocomposite film formed in the C4O6H4Na2 electrolyte.
4418 J. Cent. South Univ. (2014) 21: 4415−4423
Table 3 EDS analysis results of local points (molar fraction, %) 3.2 Growth behavior of nanocomposite film
Point Ti Al O V Si C The thickness of anodic oxide film depends on the
forming voltage, in other words, the changing rate of
A in Fig. 1 40.63 1.55 36.39 2.86 7.93 10.65
voltage and the growing rate of the film are equivalent
B in Fig. 2 41.72 1.42 44.82 3.31 4.20 6.90 [29]. The voltage–time responses of the oxide films
C in Fig. 2 39.25 1.82 38.27 2.79 8.46 8.21 formed in the C4O6H4Na2 electrolyte without and with
D in Fig. 6 26.96 3.31 64.44 0.63 1.66 2.13 addition of 1 g/L SiC particles reveal relatively steep
voltage rising to 80−83 V, associated with formation of
E in Fig. 6 27.07 3.63 68.00 1.29 — —
barrier layer (Fig. 4). Then, the forming voltage
approximately keeps steady after a slight drop, which
Figure 3 shows the XPS spectra of Si 2p and C 1s of suggests the stable growth of the outer layer. However,
the nanocomposite film. The Si 2p spectrum consists of the nanoparticle additions have comparatively minor
two peaks: one at the energy of 100.3 eV, attributed to influences on the voltages through the whole process.
Si—C, and the other at the energy of 101.8 eV, identified The most noticeable influence of the nanoparticles is to
as O—Si—C [25−27]. During synthesis, transportation increase the ultimate voltages of the oxide films without
and storage, SiC powder is inevitably oxidized, forming (79 V) and with (82 V) SiC particles, respectively.
an oxygen-rich layer on its surface. The oxidized layer is Parallel result shows that the thickness of particle-free
chemically similar to the surface of silica and when pH film is slightly thinner than the composite film (Fig. 3).
range is larger than 2.5, silanols react with OH−, leaving Gas evolution accompanies anodic oxide process for
Si—O− with negative charges on the surface of the both films.
powder [28]. The pH of C4O6H4Na2 electrolyte used in In our previous study, the growth mechanism of
this work is 7.3−7.8, hence, it is in favor of the formation porous anodic oxide films in neutral tartrate solution was
of O—Si—C. proposed [25]．However, in this work, the formation
The C 1s spectrum of the composite film shows mechanism of anodizing composite film and the
three peaks: 283.2, 286.2 and 288.4 eV. One of the peaks preservation of SiC particles in the anodic film would be
(283.2 eV) is attributed to C—Si and other two are due discussed. As SiC particles have large surface-to-volume
to contaminant carbon: C—O—H (286.5 eV), and C=O ratio and low wettability, it is extremely difficult for the
(288.4 eV) [26, 29]. XPS analysis also implies the mechanical stirring method to distribute and disperse
preservation of SiC in the nanocomposite film, which is nano-scale particles uniformly in the electrolyte [26]. In
consistent with the EDS results. this work, the surfaces of SiC particles are modified

Fig. 2 Cross-sectional SEM micrographs of oxide films formed in C4O6H4Na2 electrolyte: (a) Without SiC particles; (b) With SiC
particles; (c) and (d) High magnification of (b)
J. Cent. South Univ. (2014) 21: 4415−4423
Fig. 3 XPS spectra of Si 2p (a) and C 1s (b) of oxide films
formed in C4O6H4Na2 electrolyte with addition of SiC particles
Fig. 4 Voltage–time responses of oxide films formed in
C4O6H4Na2 electrolyte without and with addition of 1 g/L SiC
particles
using SDS anionic surfactants. The appropriate addition
of SDS can not only disperse the SiC particles in the
electrolyte but also make them have a negative charge.
Consequently, the particles with a negative charge can be
drawn toward the anode (or the film) under the effect of
the electric field and stirring. Then, they adhere firmly to
the oxide layer due to regional evaporation of the
electrolyte containing SiC particles by local high
temperature during anodic oxidation process. According
4419
to the SEM morphologies of the oxide films formed in
the C4O6H4Na2 electrolyte (Fig. 1), a number of cavities
and micro-cracks can be observed on the surface. The
SiC particles can be kept in these sites through
mechanical entrapment, physical or chemical adsorption
and electrochemical action [10, 18−19]. For example,
some particles are adjacent to the micro-cracks, some
particles are surged into holes of the film and some
particles distribute non-uniformly over the surface
(Fig. 1(c)). With the incorporation of the SiC particles,
the SiC/TiO2 composite film can be synthesized on
Ti6Al4V alloy by DC anodic oxidation.
3.3 Tribological properties
Figure 5 shows 3D morphologies of the wear traces
of TiO2 film and SiC/TiO2 nanocomposite film under a
load of 4 N for 30 min sliding. It can be seen from
Fig. 5(a) that the wear trace of the TiO2 film is wide and
deep after the sliding test and the Ti6Al4V alloy
substrate is exposed as well. According to the
corresponding profiles, the width and depth of the wear
track are around 1.1 mm and 50.2 μm, respectively
(Fig. 5(c)). However, the wear track of the SiC/TiO2
composite film is very narrow and shallow, as shown in
Fig. 5(b) and the Ti6Al4V alloy substrate is not visible
yet. The SiC/TiO2 nanocomposite film displays the width
of about 700 μm and the depth of 30.1 μm (Fig. 5(c)).
Then, wear rates of the samples are calculated. The
average wear rates of both films are shown in Fig. 5(d)
and the error bars represent the standard deviation of
three measurements. The average wear rates of TiO2 film
and SiC/TiO2 nanocomposite film are calculated to be
2.1×10−5 and 0.3×10−5 mm3/(N·m), respectively. That is
to say, SiC/TiO2 nanocomposite film with seven times
lower wear rate shows better wear resistance than TiO2
film.
The worn surfaces of both films are further
investigated by comparing their OM and SEM
morphologies, as shown in Fig. 6. It is observed from the
OM images that the wear track on SiC/TiO2
nanocomposite film becomes shallow and narrow
compared with that on the TiO2 film. Meanwhile, the
substrate of TiO2 film is absolutely exposed; however,
some residual films adhered to the SiC/TiO2
nanocomposite film suggest that wear does not reach the
substrate. These results are consistent with the 3D
morphologies of the wear tracks, which also
demonstrates that the wear resistance of SiC/TiO2
nanocomposite film is improved. Figures 6(c) and (d)
present the SEM morphologies of the wear tracks on
TiO2 film and SiC/TiO2 nanocomposite film. The
furrows along the direction of friction and some wear
debris can be clearly seen on the wear surface of TiO2
film (Fig. 6(c)). The observations imply that the wear
4420
Fig. 5 3D morphologies of wear tracks on TiO2 film (a) and SiC/TiO2 nanocomposite film (b), corresponding depth profiles (c) and
average wear rate on both films (d)
form of the TiO2 film is abrasive type which results in the
high wear rate shown in Fig. 5(d). The thin furrows in
the wear surface are brought about by the abrasive debris
which is discharged from a break on TiO2 oxide.
Nevertheless, the wear track of SiC/TiO2 nanocomposite
film is relatively smooth, without apparent scratches and
abrasive debris (Fig. 6(d)), indicating that the wear of
SiC/TiO2 nanocomposite film is comparatively mild and
slight. According to the EDS analysis results of local
J. Cent. South Univ. (2014) 21: 4415−4423
points D and E in Fig. 6(c), the black flattened plate-like
debris (D) contains Si element and is composed of TiO2,
Al2O3 and SiO2 (Table 3). It seems that SiC particles are
likely to melt and then are oxidized by frictional heat
during the sliding tests. Compared with the TiO2 film,
SiC/TiO2 nanocomposite film is a relatively hard film
which reduces the ball penetration and wear debris
ripped into the film. Further, for the wear debris already
penetrates to the film, SiC nanoparticles will increase
J. Cent. South Univ. (2014) 21: 4415−4423 4421

Fig. 6 OM images (a, b) and SEM morphologies (c, d) of wear tracks on TiO2 film (a, c) and SiC/TiO2 nanocomposite film (b, d)

the contacting frequencies with these debris in a resistance of oxide film properly.
oscillating amplitude. As a direct result, furrows will be
swerved or terminated, which can be proved by the 3.4 Corrosion resistance
discontinuous white scratches on the black plate-like The polarization behaviour of the anodized Ti6Al4V
debris (Fig. 6(d)). In summary, we suggest that the dark alloys without and with SiC particles in C4O6H4Na2
plate-like debris acts as barriers and prevents the ball to electrolyte is presented in Fig. 7. The detailed data are
cause more wear and tear of the film during the sliding given in Table 4. For the TiO2 film and SiC/TiO2
test. nanocomposite film, similar passive current potentials
It is believed that the wear resistance of material has (φcorr) are obtained that range from 250 mV to 300 mV.
much to do with its hardness, in particular, the surface The anodized alloy with SiC nanoparticles results in a
hardness. SiC is a kind of superhard particles and its reduction in passive current density to about 1.54×
hardness can be up to HV 3000 [30]. Hence, the
properties of substrate material composites with
embedded nano-sized ceramic particles (less than 100
nm) would be improved considerably even with a very
low volume fraction of these nanoparticles [26].
According to typical mechanism of nanoparticle
enhancement [21], the metal substrate with low hardness
can play a good supporting action of reinforcing particles.
As a result, the reinforcing particles embedded in the
alloy matrix could play a protective role in reducing the
incidence of wear and tear. From the above analysis, SiC
particles reserved in cavities and micro-cracks on the
surface or the internal sites of the composite film exactly
play the role in reinforcing the particles. Based on the Fig. 7 Polarization potentiodynamic curves recorded in 3.5%
particle-enhancement mechanism, SiC particles NaCl for anodized Ti6Al4V alloys without and with SiC
persevered in the composite film could enhance the wear particles in C4O6H4Na2 electrolyte
4422
Table 4 Properties of TiO2 film and SiC/TiO2 nanocomposite
film
−2
Film φcorr /V Jcorr /(A·cm )
TiO2 0.258 3.73×10-8
SiC/TiO2 nanocomposite 0.298 1.54×10-8
10−8 A/cm2, which is more than two times lower than that
of the TiO2 film (3.73×10−8 A/cm2). Although the
addition of SiC incorporated to the matrix is the second
phase, it does not make an adverse impact on the
corrosion resistance of the film.
The improved performance offered by the SiC
nanoparticles contained film is attributed to the presence
of the nanoparticle-rich sites in the surface and internal
regions, which act as barriers that block access to the
defects of the composite film. Further, SiC particles are
poor electrical conductors and due to their high electrical
resistance, some resistance is offered by the SiC particles
which do not take part in the process but rather cause
hindrance. Consequently, the composite film with good
anti-wear and anti-corrosion properties can be
synthesized on Ti6Al4V alloy by DC anodic oxidation
procedure in C4O6H4Na2 electrolyte containing dispersed
nanoparticles.
4 Conclusions
1) A SiC/TiO2 reinforced composite film is
successfully synthesized on Ti6Al4V alloy by DC anodic
oxidation in C4O6H4Na2 electrolyte containing dispersed
nanoparticles. The SiC particles distribute nonuniformly
in the film and are preferentially concentrate within
internal cavities and micro-cracks. Meanwhile, SiC
particles are embedded into the composite layer forming
an integral part of it.
2) The SiC/TiO2 composite film exhibits improved
tribological property compared with the TiO2 film under
dry sliding condition, which decreases the wear rate from
2.1×10−5 mm3/(N·m) to 0.3×10−5 mm3/(N·m). SiC
particle is likely to melt and then is oxidized by frictional
heat during the sliding tests. Based on the particle-
enhancement mechanism, the SiC particles embedded in
the film can play a protective role in reducing the
incidence of wear and tear.
3) The anodized alloy with SiC nanoparticles results
in a reduction in passive current density to about
1.54×10−8 A/cm2, which is more than two times lower
than that of the TiO2 film. The improved performance
offered by the SiC nanoparticle contained films is
attributed to the presence of the nanoparticle-rich sites in
the surface and internal regions, which act as barriers
that block access to the defects of the composite film.
J. Cent. South Univ. (2014) 21: 4415−4423
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(Edited by YANG Bing)