Applied Surface Science 347 (2015) 591595

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Applied Surface Science

journal homepage: www.elsevier.com/locate/apsusc

Preparation, corrosion resistance and hemocompatibility of the

superhydrophobic TiO2 coatings on biomedical Ti-6Al-4V alloys
J.Y. Jiang a , J.L. Xu b, , Z.H. Liu a , L. Deng a , B. Sun a , S.D. Liu a , L. Wang a , H.Y. Liu a,
a
b

The First Afliated Hospital of Harbin Medical University, Harbin, 150001, PR China
School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063, PR China

a r t i c l e

i n f o

Article history:
Received 26 January 2015
Received in revised form 3 April 2015
Accepted 10 April 2015
Available online 20 April 2015
Keywords:
Micro-arc oxidation
Superhydrophobic surface, Ti-6Al-4V alloy
TiO2 coating
Hemocompatibility

a b s t r a c t
In this paper the micro-arc oxidation (MAO) technique and subsequent superhydrophobic treatment
were applied to fabricate the superhydrophobic TiO2 coatings on biomedical Ti-6Al-4V alloys. The surface
morphology, surface roughness, water contact angle, corrosion resistance and hemocompatibility of the
MAO and superhydrophobic samples were investigated. The results showed that the single anatase TiO2
coating was formed on the surface Ti-6Al-4V alloy with rough and porous micrometer-scale structure. The
low surface energy lm was grafted on the surface of the TiO2 coating by self-assembling reaction during
the hydrophobic treatment process, which resulted in the formation of superhydrophobic surfaces with
the water contact angle of 153.39 . It was found that the corrosion resistance of the superhydrophobic
samples increased by one order of magnitude compared to those of the uncoated Ti-6Al-4V alloys. The
hemolysis ratio and platelets adhesion characteristics of the Ti-6Al-4V alloys were also improved greatly
through the MAO treatment and subsequent superhydrophobic treatment. Especially, no platelet could
be observed on the surface of the superhydrophobic samples. Therefore, the superhydrophobic TiO2
coatings of Ti-6Al-4V alloys with higher hemocompatibility would show great promise in their potential
blood-contacting applications.
2015 Elsevier B.V. All rights reserved.

1. Introduction
Titanium and its alloys have been widely used for biomedical
applications in hard tissue repair, replacement implants, bloodcontacting implants and so on because of their good mechanical
properties, high corrosion resistance and excellent biocompatibility [13]. It is well-known that blood-contacting implants such
as articial heart valves, vascular stents and circulatory support
devices, their hemocompatibility (hemolysis ratio and platelet
adhesion) and corrosion resistance are of great concern in many
research areas and wide applications though the hemocompatibility and corrosion resistance of Ti alloys are enhanced as expected
under some harsh conditions. Many inorganic lms or coatings with
Al2 O3 , TiO2 , DLC and carbon based materials such as SiC have been
frequently used to improve the hemocompatibility and corrosion
resistance of Ti alloys [46].
The superhydrophobic surfaces have been recently paid more
attention due to their unique water repellence, self-cleaning, antibiofouling, anti-adhesion and anti-corrosion properties [710].

Corresponding authors. Tel.: +86 791 83863034, +86 451 85555817.

E-mail addresses: jlxu@nchu.edu.cn (J.L. Xu), hyliu1963@163.com (H.Y. Liu).
http://dx.doi.org/10.1016/j.apsusc.2015.04.075
0169-4332/ 2015 Elsevier B.V. All rights reserved.

Especially, Yang et al. [11] and Hou et al. [12] have succeeded
especially in making the superhydrophobic surfaces to better the
anticoagulation and hemocompatibility. Generally, the superhydrophobic surfaces can be obtained by controlling the surface
roughness (micrometer-scale or nanometer-scale) and lowering
surface energy. The surface roughness can be controlled by etching [13], template [14], electrochemical deposition [15], Solgel
[16], hydrothermal synthesis [17] and anodic oxidation [11]. Lowing surface energy can be easily realized by grafting with special
low surface energy compounds during the superhydrophobic treatment process, including long alkyl chain thiols, alkyl or uorinated
organic silanes, peruorinated alkyl agents, long alkyl chain fatty
acids, polydimethylsiloxane-based polymers or other polymers, or
their combinations [7]. Micro-arc oxidation (MAO), derived from
conventional anodic oxidation, can obtain relative uniform rough
and porous in-situ ceramic coatings on Al, Mg and Ti alloys [18]. The
wear resistance, corrosion resistance, hemocompatibility and biocompatibility can be remarkably enhanced by the oxidized coatings
with strong bonding strength to the substrates [1922]. However, the best of our knowledge, there has been no report so far
on the preparation of superhydrophobic surface on biomedical
titanium alloys by the micro-arc oxidation to gain the micrometerscale or nanometer-scale surface structure. At the same time,

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J.Y. Jiang et al. / Applied Surface Science 347 (2015) 591595

the hemocompatibility and corrosion resistance of the titanium

alloys have been greatly improved by the superhydrophobic surfaces. Therefore, the current work will aim at preparing the
superhydrophobic surfaces on biomedical titanium alloys by
micro-arc oxidation with the subsequent superhydrophobic treatment, and will focus on studying the microstructure, contact angle,
surface roughness, hemocompatibility and corrosion resistance of
the superhydrophobic surfaces, the micro-arc oxidized and the polished Ti-6Al-4V samples as the controls.
2. Experimental details
2.1. Sample preparation and micro-arc oxidation
Commercially available rectangular samples of Ti-6Al-4V alloys
(13 13 1 mm) were used as the substrates. The sheets of Ti
alloys, indexed as Ti-6Al-4V samples, were rstly ground mechanically, polished by SiC sandpapers from 100# to 2000#, cleaned
ultrasonically in acetone and distilled water successively, and
nally rinsed with distilled water and dried in air.
A homemade pulsed bipolar power supply (10 kW) was
employed in the MAO treatment with the Ti-6Al-4V sample as an
anode and the wall of the stainless steel container as the cathode.
An aqueous solution containing 10 g/L sodium phosphate (Na3 PO4 )
was used as the electrolyte, stirred and cooled below 30 C under
the condition of anodic voltage 400 V, cathodic voltage 10 V, frequency 50 Hz, duty cycle 5%, and the duration time 10 min. After
the MAO treatment, the samples were rinsed with distilled water
and dried in air, marked as MAO samples.
2.2. Superhydrophobic treatment of micro-arc oxidized samples
To obtain superhydrophobic surface, the micro-arc oxidized
samples were immersed in the 1 wt.% alcohol solution of 1H, 1H,
2H, 2H-peruorooctyl-trichlorosilane (PFOTS) at room temperature for 12 h and subsequently heated at 140 C for 1 h, indexed
as MAO + PFOTS samples.
2.3. Characterization
Being pre-sputtered with a thin gold lm, the surface morphologies of the samples were observed by using a scanning electron
microscope (SEM, FEI, Quanta 200, USA). The phase composition of
the samples was analyzed by X-ray diffraction (XRD, D8 ADVANCE,
Germany) using a Cu K radiation. An optical contact angle meter
(DSA 100, Krss, Germany) with a computer-controlled liquid dispensing system were employed to measure the static water contact
angles (WCAs) at ambient temperature. The surface roughness Ra of
the samples was tested by a surface roughmeter (SJ-301, Mitutoyo,
Japan).
2.4. Corrosion resistance
The corrosion resistance of the samples in Hanks solution at
room temperature was evaluated by potentiodynamic polarization
test through CHI650D electrochemical analyzer. The electrochemical measurement was conducted by using a conventional three
electrodes electrochemical cell with a saturated calomel electrode
(SCE) as the reference, a Pt foil as the auxiliary electrode, and the
samples with the area of 1 cm2 as the working electrode. The polarization scan rate was controlled at 0.167 mV/s. The polarization
resistance (Rp ) of all the test samples is calculated by using SternGeary equation [23,24]:
RP =

a c

2.303 a + c

1
Icorr

(1)

where a and c are the slopes of anodic and cathodic Tafel plots,
respectively, and Icorr is the corrosion current density.
2.5. Platelet adhesion test
The fresh anticoagulant adult New-Zealand rabbit blood was
centrifuged at 1000 rpm for 20 min to obtain platelet-rich plasma
(PRP). The samples were soaked in PRP at 37 C for 60 min, and
then rinsed by normal saline (0.9 wt.% NaCl) 3 times to remove the
un-adhered platelets. The adhered platelets on the samples surface were xed by 2.5% glutaraldehyde solution. Subsequently, the
samples were progressively dehydrated by 30%, 50%, 70%, 90% and
100% ethanol solution for 15 min, and progressively dealcoholized
by 30%, 50%, 70%, 90% and 100% isoamyl acetate-ethanol solution
for 15 min. Being dried with CO2 , the samples were nally coated
by gold for the morphological observations of the adhered platelets
on the scanning electron microscopy (SEM, S-3400, Hitachi, Japan).
2.6. Hemolysis test
After cleaning and drying, the samples were put into the centrifuge tube. Then the diluted ACD blood, prepared by the fresh
rabbit blood and ACD solution, was dropped into the centrifuge
tube and kept at 37 C for 60 min. Subsequently, Being centrifuged
at 1000 rpm for 5 min, the upper clean solution in the tube was measured by a 722 spectrophotometer at 540 nm and the absorbance
of the solution was recorded as Dt . Under the same experimental conditions, the distilled water and diluted blood as well as the
normal saline and diluted blood were used as the positive control
and the negative control, recorded as Dpc , and Dnc respectively. The
Hemolysis ratio of the samples was calculated by the following
formula:
=

Dt Dnc
100%
Dpc Dnc

(2)

3. Results and discussion

Fig. 1 shows the surface morphology and XRD spectrum of the
MAO + PFOTS sample. It can be seen that the sample surface exhibits
uniform but rough and porous microstructure (crater-like) with the
diameter of the micropores about 0.51 m, similar to the typical MAO morphology, which indicates that the superhydrophobic
treatment does not remarkably change the surface morphology
of samples. It is shown in the XRD pattern that the MAO + PFOTS
sample is composed of single anatase TiO2 crystal phase and the
Ti-6Al-4 V substrate, which suggests that the superhydrophobic
treatment does not dramatically change the phase composition of
Ti-6Al-4V samples treated by the MAO.
Fig. 2 gives the water contact angles of the uncoated Ti-6Al-4V
alloy, the MAO and the MAO + PFOTS samples. The water contact
angle of the Ti-6Al-4V alloy slightly decreases from 69.70 to 52.11
after MAO treatment, while it abruptly increases to 153.39 after
the superhydrophobic treatment. After the MAO treatment, the
rough and porous TiO2 coating was formed on the Ti-6Al-4V, which
enhanced its hydrophilicity, leading to the decrease of the contact angle [25]. The hydrolyzation reaction could occur during the
dissolution process of PFOTS in alcohol solution, bringing about
the formation of the CF3 (CF2 )5 (CH2 )2 Si(OH)3 and Si-OH groups.
On the other hand, there were a large number of Ti-OH groups
formed on the MAO TiO2 surface [25]. At last, during the superhydrophobic treatment process, a self-assembling reaction occurred
and the low surface energy PFOTS lm (-CF3 terminated surface)
was grafted on the TiO2 coating surface through the Ti-O-Si bonds
between the Ti-OH groups and Si-OH groups [26]. In present paper,
the combination of the PFOTS lm with low surface energy and

J.Y. Jiang et al. / Applied Surface Science 347 (2015) 591595

593

Fig. 1. Surface morphology (a) and XRD spectrum (b) of the MAO + PFOTS sample.

the hierarchical micro-scale MAO structure, the superhydrophobic

surface on Ti-6Al-4V alloys was eventually achieved through MAO
treatment followed by superhydrophobic treatment. Furthermore,
the interface interaction between the TiO2 coating and PFTOS lm
was supposed to strong chemical bonding and the superhydrophobic coating was expected to possess higher bonding strength to the
substrate and more excellent stability.
The surface roughness (Ra ) of the Ti-6Al4V, MAO and MAO +
TFOS samples is shown in Fig. 3. It is clearly shown that the surface
roughness of the Ti-6Al-4V alloy increases remarkably after the
MAO treatment, while decreases slightly after the further superhydrophobic treatment. The surface roughness Ra of the polished
Ti-6Al-4 V alloys was only 0.253 m, while it increased to 0.605 m
due to the formation of rough and porous TiO2 coating on its surface. Subsequently, the Ra value decreased to 0.535 m owing to
the formation of the PFOTS lm on the TiO2 coating.
The potentiodynamic polarization curves of Ti-6Al-4V, MAO and
MAO + TFOS samples in Hanks solution are shown in Fig. 4, and
the results of corrosion test extracted from the polarization curves
using Tafel extrapolation are shown in Table 1. It is distinctively
revealed that the corrosion resistance of coated samples (MAO and
MAO + TFOS) is improved compared with the uncoated Ti-6Al-4V
alloy, which can be observed by a shift of the whole polarization
curve towards the region of lower current density and the higher
potential. Especially, the corrosion potential of the MAO + TFOS
sample is shifted in the noble direction by 221 mV relative to the
uncoated Ti-6Al-4V sample, while its corrosion current density and

Fig. 3. Surface roughness of the Ti-6Al4 V, MAO and MAO + TFOS samples.

Fig. 4. Potentiodynamic polarization curves of Ti-6Al-4 V, MAO and MAO + TFOS

samples in Hanks solution.
Table 1
Results of potentiodynamic corrosion test.

Ti-6Al-4V
MAO
MAO + TFOS
Fig. 2. Contact angles of the Ti-6Al-4 V, MAO and MAO + PFOTS samples.

Ecorr /V

Icorr /(A/cm2 )

a /(mV/dec)

c /(mV/dec)

Rp /(/cm2 )

0.404
0.221
0.183

2.21 107
1.33 107
1.41 108

244
236
333

147
105
174

1.80 105
2.37 105
3.53 106

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J.Y. Jiang et al. / Applied Surface Science 347 (2015) 591595

Fig. 5. The hemolysis ratio of Ti-6Al-4 V, MAO and MAO + TFOS samples.

is one order of magnitude lower than that of the uncoated Ti-6Al4V sample, while its corrosion current density and polarization
resistance are one order of magnitude lower and higher than that
of the uncoated Ti-6Al-4V sample. Therefore, the superhydrophobic surface can signicantly improve the corrosion resistance of
Ti-6Al-4V alloy, which is consistent with many previous reports
[710,26]. The enhanced corrosion resistance of the TiO2 superhydrophobic coating can be explained in detail as follows. First,
the electrochemical corrosion could be reduced because the TiO2
superhydrophobic coating presents low electrical conductivity and
electron transport as well as the exchange of electrical charges at
the sample surfaces [27]. Second, the corrosion intermediate Cl
can be effectively impeded to diffuse into the substrate by the PTOS
lm. Third, the corrosion solution contact area to the sample surface
can be minimized by the superhydrophobic surface and lower surface roughness. Finally, corrosive processes can be further refrained
from the air retained on the superhydrophobic surface [9,28].
Once the materials come into contact with blood, some toxic
substances will be released to destroy the red blood cells (RBCs)

in different degree and release the hemoglobin, which will lead to

the lifespan shortening of RBCs and the occurrence of hemolysis.
Therefore, hemolysis ratio is an important index to be measured in
order to investigate the blood compatibility of the blood-contacting
materials. Fig. 5 displays the hemolysis ratio of Ti-6Al-4V, MAO
and MAO + TFOS samples. It can be clearly seen that the hemolysis ratio is the largest for the Ti-6Al-4V sample, and the lowest for
the MAO + TFOS while the MAO is in between. The values of the
hemolysis ratios were 1.51%, 0.85%, and 0.39% for the Ti-6Al-4V,
the MAO, and the MAO + TFOS samples separately, which illustrated
expressly the improvement of the hemolysis properties of Ti-6Al4V alloys by the MAO and superhydrophobic treatments. Moreover,
all of the hemolysis ratio values were lower than 5%, indicating that
all of the samples can meet the requirements of hemolysis test as
blood-contacting materials.
As shown as the platelets morphologies in Fig. 6, obviously
seen are a large number of platelets adhered on the surface of the
uncoated Ti-6Al-4V alloy and the aggregation of the platelets and
the formation of pseudopodia. It can be suggested that the platelets
were seriously activated and liable to the occurrence of blood
coagulation and thrombosis formation. In contrast, the platelets
adhered on the surface of the MAO sample was reduced signicantly and they retained with their original plump spherical shape
without aggregation and pseudopodia. Especially, no platelet was
observed on the surface of the MAO + TFOS sample. Thus it can be
seen that the platelets adhesion properties of Ti-6Al-4V alloys were
greatly improved through MAO treatment and further superhydrophobic treatment.
The hemocompatibility is closely related to the surface properties of materials characterized by composition, surface roughness
and wettability [11,12,22,29,30]. Both of the hemolysis ratio and
the platelet adhesion of the MAO sample decreased signicantly
because the TiO2 coating, with well-known better hemocompatibility and biocompatibility, was emerged on its surface. The decrease
of surface roughness and the increase of contact angle might
be ascribed for the further decrease in the hemolysis ratio and
platelets adhesion for MAO + TFOS sample. The high water contact
angle (>150 ) of superhydrophobic surface is typically low adhesion so that no platelet was found to adhere on the surface of

Fig. 6. Platelets morphologies adhered on the surface of the Ti-6Al-4 V, MAO and MAO + TFOS samples.

J.Y. Jiang et al. / Applied Surface Science 347 (2015) 591595

the MAO + TFOS sample. This result was consistent with the references [11,12]. Therefore, it sufces to make a claim that the
decrease of the hemolysis ratio and platelets adhesion can greatly
improve the hemocompatibility of the Ti-6Al-4V alloy through the
formation of MAO coating on the surface, and further enhancement can be acquired through the formation of superhydrophobic
surface.
4. Conclusions
The superhydrophobic surfaces were successfully fabricated on
biomedical Ti-6Al-4V alloys by micro-arc oxidation and superhydrophobic treatment in PFOTS solution. The following conclusions
can be drawn by above detailed experiments and systematic analysis:
(1) The superhydrophobic surface was composed of angle anatase
TiO2 crystal phase with the typical MAO surface morphology
of rough and porous micrometer-scale structure. The water
angle of Ti-6Al-4V sample decreased slightly after MAO treatment, while increased dramatically to 153.39 after subsequent
hydrophobic treatment.
(2) The corrosion potential of the superhydrophobic sample was
shifted in the noble direction by 221 mV relative to the Ti6Al-4V sample, and simultaneously the polarization resistance
and the corrosion current density increased and decreased by
one order of magnitude respectively. These evidences illustrate that the corrosion resistance of the Ti-6Al-4V alloy can
be signicantly enhanced through the formation of TiO2 Superhydrophobic coatings.
(3) The in-vitro hemocompatibility of the Ti-6Al-4V alloy could
be greatly improved by the superhydrophobic surfaces since
the TiO2 Superhydrophobic coatings reduced effectively the
hemolysis ratio and platelets adhesion.
Acknowledgments
The authors gratefully acknowledge the nancial support of
the project from the National Natural Science Foundation of China
(51101085), the science and technology plan projects of Jiangxi
Province (20151BBG70039), and the Foundation of the First Afliated Hospital of Harbin Medical University (2014Y007).
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