Received 07 April 2008; accepted 12 June 2008

Projects 50535050 supported by the National Natural Science Foundation of China and NCET-06-0479 by the New Century Excellent Talents in University
Corresponding author. Tel: +86-516-83591915; E-mail address: WQL889@cumt.edu.cn
Biotribological behavior of ultra high molecular weight
polyethylene composites containing bovine bone hydroxyapatite
LIU Jin-long, ZHU Yuan-yuan, WANG Qing-liang, GE Shi-rong
School of Materials and Engineering, China University of Mining & Technology, Xuzhou, Jiangsu 221008, China
Abstract: Wear particles of ultrahigh molecular weight polyethylene (UHMWPE) are the main cause of long-term failure of total
joint replacements. Therefore, increasing its wear resistance or bioactivity will be very useful in order to obtain high quality artifi-
cial joints. In our study, UHMWPE composites filled with the bovine bone hydroxyapatite (BHA) were prepared by the method of
compression moulding. A ball-on-disc wear test was carried out with a Universal Micro-Tribometer to investigate the friction and
wear behavior of a Si
3
N
4
ceramic ball, cross-sliding against the UHMWPE/BHA composites with human plasma lubrication. At the
same time, the profiles of the worn grooves on the UHMWPE/BHA surface were scanned. The experimental results indicate that
the addition of BHA to UHMWPE had a significant effect on the biotribological behavior of UHMWPE cross-sliding against the
Si
3
N
4
ceramic ball. The addition of BHA powder enhanced the hardness and modulus of elasticity of these composites and de-
creased the friction coefficients and wear rates under conditions of human plasma lubrication. When the added amount of BHA
powders was up to 20%~30%, UHMWPE/BHA composites demonstrated the designed performance of the mechanical properties
and biotribological behavior.
Key words: UHMWPE; hydroxyapatite; biotribology; composite material
1 Introduction
Ultra high molecular weight polyethylene
(UHMWPE) is an organic polymer widely used as an
acetabular component in hip and total knee joint re-
placements, because of its excellent mechanical prop-
erties, biocompatibility and stability in the human
body
[12]
. However, in recent years it has been recog-
nized that the wear debris of UHMWPE may be a
limiting factor for the long-term success of prostheses.
At Present, most clinical results have revealed that
aseptic loosening is the primary cause of failure of
total hip replacements (THRs) and accounts for al-
most three-quarters of all revision operations
[36]
.
Aseptic loosening has been strongly linked with
UHMWPE wear debris-induced osteolysis and since
the occurrence and severity of osteolysis appears to
be related to the size and concentration of wear parti-
cles, it follows that reducing the amount and rate of
generation of wear particles should reduce the occur-
rence of long-term aseptic loosening
[78]
. Therefore, it
is believed that two effective methods to reduce asep-
tic loosening are the following:
1) improving the wear resistance to reduce the
concentration of wear debris.
2) increasing the biocompatibility and bioactivity
to decrease adverse biological reactions.
Since the wear resistance of UHMWPE appears to
be related to its mechanical properties, especially
those on the surface, it follows that an increased en-
hancement of its mechanical properties should im-
prove the wear resistance of UHMWPE. Many au-
thors have reported that the mechanical properties of
UHMWPE composites can be improved by introduc-
ing reinforced second phases of ceramics (A1
2
O
3
,
TiO
2
, quartz, wollastonite, etc.), metals or polymers
(polyurethane, phenyl p-hydroxyzoate, etc.)
[915]
. The
results show that these reinforced second phases may
improve not only the mechanical properties but also
the wear performance of UHMWPE-based compos-
ites. But, most of these filling materials have no or at
best poor biocompatibility and bioactivity.
Hydroxyapatite (HA) is currently used as a bioma-
terial for many applications in biomedicine, because
it can form a real bond with the surrounding bone
tissue when implanted
[16]
. Several studies on
UHMWPE/HA composites have been reported. Reis
et al. investigated the impact behavior of a
HA/UHMWPE composite
[17]
. Cunha et al. studied the
effect of processing conditions on the mechanical
J China Univ Mining & Technol 18 (2008) 06060612
JOURNAL OF CHINA UNIVERSITY OF
MINING &
TECHNOLOGY
www.elsevier.com/locate/jcumt
LIU Jin-long et al Biotribological behavior of ultra high molecular weight polyethylene 607
behavior of the HA/UHMWPE composite using in-
jection and compression molding
[18]
. However, few of
these efforts are related to the natural bone hy-
droxyapatite, which has been used as bone implant
material due to its improved bioactivity, structure and
components, similar to that of human bones. Knets et
al. produced an annealed compact bone tissue rein-
forced UHMWPE composite, but few processing de-
tails were given
[19]
.
In order to improve the wear resistance and bioac-
tivity of UHMWPE and reduce aseptic loosening,
bovine bone hydroxyapatite (BHA) powders (<10 m)
obtained from natural compact bones were filled in
UHMWPE. In our study, we prepared UHMWPE/
BHA composites by a method of formation pressing.
The present investigation focused on mechanical sur-
face properties and the biotribological behavior of
Si
3
N
4
ceramic cross-sliding against these composites
under conditions of human plasma lubrication.
2 Material and methods
2.1 Raw and processed material
The middle compact bone was selected from fresh
bovine femoral bones as our experimental material,
from which the parenchyma and marrow were re-
moved thoroughly. After drying at room temperature
for two weeks, this bone material was smashed and
reduced to powder with particle sizes less then 10 m.
The bovine powders were disinfected in a NaHCO
3
solution at high pressure for 30 min and then washed
by distilled water several times and dried at 80 C for
24 h. The dried powder was sintered at 800 C for 2 h
and cooled in a stove to room temperature. XRD
spectra of the bovine powder, as shown in Fig. 1a,
indicated that hydroxyapatite (HA) was the main
mineral component, which agreed with HA standard
spectra provided by JCPDS-ICDD. The size distribu-
tion curve of BHA powder in Fig. 1b shows that the
median diameter (D50) was about 1.58 m and the
specific surface area 3023.17 m
2
/kg.
Fig. 2 shows the analytical results of UHMWPE
powder with a molecular weight of 5.410
6
g/mol
(Lingen Chemicals Co., Ltd, China). The median
diameter (D50) was about 157.21 m and the specific
surface area 16.53 m
2
/kg (Fig. 2b). Prior to milling,
the BHA powder was coated by the coupling agent
KH-550 and dried in a vacuum oven at 80 C for 12 h.
The ball milling was conducted in a rotary ball mill
with adjustable rotation speed up to 35 r/min. The
mill container volume was 1.0 L and the agate ball
diameter was about 8 mm. The mill container and ball
were cleaned by rinsing in an analytical grade ethanol
before ball milling. The coated BHA powder was
compounded with the UHMWPE powder by ball
milling in ethanol for 8 h. Then the mixture was dried
in a vacuum oven at 80 C for 24 h. Finally, it was
hot pressed at 190 C to form 6 mm thick UHMWPE/
BHA composite discs of 50 mm diameter.
D
i
I
I
r
a
c
t
i
o
n

i
n
t
e
n
s
i
t
y
P
e
r
c
e
n
t
a
g
e

(

)
(m)
2
(a) XRD spectra (b) Size distribution curve
Fig. 1 XRD spectra of bovine bone powder and size distribution curve of bovine hydroxyapatite powder

P
e
r
c
e
n
t
a
g
e

(

)
(m)
(a) SEM micrograph (b) Size distribution curve
Fig. 2 SEM micrograph of UHMWPE particles and size distribution curve of UHMWPE powder
Journal of China University of Mining & Technology Vol.18 No.4 608
2.2 Friction and wear test
A ball-on-disc wear test was run on a Universal
Micro-Tribometer (Center Inc. USA) to investigate
the friction and wear behavior of the Si
3
N
4
ceramic
ball, cross-sliding against UHMWPE/BHA compos-
ites with human plasma lubrication (see Fig. 3a). The
reciprocating velocity of the upper sample is 8 mm/s,
reciprocating distance 0.2 mm and sliding speed of
lower sample 0.21 m/s. In sliding bearing, sliding
wear in a rotational direction is normally noticed. But
the bending deflection in the axial direction will
cause friction and wear. So, the friction and wear be-
havior of UNMWPE/BHA composites under cross-
sliding direction conditions have been studied for the
movement of artificial knee joints and hip joints, in-
cluding tangential and radial loads.
(a) Schematic diagram (b) Wear track
Fig. 3 Schematic diagram of abrasion testing and wear track on UHMWPE/BHA composite disc
The Si
3
N
4
ceramic ball was 4 mm in diameter and
fixed on the load arm. The UHMWPE/BHA compos-
ite disc was rotated by an electrical motor controlled
by a frequency converter. Fig. 3b shows that, when
the disc is rotated along the circumference of a circle,
the Si
3
N
4
ceramic ball cross-slid ten times. The con-
tact load was 3.9 N and the sliding speed 0.21 m/s.
The testing time was 120 min in each test. All ex-
periments were performed in human plasma lubrica-
tion at room temperature. The relative humidity was
50%~60%. Each wear test was repeated at least three
times. Prior to the wear testing, each of the
UHMWPE composite discs was ground to obtain a
smooth surface. Grinding was performed in steps
with abrasive papers of decreasing grit size. The
ground surfaces were polished with a diamond paste
with particle sizes of 0.35 m on a nylon polishing
cloth. The average surface roughness, R
a
of the pol-
ished surfaces was less than 0.2 m, measured using
a conventional profilometer.
In order to normalize the wear results in our study,
the commonly used wear rate k was calculated by
dividing the reduced wear weight m (BP211D elec-
tron analytical balance with 0.01 mg precision,
Sartorius AG, Germany) by the product of total
sliding distance S, the applied normal load N and
the density of the material
[20]
: k =m /NS.
Analysis of variance using regression analysis and
Students t-test was carried out to test for significant
differences between various sets of experimental data.
A probability level of p<0.05 was considered signifi-
cant. Steady state friction coefficients were obtained
by calculating the average friction coefficients be-
tween 60 to 120 min of sliding time.
3 Results
3.1 Surface properties
It is well known that the wear resistance of
UHMWPE is related to its mechanical properties,
especially its surface properties. The experimental
results in Fig. 4 indicate the variations of the hardness
and modulus of elasticity of these composites de-
pending on the reinforced content of BHA. As could
be expected, these values enhanced with an increase
in the amount of BHA. When this was up to
20%~30% (by weight), the maximum hardness and
modulus of elasticity were obtained. Comparison of
these results with those of pure UHMWPE, showed
that the maximum average value of hardness
achieved, 132.684.10 MPa for the UHMWPE/20%
BHA composite, about 15% higher than that of pure
UHMWPE (116.862.13 MPa). The modulus of elas-
ticity also increased with additional amounts of BHA,
i.e., from 720.2848.43 MPa for non-reinforced BHA
matrix to 1076.6751.74 MPa for the UHMWPE/
20% BHA composite. When the amount of BHA ex-
ceeded 30%, both values gradually decreased with an
increase in the amount of BHA. Therefore, it was
clear that the reinforced phases of BHA could in-
crease the surface properties of UHMWPE compos-
ites. The optimum amount of added BHA was
20%~30%, obtained from our experimental results.
LIU Jin-long et al Biotribological behavior of ultra high molecular weight polyethylene 609
H
a
r
d
n
e
s
s

(
M
P
a
)
E
l
a
s
t
i
c

m
o
l
u
d
u
s

(
M
P
a
)
Fig. 4 Effect of amount of BHA on hardness and modulus
of elasticity of UHMWPE/BHA composites
3.2 Friction coefficients
The friction coefficients of UHMWPE/BHA com-
posites of Si
3
N
4
with human plasma lubrication at
room temperature are shown in Fig. 5a. Each of the
UHMWPE/BHA composites had the same change in
the friction coefficients over time. The friction coeffi-
cients decreased rapidly for a short time of sliding
and then tended to reach a steady state at about 60
min. The variation of the friction coefficient for all
materials fluctuated little during the entire wear
process. From the average friction coefficients in Fig.
5b, it is seen that the addition of BHA clearly de-
creased the friction coefficients of the UHMWPE/
BHA composites against Si
3
N
4
. When the amount of
BHA was up to 20%~30%, the lowest friction coeffi-
cient was obtained. For example, the friction coeffi-
cient of UHMWPE was approximately 0.064, but
only about 0.042 and 0.048 for UHMWPE/20% BHA
and UHMWPE/30% BHA composites respectively,
which is only about 60% of that of UHMWPE.
However, when the increased amount of BHA ex-
ceeded 30%, the friction coefficient values increased
with the increment in the amount of BHA.
(a) Friction coefficients (b) Steady friction coefficients
Fig. 5 Friction coefficients of UHMWPE/BHA cross-sliding against Si
3
N
4
ceramic in human plasma lubrication and steady
friction coefficients acquired by calculating the average friction coefficients between 60 and 120 min of sliding time
3.3 Wear behavior
The bar charts in Fig. 6 present the wear rates of
UHMWPE/BHA composites with human plasma lu-
brication. It clearly shows that the addition of BHA to
UHMWPE can raise the wear rates of these compos-
ites. When the amount of BHA was less than 30%,
the wear rate of the composite would reduce with an
increase in the amount of BHA. The sample of
UHMWPE/20% BHA material had a wear rate of
7.6110
8
mm
3
/Nm, which was only about 60% of
the 12.3810
8
mm
3
/Nm of UHMWPE. It also shows
that the wear rate increases with an increase in the
amount of BHA when it exceeds 30%. But, these de-
creases were clearly less than that of UHMWPE. In
addition, under the cross-sliding movement the wear
rate of UHMWPE was higher than that in a single
bearing slide
[21]
.
Worn grooves on UHMWPE/BHA composite sur-
faces are presented in Fig. 7. Although it was difficult
to position the boundary of the worn groove exactly,
these worn-out areas still demonstrate that worn
grooves from UHMWPE were deeper or wider than
those of UHMWPE/BHA composites. Composites
with lower wear rates show narrower and shallower
worn grooves, which agreed with the wear rates in
our tests.
W
e
a
r

r
a
t
e

(
1
0

8
m
m
3
/
N
m
)
Fig. 6 Comparison on wear rate of UHMWPE/BHA
composites cross-sliding against Si
3
N
4
Journal of China University of Mining & Technology Vol.18 No.4 610
m
W
e
a
r

d
e
p
t
h

(






)

m
W
e
a
r

d
e
p
t
h

(






)

m
m
W
e
a
r

d
e
p
t
h

(






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m
m
W
e
a
r

d
e
p
t
h

(






)

m
m
W
e
a
r

d
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p
t
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(






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m
m
W
e
a
r

d
e
p
t
h

(






)

m
m
Fig. 7 Profiles of worn grooves on UHMWPE/BHA composite surfaces with human plasma lubrication
4 Discussion
The experimental results from our tests indicate
that the addition of BHA to UHMWPE had a signifi-
cant effect on the wear and friction behavior of
UHMWPE cross-sliding against the Si
3
N
4
ceramic
ball. It clearly showed that the addition of BHA pow-
der enhances the hardness and modulus of elasticity
of these composites and decreased both the friction
coefficients and wear rates with human plasma lubri-
cation. When the amount of BHA reached 20%~30%,
the UHMWPE/BHA composites demonstrated the
designed performance of the mechanical properties
and biotribological behavior.
It is well known that the friction force of
UHMWPE polymers against ceramic balls is com-
posed of interfacial adhesion and ploughing forces.
The adhesion force is affected by the effective
modulus of elasticity, i.e., there is an inversely pro-
portional relationship. The ploughing force depends
on the shear strength of UHMWPE surfaces. It is seen
from Fig. 4 that the modulus of elastiocity of the sur-
face of UHMWPE/BHA composites increases along
with enhanced surface hardness. The modulus of
elasticity of the surface increased from 720 to 1077
MPa, while the hardness increased from 117 to 133
MPa. In some experiments
[22]
it was reported that the
gamma irradiated UHMWPE has a modulus of sur-
face elasticity of approximately 1200 for untreated
specimens, 1450 for specimens treated with 75 kGy
and 1530 MPa for a treatment of 150 kGy, corre-
sponding to a surface hardness of about 37, 46 and 54,
respectively. (The variation in the data for UHMWPE
might be related to the different method of prepara-
tion). For this reason, the increment in the effective
modulus of elasticity might reduce the adhesive force
of the Si
3
N
4
ceramic ball on UHMWPE/BHA com-
posite surfaces. At the same time, the hardened sur-
face can increase the ploughing force against the hard
asperity of the surface of the Si
3
N
4
ball with the
hardness enhancement of the UHMWPE/BHA com-
posite surface. Consequently, the summation of the
adhesion and ploughing forces resulted in the low
friction coefficients for UHMWPE/BHA composites
in Fig. 5.
The pictures in Fig. 8 show the two worn surfaces
of UHMWPE and UHMWPE/20% BHA. It is seen
from Fig. 8a that the worn surface of UHMWPE has
a rough worn appearance, including adhered debris,
serious grooves and fatigue fractures, almost all on
the worn surfaces. For UHMWPE/BHA composite,
the worn scars have become less so, owing to its sur-
face hardness enhancement. The smoother worn sur-
face appears by reason of the shallow grooves. The
adhered debris and fatigue fractures could be found
only in one small worn-out area in Fig. 8b. These
results are likely caused by the decrease in the wear
rate of this material. When the Si
3
N
4
ball was rubbing
on the UHMWPE/BHA surface, the wear resistance
of polymer was inversely proportional to its hardness.
With an increase in hardness and the modulus of elas-
ticity shown in Fig. 4, the enhancement of ploughing
and adhesive wear resistance could have resulted in
the lower wear rates of UHMWPE/BHA composites.
Meanwhile, low wear rates of UHMWPE against
the ceramic ball were contributed by the deposition of
protein and other organic contents in plasma from the
plasma lubrication. Some authors reported that the
serum protein concentration had a significant effect
on the wear performance of CoCr alloys to PTFE
polymer and the film deposited by the serum protein
might affect the wear of UHMWPE
[2325]
. For the
UHMWPE/BHA composites, the biocompatibility
and bioactivity of BHA resulted in a good bonding
ability to the mass of the proteins in human plasma,
LIU Jin-long et al Biotribological behavior of ultra high molecular weight polyethylene 611
which greatly increased the ability of these compos-
ites to absorb the plasma protein. The concentration
of the protein deposition enhanced with an increase of
the amount of HA
[23]
. The protein deposition in hu-
man plasma lubrication made it possible to form a
thin protective film, reducing the abrasion of the
Si
3
N
4
ball on UHMWPE surface. Furthermore, lower
wear rates of UHMWPE/BHA composites were ob-
tained in human plasma lubrication and the greater
the additive amount, the lower the wear rates. How-
ever, when the amount of BHA was greater than the
optimum amount, the wear resistance of UHMWPE/
BHA composite decreased due to their lower hard-
ness and modulus of elasticity, as shown in Figs. 4
and 6.

(a) UHMWPE (b) UHMWPE/BHA 20%
Fig. 8 SEM micrographs of worn surfaces of UHMWPE cross-sliding against Si
3
N
4
ceramic
5 Conclusions
1) The addition of BHA powder to UHMWPE has
shown to be beneficial for increasing its mi-
cro-surface mechanical properties. When the amount
of BHA was less than 30%, the hardness and modulus
of elasticity clearly improved. For the UHMWPE/
20%BHA composite, the micro-surface hardness and
modulus of elasticity were about 15% and 50%
higher than that of pure UHMWPE.
2) With human plasma lubrication, the addition of
BHA to UHMWPE was effective in decreasing the
friction coefficients and wear rates of UHMWPE/
BHA composites cross-sliding against the Si
3
N
4
ce-
ramic ball. Reduction of 40% in the wear rate was
obtained for the UHMWPE/20% BHA composite.
3) Ploughing and fatigue fracture were the main
wear mechanisms of the UHMWPE/BHA composites
cross-sliding against the Si
3
N
4
ceramic with human
plasma lubrication.
Acknowledgements
The authors wish to thank for the support from Na-
tional Nature Science Foundation of China
(50535050) and Program for New Century Excellent
Talents in University (NCET-06-0479).
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