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Chen, G. Huang, H. Huang and Y. Zhao, RSC Adv., 2015, DOI: 10.1039/C5RA11826C.
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DOI: 10.1039/C5RA11826C
1. Introduction
As an excellent engineering plastic with low friction, outstanding chemical stability, low water absorption and
high wear resistance, ultrahigh molecular weight polyethylene(UHMWPE) is widely used in the field of medical
care , pipeline and bearing[1,2]. In the past few years, UHMWPE has been widely used for artificial joints because
of its outstanding mechanical properties and stability[3]. However, the application of UHMWPE has been limited
because of its low surface hardness and anti-fatigue capacity[4,5].Therefore, the improvement of the mechanical
properties and tribological properties is so highly significant that much effort has been carried out. Recently,
researchers have made significant progress in overcoming these difficulties by various studies, including
crosslinking[6], the use of inorganic fillers[7,8] and carbon nanometer materials[9,10]. Unfortunately, the high
additive amounts, expensive cost and unsatisfactory performance of these composites limit their wide use in the
future [11]. Therefore, it is an urgent and significant task to develop a new UHMWPE composites with a low cost
and satisfactory performance, which is a great challenge for further research.
Graphene, first separated in 2004 with the help of scotch tape, has excellent mechanical properties in the carbon
family. Hence, researchers turn their attention to this material excitedly to discover its potential applications in the
wide fields of science and engineering[12]. Because of its high specific surface area, extraordinary mechanical
properties and low cost compared with carbon nanotubes, graphene has caught intense attention as an effective
reinforcements for high performance composites [13-17]. But in practical application of reinforced polymer,
graphene needs to carry on the functional activation treatment to make the oxygen containing functional groups
contained in it, which make it more easily to be dispersed and dissolved into polar solvents and form intercalated
composites through the strong interaction with polymer molecules[18-19]. High specific surface area,
two-dimensional geometric structure and well interfacial adhesion of GO are beneficial to the stress transfer between
*Corresponding author.
E-mail address: Nizf@jiangnan.edu.cn (Z.F. Ni)
Zhaoyw@jiangnan.edu.cn (Y.W. Zhao)
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GO and polymer matrix. Based on previous investigation, the addition of graphene oxide or graphene nanofillers
into a series of polymers have caused advantageous enhancements in mechanical and tribological properties. Shen
et.al.[20] and Shin et.al.[21] investigated the wear behaviors of polymer filled with GO in dry friction, as results
shown deformation and fracture of composites are reduced meanwhile wear resistance is improved with the addition
of GO. Chen et al.[22] demonstrated that the addition of GO to UHMWPE not only improves the hardness and yield
strength, but also shows good biocompatibility. Tai et al.[23] explored that the hardness and wear resistance of
GO/UHMWPE composites are both improved significantly. These have drove us to explore the feasibility of GO
reinforced UHMWPE composites with enhanced mechanical properties as a new kind of seawater self-lubricating
bearing material. However, as we know, the fundamental research of GO/UHMWPE composites on thermal
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performance and impact strength aspects are rarely reported, so this study is carried out.
2. Experimental
2.1 Materials
UHMWPE was supplied from Shanghai Research Institute of Chemical Industry, China. High-purity graphite
powder(99.9%, 325 mesh) was purchased from Qingdao Jinrilai graphite Co. Ltd., China. Other reagents were
analytical grade which could commercially available.
Graphene oxide samples were prepared from natural graphite powders according to a modified Hummers’
method[25]. A range of GO/UHMWPE nanocomposites with different GO content were synthesized by a mode of
UHMWPE intercalated into the layer of GO. The prepared GO samples were stirred with alcohol for 30min and then
ultrasonicated 30min to form a well-dispersed suspension. After that, the suspensions were added into the
UHMWPE powders and ultrasonicated for 1h. At last, the alcohol was removed at 60℃ in a water bath and the solid
products were ground with the aid of a planetary ball mill to obtain the nanocomposite powders. The powders were
molded by hot-pressing which explain in details was that prepressing was conducted under the pressure of 5 Mpa
and then heated at 200℃ for 2h followed by pressing under 10 Mpa until the temperature dropped to room
temperature. In order to investigate the effects of GO on the properties of the composite materials, composites with
the GO content of virgin, 0.1, 0.3, 0.5, 0.7 and 1.0 wt.% GO were prepared.
Thermal weight loss was studied by thermo gravimetric analyzer (TGA, TGA/1, Switzerland) which temperature
range from 50 to 800℃ at a rate of 20℃/min under nitrogen atmosphere. Crystallinity and melting temperature of
the composites were determined by differential scanning calorimetry (DSC, TA, Q200) at a scanning rate of
10℃/min from 20 to 200℃ under nitrogen atmosphere. Fourier transform infrared spectrometer (FTIR, Nicolet is10,
USA) was employed to investigate the characteristics of composites. X-Ray Diffractomer (XRD, D8, Germany)
was performed using Cu-kα radiation and scanned from 10° to 90° at the rate of 6° /min.
Micro-hardness was measured by a micro-hardness tester with a load of 10g, and the reported results were the
average of twenty times each content. The tensile properties were measured by a universal testing machine. Tensile
samples sizes were 33mm in effective length, 6mm in width and 3.2mm in thickness (Fig.1a). The tensile tests were
performed at a rate of 20 mm/min. Dynamic mechanical thermal analysis (DMTA) was conducted for UHMWPE
and composites by an instrument (TA, DMA Q800), using the dual cantilever configuration. The size of the
specimens for DMTA testing was 35×12×4 mm3. The complex modulus of each sample were determined at a
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constant frequency of 1Hz, raisng the temperature from 40-180℃ at a heating rate of 3℃/min. The impact strength
was measured by a cantilever beam impact tester with the sample size of 80mm in length, 10mm in width and 4mm
in thickness (Fig.1b) and the fractured surfaces were observed under a field emission scanning electron
microscope(SEM, HITACHI, S-4800). An empirical formula of impact strength of composites was founded through
fitting by Origin. The impact tests were performed six times each content.
In the thermal forming of GO/UHMWPE composites during industrial manufacture, the properties of
GO/UHMWPE composites may be affected because of the fracture of the molecular chain which may caused by the
plasticization molding under a certain temperature conditions. Thereby, TGA was used to study the thermal stability
of composites what is very necessary for polymer materials. A sample of TGA decomposition curves of pure
UHMWPE showing demarcated temperature (T1, T2, T3) is shown in Fig.4a. As can be seen, the filling of GO
produced a notable influence on the thermal properties of UHMWPE. The initial decomposition temperature, T1
(Fig.4b), was characterized by the corresponding temperature of the weight loss of 5 wt.% in the thermogravimetric
analysis. The temperature of weight loss 5 wt.% (T1) increased gradually with the increase of GO content that may
because of the addition of GO was beneficial to the thermal stability of UHMWPE. The addition of GO increased
the end of the linear weight loss temperature, T2 (Fig.4c), at the content from 0.3% to 0.7%. The temperature of
complete volatilization, T3 (Fig.4d), increased notably due to the addition of GO and be higher than that of pure
UHMPE at all contents. This can be explained by following: on the one hand, the addition of GO could reinforce the
interaction force between GO and UHMWPE by van der waals force and chemical bonds, so the motion of
UHMWPE molecular chair is limited; but on the other hand, the slice layer structure of GO produce larger free
volume for the molecular chain motion of UHMWPE, the two aspects cancel each other out and the effect of
interaction force is greater than the effect of free space, so the thermal performance improved. Interestingly, Xu et
al.[29] reported that the increasing of GO content can improve the thermal stability of PVA/GO composites which
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exactly verify our conclusion. But what is worth noting is that Xu’s research, purpose for fire retardants, was
launched based on a large GO content which the GO content even reached 20%. In our study, there’s no necessary
to be so large additive amounts of GO although the thermal performance may be improved significantly with large
amount of GO adding. The reason why is that, as we know, mechanical properties can be significantly enhanced
with low additive amounts of nano-fillers, is one of the major advantages of nanocomposites. Therefore, we consider
that the temperature is satisfactory which could meet the requirement of manufacturing and working.
Fig.5 shows the DSC curves of GO/UHMWPE composites. As can be seen from the Fig.5a, even though the
weight fraction of GO was different, but the peak temperature of melting appeared at about 135℃, illustrating that
there is little effect on the melting point of the composites which posed by the addition of GO. Whether the initial
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decomposition temperature or the melting temperature is much higher than the working temperature of material as a
∆H (1)
xc =
(1 − φ )∆H 0
Where φ is the weight fraction of GO in the composites, ∆H is the melting enthalpy of composites which
0
actually measured from the DSC curves and ∆H is the melting enthalpy of a 100% crystalline PE taken as
293J/g [30]. As Fig.6 shown, the crystallinity of the composites which obtained from the formula (1) increased
substantially from 37.5% to 44.4% when the addition of GO reached 0.1 wt.% and undulated mildly with the
continue adding of GO, then reduced with the addition of 1 wt.% GO. Even so, the crystallinity still higher than that
of pure UHMWPE. It can be explained that because of the larger specific surface area of GO the high polymer is
adsorbed on the surface of GO and GO can be used as a heterogeneous nucleating sites of crystallization, so the
crystallinity of UHMWPE was improved. But with the GO content continued increasing, a large amount of GO
dispersed into UHMWPE matrix. The strong interaction force between GO and matrix limit the crystals to grow,
lead to the crystallinity tends to be stable in a range.
3.3 Micro-hardness
Micro-hardness value of virgin UHMPWE and GO/UHMWPE composites are detailed in Fig.7. As can be seen,
the addition of GO increases the micro-hardness of UMWPE notably. And with the content of GO increased, the
micro-hardness corresponding increased. A small adding of GO can enhance the micro-hardness of UHMWPE
significantly. This is mainly because the two-dimensional structure of GO and its remarkable mechanical properties.
The two- dimensional structure could bear load and transfer it to a large two-dimensional lamellar structure.
As can been seen in table1, although the contents of GO in all nanocomposites were low, the enhancement of
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Young’s modulus and yield strength were realized. Unfortunately, it should be noted that the ultimate tensile
strength decreased once GO were added into the UHMWPE matrix at a low content of 0.1wt.% but then the values
reached maximum at the content of 0.5wt.%. The Young’s modulus and yield strength were also increased and
then decreased with the contents of GO increased. At the GO content of 0.5wt.%, these values reached the maximum.
This is due to the strong interaction-force between GO and UHMWPE matrix. The layered structure of GO play a
role of load transfer to a larger area and the relative loosened structure could absorb some energy due to the
movement of molecular chains. The similar phenomenon was validated from other graphene/GO reinforced polymer
composites. Wang et al.[31] reported that the tensile strength of GO/polybenzimidazole had an optimal value at the
GO content of 0.3wt.% and decreased the properties of composites with too high or too low GO amounts.
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The storage modulus (E´) plots for the virgin UHMWPE and the GO/UHMWPE composites are presented in
Fig.8. It shows that the rubbery plateau level is higher for the GO/UHMWPE composites than for the virgin
UHMWPE. Moreover, the rubbery modulus significantly increases with filling of GO. The insert map in Fig.8
shows that the E´of virgin UHMWPE is about 850MPa and the E´of 0.5wt.% GO/UHMWPE composites is about
1060, i.e. an evident increase of about 210MPa. However, the E´begins to decrease as the GO content increases over
0.5wt.%. A possible reason for the deduction of E´with increasing GO content should be related to the aggregation
of GO nanosheets. The micro-sized cracks might initiate at the GO aggregate sites and propagated throughout the
samples [32,33]. As a result, the E´would be lowered by the addition of GO at the high GO concentrations.
Fig. 9a shows the variation of impact strength values with the increase of GO content in UHMWPE. It can be
seen that the impact strength of GO/UHMWPE composites increased remarkable with the adding of GO. When GO
addition reached 1.0wt.%, the impact strength increased from 17.27 to 90.96 compared with pure UHMWPE,
corresponding to an growing amount of more than 500%. It was denoted that just a little addition of GO could
remarkable enhance the impact strength of UHMWPE. This is because that the relative loosened layer structure of
composites, which caused by the slice layer structure of GO, produced larger free volume for the molecular chain
motion of UHMWPE. More than, the interaction force between the GO layers and UHMWPE matrix was increased
with the amount of polar groups of GO increasing. By the way, the larger interface of GO due to its bi-dimensional
structure result in more effective load-transfer. The external energy generated by the impact was dispersed to a larger
space and converted into heat energy through the crank motion of the main chain link in the flexible molecular
chains, so the impact strength was increased substantially. Therefore, we believe that the application of
GO/UHMWPE composites would have a bright future due to its excellent property of impact strength.
As shown in Fig.9b, the data was fitted to get an empirical formula of impact strength of GO/UHMWPE
composites, for the purpose of obtain the impact strength of composites with different GO content directly through
the empirical formula’s calculation. Because of the less filling content was one of the advantages of nano-filled
composites, so the experiment was done only to the GO adding amount of 1wt.%. Thereby, the range of GO content
in the empirical formula was from 0wt.% to 1wt.%. Empirical formula as below(Eq.2):
y=61.74x2+11.64x+17.73 (2)
Where y is impact strength of GO/UHMWPE composites; x is the content of GO. The adjusted coefficient of
determination up to 0.995, so the impact strength of the composites with GO content from 0 wt.% to 1wt.% could be
obtained directly from the empirical formula as a way for engineering prediction. In an effort to validate the
correctness of Eq.2, the impact strength of 0.7wt.% composites were tested. There is little deviation compared the
value obtained from Eq.2 which is 56.13 with the value obtained from the actual experiment which is 53.92 -+13.34
12.12 ,
illustrating that the Eq.2 holds up.
As can be seen in Fig.10, the fractured surface of pure UHMWPE was relatively flat and had obvious gaps. This
is because the structure of UHMWPE is a hybrid system which compose of crystalline phase and non-crystalline
phase and the crystalline phase is also too small to form a completed spherulite [34]. This structure of UHMWPE is
benefited to the movement of molecular chain, so UHMWPE has good impact property. The fractured surface was
significant changed with the GO adding. When adding content of GO was 0.1%wt.,the fractured surface became a
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little fluctuation uneven. Because of its less dosage, GO was sparsely dispersed in the UHMWPE matrix, but the
layered structure of GO also can be seen from the magnified image. When the GO content increase to 0.5%wt., more
GO were uniformly dispersed in the UHMWPE matrix. The fractured surface changed again to more flat than that of
0.1%wt and emerged some filamentous even mesh structure which due to the strong interaction between GO and
UHMWPE matrix. When the GO content increased to 1%wt., GO layers uniformly dispersed in the UHMWPE
matrix and the GO which embedded into the molecular chain of UHMWPE together with the polymer were tightly
pressed into a flake structure. It can be seen from the Fig.9, the lamellar structure became more and more continuous,
uniform and compacting with the increase of GO content. The interaction between GO and UHMWPE becomes
stronger with adding GO and the lamellar structure is advantageous to the load transfer, so the addition of GO could
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Table 2 Percentage variation of mechanical properties of similar composites with respect to the virgin materials
Filler
Tensile Max tensile Impact
Composites fraction Hardness Reference
modules strength energy
(wt.%)
HA/UHMWPE 22.8 +788% -13% [35]
CNTs/UHMWPE 5 +82% -13% [34]
Zeolite/UHMWPE 10 +31% -11% +24.86% [37]
Graphene/Chitosan 2.3 +112% +60% [38]
GO/Polybenzimidazole 1.0 +23% +17% [28]
GO/UHMWPE 0.5 +11% +12% +134% +8% This work
GO/UHMWPE 1.0 +7% +1% +426% +19% This work
What exactly influence the thermal and mechanical properties of GO/UHMWPE composites? Based on the
above analysis, a model of free-space effect and interaction-force effect of GO/UHMWPE nanocomposites was
established. There are two aspects, which are free-space effect and interaction force effect respectively, mainly
effecting the performance of GO/UHMWPE nanocomposites such as the thermal properties and impact strength
which have verified abrove. The free-space effect refers to the relative loosened layered structure, which caused by
the slice layer structure of GO, produced larger free space for the molecular chain motion of UHMWPE. And the
interaction-force effect refers to the interaction force between GO layers and UHMWPE and the force will increase
with the polar groups of GO increasing. Therefore, a conclusion is obtained as below. With the amounts of GO
layers increasing in GO/UHMWPE nanocomposites, the free-space effect is obvious firstly then tends to be a
constant while interaction-force effect is always increasing. Particularly, excessive addition of GO will cause uneven
dispersion phenomenon, leading to agglomeration to effect the performance of GO/UHMWPE composites. In other
words, the interaction force effect will increase and play a dominant role along with the increase of GO content.
4. Conclusions
Graphene oxide was produced using a modified Hummers’ method and GO reinforced UHMWPE composites
were prepared successfully by a way of liquid-phase ultrasonication mixing and hot pressing. GO sheets were
dispersed uniformly into polymer matrix. GO could improve the mechanical and thermal properties of UHMWPE
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with small loading compare with other fillers reported in the literature such as CNTs. Crystallinity was improved
with the increase of GO content compared with pure UHMWPE. The adding of GO improved the thermal
performance of GO/UHMWPE. The tensile strength had an optimal value at the GO content of 0.5wt.%. Moreover,
small amounts of GO could obviously increase the micro-hardness and the impact strength. There was strong
interaction effect between GO and UHMWPE matrix and the lamellar structure of GO was advantageous to the load
transfer. The empirical formula was founded to directly obtain the impact strength of GO/UHMWPE composites in
the range of virgin to 1wt.% for an engineering prediction purpose. Above all, the performance of GO/UHMWPE
composites were influenced by two aspects: the free-space effect and the interaction-force effect. For thermal
properties, these two aspects offsetted mutually. While for mechanical properties, these two aspects reinforced
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mutually. And with the addition of GO increasing, the interaction-force effect play a leading role.
This work was supported by the National Natural Science Foundation of China ( Grant No. 51305166) and the
Natural Science Foundation of Jiangsu Province, China (BK20130143).
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Figure captions:
Figure 1. Photographs of (a) tensile specimens of GO/UHMWPE composites and (b) impact
specimens of GO/UHMWPE composites.
Figure 3. XRD patterns of GO, pure UHMWPE and 1.0% GO/UHMWPE composite.
Figure 5. DSC curves of GO/UHMWPE composites: (a) heating curve, (b) cooling curve.
Figure 8. Storage modulus (E´) by the DMTA study of virgin UHMWPE and GO/UHMWPE
composites with various GO contents.
Figure 9. Impact strength curves(a) and its fitted curves(b) of GO/UHMWPE composites.
Figure 10. SEM images of the fractured surfaces of the GO/UHMWPE composites with different
amounts of GO: (a)(b) virgin, (c)(d) 0.1wt.%, (e)(f) 0.5wt.%, (g)(h) 1wt.%.
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(a) (b)
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Fig.2. FTIR spectrum of GO/UHMWPE Fig.3. XRD patterns of GO, pure UHMWPE and 1.0%
composites. GO/UHMWPE composite.
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(a) (b)
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Fig.4. Typical decomposition curve (a) of TGA and thermal stability parameters (b, c, d) for GO/UHMWPE composites.
a b
Fig.5. DSC curves of GO/UHMWPE composites: (a) heating curve, (b) cooling curve.
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Fig.8. Storage modulus (E´) by the DMTA study of virgin UHMWPE and
GO/UHMWPE composites with various GO contents.
(a) (b)
Fig.9. Impact strength curves(a) and its fitted curves(b) of GO/UHMWPE composites
with different contents of GO.
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