International Journal of Mechanical and Production Engineering Research and Development (IJMPERD) ISSN 2249-6890 Vol.

3, Issue 1, Mar 2013, 189-198 TJPRC Pvt Ltd.

EFFECT OF MELT TEMPERATURE AND CROSS LINKING ON WEAR BEHAVIOUR OF UHMWPE

MOHAMAD RAFFI. N, KANAGARAJAN. D & SRINIVASAN. V Department of Manufacturing Engineering, Annamalai University, Annamalai Nagar, Tamilnadu, India

ABSTRACT
Ultra High Molecular Weight Polyethylene (UHMWPE) has been widely used as a bearing material for artificial joint replacement over forty years. For this study the UHMWPE specimens are molded through injection molding techniques by varying the melt temperatures. The cross linking was done by irradiating the UHMWPE using gamma () irradiation where the specimens received energy dose of 25kGy. The effect of gamma irradiation on tribological properties of UHMWPE sliding against 316L stainless steel was investigated by using friction and wear hip joint simulator under bovine serum lubrication. The contact loads are varied from 50 to 100N. The study revealed that melt temperature has influenced the hardness and wear properties such as coefficient of friction and wear rate significantly. The results indicate that cross linked UHMWPE can be used as bearing materials in artificial joints for its excellent wear resistance compared to un irradiated UHMWPE. The worn out surfaces were shows with the help of scanning electron microscope and it revealed the presence of wear mechanisms like ironing, scratching, ploughing, plastic deformation and fatigue wear.

KEYWORDS: Polymer, Cross Linking, Wear, Wear Mechanism, UHMWPE, -Irradiation INTRODUCTION
Ultra High Molecular Weight Polyethylene (UHMWPE) is one of engineering thermoplastics with excellent comprehensive properties. It has been successfully applied to artificial joint replacements over forty years for its very good wear resistance [1,2]. Also due to its excellent mechanical properties such as exceptional impact resistance, high strength, low creep, low co efficient of friction, abrasion resistance and biocompatibility, it has been used in medical applications like hip joint cups, the gliding parts of knee, shoulder and elbow joint replacements [2]. However, original UHMWPE without any modification will be worn severely after it experiences long-term physiological impact in human body. The wear particles will induce macrophages to provoke a histolytic and physiological response in which the cell becomes enlarged and releases numerous inflammatory and potentially osteolytic factors [4]. The action will lead to the failure of artificial joints for osteolysis and aseptic loosening finally [5&6]. Therefore, the crucial problem for prolonging the service life of artificial joints to ensure the success of artificial joint replacements is how to furthest improve the wear resistance under long-term physiological impact condition. Modifications of UHMWPE to improve its wear resistance have been studied by several researchers [7-10]. Filling modifications for UHMWPE are studied widely, such as particle reinforced UHMWPE composite, But modification of UHMWPE by gamma irradiation, ion implantation technique is mainly adopted in manufacture of acetabular cup of artificial joint, selecting hard and smooth counter faces [11&12] The technique is often conducted by gamma rays or electron beam. Radiation cross-linked and subsequently melted UHMWPE has been successfully used in clinic since 1998. Current clinically available cross-linked UHMWPE is usually irradiated at doses ranging from 5 kGy to 100 kGy [13&14].

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The effect of gamma irradiation on hardness and tribological properties of UHMWPE was investigated in this paper. The materials used for acetabular cups are UHMWPE and gamma irradiated UHMWPE (- UHMWPE). These acetabular cups are manufactured through injection molding technique where different melt temperatures are used to mold the injection molded UHMWPE specimens. The femoral heads are made up of stainless steel (316L) rod form which is machined by computer numerical control machine with greater accuracy. The tribological studies are conducted on a hip joint simulator by varying contact loads. The coefficient of friction and wear rate are evaluated and the worn out morphologies are studied with the help of Scanning Electron Microscope (SEM).

MATERIALS AND METHODS

In this study an injection grade UHMWPE GUR5113 obtained in powder form (from Spectra polymers, Coimbatore, India.) is used. It has tensile strength of 17MPa and bulk density of 0.93 g/cc. The powder was preheated for 2 hours at 100oC in an electric oven to remove excess moisture content. A mold die design made up of mild steel was used to prepare the wear test specimens. The test specimen relevant to HIP joint wear simulator and their dimensions are shown Figure 1. Wear specimens are prepared on a Texas injection molding machine (ROBOSHOT S-2000i 50A). The machine can offer a maximum clamping force of 30 tons and a maximum injection velocity of 330 mm/s. The screw diameter is 22 mm and the maximum injection volume is 29 x 103 mm3. Three melt temperatures (260, 280 and 300oC) were used as injection molding parameters where the injection velocity and compaction time were maintained at 125mm/s and 60s respectively. After the injection molding process, all the specimens were machined to remove burrs and excess materials. Two different types of materials were used in this study, one without irradiation UHMWPE and another irradiated by gamma source (- UHMWPE). UHMWPE specimens were irradiated at 28oC using Iridium 192 (Ir192) isotopes where the specimens received a final dose of 25kGy, which is measured by dosimeter. The hardness measurements for each sample was conducted at three different regions using a Vickers hardness tester (Shimadzu, Singapore), which has a square based pyramid diamond indenter with an angle of 136 between the opposite faces at the vertex. The test conditions were maintained at a load of 9.8 N for duration of 15s at room temperature. Counter face materials stainless steel 316L is obtained from JNS Metal Suppliers, (Ekattutahngal, Chennai, India) in the cylindrical rod form. The required dimensions of the femoral heads were achieved through Computer Numerical Control machining. The wear tests were conducted on a hip joint simulator designed and fabricated in the laboratory as shown in Figure 2. The contact loads were varied from 50 N to 100 N, while the revolution frequency and the test duration were maintained at 1Hz and ten thousand rotation cycles respectively. The tests were performed synchronously on the hip joint wear simulator station with bovine serum as a lubricant procured from M/s Subra chemicals Pondicherry, India. After the tests the specimens were dried in an oven at 100o C for 1 hour to undergo weight loss measurements. The friction force is measured by using a load cell, and the co efficient friction (COF) is calculated using the relation =

, where is the F

Co efficient of friction, H is the Horizontal (or) friction force and F is the Vertical (or) normal force. The wear volume loss is calculated and finally wear rate of the specimen is calculated by using the ratio of wear volume loss to sliding distance. The worn out samples were examined by Scanning Electron microscope (JEOL Corp. Japan) to study the wear mechanisms involved in worn out process.

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RESULTS AND DISCUSSIONS

Hardness Behavior Micro hardness is considered as one of the important properties of materials, which acts as an indicator for the wear resistance of polymers. The hardness for UHMWPE and - UHMWPE with different melt temperature are shown in Figure 3. It is observed that the hardness is maximum for both unirradiated and - irradiated when the melt temperature was maintained at 2800 C. unirradiated UHMWPE. A minimum hardness is obtained for specimens obtained at 260oC melt temperature. Figure 4 shows the micro graphs of unworn UHMWPE and - UHMWPE. It is observed large number of cracks and poor bonding in the case of UHMWPE, where as - UHMWPE exposed sufficient bonding and very fewer cracks. The enhanced hardness behaviours for - UHMWPE may be due to increased crystallinity which is well correlated with the studies of Kanaga Karuppiah et al [15]. Friction Behavior Friction in a system always leads to temperature rise. Under certain condition, the temperature rise can be very high that prompts to total failure of UHMWPE in the hip joint replacement. Knowledge of the temperature rise and the corresponding wear allows the successful application of the hip joint replacement. Frictional heating generally elevates the temperature of the system, which raises the risk to increase wear, creep and degradation of the UHMWPE [16]. The variations of the coefficient of friction for UHMWPE and -UHMWPE are shown in Figure 5. The coefficient of friction of UHMWPE against stainless steel femoral head under bovine serum lubrication is in the range of 0.115 to 0.145. The coefficient of friction of -UHMWPE against stainless steel 316L femoral head is in the range of 0.115 to 0.144. The coefficient of friction for UHMWPE and -UHMWPE corresponding to 280oC MT has decreased to 0.126 and 0.125 respectively. The maximum coefficient of friction values for UHMWPE and -UHMWPE were obtained for specimens corresponding to MT of 260oC. However coefficient of friction of UHMWPE and UHMWPE corresponding to 300oC MT has intermediate values between 260oC MT and 280oC MT. The cross-linked structure formed after irradiation can increase the elastic modulus of the sample, and it can enhance the ability of resisting plastic deformation. The higher friction coefficient is mainly due to the unsteady articulation of the friction pairs. And bearing surfaces of samples cannot be adequately lubricated by bovine serum at the initial sliding process, which will also lead friction coefficients to be higher at the initial stage. The increasing trend of average friction coefficient with the lower melt temperature of 260oC have improper bonding and rough surface of the both UHMWPE and -UHMWPE specimen. As the UHMWPE is a visco elastic material, its deformation under contact will also exhibit visco elastic behavior. Due to critical surface energy of the UHMWPE, the coefficient of friction increases with increase in contact load [17]. Also the temperature raised at the surface asperities of contacting surfaces of UHMWPE could deform molecular chains of polymer [18]. The difference in the coefficient of friction between UHMWPE and -UHMWPE in very lean which may be due to adhesion of polymer to the metallic surface. The increase of friction coefficient with respect to contact loads for UHMWPE is related to the adhesion of polymer to the metallic surface. The increase in the amount of transferred polymer to the pins surface with normal load is stimulated by a marginal lubrication regime at the effective area of contact, which Also, it can be seen that - UHMWPE has more hardness when compared to that of

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is a result of localized high contact pressures that prevents a hydrodynamic regime. The most part of the testing time in the metal polymer pairs the contact was of polymerpolymer type, so the measured friction force can be related to cohesive failures instead of being a adhesive failures at the stainless steel UHMWPE interface. This above statement is well supported by the studies of Wilches et.al [19] Wear Behavior The wear rate of UHMWPE and -UHMWPE with respect to different MT and loads are shown in Figure 6. The melt temperature on UHMWPE has significant influence on the wear behavior of -UHMWPE against stainless steel. It is observed that the -UHMWPE samples molded under 280oC MT exhibits the lowest coefficient of friction and wear rate compared to UHMWPE specimens. The -UHMWPE molded in 280oC MT has the highest value of micro hardness. The UHMWPE samples prepared by 280oC MT obtains the lowest wear rate of 0.014mm3/m and the samples prepared by 260oC MT has highest wear rate of 0.0418mm3/m. The wear rate of the specimens (both UHMWPE and UHMWPE) increases with increase in contact loads. The difference in wear rate for different melt temperature conditions are attributed to the formation of frozen layers. These frozen layers are formed at different thickness for different melt temperature condition and which changes the surface property, melt density or viscosity there by a higher temperature gradient occurred near the mold wall due to heat transfer effect [20]. The cross-linked structure increases entanglement density of molecular chains so that the pulling force between macromolecules is increased. The slipping resistance under shear force for the bearing surface is enhanced so that the bearing surface will resist adhesion and plastic deformation much better. Thus wear rates of irradiated samples are decreased significantly. The UHMWPE specimen obtained at 260oC melt temperature has defused structure and the bonding strength is comparatively weak therefore ductile fracture occurs at defect point. This discontinuity of UHMWPE will result in poor mechanical properties and lower wear resistance. The SEM micrographs of the fracture surface for UHMWPE specimens molded at 280oC MT views uniform and smoother and lesser intergranular discontinuity on the frozen layer. This diffused structure of UHMWPE powders at MT of 280oC is sufficient for the molecular chain to migrate across grain boundaries. It seems that the UHMWPE specimens prepared at 280oC MT have the better mechanical property and higher wear resistance. Figure 7a-f shows the microstructure of worn out surface of UHMWPE samples. The results indicate that samples corresponding to 280oC MT were dominated by Ironing. The samples corresponding to 300oC MT were dominated by scratching and ploughing. The most destructive mechanisms like plastic deformation and fatigue wear were predominant for the samples obtained at 260oC. In addition, the images of worn surfaces explain the wear performance of samples. The obvious scratches and tears imply that adhesive and abrasive wears are the dominant wear behaviors for original UHMWPE with-out irradiation. The worn surfaces of irradiated samples are completely different from those of unirradiated samples. The ripple like appearances on the surfaces of irradiated samples should be considered as slight fatigue wear behavior. And little scratches and pitting are observed on the worn surfaces of irradiated samples. It means that irradiation can significantly reduce the degrees of adhesive and abrasive wears for UHMWPE. The decreasing wear rate and coefficient of friction for UHMWPE specimens is attributed to the formation of fine wear particles, whereas in the case of higher wear rates it is observed in plate like form. The presence of wear mechanism

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like ploughing, plastic deformation and fatigue in UHMWPE has proved that wear particles follows the pattern of plate like structures. On the other hand presence of wear mechanism like, Ironing, marking or scratching indicates the wear pattern is in the form of fine particles [21].

CONCLUSIONS
The wear behaviour of - irradiated ultra high molecular weight polyethylene sliding against 316L stainless steel was studied in a hip joint simulator. The following conclusions are drawn from the results. The micro hardness of UHMWPE corresponding to 2800C MT has high magnitude when compared to those of 260oC MT and 3000C MT. Because proper bonding is achieved for the case of 2800C MT UHMWPE specimens. The coefficient of friction and wear rate of UHMWPE and - UHMWPE are minimum when the specimens were obtained at 280oC MT where as the specimens obtained at 260oC and 300oC MT has observed with more coefficient of friction and wear rate. Ironing is the predominant mechanism for the specimens corresponding to 280oC MT where as ploughing and scratching are predominant for the specimens obtained at 300oC MT. The specimens corresponding to 260oC were dominated by plastic deformation and Fatigue wear -irradiated UHMWPE specimen has high micro hardness, frictional and wear resistance when compared to that un irradiated UHMWPE. The cross linked structure of polymer chains is mainly attributed to the increase in hardness and enhanced wear behaviour. Finally it can be concluded that the UHMWPE specimens cross linked by -irradiation with radiation dose of 25kGy has slightly improved the friction and wear behaviour of UHMWPE.

REFERENCES
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APPENDICES

Figure 1: a. Femoral Head

Figure 1: b. Acetabular Cup

1. 2. 3. 4. 5. 6. 7. 8. 9.

LOAD CELL VERTICAL ROD CUP HOLDER ACETABULAR CUP ANGEL PLATE ROTATING TABLE SHAFT PULLY ROTATING TABLE SHAFT V- BELT

10. MOTOR 11. MOTOR PULLY 12. FEMORAL HEAD 13. STRAIN GAUGE

Figure 2: Assembly of HIP Simulator

Figure 3: Effect of Different Melt Temperature on Hardness

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UHMWPE before Wear Tests

- UHMWPE before Wear Tests

Figure 4: Sem Images of Unworn Specimens

75N 75N 100N 100N

COF

50N 50N

75N 75N 100N 100N

O 260OC MT 260O C MT

280OC MT 280OC MT

O 300OC MT 300O C MT

Figure 5: Effect of Different MT and Contact Loads on COF

50N

75N

Wear rate

100N
3

50N

75N 100N

260OC MT

280OC MT

300OC MT

Figure 6: Effect of Different MT and Contact Loads on Wear Rate

UHMWPE

-UHMWPE

UHMWPE

-UHMWPE

50N 50N

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IV V IV V

Figure 7a: -UHMWPE at 260OC MT

Figure 7b: UHMWPE at 260OC MT

I I

Figure 7c: - UHMWPE at 280OC MT

Figure 7d: UHMWPE at 280OC MT

III II III II

Figure 7e: -UHMWPE at 300OC MT

Figure 7f: UHMWPE at 300OC MT

Figure 7: Sem Images of Worn Out Specimens