Materials & Methods

UHMWPE resin powder (GUR 1050, Ticona, USA) was mixed with dl-a-Tocopherol (vitamin E) at 0.3 wt% and molded under direct compression at 25 MPa and 220°C. Virgin samples were produced by the same process, but without the addition of vitamin E (VE). Cylindrical pins (length: 40 mm, diameter: 3.5 mm) were then machined from these samples, packaged in a vacuum, and irradiated by electron-beam at 300 kGy. Samples were subsequently doped with either ascorbic acid 6-palmitate (Sigma, Japan) or ethanol (Ethanol 99.5%, Kishida, Japan) and subjected to a hydrostatic pressure of 100 MPa for 7, 14, and 21 days at room temperature. Radical measurements were made using ESR at 9.44 GHz and room temperature. All ESR spectra were recorded at 0.1 mW microwave power and 0.1 mT modulation amplitude.

Materials and Methods

VE blended samples (GUR_VE xx%) were manufactured via direct compression molding following the blending of UHMWPE resin powder with VE at several concentrations (0, 0.1, 0.3, 1.0%). Cross-linking for the VE samples was achieved by 10 MeV electron beam at several irradiance doses (30, 90, 300 kGy) and annealed below the melting point of UHMWPE.

Knee and hip simulator testing were carried out according to ISO 14243 and ISO 14242, respectively, and the volumetric wear was calculated. The gel fraction was determined by measuring the weight of the samples before and after soaking in decahydronaphthalene at 150°C. The oxidative resistance of the material was determined by measuring the Oxidation Index (OI) following ASTM F2102 before and after compulsory aging (ASTM2003). Radical measurements were made using high-sensitivity X-band ESR.

MATERIALS & METHODS

Both pure UHMWPE and Vitamin E added (0.3% w/w) resin was used to produce bulk specimens via vacuum direct compression molding at 220°C under 25 MPa for 30 min. Cylindrical pins (3.5 mm diameter, 40 mm length) for ESR measurement were then machined and placed in vacuum packaging. The pins were irradiated at 300 kGy, with half of each test group annealed at 80°C for 24 hours. Free radical measurements were made using a high-sensitive X-band ESR operating at 9.44 GHz. Detection of Vitamin E radicals was performed by comparing the characteristic symmetrical spectrum of oxidized Vitamin E to the spectra observed for the pins using both g-value and linewidth as references. Crosslink density was measured via gel fraction analysis and was performed in accordance with ASTM D2765. Thin sections (20 × 40 mm², 200 μm) were machined from the bulk specimens, which were then placed in vacuum packaging, irradiated and annealed at the same conditions as those for the ESR measurements. Two of these thin sections were then placed in a stainless-steel cage (200 µm pore diameter) and were immersed in decahydronaphtalene at 200°C for 24 hours. These specimens were then extracted using soxhlet extractor at 100°C for 24 hours and dried in vacuum at 150°C for 12 hours.