Considered one of the weak links in the total hip replacement (THR), efforts to enhance the interfacial strength between bone cement and ultra-high molecular weight polyethylene (UHMWPE) acetabular cup had been conducted in this laboratory. Following the successful demonstration of high interfacial strengths for our new acetabular component design, the nature of physical, chemical, and thermal property of the compression-molded specimens, including UHMWPE, PMMA/MMA treated UHMWPE, and PMMA has been investigated in this study. Density results from a density gradient column showed that the molding processes and conditions were adequate for complete sintering of UHMWPE and PMMA powders. FTIR-ATR results gave a direct evidence that PMMA did exist in the PMMA/MMA treated UHMWPE matrix. It also revealed a clear diffusion-related behavior across the interface. Under the high temperature and pressure, the UHMWPE powders undergo drastic changes of their morphology and crystalline structures. These changes were examined by differential scanning calorimeter (DSC) which showed a large difference in terms of % crystallinity. The percent of PMMA deposited in the treated UHMWPE was 17.8%, 18.8%, and 24.3% from the analyses of density, FTIR-ATR, and DSC, respectively. Finally, an evidence of diffusive behavior at the interface exhibited diffusion of PMMA occurring across the interfaces between the treated UHMWPE and UHMWPE or PMMA.