Whisker-reinforced bioactive composites containing calcium phosphate cement fillers: effects of filler ratio and surface treatments on mechanical properties.

Abstract

Calcium phosphate cement (CPC) sets to form microporous solid hydroxyapatite with excellent osteoconductivity, but its brittleness and low strength prohibit use in stress-bearing locations. The aim of this study was to incorporate prehardened CPC particles and ceramic whiskers in a resin matrix to improve the strength and fracture resistance, and to investigate the effects of key microstructural variables on composite mechanical properties. Two types of whiskers were used: silicon nitride, and silicon carbide. The whiskers were surface-treated by fusing with silica and by silanization. The CPC particle fillers were either silanized or not silanized. Seven mass ratios of whisker-silica/CPC were mixed: 0:1 (no whisker-silica), 1:5, 1:2, 1:1, 2:1, 5:1, and 1:0 (no CPC). Each powder was blended with a bisphenol-a-glycidyl methacrylate-based resin to harden in 2 x 2 x 25 mm molds by two-part chemical curing. The specimens were tested in three-point flexure to measure strength, work-of-fracture (toughness), and elastic modulus. Two-way analysis of variance was used to analyze the data, and scanning electron microscopy was used to examine specimen fracture surfaces. The whisker-silica/CPC ratio had significant effects on composite properties (p < 0.001). When this ratio was increased from 0:1 to 1:0, the strength was increased by about three times, work-of-fracture by five times, and modulus by two times. Whisker surface treatments and CPC filler silanization also had significant effects (p < 0.001) on composite properties. Scanning electron microscopy revealed rough fracture surfaces for the whisker composites with steps and whisker pullout. Resin remnants were observed on the surfaces of the pulled-out whiskers, indicating strong whisker-matrix bonding. In conclusion, incorporating highly osteoconductive CPC fillers and ceramic whiskers yielded composites with substantially improved mechanical properties compared with composites filled with CPC particles without whiskers. The composite properties were determined by whisker-to-CPC ratio and filler surface treatments.