Control of hydroxyapatite crystallinity by mechanical grinding method

Abstract

Crystallinity of hydroxyapatite reflecting crystal size and crystal elastic strain was controlled by the mechanical grinding (MG) technique using a set of container and balls made of SUS304 stainless steel or agate. Variation in the crystallinity through MG was monitored by the XRD method and represented by the broadening of the diffraction peak. Effect of changes in crystallite size and strain on the crystallinity was also examined using the Hall-plot method. Crystallinity rapidly decreased with milling time. Significant crystallographic diffraction peaks disappeared and a broad diffraction around 2theta=32 degrees was observed after MG for 72 h. The broadening was dominantly due to an increase in crystal strain in addition to fine crystallite size. Contamination from the container and balls during MG was more suppressed using agate than SUS304 stainless steel. The recovery process of crystallinity during heating between 300 degrees C and 1200 degrees C was examined focusing on the decrease in residual elastic strain. Low crystallinity was maintained at annealing temperatures below 800 degrees C but lattice defects were recovered above 1000 degrees C.