Effect of crystallization heat treatment on the microstructure of niobium-doped fluorapatite glass-ceramics.

Our goal was to study the effect of heat treatment temperature and heating rate on the microstructure and crystalline phases and assess the domain of existence of submicrometer fluorapatite crystals in niobium-doped fluorapatite glass-ceramics for biomedical applications. Glass-ceramic specimens were prepared by casting and heat treatment between 700 and 1200°C using a fast or a slow heating rate. The microstructure was characterized by atomic force microscopy and scanning electron microscopy. Crystalline phases were analyzed by x-ray diffraction. AFM of the as-cast glass revealed that amorphous phase separation occurred in this system. XRD confirmed the presence of fluorapatite in all specimens, together with forsterite and enstatite at higher temperatures. Both heating rate and heat treatment temperature strongly influenced microstructure and crystallinity. A dual microstructure with submicrometer fluorapatite crystals and polygonal forsterite crystals was obtained when slow heating rates and crystallization temperatures between 950 and 1100°C were used. Needle-shaped fluorapatite crystals appeared after heat treatment above 1100°C. Fast heating rates led to an increase in crystal size. Heat treatment temperatures should remain below 1100°C, together with slow heating rates, to prevent crystal dissolution, and preserve a dual microstructure of finely dispersed submicrometer crystals without growth of needle-shaped crystals.