The densification and sintering behaviour of molten salt synthesized Ha whisker/Ha composites

Abstract

The hydroxyapatite (HA) whiskers were used as reinforcements in the HA powder/HA whisker (HAp/HAw) composites. The HAw was synthesized with molten salt synthesis method (MSS). NaCl, K2SO4 and NaCl-K2SO4 fluxes and HA powders were used for the synthesis of HA whiskers. The effects of various salt/HA ratios, heat treatment temperatures and time were investigated. In order to enhance the dispersibility and the elimination of the powder agglomerates ultrasonic treatment was applied to the HA-salt powder mixtures before heat treatment. Scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques were used for the examination of the whiskers. The synthesized whiskers by using NaCl had a broad particle size range (0.25 to 40 mm in length and 0.2 to 20 mm in diameter) and similar morphologies. They had relatively larger diameters than those suitable for use as reinforcements in the HAp/HAw composites. The use of K2SO4 resulted in the formation of relatively uniform and thinner HA whiskers. The length and diameter of the whiskers varied from 5 to 90 mm and 0.5 to 10 mm, respectively. The whiskers prepared from NaCl-K2SO4 salt mixture were 12 to 110 mm in length and 0.5 to 25 mm in diameter. The HA whiskers, synthesized from NaCl-K2SO4 salt mixture and HA powder at 850°C, were selected as reinforcements for the composites because of their uniform morphology and dimensional properties. For the preparation of HAp/HAw composites, HA powder was ball milled and mixed with HAw in aqueous medium with the application of 2 h ultrasonic treatment. Sintering was carried out at 1200-1350°C range for 2 h. Pure HA powder shrunk more than the composites at all sintering temperatures and attained to 98.5% theoretical density at 1350°C. Although the density increases with sintering temperature, the density increase relative to the green structures decreases with whisker content at each sintering temperature. This may be attributed to the low shrinkage rate due to the presence of whiskers at high temperatures. The HA whiskers could be observed as embedded in the fine HA matrix for both slip cast and dry pressed samples from the SEM images. It was observed that the whiskers generally aligned in one direction except the 50% HAw-50% HAp composites.