Effect of compaction pressure and atmosphere on sintering of nanometric iron powders : J. Bigot et al (CRNS, Vitry sur Seine, France)

Abstract

This study describes the effect of sintering temperature on the microstructural, calcium/phosphorus (Ca/P) ion ratios and mechanical properties of non-separated biowastes processed hydroxyapatite (HAp) prepared through a low cold compaction protocol. The HAp was produced by a sintering temperature of 900 °C. Furthermore, HAp sintered at 900 °C was subjected to sintering temperatures of 1000 and 1100 °C.The structural and morphological evolution of the fabricated biomaterials were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with electron dispersive X-ray analysis (EDX) respectively. Uniaxial compaction using a pressure of 500 pa was used to produce rectangular shaped pellets to investigate the influence of sintering temperature on the mechanical properties of the produced pellets. From XRD analysis, it was found that hydroxyapatite derived from the biowastes showed good thermal stability and did not exhibit phase instability with traces of other calcium phosphates. The SEM micrographs showed microporous structure of the biomaterials and an increase in temperature reduced the porosity and enhanced the mechanical properties. It was also noticed that the trend of transformation of the average shape of pores was from strongly flattened to round at higher sintering temperatures. Electron dispersive X-ray analysis (EDX) revealed that the atomic Ca/P ratios of the as-sintered HAp specimens ranged from 1.58 to 1.79 for sintering temperatures of 900–1100 °C. The synthesized hydroxyapatite powder showed inclusion of the fluorapatite phase at sintering temperature of 1000 °C with a reduction in the crystallite size. For both scenarios (sintering temperature and compaction pressure), a consistent trend in mechanical properties (microhardness, fracture toughness and Young's modulus) is noticed at every point of measurement except for compressive strength. The reduction in compressive strength when compaction pressure was applied could be as a result of the stress induced in the HAp powders during compaction which may have made it more susceptible to cracks. The hardness value obtained for the synthesized hydroxyapatite pellets is in the range of that of actual human femoral cortical bone.