Journal of Chemical and Pharmaceutical Research (ISSN : 0975-7384)

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Original Articles: 2014 Vol: 6 Issue: 9

Effects of hydrolyzation, aging time and temperature on rheology of sols and effects of aging and sintering temperatures on structural and thermal properties of calcium phosphate powders

Abstract

Among the various process parameters of sol-gel technique, aging time and temperature play decisive roles and affect the properties of precursors, sol and synthesized product to a large extent. A detailed analysis including various rheological properties of Calcium and Phosphorous based precursors at ambient temperature and Calcium Phosphate sol at 5°C and 25°C have been carried out in the present paper. Comprehensive effects of aging temperatures on structural and thermal properties of Calcium Phosphate based powders have also been characterized by using X-Ray Diffraction, Fourier Transform Infrared, Thermogravimetric/Differential Scanning Calorimetery, Transmission Electron Microscopy and Scanning Electron cum Energy Dispersive Microscopy. The hydrolysis of precursors was found to have profound effect on their rheology. pH and density of CaP sols were found to be independent on aging time and temperature. Formation of calcium deficient HAP, HAP, β -TCP and α - TCP in CaP powders were revealed from XRD patterns. FTIR results showed the presence of HPO4 -2and PO4 ions for all sintering temperatures in both the aged powders. SEM showed the powders have granular, irregular, loose but smooth mixture of solid rod and plate like nano regime particles. Average particle size ranged from 100-150 μm and 105-180 μm for powders aged at 25°C and 5°C respectively. EDX presented the results in line with XRD detections. Hexagonal shape of crystals having sharp edges of both the powders was observed from TEM micrographs. Larger crystals were observed in case of 25°C aged powders.