Synthesis, X-ray diffraction and solid-state 31P magic angle spinning NMR study of ?-tricalcium orthophosphate

Abstract

The effects of synthesis conditions on the quantitative preparation of α-tricalcium phosphate (α-TCP) have been investigated. The following parameters of the synthesis were considered: nature of the starting material-Ca-deficient hydroxyapatite, DAP, versus hydroxyapatite-anhydrous dicalcium phosphate mixtures (HAP-DCPA); Ca/P atomic ratio of the mixture, calcination temperature and time, and cooling rate. The yield and crystallinity of the final product have been estimated using X-ray diffraction (XRD) and solid state 31P magic angle spinning NMR (MAS-NMR) techniques. The results show that pure, well-crystallized α-TCP powders exhibiting nearly ideal MAS-NMR spectra, can be obtained by reactive sintering of HAP-DCPA (Ca/P=1.50...1.52) mixtures, at 1400°C for 8 h. The broadening of MAS-NMR spectra can be used as an indicator of structural order in the final product. The α-TCP yield with DAP was always less than 50%.