Mechanochemical synthesis and structural characterization of nano-sized amorphous tricalcium phosphate

Nano-sized amorphous tricalcium phosphate powders were synthesized through different mechanochemical reactions. The influence of milling parameters and chemical composition of reagents on the formation of amorphous tricalcium phosphate was investigated. In all the experiments, the mole ratio of calcium to phosphorous oxide was 3:1, i.e. the stoichiometric Ca/P content in the composition of amorphous tricalcium phosphate (Ca/P=1.5). Results revealed that the phase purity, structural features, and morphological characteristics of products were significantly influenced by the chemical composition of raw materials and milling parameters. For all the reactions, amorphous tricalcium phosphate was formed as the main product of mechanical activation after 10 h. After annealing at 1100 °C, crystallization of amorphous phase occurred, and consequently high crystalline β-tricalcium phosphate was generated. According to FT-IR findings, the synthesized powders had high chemical purity. After 10 h of milling, the obtained nanopowders through four distinct reactions exhibited crystallite sizes about 20, 69, 58 and 55 nm. The results from scanning electron micrographs showed that the mean size of agglomerate was in the range of 1–5 μm. Detailed study of morphological features by using transmission electron microscopy confirmed the formation of nano-sized amorphous tricalcium phosphate with spheroidal and ellipse-like morphologies.