Thermally induced crystallization and phase evolution in powders derived from amorphous calcium phosphate precipitates with a Ca/P ratio of 1:1

Calcium phosphate powders of calcium pyrophosphate α1-CPP (the metastable phase of the high-temperature polymorph α-CPP) and the polymorph β-CPP (stable in this range), of α1-CPP, β-CPP, α1-TCP (metastable polymorph of the high-temperature phase α-tricalcium phosphate) and β-tricalcium phosphate β-TCP were prepared by heating amorphous calcium phosphate (ACP) precipitates with the nominal Ca/P ratio of 1:1 by nitrate synthesis. α1-CPP/β-CPP resulted from a crystallization at 530-640 °C and subsequent heating to 980 °C of unwashed and lyophilized ACP. α1-CPP/β-CPP/α1-TCP/β-TCP was formed by crystallization at 620-720 °C, followed by heating of six-time washed and lyophilized ACP precipitates from an ultra-short synthesis. The activation energy for the crystallization of ACP to α1-CPP was determined with 165 kJ mol−1. The reason for the occurrence of the TCP phases (Ca/P ratio=1.5) from ACP (Ca/P ratio=1) is discussed. The powders are prospective biomaterials for bone substitution because they combine effective bioactive phases with the metastable polymorphs α1-CPP and α1-TCP.