In this work calcium phosphates were synthesized by modified wet chemical precipitation route. Contrary to the conventional chemical precipitation route calcium hydroxide was homogenized with planetary mill. Milling calcium oxide and water in planetary ball mill as a first step of synthesis provides a highly dispersed calcium hydroxide suspension. The aim of this work was to study the influence of main processing parameters of wet chemical precipitation synthesis product and to control the morphology, phase and functional group composition and, consequently, thermal stability and microstructure of calcium phosphate bioceramics after thermal treatment. The results showed that it is possible to obtain calcium phosphates with different and reproducible phase compositions after thermal processing (hydroxyapatite [HAp], β-tricalcium phosphate [β-TCP] and HAp/β-TCP) by modified wet-chemical precipitation route. The β-TCP phase content in sintered bioceramics samples is found to be highly dependent on the changes in technological parameters and it can be controlled with ending pH, synthesis temperature and thermal treatment. Pure, crystalline and highly thermally stable (up to 1300°C) HAp bioceramics with homogenous grainy microstructure, grain size up to 200–250 nm and high open porosity can be successfully obtained by powder synthesized at elevated synthesis temperature of 70°C and stabilizing ending pH at 9
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