Dissolution–Precipitation Synthesis and Characterization of Zinc Whitlockite with Variable Metal Content

In the present work, a series of zinc whitlockite (Ca_xZn_y(HPO₄)₂(PO₄)₁₂) powders was synthesized by a low-temperature dissolution-precipitation process for the first time. The phase conversion from calcium hydroxyapatite to zinc whitlockite occurred in an acidic medium in the presence of Zn²⁺ ions. Variable chemical composition of the synthesis products was achieved by changing Ca-to-Zn molar ratio in the reaction mixture. Investigation of the phase evolution as a function of time demonstrated that phase-pure zinc whitlockite powders can be synthesized in just 3 h. It is also demonstrated that single-phase products can be obtained when the Ca-to-Zn ratio in the reaction medium is in the range from 9 to 30. With higher or lower ratios, neighboring crystal phases such as scholzite or calcium hydroxyapatite were obtained. The morphology of the synthesized powders was found to be dependent on the chemical composition, transforming from hexagonal to rhombohedral plates with the increase of Zn content. Thermal stability studies revealed that the synthesized compounds were thermally unstable and decomposed upon heat treatment.