A Room Temperature Chemical Process for Homogeneous Mixing of Precursor Phases for Low Temperature Tetracalcium Phoshate Preparation

Abstract

The aim of this study was to prepare phase pure tetracalcium phosphate (TTCP) from the precursor phase mixtures homogeneous at the nano/microscale level at lower heat treatment temperatures in much shorter dwell times. Two different precursor powder mixtures were prepared by reacting CaCO3 with H3PO4 in ethanol or water. The resultant precursor powder mixtures were heat treated at temperatures in the 1200–1350 °C range for 2 and 5 h. Phase structures of the powders were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) and Raman spectroscopy analysis. Scanning electron microscopy (SEM) was used for the investigation of powder particle sizes and morphology. Powders synthesized by the heat treatment of both of the starting powder mixtures prepared in ethanol or water with 2 and 5 h of dwell times at 1350 °C were determined to be phase pure TTCP. SEM analysis along with the phase identification showed that the precursor powder prepared in ethanol had micron sized plates formed by aggregation of sub-micron sized thin CaHPO4 plates covering CaCO3 particles. The precursor powder prepared in water contained large aggregates of sub-micron sized CaCO3 particles whose surface was covered by precipitated nano-sized hydroxyapatite. TTCP powders were composed of large irregularly shaped particles formed by sintering of smaller equiaxed grains. Average grain and particles sizes of the TTCP powders synthesized from the precursor powder prepared in ethanol were 3.2–3.9 and 8.1–8.4 μm, respectively. Average grain and particle sizes of the TTCP powders synthesized from the precursor powder prepared in water however were measured to be 3.3–5.1 and 11.2–11.6 μm, respectively. The TTCP preparation method presented in this study provides homogeneous and well-mixed precursor powders prepared from cheap and commonly available precursors without milling and decreases the heat treatment time to 2 h at 1350 °C. © 2024 Elsevier Ltd and Techna Group S.r.l.