Solvothermal Synthesis of Calcium-Deficient Hydroxyapatite via Hydrolysis of α-Tricalcium Phosphate in Different Aqueous-Organic Media

In the present work, the effects of various organic solvents (solvent nature and fraction within the solution) and solvothermal conditions on the formation of calcium-deficient hydroxyapatite (CDHA) via hydrolysis of α-tricalcium phosphate (α-TCP) are investigated. The wet precipitation method is applied for α-TCP synthesis, and the hydrolysis reaction is performed in solutions with different water-to-organic solvent ratios under solvothermal conditions at 120˚ C for 3 h and at 200˚ C for 5 h. Ethyl alcohol, isopropyl alcohol, and butyl alcohol did not inhibit the hydrolysis of α-TCP, while methyl alcohol and ethylene glycol have a more prominent inhibitory effect on the hydrolysis, hence the formation of single-phased CDHA. From all the solvents analysed, ethylene glycol has the highest impact on the sample morphology. Under certain water to ethylene glycol ratios and solvothermal conditions, samples containing a significant fraction of rods are obtained. However, samples prepared with ethylene glycol are characterised by a particularly low BET surface area.