Hydrothermal synthesis of calcium-deficient hydroxyapatite whiskers and their thermal transformation to polycrystalline β-tricalcium phosphate short fibers

Resorbable calcium phosphate fibers are of particular interest to reinforce biodegradable bone substitutes for load-bearing applications. The aim of the present study was to prepare calcium-deficient hydroxyapatite (dHAp) whiskers with a molar Ca/P ratio of 1·5 by a hydrothermal synthesis and to transform them to β-tricalcium phosphate (β-TCP) by a subsequent thermal treatment. For the hydrothermal synthesis, calcium tripolyphosphate was used and different amounts of 2-propanol were added to adjust the pH. Average whisker lengths of 160 µm were obtained at a 2-propanol content of 27 volume-percent. However, 33% dicalcium phosphate anhydrate (DCPA) were present as a secondary phase. The amount of DCPA could be reduced by increasing the amount of 2-propanol. Whisker samples consisting of 88% dHAp and 12% DCPA were selected to investigate microstructural changes and phase transformations during thermal treatment. Polycrystalline single phase -TCP short fibers were obtained after a thermal treatment at 1125°C.