Design of the synthesis of fine HA powder for suspension plasma spraying

Hydroxyapatite (HA, Ca₁₀(PO₄)₆(OH)₂) is a bioactive material being frequently used as a coating onto implants. The typical coating technology is air plasma spraying with the use of coarse powder. The resulting coatings are relatively thick (about 200-400 µm) and porous. Much thinner coatings being 5-40 µm thick, can be obtained by emerging technology of suspension plasma spraying with the use of powder particles having the diameters ranging from a few submicrometers to a few micrometers. The paper describes the way of synthesizing and preparing such fine powder starting from an aqueous solution of ammonium phosphate (H₂(PO₄)NH₄) and calcium nitrate (Ca(NO₃)·4H₂O) using statistical design of experiments (DOE). The design was made using composite matrix including a full factorial plan, star points and 3 experiments in the centre. The crystal phases purity and the mass of powder batch were the optimized responses of the powder synthesis and the concentration of calcium ions and volume of ammonium hydroxide were the experimental variables. The synthesized material was characterized by X-ray diffraction (XRD). The powder was calcined and crushed using a milling machine with zirconia balls and resulting morphology and size of fine particles was characterized using scanning electron microscope (SEM) and laser sizer correspondingly. The powder was then formulated into water and alcohol based suspension and the zeta potential was determined to understand its capacity of agglomeration. It was found out that the formulation of the suspension with the use of ethanol slightly favours dispersion of solid particles in the suspension. The initial tests of water based suspension plasma spraying onto titanium substrate were also carried out and the XRD phase analysis of obtained coatings was carried out the presence of HA and its phases of decomposition.