The aim of this study was to investigate the sol gel synthesis of HA/FA nanoparticles and the possible formation of TCP phase or unstoichiometric calcium deficient hydroxyapatite (CDHA) from the precursors with a Ca/P ratio of 1.62. In order to prepare the sol, the solutions of Triethyl phosphite, ammonium fluoride and calcium nitrate in ethanol were used respectively as P, F and Ca precursors. The crystallinity, particle and crystallite size, powder morphology, chemical structure and phase analysis were investigated by SEM, XRD, FT-IR and Zeta sizer experiment. A multiphase compound containing hydroxyapatite (HA) and fluoroapatite (FA) nanoparticles and calcium deficient hudroxyapatite (CDHA) agglomerates was obtained. The size of the crystallites estimated from XRD patterns using Scherrer equation and the crystallinity of HA phase were about 5 nm and 66% respectively. The zeta sizer experiments for the dispersed particles in its own conditions showed an average size of 98 nm.