β-tricalcium phosphate (β-TCP) is a key com-ponent of natural bone like hydroxyapatite. Pure and uni-formly nanosized β-tricalcium phosphate powders were synthesized using a sol-gel self-propagating combustion method by using citric acid as a reductant and using fuel and nitrate as the oxidant. The thermal decomposition of nitrate-citrate xero-gel was studied by thermogravimetric-differential thermal analysis (TG/DTA) and the process mechanism of self-propagating combustion were discussed. The resulting powders calcined at 1023, 1173 and 1273 K were characterized by Ca/P ratio analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmis-sion electron microscopy (TEM). It was found that the as-prepared powders were pure β-tricalcium phosphate having regular porous surface very similar to coral.