β-Tricalcium phosphate (β-TCP) nano powders (∼80nm) were synthesized using a simple sol–gel route with calcium nitrate and potassium dihydrogenphosphate as calcium and phosphorus precursors, respectively. Double distilled water was used as a diluting media for β-TCP sol preparation and ammonia was used to adjust the pH. After aging, the β-TCP gel was dried at 40°C and calcined to different temperatures ranging from 200 to 800°C. The dried and calcined powders were characterized for phase composition using X-ray diffractrometry (XRD) and Fourier transform-infrared spectroscopy (FT-IR). The particle size and morphology was studied using Transmission electron microscopy (TEM). Calcination revealed that with increase in temperature, both the crystallinity and crystallite size of β-TCP particles increased. Particle size distribution analysis of the calcined β-TCP at 800°C showed a narrow skewed distribution plot centered between 70 and 80nm. This value was in closed agreement with particle size values obtained from XRD analysis (83±6nm). The present study showed that narrowly distributed, high crystalline, pure β-TCP could be obtained using this simple technique for biomedical applications.