Nanocrystalline potassium titanyl phosphate (KTiOPO4, KTP) powder with average particle size of 25-50 nm has been synthesized from aqueous solution of titanyl chloride through coprecipitation method, using aqueous solution of potassium dihydrogen phosphate and potassium carbonate in the presence of triethanolamine (TEA) as a capping agent. In the presence of tetrapotassium pyrophosphate as a capping agent it produces the particles having average size around 70-80 nm. The same sample with average particle size similar to 250 nm has also been synthesized without any capping agent. Initial amorphous phase after precipitation requires heat treatment at 500-550 degrees C for 2 h to generate nanocrystalline powders of KTP. Formation of the KTP phase in the heat-treated samples has been confirmed through X-ray powder diffraction, thermogravimetric and differential thermal analysis, P-31 Magic angle spinning-nuclear magnetic resonance and Fourier transform infrared spectroscopy studies, and surface area measurements.