Abstract A novel approach was employed in the synthesis of high-dispersed anatase titania (TiO 2) nanocrystals by sol–gel process with NH 4NO 3 (AN) as solid substrates. Further calcination was conducted after the hydrous TiO 2 nanoparticles were adsorbed onto the surface of AN particles. The products were investigated by TGA, XRD, and TEM. The results indicated that AN was melting and decomposing during the calcining process, which was very important to inhibit the agglomeration of anatase TiO 2 nanocrystals. The highly dispersed anatase TiO 2 nanocrystals were in needle-shape having lengths about 16–20 nm and diameter of 6–9 nm.