Doped and undoped TiCh nanoparticles were prepared by Stober method and thermally treated at 600 ℃.The effect of Nd~(3+) ion on the structure and micro structure of anatase-phase TiCh nanocrystals was studied by Rietveld refinement method using X-ray powder diffraction data.Bond lengths,bond angles,and edges distances were analyzed.The phase formation was confirmed by high-resolution transmission electron microscopy.The adjustment of Ti-0 bond length induced by the addition of Nd~(3+) ions,reduced the octahedral distortion and altered the octahedral array in the anatase-phase TiCh nanocrystal.The changes of structure and microstructure were mainly observed for TiCh nanoparticles doped with 0.1 at.%of Nd~(3+) ions and attributed to the cationic substitution of Ti~(4+) ions which promoted changes in the density of states and gap band of TiCh.The dopant insertion resulted in a better structural stability of the nanocrystals that enhanced their charge transference and photocatalytic efficiency. Doped and undoped TiCh nanoparticles were prepared by Stober method and thermally treated at 600 ° C. The effect of Nd ~ (3 +) ion on the structure and micro structure of an anatase-phase TiCh nanocrystals was studied by Rietveld refinement method using X-ray powder diffraction data. Bond lengths, bond angles, and edges detected were the high-resolution transmission electron microscopy. The adjustment of Ti-0 bond length induced by the addition of Nd ~ (3+) ions, reduced the octahedral distortion and altered the octahedral array in the anatase-phase TiCh nanocrystal. The changes of structure and microstructure were primarily observed for TiCh nanoparticles doped with 0.1 at.% of Nd ~ (3+) ions and attributed to the cationic substitution of Ti ~ (4+) ions promoted by the density of states and gap band of TiCh. Dopant insertion resulted in a better structural stability of the nanocrystals that enhanced their charge transference and photocatalytic effi ciency.