Octahedral ceria abrasives with varied microstructures were prepared by calcining a hierarchical precursor at 500–900 °C. The relationship between calcination temperature and microstructure, mechanical hardness and chemical activity was investigated.

Layered quasi-triangular Ce(OH)CO 3 assembled from primary nanoparticles was synthesized via a solvothermal method and converted into CeO 2 abrasive particles by calcination at 800−1000 °C. With the increase of calcination temperature, the primary particle size increased and the microstructure, mechanical hardness, and chemical activity of the CeO 2 particles changed, thus affecting the polishing performance. The calcined products obtained at 800, 850, and 900 °C maintained the layered edge structure of the Ce(OH)CO 3 precursor and had a relatively high specific surface area and surface Ce 3+ concentration. The samples calcined at 950 and 1000 °C lost the layered structure due to the large-scale melting of the primary particles, and their surface chemical activity decreased. The polishing experiments on K9 glass showed that, with the calcination temperature rising from 800 to 1000 °C, the material removal rate (MRR) first increased and then decreased sharply. The initial increase of MRR was attributed to the increase of mechanical hardness of the layered quasi-triangular CeO 2 , and the subsequent decrease of MRR was related to the decrease in surface chemical activity and disappearance of the layered edge structure. The product calcined at 900 °C had the highest MRR and best surface quality after polishing due to the layered edge structure and optimal match of chemical activity and mechanical hardness.