One kind of lanthanum cerium fluoride abrasive was prepared using the raw materials Ce2(CO3)3, La·Ce(CO3)3, and NH4F at temperatures of 400–1050 °C. The combined techniques of X-ray diffraction with Rietveld refinements, scanning electron microscopy, and X-ray photoelectron spectroscopy were employed to characterize the products. It was found that the materials are all made up of agglomerated irregular block-shaped particles with particle sizes in micrometer ranges. Below 850 °C, the product is a mixture of cubic CeO2and trigonal LaF3, while above 900 °C, it is a mixture of cubic CeO2and tetragonal LaOF. A higher calcination temperature suppresses the formation of the LaF3phase but enhances the LaOF phase. The Ce in the prepared material is present in mixed states of Ce3+and Ce4+, and the Ce4+/Ce3+ratio increases with increasing calcination temperature. When the material prepared at 900 °C was used in the polishing test on K9 glass, the obtained polishing surface is very clean and flat, and the thickness difference before and after grinding is moderate, indicating its potential as an abrasive for polishing the surface of optical glass.