Cerium oxide (CeO₂) catalyst was prepared by oxalate precipitation method. Effect of calcination temperature (500 to 1000 ^oC) on structure and properties of CeO₂ catalyst was studied. The catalyst was characterized by X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) method, Thermogravimetry analysis (TGA) and Scanning electron microscopy (SEM). The catalytic activity of CeO₂ for the transesterification of palm oil with methanol to biodiesel production was investigated. It was found that the CeO₂ calcined at 900 ^oCgave a high activity with fatty acid methyl ester (FAME) content of 96% under the conditions: molar ratio of methanol to oil of 30:1, catalyst loading of 10 wt%, reaction temperature of 200 ^oC, reaction pressure of 39 bar and stirring rate of 600 rpm for 5 h. The calcination temperature had significant effects on the crystallite size, surface area and total pore volume of CeO₂. The average crystallite size, surface area and total pore volume of CeO₂ catalyst calcined at 900^oC was 47.40 nm, 8.49 m²/g and 0.012 cm³/g respectively. The SEM results showed that the particle of catalyst was from less than10 nm to several microns. The large pore volume of CeO₂ catalyst was observed, which enhanced the catalytic performance for transesterification of palm oil.