Perovskite-type LaCoO 3 oxides were prepared by spray-freezing/freeze-drying method using citrate precursor. The calcination temperature for a single phase of LaCoO 3 could be lowered to 500°C without formation of any other oxides and the product had the highest surface area of 23.7m 2 /g. Below 500°C, this catalyst with the perovskite structure and the high surface area showed higher activity for complete oxidation of low concentration methane (2000ppm) and CO (1%) compared to Pt/Al 2 O 3 catalyst.