In this study, the effects of glycine-nitrate ratios and postcombustion chemical treatment on the phase evolution and surface area of CuCrO2powders were investigated. The pure phase of CuCrO2powders was obtained at a glycine-nitrate ratio of 1.2–1.4. When the glycine-nitrate ratio was higher than 1.9, the Cu ions were reduced to Cu(0) and the phase of Cu metal and Cr2O3were observed. However, when the glycine-nitrate ratio was lower than 1.1, the Cu ions were partially maintained as Cu(2+), and a bluish residue was observed. As-combusted CuCrO2powder with a high surface area (50 m2/g) was obtained at a glycine-nitrate ratio of 1.2. Furthermore, a high surface area (> 60 m2/g) was obtained by leaching as-combusted CuCrO2powder with diluted nitric acid.