Formation and decomposition of the Cu-Co alloy and Co2C were studied using in situ X-ray diffraction (XRD), TG-DTA and TEM techniques. Cu-Co alloy with ratio Cu/Co = 1:1 has been obtained under treatment of CuCoO2 with hydrogen at 230-300 degrees C. Co2C was formed from Cu-Co alloy at 280-310 degrees C and decomposed at 390-400 degrees C under CO. It was shown that the role of Cn-Co alloy consisted in formation of cobalt carbide was able to activate CO undissociatively that led to oxygenates synthesis.