One-step synthesis of dimethyl ether (DME) from H-2/CO has been studied in a fixed bed reactor over hybrid catalyst CuOZnOAl2O3/gamma-Al2O3-HZSM-5. The physicochemical properties of fresh and used catalysts were also studied by means of H-2-TPR, XRD and N2O chemisorptions. The results showed that for deactivated catalysts by sintering, redox cycle was an effective method for in-situ regeneration. There were two different regeneration mechanisms according to various atmospheres: (i) For O-2-syngas cycle, sintered Cu particles were re-dispersed and initial activity was restored mostly. The process was reversible, which was called reversible regeneration; (ii) for N2O (CO2)-syngas cycle, Cu particles could not be re-dispersed and catalytic activity was restored a little due to the regulation of surface state. On the other hand, this process could depress the deactivation velocity and was irreversible, which was called irreversible regeneration.