In this work, we confirmed that dielectric barrier discharge (DBD) plasma is excellent for the decomposition of carbonates to prepare CuO-ZnO catalysts in a rapid and energy efficient way. According to the characterization using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Field Emission Scanning Electron Microscope (FE-SEM), the DBD plasma generated CuO-ZnO catalyst was smaller in particle size with higher copper-zinc surface ratio, compared to the catalyst prepared thermally. Diffuse reflectance infrared Fourier transform (DRIFT) analysis and the activity test showed that the DBD plasma prepared catalysts had higher activities towards synthesis of methyl formate (MF) directly from syngas.