Catalysts are studied by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), thermogravimetric analysis (TG) and X-ray diffraction (XRD). Cu and Zn mix homogeneously in catalyst U8 prepared by oxalate gel-coprecipitation method. However, Cu aggregates on the surface of catalyst C9 made from conventional ammonium bicarbonate coprecipitation procedure. The difference of the element distribution makes the reduction of C9 easier than that of U8. The process used to treat the precipitates of U8 is helpful to the isomorphous substitution of Cu and Zn. ZnO exists mainly as amorphous particles or minor crystals. The methanol synthesis activity of U8 is higher than that of C9 by an order of magnitude.