Metal–organic chemical vapor deposition (MOCVD) technique has proven its potential for the preparation of the highly active catalysts. The clear advantage of this technique, comparing with the typical solution-phase method, is that unwanted effects of the solvent can be completely avoided if the loading is carried out in the gas phase. Moreover, the molecular organo-metallic precursors tend to cleanly generate the desired materials with controlled growth rate at relatively low growth temperature. There is in principle no limit in respect to the simultaneous maximization of the specific copper surface area and the Cu/ZnO interface area, and thus no limit to the increase of the catalytic activity beyond that which is currently possible. In order to maximize the specific copper surface area and the Cu/ZnO interface area, the loading of copper in the matrices can be increased by the repetition of the loading cycles. Furthermore, the combination of different Cu precursors with different zinc- and aluminium-oxide precursors opens up a certain degree of freedom to optimize the loading process. In addition, fluidized bed type chemical vapor deposition as an industrially relevant catalyst preparation technique can be applied. Current achievements of this work include successful deposition of Cu/ZnO catalysts by the MOCVD using templated silica as a support. The molecular control of the Cu/ZnO interface is achieved by variation of dimension and framework of the pores and by exploration of the precursor chemistry. After the first loading cycle, the specific copper surface area of the obtained Cu/ZnO@PMS samples was in the range of 5-6 m²Cu/g_cat, while the XRD and EXAFS studies revealed exceptionally low copper crystallite size and degree of aggregation. The methanol synthesis performance is found to be 19-130 μmol/g_cath, using a special catalytic test set-up referenced to the industrial ternary catalyst having a value of about 450 μmol/g_cath.