A metal-organic chemical vapor deposition (MOCVD) technique was used to prepare heterogeneous metallic catalyst supported on activated carbon. A new system design was built to achieve higher metal loading within a shorter preparation time. In the optimization of system parameters, higher metal loading can be achieved by using longer deposition time, optimum carrier gas flow rate, higher operating temperature of either evaporation zone or a deposition zone or a smaller amount of porous support. Several techniques were carried out to characterize the catalyst such as physisorption, X-ray diffraction, inductively coupled plasma-optical emission spectroscopy and scanning electronic microscopy assisted with the Energy dispersive X-ray spectroscopy (SEM-EDX). It was found that the BET specific surface area and total adsorption volume of the prepared catalysts were reduced after metal deposition, due to the formation of the deposited copper onto the porous media both externally and internally. The morphology of the cylindrical Cu/AC was analyzed by SEM-EDX. The results show that the metal was deposited with a reasonably uniform distribution onto the inner part of the porous support. (C) 2003 Elsevier Science Ltd. All rights reserved.