An horizontal hot-wall MOCVD reactor was used to prepare palladium and platinum catalysts supported on alumina. A conventional impregnated Pt on alumina catalyst was prepared as comparison. The solids were characterized by XRD, Auger spectroscopy, HREM and H2 -TPR. The operation conditions of the MOCVD reactor were fixed preparing several Pd catalysts until to find the appropriate deposition zone. The particle size of Pt catalysts prepared by MOCVD was at about 7 nm compared with 6 ran obtained with the Pt impregnated catalyst, measured by XRD. The HREM image of the Pt MOCVD catalyst showed a narrower particle size ranging from 1 to 4 nm. After calcination three Pt compounds were detected by TPR, which were attributed to PtO, PtO2 and Pt-Al2O3 interaction in MOCVD preparation. Additionally, a clear reduction of surface oxygens of alumina was also observed.