Carbonyl-precursor-based alumina supported rhenium catalysts were prepared by controlled gas-phase sublimation technique. Oxygen pulse chemisorption results showed the rhenium particles to be well dispersed. With successive deposition-decarbonylation cycles metal loading was increased by controlled manner, and the dispersion was better than for catalysts with similar metal content prepared in a single deposition step. Temperature-programmed reduction profiles showed that the interaction between oxidised rhenium particles and the support becomes weaker with increasing rhenium content. Reduction behaviour of the catalysts prepared with total decarbonylation steps differed from that of catalysts prepared by single-step method. Accurate oxidation temperatures were determined by temperature-programmed oxidation.