Two series of molybdenum carbides are prepared from MoO3 by temperature programmed reduction (TPR), differing in feed gas composition (20 and 40% CH4/H-2). The heating ramp consists of two steps, one from ambient temperature to 973 K, at a rate of 10 K/min; the second from 973 K up to the final temperature (1023, 1073, 1123, 1173 K), at a rate of 0.5 K/min. The Mo2C (hcp) phase is identified for the series prepared with 20% CH4/H-2 at different temperatures, with surface areas between 20 and 27 m(2)/g. Also found is a mix of the MoC and Mo2C (hcp) phases for the series prepared with 40% CH4/H-2 at temperatures above 1023 K, with surface areas between 9 and 19 m(2)/g. Both series of catalysts reach 100% conversion of cyclohexene in 5 h or less, with those catalysts prepared with a 40% CH4/H-2 gas mix reaching maximum conversion in the least time. Catalysts are compared to a commercial molybdenum carbide reagent as a reference.