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Catalytic methane decomposition is studied in a fixed bed reactor. Two sets of bimetallic catalysts are employed, namely: 30%Fe-X%Ce/Al2O3 and 30%Fe-X%Co/Al2O3, and compared with monometallic 30%Fe/Al2O3 catalyst. The effect of promoting Fe with Ce and Co and reduction temperature are investigated. The results reveal that Ce addition has shown a negative impact on H2 yield while a positive effect on H2 yield and catalyst stability are observed with Co addition. In terms of number of moles of produced hydrogen per active sites, Fe/Al2O3 has shown a higher number of moles of hydrogen compared to bimetallic catalysts. The catalyst reduced at 500 °C exhibits better activity as compared to the catalyst reduced at 950 °C. Carbon nano-tubes are deposited on the catalyst within the range of 14–73 nm diameter.