Methane decomposition reaction has been studied at three different activation temperatures (500℃
800℃ and 950℃) over mesoporous alumina supported Ni-Fe and Mn-Fe based bimetallic catalysts. On co-impregnation of Ni on Fe/Al
2
O
3
the activity of the catalyst was retained even at the high activation temperature at 950℃ and up to 180 min. The Ni promotion enhanced the reducibility of Fe/Al
2
O
3
oxides showing higher catalytic activity with a hydrogen yield of 69%. The reactivity of bimetallic Mn and Fe over Al
2
O
3
catalyst decreased at 800℃ and 950℃ activation temperatures. Regeneration studies revealed that the catalyst could be effectively recycled up to 9 times. The addition of O
2
(1 ml
2 ml
4 ml) in the feed enhanced substantially CH
4
conversion
the yield of hydrogen and the stability of the catalyst.
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