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Ni‐Fe/Al2O3 alloy catalysts obtained from Ni3‐xFexAl (x = 0‐1.2) hydrotalcite‐like compounds are tested in CH4 decomposition at 600°C to produce H2 and carbon. By calcination at 500°C, nickel‐iron‐aluminum hydrotalcite is decomposed into Ni(Fe,Al)O solid solution; upon reduction at 800°C, Ni‐Fe alloy with uniform composition and the average size of 9.4 to 10.3 nm is formed. The Ni‐Fe/Al2O3 alloy catalysts...