The effects of calcination temperature on catalyst properties were studied on fibrous Ni/Al2O3 catalysts prepared by electrospinning, utilizing its high thermal and structural stability. The average Ni particle size was increased up to 27.1 nm as calcination temperature was increased from 700 to 1000 degrees C due to the increased NiAl2O4 crystal size, which also caused the higher reduction temperature required according to temperature-programmed reduction results and the lower catalytic activity in the dry reforming of methane. Interestingly, a higher reduction temperature resulted in more and uniform Ni particles instead of catalyst aggregation. It might be the reason that the high reduction temperature thermodynamically promoted Ni nucleation on the NiAl2O4 surface to initiate Ni precipitation from ceramic bulk. The catalytic activity in the dry reforming of methane confirms the reduction temperature effect. (C) 2016 Elsevier B.V. All rights reserved.