LAUSR

NiAl2O4‐based materials are known as enhanced catalysts for several catalytic applications that have coke deposition in common. In this study, Nb as a dopant was found to occupy the octahedral sites of the spinel preferably. As a result, the cation distribution was altered between the two sub‐lattices of the cubic spinel. Therefore, ordered modifications of nickel migration, electronic profile, redox properties and surface textures were observed for these catalysts. Also, coke deposition over these catalysts was controlled using Nb doping and found to modify the original features of the fresh catalysts and lower their crystallite sizes. This study suggests reasons why NiAl2O4 spinel performs so well in the majority of the high‐temperature catalytic processes that suffer from coke deposition.