Published online by Cambridge University Press: 29 July 2019
Numerous fabrication protocols are known to yield transition metal oxides with structures related to layered double hydroxides, but the effect of fabrication protocol on the uniformity of mixed-metal compositions remain largely unexplored. We have analysed the apparent solubility limits and the structural implications of iron ions in nickel hydroxide lattices for materials prepared by four different fabrication protocols. Opposing shifts in the (100) and (001) reflection in powder X-ray diffraction results revealed a contraction of the nickel lattice upon successful incorporation of iron, with Ni-M distances exhibiting an apparently linear decrease with respect to iron content. This feature revealed the amount of iron incorporated into nickel-based materials to be dependent on fabrication protocol, varying from apparently negligible concentrations to over fifty atomic percent. The dependency of structure on fabrication protocols provides a handle to improve fundamental understanding of catalytically relevant coordination environments.