Structural evolution of Ni-based Co-catalysts on [Ca2Nb3O10]− nanosheets during heating and their photocatalytic properties

Abstract

Nickel compounds are among the most frequently used co-catalysts for photocatalytic water splitting. By loading Ni(II) precursors, submonolayer Ni(OH)2 was uniformly distributed onto photocatalytic [Ca2Nb3O10]− nanosheets. Further heating of the nanocomposite was studied both ex situ in various gas environments and in situ under vacuum in the scanning transmission electron microscope. During heating in non-oxidative environments including H2, argon and vacuum, Ni nanoparticles form at ≥200◦C, and they undergo Ostwald ripening at ≥500◦C. High resolution imaging and electron energy loss spectroscopy revealed a NiO shell around the Ni core. Ni loading of up to 3 wt% was demonstrated to enhance the rates of photocatalytic hydrogen evolution. After heat treatment, a further increase in the reaction rate can be achieved thanks to the Ni core/NiO shell nanoparticles and their large separation.