Developing catalytic systems with high efficiency and selectivity is a fundamental issue for photochemical carbon dioxide conversion. In particular, rigorous control of the structure and morphology of photocatalysts is decisive for catalytic performance. Here, we report the synthesis of zinc oxide-copper(I) oxide hybrid nanoparticles as colloidal forms bearing copper(I) oxide nanocubes bound to zinc oxide spherical cores. The zinc oxide-copper(I) oxide nanoparticles behave as photocatalysts for the direct conversion of carbon dioxide to methane in an aqueous medium, under ambient pressure and temperature. The catalysts produce methane with an activity of 1080 μmol g_cat⁻¹ h⁻¹, a quantum yield of 1.5% and a selectivity for methane of >99%. The catalytic ability of the zinc oxide-copper(I) oxide hybrid catalyst is attributed to excellent band alignment of the zinc-oxide and copper(I) oxide domains, few surface defects which reduce defect-induced charge recombination and enhance electron transfer to the reagents, and a high-surface area colloidal morphology.

The evolution of the phase and morphology of FeOOH nanorods prepared by a hydrothermal method is studied via X-ray diffraction (XRD) and in situ transmission electron microscopy. The FeOOH nanorod with a tetragonal structure (β-FeOOH) is gradually converted into a rhombohedral Fe₂O₃ nanorod by a simple thermal treatment. The existence of an intermediate FeOOH structure with high lattice strains during the phase transition is identified by Rietveld analysis using XRD. The electrochemical properties of the nanorods are investigated based on the crystal phases to elucidate their relative catalytic activities. The strained-FeOOH nanorods exhibited enhanced catalytic water oxidation activity and stability. Typically, the strained-FeOOH nanorods showed high electrochemical stability under neutral conditions, while tetragonal FeOOH nanorods under the same conditions showed rapid deactivation for water oxidation reaction.

Electrochemical and chemical phase transformations of α-Co(OH)₂ into various other cobalt hydroxides were performed, and their structures were characterized to discern the correlation between electrocatalytic activity and crystal structure.