Amorphous hierarchical NiCo2O4–CoNiO2hybrids have been successfully fabricatedviaa facile one-pot hydrothermal route, followed by morphologic conversion into urchin-like structured NiCo2O4–CoNiO2nanorods and irregular-shaped hierarchical NiCo2O4–CoNiO2polyhedral nanocrystals through air-annealing treatment at 450 °C and 650 °C, respectively.

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Uniform multishelled NiO, Co3 O4 , ZnO, and Au@NiO hollow spheres were synthesized (NiO and Co3 O4 hollow spheres for the first time) by a simple shell-by-shell self-assembly allowing for tuning of the the size, thickness and shell numbers by controlling the heat treatment, glucose/metal salt molar ratio, and hydrothermal reaction time. These findings further the development of synthetic methodologies for multishelled hollow structures and could open up new opportunities for deeper understanding of the mechanisms of shell-by-shell self-assembly. Moreover, the double-shelled NiO hollow sphere exhibits a higher photocatalytic activity for degradation of methyl orange than its morphological counterparts.