In this work, mesoporous nickel oxide (NiO) hierarchical nanostructures were synthesized by a facile approach by hydrothermal reaction and subsequent calcination. The phase structure, microstructure, element composition, surface area, and pore size distribution of the as-prepared products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and the Brunauer–Emmett–Teller (BET) technique. The precursor of Ni3(NO3)2(OH)4 nanosheet, Ni3(NO3)2(OH)4 microsphere, and Ni(HCO3)2 sub-microsphere was obtained by hydrothermal reaction at 160 °C for 4 h when the ratio of Ni2+/HMT (hexamethylenetetramine) was 2:1, 1:2, and 1:3, respectively. After calcination at 400 °C for 2 h, the precursors were completely transformed to mesoporous NiO hierarchical nanosheet, microsphere, and sub-microsphere. When evaluated as additives of the thermal decomposition of ammonium perchlorate (AP), these NiO nanostructures significantly reduce the decomposition temperature of AP, showing obvious catalytic activity. In particular, NiO sub-microsphere have the best catalytic role, which can reduce the high temperature decomposition (HTD) and low temperature decomposition (LTD) temperature by 75.2 and 19.1 °C, respectively. The synthetic approach can easily control the morphology and pore structure of the NiO nanostructures by adjusting the ratio of Ni2+/HMT in the reactants and subsequent calcination, which avoids using expensive templates or surfactant and could be intended to prepare other transition metal oxide.
HMT-Controlled Synthesis of Mesoporous NiO Hierarchical Nanostructures and Their Catalytic Role towards the Thermal Decomposition of Ammonium Perchlorate