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In the present work, a series of two-component Ni-Mg-O oxide systems were prepared using a sol–gel technique at varied pH of hydrolysis procedure. The aqueous solutions of nitric acid or ammonia were added to control the pH values. The xerogel samples obtained after drying were analysed using a thermogravimetric approach. The oxide systems were characterized by a set of physicochemical methods (low-temperature nitrogen adsorption, X-ray diffraction analysis, scanning electron microscopy, UV-vis spectroscopy, and temperature-programmed reduction method). The thermal stability of the samples was examined in a testing reaction of CO oxidation in a prompt thermal aging regime. It was revealed that the pH value during the magnesium methoxide hydrolysis stage significantly affects the properties of the intermediate hydroxide and final oxide nanomaterials. The thermal decomposition of nitric acid or ammonia is accompanied by exothermal effects, which noticeably influence the textural characteristics. Moreover, the pH of the hydrolysing solution defines the strength of the nickel interaction with the MgO matrix. An increase in pH facilitates the formation of the NixMg1−xO solid solution with a higher amount of incorporated nickel, which is characterized by the reproducible broad temperature range of the hydrogen uptake and the enhanced thermal stability.

Preparation of the Nanostructured Ni-Mg-O Oxide System by a Sol–Gel Technique at Varied pH