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The present work aimed to prepare Ni-Mo particles distributed within the MgO matrix. With this purpose in mind, a ternary Ni-Mo-Mg oxide system was synthesized by a sol−gel approach. The samples were studied by low-temperature nitrogen adsorption, X-ray diffraction analysis, and transmission electron microscopy equipped with energy dispersive X-ray analysis. Both the nickel and molybdenum species in the prepared samples were characterized by a fine and uniform distribution. The diffraction pattern of the ternary system was predominantly represented by the MgO reflections. The catalytic activity of the samples was tested in the decomposition of 1,2-dichloroethane used as a representative of the chlorinated organic wastes. The nanostructured carbon filaments resulting from the decomposition of the halogenated substrate were found to be characterized by a narrow diameter distribution, according to the transmission electron microscopy data, thus confirming the fine distribution of the active Ni-Mo particles. The results obviously show the advantages of the sol−gel technique for obtaining efficient catalysts.

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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.

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Two different approaches to modify the structure and reaction ability of nanocrystalline MgO have been discussed. In the first case, a series of two-component x%MOx–MgO systems (M = Fe, Co and Ni, x = 1–45 wt.%) was synthesized via sol–gel technique. Aqueous solution of inorganic salt precursor was used as a hydrolyzing agent. Samples obtained were characterized by number of physicochemical methods (differential thermal analysis, X-ray diffraction analysis, low-temperature adsorption, etc.). It was shown that presence of inorganic salt in magnesium hydroxide matrix shifts the temperature of decomposition of latter towards lower values. Structural and textural characteristics of MgO-based oxide systems were found to be strongly affected by the presence of additive and their concentration. Formation of joint phase was observed in the case of cobalt oxide only. Second way of MgO modification was represented by creating a controlled carbon coating over its surface via decomposition of C4H10 at 400 °C. The obtained x%C/MgO (x = 1–10 wt.%) samples were shown to possess the improved reaction ability in destruction sorption of CF2Cl2 as well as in catalytic dehydrochlorination of 1-chlorobutane in presence of water vapors.