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In this work two approaches to the synthesis of energetic complex compound Ni(Im)6(NO3)2 from imidazole and nicklel (II) nitrate were applied: a traditional synthesis from solution and a solvent-free melting-assisted method. According to infrared spectroscopy, X-ray diffraction, elemental and thermal analysis data, it was shown that the solvent-free melt synthesis is a faster, simpler and environmentally friendly method of Ni(Im)6(NO3)2 preparation. The results show that this compound is a promising precursor for the production of nanocrystalline Ni-NiO materials by air-assisted combustion method. The combustion of this complex together with inorganic supports makes it possible to synthesize supported nickel catalysts for different catalytic processes.

The development of solvent-free techniques for nanoparticles synthesis is one of the challenges of Green chemistry. In this work, the principled opportunity to obtain copper-containing nanosized particles without use of any solvents was shown. The copper complexes were prepared as precursors by the melting-assisted solvent-free synthesis. The formation of tetra(imidazole)copper(II) nitrate complex was confirmed by XRD, elemental analysis, FTIR spectroscopy, and thermal analysis. It was noted that their thermal decomposition occurs in two stages: (I) the low-temperature step may be related to redox interaction between organic ligands and nitrate-anions; (II) the high-temperature step may be related to the oxidation of the products of incomplete imidazole decomposition. TEM and XRD studies of solid products of complex combustion have shown that they are oxides with particle size less than 40 nm. Thus, the combustion of [Cu(Im)4](NO3)2 complex under air can be considered as a new approach to prepare nanosized particles of copper oxides without the use of solvents.

A solvent-free method was proposed for the synthesis of hexaimidazolecobalt(II) nitrate and perchlorate complexes—[Co(C3H4N2)6](NO3)2 and [Co(C3H4N2)6](ClO4)2—by adding cobalt salts to melted imidazole. The composition, charge state of the metal, and the structure of the resulting complexes were confirmed by elemental analysis, XPS, IR spectroscopy, and XRD. The study of the thermochemical properties of the synthesized complexes showed that [Co(C3H4N2)6](NO3)2 and [Co(C3H4N2)6](ClO4)2 are thermally stable up to 150 and 170 °C, respectively. When the critical temperature of thermal decomposition is reached, oxidative two-stage gasification is observed. In this case, the organic component of the [Co(C3H4N2)6](NO3)2 complex undergoes almost complete gasification to form Co3O4 with a slight admixture of CoO, which makes it attractive as a component of gas-generation compositions, like airbags.