A solvent-free method was proposed for the synthesis of hexaimidazolecobalt(II) nitrate and perchlorate complexes-[Co(CHN)](NO) and [Co(CHN)](ClO)-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(CHN)](NO) and [Co(CHN)](ClO) are thermally stable up to 150 and 170 °C, respectively.
View Article and Find Full Text PDFCO methanation was studied in the presence of nickel catalysts obtained by the solid-state combustion method. Complexes with a varying number of ethylenediamine molecules in the coordination sphere of nickel were chosen as the precursors of the active component of the catalysts. Their synthesis was carried out without the use of solvents, which made it possible to avoid the stages of their separation from the solution and the utilization of waste liquids.
View Article and Find Full Text PDFThis work describes the mathematical modeling of the thermal decomposition of the complex compound [Ni(En)](ClO) (En = CHN = ethylenediamine) in an inert atmosphere under non-isothermal conditions. This process is characterized by several simultaneous and intense stages: elimination of ethylenediamine from the nickel coordination sphere, decomposition of perchlorate anions, and explosive-like oxidation of free or bound ethylenediamine. These stages overlap and merge into a one step on the differential thermogravimetric curve.
View Article and Find Full Text PDFIn this work two approaches to the synthesis of energetic complex compound Ni(Im)(NO) 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)(NO) preparation. The results show that this compound is a promising precursor for the production of nanocrystalline Ni-NiO materials by air-assisted combustion method.
View Article and Find Full Text PDFThe paper presents a comparative study of the activity of magnetite (FeO) and copper and cobalt ferrites with the structure of a cubic spinel synthesized by combustion of glycine-nitrate precursors in the reactions of ammonia borane (NHBH) hydrolysis and hydrothermolysis. It was shown that the use of copper ferrite in the studied reactions of NHBH dehydrogenation has the advantages of a high catalytic activity and the absence of an induction period in the H generation curve due to the activating action of copper on the reduction of iron. Two methods have been proposed to improve catalytic activity of FeO-based systems: (1) replacement of a portion of Fe cations in the spinel by active cations including Cu and (2) preparation of highly dispersed multiphase oxide systems, involving oxide of copper.
View Article and Find Full Text PDFThe Mn-Ce oxide catalysts active in the oxidation of CO were studied by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), temperature-programmed reduction (TPR), transition electron microscopy (TEM), energy dispersive X-Ray (EDX), and a differential dissolution technique. The Mn-Ce catalysts were prepared by thermal decomposition of oxalates by varying the Mn:Ce ratio. The nanocrystalline oxides with a fluorite structure and particle sizes of 4-6 nm were formed.
View Article and Find Full Text PDFToday, Fs defects in MgO as isolated surface neutral oxygen vacancies are in the focus of surface science, catalysis research, and emission coating of microchannel plates. With the 10 atom % content at 750 K and under = 10 Torr, estimated by us from the known equilibrium - and -- diagrams of MgO, Fs defects remain invisible or difficult-to-detect objects. The MgO(100) → MgO(100) + Fs + /O phase transition was studied in MgO films deposited by the metal-organic chemical vapor deposition (MOCVD) procedure from the mixed-ligand Mg precursor on Si substrates at 725 K in the O flow where the nonstoichiometric phase (MgO/Fs) is formed in the gas medium containing simultaneous H, CO, HO, CO, and O species in unbalanced concentrations.
View Article and Find Full Text PDF