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The mechanism and kinetics of nickel oxide reduction by Mg + C combined reducer at non-isothermal conditions in a wide range of high heating rates (100–1200 °C min−1) were studied by high-speed temperature scanner technique. It was shown that both the magnesiothermal and magnesiocarbothermal reduction processes, unlike low heating rates (5–20 °C min−1, DTA/DTG method), start beyond the melting point of magnesium and proceed via solid + liquid scheme. It was found out that the utilization of Mg + C combined reducer allows to significantly lower the reduction temperature (by about 200–400 °C) of nickel oxide as compared with exclusively magnesium or carbon reducers evidencing on the synergetic effect of combined reducers in the ternary mixture. The effective values of activation energy (Ea) for the NiO + Mg and 2NiO + Mg + C reactions were determined to be 185 ± 15 kJ mol−1 and 195 ± 15 kJ mol−1, respectively.

Functional features of Ni-W composite materials combined with successful performance enabled a breakthrough in their broad application. To disclose the formation pathway of Ni-W composite materials at extreme conditions of combustion synthesis in the NiO-WO3-Mg-C and NiWO4-Mg-C systems for the optimization of the synthesis procedure, the process was modeled under programmed linear heating conditions by thermal analysis methods. The reduction kinetics of tungsten and nickel oxides mixture and nickel tungstate by Mg + C combined reducer at non-isothermal conditions was studied at high heating rates (100–1200 °C min−1) by high-speed temperature scanner techniques. It was shown that when moving from low heating to high heating rates, the mechanism of both the magnesiothermic and magnesio-carbothermic reductions of the initial mixtures changes; that is, the transition from a solid-solid scheme to a solid-liquid scheme is observed. The strong influence of the heating rate on the reduction degree and kinetic parameters of the systems under study was affirmed. The simultaneous utilization of magnesium and carbon as reducers allowed the lowering of the starting and maximum temperatures of reduction processes, as evidenced by the synergetic effect at the utilization of a combined reducer. The effective values of activation energy (Ea) for the reactions proceeding in the mixtures NiO + WO3 + 4Mg, NiO + WO3 + 2.5Mg + 1.5C, NiWO4 + 4Mg and NiWO4 + 2Mg + 2C were estimated by Kissinger isoconversional method and were 146 ± 10, 141 ± 10, 216 ± 15 and 148 ± 15 kJ mol−1, respectively.

Manufacturing W-Cu composite nanopowders was performed via joint reduction of CuO and WO3 oxides with various ratios (W:Cu = 2:1, 1:1, 1:3, 1:13.5) using combined Mg–C reducer. Combustion synthesis was used to synthesize homogeneous composite powders of W-Cu and hot explosive consolidation (HEC) technique was utilized to fabricate dense compacts from ultrafine structured W-Cu powders. Compact samples obtained from nanometer sized SHS powders demonstrated weak relation between the susceptibility and the applied magnetic field in comparison with the W and Cu containing micrometer grain size of metals. The density, microstructural uniformity and mechanical properties of SHS&HEC prepared samples were also evaluated. Internal friction (Q-1) and Young modulus (E) of fabricated composites studied for all samples indicated that the temperature 1000 °С is optimal for full annealing of microscopic defects of structure and internal stresses. Improved characteristics for Young modulus and internal friction were obtained for the W:Cu = 1:13.5 composite. According to microhardness measurement results, W-Cu nanopowders obtained by SHS method and compacted by HEC technology were characterized by enhanced (up to 85%) microhardness.

The exothermic reactions in the ZrF4−Mg-Si and ZrF4-Al-Si systems are investigated by a fast temperature recording (thermocouple) technique, differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). A quenching method is used to arrest the combustion process and conduct a layer-by-layer analysis of the products by x-ray diffraction (XRD) and electron microscopy. Two seemingly similar reactive systems exhibited considerably different combustion characteristics, composition, and morphology. Based on these investigations, we propose and discuss phase formation mechanisms at the early stages for each system. Three different pathways involving the reaction of ZrF4 with other reagents and the Mg2Si intermediate are identified to occur in the ZrF4−Mg-Si system. Contrary to the complex mechanism in the ZrF4−Mg-Si system, the early stage of the combustion process for the ZrF4-Al-Si system involves the interaction of ZrF4 with Al-Si eutectic melt. The exothermic reaction between reduced solid Zr and Si melt is the primary heat-generating step for both systems in spite of substantial differences in the early stages of the reactions. The silicon content in the reactive mixtures governs the phase composition of products. The ZrSi2 phase, with a high growth rate, forms first on the Zr particle surfaces and then grows by a reactive diffusion mechanism. The ZrSi2+Zr reaction produces silicon-lean phases (e.g., ZrSi) when the silicon supply is limited. The combustion temperature also has a considerable influence on the phase compositions of the products. High combustion temperature in the ZrF4+2Mg+Si mixture enables the formation of multiphase products (α-ZrSi and β-ZrSi), whereas the relatively lower temperatures in the 3ZrF4+4Al+3Si mixture yields a single-phase α-ZrSi. Lower combustion temperatures also make the ZrF4-Al-Si system more advantageous for the preparation of zirconium silicides.

In the work, the preparation of fine-grained silicon was performed in combustion mode by magnesiothermic reduction of silica, obtained from serpentine mineral, which is characterized by a high specific surface area (about 560 m2/g) and high reaction activity. It is manifested by the fact that the measured combustion temperature exceeded the adiabatic combustion temperature calculated with the ISMAN THERMO software, by about 200 °C. In order to mitigate the synthesis conditions, combustion products (Si+2MgO) were used as diluting agents allowing a significant decrease of combustion temperature and a finer silicon powder without contaminating the target product with incidental reagents and without decreasing the yield of the target product. Based on the measured values of combustion parameters (combustion temperature and combustion wave propagation velocity) vs diluent amount, it was estimated that the effective activation energy for SiO2+2Mg reaction by the solid+liquid mechanism in the temperature interval 1400–2100 °C was about 65±3 kJ/mol.

W-Cu composite materials with various molar ratio of constituent metals (W:Cu = 2:1 and 1:3) were synthesized via co-reduction of WO 3 and CuO oxides precursors with Mg + C combined reducer in the combustion mode by applying reaction's thermo-kinetic coupling approach. The interaction mechanism and phase and microstructure formation laws in the 2WO 3 -CuO-yMg-xC and WO 3 -3CuO-yMg-xC quaternary systems were explored. According to experimental results obtained by stopped combustion front technique in bulk copper wedge, it was shown that firstly the copper oxide carbothermal reduction into copper and then magnesio-carbothermal reduction of the tungsten oxide into tungsten take place. It was revealed that the growth of C/Mg ratio leads to decrease both the combustion temperature and velocity conditioned by growth in the portion of low-caloric reaction and allows to control interaction conditions for the preparation of nanosized 2 W-Cu and W-3Cu composite powders. Combustion products obtained at optimum conditions represent as W-Cu nanocomposite powder with 30–50 nm in size.

Kinetic studies were performed utilizing high-speed temperature scanner in the Ni-Al system including those with and without mechanical activation (MA) of different duration in a planetary ball mill, with and without using carbon nanoadditives (NA). The temperature profiles were taken and treated at different heating rates from 100 up to 2600 °C/min considering the influence of activation duration and the role of nanoadditive on the characteristic points of thermograms. Kissinger method allowed to evaluate activation energy (Ea) for non-activated, activated (1, 2, 3, 5 min), nanoadditive (1 wt.%) containing and nanoadditive (1 wt.%) containing mechanoactivated (1, 3, 5 min) mixtures. The beneficial influence of NA on the interaction between Ni and Al in the non-activated and moderately mechanoactivated mixtures was demonstrated. The influence of MA and NA on the microstructure features and phase formation sequence at various heating rates were revealed. For all the mixtures under study, T* characteristic temperatures (the temperature, where the maximum exothermic effect was observed) were found to increase with increasing heating rates. It was unravelled that mechanical treatment leads to significant changes in the reaction kinetics and phase formation laws. Particularly, in an activated mixture, the formation of Ni3Al is followed by NiAl intermetallic, in contrast to non-activated mixture, where the reaction proceeds only with the NiAl formation. The both MA in 1 min and addition of 1 wt.% NA decreased the activation energy of the Ni-Al reaction, exhibiting commensurate impact on the effective activation energy value of the Ni-Al system. However, > 3 min MA in the presence of 1 wt.% NA have prohibitive effect on the reaction in the Ni-Al system.