The MAX phases exhibit outstanding combination of strength and ductility which are unique features of both metals and ceramics. The preparation of pure MAX phases has been challenging due to the thermodynamic auspiciousness of intermetallic formation in the ternary systems. This review demonstrates the power of the self-propagating, high-temperature synthesis method, delivers the main findings of the combustion synthesis optimization of the MAX phases, and reveals the influence of the combustion wave on the microstructure features thereof. The possibility of using elements and binary compounds as precursors, oxidizers, and diluents to control the exothermicity was comparatively analyzed from the point of view of the final composition and microstructure in the following systems: Ti-Al-C, Ti-V-Al-C, Cr-V-Al-C, Ti-Cr-Al-C, Ti-Nb-Al-C, Ti-Al-Si-C, Ti-Al-Sn-C, Ti-Al-N, Ti-Al-C-N, Ti-Al-B, Ti-Si-B, Ti-Si-C, Nb-Al-C, Cr-Al-C, Cr-Mn-Al-C, V-Al-C, Cr-V-Al-C, Ta-Al-C, Zr-S-C, Cr-Ga-C, Zr-Al-C, and Mo-Al-C, respectively. The influence of sample preparation (including the processes of preheating, mechanical activation, and microwave heating, sample geometry, porosity, and cold pressing) accompanied with the heating and cooling rates and the ambient gas pressure on the combustion parameters was deduced. The combustion preparation of the MAX phases was then summarized in chronological order. Further improvements of the synthesis conditions, along with recommendations for the products quality and microstructure control were given. The comparison of the mechanical properties of the MAX phases prepared by different approaches was illustrated wherever relevant.

This work reports on the spark plasma sintering (SPS) of self-propagating high-temperature-synthesis (SHS)-derived Ni-W and Ni-W-2wt%hBN (4:1 molar ratio of metals) powders. The synthesis was carried out from a mixture of NiO and WO₃ using Mg + C combined reducers through a thermo-kinetic coupling approach. Experiments performed in the thermodynamically optimal area demonstrated the high sensitivity of combustion parameters and product phase composition to the amount of reducers and hBN powder. The powder precursors with and without the addition of hBN were consolidated using SPS at a temperature and pressure of 1300 °C and 50 MPa, respectively, followed by a thorough phase and microstructural characterization of the obtained specimens. SHS-derived powders comprised the nano-sized agglomerates and were characterized by a high sinterability. The specimens of >95% density were subjected to ball-on-plate dry sliding wear tests at a sliding speed of 0.1 ms⁻¹ and a distance of 1000 m utilizing an alumina ball of 10 mm in diameter under a 15 N normal load. The tests were performed at a temperature of 800 °C. A significant improvement in wear behavior was demonstrated for SHS-processed composites in comparison with their counterparts produced via conventional high-energy ball milling technique owing to the phenomena of ‘micro-polishing’, cyclic ‘self-healing’ and fatigue. However, the decisive effect of hBN addition in imparting lubrication during an HT wear test was not confirmed.

A novel pathway for the magnesiothermic reduction of boron oxide and magnesium dodecaboride (MgB₁₂) in the presence of carbon by a self-propagating high-temperature synthesis method was proposed that was aimed at the direct preparation of boron carbide nanopowder. The combined utilization of two boron sources, boron oxide and MgB₁₂, allowed tailoring the overall caloric effect of the process, increasing the yield of the target product and lessening the laborious leaching process. In addition, it is an alternative way to utilize magnesium borides, which are inevitable side products at boron production. Multivariate thermodynamic calculations performed in the B₂O₃-MgB₁₂-Mg-C system allowed estimating equilibrium compositions of the products and deducing the optimum composition of the initial mixture for obtaining B₄C. For the latter, the adiabatic temperature (T_ad) is 2100 °C, which is theoretically enough for the implementation of the self-propagating reaction. The combustion reaction was shown to be extremely sensitive to the initial mixture composition, external pressure, as well as sample diameter (heat losses). It proceeds in self-oscillatory mode and leads to the product of a layered macrostructure. The combustion product was then consolidated by the spark plasma sintering technique at different conditions. Vickers microhardness was measured, and the wear erosion behavior was examined. The variation in lattice parameters of boron carbide reflected the influence of synthesis, sintering and erosion conditions on the ordering/disordering of the boron carbide structure.

Understanding of the decisive role of non-isothermal treatment on the interaction mechanism and kinetics of the MoO₃-CuO-Mg-C system is highly relevant for the elaboration of optimal conditions at obtaining Mo-Cu composite powder in the combustion processes. The reduction pathway of copper and molybdenum oxides with combined Mg + C reducing agents at high heating rates from 100 to 5200 K min⁻¹ was delivered. In particular the sequence of the reactions in all the studied binary, ternary and quaternary systems contemporaneously demonstrating the effect of the heating rate on products’ phase composition and microstructure was elucidated. The combination of two highly exothermic and speedy reactions (MoO₃ + 3Mg and CuO + Mg vs. MoO₃ + CuO + 4Mg) led to a slow interaction with weak self-heating (dysynergistic effect) due to a change in the reaction mechanism. Furthermore, it has been shown that upon the simultaneous utilization of the Mg and C reducing agents, the process initiates exclusively with carbothermic reduction, and at relatively high temperatures it continues with magnesiothermic reaction. The effective activation energy values of the magnesiothermic stages of the studied reactions were determined by Kissinger isoconversional method.