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In this study, we present two distinct solid-flame combustion synthesis (SF-CS) methods for the fabrication of two-dimensional (2D) nanosheets of carbon and nanocrystals of molybdenum carbide (Mo2C). To synthesize 2D carbon nanosheets, poly-(vinyl chloride) polymer powder is combusted in conjunction with magnesium (Mg). In contrast, Mo2C is generated through the combustion–reduction of MoO3 using an excess of Mg. It is observed that the crystallization of Mo2C within liquid Mg yields well-defined nanocrystals with {101} facets. Combining these nanocrystals with 2D carbon nanosheets results in hydrogen evolution reaction (HER) catalysts with a significantly improved performance. A comprehensive comprehension of the underlying mechanisms responsible for the heightened HER performance is elucidated, particularly with regard to the synergistic effects arising from the combination of Mo2C and graphene-like 2D carbon nanosheets. Furthermore, a density functional theory (DFT) analysis of Mo2C/interface energies indicates that the presence of a few layers of graphene on the Mo2C facet surface can enhance the catalytic properties. This is attributed to the fact that carbon layers do not form bonds with hydrogen atoms, which gradually reduces the adsorption energies of hydrogen and facilitates the formation of H2 molecules. [ABSTRACT FROM AUTHOR]

Efficient hydrogen production relies on cost-effective and durable non-noble metal electrocatalysts for the hydrogen evolution reaction (HER). In this work, a liquid metal-assisted solid-flame combustion synthesis (SF-CS) method was used to create transition metal carbide TMC) nanocrystals with exposed facets. The TMCs include TiC, VC, NbC, TaC, Ta 2 C, WC, and Mo 2 C. In acidic solutions, the TMC nanocrystals show enhanced conductivity and superior HER performance, as evidenced by their lower Tafel slope, higher current density, and decreased overpotential. In particular, Mo 2 C nanocrystals exhibit an overpotential of 95 mV and a Tafel slope of 26 mV dec−1. These findings highlight a noteworthy improvement over previously reported nanostructures in recent years in terms of the HER properties of Mo 2 C with particular facets. This improvement is attributed to the unique surface characteristics, such as energy and active sites, which are impacted by various factors and require more investigation to meet the intended goals. [Display omitted] [ABSTRACT FROM AUTHOR]

In this study, tantalum network nanoparticles are prepared from a Ta 2 O 5 + k Mg system via a liquid magnesium-controlled combustion reaction. Super-stoichiometric amounts of magnesium are used in the preparation of a reaction mixture to produce a liquid magnesium pool capable of lowering the combustion temperature and leading to the formation of Ta network structures. The heat transfer kinetics from the hot reaction zone of 'cold' Mg particles is determined using heat transfer-coupled fluid dynamics simulation software. The formation of network structures is characterized through SEM, TEM, XRD, and BET analysis techniques. The mechanism of network formation is explained based on solid particle collisions in liquid media. Our method is able to produce Ta network structures in which the size of individual particles ranges between 50 and 700 nm. [ABSTRACT FROM AUTHOR]

Abstract The adiabatic temperatures and equilibrium phases in the FeTiO 3 - α Mg-C(B, Si)- k NaCl system (where α = 0.2–15, k = 0–3) were analyzed to predict the formation of fine powders of titanium compounds from natural ilmenite sand. From the parametric study, the critical variables were identified and optimized for the synthesis of FeTi, TiC, TiB 2 , and TiFeSi 2 under a combustion regime. The experimentally measured temperatures were in good agreement with those predicted from thermochemical calculations in the 900–1800 °C range. The purified products were characterized using X-ray diffraction, transmission electron microscopy, and Raman spectroscopy. The fine powders of titanium compounds were mainly single phase with a purity of at least 95 wt%. Considering the various stages of the synthetic process, a mechanism is proposed to explain how the process of ilmenite recovery occurred. Graphical abstract Image Highlights • Natural ilmenite was used as a precursor for synthesizing Ti compounds. • Combustion temperatures and phases were determined in FeTiO 3 -αMg-C(B, Si)- k NaCl system. • The effect of Mg and NaCl concentration on the combustion temperature was revealed. • The ilmenite was converted into FeTi, TiC, TiB 2, and FeTiSi 2 fine powders. • A reduction pathway in the synthesis of Ti compounds was proposed. [ABSTRACT FROM AUTHOR]

Abstract This paper reports the preparation of Ti microparticles that are angular and spherical in shape through the combustion of a TiO 2 + αCa (where α is moles of Ca) exothermic mixture in an inert atmosphere. The relationship between the combustion parameters and the properties of the resultant Ti particles is discussed with consideration of the effect of Ca concentration. Using excess amounts of Ca in the experiment was effective in modifying the shape of the particles from angular to spherical. The Ti powder was found to be well-dispersed and the diameter of individual particles ranged from 5 µm to 50 µm. Based on the combustion parameters, the activation energy for the redox reaction was calculated as ∼ 138 kJ/mol. This paper discusses the chemistry of the reduction process and highlights the effects of combustion temperature and the amount of liquid calcium on the characteristics of the Ti particles. Graphical abstract The combustion process in TiO 2 + Ca mixture developed a maximum temperature of about 1820 °C and resulted in Ti spherical particles. fx1 [ABSTRACT FROM AUTHOR]

Abstract We developed an attractive combustion approach for synthesizing uniformly shaped AlN dendritic crystals by combustion of Al + 0.1AlF 3 + k Al 2 O 3 powder mixtures in a nitrogen atmosphere. The combustion temperature measured for various k values was between 1650 and 1750 °C and the micro-droplets of Al formed in the beginning stages of the process were enveloped by the solid layers of Al 2 O 3 , and the subsequent multipoint nucleation and crystallization produced morphologically and size uniform dendritic crystals. We proposed a theoretical model for calculating the thickness and the number of Al 2 O 3 layers around of Al microdroplets at known concentration of Al 2 O 3. Depending on the concentration of Al 2 O 3 , these structures were simple stars with six points and stellar dendrites with multiple petals. [ABSTRACT FROM AUTHOR]

In this study, a single-step combustion process for the synthesis 1-D, 2-D, and 3-D micro and nanostructures of AlN was developed. The structures were grown by combustion of Al+ k AlF 3 (or ZnF 2 )+ m NH 4 Cl reaction mixture under 4.0 MPa nitrogen atmosphere. Based on experimental data, the growth conditions, morphology, and composition, optical, and thermal properties of AlN micro and nanostructures were determined. The formation of structures was associated with the combustion temperature, liquid and gas-phase reactions, and the type of additives used in the experiments. The new insight, we gleaned from this study may help in the selective growth of AlN micro and nanostructures of different morphology, enhancing their functionality. [ABSTRACT FROM AUTHOR]

In this study, we examined the effect of potassium perchlorate (KClO 4 ) and magnesium hydroxide (Mg(OH) 2 ) additives on the combustion behavior of a ZrO 2  + 2Mg mixture to produce a fine powder of zirconium metal. The results of thermodynamic analysis and experiments imply that nearly 0.04 mol of KClO 4 is needed to initiate a combustion reaction in the ZrO 2  + 2Mg system. As the amount of KClO 4 increases from 0.04 to 0.1 mol, the combustion temperature increases from 1250 to 1850 °C. This results in formation of fine zirconium powder with a typical particle size of less than 5 µm, and with 1.4–2.2 wt% residual oxygen. Subsequent reduction of particle size to 100–500 nm, and oxygen content to <1.0 wt% was achieved by adding Mg(OH) 2 . The as-prepared Zr powder was mixed with nitrocellulose and printed onto 10–100 µm thin-layers to study their burning stability. The wave propagation in a thin layer was on the order of 0.35–30 cm/s, which is suitable for applications requiring localized power generation. [ABSTRACT FROM AUTHOR]

The exothermic reduction of oxides mixture (MoO 3 +2SiO 2 ) by magnesium in NaF melt enables the synthesis of nanocrystalline MoSi 2 powders in near-quantitative yields. The combustion wave with temperature of about 1000–1200 °C was recorded in highly diluted by NaF starting mixtures. The by-products of combustion reaction (NaF and MgO) were subsequently removed by leaching with acid and washing with water. The as-prepared MoSi 2 nanopowder composed of spherical and dendritic shape particles was consolidated using the spark plasma sintering method at 1200–1500 °C and 50 MPa for 10 min. The result was dense compacts (98.6% theoretical density) possessing submicron grains and exhibiting hardness of 8.74–12.92 GPa. [ABSTRACT FROM AUTHOR]

In this study, a combustion process for a TiO 2 + 0.12Al + (2.5 + 6 k )Mg + 0.021V 2 O 5 + k MgCl 2 ·6H 2 O mixture was studied to fabricate Ti-6Al-4V alloy spherical particles. From the temperature-time profiles, the average value of the synthesis temperature was estimated to be 1650 ± 20 °C. Based on FESEM observations, spherical shape particles were obtained when 0.05–0.1 mol MgCl 2 ·6H 2 O was added to the initial reaction mixture. Therefore, spherical alloy particles were achieved by consecutive processes of cooling and acid purification of the burned down sample. According to laser particle size analysis, the average diameter of the spheres was between 5 and 25 μm. A selective laser melting process was applied to build dense Ti-6Al-4V alloy samples. The tensile properties and the microhardness were evaluated and compared to those characteristics of a reference sample prepared from commercial Ti-6Al-4V alloy spherical powder. [ABSTRACT FROM AUTHOR]

This study deals with combustion behavior of B 2 O 3 /Mg/NH 4 Cl/C complex systems for the synthesis of amorphous boron (B), boron carbide (B 4 C), and boron nitride (BN) nanostructures. The raw mixtures used in the experiments were prepared on the base of a B 2 O 3 –Mg precursor mixture, which is sufficiently exothermic to maintain a self-propagating regime of the combustion reaction. Thermodynamic analysis of the combustion temperatures and experimental validation indicate that the 1000–1500 °C temperature range is very effective for synthesizing the nanostructures of B, B 4 C, and BN. It was found that B-containing functional nanostructures are mainly spherical nanoparticles (B) or nanosheets (B 4 C, BN). The phase composition and microstructural characteristics of the final products were evaluated based on the combustion temperature and solid/liquid phase changes. [ABSTRACT FROM AUTHOR]

A melt-assisted solid flame synthesis approach was applied to synthesize boron nanoparticles in argon gas and air atmospheres. For this purpose, we investigated the characteristics of a thermally induced combustion wave in B 2 O 3 + α Mg mixtures ( α = 1.0–1.5 mol) in argon and air atmospheres. Utilizing stoichiometrically insufficient amounts of magnesium ensured that a large portion of molten B 2 O 3 remained in the sample, which reduced the combustion parameters and favored the formation of boron nanoparticles. Under these conditions the combustion temperature and burning velocity were controlled in the range of 1300–1580 °C and 0.065–0.18 cm/s, respectively, and boron nanoparticles in a ∼20–200 nm size range were obtained. The characteristics of boron nanoparticles (morphology, purity, specific surface area, oxidation activity, etc.) were analyzed and a reaction pathway leading to boron nanoparticles synthesis was proposed. [ABSTRACT FROM AUTHOR]

We have investigated a thermally induced combustion route for preparing 2D hexagonal BN nanoplates from B 2 O 3 +(3+0.5 k )Mg+ k NH 4 Cl solid system, for k =1–4 interval. Temperature–time profiles recorded by thermocouples indicated the existence of two sequential exothermic processes in the combustion wave leading to the BN nanoplates formation. The resulting BN nanoplates were characterized by X-ray diffraction (XRD), field-emission scanning electron microscopy, PL spectrometry, and Brunauer–Emmett–Teller surface area analysis. It was found that B 2 O 3 was converted into BN completely (by XRD) at 1450–1930 °C within tens of seconds in a single-step synthesis process. The BN prepared at a k =1–4 interval comprised well-shaped nanoplates with an average edge length ranging from 50 nm to several micrometer and thickness from 5 to 100 nm. The specific surface area of BN nanoplates was 13.7 g/m 2 for k =2 and 28.4 m 2 /g for k =4. [ABSTRACT FROM AUTHOR]

The synthesis of AlN nanoparticles in non-isothermal high-temperature conditions was developed. The process involved Al 2 O 3 –Mg–NH 4 Cl mixtures preparation and combustion in nitrogen atmosphere. Temperature profiles in the combustion waves were recorded by thermocouples, and the values of combustion temperature and wave velocity were determined from the recorded profiles. The existence of two independed combustion regimes with maximum temperatures of about 850 °C and 1400–1600 °C were revealed based on concentrations of NH 4 Cl. AlN nanocrystals were obtained and investigated by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, and Brunauer–Emmett–Teller surface area. AlN nanocrystals prepared under non-isothermal combustion process were comprised well distributed multi-faceted particles with an average size of 50–200 nm. The chemical reactions in the combustion wave were discussed and a possible thermochemical pathway for the synthesis of AlN nanoparticles was proposed. [ABSTRACT FROM AUTHOR]

Tantalum nitride nanoparticles were produced from a (K2TaF7 +5NaN3) exothermic mixture under the combustion regime. The effects of the K2TaF7/NaN3 ratio and KF and NH4F concentrations on the combustion parameters, product composition, and size of the tantalum nitride particles were studied. Depending on the synthesis conditions, the combustion temperature was maintained in the 700–1200°C range, resulting in hexagonal ε-TaN, TaN0.8, and Ta2N phases. The dominant phases were TaN and TaN0.8 in the 1000–1200°C range, whereas only the Ta2N phase was present in the 700–100°C range. Pure-phase cubic tantalum nitride (δ-TaN) was produced with 4.0mol of NH4F at a combustion temperature of ~800°C. Under controlled reaction conditions, the size of the tantalum nitride particles was about 10–50nm. We also found that during the synthesis, the stainless steel tube located inside of the reaction mixture was partially coated with fine TaN crystals. The mechanism of the combustion process is discussed in regards to the experimental results. [ABSTRACT FROM AUTHOR]

Abstract: In this paper, we describe an attractive and rapid process for preparing zirconium metal (sponge and powder) by reacting zirconium tetrachloride with magnesium powder. The process was carried out in the combustion synthesis (shortly CS) mode using a ZrCl4–2Mg exothermic mixture, which provided a temperature of 1000–1100°C and a final product consisting of MgCl2 and Zr sponge. The separation of Zr sponge from the reaction product was accomplished by dissolving MgCl2 into warm acidified water. The average size of the Zr sponge particles ranged from about 1mm to about 10mm. Micrometer-sized (from 10 to 300μm) Zr powders were also obtained after mechanical processing of sponge. The characteristics of the Zr metal were established by X-ray diffraction, scanning electron microscopy, and inductively coupled plasma spectroscopy techniques. [Copyright &y& Elsevier]

Abstract: Quasi-aligned, high-aspect-ratio AlN micro- and nanostructures were synthesized under high nitrogen pressure by the exothermic reaction of an Al+0.015mol (C2F4) n mixture. Structurally uniform AlN micro- and nanofibers with hexagonal and cylindrical morphologies were obtained when the system temperature was maintained within the range of 1600–1700°C. The fibers had aspect ratios as high as 2000, diameters in the range of ∼0.05–20μm, and were ∼100–1000μm in length. High-resolution transmission electron microscopic and selected area diffraction analyses indicated that the as-synthesized AlN micro- and nanostructures are perfectly single crystalline with preferential growth along the [001] direction. Branching was also observed in some of the micro-fibers, giving rise to randomized, two-dimensional comb textures. Based on the results obtained in the present study, a mechanism for the formation of AlN micro- and nanostructures under combustion conditions was proposed. [Copyright &y& Elsevier]

Abstract: An experimental study on the preparation of zirconium silicides was conducted using ZrSiO4–Mg, ZrSiO4–SiO2–Mg and ZrSiO4–ZrO2–Mg powder mixtures by the combustion synthesis (CS) technique. Test specimens having different composition ratios including Zr:Si=1:2, 1:1, 5:4, 5:3, 2:1, and 3:1 were employed in this study. Temperature profiles relative to all the starting compositions were measured using thermocouples, and the values of the combustion parameters (combustion temperature and wave velocity) were estimated using the same. The formation of ZrSi, ZrSi2, Zr5Si3, and Zr3Si2 phases was confirmed by X-ray analysis; however, only ZrSi was produced as a single-phase product. The proposed method was also extended to synthesize spherical ZrSi particles having mean diameters of 0.2–3.0μm. A comprehensive chemical pathway to describe the sequence of chemical reactions in the combustion wave was also proposed. [ABSTRACT FROM AUTHOR]

The present study demonstrates the synthesis of fine hafnium (Hf) metal powders via a chemically activated combustion synthesis (CS) approach, which develops temperatures in the range of 1000–1600 °C. The current CS approach can be employed to obtain Hf powders with a single-crystalline hexagonal close-packed (hcp) structure in addition to high compositional uniformity and average particle sizes ranging from 0.05 to 2.0 μm. The mechanism of Hf particle formation can be understood by analyzing the process thermodynamics, including adiabatic temperatures and equilibrium reaction phases. In addition, analytical methods, including X-ray diffraction, SEM/TEM BET, FTIR, and oxygen analysis, were employed to characterize the synthesized Hf powders. Theoretical analysis was also conducted to predict the oxygen content according to Hf particle size. To the author's best knowledge, this work is the first known report demonstrating the preparation of hafnium micro- and nanopowders by the combustion synthesis method. • The combustion of HfO 2 +0.08KClO 4 + k Mg systems was studied for k = 2.7–7. • Synthesis temperatures ranging from 1570 to 1000 °C were recorded. • Hf powder with particle sizes of 0.05–2.0 μm and 0.8–2.0 wt% oxygen was obtained. • Deoxidation using a Ca/Mg alloy powder produced Hf metal with less than 0.1 wt% O 2. • A theoretical model, for predicting oxygen concentration in Hf particles is proposed. [ABSTRACT FROM AUTHOR]