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Abstract This study investigated the high-temperature stability of CSZ, YSZ, and MSZ specimens in a CaCl 2 -CaF 2 -CaO molten salt at 1200 °C for the application of the materials as oxygen-ion-conducting solid-oxide membrane anodes in the electroreduction process of metal oxides. YSZ exhibited the lowest degradation among the tested specimens in a high-temperature stability test, whereas CSZ showed the highest degradation. The weight loss was not severe with concentrations of CaO up to 10 wt%. CSZ showed peaks for m-ZrO 2 , YSZ showed peaks for t-ZrO 2 and CaZrO 3 , and MSZ showed peaks for t-ZrO 2 and m-ZrO 2 in 0 wt% CaO. In the case of 5 wt% CaO, all specimens exhibited m-ZrO 2 and CaZrO 3 peaks, In the cases of 10 wt% and 20 wt% CaO, CSZ and MSZ showed peaks for CaZrO 3 , and YSZ showed peaks for m-ZrO 2 and CaZrO 3. While CSZ and MSZ became significantly looser as the CaO concentration was increased to 10 wt%, YSZ became significantly denser due to the formation of a protective layer and attack dependent on the solubility of CaO in the molten CaCl 2. In terms of long-term operation, YSZ was demonstrated to possess superior high-temperature stability compared to CSZ and MSZ, and CaO concentrations from 5 wt% to 10 wt% were found to be significantly more stable than other concentrations. Highlights • The degradation mechanism of CSZ, YSZ, and MSZ in CaCl 2 -CaF 2 -CaO molten salt is proposed. • The formation of CaZrO 3 acts as a protective layer. • YSZ shows high degradation resistance to CaCl 2 -CaF 2 molten salt that contains up to 10 wt% of CaO. • In view of long-term operation, YSZ is demonstrated to possess superior high-temperature stability compared to CSZ and MSZ. [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]

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]

Combustion based synthesis of AlN nanoparticles using the "solid nitrogen" promotion reaction was investigated in Al2O3 + 3Mg system in nitrogen atmosphere. A controlled amount of Mg + 0.5NH4Cl mixture as a solid source of nitrogen was blended with the Al2O3 + 3Mg starting system and the synthesis reaction of AlN nanoparticles was conducted using the exothermic heat of the entire reaction system. The resulting AlN nanoparticles were characterized by X-ray diffraction (XRD), Raman and Fourier transform infrared spectroscopy (FTIR), PL spectroscopy, field-emission scanning electron microscopy, transmission electron microscopy, and Brunauer-Emmett-Teller surface area techniques. The analysis results confirmed that single phase and crystalline AlN nanoparticles with an average size of 50-500 nm were obtained from the developed approach. Photoluminescence spectra of AlN nanopowders under the excitation of 230-270 nm UV light revealed that AlN emits yellow-red light having a wavelength near to 590 nm. The chemistry of the combustion process is discussed and the basic reactions that led to the formation of AlN are presented. [ABSTRACT FROM AUTHOR]

High-quality two-dimensional (2D) nanosheets of B 4 C were synthesized using a facile combustion reaction with a reaction mixture comprising boron oxide (B 2 O 3 ), magnesium (Mg), and polyvinylchloride (C 2 H 3 Cl) n . The ability to tune the nanosheets of boron carbide was achieved by controlling the combustion temperature within a range of 1500–1700 °C and by using polyvinylchloride powder as the carbon source. FE-SEM and TEM images of the acid leached combustion products show sheet-like B 4 C particles with thicknesses of about 10–50 nm and edge lengths from 0.1 to several micrometers. The chemistry of the combustion process and the formation mechanism of B 4 C nanosheets are discussed based on the experimental findings. [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]

Amorphous boron nanoparticles were synthesized by heating a B 2 O 3 + 3 Mg + k NaCl ( k is the number of moles of NaCl) exothermic mixture in a laboratory oven at 800 °C under argon flow. NaCl was used as inert material to decrease the maximum combustion temperature of the reaction mixture when it was self-ignited after the melting of Mg at 650 °C. The size of the boron nanoparticles extracted from the final product by acid leaching ranged between 30 and 300 nm for k values ranging from 1 to 5. Moreover, increasing the value of k from 1 to 5 resulted in an increase in the specific surface area of the nanoparticles from 40 to 74 m 2 g −1 . However, at k = 10, a decrease in the specific surface area to 47.56 m 2 g −1 was recorded due to incomplete reduction of B 2 O 3 . The ignition point of boron nanoparticles in air as estimated using a thermocouple was approximately 300 °C. Digital camera recording of the combustion process of boron nanoparticles in air revealed that the burning speed of the nanoparticles increased significantly from 0.3 to 15 cm/s when k increased from 1 to 5. [ABSTRACT FROM AUTHOR]

Highlights: [•] A facile synthesis has been developed to convert directly solid Na2SiO3. [•] The synthesis has been carried out at ambient pressure and temperature. [•] Hydrolysis was performed using ethanol, Na2SiO3 particles and HCl solution. [•] Other precipitants (NH4Cl, (NH4)2SO4, B2O3) were tested. [•] The particle characteristics were investigated by TGA, FE-SEM, XRD, and BET. [Copyright &y& Elsevier]

This paper demonstrates for the first time the fabrication of Zr-Cu alloy ingots from a Hf- free ZrO2 precursor in a molten CaCl2 medium to recover nuclear-grade Zr. The reduction of ZrO2 in the presence of CaO was accelerated by the formation of Ca metal in the intermediate stage of the process. Tests conducted with various amounts of ZrO2 indicate that the ZrO2 was reduced to the metallic form at low potentials applied at the cathode, and the main part of the zirconium was converted to a CuZr alloy with a different composition. The maximum oxygen content values in the CuZr alloy and Zr samples upon using liquid Cu were less than 300 and 891 ppm, respectively. However, Al contamination was observed in the CuZr during the electroreduction process. In order to solve the Al contamination problem, the fabrication process of CuZr was performed using the metallothermic reduction process, and the produced CuZr was used for electrorefining. The CuZr alloy was further purified by a molten salt electrorefining process to recover pure nuclear-grade Zr in a LiF-Ba2ZrF8-based molten salt, the latter of which was fabricated from a waste pickling acid of a Zr clad tube. After the electrorefining process, the recovered Zr metal was fabricated into nuclear-grade Zr buttons through arc melting following a salt distillation process. The results suggest that the removal of oxygen from the reduction product is a key reason for the use of a liquid CaCu reduction agent. [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]

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]

Hollow carbon nanospheres as potential cathode materials for lithium-sulfur (Li-S) batteries were successfully synthesized using a metathesis reaction between sodium azide and halogen polymer. The reaction was driven by thermal heat from the exothermic recombination of Na + and Cl − (or F − ) ions into NaCl (or NaF) salts. The result was an increase of the overall system temperature up to 1320–1750 °C followed by the simultaneous formation of sodium halide-carbon core–shell nanoparticles. Therefore, hollow carbon nanospheres with diameter and shell thickness of ∼50–500 nm and ∼10–50 nm, respectively, were produced after water washing of the reaction product. The composite cathode materials for Li-S batteries were manufactured by infiltrating sulfur into the hollow core of nanospheres. The electrochemical cycling showed discharge capacity of ∼700 mAh g −1 (after 100 cycles) at 0.5 C current rate which is more than ∼2.4 times larger than that for the sulfur/carbon black composites prepared by the same technique. The enhancement of battery performance was attributed to the well-organized and unique 3D structure of hollow carbon, enabling better utilization of sulfur. [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]

Recent developments have seen breakthroughs in zero-, one-, two-, and three-dimensional AlN micro- and nanostructures, such as nanoparticles, nanowires, nanotubes, thin films and 3D multifold symmetry crystals. The attractive electrical, optical, and thermal properties of AlN make these materials irreplaceable for microelectrochemical systems (MEMS), surface acoustic waves (SAWs) and light emitting diodes (LED). The significant interest in the field of AlN nanostructure synthesis and application encouraged us to summarise the reported data to better understand the physical and chemical aspects of AlN crystal growth processes. Four main topics are covered in this review article: (1) the morphological diversity of AlN nano- and microstructures; (2) formation mechanisms and growth dynamics; (3) theoretical simulation of growth processes based on density functional theory (DFT) and phase field (PF) modelling approaches; (4) application and devices. This article also provides a perspective on future research relevant to AlN micro- and nanostructures. [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]

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]

Combustion of inorganic powder mixtures is not only one of the chemical routes of fabrication of advanced inorganic materials but is also drawing attention as a high-temperature process to grow inorganic nanocrystals of various shapes and morphologies. Here, we demonstrate the formation of AlN 3-D structures with diverse morphologies: from 6-fold patterned crystals to multilayer hierarchical structures. We examined the possible chemical mechanisms governing the formation of AlN crystals and the growth behaviour based on FESEM and TEM observations. [ABSTRACT FROM AUTHOR]

In this paper we describe a progressive two-step process that allows zirconium fluoride (ZrF 4 ) contained in spent baths for etched zirconium alloys to be effectively recycled on a pilot scale and produce a high purity regenerated pickling acid. In the first step, a spent pickling liquor is treated by a BaF 2 suspension to produce water insoluble Ba 2 ZrF 8 . After filtration of Ba 2 ZrF 8 more than 99.9 wt % purity pickling acid is regenerated. The precipitation mechanism of Ba 2 ZrF 8 is discussed and the role of BaF 2 particles size on the precipitation process is demonstrated. In the second step the as-precipitated Ba 2 ZrF 8 is mixed with Mg and Cu metal powders and heat-treated at 1200 °C (or above) to produce CuZr alloy ingot. The characteristics of the ingot are discussed in regard to Cu concentration and the heating temperature. [ABSTRACT FROM AUTHOR]

• Ba 2 ZrF 8 and BaTiF 6 fluorides are precipitated from the spent liquors using BaF 2. • The heating of Ba 2 ZrF 8 (BaTiF 6) + Mg + k Cu mixtures yield a self-ignition at 600 °C. • CuTi and CuZr alloy ingots and BaMgF 4 slag are produced after the heating process. • The chemistry of liquor purification and CuTi (CuZr) ingots formation is highlighted. In this paper, we describe a progressive two-step process that allows titanium and zirconium fluorides (TiF 4 , ZrF 4) contained in spent liquors of etched Ti and Zr alloys to be effectively recycled into CuTi and CuZr alloy compositions and a regenerated pickling acid of high purity. In the first step, spent pickling liquor is treated with a BaF 2 suspension to produce water-insoluble BaTiF 6 and Ba 2 ZrF 8 fluoride salts. In the second step, the as-precipitated BaTiF 6 and Ba 2 ZrF 8 fluoride salts are mixed with Mg and Cu metals powder and heat-treated at 1300 °C to produce CuTi and CuZr alloy ingots. The microstructures of the ingots are discussed in regard to Cu concentration. [ABSTRACT FROM AUTHOR]