Dual role of activated carbon as fuel and template for solution combustion synthesis of porous zinc oxide powders

In this work, nanosized zinc oxide (ZnO) powders were fabricated by urea–nitrate solution combustion synthesis using activated carbon as a structure-directing template and secondary fuel at different fuel–oxidant ratios. The as-synthesized powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), N₂ adsorption–desorption measurements, UV–Vis diffuse reflectance spectroscopy, and photoluminescence. The effect of fuel amount on photocatalytic activity of ZnO powders was evaluated by the degradation of an azo dye Orange G. It was observed that combustion synthesis with activated carbon as a secondary fuel had a profound effect on reducing crystallite size and enhancement of specific surface area. The crystallite size of the as-synthesized powders varied from 46 to 26 nm. The ZnO powder prepared at a fuel–oxidant ratio of 1.8 possessed the small crystallite size and high specific surface area of 69 m²/g. It correspondingly resulted in the highest dye removal percentage of 99% with a rate constant of 0.027 min⁻¹. The improvement in dye degradation can be due to the synergistic interaction and interplay of enhanced surface area and catalytic ability of the photocatalyst. This study provides a simple single-step synthesis methodology to produce metal oxide nanopowders with tunable surface properties for high potential applications in catalysis, optoelectronics, and gas sensors.     

Effects of excess NaClO4 on phases,size and magnetic properties of Ni–Zn ferrite powders prepared by combustion synthesis

Ni_0.4Zn_0.6Fe₂O₄ powders were prepared by combustion synthesis with different amount of NaClO₄. Phases, particle size and magnetic properties of the powders and annealed powders were systematically investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectrometer (EDS) and vibrating sample magnetism (VSM). The excess content of NaClO₄ offered significant advantages with respect to the size, morphology and magnetic properties of the powders. After annealing, sub-micro ferrite spherical powders with spinel phase in a range of 500–800 nm can be obtained. With the increase of the NaClO₄ content, the saturation magnetization of the powders shows a maximum value at 68.8 emu/g when w=0.4, whereas the coercivity stayed nearly constant. The maximum saturation of annealed powders by combustion synthesis is much higher than the range reported in the literature.     

Preparation and Optical Properties of Transparent (Ce,Gd)3Al3Ga2O12 Ceramics

Transparent (Ce,Gd)₃Al₃Ga₂O₁₂ (Ce:GAGG) ceramics are promising scintillators for use in high‐energy particle detection application such as nuclear medical imaging. In this study, we report a novel method for the preparation of transparent Ce:GAGG ceramic in oxygen atmosphere without sintering aid. The highest transmittance of as prepared samples with thickness of 1 mm around wavelength of 558 nm reaches 62%, which is close to that value of its comparative single crystal. The average grain size of samples sintered at 1650°C for 10 h is about 11 μm. The spectroscopic properties have also been investigated. The emission peak around 558 nm, which is consistent with that of Ce:GAGG single crystals, matches well with the detection wavelength of photomultiplier.     

Dicalcium silicate (2CaO·SiO2) synthesized through flame spray pyrolysis and solution combustion synthesis methods

Synthesis of dicalcium silicate (2CaO.SiO₂ or C₂S) through flame spray pyrolysis and a solution combustion method was investigated by the variation of flames and fuels. The synthesized powders were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM). X-ray diffraction analysis revealed the formation of dicalcium silicate polymorphs with presence of calcium oxide, calcium carbonates and amorphous materials as impurities. Results suggest that some flames and fuels favor the formation of calcite during the synthesis process due to an excess of carbon atoms in the combustion. Fourier transform infrared spectra of all samples showed the main silicates reflections located near to 500?cm^?1 and 1000?cm^?1 and scanning electron microscopy showed the formation of spherical agglomerates of nanoparticles in both methods. By these two alternative methods of synthesis it was possible to obtain C₂S with nanometric particle size.     

Mechanical properties of 1 mol% CeO2‐10 mol% Sc2O3 co‐doped and stabilized ZrO2 synthesized through hydro/solve‐thermal method

Ultra‐fine 1 mol% CeO₂‐10 mol% Sc₂O₃ co‐doped and stabilized ZrO₂ (1Ce10ScSZ) powders with average grain size less than 10 nm in diameter were prepared by hydro/solve‐thermal method using either deionized water, ethanol, or methanol as solvent. As‐synthesized powders were characterized in terms of phase structure, particle morphology, and chemical composition by X‐ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), high‐resolution transmission electron microscopy (HRTEM), and inductively coupled plasma‐optical emission spectroscopy (ICP‐OES), respectively. Sintering studying was conducted on pellets of 15 mm in diameter and 3 mm in thickness under uniaxial compaction using 25 MPa at either 600, 800, 1000, 1100, 1200, 1400, or 1500°C for 1 hour. Phase transitions and grain morphologies of those sintered samples were characterized by XRD and field emission scanning electron microscopy (FESEM). Mechanical properties were characterized on dense pellets sintered at 1500°C by nanoindentation. Experimental results showed that ethanol was more effective to synthesize agglomerate‐free 1Ce10ScSZ powders as compared with deionized water and methanol. Choice of solvent affected the environment of hydro/solve‐thermal solution, which led to variation of chemical compositions of powders and porosities of sintered pellets, and therefore, influenced their mechanical performance. Our study showed that solvent was important to make dense, thin, and mechanically robust 1Ce10ScSZ electrolyte for potential applications in electrochemical devices. Absolute values of hardness (H) and Young's modulus (E) measured from our samples are much higher and more consistence than those results obtained from commercial vendors reported in literatures.     

Mechanical activation-assisted combustion synthesis of in situ aluminum matrix hybrid (TiC/Al2O3) nanocomposite

The aim of this study is the synthesis of aluminum-based metal matrix nanocomposites reinforced with in situ TiC and Al₂O₃ hybrid reinforcements by the mechanically activated combustion synthesis. The composites were fabricated from the powder blends consisting of aluminum, rutile and graphite with an excess amount of aluminum following the 14Al–3TiO₂−3C system and milled up to 30 h. Phase evolutions and structural changes during ball milling and combustion synthesis were studied by X-ray diffraction technique, field-emission gun scanning electron microscopy and transmission electron microscopy. The results showed that even after 10 h of milling, no new phases were formed. The increasing of milling time caused the broadening of all the peaks indicating a decrease in the crystallite size and an increase in the lattice strain. These results showed that Al, C and TiO₂ nanocrystallites could be obtained during the ball-milling process. The result of combustion synthesis of un-milled powders confirmed that no new phases were found. In comparison with un-milled powder mixture, the 10 h milled powder could be easily ignited and XRD, HRSEM and TEM results confirmed that Al/TiC–Al₂O₃ nanocomposite was successfully synthesized through combustion method from the mechanical activated powder mixture. Mechanical activation via high energy ball-milling provided to the initial powder mixture extra energy, which is needed to increase the reactivity of powder mixture and to make possible the ignition and the sustaining of combustion.     

Synthesis and Spark Plasma Sintering of Mg2Si Nanopowder by Mechanical Alloying and Heat Treatment

In this investigation, a two‐step method for the preparation of magnesium silicide (Mg₂Si) nanopowder was studied. This method is known as mechanical alloying followed by heat treatment. The results showed that the compositions of the combustion products depended on the milling time, heat treatment temperature, and starting mixtures. Pure Mg₂Si nanopowder was formed after short milling time and heat treatment, from Mg and Si powders with the mole ratio of 2.1:1 (Mg:Si) at 500°C in Ar atmosphere. Using the Mg₂Si nanopowder, Mg₂Si ceramic was produced by spark plasma sintering at 800°C under 50 MPa for 15 min. Composition and structure of reactants and products were examined by X‐ray diffraction (XRD), field emission scanning electron microscopy (FE‐SEM) and high‐resolution transmission electron microscopy (HR‐TEM).     

Investigation on mechanochemical combustion behavior of Mg–V2O5–Co3O4-C reactive system to synthesize VC–Co nanocomposite powder

VC–Co nanocomposite powders were obtained by mechanochemical combustion synthesis from a mixture of V₂O₅, Co₃O₄, C and Mg powders. The synthesized powders were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). VC–Co nanocomposite was directly produced after 10 min milling through a mechanically induced self-sustaining reaction without further heat treatment. TEM analysis showed that a nanostructured powder with a mean particle size of 100 nm was procured in the sample milled for 10 min.     

Synthesis of nanocrystalline gadolinium doped ceria via sol–gel combustion and sol–gel synthesis routes

Gadolinium doped ceria (GDC) has been investigated as a promising material for application as an electrolyte in intermediate temperature solid oxide fuel cells (IT-SOFC). In this work, 10GDC powders (Gd_0.1Ce_0.9O_1.95) were synthesized by sol–gel combustion and sol–gel synthesis routes using the same complexing agents in both procedures. The thermal behavior of Gd–Ce–O precursor gels was investigated by TG–DSC measurements. X-ray diffraction (XRD) analysis was used for the characterization of phase purity and crystallinity of synthesized samples. Scanning electron microscopy (SEM) was employed for the estimation of surface morphological features. Nitrogen adsorption–desorption (BET model) was used for evaluation of specific surface area. The surface composition was determined by X-ray photoelectron spectroscopy (XPS). Electrical properties of synthesized ceramic samples were studied by means of impedance spectroscopy.     

Effects of pH value on the microstructure and magnetic properties of solution combusted Fe3O4 powders

Magnetite (Fe₃O₄) powders were prepared by solution combustion synthesis method using conventional and microwave ignition at various pH values of starting solution, adjusted by NH₄OH. The chelated species in dried gels were predicted by theoretical calculations and Fourier transform infrared spectroscopy. The combustion reaction rate strongly depended on pH values as investigated by thermal analysis. Phase evolution and structure characterized by X-ray diffraction method showed single phase and well-crystalline Fe₃O₄ powders which were achieved using conventional ignition at pH ≥ 7. However, the microwave ignition led to the formation of impure FeO phase together with Fe₃O₄. The microwave combusted powders exhibited the disintegrated structure in comparison with the bulky microstructure for conventionally combusted powders, as observed by scanning electron microscopy. Magnetic properties of the as-combusted powders studied by vibration sample magnetometry showed the highest saturation magnetization of 81.3 emu/g for conventional ignition at pH of 7, due to the high purity and large crystallite size.     

Comparison of the microwave-induced combustion and solid-state reaction for the synthesis of LiMn2O4 powder and their electrochemical properties

In the current research, we proposed a new method called microwave-induced combustion synthesis to produce LiMn₂O₄ powders. The microwave-induced combustion synthesis entails the dissolution of metal nitrates, and urea in water, and then heating the resulting solution in a microwave oven. Spinel LiMn₂O₄ powders were successfully synthesized by microwave-induced combustion. The microwave-heated LiMn₂O₄ powders annealed at various temperatures in the range of 600–800 °C were determined. The resultant powders were characterized by X-ray diffractometer (XRD), and scanning electron microscopy (SEM). The annealed samples were used as cathode materials for lithium-ion battery, for which their discharge capacity and electrochemical characteristic properties in terms of cycle performance were also investigated. The LiMn₂O₄ cell provides a high initial capacity of 133 mAh/g and excellent reversibility. The excellent capacity and reversibility were attributed to LiMn₂O₄ powders with small and uniform particle size produced by microwave-induced combustion synthesis.     

Molten-salt-assisted combustion synthesis of B4C powders: Synthesis mechanism and dielectric and electromagnetic wave absorbing properties

A novel electromagnetic wave (EMW) absorber was prepared by combustion synthesis. Boron carbide (B₄C) powders with different grain sizes using a molten-salt-assisted combustion technique with B₂O₃, CB (carbon black), and Mg powders as starting materials, and NaCl as an additives. The effects of the NaCl content on the phase compositions and the microstructure of the products were characterized. A combustion front quenching method was used to elucidate the mechanism for the B₄C powders synthesis. The dielectric, and EMW absorbing properties in the X-band were also investigated. The results showed that the addition of NaCl significantly reduced the grain size of B₄C powders. Nanoscale B₄C powders with cubic polyhedral structures were synthesized using 6 wt% NaCl (labeled as N-6). According to the quenching test results can be obtained that the first step in the combustion synthesis was melting B₂O₃ into a glassy substance. At the same time, Mg melted and formed a liquid pool into which the NaCl dissolved, followed reduction of the B₂O₃ to B. The formed B eventually reacted with CB to form B₄C, and the B₄C particles precipitated from the matrices. The N-6 sample exhibits optimal dielectric and EMW absorbing properties, because of a high specific surface area that enhances interfacial and space charge polarization.     

Effect of fuel type on the microstructure and magnetic properties of solution combusted Fe3O4 powders

Porous magnetite (Fe₃O₄) powders were synthesized by solution combustion method using the glycine and urea at different fuel to oxidant ratios (ϕ). The combustion behavior depended on the fuel type as characterized by thermal analysis. The structure and phase evolution investigated by X-ray diffraction method showed nearly single phase Fe₃O₄ powders which were achieved only by using the glycine fuel at ϕ=1. The specific surface area and porous structures of the as-combusted Fe₃O₄ powders were characterized by N₂ adsorption-desorption isotherms and scanning electron microscopy, respectively. The surface area using the glycine fuel (62.6 m²/g) was higher than that of urea fuel (42.5 m²/g), due to different combustion reactions. Magnetic properties of the as-combusted powders were studied by vibration sample magnetometry which exhibited the highest saturation magnetization of 74 emu/g using the glycine fuel at ϕ=1 on account of its high purity and large crystallite size.     

Combustion assisted synthesis of hardystonite nanopowder

In this study, single-phase hardystonite (Ca₂ZnSi₂O₆) nanopowder was synthesized by combustion synthesis method from aqueous solution of Calcium nitrate, Zinc nitrate and Tetraethyl orthosilicate. In order to characterize the obtained powders, X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were used. The effect of sucrose concentration on the purity and morphology of the obtained hardystonite powder, and its initial annealing temperature was investigated. The optimum sucrose to metal ratio was found to be 2:1. The average particle size and the maximum crystallite size of the produced hardystonite nanopowder were 220 and 40 nm, respectively.     

Synthesis and characterization of pyrochlore lanthanide (Pr,Sm) zirconate ceramics

Three different lanthanide zirconate powders: Pr₂Zr₂O₇, Sm₂Zr₂O₇ and PrSmZr₂O₇ were prepared by combustion synthesis. The synthesis initially yielded amorphous powders, which crystallized after subsequent thermal treatment. Well-crystallized compounds were formed after calcination at temperature as low as 950 °C. Effect of the thermal treatment on the phase evolution was studied by X-ray powder diffraction (XRD). The powders calcined at the highest temperature (1550 °C) showed that all compositions possess the pyrochlore structure with the space group No. 227. The obtained powders were compacted and pressureless sintered without additive at 1600 °C for 4 h in the air. Microstructure development was examined by field emission scanning electron microscopy, as well as by transmission electron microscopy. It was found that the lowest value for thermal conductivity, 1.2 W/m K, was obtained for mixed lanthanide composition with pyrochlore structure (PrSmZr₂O₇). The effect of chemical composition on micro-hardness and thermal conductivity of the obtained zirconates was studied.     

Combustion synthesis of B4C/Al2O3/C composite powders and their effects on properties of low carbon MgO-C refractories

To improve the dispersity and oxidation resistance of nano carbon black (CB) in low carbon MgO-C refractories, B₄C/Al₂O₃/C composite powders were prepared by a combustion synthesis method using B₂O₃, CB and Al powders as the raw materials. The phase compositions and microstructures of the synthesized products were characterized by X-ray diffraction (XRD), Raman spectroscopy, and a scanning electron microscopy/energy dispersive spectrometry (SEM/EDS). The results show that an 80 wt% excess of CB is the maximum amount of CB that can be added under the condition of a self-propagating combustion wave, and the phase compositions of the products are B₄C, α-Al₂O₃ and CB. B₄C particles with uniform sizes and cubic polyhedral structures are embedded in the Al₂O₃ matrix. The combustion-synthesized B₄C/Al₂O₃/C powders and mechanically mixed B₄C/Al₂O₃/C powders were added to the low carbon MgO-C refractories, and their corresponding properties were compared. The apparent porosity (AP) of the refractories with the synthesized powders (labelled as M3) is lower than those of the refractories with mechanically mixed powders (labelled as M2) and without composite powders (labelled as M1). The oxidation ratio and slag erosion depth of M3 were lower than those of M2 and M1. The thickness of the decarburized layer of M3 was 10.2% and 22.4% less than that of M2 and M1, respectively. The penetration depth of M3 was 12.0% and 27.9% less than that of M2 and M1, respectively. The thermal shock resistance of M3 was better than that of M2 and M1. The residual strength ratio of M3 was 15.8% and 17.2% more than that of M2 and M1, respectively. These results suggest that the combustion-synthesized B₄C/Al₂O₃/C composite powders can be used as new and promising additives for low carbon MgO-C refractories.     

Synthesis of Cerium‐Doped Gd3(Al,Ga)5O12 Powder for Ceramic Scintillators with Ultrasonic‐Assisted Chemical Coprecipitation Method

Cerium‐doped Gd₃(Al,Ga)₅O₁₂ powders have been synthesized with ultrasonic‐assisted chemical coprecipitation method (UACC), and the traditional chemical coprecipitation method (CC) was also employed for comparison. The structure and morphology of powders were investigated by XRD, BET, and TEM. The powders were used for preparing ceramics at different temperatures. The specific surface areas of UACC and CC powders calcined at 800°C were 66 and 29 m²/g, respectively. Ceramics derived from UACC and CC powders were sintered at 1600°C, and the densities are 6.67 and 6.48 g/cm³, respectively. UACC is an attractive method for synthesizing GAGG powder for preparing ceramic scintillators.     

Solution combustion synthesis of cerium oxide nanoparticles as corrosion inhibitor

In this study, combustion synthesis of cerium oxide nanoparticles was reported using cerium nitrate hexahydrate as starting material as well as urea, glycine, glucose, and citric acid as fuels. The influence of fuel type on structure, microstructure, band gap, and corrosion inhibition was investigated. X-ray diffraction (XRD) patterns and scanning electron microscopy micrographs showed that CeO₂ nanoparticles with different morphologies were obtained depending on the fuel type. Microstructural changes from unreacted gel to sponge-like morphologies were resulted by varying the fuel type from urea, glycine, and glucose to citric acid. In addition to Ce–O bonds, Fourier transform infrared analysis showed carbon bonds of carbonaceous compositions from incomplete combustion which were declined during combustion reaction. Furthermore, corrosion analyses showed that samples synthesized using urea fuel released the most Ce⁺⁴ ions and could have better protection than other samples.     

Mechanism and microstructural evolution of combustion synthesis of ZrB2–Al2O3 composite powders

Mechanism of combustion synthesis (CS) of ZrB₂–Al₂O₃ composite powders was systematically analyzed by a combustion front quenching method (CFQM). The microstructural evolution during the CS process was investigated by field-emission scanning electron microscopy (FESEM) equipped with energy dispersive X-ray spectrometer (EDS). The combustion temperature and wave velocity were measured by the data acquisition system. Moreover, the phase constituents of the final product were examined by X-ray diffraction (XRD). The thermal behaviors of the stoichiometic powders under the thermal exposure were characterized using differential scanning calorimetry (DSC) and thermogravimetric (TG). The results showed that the combustion reaction started from the melting of the B₂O₃ and Al particles, which was followed by the formation of ZrO₂–B₂O₃–Al solution. The ignition temperature of this system was determined to be around 800 °C. B and Al₂O₃ were then precipitated from the solution. As the CS reaction proceeded, Zr and Al₂O₃ were produced by the reaction between ZrO₂ particles and Al and precipitated from the solution. ZrB₂ could then be formed by the direct reaction between Zr and B. Finally, the ZrB₂–Al₂O₃ composite powders were obtained. Furthermore, a model corresponding to the dissolution–precipitation mechanism was proposed.     

Formation of metastable tungsten tetraboride by reactive hot-pressing

The synthesis of tungsten tetraboride (WB₄) powders prepared by reactive hot-pressing in a vacuum from elemental tungsten (W) and amorphous boron (B) powders is reported in this work. This study systematically investigates the effects of the synthesizing temperature, B/W molar ratio, pressure and time on phase formation. The XRD pattern for the as-synthesized powders was analysed. Metastable tungsten tetraboride was synthesized in a vacuum at 1350 °C with a B/W molar ratio of 8.0 under a low uniaxial pressure (30 MPa) for 1 h. The scanning electron microscopy and transmission electron microscopy results showed that the particles had a tendency to form agglomerates. Amorphous boron was found to exist in the final product, and formation of the crystal phase WB₄ was confirmed.