Single step synthesis of tungsten carbide (WC) nanoparticles from scheelite ore

To prepare tungsten carbide (WC) nanoparticles high purity precursors like W, WO₃, WCl₄, WCl₆ and W(CO)₆ are used. Moreover, these precursors are obtained after high temperature and multistage processing of the ore. In this article a single step synthesis method is reported to get tungsten carbide (WC) nanoparticles directly from scheelite ore. The mixture of scheelite, activated charcoal and magnesium was heated for 20 h at 800 °C in an autoclave which led to the direct conversion of scheelite to nanocrystalline WC. The undesired reaction products and impurities (CaO, MgO and SiO₂) were washed firstly with dilute HCl (1:1) and then with base (0.25 M NaOH). The obtained powders were characterized by high resolution scanning electron microscopy (HRSEM), high resolution transmission electron microscopy (HRTEM) and X-ray diffraction.     

Preparation and electrocatalytic property of WC/carbon nanotube composite

Tungsten carbide/carbon nanotube composite was prepared by surface decoration and in situ reduction-carbonization. The samples were characterized by XRD, SEM, EDS, TEM, HRTEM and BET, respectively. The XRD results show that the sample is composed of carbon nanotube, tungsten carbide and tungsten oxide. The EDS results show that the distribution of tungsten oxide is consistent with that of tungsten carbide. SEM, TEM and HRTEM results show that the tungsten carbide nanoparticle with irregular granule grows on the outside surface of carbon nanotube homogenously. The electrocatalytic activity of the sample for p-nitrophenol reduction was tested by a powder microelectrode in a basic solution. The results show that the electrocatalytic activity of the sample is higher than that of granular tungsten carbide, hollow globe tungsten carbide with mesoporosity and carbon nanotube purified. The improvement of the electrocatalytic activity of the sample can be attributed to its components and composite structure. These results indicate that tungsten carbide/carbon nanotube composite is one of the effective ways to improve the electrocatalytic activity of tungsten carbide.     

Effect of the starting materials on the reaction synthesis of Ti3SiC2

Ternary carbide of titanium and silicon was produced via mechanical milling and following heat treatment. Effects of the starting materials, milling time and heat treatment temperature were studied. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were utilized to evaluate the structural and morphological evolutions of the ball-milled and annealed powders. Results showed that the ball milling of TiO–Si–C as the starting materials failed to synthesize Ti₃SiC₂. Additionally, ball milling the elemental powders for shorter milling times resulted in the activation of the powders. However, after longer milling times, Ti–TiC nanocomposite was obtained. Furthermore, during annealing the milled powders, Ti₃SiC₂–TiC nanocomposite with the mean grain size of 16 nm was synthesized. After 20 h of milling, a very fine microstructure with narrow size of distribution and spheroid particles was achieved.     

Oxyacetylene torch ablation resistance of Co-modified WC coating deposited on C/C composites by supersonic atmosphere plasma spraying

Cobalt (Co) was chosen as an additive to improve the ablation resistance of WC coating for SiC coated C/C composites, SiC modified WC coating and pure WC coating which were prepared and tested for comparative purposes. Results showed that the thermal shock resistance of WCC (WC-10%Co) coating was better than pure WC coating and WCS (WC-10%SiC) coating. Furthermore, the produced oxide layer on WCC coating was found to be more stable due to the reaction of CoO and WO₃. As a result, during oxyacetylene torch ablation test, compared with pure WC coating and WCS coating, WCC coating keeps excellent dimensional stability with the linear ablation rate decreased by 67% and 62%, respectively, showing a significant improvement of the ablation resistance.     

The synthesis and microstructure of morph-genetic TiC/C ceramics

Wood is a natural material with a novel and ordered hierarchical structure. In the present work, it is used as a bio-template to produce morph-genetic TiC/C ceramics. This is obtained by infiltrating the carbon preform pyrolyzed from wood with tetrabutyl titanate. It was subsequently sintered at 1400 °C to produce the final ceramic structure.By observing the microstructure under the scanning electron microscope and the transmission electron microscope, the morph-genetic TiC/C ceramics are shown retaining the complex morphology of the original template structure. The crystalline TiC was formed through the reaction of tetrabutyl titanate with carbon preform, and it was distributed mainly at the surface layer of the cellular wall. During the conversion of wood into carbon preform, the specific surface area of samples increased from 28.2 to 35.7 m² g⁻¹, and its porosity also increased from 64.4% to 80.3%. However, during the conversion of carbon preform into morph-genetic ceramics, the specific surface area of samples decreased from 35.7 to 33.8 m² g⁻¹, and its porosity also decreased from 80.3% to 76.5%. At the synthesis process, the variation of pore-size distribution is mainly in the range from 0.1 to 1 μm.     

The influence of polyelectrolyte on the synthesis of B4C/BN nanocomposite powders via sol-gel method

In the present study, B₄C-BN nanocomposite powders were synthesized by using the sol-gel method. To investigate the effects of polyelectrolyte on phase content, particle size, and final morphology of synthesized powders different amounts of ammonium polycarboxylate were used as a gel dispersing agent and a nitrogen source. Highly crystalline, sub-micron/micron-sized boron carbide particles with varying morphologies including polyhedral-equiaxed, belt-like, needle-like, and complex-shaped hierarchical structures were produced from the polymeric gel containing glycerine, tartaric acid, and citric acid as carbon sources, and boric acid as boron source. With the addition of ammonium polycarboxylate as a polymeric gel network modifier, nanocomposite powders containing micron-sized polyhedral-equiaxed boron carbide particles and boron nitride nanoflakes were obtained. The results indicated that the particles dimensions, crystallinity, and B₄C to BN phase ratio of the synthesized powders are directly related to the preliminary formation of borate-ammonium and/or amine complexes in the polymeric gel. The SEM inspections revealed that the size of boron carbide particles tends to increase from 2 μm up to 40 μm as a function of ammonium polycarboxylate content. It was also observed that the average size and thickness of boron nitride nanoflakes within the range of 80 nm to 3 μm and 10–150 nm, respectively. B₄C/BN nanocomposite powders were synthesized with up to 32% BN content using a 43 wt% ammonium polycarboxylate additive.     

Thermal shock behavior of 3-dimensional C/SiC composite

The thermal shock behavior of a three-dimensional carbon fiber reinforced SiC matrix fabricated by chemical vapor infiltration (CVI) technique was studied using the air quenched method. Damage to composites was assessed by a destructive technique of measuring mechanical properties using three-point flexure and SEM characterization. C/SiC composites displayed good resistance to thermal shock, and retained 83% of the original strength after quenching from 1300 to 300°C 100 times. The critical ΔT of C/SiC in combustion environment was 700°C. The critical number of thermal shocks for the C/SiC composite was about 50 times. When the number of thermal shocks was less than 50 times, the residual flexural strength of C/SiC composites decreased with the increase of thermal shock times. When the number of thermal shocks of C/SiC was greater than 50, the strength of C/SiC did not further decrease because the crack density was saturated.     

One-pot hydrothermal synthesis of MoS2 nanosheets/C hybrid microspheres

Uniform MoS₂ nanosheets/C hybrid microspheres with mean diameter of 320 nm have been successfully synthesized via a facile one-pot hydrothermal route by sodium molybdate reacting with sulfocarbamide in d-glucose solutions. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). XRD patterns showed that the MoS₂ was kept as a two-dimensional nanosheet crystal and C was retained as amorphous even after their annealing treatment at 800 °C. TEM and SEM images indicated that the MoS₂ nanosheets were uniformly dispersed in the amorphous carbon. The experiment results also revealed that the appropriate amount of d-glucose had an obvious effect on the formation of uniform MoS₂ nanosheets/C hybrid microspheres. A possible formation process of MoS₂ nanosheets/C hybrid microspheres was preliminarily presented.     

Investigation on mechanochemical synthesis of Al2O3/BN nanocomposite by aluminothermic reaction

Alpha-alumina–boron nitride (α-Al₂O₃–BN) nanocomposite was synthesized using mixtures of aluminum nitride, boron oxide and pure aluminum as raw materials via mechanochemical process under a low pressure of nitrogen gas (0.5 MPa). The phase transformation and structural evaluation during mechanochemical process were investigated by X-ray diffractometry (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and differential thermal analysis (DTA) techniques. The results indicated that high exothermic reaction of Al–B₂O₃ systems under the nitrogen pressure produced alumina, aluminum nitride (AlN), and aluminum oxynitride (Al₅O₆N) depending on the Al value and milling time, but no trace of boron nitride (BN) phases could be identified. On the other hand, AlN addition as a solid nitrogen source was effective in fabricating in-situ BN phase after 4 h milling process. In Al–B₂O₃–AlN system, the aluminothermic reaction provided sufficient heat for activating reaction between B₂O₃ and AlN to form BN compound. DTA analysis results showed that by increasing the activation time to 3 h, the temperature of both thermite and synthesis reactions significantly decreased and occurred as a one-step reaction. SEM and TEM observations confirmed that the range of particle size was within 100 nm.     

ZnO nanorods surface-decorated by WO3 nanoparticles for photocatalytic degradation of endocrine disruptors under a compact fluorescent lamp

Nanoscaled tungsten oxide (WO₃) particles coated on ZnO nanorods (ZNRs) were newly synthesized by combining a hydrothermal technique with a chemical solution process. The structure, morphologies and compositions of the as-prepared WO₃–ZNR nanocomposites were characterized through XRD, FESEM, TEM and Raman measurements. The results revealed that pure monoclinic WO₃ nanoparticles with an average size range of 18–26 nm were distributed on the surfaces of ZNRs and attached strongly. Particularly, the optical properties as well as photocatalytic characteristics of pure ZNRs and WO₃–ZNR nanocomposites with different loadings of WO₃ were also examined. The absorption of WO₃–ZNR nanocomposites was redshifted due to effective immobilization of WO₃ on ZNRs. Under irradiation of a 55 W compact fluorescence lamp, the photocatalytic activities of the WO₃–ZNR nanocomposites were superior to those of pure ZNRs and P25 in the degradation of resorcinol (ReOH). Furthermore, WO₃–ZNR nanocomposites showed very favorable recycle use potential and high sedimentation rate. Other endocrine disrupting chemicals (EDCs) such as phenol, bisphenol A (BPA) and methylparaben were also successfully photodegraded under identical conditions. These characteristics showed the practical applications of the WO₃–ZNR nanocomposites in indoor environmental remediation.     

Microstructure of high battery-performance Li2FeSiO4/C composite powder synthesized by combining different carbon sources in spray-freezing/freeze-drying process

Spray-freezing/freeze-drying technique was applied to the synthesis of Li₂FeSiO₄/C composite powders using solutions containing various carbon sources, water-soluble and colloidal carbon, followed by heat treatment. The effects of the carbon sources on the microstructure and battery performance of the synthesized composite powders were investigated. The microstructures of the composite powders were clearly different when different carbon sources were used, ascribed from the thermal behavior of the carbon sources during the heat treatment. It was possible to control the microstructures of Li₂FeSiO₄/C composite powders by combining different carbon sources, and the synthesized composite powders exhibited high discharge capacities by mixing with only a binder for cathode. The composite powders using glucose and Ketjenblack dispersion as carbon sources delivered 165 mAh/g at first discharge capacity at 0.1?C. The developed chain structure suitable for conducting paths in the electrodes and a higher-specific BET surface area, attributed from Ketjenblack, were likely responsible for the higher performance.     

One-step hydrothermal synthesis and microwave electromagnetic properties of RGO/NiFe2O4 composite

The reduced graphene oxide (RGO)/NiFe₂O₄ composite was synthesized by a facile one-pot hydrothermal route, which avoided the usage of chemical reducing agent. The reduction of graphene oxide (GO) and the crystallization of NiFe₂O₄ crystals happened in a one-step hydrothermal process. The morphology, microstructure and magnetic properties of the composite were detected by means of XRD, XPS, TEM, EDX, TG-DSC and VSM. The maximum R_L of the RGO/NiFe₂O₄ composite is −39.7 dB at 9.2 GHz with the thickness of 3.0 mm, and the absorption bandwidth with the R_L below −10 dB is up to 5.0 GHz (from 12.7 to 17.7 GHz) with a thickness of 1.9 mm. The introduction of RGO signally enhanced microwave absorption performance of the NiFe₂O₄ NPs. It is believed that such composite will be applied widely in microwave absorbing area.     

An aqueous synthesis of photocatalyst by selective dissolution of titanium oxide/hydroxyapatite composite

A novel synthesis method of a highly active photocatalyst was proposed. Titanium dioxide (TiO₂) nano-particles were prepared by three-step procedure, precipitation of hydroxyapatite (HAp) on TiO₂ particles, heat treatment of the TiO₂/HAp composites, and acid treatment in hydrochloric acid. The unique point of this procedure is the selective dissolution of HAp to obtain exposed TiO₂ surfaces. The HAp precipitation was achieved by stirring TiO₂ powders in the mixtures of Ca(NO₃)₂ and NH₄H₂PO₄ aqueous solutions at pH 8.5. Then, the heat-treated TiO₂/HAp composites were treated with hydrochloric acid. The precipitated HAp avoided the direct contact of TiO₂ particles and suppressed the phase transformation from anatase-to-rutile >200 °C. The HAp also suppressed a decrease of specific surface area of TiO₂ during the heat treatment. The photocatalytic activities were evaluated from an absorbance decrease of methylene blue (MB) under ultraviolet (UV) irradiation. The MB photodecomposition was approximated to the first-order reaction and the reaction rate constants of the obtained TiO₂ powders heated at various temperatures were higher than those of conventional TiO₂ powders heated at same temperatures. The enhanced photocatalytic activity is attributed to the suppression effects for the phase transformation to rutile phase and the decreasing of specific surface area in the heat treatment.     

Electrically induced liquid infiltration for the synthesis of carbon/carbon–silicon carbide composite

The electrically induced liquid infiltration (EILI) method for the synthesis of carbon/carbon–silicon carbide (C/C–SiC) materials was developed. The method involves Joule preheating of a porous carbon/carbon preform surrounded by silicon media, followed by silicon infiltration into the pore structure, and its reaction with carbon to form pore-free C/C–SiC composite. This technique is characterized by high heating rates (10²–10³ K/s) and short processing times (5–20 s), which distinguish it from conventional approaches. The influence of maximum treatment temperature, as well as preheating rate on the depth of infiltration, reaction kinetics, and the material microstructure was investigated. C/C–SiC composite with a compressive strength which was twice that of the initial C/C material was synthesized.     

Intermediate phases formation during the synthesis of Bi4Ti3O12 by solid state reaction

In this work, the formation of Bi₄Ti₃O₁₂ by solid state reaction from Bi₂O₃ and TiO₂ starting powders has been studied. The Bi₄Ti₃O₁₂ formation occurs through an intermediate Bi₁₂TiO₂₀ sillenite phase formed at temperatures sligthly over 300 °C. This sillenite phase is stable up to ∼750 °C, but in the presence of TiO₂ reacts to form Bi₄Ti₃O₁₂ at temperatures >500 °C. Raman spectroscopy has been used to evidence the amorphization of TiO₂, demonstrating that the Bi₄Ti₃O₁₂ formation occurs through the reaction of sillenite Bi₁₂TiO₂₀ and TiO₂.     

Solution combustion synthesis of bioceramic calcium phosphates by single and mixed fuels—A comparative study

Calcium phosphate based bioceramics have been synthesized by a modified combustion synthetic route using both citric acid and succinic acid separately and in mixture as fuels and nitrate and nitric acid as oxidants. Calcium nitrate and diammonium hydrogen phosphate were used as calcium and phosphate sources. The effects of citric acid to succinic acid ratio on the phase formation have been investigated. The precursors and the calcined products have been characterized by powder X-ray diffraction, Fourier-transform infrared spectroscopy and scanning electron microscopy. Succinic acid has been used as a fuel for the first time to synthesize hydroxyapatite.     

Large-scale synthesis of WO3 nanoplates by a microwave-hydrothermal method

Tungsten oxide (WO₃) nanoplates were synthesized by a 270 W microwave-hydrothermal reaction of Na₂WO₄·2H₂O and citric acid (C₆H₈O₇·H₂O) in deionized water. X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), and selected area electron diffraction (SAED) were used to reveal the synthesis of WO₃ complete rectangular nanoplates in the solution of 0.2 g citric acid for 180 min, with O-W-O FTIR stretching modes at 819 and 741 cm⁻¹, and two prominent O-W-O Raman stretching modes at 804 and 713 cm⁻¹. The 2.71 eV indirect energy gap, and 430-460 nm blue emission wavelength range of WO₃ complete rectangular nanoplates were determined using UV-visible and photoluminescence (PL) spectrometers. The formation mechanism was also proposed according to the experimental results.     

Mechanochemical synthesis of Ti1−xZrxB2 and Ti1−xHfxB2 solid solutions

Solid solutions of TiB₂-ZrB₂ and TiB₂-HfB₂ were obtained under an inert atmosphere by high-energy ball-milling mixtures of Ti/Zr/B and Ti/Hf/B, respectively. Milling promoted mechanically induced self-sustaining reactions (MSR), and the ignition time was dependent on the initial composition of the mixture. The stoichiometry of Ti_1−xZr_xB₂ and Ti_1−xHf_xB₂ solid solutions was controlled by adjusting the atomic ratio of the reactants. The solid solutions were characterised by X-ray diffraction, transmission electron microscopy, electron diffraction, and energy dispersive X-ray spectroscopy. The results revealed that TiB₂-ZrB₂ possessed a nanometric microstructure and good chemical homogeneity. However, in the TiB₂-HfB₂ system, an inhomogeneous solid solution was obtained when a Ti-rich mixture was employed. The solid solutions showed good thermal stability; thus, can be used as raw materials for the development of technological materials for structural applications.     

Synthesis of CuGa2O4 nanoparticles by precursor and self-propagating combustion methods

Copper gallate spinels, CuGa₂O₄, have been synthesized by two wet chemical routes: precursor method and self-propagating combustion involving a glycine-nitrate system. All complex precursors have been characterized by chemical analysis, infrared spectroscopy (IR), ultraviolet visible spectroscopy (UV–vis), electron paramagnetic resonance spectroscopy (EPR), thermal analysis and scanning electron microscopy (SEM). The copper gallate spinel oxides have been further investigated by X-ray diffraction (XRD), SEM, IR, UV–vis, magnetic measurements and EPR. The crystallite size of the copper gallate was found about 280 Å.