Simultaneous synthesis and consolidation of nanostructured TaSi2–Si3N4 composite by pulsed current activated combustion

Dense nanostructured 4TaSi₂–Si₃N₄ composite was synthesized by pulsed current activated combustion synthesis (PCACS) method within 3 min in one step from mechanically activated powders of TaN and Si. Simultaneous combustion synthesis and densification were accomplished under the combined effects of a pulsed current and mechanical pressure. Highly dense 4TaSi₂–Si₃N₄ composite with relative density of up to 98% was produced under simultaneous application of a 60 MPa pressure and the pulsed current. The average grain size and mechanical properties (hardness and fracture toughness) of the composite were investigated.     

Simultaneous pulsed current activated combustion synthesis and densification of NbSi2–SiC composite

Dense ultrafine NbSi₂–SiC composite was synthesized by the pulsed current activated combustion synthesis (PCACS) method within 3 min in one step from mechanically activated powders of NbC and 3Si. Simultaneous combustion synthesis and densification were accomplished under the combined effects of a pulsed current and mechanical pressure. Highly dense NbSi₂–SiC composite with relative density of up to 97% was produced under simultaneous application of a 60 MPa pressure and the electric current. The average grain size and mechanical properties (hardness and fracture toughness) of the composite were investigated.     

Mechanical synthesis and rapid consolidation of nanostructured FeAl–Al2O3 composites by high-frequency induction heated sintering

Nanopowders of FeAl and Al₂O₃ were synthesized from Fe₂O₃ and Al by high energy ball milling. The sizes of FeAl and Al₂O₃ were 4 and 57 nm, respectively. A dense nanostuctured FeAl–Al₂O₃ composite was consolidated by a high-frequency induction heated sintering method within two minutes from mechanically synthesized powders of FeAl and Al₂O₃. The grain size, sintering behavior and hardness of the sintered FeAl–Al₂O₃ composite were investigated.     

Spark plasma sintering of Al-doped ZrB2–SiC composite

This research presents the influence of Al addition on microstructure and mechanical behavior of ZrB₂–SiC ultra-high temperature ceramic matrix composite (UHTCMC) fabricated by spark plasma sintering (SPS). A 2.5?wt% Al-doped ZrB₂–20?vol% SiC UHTCMC was produced by SPS method at 1900?°C under a pressure of 40?MPa for 7?min. The microstructural and phase analysis of the composite showed that aluminum-containing compounds were formed in-situ during the SPS as a result of chemical reactions between Al and surface oxide films of the raw materials (i.e. ZrO₂ and SiO₂ on the surfaces of ZrB₂ and SiC particles, respectively). The Al dopant was completely consumed and converted to the intermetallic Al₃Zr and Al₄Si compounds as well as Al₂O₃ and Al₂SiO₅. A relative density of 99.8%, a hardness (HV5) of 21.5?GPa and a fracture toughness (indentation method) of 6.3?MPa?m^1/2 were estimated for the Al-doped ZrB₂–SiC composite. Crack bridging, branching, and deflection were identified as the main toughening mechanisms.     

The effect of EEMAO processing on surface mechanical properties of the TiO2–ZrO2 nanostructured composite coatings

We report fabrication of TiO₂–ZrO₂ nanostructured composite coatings by EPD-Enhanced MAO (EEMAO) technique on titanium substrates where especial emphasis was placed on improving the surface hardness of the substrates and establishing a microstructure-property correlation. Based on the XRD and the EDX results, the layers consisted of anatase, rutile, monoclinic zirconia, and tetragonal zirconia. It was observed that the anatase/rutile and tetragonal/monoclinic zirconia rations increased with the processing time and the electrolyte concentration. The zirconia content also increased with the processing time and the electrolyte concentration. XPS technique was also employed to further confirm the surface chemical composition and stoichiometry of the layers. A uniform distribution of zirconia across the titania matrix was evident in the SEM images. The surface hardness of the TiO₂-ZrO₂ composite layers was observed to increase with the zirconia concentration. Employing EEMAO technique, the surface harness of the titanium substrates was successfully improved from ∼190 Hv to ∼700 Hv.     

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.     

Microstructural development during spark plasma sintering of ZrB2–SiC–Ti composite

The present study investigates the effect of Ti addition on the microstructure development and phase evolution during spark plasma sintering of ZrB₂–SiC ceramic composite. A ZrB₂–20?vol% SiC sample with 15?wt% Ti was prepared by high-energy milling and spark plasma sintering at 2000?°C for 7?min under 50?MPa. The X-ray diffraction test, microstructural studies and thermodynamic assessments indicated the in-situ formation of several compounds due to the chemical reactions of Ti with ZrB₂ and SiC. The Ti additive was completely consumed during the sintering process and converted to the ceramic compounds of TiC, TiB and TiSi₂. In addition, another refractory phase of ZrC was also formed as a result of sidelong reaction of ZrB₂ and SiC with the Ti additive.     

Physicochemical characterization and catalytic applications of MoO3–ZrO2 composite oxides towards one pot synthesis of amidoalkyl naphthols

A series of MoO₃–ZrO₂ composite oxide catalysts were prepared by coprecipitation and impregnation methods and characterized by XRD, Raman, UV–Vis, TEM and sorptometric techniques. Characterization studies indicated the presence of tetragonal zirconia phase and well dispersed MoO₃ species as isolated and polymolybdate clusters in the composite oxide. The MoO₃(20 mol%)–ZrO₂ material was used as efficient catalyst for synthesis of amidoalkyl naphthols under solvent free conditions using conventional as well as microwave heating. The results obtained clearly showed that the composite oxide catalyst was recyclable and highly efficient for the reaction giving good yield and purity of the products.     

Combustion synthesis of TiC–NiAl composite by induction heating

The aim of this work was to develop a new process for the synthesis of TiC and NiAl/TiC composite in which the combustion reaction was ignited using a high frequency induction heater. High density, two-layer TiC–NiAl composites were also produced using this process. Temperature profiles during synthesis were measured with an IR thermometer and a high resolution thermal image camera was used to monitor the reaction process. Phase transformation was investigated using XRD and SEM was used to characterize the microstructure of the synthesized composites. The mechanical properties of the products were evaluated by measuring hardness. The results show that the reaction was complete and that stoichiometric products of NiAl and TiC were produced. The properties of NiAl/TiC composites were found to be functions of composition and processing parameters. The reaction mechanism was analyzed using temperature monitoring, thermodynamic analysis and microstructure investigation.     

Ablation of C/SiC,C/SiC–ZrO2 and C/SiC–ZrB2 composites in dry air and air mixed with water vapor

C/SiC composites with different additives (ZrO₂ and ZrB₂) were fabricated by CVI and CVD and their oxidation and ablation properties at 1700–1800 °C were investigated. Two different ablation test conditions, dry air and air mixed with water vapor, are compared. The ablation test results are reviewed, the weight loss rates are presented and the corresponding micro-structures are investigated in detail. The results show that in dry air, the weight loss rate of C/SiC composites is greater than those with ZrO₂ and ZrB₂ additives. However, in air mixed with water vapor (5 wt%) to simulate the hygrothermal condition, the weight loss rates of these three composites all become relatively smaller. A model is proposed to predict the weight loss of C/SiC composites and it agrees well with the experimental data.     

Synthesis,densification and characterization of TaB2–SiC composites

The TaB₂–27.9 vol% SiC composite was synthesized by self-propagating high-temperature synthesis starting from mechanically activated Ta, B₄C and Si reactants. The obtained powders were spark plasma sintered at 1800 °C and 20 MPa for 30 min total time, thus obtaining a 96% dense product. The latter one was characterized in terms of microstructure, hardness, fracture toughness, and oxidation resistance. The obtained results, particularly the fracture toughness, are promising when compared to those related to analogous materials reported in the literature and fabricated with similar and different processing routes.     

Simultaneous synthesis and densification of α-Zr(N)/ZrB2 composites by self-propagating high-temperature combustion under high nitrogen pressure

Simultaneous synthesis and densification of α-Zr(N)/ZrB₂ composites from a 85 mol% Zr/15 mol% B mixed-powder compacts have been achieved by self-propagating high-temperature under a nitrogen pressure of 10 MPa. Composites consist of fine and short rodlike ZrB₂ grains (0.1 μm^?–0.5 μm^l) dispersed into α-Zr(N) matrix (3 μm). Dense composite materials (96.5% of theoretical) exhibit excellent mechanical properties, in which their bending strength and H_v are 560 MPa and 6.5 GPa, respectively. This bending strength is much superior to those (205 and 480 MPa) of dense equi-axial α-Zr(N) (10 μm) and dense ZrB₂ (6 μm). Fine and rodlike ZrB₂ grains greatly enhanced their mechanical properties.     

Structure and properties of nanostructured ceramic matrix composite coatings prepared in-situ by reactive plasma spraying micro-sized Al–Fe2O3–Cr2O3 powders

Nanostructured FeAl₂O₄-based ceramic matrix composite coatings were prepared in-situ by reactive plasma spraying micro-sized Al–Fe₂O₃ and Al–Fe₂O₃–Cr₂O₃ powders. The microstructure, toughness, Vickers hardness, and adhesive strength of these coatings were investigated by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and mechanical tests. The results indicated that both the coatings exhibited a nanostructured microstructure. The grains of coating AFC sprayed with Al–Fe₂O₃–Cr₂O₃ powders are finer than those of the coating AF sprayed with Al–Fe₂O₃ powders. The composite nano-coating sprayed with Al–Fe₂O₃–Cr₂O₃ powders exhibited higher hardness and better wear resistance compared with those of the composite nano-coating sprayed with Al–Fe₂O₃ powders. The adhesive strength, toughness, and wear resistance of the composite coating sprayed with Al–Fe₂O₃–Cr₂O₃ powders were significantly enhanced compared with those of the composite coating sprayed with Al–Fe₂O₃ powders, which were attributed to the Cr₂O₃ addition.     

Effect of SiC and Al2O3 particles on the electrodeposition of Zn, Co and ZnCo: II. Electrodeposition in the presence of SiC and Al2O3 and production of ZnCo–SiC and ZnCo–Al2O3 coatings

SiC or Al₂O₃ microsized particles were added to acid sulfate-based solutions for the electrodeposition of Zn, Co, and ZnCo. Initially, their effects on the electrochemical processes were evaluated. The Zn electrodeposition rate was increased in both SiC and Al₂O₃-loaded solutions. The Co electrodeposition rate was also increased by SiC. However, Al₂O₃ decreased it, especially at the beginning. Both SiC and Al₂O₃ influenced the electrodeposition of ZnCo positively at moderate loadings. The factors involved in producing ZnCo–SiC and ZnCo–Al₂O₃ composites were evaluated. ZnCo–SiC composites could be deposited with a higher [Co/Zn] ratio in the metal matrix than for pure ZnCo. In ZnCo–Al₂O₃, the [Co/Zn] ratio was smaller than in ZnCo and ZnCo–SiC. It was necessary to reduce the CoSO₄ concentration to improve the Al₂O₃ co-deposition. The variation in [Co/Zn] ratio could, in principle, be related to the effects of SiC and Al₂O₃ on the individual Zn and Co electrodeposition.     

Fast synthesis of MgAl2O4‒W and MgAl2O4‒W‒W2B composite powders by self-propagating high-temperature synthesis reactions

MgAl₂O₄?W and MgAl₂O₄?W?W₂B composite powders were obtained rapidly in a single step by self-propagating high-temperature synthesis of WO₃?Mg?xAl₂O₃ and WO₃?B₂O₃?Mg?yAl₂O₃ systems. The addition of various Al₂O₃ contents (x and y-values) to the starting materials was considered as the main synthesis parameter. Thermodynamic calculations revealed that the adiabatic temperature of both systems was decreased with increasing Al₂O₃ content. The XRD results indicated that after acid leaching of the WO₃?Mg?xAl₂O₃ combustion products, W and MgAl₂O₄ were formed as the main phases and WO₂, MgWO₄ and Al₂O₃ as the minor constituents in the final composite. On the other hand, MgAl₂O₄?W composites were synthesized in the WO₃?B₂O₃?Mg?yAl₂O₃ system at y<1.4 mol. By increasing the y-value to 2.1 mol, W₂B was formed as a new product leading to production of MgAl₂O₄?W?W₂B composite. The formation of spinel was confirmed by the Fourier transformed infrared spectroscopy analysis. Microstructure observations represented the uniform distribution of MgAl₂O₄ blocks within the fine spherical W particles. The melting of Al₂O₃ was found as a vital step for rapid synthesis of MgAl₂O₃ by the SHS route. Finally, the possible formation mechanism of MgAl₂O₄ during the combustion synthesis was proposed.     

Microwave assisted combustion synthesis of coupled ZnO–ZrO2 nanoparticles and their role in the photocatalytic degradation of 2,4-dichlorophenol

Zinc oxide (ZnO), zirconium oxide (ZrO₂) and their coupled oxides in the molar ratio 1:1, 2:1 and 1:2 (labeled as ZnZr, Zn₂Zr, and ZnZr₂ respectively) were successfully prepared by a microwave assisted urea–nitrate combustion synthesis. The structure and morphology of the pure ZnO, ZrO₂ and coupled ZnZr, Zn₂Zr, and ZnZr₂ were characterized by powder X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), photoluminescence spectroscopy (PL), high resolution scanning electron microscopy (HRSEM), energy dispersive X-ray spectrometry (EDX) and Brunauer–Emmett–Teller (BET) methods. The results of the photocatalytic degradation of 2,4-dichlorophenol (2,4-DCP) in aqueous solution indicated that the coupled metal oxide, Zn₂Zr is more effective towards the degradation of 2,4-DCP when compared to ZnO, ZrO₂, ZnZr and ZnZr₂.     

Sol–gel auto combustion synthesis of CoFe2O4/1-methyl-2-pyrrolidone nanocomposite: Its magnetic characterization

A magnetic nanocomposite was generated by the sol–gel auto-combustion method in the presence of 1-methyl-2-pyrrolidone, a functional solvent. The temperature-dependent magnetic properties of the CoFe₂O₄ nanoparticles have been extensively studied in the temperature range of 10–400 K and magnetic fields up to 80 kOe. Zero field cooled (ZFC) and field cooled (FC) curves indicate that the blocking temperature (T_B) of the CoFe₂O₄ nanoparticles is above 400 K. It was found from M–H curves that the low temperature saturation magnetization values are higher than bulk value of CoFe₂O₄. The saturation magnetization (M_s), remanence magnetization (M_r), reduced remanent magnetization (M_r/M_s) and coercive field (H_c) values decrease with increasing temperature. The M_r/M_s value of 0.75 at 10 K indicates that the CoFe₂O₄ nanoparticles used in this work have, as expected, cubic magnetocrystalline anisotropy according to the Stoner–Wohlfarth model. T^1/2 dependence of the coercive field was observed in the temperature range of 10–400 K according to Kneller's law. The extrapolated T_B and the zero-temperature coercive field values calculated according to Kneller's law are almost 427 K and 13.2 kOe, respectively. The room temperature H_c value is higher than that of the previously reported room temperature bulk values. The effective magnetic anisotropy constant (K_eff) was calculated as about 0.23×10⁶ erg/cm³ which is lower than that of the bulk value obtained due to disordered surface spins.     

Synthesis of SiC/SiO2 core–shell powder by rotary chemical vapor deposition and its consolidation by spark plasma sintering

SiC (core) and SiO₂ (shell) powders were synthesized via rotary chemical vapor deposition (RCVD). The SiC particles (3C, <1 μm in diameter) were coated with a layer of SiO₂ (10–15 nm in thickness). Using spark plasma sintering, the SiC/SiO₂ nanopowders were then synthesized into SiC/SiO₂ composite bodies. Although a phase transformation from 3C to 6H was observed at above 2123 K in the sintered monolithic SiC bodies, sintered SiC/SiO₂ bodies did not display such phase transformation. In addition, SiC/SiO₂ bodies did not exhibited grain growth until the sintering temperature reached 2223 K. The density and Vickers hardness of the sintered SiC/SiO₂ bodies increased with increasing sintering temperature. The highest density and hardness of SiC/SiO₂ composite bodies were 98.1% and 24.4 GPa at 2223 K, respectively, which were higher than the corresponding values of 90% and 14 GPa for monolithic SiC bodies.     

Effects of liquid phases on densification of TiO2-doped Al2O3–ZrO2 composite ceramics

This study investigated the densification behaviors and microstructural evolution of Al₂O₃–ZrO₂ (3Y) composite ceramics doped with four different amounts of TiO₂ (0, 1, 4, and 8 wt%; denoted as 0T, 1T, 4T, and 8T, respectively) to clarify the effect of TiO₂ dopants on densification. The shrinkage rate during densification increased with the increase in the amount of TiO₂. The development of grain boundary feature was also examined. The undoped ceramic showed clean grain boundaries. Thin liquid grain boundary phases were observed in 1T, whereas large liquid phases were found on the grain boundary and at the junction pockets in 4T and 8T. The results were discussed in terms of the relationship between densification and grain boundary feature.     

Synthesis and characterization of MgAl2O4–ZrO2 composites

Different types of dense 5–97% ZrO₂–MgAl₂O₄ composites have been prepared using a MgAl₂O₄ spinel obtained by calcining a stoichiometric mixture of aluminium tri-hydroxide and caustic MgO at 1300 °C for 1 h, and a commercial yttria partially stabilized zirconia (YPSZ) powder as starting raw materials by sintering at various temperatures ranging from 1500 to 1650 °C for 2 h. The characteristics of the MgAl₂O₄ spinel, the YPSZ powder and the various sintered products were determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), BET surface area, particle size analysis, Archimedes principle, and Vickers indentation method. Characterization results revealed that the YPSZ addition increases the sintering ability, fracture toughness and hardness of MgAl₂O₄ spinel, whereas, the MgAl₂O₄ spinel hampered the sintering ability of YPSZ when sintered at elevated temperatures. A 20-wt.% YPSZ was found to be sufficient to increase the hardness and fracture toughness of MgAl₂O₄ spinel from 406 to 1314 Hv and 2.5 to 3.45 MPa m^1/2, respectively, when sintered at 1600 °C for 2 h.