Effect of WC content on microstructure and mechanical properties of Ni3Al-bonded cermets

The effect of WC content on microstructure and mechanical properties of the TiC–Ni₃Al system cermets was investigated. Ni₃Al-bonded cermets showed a core–rim structure with carbide particle coupled with rim embedded in Ni₃Al binder. With WC content increasing, TiC grains were refined and the white rim became complete and got thicker gradually. Interface between core and rim showed a completely coherent relationship. The rim enriched in W constituted an ideal coherence between hard phase and Ni₃Al binder phase. With WC content increasing, the densification of cermets was enhanced, and hardness and TRS were increased firstly and then reduced, reaching peak values 90.9 HRA (HV₃₀ 15 GPa) and 1629 MPa, respectively in cermet N5 (25 wt% WC). Similarly, fracture toughness got a peak value (11.6 MPa m^1/2), at the composition with 20 wt% WC.     

Tribo-mechanical characterization of spark plasma sintered chopped carbon fibre reinforced silicon carbide composites

Short carbon fibre (C_f) reinforced silicon carbide (SiC) composites with 7.5 wt% alumina (Al₂O₃) as sintering additive were fabricated using spark plasma sintering (SPS). Three different C_f concentrations i.e. 10, 20 and 30 wt% were used to fabricate the composites. With increasing C_f content from 0 to 20 wt%, micro-hardness of the composites decreased ~28% and fracture toughness (K_IC) increased significantly. The short C_f in the matrix facilitated enhanced fracture energy dissipation by the processes of crack deflection and bridging at C_f/SiC interface, fibre debonding and pullout. Thus, 20 wt% C_f/SiC composite showed >40% higher K_IC over monolithic SiC (K_IC≈4.51 MPa m^0.5). Tribological tests in dry condition against Al₂O₃ ball showed slight improvement in wear resistance but significantly reduced friction coefficient (COF, μ) with increasing C_f content in the composites. The composite containing 30 wt% C_f showed the lowest COF.     

Effect of nano-titania (η-TiO2) content on the mechano-physical properties of a magnesia refractory composite

The mechano-physical properties of a sintered magnesia matrix containing 0–8 wt% nano-titania (η-TiO₂) have been investigated. The crystalline phases and microstructure characteristics of the refractory specimens sintered by solid state at 1500 °C for 4 h in an electric furnace were studied by X-ray diffraction (XRD), and scanning electron microscopy (SEM) with microanalysis (EDS), respectively. The physical properties are reported in terms of density and porosity. The mechanical behavior was evaluated by a cold crushing strength (CCS) test. As a result, it was found that the presence of η-TiO₂ in the magnesia matrix induced titanates formation (Mg₂TiO₄ and CaTiO₃), which improved the sintering process. Nano-titania also produced a fine-grained microstructure with intergranular second phase particles, which remain at the boundary and exert a pinning effect. In general, the addition of 5 wt% of η-TiO₂ contributed to reach a maximum increment in physical and mechanical properties.     

Pressureless sintering of HfB2–SiC ceramics doped with WC

Using WC as sintering aid, nearly full dense (～99%) HfB₂–20 vol% SiC ceramics were sintered at 2200 °C for 2 h without external pressure. The densification mechanism, microstructure evolution, mechanical properties and oxidation resistance were investigated. The results indicated that complex chemical reactions of WC in HfB₂–SiC system strongly related to the densification, microstructure and properties. The Young's modulus, fracture toughness and 3-pt bending strength of HfB₂–20 vol% SiC with 10 wt% WC were 511 GPa, 4.85 Mpa m^1/2 and 563 MPa, respectively, which were comparable to some hot pressed HfB₂–SiC ceramics in literature. The oxidation of HfB₂–20 vol% SiC with 10 wt% WC at 1500 °C in air exhibited parabolic kinetics. After oxidation at 1500 °C for 10 h, its weight gain and SiC-depleted layer thickness were 3.7 mg/cm² and 43 μm, respectively, and its residual flexural strength was comparable to or even a little higher than the value before oxidation.     

Effect of SiC addition on the formation of ZrB2 through reaction of ZrO2, boric acid (H3BO3) and carbon black

ZrB₂-SiC powders with different amounts of SiC (10–30 wt%) were in-situ synthesized at 1600 °C for 90 min in Ar atmosphere. Effects of SiC addition on the formation of ZrB₂ via carbothermal reduction of ZrO₂, H₃BO₃ and carbon black were investigated. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive spectrometer (EDS) and transmission electron microscope (TEM). The grain size of ZrB₂ in final powders decreased with adding SiC. Columnar ZrB₂ and granular SiC were combined interactively when the SiC content was 25 wt%. Layer-like hexagonal SiC was obtained in the product containing 30 wt% SiC, whereas the ZrB₂ grain growth was strongly inhibited. Furthermore, the growth mechanisms of ZrB₂ and SiC were studied.     

Preparation of Fe3O4 particles from copper/iron ore cinder and their microwave absorption properties

In this study, magnetic Fe₃O₄ particles were prepared from copper/iron ore cider by precipitation oxidization method. The yield of Fe was 82.6 at%. XRD, TEM, SEM, EDS and microwave network analyzer were used to characterize the particles. The results showed that Fe₃O₄ particles were well crystallized and possessed an octahedral morphology, and the crystal size was about 200 nm; the sample with 70 wt% Fe₃O₄ exhibited the optimal absorbing ability, the minimum reflection loss was ?42.7 dB at 14.08 GHz and the bandwidth less than ?10 dB was about 4.2 GHz when the sample thickness was 1.9 mm. It was clearly demonstrated that the Fe₃O₄ particles prepared from copper/iron ore cider could be used as an effective microwave absorbing material.     

Hydration of Ca7ZrAl6O18 phase

The hydraulic properties of the Ca₇ZrAl₆O₁₈ (C₇A₃Z) phase as well as the hydration products and thermal decomposition mechanism of this hydrated phase were studied. Microcalorimetric analysis has shown that the C₇A₃Z phase reacts with water very quickly, especially in the first 2 h after the start of the experiment. Hydration of calcium zirconium aluminate proceeds with the formation of high refractory calcium zirconate (with melting point 2345 °C), apart from the hydrated, nearly amorphous material. According to the DTA–TG–EGA, FT-IR and SEM/EDS examinations it has been found that not only the hydrates CAH₁₀, C₂AH₈ and C₄AH₁₉ are present, but also C₃AH₆ (C = CaO, A = Al₂O₃, H = H₂O), the only hydrated calcium aluminate which is a thermodynamically stable phase above 40 °C. Unhydrated Ca₇ZrAl₆O₁₈ and CaZrO₃ phases have been found by XRD, but crystalline hydrates have not been detected.     

Effect of milling type on the microstructural and mechanical properties of W-Ni-ZrC-Y2O3 composites

This study reports the effect of milling type on the microstructural, physical and mechanical properties of the W-Ni-ZrC-Y₂O₃ composites. Powder blends having the composition of W-1 wt% Ni-2 wt% ZrC-1 wt% Y₂O₃ were milled at room temperature for 12 h using a Spex™ 8000D Mixer/Mill or cryomilled in the presence of externally circulated liquid nitrogen for 10 min using a Spex™ 6870 Freezer/Mill or sequentially milled at room temperature and cryogenic condition. Then, powders were compacted in a hydraulic press under a uniaxial pressure of 400 MPa and green bodies were sintered at 1400 °C for 1 h under Ar/H₂ atmosphere. Phase and microstructural characterization of the milled powders and sintered samples were performed using X-ray diffractometer (XRD), TOPAS software, scanning electron microscope/energy dispersive spectrometer (SEM/EDS), X-ray fluorescence (XRF) spectrometer and particle size analyzer (PSA). Archimedes density and Vickers microhardness measurements, and sliding wear tests were also conducted on the sintered samples. The results showed that sequential milling enables the lowest average particle size (214.90 nm) and it is effective in inhibiting W grain coarsening during sintering. The cryomilled and sintered composite yielded a lower hardness value (5.80±0.23 GPa) and higher wear volume loss value (149.42 µm³) than that of the sintered sample after room temperature milling (6.66±0.39 GPa; 102.50 µm³). However, the sequentially milled and sintered sample had the highest relative density and microhardness values of 95.09% and 7.16±0.59 GPa and the lowest wear volume loss value of 66.0 µm³.     

Enhanced thermal conductive 3D-SiC/Al-Si-Mg interpenetrating composites fabricated by pressureless infiltration

A high thermal conductive 3D-SiC/Al-Si-Mg interpenetrating composite (IPC) with three dimensional mutually interpenetrated structure was fabricated by mold-forming and pressureless infiltration method. Al-15Si-10Mg was used as the infiltration aluminum alloy. The obtained composite was treated with a T6 procedure. The composed phases, microstructure, thermal conductivity, mechanical strength and fractography of the prepared 3D-SiC/Al-Si-Mg IPC were either analyzed or measured with X-ray diffraction (XRD), optical metallography, laser thermal conductivity instrument, universal testing machine, field emission electron scanning microscopy (SEM) with energy dispersive spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM), and etc. The results showed that both SiC ceramic and aluminum alloy phases distribute evenly and form a three-dimensional mutually interpenetrated structure in the obtained IPC. No clear brittle and harmful Al₄C₃ phase was found in the composite. The obtained IPC contains a SiC volume fraction of 67 vol% and has the properties of a density of 3.02 g/cm², a thermal conductivity of 233.6 W/(m °C), a thermal expansion coefficient (RT~300 °C) of 7.03×10⁻⁶/°C and a bending strength of 288 MPa.     

Formation of hollow MgO-rich spinel whiskers in low carbon MgO–C refractories with Al additives

MgO–C refractories with different carbon contents have been developed to meet the requirement of steel-making technologies. Actually, the carbon content in the refractories will affect their microstructure. In the present work, the phase compositions and microstructure of low carbon MgO–C refractories (1 wt% graphite) were investigated in comparison with those of 10 wt% and 20 wt% graphite, respectively. The results showed that Al₄C₃ whiskers and MgAl₂O₄ particles formed for all the specimens fired at 1000 °C. With the temperature up to 1400 °C, more MgAl₂O₄ particles were detected in the matrix and AlN whiskers occurred locally for high carbon MgO–C specimens (10 wt% and 20 wt% graphite). However, the hollow MgO-rich spinel whiskers began to form locally at 1200 °C and grew dramatically at 1400 °C in low carbon MgO–C refractories, whose growth mechanism was dominated by the capillary transportation from liquid Al at these temperatures.     

Effect of pressure on corrosion of Inconel 625 in supercritical water up to 100 MPa with acids or oxygen

The corrosion behavior of Inconel 625 in supercritical water was investigated under high pressure (30–100 MPa at 400 °C) with the addition of acids (5 mmol/kg CH₃COOH or 0.5 mmol/kg HNO₃) or O₂ (2.5–250 mmol/kg). Ni and Cr ions were the main dissolved metal ions in the effluent. The Ni ion concentration showed no clear dependence on the O₂ concentration or pressure in the experiment with O₂; the concentration was lower than 0.05 ppm. The concentration increased with pressure up to 0.09 ppm and 3 ppm (at 100 MPa) in the experiment with CH₃COOH and HNO₃, respectively. The Cr ion concentration increased with the O₂ concentration and pressure; the maximum value of the concentration was about 0.5 ppm. The Cr ion concentration was lower than 0.01 ppm in the experiment with CH₃COOH, while the concentration was considerably higher in the experiment with HNO₃: the concentration increased with pressure up to 0.87 ppm at 100 MPa. The effect of pressure on the corrosion behavior of Inconel 625 was discussed using potential-pH diagrams, metal oxide solubilities, pH, and equilibrium of ionic reactions. Pressure dependence of the metal ion concentrations was analyzed using a model with water density as a parameter; the log–log plots revealed a linear relationship.     

Influence of TiO2 additive on sintering temperature and microwave dielectric properties of Mg0.90Ni0.1SiO3 ceramics

(1-x)Mg_0.90Ni_0.1SiO₃-xTiO₂ (x = 0, 0.01, 0.03, 0.05) ceramics were successfully formed by the conventional solid-state methods and characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDS), and their microstructure and microwave dielectric properties systematically investigated. It was observed that when TiO₂ content increased from 0 to 5 wt%, the Q_uf_o of the sample decreased from 118,702 GHz to 101,307 GHz and increases the τ_f value from −10 ppm/°C to +3.14 ppm/°C accompanied by a notable lowering in the sintering temperature (125 °C). A good combination of microwave dielectric properties (ε_r ∼ 8.29, Q_uf_o ∼ 101,307 GHz and τ_f ∼ −2.98 ppm/°C) were achieved for Mg_0.90Ni_0.1SiO₃ containing 3 wt% of TiO₂ sintered at 1300 °C for 9 h which make this material of possible interest for millimeter wave applications.     

A novel CO and C3H8 sensor made of CuSb2O6 nanoparticles

Trirutile-type CuSb₂O₆ nanoparticles were synthesized by a simple and economical route, starting from copper nitrate, antimony chloride, ethylenediamine, and ethyl alcohol as solvent. The latter was evaporated by microwave radiation at 140 W. The precursor material was calcined at 200, 300, 400, 500, and 600 °C, and analyzed by powder XRD. The oxide phase was obtained at the last calcination step (600 °C), whose powders were analyzed by field-emission scanning electron (FE-SEM) and transmission electron (TEM) microscopies. Microrods, hexagonal microplates, and nanoparticles with an average size of ~ 51.2 nm were observed. A forbidden bandwidth of 3.41 eV was detected for the direct transition with UV–vis. Tests were carried out on pellets made of the powders in carbon monoxide (CO) and propane (C₃H₈) atmospheres at different concentrations and operating temperatures, obtaining high response at 300 ppm of CO and 500 ppm of C₃H₈, both at 300 °C.     

Preparation and characterization of the one-piece wall ceramic board by using solid wastes

For the purpose of building energy-saving, a novel one-piece wall ceramic board was prepared by using fly ash and ceramic waste as the main raw materials for its matrix part and foam part, respectively. The effects of raw material composition, sintering temperature on the macro and micro properties were systematically investigated. The optimum parameter for the matrix part was obtained at 1220 °C with 70 wt% fly ash and 4 wt% quartz, while that for the foam part was 1220 °C with 97 wt% ceramic waste and 3 wt% silicon carbide. For the matrix sample, the highest rupture modulus reaches 53.97 MPa, and the corresponding water absorption capacity and thermal conductivity are 1.08% and 0.54396 W/(m K), respectively. For the foam part, the best bulk density and thermal conductivity are 443 kg/m³ and 0.10528 W/(m K), respectively. Subsequently, the optimal matrix and foam samples were introduced into the co-fired process (1220 °C), and the results show that the new method for the preparation of one-piece wall ceramic board was fully acceptable. Furthermore, the simulated results indicate that the proposed one-piece wall ceramic board can efficiently reduce the thermal bridges and exerts excellent energy conservation effect.     

Fabrication and microstructure of in situ vanadium carbide ceramic particulates-reinforced iron matrix composites

In this work, a novel process that combines infiltration casting with subsequent heat treatment was applied to fabricate in situ vanadium carbide (V₈C₇) ceramic particulates-reinforced iron matrix composites. Based on the differential scanning calorimetry (DSC) data, the as-cast samples were subjected to heat treatment at 1164 °C for different dwelling times (0, 10, 15, and 20 min). The effects of different heat treatment times on the phase evolution, microstructure, and microhardness of the as-prepared composites were investigated using X-ray diffraction (XRD), scanning electron microscope (SEM), energy dispersive X-ray spectrometer (EDS), and Vickers hardness tester, respectively. The experimental results revealed that only graphite, α-Fe, and V₈C₇ phases dominate in the composite samples after heat treatment at 1164 °C for 20 min. The average microhardness of the as-prepared composites varied among the different regions as follows: 458 HV_0.05 (vanadium wire), 1055 HV_0.05 (composite area), and 235 HV_0.05 (iron matrix). The microhardness of the composite region is four times higher than that of the iron matrix and two times higher than that of the vanadium wire because of the formation of the vanadium carbide phases (V₂C and V₈C₇) as reinforcement within the iron matrix.     

Microstructure and mechanical properties of B4C based ceramics with Fe3Al as sintering aid by spark plasma sintering

B₄C based ceramics were fabricated with different Fe₃Al contents as sintering aids by spark plasma sintering at relatively low temperature (1700 °C) in vacuum by applying 50 MPa pressure and held at 1700 °C for 5 min. The effect of Fe₃Al additions (from 0 to 9 wt%) on the microstructure and mechanical properties of B₄C has been studied. The composition and microstructure of as-prepared samples were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM) and electron probe microanalyzer (EPMA) equipped with WDS (wavelength dispersive spectrometry) and EDS. The mixtures of B₄C and Fe₃Al underwent a major reaction in which the metal borides and B₄C were encountered as major crystallographic phases. The sample with 7 wt% of Fe₃Al as a sintering aid was found to have 32.46 GPa Vickers hardness, 483.40 MPa flexural strength, and 4.1 MPa m^1/2 fracture toughness which is higher than that of pure B₄C.     

Synergetic effects of SiC and Csf in ZrB2-based ceramic composites. Part II: Grain growth

The synergetic effects SiC particles and short carbon fibers (C_sf) as well as hot pressing parameters (sintering temperature, dwell time and applied pressure) on the grain growth of ZrB₂-based composites were investigated. Taguchi methodology was employed for the design of experiments to study the microstructure and grain growth of ZrB₂–SiC–C_sf ceramic composites. Three hot pressing parameters and SiC/C_sf ratio were selected as the scrutinized variables. The sintering temperature and SiC/C_sf ratio were identified by ANOVA as the most effective variables on the gain growth of ZrB₂-based samples. Removal of oxide impurities from the surface of starting particles by the reactant C_sf, not only hindered the extraordinary grain growth of ZrB₂ matrix, but also improved the sinterability of the ceramics. A fully dense ceramic with an average grain size of 8.3 µm was obtained by hot pressing at 1850 °C for 30 min under 16 MPa through adding 20 vol% SiC and 10 vol% C_sf to the ZrB₂ matrix. SEM observations and EDS analysis verified the in-situ formation of ZrC which can restrain the growth of ZrB₂ particles, similar to the role of SiC, by the pinning of grain boundaries as another stationary secondary phase.     

The influence of silica nanoparticles addition on the physical,mechanical, thermo-mechanical as well as microstructure of Mag-Dol refractory composites

The high hydration potential of CaO and MgO phases restricted the application of Mag-Dol refractory composites. In this study, the impact of nano-silica (SiO₂) addition on the physical, mechanical, thermo-mechanical as well as microstructure of Mag-Dol refractory composites is investigated. Mag-Dol compositions were prepared by using calcined dolomite and magnesite particles (micron, 0–1, 1–3, 3–5, and 5–8 mm), liquid resin, and 0, 0.5, 1, 1.5, 2, and 2.5 wt% nano SiO₂ as additives. Specimens were heated up to 1650 °C for the 3 h soaking period. Fired specimens were characterized by physical (apparent porosity, bulk density, and hydration resistance), mechanical (cold crushing strength), and thermo-mechanical (flexural strength at 1200 °C) measurements. XRD and SEM/EDS analysis were done to study phases and microstructure analysis of the fired samples, respectively. Results showed that by adding up to 2.5 wt% nano-SiO₂, due to the formation of CaO·MgO·2SiO₂ (Diopside), 2CaO·MgO·2SiO₂ (Akermanite), and CaO·MgO·SiO₂ (Monticellite) phases, physical and mechanical properties were enhanced. But the highest flexural strength value is achieved for 1 wt% nano-SiO₂ containing sample.     

Improvements in microstructural and mechanical properties of ZrO2 ceramics after addition of BaO

The effects of the addition of BaO on the sinterability, phase balance, microstructure, and mechanical properties of 8 mol% yttria-stabilized cubic zirconia (8YSZ) were investigated using scanning electron microscopy, X-ray diffraction (XRD) analyses, and micro-hardness testing. The 8YSZ powder was doped with 0–15 wt% BaO using a colloidal process. The undoped and BaO-doped 8YSZ specimens were sintered at 1550 °C for 1 h. The XRD analyses results showed that the specimens doped with up to 1 wt% BaO did not exhibit BaO-related peaks, indicating that BaO was completely solubilized in the 8YSZ matrix. However, when more than 1 wt% BaO was added, BaZrO₃-related peaks appeared, suggesting that the overdoped BaO did not dissolve in the 8YSZ matrix but formed a secondary phase of BaZrO₃ at high temperatures. Grain size measurements showed that the grain size of 8YSZ decreased with an increase in the amount of BaO added. The decrease in the grain size was owing to the fact that the grains of BaZrO₃, which precipitated at the grain boundaries and grain junctions of 8YSZ, increased the grain boundary cohesive resistance because of the pinning effect. This resulted in a decrease in the grain boundary mobility, and an increase in the grain boundary energy. Furthermore, while the addition of BaO to 8YSZ caused a slight decrease in the hardness of 8YSZ, the fracture toughness of 8YSZ increased from 1.64 MPa m^1/2 to 2.08 MPa m^1/2, owing to the resulting decrease in the grain size.     

Chemical corrosion of basic refractories by cement kiln materials

The study of basic refractories corrosion by cement kiln materials was carried out with powder tests and coating tests at the typical temperature range of the sintered material in the transition zone and the sintering zone (1200–1450 °C). The tested basic refractories were magnesia-spinel (MSp) and magnesia–zirconia (MZ) refractory bricks. The industry cement kiln materials were rich of sulphur and chlorine. The microstructures of the as-delivered and tested samples were researched by XRD and SEM–EDS techniques. The new phases detected in the samples with MSp (with and without ZrO₂) bricks after tests at the temperature of 1200 °C were binary (C₁₂A₇ t_mp ? 1392 °C, CaZrO₃: t_mp ? 2345 °C)¹: and ternary (C₂AS: t_mp ? 1593 °C or C₃MS₂: t_dp ? 1573 °C) phases. After tests at the temperature of 1300 °C and higher, ternary phases of C₇A₃Z (t_mp ? 1550 °C) and CaZrO₃ and quaternary phases Q-C₂₀A₁₃M₃S₃ or C₆A₄(M,f)S (t_dp ? 1380 °C) were detected. The C₃A₃·CaSO₄ phase was formed in the samples after the corrosion tests performed up to the temperature of 1300 °C. The new phases formed in the sample with the MZ bricks were clinker phases (β-C₂S, C₃A and C₂(A,F)/C₄AF) and the C₇A₃Z phase.