Effect of SiC whiskers and graphene nanosheets on the mechanical properties of ZrB2-SiCw-Graphene ceramic composites

Ultrahigh temperature ZrB₂-SiC_w-Graphene ceramic composites are fabricated by hot pressing ZrB₂-SiC_w-Graphene oxide powders at 1950 °C and 30 MPa for 1 h. The microstructures of the composites are characterized by Scanning electron microscopy, Raman spectroscopy and X-ray diffraction. The results show that multilayer graphene nanosheets are achieved by thermal reduction of graphene oxide during sintering process. Compared with monolithic ZrB₂ materials, flexural strength and fracture toughness are both improved due to the synergistic effect of SiC whisker and graphene nanosheets. The toughening mechanisms mainly are the combination of SiC whisker and graphene nanosheets crack bridging, pulling out.     

Efficient multiscale strategy for toughening HfB2 ceramics: A heterogeneous ceramic–metal layered architecture

A multiscale structural design was innovatively adopted herein to increase the toughness of monolithic HfB₂ ceramics. SiC whiskers (SiC_w) and graphene oxide (GO) were used as fillers for the HfB₂ matrix, whereas a ductile W foil was introduced as an interlayer to synthesize laminated HfB₂-SiC_w-rGO/W ceramics. Monolithic HfB₂-SiC_p (particulate) and laminated HfB₂-SiC_p/W ceramics were prepared using the same routes and used as controls. Following tape casting and spark plasma sintering at 1800°C, the toughness of the prepared laminated HfB₂-SiC_w-rGO/W samples was increased to 14.2 ± 0.6 MPa·m^1/2, with minimal sacrifice in flexural strength (421 ± 16 MPa). Morphological analysis of the fracture surface revealed the synergistic effects of micro-toughening (including bridging and pullout of whiskers and rGO) and macro-toughening (including crack deflection, bifurcation, and delamination) mechanisms responsible for improving the fracture toughness of the laminated HfB₂-SiC_w-rGO/W composites.     

Fabrication of SiCw reinforced ZrB2-based ceramics

ZrB₂-based ceramics with SiC_w were produced by hot pressing at 1750 °C for 1 h from mixed powders after adding liquid polycarbosilane. The obtained ZrB₂-SiC_w composites had toughness up to 7.57 MPa m^1/2, which was much higher than those for monolithic ZrB₂, SiC particles reinforced ZrB₂ composites, and other ZrB₂–SiC_w composites directly sintered at high temperatures. The added liquid polycarbosilane could reduce the sintering temperatures and restrict the reaction of matrix with whisker, which led to fewer damages to the whisker and high fracture toughness.     

Mechanical properties and microstructure of Al2O3-SiCw ceramic tool material toughened by Si3N4 particles

Al₂O₃-SiC_w toughened ceramic tools play vital role in high-speed machining of nickel-based superalloys due to their superior mechanical properties. Herein, owing to synergistic toughening mechanism, α-Si₃N₄ particles are employed as reinforcement phase into Al₂O₃-SiC_w ceramic composite to optimize mechanical properties of Al₂O₃-SiC_w ceramic tools. Moreover, the influence of Si₃N₄ content and sintering parameters on microstructure and mechanical properties of Al₂O₃-20 vol%SiC_w ceramic tool material is systematically investigated. Results reveal that appropriate amount of Si₃N₄ particles is required to effectively increase the density of Al₂O₃-SiC_w ceramic composites. The presence of Si₃N₄ particles leads to formation of novel β-sialon phase during hot-press sintering, which effectively enhances fracture toughness and flexural strength of Al₂O₃-SiC_w ceramic composites. It is observed that grain size of newly formed β-sialon phase is extremely sensitive to hot-pressing sintering conditions. The degree of chemical transformation of α-Si₃N₄ into Si_6-zAl_zO_zN_8-z (β-sialon) and z-value of Si_6-zAl_zO_zN_8-z are significantly influenced by sintering temperature. Overall, Al₂O₃-20 vol%SiC_w-15 vol%Si₃N₄ ceramic tool material, with 1.5 vol%Y₂O₃-0.5 vol%La₂O₃-0.5 vol%CeO₂ (YLC) sintering additive, rendered optimal mechanical properties after sintering at 1600 °C under 32 MPa for 30 min. Improved mechanical performance can be ascribed to synergistic toughening and strengthening influence of whiskers and particles.     

Green synthesis of blue-green photoluminescent β-SiC nanowires with core-shell structure using coconut shell as carbon source

This work proposes a green method for synthesizing SiC nanowires (NWs) via the chemical vapor deposition (CVD) technique using coconut shell and silicon as raw materials. Using coconut shell as carbon source decreases the synthesis temperature of SiC. A large number of core-shell SiC NWs were obtained after firing at 1200 °C, a thin SiO₂ layer is distributed on the outer shell of SiC NWs. The synthesized SiC NWs grow along the [111] direction, up to dozens of micrometers in length and diameters of 10–75 nm. However, the chain-bead structure of SiC NWs is formed after firing at 1400 °C due to the SiO₂ bead embedded in SiC NWs. The synthesized core-shell SiC NWs fired at 1200 °C emit strong violet-blue light, which has good application prospects in optoelectronic devices.     

Bonding strength and thermal shock resistance of a novel bilayer (c-AlPO4-SiCw-mullite)/SiC coated carbon fiber reinforced CMCs

Mullite coating, SiC whiskers toughened mullite coating (SiC_w-mullite), and cristobalite aluminum phosphate (c-AlPO₄) particle modified SiC_w-mullite coating (c-AlPO₄-SiC_w-mullite) were prepared on SiC coated C/SiC composites using a novel sol-gel method combined with air spraying. Results show that molten SiO₂ formed by the oxidation of SiC whiskers and molten c-AlPO₄ improved the bonding strength between mullite outer coating and SiC–C/SiC composites due to their high-temperature bonding properties. The bonding strength between mullite, SiC_w-mullite, c-AlPO₄-SiC_w-mullite outer coatings and SiC–C/SiC composites were 2.41, 4.31, and 7.38 MPa, respectively. After 48 thermal cycles between 1773 K and room temperature, the weight loss of mullite/SiC coating coated C/SiC composites was up to 11.61%, while the weight losses of SiC_w-mullite/SiC and c-AlPO₄-SiC_w-mullite/SiC coatings coated C/SiC composites were reduced to 7.40% and 5.12%, respectively. The addition of appropriate SiC whiskers can considerably improve the thermal shock resistance of mullite coating owing to their excellent mechanical properties at high temperature. In addition, c-AlPO₄ particles can further improve the thermal shock resistance of SiC_w-mullite coating due to their high-temperature bonding and sealing properties. No obvious micro-pores and cracks were observed on the surface of c-AlPO₄-SiC_w-mullite coating after 48 thermal cycles due to timely healing effect by formation of secondary mullite.     

Preparation and mechanical properties of the 2.5D ASf/ZrO2 composites after high-temperature heat treatment

In the paper, the aluminosilicate fiber-reinforced zirconia (AS_f/ZrO₂) ceramic composites were successfully fabricated by polymer impregnation and pyrolysis (PIP) method. The microstructure and high-temperature mechanical properties of the original composites were well studied. The results revealed that the composites could maintain the stability of microstructure at 1000 °C. The flexural strength increased from 58.82 ± 2.83 MPa to 88.74 ± 6.20 MPa and the flexural modulus increased from 29.26 ± 4.67 GPa to 40.76 ± 8.76 GPa. The thermal exposure improved the interfacial bonding and made the load transfer more effective. After heat treatment from 1200 °C to 1400 °C, the flexural strength gradually declined due to the crystallization of the AS fibers and ZrO₂ matrix, while the flexural modulus increased in a completely different trend. After heat treatment at 1400 °C, the composites could maintain a flexural strength of 66.95 ± 4.24 MPa with a flexural modulus of 60.42 ± 7.25 GPa. But the fracture mode gradually evolved to brittleness.     

Controlled sintering and phase transformation of yttria-doped tetragonal zirconia polycrystal material

In this paper, 3 mol% yttria-doped tetragonal zirconia polycrystal material (3 mol% Y₂O₃–ZrO₂) was prepared using an optimised pressureless sintering process. The phase change and particle size distribution of Y₂O₃–ZrO₂ during sintering were studied, and the effect of sintering temperature on the properties of Y₂O₃–ZrO₂ was analysed. The raw materials and prepared samples were analysed using XRD, Raman spectroscopy, SEM, and Gaussian mathematical fitting. The results show that sintering encourages the transformation of the monoclinic phase into the tetragonal phase, thus improving the crystallinity of the sample. The relative content of the tetragonal phase in the sample increased from 57.43% to 99.80% after sintering at 1200 °C for 1 h. In the range of sintering temperatures studied in this paper (800–1200 °C), the zirconia material sintered at 1000 °C presented the lowest porosity and the best density.     

Crack tolerant silicon carbide ceramics prepared by liquid-phase assisted oscillatory pressure sintering

Silicon carbide ceramics were prepared by liquid-phase assisted oscillatory pressure sintering (OPS) with graphene and in-situ synthesized SiC whisker as the reinforcements. The effects of sintering temperature on the densification, morphology and mechanical performances of the SiC_p-SiC_w-graphene ceramics were investigated. In the temperature range from 1700 to 1800 °C, the densification rate of SiC_p-SiC_w-graphene ceramics was accelerated, ascribing to the reduction in viscosity of the glassy phase. At 1800 °C, the flexural strength and fracture toughness of the OPS ceramics corresponded to 697 MPa and 5.8 MPa m^1/2, respectively, which were higher than that of the hot-pressed ceramics under the same temperature conditions. Multiphase toughening mechanisms, such as whisker bridging and pullout, graphene bridging and delamination, were considered as the primary mechanisms. This work demonstrates an effective strategy to prepare silicon carbide ceramics at low sintering temperature.     

High-surface-area mesoporous silica-yttria-zirconia ceramic materials prepared by coprecipitation method ― the role of silicon

A high surface area is one of desired properties for yttria-zirconia (Y₂O₃–ZrO₂) ceramic materials given their catalytic applications. The objective of this study is to develop high-surface-area Y₂O₃–ZrO₂ materials by silicon (Si) modification and investigate the role of Si. Si-modified yttrium-zirconium hydroxides were prepared via a one-step precipitation process and calcined at 800 or 950 °C to form Si-modified Y₂O₃–ZrO₂ (denoted as SiO₂–Y₂O₃–ZrO₂) materials containing 0-20 wt% Si as SiO₂. These hydroxides or materials were characterized by ²⁹Si NMR, XPS, TG-DSC, XRD, UV Raman, TEM, and N₂ physisorption measurements. Si species uniformly distributed in the hydroxides tended to be enriched on the material surface at high temperatures. These Si species dominated by the silicates blocked the migration of Y and Zr atoms, which resisted the crystallite growth of Y₂O₃–ZrO₂ components and reduced their crystallite size. Therefore, the SiO₂–Y₂O₃–ZrO₂ possessed a surface area of 59-112 m²/g after calcination at 950 °C for 9 h, which was significantly higher than that of the Y₂O₃–ZrO₂ (23 m²/g). This study may stimulate ideas for developing high-surface-area crystalline ceramic materials calcined at high temperatures.     

Preceramic paper-derived Ti3Al(Si)C2-based composites obtained by spark plasma sintering

The paper describes the structure and properties of preceramic paper-derived Ti₃Al(Si)C₂-based composites fabricated by spark plasma sintering. The effect of sintering temperature and pressure on microstructure and mechanical properties of the composites was studied. The microstructure and phase composition were analyzed by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. It was found that at 1150 °C the sintering of materials with the MAX-phase content above 84 vol% leads to nearly dense composites. The partial decomposition of the Ti₃Al(Si)C₂ phase becomes stronger with the temperature increase from 1150 to 1350 °C. In this case, composite materials with more than 20 vol% of TiC were obtained. The paper-derived Ti₃Al(Si)C₂-based composites with the flexural strength > 900 MPa and fracture toughness of >5 MPa m^1/2 were sintered at 1150 °C. The high values of flexural strength were attributed to fine microstructure and strengthening effect by secondary TiC and Al₂O₃ phases. The flexural strength and fracture toughness decrease with increase of the sintering temperature that is caused by phase composition and porosity of the composites. The hardness of composites increases from ~9.7 GPa (at 1150 °C) to ~11.2 GPa (at 1350 °C) due to higher content of TiC and Al₂O₃ phases.     

Fabrication of in situ elongated β-Sialon grains bonded to tungsten carbide via two-step spark plasma sintering

In order to reduce the difficulty of preparing binder-less cemented carbide and further broaden its application prospects, tungsten carbide toughened by in situ elongated β-Sialon grains was developed via sintering ball-milled WC and α-Si₃N₄ powders using Al₂O₃–ZrO₂ as a sintering aid and transformation additive. The two-step spark plasma sintering of the mixture at 1650 °C with dwelling at 1500 °C for 10 min was conducted under 30 MPa uniaxial pressure, and the densification behaviors, phase transformations, mechanical properties, and microstructures of the produced composites were investigated. The addition of Al₂O₃–ZrO₂ reduced the initial temperature of the densification process by approximately 100 °C and its final temperature by 200 °C (compared with the densification temperatures of pure WC and Si₃N₄ materials) and fully transformed α-Si₃N₄ to Sialon (Si–Al–O–N) phases. Microstructural characterization data showed that the WC matrix contained homogeneously distributed equiaxed and elongated β-Si₅AlON₇ grains. The WC composites containing in situ elongated β-Sialon grains exhibited an optimal hardness of 18.93 ± 0.03 GPa and enhanced fracture toughness of 10.43 ± 0.27 MPa m^1/2. The toughening mechanism of the β-Sialon phase involved the pull-out of elongated grains and crack bridging.     

Investigation of the electrical conductivity of sintered monoclinic zirconia (ZrO2)

High-density monoclinic ZrO₂ was manufactured through sintering at ~1200 °C by using nanosized powders. Then, the electrical conductivity was measured at a range of high temperatures (700–900 °C) by electrical impedance spectroscopy (EIS). For the as-sintered monoclinic ZrO₂, the measured electrical conductivity was 3.2×10⁻⁵ s/cm (for 80% TD) and 4.4×10⁻⁵ s/cm (for 89% TD) at 900 °C. After aging at 900 °C for 100 h, the electrical conductivity of the monoclinic ZrO₂ of 80%-TD decreased by more than 50%. However, after reheating at 1200 °C for 1 h, approximately 80% of the conductivity was recovered compared to the value of the as-sintered monoclinic ZrO₂. The pure monoclinic crystal structure was retained despite the aging and reheating treatment. Based on microstructural observations of the aged and reheated monoclinic ZrO₂, the changes in electrical conductivity after aging and reheating were explained by the formation and recovery of micro-cracks, respectively.     

In situ reactive spark plasma sintering of WSi2/MoSi2 composites

MoSi₂ based materials have the potential for use in high temperature structural parts. In this work, WSi₂ reinforced MoSi₂ composites were successfully prepared by mechanical activation followed by in situ reactive spark plasma sintering of Mo, Si, and W elemental powders. Benefiting from the high energy raw materials prepared through ball milling, these mechanically activated reactants started to transform into MoSi₂ at 1000 °C. Full density composites were obtained at a low sintering temperature (1200 °C) within 5 min. The addition of W to the reactants led to a finer microstructure than that obtained using pure MoSi₂, resulting in a significant improvement of mechanical properties. The Vicker's hardness of 20 vol% WSi₂/MoSi₂ was as high as 16.47 GPa.     

Reaction mechanisms and properties of in situ porous Al2O3-ZrO2-mullite composites

Customized porous Al₂O₃-ZrO₂-mullite composites were designed and prepared by reaction sintering of zircon (ZrSiO₄) and alumina (Al₂O₃) at sintering temperatures from 1400 to 1600 °C for 3 h. The mechanical properties, microstructural evolution, and reaction mechanisms of the composites were investigated. The reactions between ZrSiO₄ and Al₂O₃ were studied by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectrometer (EDS). The results indicate that ZrSiO₄ and Al₂O₃ react and form ZrO₂ and mullite. Sintering temperature has an important effect on the reaction process. At 1400 °C, Al₂O₃ reacts directly with SiO₂ of ZrSiO₄ to form mullite and ZrO₂, which reduces the decomposition temperature of ZrSiO₄ and promotes the decomposition of ZrSiO₄. However, at 1600 °C, ZrSiO₄ first decomposes to form SiO₂ and ZrO₂, and then generates mullite by the diffusion of Si. The migration of Si is the key factor for the formation of mullite. The thermal shock resistance of the composites can be significantly improved by phase transformation toughening of in-situ ZrO₂. Therefore, increasing the proportion of ZrSiO₄ can significantly improve the mechanical properties of sample. The residual ratio of the flexural strength after thermal shock exceeded 90%, when the mass ratio of ZrSiO₄ to Al₂O₃ was 3:1. Besides, the addition of polymethyl methacrylate could improve the porosity of materials and has a direct effect on the thermal conductivity of composites.     

The influence of MgO,Y2O3 and ZrO2 additions on densification and grain growth of submicrometre alumina sintered by SPS and HIP

Spark plasma sintering followed by hot isostatic pressing was applied for preparation of polycrystalline alumina with submicron grain size. The effect of additives known to influence both densification and grain growth of alumina, such as MgO, ZrO₂ and Y₂O₃ on microstructure development was studied. In the reference undoped alumina the SPS resulted in some microstructure refinement in comparison to conventionally sintered materials. Relative density >99% was achieved at temperatures >1200 °C, but high temperatures led to rapid grain growth. Addition of 500 ppm of MgO, ZrO₂ and Y₂O₃ led, under the same sintering conditions, to microstructure refinement, but inhibited densification. Doped materials with mean grain size <400 nm were prepared, but the relative density did not exceed 97.9%. Subsequent hot isostatic pressing (HIP) at 1200 and 1250 °C led to quick attainment of full density followed by rapid grain growth. The temperature of 1250 °C was required for complete densification of Y₂O₃ and ZrO₂-doped polycrystalline alumina by HIP (relative density >99.8%), and resulted in fully dense opaque materials with mean grain size<500 nm.     

High compressive strength in nacre-inspired Al−7Si−5Cu/Al2O3–ZrO2 composites at room and elevated temperatures by regulating interfacial reaction

Al−7Si−5Cu/Al₂O₃−ZrO₂ composites with nacre-like structures were prepared via ice-templating and gas pressure infiltration techniques. The composites were subsequently heat-treated at 850 °C for 0, 30, 60, 90 and 120 min to regulate the interfacial reaction between Al and ZrO₂. The yield of larger (Al_1−m, Si_m)₃Zr and ZrSi₂ phases increased with longer dwell times. The compressive strength initially increased and then decreased. The highest strength was observed in composites treated for 60 min and reached 1600±40, 1261±30 and 1033±22 MPa at temperatures of 20, 150 and 300 °C, respectively. These values increased by 30−40% as compared to those of the non-treated counterparts and were 2-, 5- and 12-fold more than those of the matrix alloy, respectively, which is demonstrative of the material's excellent load-bearing capacity, particularly at elevated temperatures.     

Phase formation in Al2O3-C refractories with Al addition

Depending on the recipe and the firing conditions, several non-oxides can be formed in Al₂O₃-C refractories. In this paper, the effect of the purity of the recipe components on the phase formation in Al₂O₃-C refractories with Al addition was investigated. Two test series were sintered from 800 °C to 1600 °C under air embedded in coke breeze. One test series was with brown fused alumina, and the other was with tabular alumina. At temperatures of up to 1200 °C the phase formation was the same for both recipes. For temperatures greater than 1400 °C, the impurities of brown fused alumina enhanced the formation of a polytype, while Al₄O₄C and Al₂₈O₂₁C₆N₆ were formed in the other series. The findings explain the occurrence of several non-oxides in disequilibrium at the chosen temperatures. The occurrence of Al₄C₃ was of particular interest due to its low hydration resistance. It was formed at 1200 °C.     

Enhanced nitridation of silicon compacts by Yb2O3 addition

The catalytic effect of ytterbium oxide (Yb₂O₃) on the nitriding reaction of Si compacts was investigated. Si powder mixtures containing Yb₂O₃ were prepared and nitrided in the form of compacts with a multi-step heating schedule over the range of 1200 °C–1450 °C. The nitriding profiles of the powder mixture with increasing temperature indicated that Yb₂O₃ clearly promoted the nitridation of Si compacts at 1200 °C compared with the pure Si compact containing no additives. The critical role of Yb₂O₃ on the nitridation of Si, was elucidated that Yb₂O₃ promotes the loss of initial SiO₂ of the raw Si powder via the measurement of the weight changes at low temperature (1100 °C) and thermogravimetric analysis under N₂ atmosphere. It was also found that the β-ratio of fully nitrided Si was closely related to the intermediate degree of nitridation at 1200 °C and 1300 °C.     

High-temperature water-vapor reaction mechanism of barium strontium aluminosilicate (BSAS)

Environmental barrier coatings (EBCs) are used in commercial turbine engine applications as protection for ceramic matrix composites, yet the high-temperature water vapor reaction mechanism for EBC materials is not fully understood. Here, the water vapor reaction mechanism for barium strontium alumino-silicate (BSAS), an early generation EBC candidate, was determined from the time and temperature dependences of material loss. BSAS water vapor exposures were performed at 1200 °C, 1300 °C, and 1400 °C for 24, 48, and 72 h, at maximum gas velocities of ~ 240 m/s. FactSage thermodynamic calculations were shown to support the experimental findings, where the steam reaction mechanism consisted of volatilization of all BSAS oxide constituents as gaseous metal hydroxide species, i.e. Ba(OH)₂, Sr(OH)₂, Al(OH)₃, and Si(OH)₄ (g).