The preparation of mullite foamed ceramics reinforced by in-situ SiC whiskers and their reinforcement mechanism

A SiC whisker-bonded mullite foamed ceramic was prepared by using white clay, industrial alumina and silicon powder as raw materials without solid carbon sources. The XRD, SEM, EDS, and Factsage® software were used to investigate the effect of sintering temperature on the phase composition, microstructure, compressive strength, and Young's modulus of foamed ceramics. Additionally, the synthesis reaction of in-situ SiC whiskers and the effect of their formation on the properties of ceramics were studied. The results showed that the in-situ SiC whiskers with dendrite shapes were formed after firing above 1300 °C at the expense of Si/SiO vapors as well as CO vapor, though there were no solid carbon sources in raw materials, which provided a new idea for the synthesis of SiC whiskers. The formation of SiC whiskers was helpful for improving the compressive strength and Young's modulus of mullite foamed ceramics remarkably. Furthermore, the reinforcement mechanism has been investigated systematically.     

Fibrous porous mullite ceramics modified by mullite whiskers for thermal insulation and sound absorption

In order to meet the demand for thermal insulation and sound absorption, fibrous porous mullite ceramics (FPMC) with high porosity and an interconnected pore structure were prepared, followed by a pore structure modification with in situ grown mullite whiskers on the three-dimensional framework of the FPMC. The resultant hierarchical material exhibited superior sound absorption performance in the low-to-medium frequency to most reported sound-absorbing materials, as well as a sufficient compressive strength of 1.26 MPa with low thermal conductivity of 0.117 W·m^?1·K^?1. Moreover, the effects of solid content and mullite whiskers on the microstructure and physical properties of the material were analyzed. The increase of solid content led to increased compressive strength and thermal conductivity and decreased frequency corresponding to the first sound absorption peak. The thermal conductivity and compressive strength of the material increased as the mullite whiskers grew, while the median pore size decreased.     

Fabrication of in-situ self-reinforced Si3N4 ceramic foams for high-temperature thermal insulation by protein foaming method

To meet demand for lightweight and high-strength ceramic foams, in-situ self-reinforced Si₃N₄ ceramic foams, with compressive strength of 13.2–45.9 MPa, were fabricated by protein foaming method combined with sintered reaction-bonded method. For comparison, ordinary protein foamed ceramics with irregular block microstructure were fabricated via reaction-bonded method, which had compressive strength of 3.6–20.5 MPa. Physical properties of these two types of samples were systematically compared. When open porosity was about 80%, both types of Si₃N₄ ceramic foams had excellent thermal insulation properties (<0.15 W m^?1 K^?1), while compressive strength of in-situ self-reinforced samples increased by more than 158% compared with ordinary samples. Under high-temperature oxidation conditions, microstructures of both types of samples were deformed with increase in oxidation temperature. Moreover, after oxidation temperature was increased to 1400 °C, oxidation weight gain decreased from 18.07% for ordinary samples to only 2.18% for self-reinforced samples. Thus, high-temperature oxidation resistance of Si₃N₄ ceramic foams was greatly improved.     

Formation of SiC whiskers/leucite-based ceramic composites from low temperature hardening geopolymer

In this study, SiC whiskers (SCWS) reinforced geopolymer composites (SCWS/KGP) and their ceramic products (SCWS/leucite) were prepared, and effects of SiC whiskers contents on the microstructure and flexural strength of the SCWS/KGP and SCWS/leucite composites were investigated. The results show that the whisker addition has little influence on both phase composition and thermal shrinkage of the KGP composites, but a suitable content of whisker will result in the improved flexural strength, and when the SCWS content is 2 wt%, flexural strength of the SCWS/KGP composite is enhanced by 95% compared with the neat geopolymer. The flexural strength of the composites can be further enhanced significantly after the composites being treated at 1100 °C and 1200 °C and flexural strength of the composite with SCWS content of 2 wt% was 107% and 125% higher than the untreated counterpart, respectively. The increase in flexural strength of the composites should be attributed to the strong leucite formation, whisker debonding and pulling out from matrix during the fracturing process based on the good interfacial bonding state between whisker and leucite matrix.     

Preparation and characterization of mullite microspheres based porous ceramics with enhancement of in-situ mullite whiskers

High-strength insulating ceramic materials were prepared using lightweight mullite microspheres with dense surfaces and high internal porosity as the main raw material and silica sol as a binder. The effects of AlF₃·3H₂O content on the in situ formation and growth of mullite whiskers were analyzed by X-ray diffraction and scanning electron microscopy. The obtained results showed that mullite whiskers were formed in large quantities at 1200 °C using AlF₃·3H₂O and V₂O₅ as additives; their optimal growth was observed at 4 wt% AlF₃·3H₂O and 1 wt% V₂O₅. The apparent porosity of the produced specimens was 39%; the MOR and CCS of the specimens were 31 and 152 MPa, respectively; the HMOR at 1300 °C was 11.32 MPa; and the thermal conductivity at 900 °C was 0.783 W m⁻¹ K⁻¹. The staggered whisker network structure formed between mullite microspheres not only improved the mechanical properties of the material, but also refined its pore size, reduced the thermal conductivity, and enhanced the thermal insulation properties.     

Constructing secondary-pore structure by in-situ synthesized mullite whiskers to prepare whiskers aerogels with ultralow thermal conductivity

Ultralow thermal conductivity and ultralight mullite fibers/mullite whiskers composite aerogels (MF/MW) with secondary-pore structure have been prepared via vacuum impregnation and high-temperature treatment. The in-situ generation of mullite whiskers during vapour-solid reaction process and the mechanism of improving thermal stability have been discussed in detail. Under catalysis condition at 1200 °C, the zero-dimensional nanoparticles of SiO₂-Al₂O₃ aerogels are guided to in-situ transform into one-dimensional mullite whiskers. The secondary-pore structure formed by the overlapped fibers and whiskers in MF/MW reduces the thermal conductivity [as low as 0.0488 W/m^?1 K^?1 compared with that of MF preform (0.0698 W/m^?1 K^?1)] and exhibits excellent thermal stability after 1400 °C heat treatment (0.0503 W/m^?1 K^?1) due to the macropores are decreased and gaseous heat transfer being further weakened effectively. Moreover, the MF/MW exhibits good mechanical performance with high critical compressive stress of 0.2809 MPa, which is more than 317% higher than that of MF preform (0.0673 MPa) at room temperature.     

Polymer-derived SiC ceramic aerogels with in-situ growth of SiC nanowires

Herein, the SiC ceramic aerogels with in-situ growth of SiC nanowires (SiC_w/SiC CAs) have been synthesized by polymer‐derived ceramics (PDCs) method. The morphology, microstructure, and phase composition of the as-prepared samples were systematically investigated through SEM, XRD, TEM, Raman spectrum, FT-IR spectrum, and XPS spectrum techniques. The results showed that the as-obtained SiC_w has a diameter of about 80 nm and a length of 1–3.5 μm. In addition, the formation mechanism and evolution process of growth SiC_w were systematically studied using a VLS growth mechanisms. The way in this work could be expanded to synthesize other Si-based porous ceramic aerogel nanostructed with nanowires.     

Multifunction properties of SiOC reinforced with carbon fiber and in-situ SiC nanowires

Herein, the SiC nanowires were successfully fabricated via chemical vapor infiltration (CVI) into carbon fiber felts (CFs) and then the SiOC/SiCnws/CFs composites were synthesized by precursor infiltration and pyrolysis (PIP) processes. Results indicated that the lightweight composites possessed enhanced mechanical performance, low thermal conductivity, and excellent electromagnetic wave absorption properties. Detailedly, the compressive strength reached to 22.0 MPa and 9.6 MPa after two PIP processes cycles in z and x/y directions, respectively. Meanwhile, the composites exhibited tailored electromagnetic wave absorption performance with the effective absorption bandwidth of 3.06 GHz, and the minimum reflection loss (RL_min) was -48.2 dB with a thickness of 3.6 mm. The present work has a guidance to prepare and design multifunction properties for application in harsh environment.     

In-situ growth of mullite whiskers and their effect on the microstructure and properties of porous mullite ceramics with an open/closed pore structure

Porous mullite ceramics with an open/closed pore structure were prepared by protein foaming method combined with fly ash hollow spheres. Both the open porosity and total porosity of samples were enhanced by increasing the hollow sphere content. Mullite whiskers with a diameter of 0.2–4 μm were grown in-situ in the porous mullite ceramics with an AlF₃ catalyst, conforming to a vapor-solid growth mechanism. The pore structure of the porous mullite ceramics was significantly affected by the mullite whiskers which increased the open porosity and total porosity. Moreover, the median pore size was reduced from 65.05 μm to 36.92 μm after the introduction of mullite whiskers. The flexural strength and the thermal conductivity of the samples decreased with increasing total porosity. The porosity dependence of the thermal conductivity was well described by the universal model, providing a reference for the prediction of thermal conductivity of porous ceramics with open/closed pores.     

Synthesis of SiC whiskers by VLS and VS process

This study investigates the mechanisms of SiC whisker formation in the carbothermal reduction of quartz to SiC in different gas atmospheres. Reduction of quartz by graphite was studied in Ar, H₂, and CH₄–H₂–Ar gas mixture in a laboratory fixed bed reactor. The reduction products were characterised by XRD, SEM and TEM. Whiskers were not formed in the carbothermal reduction of quartz in argon. Two types of SiC whiskers were observed in the carbothermal reduction of quartz in H₂ and CH₄–H₂–Ar gas mixture. In the process of reduction at 1400–1600 °C in H₂ and at 1200–1600 °C in CH₄–H₂–Ar gas mixture, whiskers with hexagonal shape with diameter 100–800 nm and length up to tens of microns were formed by the VLS mechanism under catalytic effect of iron. The whiskers with the characteristics of cylindrical shape and high aspect ratio were synthesized in CH₄–H₂–Ar gas mixture at 1400–1600 °C by VS mechanism.     

Processing and properties of silica-bonded porous nano-SiC ceramics with extremely low thermal conductivity

Silica-bonded porous nano-SiC ceramics with extremely low thermal conductivity were prepared by sintering nano-SiC powder-carbon black template compacts at 600–1200 °C for 2 h in air. The microstructure of the silica-bonded porous nano-SiC ceramics consisted of SiC core/silica shell particles, a silica bonding phase, and hierarchical (meso/macro) pores. The porosity and thermal conductivity of the silica-bonded porous nano-SiC ceramics can be controlled in the ranges of 8.5–70.2 % and 0.057–2.575 Wm⁻¹ K⁻¹, respectively, by adjusting both, the sintering temperature and template content. Silica-bonded porous nano-SiC ceramics with extremely low thermal conductivity (0.057 Wm⁻¹ K⁻¹) were developed at a very low processing temperature (600 °C). The typical porosity, average pore size, compressive strength, and specific compressive strength of the porous nano-SiC ceramics were ∼70 %, 50 nm, 2.5 MPa, and 2.7 MPa·cm³/g, respectively. The silica-bonded porous nano-SiC ceramics were thermally stable up to 1000 °C in both air and argon atmospheres.     

Oxidation protection and mechanism of the HfB2-SiC-Si/SiC coatings modified by in-situ strengthening of SiC whiskers for C/C composites

To improve the oxidation resistance and alleviate the thermal stress of the HfB₂-SiC-Si/SiC coatings for C/C composites, in-situ formed SiC whiskers (SiC_w) were introduced into the HfB₂-SiC-Si/SiC coatings via chemical vapor deposition (CVD). Effects of SiC_w on isothermal oxidation and thermal shock resistance for the HfB₂-SiC-Si/SiC coatings were investigated. Results showed that the SiC_w-HfB₂-SiC-Si/SiC coatings exhibited excellent oxidation resistance for C/C composites with only 0.88% weight loss after oxidation for 468?h at 1500?°C, which was markedly superior to 4.86% weight loss for coatings without SiC_w. Meanwhile, after 50 times thermal cycling, the weight loss of the SiC_w-HfB₂-SiC-Si/SiC coated samples was 4.48%, which showed an obvious decrease compared with that of the HfB₂-SiC-Si/SiC coated samples. The SiC_w-HfB₂-SiC-Si/SiC coatings exhibited excellent adhesion to the C/C substrate and had no penetrating cracks after oxidation. The improved performance of the SiC_w-HfB₂-SiC-Si/SiC coatings could be ascribed to the SiC_w, which effectively relieved CTE mismatch and remarkably suppressed the cracks through toughening mechanisms including whiskers pull-out and bridging strengthening. The above results were confirmed by thermal analysis based on the finite element method, which demonstrated that SiC_w could effectively alleviate thermal stress generated by temperature variation. Furthermore, the SiC_w-HfB₂-SiC-Si/SiC coating can provide a promising fail-safe mechanism during the high temperature oxidation by the formation of HfSiO₄ and SiO₂, which can deflect cracks and heal imperfections.     

Theoretical design and preparation of SiC whiskers catalyzed by Fe-oxides on carbon fibers

This work reported an in-situ vapor-liquid-solid (VLS) preparation method of SiC whiskers (SiC_w) catalyzed by Fe-oxides on carbon fibers, which could provide a method for preparing SiC_w/carbon fiber composites. The mechanism of the SiC_w was theoretically designed and then experimentally validated using XRD, SEM, and TEM. Fe₂O₃ was chosen as a Fe-oxide catalyst and directly loaded on carbon fibers by the impregnation process. The results showed that SiC_w were successfully prepared on carbon fibers at 1600 °C under the protection of flowing nitrogen, utilizing quartz and graphite as gas-phase generation sources. The prepared SiC_w were β-SiC and grew along the (111) crystal plane, with spherical droplets on top formed by Fe₂O₃ catalysts. SiC_w were microstructurally observed to have widths of 500–1000 nm and lengths of more than 15 μm, respectively.     

Preparation,characterization, and physicomechanical properties of glass-ceramic foams based on alkali-activation and sintering of zeolite-poor rock and eggshell

This study reports the fabrication of novel glass-ceramic foams for thermal insulation to minimize the energy consumption in the buildings. Different combinations of zeolite-poor rock/eggshell powders (with eggshell content varying from 0 to 20 wt%) have been used to produce the foams through alkali-activation and reactive sintering techniques. The produced glass-ceramic foams were characterized based on their structural, thermal, and mechanical characteristics. The heat treatment process and the foaming patterns are examined by a heating microscope, and the findings reveal an excellent foamability of the utilized alkali-activated mixture in the range of 800–950 °C. The microstructure and the pore size of the acquired foams are investigated using a scanning electron microscope (SEM) and computed tomography (CT) analysis. The crystallinity and phase composition of the prepared samples were investigated via X-ray diffraction (XRD). The experiment findings reveal that raising the eggshell content is favorable to gas production, but it affects the liquid phase creation resulting in inconsistent pore size distribution. The appropriate eggshell content is 4%, and the optimal heat treatment temperature is 900 °C. The produced ceramic foams possess a density ranging from 0.54 to 1 g/cm³, thermal conductivity around 0.07–0.4 W/mK, and compressive strength values between 1.2 and 6.7 MPa. The results indicate that the ceramic foams created could be a feasible choice for applications in constriction as thermal insulation materials.     

Fabrication and mechanical properties of carbon fibers/lithium aluminosilicate ceramic matrix composites reinforced by in-situ growth SiC nanowires

To improve the mechanical properties of carbon fibers/lithium aluminosilicate (C_f/LAS) composites, C_f/LAS with in-situ grown SiC nanowires (SiC_nw-C_f/LAS) were prepared by chemical vapor phase reaction, precursor impregnation, and hot press sintering, consecutively. The effect of multi-scaled reinforcements (micro-scaled C_f and nano-scaled SiC_nw) on the mechanical properties was investigated. The phase composition, microstructure and fracture surface of the composites were characterized by XRD, Raman Spectrum, SEM, and TEM. The morphology of SiC_nw has a close relation with the content of Si. Microstructure analysis suggests that the growth of SiC nanowires depends on the VLS mechanism. The multi-scale reinforcement formed by C_f and SiC_nw can significantly improve the mechanical properties of C_f/LAS. The bending strength of SiC_nw-C_f/LAS reaches to 597 MPa, achieving an increase of 19% to C_f/LAS. Moreover, the samples show a maximum fracture toughness of 11.01 MPa m^1/2, achieving an increase of 46.4% to C_f/LAS. Through analysis of the fracture surface, the improved mechanical properties could be attributed to the multi-scaled reinforcements by the pull-out and debonding of C_f and SiC_nw from the composites.     

Influence of bonding phases on properties of in-situ bonded porous SiC membrane supports

Porous SiC ceramic membrane supports are widely employed in a wide variety of high-temperature applications, such as hot flue gas filtration, porous burners and molten metal filters. Herein, SiC supports, with a porosity of ~37%, were prepared by using low-temperature bonding techniques and the influence of different bonding phases, such as mullite, cordierite and glass, on ambient-temperature flexural strength, hot modulus of rupture (HMOR), thermal shock resistance and oxidation resistance were systematically investigated. The results reveal that the glass-bonded SiC (GBSC) support exhibited the highest ambient-temperature flexural strength of 33.6 MPa, whereas the flexural strength of mullite-bonded SiC (MBSC) and cordierite-bonded SiC (CBSC) supports ranged from 22 to 25 MPa. However, the presence of glass phase deteriorated the high-temperature properties of the support. MBSC support rendered superior mechanical strength at high temperature and self-strengthening in a certain temperature range, such as HMOR improved 47.5% at 900 °C, but HMOR of glass-bonded support was only 57.4% of the ambient-temperature strength. Moreover, MBSC and CBSC supports exhibited better thermal shock resistance than GBSC supports and the critical temperature difference of water quenching for MBSC supports was ~200 °C higher than GBSC supports. In addition, MBSC support rendered superior oxidation resistance and exhibited a weight gain rate of ~0.1% at 1150 °C for 24 h, which is 54.4% and 42.2% lower than CBSC and GBSC supports, respectively.     

Effects of SiC whiskers on the mechanical properties and microstructure of SiC ceramics by reactive sintering

As-received and pre-coated SiC whiskers (SiC_w)/SiC ceramics were prepared by phenolic resin molding and reaction sintering at 1650 °C. The influence of SiC_w on the mechanical behaviors and morphology of the toughened reaction-bonded silicon carbide (RBSC) ceramics was evaluated. The fracture toughness of the composites reinforced with pre-coated SiC_w reached a peak value of 5.6 MPa m^1/2 at 15 wt% whiskers, which is higher than that of the RBSC with as-received SiC_w (fracture toughness of 3.4 MPa m^1/2). The surface of the whiskers was pre-coated with phenolic resin, which could form a SiC coating in situ after carbonization and reactive infiltration sintering. The coating not only protected the SiC whiskers from degradation but also provided moderate interfacial bonding, which is beneficial for whisker pull-out, whisker bridging and crack deflection.     

Preparation and characterization of aluminum borate whiskers reinforced ceramics with MnO2 addition

Ceramics with aluminum borate whiskers (ABWs) were prepared from H₃BO₃ and Al₂O₃ reagent, with and without 6 wt% MnO₂ used as an addition. The microstructures, phase composition, and crystal structure of the ceramics were analyzed via scanning electron microscopy, energy dispersive spectroscopy, and X-ray diffraction, respectively. The results show that MnO₂ is an effective addition for enhancing the flexural strength of ceramics. The MnO₂ could lead to the distortion of lattice, and improve the mechanical strength via a solid solution strengthening mechanism. Moreover, the content of H₃BO₃ and the sintering temperature were also key factors in the manufacture of optimal ceramics. The ceramic made from 6 wt% MnO₂ addition, 25 wt% H₃BO₃, and sintered at 1200°C, showed the highest flexural strength of 88.5 (±1.9) MPa, and had a bulk density of 1.64 g/cm³ and porosity of 44.2%.     

Effect of recoating slurry compositions on the microstructure and properties of SiC reticulated porous ceramics

Silicon carbide reticulated porous ceramics (SiC RPCs) were fabricated by polymer sponge replica technique, followed by recoating with SiC slurries of two different sintering additives of MgO–Al₂O₃–SiO₂ (Slurry 1) and polycarbosilane (Slurry 2). The sintering temperature of SiC RPCs recoated with Slurry 2 was 1100 °C, which was 200 °C lower than that for one recoated with Slurry 1. The prepared SiC RPCs exhibited homogeneous microstructure and contained pores with different sizes which was entrapped in the strut of SiC RPCs, small pores with diameter lower than 4 μm and large pores with diameter higher than 10 μm. Bending strength of SiC RPCs recoated with Slurry 1 was two times higher than that for the non-recoated samples, which was 1.88 MPa and was a little higher than that for one recoated with slurry 2. At the same time, high thermal shock resistance and high refractoriness were achieved for SiC RPCs recoated with Slurry 2.     

A novel approach to prepare reticulated porous TiN ceramics with high strength and high porosity by in-situ synthesis

Titanium nitride (TiN) with high porosity (90%) was successfully in-situ prepared by a novel approach with the combination of carbothermic reduction nitriding method and replication template method. The microstructure of porous TiN prepared with different temperature and phenolic resin (PF) content were revealed by XRD, Raman spectrum, SEM, TEM, respectively. The results show that when the mass ratio of PF and TiO₂ is 1:2 and the sintering temperature is 1850 ℃, porous TiN with high purity and ideal strength could be synthesized. In addition, the synthesis path and thermodynamic mechanism of porous TiN were analyzed by TG-DSC and Gibbs free energy calculation. The mechanical properties and corrosion resistance were preliminarily explored.