Effect of interface types on the heat-resistance of Cansas-II SiCf /SiC composites

The heat-resistance of the Cansas-II SiC/CVI-SiC mini-composites with a PyC and BN interface was studied in detail. The interfacial shear strength of the SiC/PyC/SiC mini-composites decreased from 15 MPa to 3 MPa after the heat treatment at 1500 °C for 50 h, while that of the SiC/BN/SiC mini-composites decreased from 248 MPa to 1 MPa, which could be mainly attributed to the improvement of the crystallization degree of the interface and the decomposition of the matrix. Aside from the above reasons, the larger declined fraction of the interfacial shear strength of the SiC/BN/SiC mini-composites might also be related to the gaps in the BN interface induced by the volatilization of B₂O₃·SiO₂ phase, leading to a significant larger declined fraction of the tensile strength of the SiC/BN/SiC mini-composites due to the obvious expansion of the critical flaws on the fiber surface. Therefore, compared with the CVI BN interface, the CVI PyC interface has better heat-resistance at high temperatures up to 1500 °C due to the fewer impurities in PyC.     

Microstructural and mechanical characterization of a mullite fiber

The effect of thermal exposure on a mullite fiber was analyzed. This type of mullite fiber, consisting of γ-Al₂O₃ and amorphous SiO₂, was developed for high-temperature applications. Heat treatments at temperatures ranging from 900 °C to 1500 °C for 1h were performed in air. Investigations showed that the tensile strength of the initial fiber was about 1.60 GPa. And the elastic modulus was about 133.51 GPa. The bundles’ strength decreased at 900 °C slightly after thermal treatment, then increased and got a maximum at 1100 °C with 1.65 GPa. At above 1100 °C, the strength degraded sharply due to the mullite phase transformation and the exaggerated grain growth. At 1300 °C, the phase reaction almost finished with a tensile strength of 0.86 GPa. And the strength retention was only 47.50%. When the heat-treated temperature got to 1500 °C, the density of surface defects in the fiber surged, making it too fragile and weak to go through the tensile tests.     

Evolution of the structure and mechanical performance of Cansas-II SiC fibres after thermal treatment

Herein, an in-depth analysis of the effect of heat treatment at temperatures between 900 and 1500 °C under an Ar atmosphere on the structure as well as strength of Cansas-II SiC fibres was presented. The untreated fibres are composed of β-SiC grains, free carbon layers, as well as a small amount of an amorphous SiC_xO_y phase. As the heat-treatment temperature was increased to 1400 °C, a significant growth of the β-SiC grains and free carbon layers occurred along with the decomposition of the SiC_xO_y phase. Moreover, owing to the decomposition of the SiC_xO_y phase, some nanopores formed on the fibre surface upon heating at 1500 °C. The mean strength of the Cansas-II fibres decreased progressively from 2.78 to 1.20 GPa with an increase in the heat-treatment temperature. The degradation of the fibre strength can be attributed to the growth of critical defects, β-SiC grains, as well as the residual tensile stress.     

Mechanical behaviour of carbon fibre reinforced TaC/SiC and ZrC/SiC composites up to 2100°C

The microstructure and elevated temperature mechanical properties of continuous carbon fibre reinforced ZrC and TaC composites were investigated. Silicon carbide was added to both compositions to aid sintering during hot pressing. Fibres were homogeneously distributed and no fibre degradation was observed at the interface with the ceramic matrix even after testing at 2100 °C. The flexural strength increased from 260 to 300 MPa at room temperature to ∼450 MPa at 1500 °C, which was attributed to stress relaxation. At 1800 °C, the strength decreased to ∼410 MPa for both samples. At 2100 °C plastic deformation resulted in lower strength at the proportional limit (210–320 MPa), but relatively high ultimate strength (370–440 MPa). The sample containing ZrC had a lower ultimate strength, but higher failure strain at 2100 °C due to the weak fibre/matrix interface that resulted in fibre-dominated composite behaviour.     

Oxidation resistance and thermal stability of the SiC-ZrB2 composite ceramic fibers

In this study, continuous SiC-ZrB₂ composite ceramic fibers were synthesized from a novel pre-ceramic polymer of polyzirconocenecarbosilane (PZCS) via melt spinning, electron beam cross-linking, pyrolysis, and finally sintering at 1800°C under argon. The ZrB₂ particles with an average grain size of 30.7 nm were found to be uniformly dispersed in the SiC with a mean size of 59.7 nm, as calculated using the Scherrer equation. The polycrystalline fibers exhibit dense morphologies without any obvious holes or cracks. The tensile strength of the fibers was greater than 2.0 GPa, and their elastic modulus was ~380 GPa. After oxidation at 1200°C for 1 hour, the strength of the fibers did not decrease despite a small loss of elastic modulus. Compared to the advanced commercial SiC fibers of Tyranno SA, the fibers exhibited improved high-temperature creep resistance in the temperature range 1300-1500°C.     

Mechanical properties of borothermally synthesized zirconium diboride at elevated temperatures

The mechanical properties of a nominally phase pure ZrB₂ ceramic were measured up to 2300°C in an argon atmosphere. ZrB₂ was hot pressed at 2000°C utilizing borothermally synthesized powder from high purity ZrO₂ and B raw materials. The relative density of the ceramics was about 95% with an average ZrB₂ grain size of 8.8 µm. The room temperature flexural strength was 447 MPa, with strength decreasing to 196 MPa at 1800°C, and then increasing to 360 MPa at 2300°C. The strength up to 1800°C was likely controlled by a combination of effects: surface damage from oxidation of the specimens, stress relaxation, and decreases in the elastic modulus. The strength above 1800°C was controlled by flaws in the range consistent with sizes of the maximum ZrB₂ grain size and the largest pores. Fracture toughness was 2.3 MPa·m^1/2 at room temperature, increasing to 3.1 MPa·m^1/2 at 2200°C. The use of higher purity starting materials improved the mechanical behavior in the ultra-high temperature regime compared to previous studies.     

Heat treatment effects on microstructure and mechanical properties of CVI SiCf/PyC/SiC composites with Cansas-Ⅲ SiC fibers

The microstructure and mechanical properties of CVI-Cansas-III/PyC/SiC composites were systematically investigated after heat treatment under high temperature argon atmosphere, ranging from 1000 °C to 1500 °C, for different time durations. The results showed that the Cansas-III fibres degraded with increasing heat treatment temperature, resulting in degradation of the fibre properties due to pyrolysis of the SiOC phase inside the fibres. The bending strength of the composites remained nearly constant upon heat treatment at 1000 °C and 1250 °C, while a decline in bending strength was observed upon increasing the heat treatment temperature and time, specifically at 1350 °C and above. Moreover, the composites maintained their pseudo-plastic fracture behaviour below 1450 °C, while displaying brittle fracture of the ceramic after 100 h of heat treatment at 1500 °C, due to the complete crystallisation of the fibres.     

Complete characterisation of BN fibres obtained from a new polyborylborazine

A new polymer was prepared at room temperature from a di-chloroborazine and a reactive aminoborane. It displays borazine rings unambiguously linked through three atoms N–B–N bridges. This connecting mode was evidence by ¹⁵N solid state NMR. This polyborazine was processed into a continuous polymer fibre of about 21 μm diameter, which was subsequently heat-treated under NH₃/N₂ up to 1800 °C for conversion into BN fibres. The achievement of hexagonal boron nitride was confirmed by X-ray diffraction and Raman spectroscopy. Tensile tests were carried out on the ceramic fibres. The average tensile strength is about 1000 MPa and the Young's modulus is close to 200 GPa. Structural characterisation of the BN fibres was undertaken by polarised light and transmission electronic microscopies.     

Microstructural evolution under load and high temperature deformation mechanisms of a mullite/alumina fibre

A two-phase mullite alumina fibre, the 3M Nextel 720 fibre, has been studied in tension and creep. The fibre shows the highest creep resistance of all current commercial fine oxide fibres up to 1500 °C. The creep mechanisms involve progressive dissolution of mullite and simultaneous reprecipitation of alumina into elongated oriented grains and grain boundary sliding by a thin alumino-silicate liquid phase. The rate of grain growth in creep at a given temperature is dependant on the applied stress. The combination of sub-micron size mullite crystallites and alumina grains gives rise to a high sensitivity to alkaline contamination. Stress enhanced diffusion of the contaminants from the fibre surface results in crack nucleation, dissolution of mullite, formation of a liquid phase and slow crack growth. From 1200 °C, this process is coupled with a fast α-alumina grain growth at the fibre surface.     

Heat treatment effects on microstructure and properties of CVI SiC/SiC composites with Sylramic™-iBN SiC fibers

Chemical-vapor-infiltrated (CVI) SiC/SiC composites with Sylramic?-iBN SiC fibers and CVI carbon, BN, and a combination of BN/C interface coating were heat treated in 0.1-MPa argon or 6.9-MPa N₂ at temperatures to 1800 °C for exposure times up to 100 hr. The effects of thermal treatment on constituent microstructures, in-plane tensile properties, in-plane and through-the-thickness thermal conductivities, and creep behavior of the composites were investigated. Results indicate that heat treatment affected stoichiometry of the CVI SiC matrix and interface coating microstructure, depending on the interface coating composition and heat treatment conditions. Heat treatment of the composites with CVI BN interface in argon caused some degradation of in-plane properties due to the decrease in interface shear strength, but it improved creep resistance significantly. In-plane tensile property loss in the composites can be avoided by modifying the interface composition and heat treatment conditions.     

Carbothermal synthesis of boron nitride coating on PAN carbon fiber

Boron nitride (BN) thin coating has been formed on the surface of chemically activated polyacrylonitrile (PAN) carbon fiber by dip coating method. Dip coating was carried out in saturated boric acid solution followed by nitridation at a temperature of 1200 °C in nitrogen at atmospheric pressure to produce BN coating. Chemical activation improved surface area of PAN fiber which favours in situ carbothermal reduction of boric acid. Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) have shown the formation of boron nitride. The X-ray photoelectron spectroscopy reveals that the coating forms a composite layer of carbon, BN/BO_xN_y and some graphite like BCN with local structure of B–N–C and B(N–C)₃. The oxidation resistance of the coated fiber was significantly higher than uncoated carbon fiber. Tensile strength measurement reveals that the BN coated fiber maintained 90% of its original strength. As compared to chemical vapor deposition (CVD), this process is simple, non-hazardous and is expected to be cost effective.     

Ultra-high strength medium-entropy (Ti,Zr,Ta)C ceramics at 1800°C by consolidating a core-shell structured powder

We report for the first time the synthesis of a core-shell structured composite powder with a core of Zr(Ti,Ta)C and a shell of Ti,Ta(Zr)C at 1700°C and investigate the formation mechanism for the core-shell structure. The medium-entropy (Ti,Zr,Ta)C ceramics with fine grains (1.1 ± 0.4 μm) and relative density of 94.8% was prepared by hot-pressing at 2100°C. The flexural strength of (Ti,Zr,Ta)C at 1000°C (493 ± 21 MPa) was close to the room temperature (511 ± 52 MPa). As the temperature increased from 1600°C to 1800°C, the flexural strength was increased significantly, with an ultra-high flexural strength of 725 ± 32 MPa at 1800°C. The existence of the core-shell structure in the powder suppressed the grain growth due to the sluggish diffusion effect. The ultra-high strength of (Ti,Zr,Ta)C ceramics was attributed to its fine microstructures, high fracture toughness, and the reinforced the grain boundary strength.     

High temperature mechanical properties of laminated ZrB2–SiC based ceramics

Two laminated ZrB₂-SiC based ceramics were prepared by tape casting and subsequent hot pressing, with BN (LZB) and graphite (LZG ) as interface layers. The LZB specimen presents flexural strength of 381 MPa at room temperature and 111 MPa at 1500 °C; while the LZG specimen shows flexural strength of 414 MPa at room temperature and 377 MPa at 1500 °C. In addition, the flexural strength of LZG specimen is always higher than that of the LZB specimen in the temperature range from room temperature to 1500 °C. Such higher strength is attributed to the healing of surface microcracks and pores by the SiO₂ glass phase, producing less glass phase in graphite interface layers at high temperature.     

Oxidation resistance and microstructure evolution of ZrB2–SiC–La2O3/SiC dual-layer coating on siliconized graphite at 1800 °C under low air pressures

The oxidation behaviors of a ZrB₂–SiC–La₂O₃/SiC dual-layer coating on siliconized graphite at 1800 °C under low air pressures (50, 5 and 0.5 kPa) were investigated. The results showed that with the decrease of air pressure, the oxidation kinetics of the coated samples changed from parabolic weight gain to linear weight loss. A protective oxide scale consisted of ZrO₂ and SiO₂ with La dispersed was formed on the coating surface after oxidation in 50 kPa air. The oxide scale formed in 5 kPa air was full of bubbles. Only porous ZrO₂ layer was left on the coating surface after oxidation in 0.5 kPa air. At 1800 °C, the active oxidation of SiC occurred and gaseous SiO formed at the coating/oxide interface. The surface volatilization of SiO became severe with the decrease of air pressure, resulting in the presence of non-protective oxide scale.     

The sintering behaviour,mechanical properties and creep resistance of aligned polycrystalline yttrium aluminium garnet (YAG) fibres,produced from an aqueous sol–Gel precursor

Continuous ceramic fibres are finding applications as reinforcements in ceramic matrix composites, and yttrium aluminium garnet (YAG) is a particularly attractive candidate material on account of its creep resistance at high temperatures. A continuous, aligned, 5·5 μm diameter polycrystalline YAG fibre was manufactured from an aqueous sol–gel precursor which contained chlorine, and compared to a similar nitrate containing YAG precursor fibre we have reported previously. The precursor sol was found to be stable at a higher concentration than the nitrate containing sol, and this resulted in denser gel fibres which demonstrated better sintering at equivalent temperatures, giving a 98·5% sintered YAG fibre at 1550°C with a grain size of only 1 μm. However, on firing in air, the fibres formed fully crystalline YAG between 800 and 900°C, a temperature 100°C higher than the fibres containing nitrate, and they were weakened by the presence of many hemispherical faults. It was shown that both of these features were due to the retention of chlorine until the onset of formation of the crystalline YAG phase, and a series of steaming experiments were devised to remove the halide before this process could occur. It was found that steaming the precursor fibre from 200 to 500°C over 3 h, followed by firing to the required temperature in air, removed the chlorine and the problems it caused in the formation of the YAG phase without any change in the sintering characteristics or grain size. The steamed fibres were of a strength and quality comparable to fibres drawn from organometallic precursors. Empirical friability measurements showed the strength was maintained after firing to 1550°C, although there was a deterioration in apparent strain to break of the aligned blanket product above 1200°C. Conversely, the creep resistance, measured using the BSR test, improved with increase in temperature. The fibres fired to 1550°C were fully relaxed at temperatures 100–150°C below that of coarser, larger YAG fibres previously reported with a 3 μm grain size and 120 μm diameter. However, when allowance was made for grain size, the difference in creep rates was within the range obtained by extrapolating previous data using lattice diffusion and grain boundary effect models. Fibres fired to 1400°C were much finer grained but only slightly inferior to the 1550°C fibre in terms of creep. The alumina sol used in this work contained a significant level of sodium, and this suggests that the creep rates are effected by grain boundary impurities, especially sodium. A sodium free sol has been procured and further work is recommended to clarify the effect of impurities and improve fibre properties.     

Microstructural evolution,mechanical and thermal properties of LaB6 embedded in Si-B-C-N prepared by spark plasma sintering

Si-B-C-N monoliths with 5 wt% LaB₆ additives were prepared by spark plasma sintering at 1250–2000 °C and 50 MPa using a mechanically alloyed mixture of graphite, c-Si, h-BN and LaB₆ powders as the starting materials. Microstructural evolution, mechanical and thermal properties of the as-prepared La/Si-B-C-N monoliths were investigated. The densification of the ceramics starts at 1160° and ends at 1800 °C with the formation of La-containing compounds coupled with SiC and BN(C) phases. La-containing BN(C) grains develop into a lamellar structure at 1900 °C offering improved fracture toughness and decreased Vickers hardness, flexural strength and elastic modulus. The formation of lamellar BN(C) is also responsible for a high thermal expansion coefficient of 4.2×10⁻⁶ /°C.     

Strength of single-phase high-entropy carbide ceramics up to 2300°C

The mechanical properties of single-phase (Hf,Zr,Ti,Ta,Nb)C high-entropy carbide (HEC) ceramics were investigated. Ceramics with relative density >99% and an average grain size of 0.9 ± 0.3 µm were produced by a two-step process that involved carbothermal reduction at 1600°C and hot pressing at 1900°C. At room temperature, Vickers hardness was 25.0 ± 1.0 GPa at a load of 4.9 N, Young's modulus was 450 GPa, chevron notch fracture toughness was 3.5 ± 0.3 MPa·m^1/2, and four-point flexural strength was 421 ± 27 MPa. With increasing temperature, flexural strength stayed above ~400 MPa up to 1800°C, then decreased nearly linearly to 318 ± 21 MPa at 2000°C and to 93 ± 10 MPa at 2300°C. No significant changes in relative density or average grain size were noted after testing at elevated temperatures. The degradation of flexural strength above 1800°C was attributed to a decrease in dislocation density that was accompanied by an increase in dislocation motion. These are the first reported flexural strengths of HEC ceramics at elevated temperatures.     

The enhanced thermal shock resistance and combustion efficiency of SiC reticulated porous ceramics via the construction of multi-layer coating

SiC reticulated porous ceramic (SRPC) as the key component determined the service life and combustion characteristics of porous burner. The novel multi-layer struts were constructed to synergistically improve the oxidation resistance and infrared radiation of SRPC, including microporous cordierite coating, dense mullite transition layer, SiC skeleton and filling layer. The continuous mullite transition layer significantly improved the resistance to water vapor oxidation of SRPC, also their strength and thermal shock resistance were enhanced because the elimination of strut defects in multi-layer struts. In addition, the microporous cordierite coating generated from the burnt out of pitch increased the burner surface temperature from 764.4 °C to 1061.7 °C, and obviously reduced the CO/NOx emission due to its improved infrared radiation property. Furthermore, the porous cordierite coating enhanced the heat radiation of SRPC, thus increasing the heating rate of the burner from 29.4 °C/min to 33.1 °C/min in the process of water heating.     

Novel process for recrystallized silicon carbide through β-α phase transformation

A novel process was investigated to produce recrystallized silicon carbide through β-α phase transformation. The specimen was prepared from carbon and β-SiC powder mixture, first by infiltration with liquid silicon at 1500 °C to form β-SiC preform with a high density, and then by heating it further up to 2200 °C. When the β-SiC particles were transformed into α-SiC at 2200 °C, the rapid grain growth occurred of the α-SiC by consuming β-SiC particles, resulting in an interconnected network structure with huge and elongated α-SiC grains. The specimen recrystallized at 2200 °C had a measured density of 2.7 g/cm³ and strength of 134 MPa. The infiltration behavior, microstructure evolution and mechanical properties of the recrystallized silicon carbide were examined and discussed.     

Fabrication and properties of ZrB2–SiC–BN machinable ceramics

ZrB₂–SiC–BN ceramics were fabricated by hot-pressing under argon at 1800 °C and 23 MPa pressure. The microstructure, mechanical and oxidation resistance properties of the composite were investigated. The flexural strength and fracture toughness of ZrB₂–SiC–BN (40 vol%ZrB₂–25 vol%SiC–35 vol%BN) composite were 378 MPa and 4.1 MPa m^1/2, respectively. The former increased by 34% and the latter decreased by 15% compared to those of the conventional ZrB₂–SiC (80 vol%ZrB₂–20 vol%SiC). Noticeably, the hardness decreased tremendously by about 67% and the machinability improved noticeably compared to the relative property of the ZrB₂–SiC ceramic. The anisothermal and isothermal oxidation behaviors of ZrB₂–SiC–BN composites from 1100 to 1500 °C in air atmosphere showed that the weight gain of the 80 vol%ZrB₂–20 vol%SiC and 43.1 vol%ZrB₂–26.9 vol%SiC–30 vol%BN composites after oxidation at 1500 °C for 5 h were 0.0714 and 0.0268 g/cm², respectively, which indicates that the addition of the BN enhances oxidation resistance of ZrB₂–SiC composite. The improved oxidation resistance is attributed to the formation of ample liquid borosilicate film below 1300 °C and a compact film of zirconium silicate above 1300 °C. The formed borosilicate and zirconium silicate on the surface of ZrB₂–SiC–BN ceramics act as an effective barriers for further diffusion of oxygen into the fresh interface of ZrB₂–SiC–BN.