Creep of SiC–SiC microcomposites

The creep behavior of SiC/C/SiC microcomposites at 1200–1400 °C and 140–450 MPa was investigated in the presence and absence of matrix cracking. The microcomposites consisted of single Hi Nicalon or Carborundum fibers coated with a CVD carbon interlayer and a CVD SiC matrix. Since the fibers and matrix had been examined by the identical experimental technique, direct comparisons of the creep of the composite and of the constituents were performed. The creep of uncracked microcomposites was successfully modeled using a simple rule of mixtures algorithm. When matrix cracks were present, the microcomposites were modeled using a series composite consisting of intact microcomposite, exposed fiber at the matrix crack, and the debonded region in between. Trends for behavior with respect to the various mechanical and structural parameters that control creep are presented.     

A ZrB2–SiC/SiC oxidation protective dual-layer coating for carbon/carbon composites

In order to improve the oxidation resistance of C/C composites, a ZrB₂–SiC/SiC oxidation protective dual-layer coating was prepared by a pack cementation combined with the slurry paste method. The phase and microstructure of the coating were characterised by X-ray diffraction, scanning electron microscope and energy-dispersive spectrometer analyses. The anti-oxidation and thermal shock resistance of the coating were also investigated. It was found that the ZrB₂–SiC/SiC coating could effectively improve the oxidation resistance of the C/C composites. The weight loss of the coated samples was only 1.8% after oxidation at 1773?K for 18?h in air. The coating endured 20 thermal shock cycles between 1773?K and room temperature with only 4.6% weight loss.     

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

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

C/C–ZrB_2–SiC复合材料的制备及其性能

结合化学气相渗透工艺(chemical vapor infiltration)与前驱体浸渍裂解(precursor infiltration and pyrolysis,PIP)工艺,制备了C/C–Zr B_2–Si C复合材料,并对材料的力学性能和烧蚀性能进行了分析。结果表明:PIP工艺制备的C/C–Zr B_2–Si C复合材料的拉伸、弯曲及剪切强度分别为91.2、214和35.8 MPa,优于通过浆料浸渍工艺制备的复合材料。同时,热流3 200 k W/m~2,时间600 s的氧乙炔火焰试验表明,PIP工艺制备的C/C–Zr B_2–Si C复合材料具有良好的抗氧化烧蚀性能,其线烧蚀率和质量烧蚀率分别为0.002 mm/s和0.7 mg/s。     

SiC/SiC复合材料及其应用

日本开发的Nicalon和Tyranno两种品牌的SiC纤维占有世界上绝对性的市场份额。SiC/SiC复合材料典型的界面层是500 nm厚的单层热解碳(PyC)涂层或多层(PyC-SiC)n涂层,在湿度燃烧环境及中高温条件下界面层的稳定性是应用研究的重点。SiC/SiC复合材料,包括CVI-SiC基体和日本开发的Tyranno hex和NITE-SiC基体等,具有耐高温、耐氧化性和耐辐射性的特点,在航空涡轮发动机部件、航天热结构部件及核聚变反应堆炉第一壁材料等方面正开展工程研制应用。     

SiC–AlN Particulate Composite

A SiC–AlN composite was fabricated by mechanical mixing of SiC and AlN powders, hot pressed under 40 MPa at 1950°C in Ar atmosphere. The object of this attempt was to achieve full density and a little solid solution formation. Fine microstructure and crack deflection behaviour are to improve the mechanical properties of the SiC–AlN composite. The bending strength and fracture toughness were achieved 800 MPa and 7·6 MPa m^1/2 at room temperature, respectively. The fracture toughness of the SiC–AlN composite shows minimal change between room temperature and 1400°C. Post-HIP improves the surface densification of the SiC–AlN composite resulting in an increase of the strength and the ability to resist oxidization. The bending strength of SiC–AlN composite increases from 800 to 1170 MPa after HIP treatment for 1 h under 187 MPa at 1700°C in N₂ atmosphere.     

不同SiC源对C_f/ZrB_2–SiC复合材料微结构和力学性能的影响

采用新型浆料注射/真空浸渍工艺实现了超高温陶瓷组分与碳纤维的有效复合,并结合低温(1 450℃)热压烧结实现了C_f/ZrB_2–SiC复合材料的制备。研究了不同SiC源(SiC粉体和聚碳硅烷PCS)对复合材料微结构和力学性能的影响,结果表明:基于聚碳硅烷优异的流动性实现了陶瓷组分在纤维束内和束间的有效填充,并经低温热压烧结后C_f/ZrB_2–PCS复合材料的相对密度为91.3%,主要归结于聚碳硅烷裂解后残留的微量无定性碳起到了表面除氧的作用而促进致密化,但该无定性碳弱化了晶界强度而导致力学性能降低。同时C_f/ZrB_2–PCS复合材料表现出非脆性断裂模式且断裂功高达539 J/m~2,较C_f/ZrB_2–SiC_p复合材料提升高达84.6%;该复合材料断裂功的提升主要归结于裂纹偏转、裂纹分叉和纤维桥联等多种增韧机制的协同效应,大幅度改善了ZrB_2基超高温陶瓷材料的损伤容限和可靠性。     

Effect of oxidation treatment on KD–II SiC fiber–reinforced SiC composites

Continuous silicon carbide fiber–reinforced silicon carbide matrix (SiC_f/SiC) composites have developed into a promising candidate for structural materials for high–temperature applications in aerospace engine systems. This is due to their advantageous properties, such as low density, high hardness and strength, and excellent high temperature and oxidation resistance. In this study, SiC_f/SiC composites were fabricated via polymer infiltration and pyrolysis (PIP) with the lower–oxygen–content KD–II SiC fiber as the reinforcement; a mixture of 2,4,6,8–tetravinyl–2,4,6,8–tetramethylcyclotetrasiloxane (V4) and liquid polycarbosilane (LPCS), known as LPVCS, was used as the precursor; while pyrolytic carbon (PyC) was used as the interface. The effects of oxidation treatment at different temperatures on morphology, structure, composition, and mechanical properties of the KD–II SiC fibers, SiC matrix from LPVCS precursor conversion, and SiC_f/SiC composites were comprehensively investigated. The results revealed that the oxidation treatment greatly impacted the mechanical properties of the SiC fiber, thereby significantly influencing the mechanical properties of the SiC_f/SiC composite. After oxidation at 1300 °C for 1 h, the strength retention rates of the fiber and composite were 41% and 49%, respectively. In terms of the phase structure, oxidation treatment had little effect on the SiC fiber, while greatly influencing the SiC matrix. A weak peak corresponding to silica (SiO₂) appeared after high–temperature treatment of the fiber; however, oxidation treatment of the matrix led to the appearance of a very strong diffraction peak that corresponds to SiO₂. The analysis of the morphology and composition indicated cracking of the fiber surface after oxidation treatment, which was increasingly obvious with the increase in the oxidation treatment temperature. The elemental composition of the fiber surface changed significantly, with drastically decreased carbon element content and sharply increased oxygen element content.     

Microstructure and ablation mechanism of C/C–SiC composites

C/C–SiC composites were prepared by molten infiltration of silicon powders, using porous C/C composites as frameworks. The porosities of the C/C–SiC composites were about 0.89–2.8 vol%, which is denser than traditional C/C composites. The ablation properties were tested using an oxyacetylene torch. Three annular regions were present on the ablation surface. With increasing pyrocarbon fraction, a white ceramic oxide layer formed from the boundary to the center of the surface. The ablation experimental results also showed that the linear and mass ablation rates of the composites decreased with increasing carbon fraction. Linear SiO₂ whiskers of diameter 800 nm and length approximately 3 μm were formed near the boundaries of the ablation surfaces of the C/C–SiC composites produced with low-porosity C/C frameworks. The ablation mechanism of the C/C–SiC composites is discussed, based on a heterogeneous ablation reaction model and a supersaturation assumption.     

Development of SiC–Si composites with fine-grained SiC microstructures

This work summarises the influence of the original particle-size of the SiC powder on the mechanical properties of silicon infiltrated SiC (SiC-Si) composite. These composites are based on a defined SiC particle-size structure. Using α-SiC powders with a mean particle-size of 12·8, 6·4, 4·5 and 3 μm, a clear linear enhancement of the bending strength with decrease of SiC-particle-size was observed. However, a further decrease of the SiC particle-size (from 3 to 0·5 μm) brought no increase of the strength and toughness, respectively. ©     

C/C–SiC composite prepared by Si–10Zr alloyed melt infiltration

A high performance and low cost C/C–SiC composite was prepared by Si–10Zr alloyed melt infiltration. Carbon fiber felt was firstly densified by pyrolytic carbon using chemical vapor infiltration to obtain a porous C/C preform. The eutectic Si–Zr alloyed melt (Zr: 10 at.%, Si: 90 at.%) was then infiltrated into the porous preform at 1450 °C to prepare the C/C–SiC composite. Due to the in situ reaction between the pyrolytic carbon and the Si–Zr alloy, SiC, ZrSi₂ and ZrC phases were formed, the formation and distribution of which were investigated by thermodynamics. The as-received C/C–SiC composite, with the flexural strength of 353.6 MPa, displayed a pseudo-ductile fracture behavior. Compared with the C/C preform and C/C composite of high density, the C/C–SiC composite presented improved oxidation resistance, which lost 36.5% of its weight whereas the C/C preform lost all its weight and the high density C/C composite lost 84% of its weight after 20 min oxidation in air at 1400 °C. ZrO₂, ZrSiO₄ and SiO₂ were formed on the surface of the C/C–SiC composite, which effectively protected the composite from oxidation.     

Cyclic ablation behavior of C/C–ZrC–SiC composites under oxyacetylene torch

Cyclic ablation behavior of C/C–ZrC–SiC composites prepared by precursor infiltration and pyrolysis process was studied using oxyacetylene torch. After repeated 30 s ablation for four times, the composites exhibited better ablation properties than those under single ablation for 120 s because of the lower surface temperature, and their linear and mass ablation rates were −3×10^–4 mm/s and −2.29×10^–3 g/s, respectively. A continuous ZrO₂–SiO₂ layer formed on the surface of center ablation region and acted as an effective barrier to the transfer of heat and oxidative gases into the inner material. Thermal stress induced by repeated impact of oxyacetylene led to some cracks on the ZrO₂–SiO₂ layer; however its destructive power was weaker than that of higher temperature. Stick like silica as grown silica nanowires were generated in the transition ablation region due to the evaporation of silicon oxide at appropriate temperature.     

C/C–SiC composite fabricated via PCS–Si slurry reactive melt infiltration

The slurry reactive melt infiltration (RMI) method was used to overcome the shortcomings of the traditional RMI method utilized in preparing the large-irregular shaped C/C preform. C/C–SiC composite was successfully fabricated via PCS–Si slurry RMI. Results show that it has a favorable physical bonding between the PCS–Si slurry and the C/C preform. After RMI, most of the Si in the PCS–Si slurry coating infiltrated into the C/C preform, the density of the C/C preform increased from 1.24 to 1.52g cm⁻³, and the open porosity decreased from 27.22% to 18.04%. SiC was formed on the surface as well as in the pores of the C/C preform. The as-received C/C–SiC composite showed a pseudo-ductile fracture behavior with a flexural strength of 76.4MPa. The mass ablation rate of the C/C–SiC composite is 0.34 mg s⁻¹, exhibiting much better ablation resistance than the C/C preform with a mass ablation rate of 1.80 mg s⁻¹.     

碳/碳复合材料SiC–HfSi_2–TaSi_2抗烧蚀复合涂层

采用包埋技术在碳纤维增强碳(carbon fiber reinforced carbon,C/C)复合材料表面制备了碳化硅-硅化铪-硅化钽(SiC-HfSi2-TaSi2)抗烧蚀复合涂层.采用氧已炔火焰烧蚀试验评价了. C/C复合材料样品的抗烧蚀性能.通过X射线衍射分析、扫描电镜观察及能谱分析研究了SiC-HfSi-TaSi2作为 C/C复合材料抗烧蚀涂层的表面和断面相组成、元素分布及形貌.结果表明:由于烧蚀过程中生成的Hf02,Ta205具有高温稳定性,使得该涂层表现 出良好的抗烧蚀性能,在3 000℃下烧蚀20s后,线烧蚀率为0.009 mm/s,质量烧蚀率为0.003 85 g/s.     

Pressureless sintered Al2O3–SiC nanocomposites

Al₂O₃ + 5 vol% SiC composite ceramics were prepared via a conventional powder processing route followed by pressureless sintering. Commercially available Al₂O₃ and SiC powders were milled together in an aqueous suspension. The slurry was freeze granulated, and green bodies were obtained by cold isostatic pressing of the granules. Pressureless sintering was carried out in a nitrogen atmosphere at 1750 and 1780 °C. Near full density (>99%) was achieved at 1780 °C. Densification at the lower sintering temperature was promoted by smaller additions of MgO. Vickers hardness and indentation fracture toughness varied around 18 GPa and 2.3 MPa m^1/2 after sintering at 1780 °C. Transmission electron microscopy revealed that the SiC particles were located predominantly to the interior of the matrix grains and well distributed throughout the composite microstructures. The intragranular particles had sizes in the range 50–200 nm while the intergranular particles were larger, typically 200–500 nm in diameter.     

Fiber/matrix interfacial shear strength of C/C composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers

The fiber/matrix (F/M) interfacial shear strength (IFSS) of carbon/carbon (C/C) composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers was investigated. To obtain C/C composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers, a thin layer of PyC was deposited on carbon fibers. After this, TaC and SiC–TaC layer(s) were uniformly deposited on the PyC coated carbon fibers. As an outer-layer, a PyC layer was deposited on these TaC and/or SiC–TaC coated carbon fibers by isothermal chemical vapour infiltration (CVI) and then densified with resin carbon by impregnation and carbonization. Finally, C/C composites with PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers were obtained. The effects of PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers on interfacial shear strength (IFSS) of C/C composites were investigated. Single fiber push-out tests were conducted on the fibers aligned perpendicularly on the thin slices specimen surface using nano-indentation. Results showed that the IFSS of C/C composites decreased with the introduction of PyC–TaC–PyC and PyC–SiC–TaC–PyC multi-interlayers. After heat treatment (at temperatures ranging from 1400 to 2500 °C) of C/C composites with PyC–TaC–PyC multi-interlayers, it was found that the IFSS decreased with the increase in temperature. This decrease in IFSS is explained by taking into account the microstructural variations on heat treatment.     

Friction and wear properties of C/C–SiC braking composites

Two series of C/C–SiC composites were fabricated via precursor infiltration pyrolysis (PIP) and chemical vapor infiltration (CVI) using porous C/C composites with different original densities as preforms, respectively. The tribological characteristics of C/C–SiC braking composites were investigated by means of MM-1000 type of friction testing machine. The friction and wear behaviors of the two series of composites were compared and the factors that influence the friction and wear properties of C/C–SiC composites were discussed. Results show that the friction and wear properties relate close-knit to the content of SiC and porosity. As the original preform density increasing, the content of SiC and porosity decrease, and then the friction coefficient increases obviously, the braking time and the wear rate both decrease. Preparation techniques play an important role in the tribological properties of C/C–SiC composites. Compared with PIP process, the samples from CVI have a little higher friction coefficient, shorter braking time and higher wear rate.     

ZrB2–SiC多层陶瓷的抗氧化性

用传统陶瓷的流延工艺制备ZrB2–SiC多层陶瓷。用Archimedes法测定ZrB2–SiC多层陶瓷的相对密度。用扫描电子显微镜观察其显微结构,并进行循环抗氧化性能评价。结果表明：ZrB2–SiC多层陶瓷在1 950℃烧结的致密度达到99.7%,材料的抗氧化过程主要可分为两个阶段：第一阶段低熔点相的挥发,出现质量损失;第二阶段氧化层的形成,降低进一步氧化速率。抗氧化性能较ZrB2–SiC复相陶瓷有很大提高。     

Fabrication and mechanical properties of laminated HfC–SiC/BN ceramics

Laminated HfC–SiC/BN ceramics were successfully fabricated by tape casting and hot pressing. Fully dense HfC–SiC ultra-high temperature ceramics with homogeneous structure were obtained. The introduction of the weak BN layer resulted in a slight decrease of the flexural strength but significantly improved the fracture toughness compared with monolithic HfC–SiC ceramics. The fracture toughness of laminated HfC–SiC/BN ceramics in the parallel direction peaked at 8.06 ± 0.46 MPa m^1/2, which increased by 115% than that of monolithic HfC–SiC ceramics. The composites showed non-catastrophic fracture behaviors in both parallel and perpendicular directions. It indicates that laminated structure design is a promising approach to obtain full density HfC–SiC ceramics with high fracture toughness.     

Effect of SiC nanoparticles on in-situ synthesis of SiC whiskers in corundum–mullite–SiC composites obtained by carbothermal reduction

Corundum–mullite–SiC composites were synthesised using a carbothermal reduction method. The effects of SiC nanoparticles and sintering temperatures on the phase transformation of the composites and the synthesis of SiC whiskers were studied by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Results indicated that corundum, mullite, and SiC whiskers were produced as final products at 1600–1650 °C. SiC whiskers were formed through the vapor–solid mechanism. The added SiC nanoparticles worked as nucleating agents to facilitate the carbothermal reduction of aluminosilicates and formation of SiC whiskers. The sample with the added SiC nanoparticles exhibited a high yield of β-SiC of 17.1%. Furthermore, the SiC nanoparticles decreased the formation temperature of SiC whiskers from the original 1600 °C to 1500 °C, and the porosity of the composites was increased from 56.7% to 64.7% by increasing the partial pressure of SiO gas. This study provides an insight into the more efficient synthesis of composites with SiC whiskers through the carbothermal reduction of aluminosilicates.