Effect of additive content on transient liquid phase sintering in SiC nanopowder infiltrated SiCf/SiC composites

SiC nanopowder infiltrated SiC_f/SiC composites with a high fiber volume fraction above 50 vol.% were prepared at a relatively low fabrication temperature of 1800 °C by transient liquid phase sintering using Al₂O₃-Y₂O₃-SiO₂ additives. The effects of additive content with 6-18 wt.% were investigated, based on densification, microstructure, mechanical properties and fracture behaviors of the composites. The results showed that the densification and mechanical properties of the composites were greatly improved with the additive content. Microstructural observation indicated that the infiltration of SiC nanopowder inside fiber-bundles were enchanced with the increase of additive content due to the effectively widen space by the reaction between pyrocarbon (PyC) interface and the additives especially with the addition of SiO₂. It proven that the enchanced matrix-PyC interface bonding by the high densification inside fiber-bundles played a key role in the improved mechanical properties and fracture behaviors of the composites.     

Enchanced high-temperature performances of SiC/SiC composites by high densification and crystalline structure

We report the enchanced in situ performances of tensile strength and thermal conductivity at elevated temperatures of the PCS-free SiC/SiC composite with a high fiber volume fraction above 50% fabricated by NITE process for nuclear applications. The composite was fabricated by the optimized combination of the fiber coating, the matrix slurry and the pressure-sintering conditions, based on our previous composites’ study history. The composite showed the excellent tensile strength up to 1500 °C, that it retained approximately 88% of the room-temperature strength. Also, the thermal conductivity of the composites represented over 20 W/m K up to 1500 °C, which was enough high to take the advantage of the assumed design value for nuclear applications. Microstructural observation indicated that the excellent high-temperature performances regarding tensile strength and thermal conductivity up to 1500 °C were the contribution to the high densification and crystalline structure in matrix.     

The effect on the tensile properties of PIP-processed SiC/SiC composite of a chemical vapor-infiltrated SiC layer overlaid on the pyrocarbon interface layer

A chemical vapor-infiltrated (CVI) SiC layer is often deposited on the pyrocarbon (PyC) fiber–matrix interface layer in SiC fiber-reinforced SiC matrix (SiC/SiC) composites. It is normally applied to protect the PyC layer from reacting with molten Si or sintering aids during manufacturing, and to guard against the effects of high temperature, oxidation and moisture during use. In this study, we investigated the effect of this SiC layer on the tensile properties of a composite. Tensile tests of our composite samples showed the SiC layer to have no noticeable effects on its ultimate load or fracture strain, whereas it decreased the load-to-strain ratio and proportional limit. The test results were analyzed by carrying out element tests on filaments and fiber bundle samples, fracture mirror analysis of pullout fibers, and finite element analysis (FEA) of residual thermal stress around the interface.     

Mechanical properties of 3D KD-I SiCf/SiC composites with engineered fibre-matrix interfaces

Three-dimensional (3D) silicon carbide (SiC) matrix composites reinforced with KD-I SiC fibres were fabricated by precursor impregnation and pyrolysis (PIP) process. The fibre-matrix interfaces were tailored by pre-coating the as-received KD-I SiC fibres with PyC layers of different thicknesses or a layer of SiC. Interfacial characteristics and their effects on the composite mechanical properties were evaluated. The results indicate that the composite reinforced with as-received fibre possessed an interfacial shear strength of 72.1 MPa while the composite reinforced with SiC layer coated fibres had a much higher interfacial shear strength of 135.2 MPa. However, both composites showed inferior flexural strength and fracture toughness. With optimised PyC coating thickness, the interface coating led to much improved mechanical properties, i.e. a flexural strength of 420.6 MPa was achieved when the interlayer thickness is 0.1 μm, and a fracture toughness of 23.1 MPa m^1/2 was obtained for the interlayer thickness of 0.53 μm. In addition, the composites prepared by the PIP process exhibited superior mechanical properties over the composites prepared by the chemical vapour infiltration and vapour silicon infiltration (CVI-VSI) process.     

Interfacial control of uni-directional SiCf/SiC composites based on electrophoretic deposition and their mechanical properties

Interfacial control of uni-directional SiC_f/SiC composites were performed by EPD, and their mechanical properties at room temperature were evaluated. The effect of the thickness of carbon interphase on SiC fibers by EPD on mechanical properties of uni-directional SiC_f/SiC composites was also investigated. The average thickness of carbon coating on SiC fibers increased from 42 nm to 164 nm with an increase in the concentration of colloidal graphite suspension for EPD. Dense SiC_f/SiC composites were achieved and their fiber volume fraction was 47–51%. The SiC_f/SiC composites had a bending strength of 210–240 MPa. As the thickness of carbon coating was below 100 nm, the SiC_f/SiC composites (SC01 and SC02) fractured in almost brittle manner. In contrast, the SiC_f/SiC composites (SC03) showed a pseudo-ductile fracture behavior with a large number of fiber pullout as the thickness of carbon coating was above 100 nm. The fracture energy of SC03 was 3–4 times as high as those of SC01 and SC02 and the value was about 1.7 kJ/m². In consideration of the results of mechanical properties, the thickness of carbon coating on SiC fibers should be at least 100 nm to obtain high-performance SiC_f/SiC composites. The fabrication process based on EPD method is expected to be an effective way to control the interfaces of SiC_f/SiC composites and to obtain high-performance SiC_f/SiC composites.     

Improvement of SiCf/SiC density by slurry infiltration and tape stacking

SiC fiber-reinforced SiC–matrix ceramic composites (SiC_f/SiC) were fabricated by vacuum infiltration of a SiC slurry into Tyranno™-SA grade-3 fabrics coated with a 200 nm-thick pyrolytic carbon (PyC) layer followed by hot pressing using a transient eutectic-phase. The density of the composite was improved using a special infiltration apparatus with a pressure gradient and alternating tape insertion between fabrics. Their overall properties were compared with those of monolithic SiC and composite containing chopped fibers. Although the density of the composites decreased with increasing fiber fraction, SiC_f/SiC containing 50 vol.% fibers had a density of 3.13 g/cm³, which is the highest reported thus far. The composites containing continuous fibers had a maximum flexural strength of 607 MPa and a step increase in the stress–displacement behavior during the three-point bending test due to fiber reinforcement, which was not observed in the monolith.     

Mechanical behavior of SiCf/SiC composites with alternating PyC/SiC multilayer interphases

In order to tailor the fiber–matrix interface of continuous silicon carbide fiber reinforced silicon carbide (SiC_f/SiC) composites for improved fracture toughness, alternating pyrolytic carbon/silicon carbide (PyC/SiC) multilayer coatings were applied to the KD-I SiC fibers using chemical vapor deposition (CVD) method. Three dimensional (3D) KD-I SiC_f/SiC composites reinforced by these coated fibers were fabricated using a precursor infiltration and pyrolysis (PIP) process. The interfacial characteristics were determined by the fiber push-out test and microstructural examination using scanning electron microscopy (SEM). The effect of interface coatings on composite mechanical properties was evaluated by single-edge notched beam (SENB) test and three-point bending test. The results indicate that the PyC/SiC multilayer coatings led to an optimum interfacial bonding between fibers and matrix and greatly improved the fracture toughness of the composites.     

不同界面SiC/SiC复合材料的断裂行为研究

碳化硅纤维增强碳化硅复合材料(SiC/SiC)是极具前景的高温结构材料。通过先驱体浸渍裂解(PIP)工艺分别制备了PyC界面和CNTs界面SiC/SiC复合材料, 对两种SiC/SiC复合材料的整体力学性能以及界面剪切强度等进行了测试表征, 并对材料中裂纹的产生与扩展进行了原位观测。结果表明, 两种界面SiC/SiC复合材料弯曲强度相近, 但PyC界面SiC/SiC复合材料的断裂韧性约为CNTs界面SiC/SiC复合材料的两倍。在PyC界面SiC/SiC复合材料中, 裂纹沿纤维-基体界面扩展, PyC涂层能够偏转或阻止裂纹, 材料呈现伪塑性断裂特征; 而在CNTs界面SiC/SiC复合材料中, 裂纹在扩展路径上遇到界面并不偏转, 初始裂纹最终发展为主裂纹, 材料呈现脆性断裂模式。     

Fabrication of SiCf/SiC composites by chemical vapor infiltration and vapor silicon infiltration

Three-dimensional (3D) silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites, employing KD-1 SiC fibers (from National University of Defense Technology, China) as reinforcements, were fabricated by a combining chemical vapor infiltration (CVI) and vapor silicon infiltration (VSI) process. The microstructure and properties of the as prepared SiC_f/SiC composites were studied. The results show that the density and open porosity of the as prepared SiC_f/SiC composites are 2.1 g/cm³ and 7.7%, respectively. The SiC fibers are not severely damaged during the VSI process. And the SiC fibers adhere to the matrix with a weak interface, therefore the SiC_f/SiC composites exhibit non-catastrophic failure behavior with the flexural strength of 270 MPa, fracture toughness of 11.4 MPa·m^1/2 and shear strength of 25.7 MPa at ambient conditions. Moreover, the flexural strength decreases sharply at the temperature higher than 1200 °C. In addition, the thermal conductivity is 10.6 W/mk at room temperature.     

Fabrication and mechanical properties of oriented SiC short-fiber-reinforced SiC composite by tape casting

SiC fiber-reinforced SiC composites with nearly unidirectionally and randomly aligned SiC short fiber were prepared by tape-casting and hot-pressing (HP). Volume fractions of fibers were 10 and 20 vol.%. Three-point bending test was carried out at room temperature. The SiC short-fiber-reinforced SiC composites showed completely brittle fracture for any fiber volume fraction and orientation. The maximum strength increased with increasing sintering temperature regardless of orientation of short fiber. In the unidirectionally and randomly aligned composites sintered at 1700 °C containing 20 vol.% fiber, the maximum bending strength was about 390 and 280 MPa, respectively.     

Mechanical properties and damping capacity of SiCp/TiNif/Al composite with different volume fraction of SiC particle

SiC_p/TiNi_f/Al composite with 20 Vol.% TiNi fibers were fabricated by pressure infiltration method. The effect of volume fraction of SiC particle on the mechanical properties and damping capacity of the composite were studied. Four different volume fractions of SiC particle in the composite were 0%, 5%, 20% and 35% respectively. The microstructure and damping capacity of the composites was studied by SEM and DMA respectively. As the gliding of dislocation in the Al matrix was hindered by SiC particle, the yield strength and elastic modulus of the composites increased, while the elongation decreased with the increase in volume fraction of SiC particle. Furthermore, the damping capacity of the composites at room temperature was decreased when the mount of strain was more than 1 × 10⁻⁴. In the heating process, the damping peak at the temperature of 135 °C was attributed to the reverse martensitic transformation from B19′ to B2 in the TiNi fibers.     

Design,Fabrication, Characterization and Simulation of PIP-SiC/SiC Composites

Continuous SiC fiber reinforced SiC matrix composites (SiC/SiC) have been studied and developed for high temperature and fusion applications. Polymer impregnation and pyrolysis (PIP) is a conventional technique for fabricating SiC/SiC composites. In this research, KD-1 SiC fibers were employed as reinforcements, a series of coatings such as pyrocarbon (PyC), SiC and carbon nanotubes (CNTs) were synthesized as interphases, PCS and LPVCS were used as precursors and SiC/SiC composites were prepared via the PIP method. The mechanical properties of the SiC/SiC composites were characterized. Relationship between the interphase shear strength and the fracture toughness of the composites was established. X-ray tomographic scans of the SiC/SiC composites were performed and the closed porosities of the composites were calculated. The compatibility of the SiC/SiC composites with liquid LiPb at 800 °C and 1000 °C was investigated. High-resolution synchrotron X-ray tomography was applied to the SiC/SiC composite and digital volume correlation was employed for Hertzian indentation testing of the SiC/SiC composite. A Cellular Automata integrated with Finite Elements (CAFE) method was developed to account for the effect of microstructure on the fracture behavior of the SiC/SiC composite.     

Reactive and dense sintering of reinforced-toughened B4C matrix composites

Reactive hot-press (1800-1880 °C, 30 MPa, vacuum) is used to fabricate relatively dense B₄C matrix light composites with the sintering additive of (Al₂O₃ +Y₂O₃). Phase composition, microstructure and mechanical properties are determined by methods of XRD, SEM and SENB, etc. These results show that reactions among original powders B₄C, Si₃N₄ and TiC occur during sintering and new phases as SiC, TiB₂ and BN are produced. The sandwich SiC and claviform TiB₂ play an important role in improving the properties. The composites are ultimately and compactly sintered owing to higher temperature, fine grains and liquid phase sintering, with the highest relative density of 95.6%. The composite sintered at 1880 °C possesses the best general properties with bending strength of 540 MPa and fracture toughness of 5.6 MPa m^1/2, 29 and 80% higher than that of monolithic B₄C, respectively. The fracture mode is the combination of transgranular fracture and intergranular fracture. The toughening mechanism is certified to consist of crack deflection, crack bridging and pulling-out effects of the grains.     

PyC/SiC界面相对PIP法制备3D HTA C/SiC复合材料性能的影响

利用三维编织炭纤维预制件通过先驱体浸渍裂解法制备C／SiC复合材料。研究了热解碳（PyC）／SiC界面相对复合材料的微观结构和力学性能的影响。弯曲性能通过三点弯曲法测试，复合材料的断口和抛光面通过扫描电镜观察。结果表明：通过等温化学气相沉积法在纤维表面沉积PyC／SiC界面相以后，复合材料的三点抗弯强度从46MPa提高到247MPa。沉积界面的复合材料断口有明显的纤维拔出现象，纤维与基体之间的结合强度适当，起到了增韧作用；而未沉积界面相复合材料的断口光滑、平整，几乎没有纤维拔出，纤维在热解过程中受到严重的化学损伤，性能下降严重，材料表现为典型的脆性断裂。     

Localized mechanical property assessment of SiC/SiC composite materials

SiC fiber-reinforced SiC matrix composites (SiC/SiC) are under consideration as a structural material for a range of nuclear applications. While these materials have been studied for decades, recently new small scale materials testing techniques have emerged which can be used to characterize SiC/SiC materials from a new perspective. In this work cross section nanoindentation was performed on SiC/SiC composites revealing that both the hardness and Young’s modulus was substantially lower in the fiber compared to the matrix despite both being SiC. Using scanning electron microscopy it was observed that the grain growth of the matrix during formation was radially out from the fiber with a changing grain structure as a function of radius from the fiber center. Focused ion beam machining was used to manufacture micro-cantilever samples and evaluate the fracture toughness and fracture strength in the matrix as a function of grain orientation in the matrix. Additionally microstructural characterization techniques like Raman spectroscopy, X-ray diffraction, and microtomography were used to evaluate differences in the matrix and fibers of the composite.     

Microstructure and mechanical properties of carbon fiber reinforced multilayered (PyC–SiC)n matrix composites

Carbon fiber reinforced multilayered (PyC–SiC)_n matrix (C/(PyC–SiC)_n) composites were prepared by isothermal chemical vapor infiltration. The phase compositions, microstructures and mechanical properties of the composites were investigated. The results show that the multilayered matrix consists of alternate layers of PyC and β-SiC deposited on carbon fibers. The flexural strength and toughness of C/(PyC–SiC)_n composites with a density of 1.43 g/cm³ are 204.4 MPa and 3028 kJ/m³ respectively, which are 63.4% and 133.3% higher than those of carbon/carbon composites with a density of 1.75 g/cm³. The enhanced mechanical properties of C/(PyC–SiC)_n composites are attributed to the presence of multilayered (PyC–SiC)_n matrix. Cracks deflect and propagate at both fiber/matrix and PyC–SiC interfaces resulting in a step-like fracture mode, which is conducive to fracture energy dissipation. These results demonstrate that the C/(PyC–SiC)_n composite is a promising structural material with low density and high flexural strength and toughness.     

先驱体转化法制备碳纤维增强碳化硅复合材料的研究

本文采用有机硅先驱体聚碳硅烷转化成碳化硅制备连续碳纤维增强的碳化硅基复合材料。对其制备工艺,如碳纤维体积分数的控制、液相浸渍聚碳硅烷热解转化成碳化硅基体的致密化等进行了研究。结果表明,该工艺对制备连续纤维增强的陶瓷基复合材料是一种有效的方法,易于实现纤维和基体的成型、复合。致密化过程不损伤纤维。对其C/SiC复合材料的性能进行了表征,C纤维具有明显增韧碳化硅的效果,其断裂机制表现为韧性特征。     

From random chopped to oriented continuous SiC fibers–ZrB2 composites

ZrB₂–continuous SiC fiber composites were prepared by vacuum-bag infiltration and hot pressing, using homemade 1D fabric preforms of Tyranno SA3 SiC fibers. Sintering behavior and microstructural features such as secondary phases and matrix/fiber interface were compared to those of chopped SiC fibers-reinforced composites. The infiltration process allowed the overall fiber content to be increased up to 40 vol%, because of the ordered arrangement of fibers. When the fiber preforms were properly infiltrated, the composites were nearly fully dense and the densification mechanisms were the same as those of unreinforced matrices. Different from composites containing short discontinuous fibers, the degree of chemical interaction at the fiber/matrix interface was very limited and this resulted in an easier pull out in the fractured surfaces, even in absence of fiber protective coating.     

Interface engineering of fiber-reinforced all-oxide composites fabricated by the sol–gel method with fugitive pyrolytic carbon coatings

This paper describes the interface engineering of three–dimensional (3D) Nextel™440 fiber-reinforced aluminosilicate composites fabricated by the sol–gel method with fugitive pyrolytic carbon (PyC) coatings. The coating thickness on the fiber strength, interfacial characteristics and there corresponding effects on mechanical properties of the composites were investigated. The study shows that the fiber strength was influenced by the coating thickness and optimized with the thickness of 0.15 μm. The composites with uncoated fibers showed brittle fracture behavior without fiber pullout because of strong interactions between the fiber and the matrix. However, higher strengths and pseudo-ductile fracture behaviors were obtained in the composites with PyC interphases, where different deflections and branches of propagating cracks and fiber pullout patterns were observed. Moreover, induced fugitive PyC interface conditions have great effects on the density, microstructure and mechanical properties of the resultant composites.     

SiC<Subscript>f</Subscript>/SiC composites reinforced by randomly oriented chopped fibers prepared by semi-solid mechanical stirring method and hot pressing

SiC short fibers, with an average diameter of 13 μm, length of 300–1,000 μm and chopped from SiC continuous fibers, were surface modified by the semi-solid mechanical stirring method to produce a discrete coating of aluminum particles. Then the starting mixtures, which consist of SiC short composite fibers, aluminum powder less than 50 μm and α-SiC powder of an average diameter of 0.6 μm, were mechanically mixed in ethanol for about 3 h, dried at 80 °C in air, and hot pressed under 30 MPa pressure at 1,650, 1,750 and 1,850 °C with 1 h holding time to prepare SiC_f/SiC composites. Volume fraction of SiC short fibers in the starting powder for SiC_f/SiC composites was about 25 vol.%. The composites were characterized in terms of bulk density, phase composition, and mechanical properties at room temperature. In addition, the distribution of SiC short fibers in the matrix and the cracking pattern in the composites were examined by optical microscope. Fracture surface of the composites were performed by a scanning electron microscope (SEM). The effect of hot-pressing temperature on bulk density and mechanical properties was investigated. The results indicated that SiC short fibers were uniformly and randomly distributed in the matrix, bending strength and bulk density of the composites increased with increasing sintering temperature. The composite, hot-pressed at 1,850 °C, exhibited the maximum bulk density and bending strength at room temperature, about 3.01 g/cm³ and 366 MPa, respectively. SEM analyses showed that there were a few of fiber pullout on the fracture surface of samples sintered at 1,650 °C and 1,750 °C, which was mainly attributed to lower densities. But few of fiber pullout was observed on the fracture surface of sample sintered at 1,850 °C, the combined effects of high temperature and a long sintering time were considered as a source of too severe fiber degradation because of the large amount of oxygen in the fibers.