Fabrication of scalable,aligned and low density carbon nanotube/silicon carbide hybrid foams by polysilazane infiltration and pyrolysis

Polymer-derived ceramic (PDC) process is an attractive technique that has high ceramic yield. This versatile method allows for fabrication of porous carbon nanotube (CNT)/ silicon carbide (SiC) hybrid materials that is important high temperature structural applications. Although several forms of CNT assemblies have been used with the PDC approach, the fabricated CNT/ceramic nanocomposites were either one or two dimensional. Herein, we report, for the first time, the fabrication of a low density, three-dimensional (3D) and scalable CNT/SiC structure using PDC technique. It was synthesized by impregnating preceramic polysilazane (PSZ) into ultralow density, anisotropic, and highly aligned CNT foams, followed by thermosetting and pyrolysis processes. The ceramic phase conformally coated the CNTs. The X-ray diffraction (XRD) diffractogram confirmed the presence of β-SiC crystalline phase. The resulting hybrid foam inherited the morphology and form factor of the original CNT foam, and possessed mechanical robustness, improved electrical properties, and extraordinary thermal stability.     

Effects of heat treatment on the mechanical properties at elevated temperatures of plain-woven SiC/SiC composites

The effects of heat treatment on the mechanical properties of plain-woven SiC/SiC composites at 927 °C and 1200 °C in argon were evaluated through tensile tests at room temperature and at elevated temperature on the as-received and heat-treated plain-woven SiC/SiC composites, respectively. Heat treatment can improve the mechanical properties of composites at room temperature due to the release of thermal residual stress. Although heat treatment can damage the fiber, the effect of this damage on the mechanical properties of composites is generally less than the effect of thermal residual stress. Heat treatment will graphitize the pyrolytic carbon interface and reduce its shear strength. Testing temperature will affect the expansion or contraction of the components in the composites, thereby changing the stress state of the components. This study can provide guidance for the optimization of processing of ceramic matrix composites and the structural design in high-temperature environments.     

Microstructure and mechanical properties of hot-pressed SiC/(W,Ti)C ceramic composites

SiC/(W, Ti)C ceramic composites with different content of (W, Ti)C solid-solution were produced by hot pressing. The effect of (W, Ti)C content on the microstructure and mechanical properties of SiC/(W, Ti)C ceramic composites has been studied. Densification rates of the SiC/(W, Ti)C ceramic composites were found to be affected by addition of (W, Ti)C. Increasing (W, Ti)C content led to increase the densification rates of the composites. The sintering temperature was lowered from 2100 °C for monolithic SiC to 1900 °C for the SiC/(W, Ti)C composites. Results show that additions of (W, Ti)C to SiC matrix resulted in improved mechanical properties compared to pure SiC ceramic. The fracture toughness and flexural strength continuously increased with increasing (W, Ti)C content up to 60 vol.%, while the hardness decreased with increasing (W, Ti)C content.     

Advances in modifications and high-temperature applications of silicon carbide ceramic matrix composites in aerospace: A focused review

This article is a detailed review of the measures to modify the high-temperature mechanical properties of silicon carbide ceramic matrix composites (SiC CMCs), namely toughness, high-temperature stability and wear resistance. Additionally, it briefly describes the common processing methods of the SiC CMCs and their application in the high-temperature field of aerospace. The advantages and disadvantages of various existing processing and molding methods for the SiC CMCs are also discussed. The high-temperature mechanical properties of the SiC CMCs are mainly affected by the properties of the matrix, added phase and interface. It is crucial to reduce the crystal defects of the matrix and select a suitable enhancement phase for an elevated performance. Moreover, it is important to improve the bonding at the interface between the enhancement phase and the matrix. This review is expected to provide useful information for the subsequent development of complex SiC CMCs for high-temperature applications.     

Low density,three-dimensionally interconnected carbon nanotube/silicon carbide nanocomposites for thermal protection applications

Synthesis of silicon carbide (SiC) nanostructures and their composites has been a topic of interest for the scientific community due to the unique properties that can be obtained with nanoscale features. Herein, we report the scalable fabrication of anisotropic and low density, carbon nanotube/SiC (CNT/SiC) core-shell structures synthesized via chemical vapor infiltration (CVI) of silicon on aligned CNT foams followed by heat treatment at 1350 °C. Structures made of CNT/SiC nanotube networks with a thickness of 1 cm and length of 9 cm were prepared in the present work. Upon the removal of the CNT foam via calcination of the hybrid nanocomposite in air, a free-standing mechanically robust three-dimensional network of pure SiC nanotubes was left behind. The density of the synthesized CNT/SiC is the lowest reported for any C/SiC structure. Furthermore, the CNT/SiC hybrid nano-architecture demonstrated superb heat resistance and stability in ultrahigh temperature environment.     

Aligned carbon nanotube-reinforced silicon carbide composites produced by chemical vapor infiltration

A chemical vapor infiltration (CVI) technique was used to overcome most of the challenges involved in fabricating exceptionally-tough CNT/SiC composites. Nanotube pullout and sequential breaking and slippage of the walls of the CNTs during failure were consistently observed for all fractured CNT/SiC samples. These energy absorbing mechanisms result in the fracture strength of the CNT/SiC composites about an order of magnitude higher than the bulk SiC. The CVI-fabricated CNT/SiC composites have an strongly-bonded tube/matrix interface and an amorphous, crack-free SiC matrix, enabling the composites to withstand oxidization at 700–1600 °C in air.     

裂解碳包覆对SiC纳米纤维增强SiC陶瓷基复合材料性能的影响

以SiC纳米纤维(SiC_nf)为增强体,通过化学气相沉积在SiC纳米纤维表面沉积裂解碳(PyC)包覆层,并与SiC粉体、Al₂O₃-Y₂O₃烧结助剂共混制备陶瓷素坯,采用热压烧结工艺制备质量分数为10%的SiC纳米纤维增强SiC陶瓷基(SiC_nf/SiC)复合材料。研究了PyC包覆层沉积时间对SiC_nf/SiC陶瓷基复合材料的致密度、断裂面微观形貌和力学性能的影响。结果表明:在1 100 ℃下沉积60 min制备的PyC包覆层厚度为10 nm,且为结晶度较好的层状石墨结构;相比于纤维表面无包覆层的复合材料,复合材料的断裂韧性提高了35%,达到最大值(19.35±1.17) MPa·m^1/2,抗弯强度为(375.5±8.5) MPa,致密度为96.68%。复合材料的断裂截面可见部分纳米纤维拔出现象,但SiC_nf/SiC陶瓷基复合材料界面结合仍较强,纳米纤维拔出短,表现为脆性断裂。     

Highly conductive and high-strength carbon nanotube film reinforced silicon carbide composites

Film formed by carbon nanotubes is usually called carbon nanotube film (CNT_f). In the present study, CNT_f fabricated by floating catalyst method was used to prepare CNT_f/SiC ceramic matrix composites by chemical vapor infiltration (CVI). Mechanical and electrical properties of the resulting CNT_f/SiC composites with different CVI cycles were investigated and discussed, and the results revealed that the CNT_f has a good adaptability to CVI method. Tensile test demonstrated an excellent mechanical performance of the composites with highest tensile strength of 646 MPa after 2 CVI cycles, and the strength has a decline after 3 CVI cycles for an excessively dense matrix. While, the elastic modulus of the composite increased with the CVI cycles and reached 301 GPa after 3 CVI cycles. Tensile fracture morphologies of the composites were analyzed by scanning electron microscope to study the performance change laws with the CVI cycles. With SiC ceramic matrix infiltrated into the CNT_f, enhanced electrical conductivity of the CNT_f/SiC composite compared to pure CNT_f was also obtained, from 368 S/cm to 588 S/cm. Conductivity of the SiC matrix with free carbon forming in the CVI process was considered as the reason.     

Anisotropic compressive properties of porous CNT/SiC composites produced by direct matrix infiltration of CNT aerogel

Carbon nanotube‐reinforced silicon carbide composites (CNT/SiC) produced by direct infiltration of matrix into a porous CNT arrays have been demonstrated to possess a unique microstructure and excellent micro‐mechanical properties. However, the thickness of the array preforms is usually very small, typically less than 2 mm. Therefore, fabrication of macroscopic CNT/SiC composites by chemical vapor infiltration (CVI) process requires that the nanoscale fillers could form macroscopic architectures with an open pore network. Here, this study reports an experimental strategy for the fabrication of SiC matrix composites reinforced by CNT based on an ice‐segregation‐induced self‐assembly (ISISA) technique. Macroscopic CNT aerogel with well‐defined macroporous network was produced by ISISA technique and was subsequently infiltrated by SiC in a CVI reactor. After five CVI cycles, the porosity of as‐fabricated composites was 11.6±0.3% and the machined specimens exhibited lamellar structure with parallel lamellaes intersected at discrete angles. By observed, there are in fact five different representative anisotropic macrostructures, the compressive strengths of these five different loading modes with respect to lamella orientation were 933±55, 619±34, 200±45, 199±21, and 297±41 MPa, respectively, and the failure mechanisms were attributed to the anisotropic nature of the macrostructures. Energy dissipation toughening mechanism at the nanoscale such as CNT pull‐out was observed and the phase composition of the fabricated materials included β‐SiC, CNT, and SiO₂.     

Effect of the fabrication process on the microstructural evolution of carbon fibers and flexural property on C/SiC composites by the NITE method

Nano-infiltration and transient eutectic phase (NITE) SiC matrix composites are designed for application in aerospace propulsion systems, particularly in fasteners and thrusters. A variety of carbon fibers with different properties have been selected as reinforcements for SiC matrix composites. Carbon fibers are known to be stable at high temperatures; however, the effects of high applied pressure at high temperatures on the fiber microstructure evolution and mechanical properties are not well-known. As a scoping study for fabricating NITE C/SiC composites, the behaviors of various carbon fibers in SiC composites. Pitch-based fibers, namely, GRANOX XN-05 and YS-90A, and a polyacrylonitrile-based fiber, namely, TORAYCA T-300B, were selected for matrix reinforcement. The 3-point bending test results indicated pseudo-ductile behaviors in the cases of YS-90A and T-300B fiber reinforcements. Fracture resistance evaluation based on the single-notch bending test indicated that the YS-90A fiber reinforced composite afforded the highest fracture resistance among the three C/SiC composites. The microstructure evolution on YS-90A and T-300B fibers was limited to near the fiber surface. Therefore, YS-90A and T-300B carbon fibers are potential candidates for reinforcement in NITE C/SiC composites.     

Poly(propylene) composite with hybrid nanofiller: Dynamic properties

Mechanical, impact, and relaxation properties of in situ synthesized carbon nanotubes‐polyaniline (CNT‐PANi) hybrid nanoparticle‐filled poly(propylene) (PP) composites with or without an amphiphilic dispersing agent were investigated using tensile testing, notched Charpy impact testing, and dynamical mechanical testing methods. The reference material was MWCNT filled PP composite. Ethyl gallate (EG) was the dispersing agent which realizes high conductivity in PP composites with hybrid filler. Measured properties showed quite similar behavior of CNT‐PANi hybrid and neat CNT filled composites. Addition of 20% EG in PP did not cause essential differences compared to the neat PP. When the dispersing agent was added in filler containing PP composites, remarkable effects were observed, especially in PP‐hybrid composites. Mechanically, these materials had improved tensile properties, but they were brittle compared to the materials without dispersing agent. Dynamic mechanical analysis showed improvement in storage modulus, and in loss modulus the α transition was well observable. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013     

Preparation and mechanical behaviors of SiOC-modified carbon-bonded carbon fiber composite with in-situ growth of three-dimensional SiC nanowires

Carbon-bonded carbon fiber (CBCF) composites are novel and important high-temperature insulation materials owing to their light weight, low thermal conductivity and high fracture tolerance. To further improve the mechanical property of CBCF composite, we propose a three-dimensional (3D) SiC nanowires structure, which is in situ grown on a CBCF matrix via directly annealing silicon oxycarbide (SiOC) ceramic precursor. The synthesized multiscale reinforcements including microscale SiOC ceramics and nanoscale SiC nanowires are mainly attributed to the initial phase separation of SiOC phase and subsequent solid-phase reaction of SiO and C phases. Compared to SiOC/CBCF composite, the resulting 3D SiC nanowires/SiOC/CBCF hybrid structure exhibited high flexural/tensile strength and fractured strain due to the pull-out and bridging behavior of SiC nanowires. This one-step process supplied a feasible way to synthesize 3D SiC nanowires to reinforce and toughen SiOC-modified CBCF composite.     

Effect of Processing Temperature on the Morphology of Silicon Carbide Whiskers

Two kinds of SiC whiskers were annealed at temperatures similar to those for the processing of ceramic matrix composites. The morphology and structure of the as-received and postannealed whiskers were investigated by SEM, TEM, and XRD, and the influence of processing temperature on the mechanical properties of ceramic matrix composites was discussed.     

Unified tensile model for unidirectional ceramic matrix composites with degraded fibers and interface

In order to overcome the roughness of the previously proposed micromechanical model [Acta Mech. Sin. (2011) 382], an enhanced multiscale analytical model was thus developed based on the rule of mixture, shear-lag theory and statistical approach to forecast the load carrying capacity of the prestressed ceramic matrix composites (CMCs) subjected to high-temperature oxidation. For comprehensive characterization of the mechanical degradation mechanisms, the oxidation induced fiber necking (or embrittlement) and fiber-matrix interface weakening were both taken into account. The suggested model was then applied to 2D-C/SiC composites. The influences of interface friction resistance, interface recession length, fiber necking factor and oxidation duration upon the residual mechanical property were investigated. Parametric analysis demonstrates that the modified formulations are much more reasonable than the previous model. The predicted residual tensile modulus and strength for the 2D-C/SiC composite agree well with the experimental data and furthermore the microscopic damage mechanisms were correlated properly with the macroscopic fracture morphologies.     

模压压力对SiC/SiC复合材料力学性能及力学行为的影响

采用热模压辅助聚合物先驱体浸渍裂解工艺制备了国产近化学计量比SiC纤维增强SiC陶瓷基复合材料,通过阿基米德排水法和SEM技术对SiC/SiC复合材料致密化过程进行表征,采用弯曲强度、拉伸强度和断裂韧性对SiC/SiC复合材料力学性能和力学行为进行评价。研究表明,热模压压力是影响材料结构和性能的重要因素,热模压在提升材料致密度的同时,亦造成纤维的损伤。随着热模压压力的增加,SiC/SiC复合材料力学性能先增加后降低。热模压压力适中时,致密度增加因素占优,材料力学性能较为优异;热模压压力较大时候,热模压操作对纤维性能的损伤因素逐渐凸显,基体致密化和纤维损伤两种作用机制相当。     

Microstructure and mechanical properties of SiC platelet reinforced BaOAl2O32SiO2 (BAS) composites

BaOAl₂O₃2SiO₂ (BAS) glass–ceramic powders were prepared by sol–gel technique. SiC platelet reinforced BAS glass–ceramic matrix composites with high density and uniform microstructure were fabricated by hot-pressing. The effect of additional crystalline seeds on hexagonal to monoclinic phase transformation of Barium aluminosilicate was studied. The effects of SiC platelet content on the microstructure and mechanical properties of the composites were also investigated. The results showed that the flexural strength and fracture toughness of the BAS glass–ceramic matrix composites can be effectively improved by the addition of silicon carbide platelets. The main toughening mechanism was crack deflection, platelets' pull-out and bridging. The increased value of flexural strength is contributed to the load transition from the matrix to SiC platelets.     

Effect of strain rate on the tensile properties of mini-SiC/SiC composites

SiC/SiC composites are the ideal candidates for hot-end components in aerospace and other high-tech fields. In recent years, as one type of material with simple structures, mini-composites have been widely used to study or initially verify the properties of ceramic matrix composites (CMC). Nevertheless, attentions were rarely paid on the influence of strain rate on the mechanical properties of mini-composites. In this study, based on mini-SiC/SiC composites, we investigated the effect of the strain rate on their tensile strength, initial tensile modulus, Weibull modulus, and fracture work. Furthermore, the underlying mechanisms were discussed and the exact constitutive model of the as-prepared mini-SiC/SiC composites was constructed according to the Michaelis-Menten and generalized linear models. This work can fill the gaps in the CMC research in some degree and provide a preliminary theoretical basis for the formulation of tensile properties test standards of mini-composites.     

Effect of SiC Particles on Mechanical Properties of Laminated (SiCw+SiCp)/SiC Ceramic Composites

Laminated (SiC_w+SiC_p)/SiC ceramic composites were fabricated by tape casting and chemical vapor infiltration (CVI), and the effect of SiC particles on strengthening/toughening of the composites was investigated. When the SiC particle content was constant, the mechanical properties of (SiC_w+SiC_p)/SiC composites were increased with increasing SiC whisker content. When the SiC particle content was varied, the mechanical properties of (SiC_w+SiC_p)/SiC composites were dependent on SiC particle content. The addition of SiC particles can increase the strength of the matrix and the crack propagation resistance, the former increased the strength and the latter increased the toughness.     

Establishing microstructure-mechanical property correlation in ZrB2-based ultra-high temperature ceramic composites

The current work focuses on enhancing the flexural strength and fracture toughness of zirconium diboride (ZrB₂) reinforced with silicon carbide (SiC) and carbon nanotubes (CNT). The flexural strength has shown to increase by ~ 1.2 times from 322.8 MPa (for ZrB₂) to 390.7 MPa and fracture toughness up to 3 times from 3.2 MPam^0.5 (for ZrB₂) to 9.5 MPam^0.5 with the synergistic addition of both SiC and CNT in ZrB₂ matrix through energy dissipating mechanisms such as deflection, branching and strong interfacial bonding evidenced from the transmission electron microscopy (TEM). A modified fractal model is used to evaluate the fracture toughness and delineate the contribution of residual stresses, and reinforcements (SiC and CNT) in enhancing the fracture toughness. Interfacial bonding, in terms of a debonding factor, was also evaluated by theoretically predicting the elastic modulus and then correlated with the microstructure along with other mechanical properties of ZrB₂-SiC-CNT composites.     

Strengthening/toughening of 2D C/SiC composites by coating

SiC and SiC_w/SiC coatings were prepared on two-dimensional carbon fiber reinforced silicon carbide ceramic matrix composites (2D C/SiC), and strengthening/toughening of the composite by the coatings was investigated. After coating, the density of the C/SiC composites was increased effectively and the mechanical properties were improved significantly. Compared with SiC coating, SiC_w/SiC coating showed the more significant effect on strength/toughness of the composites. Coatings had two effects: surface strengthening and matrix strengthening. The latter was the dominant effect. The surface strengthening can increase the crack initiation stress, while the matrix strengthening can enhance the crack propagation resistance. The former effect increased the strength and the latter effect increased the toughness.