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。     

界面类型对三维Nextel 720纤维增韧莫来石陶瓷基复合材料力学性能的影响

采用化学气相渗透工艺在Nextel 720纤维表面制备PyC和PyC／SiC两种涂层，然后以正硅酸乙酯和异丙醇铝作为先驱体，以先驱体浸渗热解法制备三维Nextd 720纤维增韧莫来石陶瓷基复合材料，比较分析了两种涂层复合材料的力学性能和断裂模式。结果表明：具预先涂覆PyC的复合材料中纤维与基体直接接触，发生烧结形成强结合界面，复合材料脆性断裂，三点抗弯强度仅56MPa。PyC／SiC涂层则演化为间隙／SiC复合界面层，SiC成为阻滞纤维与基体接触的阻挡层，间隙保证了纤维拔出，复合材料韧性断裂且三点抗弯强度高达267．2MPa。     

Influence of Interface Characteristics on the Mechanical Properties of Hi-Nicalon type-S or Tyranno-SA3 Fiber-Reinforced SiC/SiC Minicomposites

The tensile behavior of CVI SiC/SiC composites with Hi-Nicalon type-S (Hi-NicalonS) or Tyranno-SA3 (SA3) fibers was investigated using minicomposite test specimens. Minicomposites contain a single tow. The mechanical behavior was correlated with microstructural features including tow failure strength and interface characteristics. The Hi-NicalonS fiber-reinforced minicomposites exhibited a conventional damage-tolerant response, comparable to that observed on composites reinforced by untreated Nicalon or Hi-Nicalon fibers and possessing weak fiber/matrix interfaces. The SA3 fiber-reinforced minicomposites exhibited larger interfacial shear stresses and erratic behavior depending on the fiber PyC coating thickness. Differences in the mechanical behavior were related to differences in the fiber surface roughness.     

High-dose,intermediate-temperature neutron irradiation effects on silicon carbide composites with varied fiber/matrix interfaces

SiC/SiC composites are promising structural candidate materials for various nuclear applications over the wide temperature range of 300–1000 °C. Accordingly, irradiation tolerance over this wide temperature range needs to be understood to ensure the performance of these composites. In this study, neutron irradiation effects on dimensional stability and mechanical properties to high doses (11–44 dpa) at intermediate irradiation temperatures (?600 °C) were evaluated for Hi-Nicalon Type-S or Tyranno-SA3 fiber–reinforced SiC matrix composites produced by chemical vapor infiltration. The influence of various fiber/matrix interfaces, such as a 50–120 nm thick pyrolytic carbon (PyC) monolayer interphase and 70–130 nm thick PyC with a subsequent PyC (?20 nm)/SiC (?100 nm) multilayer, was evaluated and compared with the previous results for a thin-layer PyC (?20 nm)/SiC (?100 nm) multilayer interphase. Four-point flexural tests were conducted to evaluate post-irradiation strength, and SEM and TEM were used to investigate microstructure. Regardless of the fiber type, monolayer composites showed considerable reduction of flexural properties after irradiation to 11–12 dpa at 450–500 °C; and neither type showed the deterioration identified at the same dose level at higher temperatures (>750 °C) in a previous study. After further irradiation to 44 dpa at 590–640 °C, the degradation was enhanced compared with conventional multilayer composites with a PyC thickness of ?20 nm. Multilayer composites have shown comparatively good strength retention for irradiation to ?40 dpa, with moderate mechanical property degradation beginning at 70–100 dpa. Irradiation-induced debonding at the F/M interface was found to be the major cause of deterioration of various composites.     

Siliconization elimination for SiC coated C/C composites by a pyrolytic carbon coating and the consequent improvement of the mechanical property and oxidation resistances

Carbon/carbon (C/C) composites have a wide application as the thermal structure materials because of their excellent properties at high temperatures. However, C/C composites are easily oxidized in oxygen-containing environment, which limits their potential applications to a great degree. Silicon carbide (SiC) ceramic coating fabricated via pack cementation (PC) was considered as an effective way to protect C/C composites against oxidation. But the mechanical properties of C/C composites were severely damaged due to chemical reaction between the molten silicon and C/C substrate during the preparation of SiC coating by PC. In order to eliminate the siliconization erosion, a pyrolytic carbon (PyC) coating was pre-prepared on C/C composites by the chemical vapor infiltration (CVI) prior to the fabrication of SiC coating. Due to the retardation effect of PyC coating on siliconization erosion, the flexural strength retention of the SiC coated C/C composites with PyC coating increased from 46.27 % to 107.95 % compared with the specimen without PyC coating. Furthermore, the presence of homogeneous and defect-free PyC coating was beneficial to fabricate a compact SiC coating without silicon phase by sufficiently reacting with molten silicon during PC. Therefore, the SiC coated C/C composites with PyC coating had better oxidation resistances under dynamic (between room temperature and 1773 K) and static conditions in air at different temperatures (1773?1973 K).     

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.     

Mechanical properties and strengthening mechanism of SiCf/SiC mini-composites modified by SiC nanowires

The effects of the SiC nanowires (SiCNWs) and PyC interface layers on the mechanical and anti-oxidation properties of SiC fiber (SiC_f)/SiC composites were investigated. To achieve this, the PyC layer was coated on the SiC_f using a chemical vapour infiltration (CVI) method. Then, SiCNWs were successfully coated on the surface of SiC_f/PyC using the electrophoretic deposition method. Finally, a thin PyC layer was coated on the surface of SiC_f/PyC/SiCNWs. Three mini-composites, SiC_f/PyC/SiC, SiC_f/PyC/SiCNWs/SiC, and SiC_f/PyC/SiCNWs/PyC/SiC, were fabricated using the typical precursor infiltration and pyrolysis method. The morphologies of the samples were examined using scanning electron microscopy and energy dispersive X-ray spectrometry. Tensile and single-fibre push-out tests were carried out to investigate the mechanical performance and interfacial shear strength of the composites before and after oxidization at 1200 °C. The results revealed that the SiC_f/PyC/SiCNWs/SiC composites showed the best mechanical and anti-oxidation performance among all the composites investigated. The strengthening and toughening is mainly achieved by SiCNWs optimization of the interfacial bonding strength of the composite and its own nano-toughening. On the basis of the results, the effects of SiCNWs on the oxidation process and retardation mechanism of the SiC_f/SiC mini-composites were investigated.     

The improvement of mechanical properties of SiC/SiC composites by in situ introducing vertically aligned carbon nanotubes on the PyC interface

In order to improve the mechanical properties, vertically aligned carbon nanotubes (VACNTs) were in situ introduced on the pyrocarbon (PyC) interfaces of the multilayer preform via chemical vapor deposition (CVD) process under tailored parameters. Chemical vapor infiltration (CVI) process was then employed to densify the multilayer preform to acquire SiC/SiC composites. The results show that the growth of VACNTs on PyC interface is highly dependent to the deposition temperature, time and constituent of gas during CVD process. The preferred orientation and high graphitization of VACNTs were obtained when temperature is 800?℃ and C₂H₄/H₂ ratio is 1:3. The bending strength and fracture toughness of SiC/SiC composites with PyC and PyC-VACNTs interfaces were compared. Compared to the SiC/SiC composite with PyC interface, the bending strength and fracture toughness increase 1.298 and 1.359 times, respectively after the introduction of PyC-VACNTs interface to the SiC/SiC composites. It is also demonstrated that the modification of PyC interface with VACNTs enhances the mechanical properties of SiC/SiC composites due to the occurrence of more fiber pull-outs, interfacial debonding, crack branching and deflection     

Fabrication of C/SiC composites by siliconizing carbon fiber reinforced nanoporous carbon matrix preforms and their properties

Reactive melt infiltration (RMI) has been proved to be one of the most promising technologies for fabrication of C/SiC composites because of its low cost and short processing cycle. However, the poor mechanical and anti-ablation properties of the RMI-C/SiC composites severely limit their practical use due to an imperfect siliconization of carbon matrixes with thick walls and micron-sized pores. Here, we report a high-performance RMI-C/SiC composite fabricated using a carbon fiber reinforced nanoporous carbon (NC) matrix preform composed of overlapping nanoparticles and abundant nanopores. For comparison, the C/C performs with conventional pyrocarbon (PyC) or resin carbon (ReC) matrixes were also used to explore the effect of carbon matrix on the composition and property of the obtained C/SiC composites. The C/SiC derived from C/NC with a high density of 2.50 g cm^?3 has dense and pure SiC matrix and intact carbon fibers due to the complete ceramization of original carbon matrix and the almost full consumption of inspersed silicon. In contrast, the counterparts based on C/PyC or C/ReC with a low density have a little SiC, much residual silicon and carbon, and many corroded fibers. As a result, the C/SiC from C/NC shows the highest flexural strength of 218.1 MPa and the lowest ablation rate of 0.168 µm s^?1 in an oxyacetylene flame of ～ 2200 °C with a duration time of 500 s. This work opens up a new way for the development of high-performance ceramic matrix composites by siliconizing the C/C preforms with nanoporous carbon matrix.     

High-temperature flexural strength of I-CVI processed Cf/SiC composites with variable interphases

The effect of single-layer pyrocarbon (PyC) and multilayered (PyC/SiC)_n=4 interphases on the flexural strength of un-coated and SiC seal-coated stitched 2D carbon fiber reinforced silicon carbide (C_f/SiC) composites was investigated. The composites were prepared by I-CVI process. Flexural strength of the composites was measured at 1200 °C in air atmosphere. It was observed that irrespective of the type of interphase, the seal coated samples showed a higher value of flexural strength as compared to the uncoated samples. The flexural strength of 470 ± 12 MPa was observed for the seal coated C_f/SiC composite samples with multilayered interphase. The seal coated samples with single layer PyC interphase showed flexural strength of 370 ± 20 MPa. The fractured surfaces of tested samples were analyzed in detail to study the fracture phenomena. Based on microstructure-property relations, a mechanism has been proposed for the increase of flexural properties of C_f/SiC composites having multilayered interphase.     

Oxidation and erosion resistance of multi-layer SiC nanowires reinforced SiC coating prepared by CVD on C/C composites in static and aerodynamic oxidation environments

A multi-layer SiC nanowires reinforced SiC (SiCnws-SiC) coating was prepared in-situ on carbon/carbon (C/C) composites by three chemical vapor deposition (CVD) processes. The microstructure and phase composition of the nanowires fabricated on the first-layer SiCnws-SiC coating and the coatings were examined by SEM, TEM, and XRD. The bamboo-like SiC nanowires with a 50?nm diameter and a length of several tens of micrometers are straight, randomly orientated and distributed like a net on the first-layer SiCnws-SiC coating. The growth direction is [111], and the growth mechanism is VS. The multi-layer SiCnws-SiC coating has three layers: the thickness of the first-layer is roughly 400?µm, and the outer two layers are about 200?µm. Each layer has a sandwich structure. The isothermal oxidation and erosion resistance of the multi-layer SiCnws-SiC coating were investigated in an electrical furnace and a high temperature wind tunnel. The results indicated that the weight loss of the multi-layer SiCnws-SiC coated C/C composites was only 1.8% after oxidation in static air at 1773?K for 361?h. Further, the coated sample failed due to fracture of the coating at the clamping position (i.e. 80?mm) after erosion at 1873?K for 130?h in the wind tunnel. The weight loss of the coated C/C composites occurred due to the formation of penetrating cracks in the coating during the oxidation thermal shock. The maximum bending moment and the larger clamping force caused the coating fracture and resulted in intense oxidation of the substrate and the failure of the specimen.     

Environment-friendly deposition of SiCN interlayer for reinforcing carbon fibers in C/SiC composites

Several C/SiC composites with no interlayer, single pyrocarbon (PyC) interlayer and PyC/SiCN interlayer were fabricated by polymer infiltration and pyrolysis process. The microstructure and mechanical properties were investigated. The results verified that SiCN interlayer was formed on carbon fibers. Both bulk density and flexural stress of C/SiC composite with PyC/SiCN interlayer were slightly higher than composite fabricated with single PyC interlayer. When the weight fraction of SiCN interlayer in the composite was about 18 wt%, the flexural stress of the composite was enhanced to 416 MPa from 352 MPa for composite with single PyC interlayer. The observations of pulled-out fibers on fracture surfaces revealed non-catastrophic fracture features for PyC/SiCN deposited C/SiC composite.     

Fabrication and characteristic of non-oxide fiber tow reinforced silicon nitride matrix composites by low temperature CVI process

Non-oxide fiber tow reinforced silicon nitride matrix composite was fabricated by low temperature CVI process with PyC as interphase. The tensile strength of the C and SiC fiber tow composites were 547 MPa and 740 MPa, respectively. The difference in tensile strength was analyzed based on the length, amount of pull-out fiber and also interface bonding. The infiltration uniformity of CVI silicon nitride (SiN) matrix within SiC fiber tow was comparable with that of CVI SiC matrix. These results suggested that the low temperature CVI process is suitable for the fabrication of fiber reinforced SiN matrix composites with proper interface bonding and high strength.     

Flexural modulus of SiC/SiC composites sintered by microwave and conventional heating

To deeply study the variation mechanisms of mechanical properties, flexural modulus of SiC fibers reinforced SiC matrix (SiC/SiC) composites prepared by conventional and microwave heating at 800?°C–1100?°C was discussed in detail. The elastic modulus of fibers and matrix, interface bonding strength and porosity of SiC/SiC composites were considered together to analyze the changing tendencies and differences in their flexural modulus. The elastic modulus of fiber and matrix was determined by nanoindentation technique and interface characteristics applying fiber push-out test. The porosity and microstructure examinations were characterized by mercury intrusion method, X-ray Diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). Moreover, two conflicts between the changing trends of elastic modulus and chemical compositions of composite components were focused and explained. Results indicate that three factors played different roles in the flexural modulus of SiC/SiC composites and residual tensile stress in composite components led to the conflicts between their elastic modulus and chemical compositions.     

Tailoring Carbon Fiber/Carbon Nanotubes Interface to Optimize Mechanical Properties of Cf‐CNTs/SiC Composites

C_f/SiC composites were fabricated using fiber coatings including CNTs and matrix infiltration using the polymer impregnation and pyrolysis process. Interface between fiber and CNTs (CF/CNTs) was tailored to optimize mechanical properties of hybrid composites. The tailored interphases, such as Pyrocarbon (PyC) and PyC/SiC, protect fibers from degradation during the growth of CNTs successfully. Hybrid composites with well‐tailored CF/CNTs interface displayed significantly increased mechanical strength (352 ± 21 MPa) compared with that (34 ± 3 MPa) of composites reinforced with CNTs, which grown on carbon fibers directly. The interfacial bonding strength of hybrid composites was improved and optimized by tailoring the CF/CNTs interface. Interfacial failure modes were studied, and a firm interface bonding at the joint where CNTs grown was observed.     

Effect of pyrolytic carbon interphase on mechanical properties of mini T800-C/SiC composites

The effect of pyrolytic carbon(PyC) thickness on the tensile property of mini T800 carbon fiber reinforced SiC matrix composites(C/SiC) was studied. PyC interphase was prepared by chemical vapor infiltration(CVI) process using C3H6–Ar as gas source, the PyC thickness was adjusted from 0 to 400 nm, and then the SiC matrix was prepared by CVI process using methyltrichlorosilane(MTS)–H2–Ar as precursor and gas source. The results showed that the tensile strength of mini T800-C/SiC increased first and then decreased with the increase of the PyC thickness. When the thickness of PyC was 100 nm, the average strength reached the maximum value of 393 ± 70 MPa. The Weibull modulus increased from 2.0 to 8.06 with the increase of PyC thickness, and the larger the Weibull modulus, the smaller the dispersion, which indicated that the regulation of PyC thickness was conducive to improve tensile properties.     

低压化学气相渗透法制备2.5维SiCf/SiC复合材料

采用低压化学气相渗透法制备了具有和不具有热解炭界面层的2.5维连续SiC纤维增强的SiC复合材料(SiCf/SiC).SiC纤维的体积分数为30%和41%.所制备复合材料的气孔率为20%左右.当纤维为30%时,沉积有0.1 μm热解炭界面层的复合材料的弯曲强度由未加热解炭界面层的232MPa增加到328MPa,而且材料由灾难性断裂转变为非灾难性断裂.在同一制备条件下,纤维体积分数为41%的SiCf/SiC比30%的SiCf/SiC具有更高的气孔率.纤维为41%时,热解炭界面层厚度为0.1 μm的SiCf/SiC的弯曲强度只有244MPa,但是它具有更高的韧性和更长的纤维拔出长度.     

空间望远镜用C/SiC镜面研制综述

综述了空间望远镜的主镜用高强度、高表面精度、低热膨胀系数的低温（约4K）用镜面的制备和检测过程.日本将Φ710mm的高强度反应烧结SiC材料已用于红外望远镜镜面.在短切炭纤维增强C/C复合材料毛坯的基础上进行液相硅渗透（LSI）而制备的C/SiC复合材料在光学镜面方面具有更大的优势.通过提高C/C复合材料毛坯中沥青基炭纤维体积分数及控制硅化速度,可有效地提高LSI-C/SiC复合材料的机械性能和表面光学精度;通过不同规格的炭纤维的混杂化,可使C/SiC复合材料热膨胀系数的各向异性降低至小于4％的差异.SiC、Si-SiC浆料涂层处理可有效地提高表面精度至2 nm rms的极高要求.     

Fiber Coatings for SiC-Fiber-Reinforced BMAS Glass-Ceramic Composites

Interfaces in SK-fiber-reinforced glass-ceramic matrix composites were modified by applying different coatings to the fibers and varying the coating thickness. Coatings of SiC/BN, Si₃N₄/BN, and BN were applied to the fibers by CVD prior to composite fabrication. Interfacial microstructures were characterized using high-resolution and analytical transmission electron microscopy. Oxidation of the SiC fibers during composite fabrication was suppressed by the fiber coatings, provided that the coatings were sufficiently thick to prevent oxygen diffusion from the matrix. The SiC/RN and BN coatings were stable during high-temperature exposures, while the Si₃N₄/BN coating underwent chemical reactions.     

The effects of phenolic resin-derived PyC interlayers on microstructure and mechanical properties of Cf/SiC composites

A novel, easy and cost-effective way, infiltration and pyrolysis of phenolic resin solution, was exploited to prepare pyrolytic carbon (PyC) interlayers for carbon fiber/silicon carbide (Cf/SiC) mini-composites. X-ray photoelectron spectroscopy, dynamic contact angle measurement and scanning electron microscope were carried out to characterize chemical structure of carbon fibers (CFs), wetting properties between CFs and phenolic resin solution and microstructure of CFs and their composites, respectively. Remarkably, SEM results showed regulation of uniformity and thicknesses of PyC interlayer could be achieved through controlling the concentration of phenolic resin solution and oxidation condition of CFs. When CFs were treated by 10?min' oxidation with 40?mg/L ozone followed by dip-coating with 4?wt% phenolic solution, uniform PyC interlayer with approximately 120?nm were prepared on CFs. The corresponding Cf/SiC specimens had the largest increase in tensile strength and work of fracture with the improvement of 26.2% and 71.6% from the PyC-free case.