Fabrication and Properties of Ti3SiC2/SiC Composites

Ti3SiC2/SiC composites were fabricated by reactive hot pressing method. Effects of hot pressing temperature, the content and particle size of SiC on phase composition, densification, mechanical properties and behavior of stress-strain of the composites were investigated. The results showed that ： （ 1 ） Hot-pressing temperature influenced the phase composition of Ti3SiC2/SiC composites. The flexural strength and fracture toughness of composites increased with hot pressing temperature. （2） It became more difficult for the composites to densify when the content of SiC in composites increased. It need be sintered at higher temperature to get denser composite. The flexural strength and fracture toughness of composites increased when the content of SiC added in composites increased. However, when the content of SiC reached 50 wt%, the flexural strength and fracture toughness of composites decreased due to high content of pore in composites. （3） When the content of SiC was same, Ti3SiC2/SiC composites were denser while the particle size of SiC added in composites is 12. 8 μm compared with the composites that the particle size of SiC added is 3 μm. The flexural strength and fracture toughness of composites increased with the increase of particle size of SiC added in composites. （4） Ti3SiC2/SiC composites were non-brittle fracture at room temperature.     

Appropriate thickness of pyrolytic carbon coating on SiC fiber reinforcement to secure reasonable quasi-ductility on NITE SiC/SiC composites

Pyrolytic carbon (PyC) coating of silicon carbide (SiC) fibers is an important technology that creates quasi-ductility to SiC/SiC composites. Nano-infiltration and transient eutectic-phase (NITE) process is appealing for the fabrication of SiC/SiC composites for use in high temperature system structures. However, the appropriate conditions for the PyC coating of the composites have not been sufficiently tested. In this research, SiC fibers, with several thick PyC coatings prepared using a chemical vapor infiltration continuous furnace, were used in the fabrication of NITE SiC/SiC composites. Three point bending tests of the composites revealed that the thickness of the PyC coating affected the quasi-ductility of the composites. The composites reinforced by 300?nm thick coated SiC fibers showed a brittle fracture behavior; the composites reinforced 500 and 1200?nm thick PyC coated SiC fibers exhibited a better quasi-ductility. Transmission electron microscope research revealed that the surface of the as-coated PyC coating on a SiC fiber was almost smooth, but the interface between the PyC coating and SiC matrix in a NITE SiC/SiC composite was very rough. The thickness of the PyC coating was considered to be reduced maximum 400?nm during the composite fabrication procedure. The interface was possibly damaged during the composite fabrication procedure, and therefore, the thickness of the PyC coating on the SiC fibers should be thicker than 500?nm to ensure quasi-ductility of the NITE SiC/SiC composites.     

Enhancement of the microwave absorption properties of PyC-SiCf/SiC composites by electrophoretic deposition of SiC nanowires on SiC fibers

The employment of coating technique on the silicon carbide fibers plays a pivotal role in preparing SiC fiber-reinforced SiC composites (SiC_f/SiC) toward electromagnetic wave absorption applications. In this work, SiC nanowires (SiCNWs) are successfully deposited onto the pyrolytic carbon (PyC) coated SiC fibers by an electrophoretic deposition method, and subsequently densified by chemical vapor infiltration to obtain SiCNWs/PyC-SiC_f/SiC composites. The results reveal that the introduction of SiCNWs could markedly enhance the microwave absorption properties of PyC-SiC_f/SiC composites. Owing to the increasing of SiCNWs loading, the minimum reflection loss of composites raises up to −58.5 dB in the SiCNWs/PyC-SiC_f/SiC composites with an effective absorption bandwidth (reflection loss ≤ −10 dB) of 6.13 GHz. The remarkable enhancement of electromagnetic wave absorption performances is mainly attributed to the improved dielectric loss ability, impedance matching and multiple reflections. This work provides a novel strategy in preparing SiC_f/SiC composites with excellent electromagnetic wave absorption properties.     

纳米SiC粒子的表面处理对PTFE/纳米SiC复合材料的性能影响

对表面处理与未处理纳米SiC填充的聚四氟乙烯(PTFE)复合材料进行力学与摩擦学性能测试,研究了纳米SiC含量和表面处理对复合材料力学和摩擦磨损性能的影响,用扫描电子显微镜对拉伸断面形貌进行观察,探讨了复合材料的增强机理。结果表明,未处理纳米SiC填充PTFE后,其复合材料的硬度和耐磨性均有不同程度的提高;表面处理纳米SiC后,PTFE/纳米SiC复合材料的拉伸强度、冲击强度、减摩性能均比未处理的有所提高;表面处理SiC在PTFE基体中有较好的分散性,与PTFE基体界面的结合较好,未处理纳米SiC在PTFE基体中分散性较差。     

Pressure‐less joining of C/SiC and SiC/SiC by a MoSi2/Si composite

A MoSi₂/Si composite obtained in situ by reaction of silicon and molybdenum at 1450°C in Ar flow is proposed as pressure‐less joining material for C/SiC and SiC/SiC composites. A new “Mo‐wrap” technique was developed to form the joining material and to control silicon infiltration in porous composites. MoSi₂/Si composite joining material infiltration inside coated and uncoated C/SiC and SiC/SiC composites, as well as its microstructure and interfacial reactions were studied. Preliminary mechanical strength of joints was tested at room temperature and after aging at service temperatures, resulting in interlaminar failure of the composites in most cases.     

Effect of BN nanoparticle content in SiC matrix on microstructure and mechanical properties of SiC/SiC composites

BN-nanoparticle-containing SiC-matrix-based composites comprising SiC fibers and lacking a fiber/matrix interface (SiC/BN + SiC composites) were fabricated by spark plasma sintering (SPS) at 1800°C for 10 min under 50 MPa in Ar. The content of added BN nanoparticles was varied from 0 to 50 vol.%. The mechanical properties of the SiC/BN + SiC composites were investigated thoroughly. The SiC/BN + SiC composites with a BN nanoparticle content of 50 vol.%, which had a bulk density of 2.73 g/cm³ and an open porosity of 5.8%, exhibited quasiductile fracture behavior, as indicated by a short nonlinear region and significantly shorter fiber pullouts owing to the relatively high modulus. The composites also exhibited high strength as well as bending, proportional limit stress, and ultimate tensile strength values of 496 ± 13, 251 ± 30, and 301 MPa ± 56 MPa, respectively, under ambient conditions. The SiC fibers with contents of BN nanoparticles above 30 vol.% were not severely damaged during SPS and adhered to the matrix to form a relatively weak fiber/matrix interface.     

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。     

Effect of SiC nanowires on the high-temperature microwave absorption properties of SiCf/SiC composites

SiC-nanowire-reinforced SiC_f/SiC composites were successfully fabricated through an in situ growth of SiC nanowires on SiC fibres via chemical vapour infiltration. The dielectric and microwave absorption properties of the composites were investigated within the frequency range of 8.2–12.4 GHz at 25–600 °C. The electric conductivity and complex permittivity of the composites displayed evident temperature-dependent behaviour and were enhanced with increasing temperature. The composites exhibited superior microwave absorption abilities with a minimum reflection loss value of ?47.5 dB at 11.4 GHz and an effective bandwidth of 2.8 GHz at 600 °C. Apart from the contribution of the interconnected SiC nanowire network and multiple reflections, the excellent microwave absorption performance was attributed to dielectric loss that originated from SiC nanowires with abundant stacking faults and heterostructure interfaces. Results suggested that the composites are promising candidates for high-temperature microwave absorbing materials.     

Removal mechanism of SiC/SiC composites by underwater femtosecond laser ablation

Silicon carbide Ceramic matrix composites (SiC matrix with SiC fibers, abbreviated as SiC/SiC composites) are widely used in aerospace and energy applications due to their excellent resistance to high temperatures, corrosion, wear, and low density. However, the difficult machinability and surface oxidation of SiC/SiC composites are the main factors restricting their further application. To address these issues, this paper explores a novel method for underwater femtosecond laser ablation of SiC/SiC composites to obtain high cleanliness, low-oxidation microporous surfaces. This paper systematically analyses the changes in hole depth, material removal rate (MRR), surface morphology, and material components during underwater femtosecond laser ablation of SiC/SiC composites, and explains the formation of typical features such as induced cones, small banded pits, fiber debonding and shedding. Our work provides new research ideas for understanding the removal mechanism and surface oxidation resistance of SiC/SiC composites.     

Influence of precursor concentration on the densification efficiency and properties of SiC/SiC composites

The SiC/SiC composites were manufactured by polymer precursor impregnation pyrolysis process with near stoichiometric SiC fiber 2D preform as the reinforcing phase, the mixed solution of polycarbosilane (PCS), and xylene as impregnant. The effects of PCS concentration on the densification process, microstructure, and mechanical behavior of SiC/SiC composites were investigated using mechanical property testing, scanning electron microscopy, and other characterization techniques. Results showed the porosity and flexural strength of SiC/SiC composites increased first and then decreased with the increase of PCS concentration. When the concentration of PCS was 55% and 60%, the flexural strength of SiC/SiC composites reached 565.77 and 573.02 MPa, respectively. The mechanical behavior of SiC/SiC composites presented typical pseudoplastic characteristics such as fiber pulling-out, fiber bridging, and interface layer peeling, which would meet the dual requirements of optimizing the matrix and interface structure.     

Ni包裹SiC对SiC(Ni)/Fe复合材料性能的影响

分别以SiC粉体和Ni包裹的SiC复合粉体为硬质相,采用热压工艺(1000°C,20°C/min,40 MPa和45 min)制备了SiC含量为1 wt%~9 wt%的SiC/Fe复合材料。采用扫描电镜(SEM)、能谱仪(EDS)和X射线衍射仪(XRD)等研究了复合材料的界面反应物。研究结果表明:Ni过渡层的存在有效避免了SiC颗粒与Fe基体之间的化学反应。随着Ni包裹SiC粉体含量的增加,复合材料的相对密度和抗弯强度先增加后减小,当SiC(Ni)粉体含量为5 wt%时达到最大值。     

Effects of fabrication processes on the properties of SiC/SiC composites

Precursor infiltration and pyrolysis (PIP) and chemical vapor infiltration (CVI) were used to fabricate SiC/SiC composites on a four-step 3D SiC fibre preform deposited with a pyrolytic carbon interface. The effects of fabrication processes on the microstructure and mechanical properties of the SiC/SiC composites were studied. Results showed the presence of irregular cracks in the matrix of the SiC/SiC composites prepared through PIP, and the crystal structure was amorphous. The room temperature flexural strength and modulus were 873.62 MPa and 98.16 GPa, respectively. The matrix of the SiC/SiC composites prepared through CVI was tightly bonded without cracks, the crystal structure had high crystallinity, and the room temperature bending strength and modulus were 790.79 MPa and 150.32 GPa, respectively. After heat treatment at 1300 °C for 50 h, the flexural strength and modulus retention rate of the SiC/SiC composites prepared through PIP were 50.01% and 61.87%, and those of the composites prepared through CVI were 99.24% and 96.18%, respectively. The mechanism of the evolution of the mechanical properties after heat treatment was examined, and the analysis revealed that it was caused by the different fabrication processes of the SiC matrix. After heat treatment, the SiC crystallites prepared through PIP greatly increased, and the SiOxCy in the matrix decomposed to produce volatile gases SiO and/or CO, ultimately leading to an increase in the number of cracks and porosity in the material and a decrease in the material load-bearing capacity. However, the size of the SiC crystallites prepared through CVI hardly changed, the SiC matrix was tightly bonded without cracks, and the load-bearing capacity only slightly changed.     

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.     

连续碳化硅纤维增强碳化硅陶瓷基复合材料研究进展

碳化硅纤维增强碳化硅陶瓷基(SiC/SiC)复合材料具有轻质、耐高温、抗氧化的优异特性,在航空领域,如航空发动机的热端构件、高温结构功能一体化构件,航天及空天飞行器热防护结构部件、动力系统热端部件等领域具有广泛的应用前景,受到美国、欧洲、日本等国研究人员的广泛关注。本文从组成、制备工艺、加工工艺和考核应用等方面,综述了SiC/SiC复合材料的国内外研究进展,并指出了目前面临的问题和机遇。     

Interaction of fiber matrix bonding in SiC/SiC ceramic matrix composites

Non-oxide ceramic matrix composites (CMC) based on SiC fibers with SiC matrix were fabricated by polymer infiltration and pyrolysis (PIP) and characterized regarding their microstructural features and their mechanical properties. The fiber preform was made using winding technology. During the winding process, the SiC fiber roving was impregnated by a slurry containing SiC powder and sintering additives (Y₂O_3, Al₂O₃ and SiO₂). This already helped to achieve a partial matrix formation during the preform fabrication. In this way, the number of PIP cycles to achieve composites with less than 10% open porosity could be reduced significantly. Additionally, damage-tolerant properties of the composites were obtained by an optimal design of the matrix properties although only uncoated fibers were used. Finally, composites with a strength level of about 500 MPa and a damage-tolerant fracture behavior with about 0.4% strain to failure were obtained.     

SiC fiber reinforced geopolymer composites,part 2: Continuous SiC fiber

In this paper, unidirectional SiC fiber (SiC_f) reinforced geopolymer composites (SiC_f/geopolymer) were prepared and effects of fiber contents on the microstructure and mechanical properties of the composites in different directions were investigated. The XRD results showed that addition of SiC_f retarded geopolymerization process of geopolymer matrix by weakening the typical amorphous hump. SiC_f in all the composites were well infiltrated by geopolymer matrix, but microcracks which were perpendicular to the fiber axial direction were noted in the interface area due to the thermal shrinkage of matrix during the curing process. With the increases in fiber contents, although Young's modulus of the composites increased continuously, flexural strength, fracture toughness and work of fracture increased at first, reached their peak values and then decreased. And when fiber content was 20 vol%, the composites showed the highest flexural strength, fracture toughness and work of fracture, which were 14.2, 15.2 and 81.6 times as high as those of pristine geopolymer, respectively, indicating significant strengthening and toughening effects from SiC_f. Meanwhile, SiC_f/geopolymer composites failed in different failure modes in the different directions, i.e., tensile failure mode in the x direction (in-plane and perpendicular to the fiber axial direction) and shear failure mode in the z direction (laminate lay-up direction).     

Mechanistic modeling of lifetime distribution of SiC/SiC composite claddings

Silicon carbide (SiC) fiber-reinforced SiC matrix (SiC/SiC) composites have emerged as a new material candidate for fuel claddings in light water reactors. Recent studies showed that the load capacity of SiC/SiC materials exhibits a considerable statistical variation. Therefore, reliability analysis plays a critical role in design of SiC/SiC composite claddings. This paper presents a probabilistic model for the lifetime distribution of SiC/SiC composites. The model is anchored by a multiaxial stress-based failure criterion and subcritical damage accumulation mechanism. Based on the kinetics of subcritical damage growth, the lifetime distribution of a laboratory test specimen for any given loading history can be calculated. A finite weakest-link model is used to extrapolate the lifetime distribution of test specimens to full-length claddings. It is shown that the damage accumulation mechanism has a strong influence on the lifetime distribution of the cladding. This finding highlights the importance of understanding the static fatigue behavior of SiC/SiC composites. The present analysis also demonstrates an intricate length effect on the failure probability of the cladding, which is expected to play a crucial role in design extrapolation.     

Toughened ZrB2-based ceramics through SiC whisker or SiC chopped fiber additions

In order to improve the fracture toughness, SiC whiskers or SiC chopped fibers were added to a ZrB₂ matrix in volumetric fraction of 10 and 20 vol.%. The composites were hot-pressed between 1650 and 1730 °C and their final relative densities were higher than 95%. Even at the lowest sintering temperature, the whiskers showed an evident degradation. On the other hand, the fibers maintained their initial shape and a strong interface formed between matrix and reinforcement. The fracture toughness of the composites increased from 30 to 50% compared to the baseline material, with the fibers showing a slightly higher toughening effect. In the whiskers-reinforced composites, the room-temperature strength increased when 10 vol.% whiskers were added. In the fibers-reinforced composites, the room-temperature strength decreased regardless the amount of fibers added. The high-temperature strength of the composites was higher than that of the baseline material for both types of reinforcement.     

Correlating Electrical Resistance Change with Mechanical Damage in Woven SiC/SiC Composites: Experiment and Modeling

Silicon carbide (SiC) fiber‐reinforced SiC matrix composites are inherently multifunctional materials. In addition to their primary function as a structural material, the electric properties of the SiC/SiC composites could be used for the sensing and monitoring of in situ damage nucleation and evolution. To detect damage and use that information to further predict the useful life of a particular component, it is necessary to establish the relationship between damage and electrical resistance change. Here, two typical SiC/SiC composites, melt infiltrated (MI), and chemical vapor infiltrated (CVI) woven SiC/SiC composites, were tested to establish the relationship between the electrical response and mechanical damage in unload–reload tensile hysteresis tests. Compared to the 55% resistance increase seen for CVI composites, the MI SiC/SiC composites exhibit a maximum resistance change in 450% in response to mechanical loading (damage), which is the highest sensitivity known among various composites. An analytic model accounting for fiber breakage and matrix cracks was developed to link the electrical resistance to mechanical damage in the composites. The predictions from the models agree well with the experimental data for both composites with high and low conductive matrices. The residual resistance change after unloading is also correlated to the loading history by the analytical relationship. This study demonstrates that resistance change is sensitive to damage in a predictable manner and can be used to improve the reliability of damage assessment of SiC/SiC composites.     

Synthesis of SiC whiskers via catalytic reaction method in self-bonded SiC composites

Catalyzed by in-situ formed Fe nanoparticles (NPs), 3C–SiC whiskers were prepared from expanded graphite and Si powders after firing at 1573 K for 3 h in Argon. The density functional theory calculations revealed that Fe catalysts facilitated the formation of SiC nucleus and the epitaxial growth of SiC whiskers via reducing the bonding strength in CC dimer as well as Si–O and C–O bonds. Moreover, using SiC, expanded graphite and silicon powders as starting materials Fe-catalyzed self-bonded SiC composites were fabricated. Lots of SiC whiskers were synthesized in the as-prepared composites, leading to remarkable enhancements in high temperature mechanical behavior, oxidation resistance and cryolite resistance of the self-bonded SiC composites.