Formation of Ti3SiC2 interphase coating on SiCf/SiC composite by electrophoretic deposition

To improve the oxidation resistance of SiC composites at high temperature, the feasibility of using Ti₃SiC₂ coated via electrophoretic deposition (EPD) as a SiC fiber reinforced SiC composite interphase material was studied. Through fiber pullout, Ti₃SiC₂, due to its lamellar structure, has the possibility of improving the fracture toughness of SiC_f/SiC composites. In this study, Ti₃SiC₂ coating was produced by EPD on SiC fiber; using Ti₃SiC₂‐coated SiC fabric, SiC_f/SiC composite was fabricated by hot pressing. Platelet Ti₃SiC₂ powder pulverized into nanoparticles through high‐energy wet ball milling was uniformly coated on the SiC fiber in a direction in which the basal plane of the particles was parallel to the fiber. In a 3‐point bending test of the SiC_f/SiC composite using Ti₃SiC₂‐coated SiC fabric, the SiC_f/SiC composite exhibited brittle fracture behavior, but an abrupt slope change in the strength‐displacement curve was observed during loading due to the Ti₃SiC₂ interphase. On the fracture surface, delamination between each layer of SiC fabric was observed.     

The design of zirconium and hafnium germanate interphase in SiCf/SiC composites

Unidirectional SiC_f/SiC minicomposites with SiC matrix derived by polymer-impregnation pyrolysis (PIP), reinforced with SiC fibers coated with zirconium or hafnium germanate were fabricated. Microdebonding indentation tests for SiC_f/SiC composites with one- and multilayered germanate interphase were performed. Interfacial shear stress depending on the number of germanate interfacial layers and morphology was determined. The microstructure of the minicomposites and indented fracture surfaces were studied by scanning electron microscopy (SEM). It was stated that an increase in the number of interfacial coatings leads to a decrease in the interfacial frictional stress in SiC_f/SiC minicomposites with germanate interphases. The key factor of interphase weakening is the formation of a weak interlayer bonding within the interphase but not germanate layered crystal structure itself. Thus, bonding at the fiber/matrix boundary could be regulated by the number of layers of ZrGeO₄ or HfGeO₄ in the interphase zone.     

Characterisation of joined surface modified SiCf/SiC composites

This work has focused on surface engineering coupled with brazing to join SiC_f/SiC composites and to improve the joint strength. The surface engineering was carried out through the Selective Thermal Removal (STR) of SiC fibres from a SiC_f/SiC composite to obtain “brush-like” surfaces; the modified composites were then joined by means of an AgCuTi braze alloy. In order to investigate whether a “brush-like” interface could enhance the mechanical strength of the joint by increasing mechanical interlocking with the brazing alloy at the micron scale, the joints were tested with and without surface engineering by means of single lap offset under compression.The treatment to form a roughened surface suitable for mechanical keying of the braze metal led to an improved ductility of the joint; the fracture surfaces demonstrated that the proposed method is promising, even though the treatment damages locally the composite.     

Enhanced microwave‐absorbing property of precursor infiltration and pyrolysis derived SiCf/SiC composites at X band: Role of carbon‐rich interphase

Ceramic matrix composites (CMCs) can be microwave‐absorbent when endowing the composite constituents with proper dielectric properties. In this work, we report a new method to enhance the microwave‐absorbing property of CMCs by in situ fabrication of a carbon‐rich interphase at the fiber/matrix interface. This was achieved in a SiC fiber reinforced SiC matrix (SiCf/SiC) composite fabricated by precursor infiltration and pyrolysis (PIP). We found that as the PIP temperature increased from 800 to 1000°C, the microwave‐absorbing property of the SiCf/SiC composite was significantly enhanced at X band, which also surpassed those of the SiC fiber and monolithic SiC ceramic fabricated at the same temperature. The dominant mechanism was studied by decoupling the effect of individual SiC fibers, SiC matrix, and fiber/matrix interface. The results showed that the SiC fiber and SiC matrix were barely microwave‐absorbent, due to their low dielectric losses. The microwave‐absorbing mechanism was finally ascribed to the fiber/matrix interface, which was carbon‐rich, containing Si and O elements. The interphase showed a conductivity that was superior to that of the fiber and the matrix, and mainly dominated the dielectric property of the overall composite. The results highlight the role of carbon‐rich interphase on the microwave‐absorbing property of CMCs.     

Hertzian crack propagation in graded glass/ceramic composites

In literature, the concept of material gradation is shown to inhibit surface crack initiation in glass/ceramic composites subjected to Hertzian indentation. However, surface cracks could yet initiate due to relatively higher loadings or in the presence of surface flaws/defects. Hence, characterization of graded composites concerning the resistance against Hertzian crack initiation and propagation manifests itself as a prominent matter. In this study, axisymmetric Hertzian cracks evolving in graded glass/ceramic composites propelled by a rigid cylindrical punch are investigated employing a novel recursive method, called the stacked-node propagation procedure. Crack trajectories and their propagation susceptibilities are predicted via the minimum strain energy density (MSED) criterion regarding the crack growth resistance (R-curve) of ceramics. The stress trajectory approach is also considered for a homogeneous glass to reveal the reliance and effectiveness of the MSED criterion in the present crack problems. The Mori–Tanaka relations are adopted to model the elastic modulus and Poisson's ratio variations through the composites, which are implemented on the simulations via the homogeneous finite element approach. Hertzian crack problem of a practically producible graded composite comprised of oxynitride glass and a fine-grained silicon nitride ceramics (Si₃N₄) is treated as a case study. The degree of material gradation is assessed for the mitigation of surface crack initiation and propagation risks.     

Microstructure and strengthening behavior in high content SiC nanowires reinforced SiC composites

In this study, the high-content SiC_nw reinforced SiC ceramic matrix composites (SiC_nw/SiC CMC) were successfully fabricated by hot pressing β-SiC and sintering additive (Al₂O₃-Y₂O₃) with boron nitride interphase modification SiC_nw. The effects of sintering additive content and mass fraction (5–25 wt%) of SiC_nw on the density, microstructure, and mechanical properties of the composites were investigated. The results showed that with the increase of sintering additives from 10 wt% to 12 wt%, the relative density of the SiC_nw/SiC CMC increased from 97.3% to 98.9%, attributed to the generated Y₃Al₅O₁₂ (YAG) liquid phase from the Al₂O₃-Y₂O₃ that promotes the rearrangement and migration of SiC grains. The comprehensive performance of the obtained composite with 15 wt% SiC_nw possessed the optimal flexural strength and fracture toughness of 524 ± 30.24 MPa and 12.39 ± 0.49 MPa·m^1/2, respectively. Besides, the fracture mode of the composites with 25 wt% SiC_nw content revealed a pseudo-plastic fracture behavior. It concludes that the 25 wt% SiC_nw/SiC CMC was toughened by the fiber pull-outs, debonding, bridging, and crack deflection that can consume plenty of fracture energy. The strategy of SiC nanowires worked as a main bearing phase for the fabrication of SiC/SiC CMC providing critical information for understanding the mechanical behavior of high toughness and high strength SiC nanoceramic matrix composites.     

High-temperature fatigue crack propagation mechanism of orthogonal 3-D woven amorphous SiC Fiber/SiC/YSi2-Si matrix composites

To elucidate degradation mechanisms attributable to high-temperature fatigue crack propagation, a study was conducted of 3-D woven SiC_f/SiC CMC in which amorphous SiC fiber was used as a reinforcement material and in which a matrix was formed through low-temperature melt infiltration. From a high-temperature fatigue test conducted at 1373 K in the atmosphere with stress of 142 MPa or more, the fracture lifetime of newly developed SiC_f/SiC CMC was found to be longer than that of SiC_f/SiC CMC, which uses crystalline SiC fiber. Furthermore, repeatedly applying high temperatures during high-temperature fatigue tests and using X-ray computed tomography, fatigue cracks were found to propagate in a direction across 0-degree fiber bundles that undergo stress. Electron mapping of regions with crack propagation revealed that oxidation eliminates boron nitride (BN), which has a crack deflection effect. The SiC fibers and matrix are fixed through the formation of oxides. Cracks propagate because of the consequent decrease in toughness of the SiC_f/SiC CMC. In regions without crack propagation, fracture surfaces were not covered with oxides. These regions underwent forcible fracture in the final stage of the high-temperature fatigue tests. From the test results presented above, SiC_f/SiC CMC is considered to undergo fracture when the effective cross-sectional area is reduced because of crack propagation accompanying oxidation and when the test load exceeds the tensile strength of the residual cross-sectional area. However, some cracks in the matrix produced by a low-temperature melt infiltration process were closed by oxides derived from YSi₂. Because of crack closing, crack propagation is presumed to be avoided. Also, LMI-CMC showed excellent high-temperature fatigue properties at pressures higher than 150 MPa, which exceeds the proportional limit.     

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。     

Damage evolution in SiC/SiC unidirectional composites by X-ray tomography

Melt infiltrated SiC/SiC ceramic matrix composite unidirectional (UD) composite specimens were imaged under load using X-ray microtomography techniques in order to visualize the evolution of damage accumulation and to quantify damage mechanisms within the composite such as matrix cracking and fiber breaking. The data obtained from these in situ tensile tests were used in comparison with current models and literature results. Three-dimensional (3D) tomography images were used to measure the location and spacing of matrix cracking that occurred at increasing stress increments during testing within two UD composite specimens. The number of broken fibers and the location of each fiber break gap that occurred within the volume of both specimens were also quantified. The 3D locations of fiber breaks were correlated with the location of each matrix crack within the volume of the specimen and it was found that at the stress scanned directly before failure, most of the fiber breaks occur within 100 microns of a matrix crack.     

In-situ characterization on crack propagation behavior of SiCf/SiC composites during monotonic tensile loading

The microstructure and crack propagation path of 2.5D SiC_f/SiC composites were observed by synchrotron radiation x-ray computed micro tomography (SR-μCT) equipped with in-situ tensile device. The results showed that the pore morphologies of the SiC_f/SiC composites are mainly divided into three types in three-dimension space: interconnected pores, isolated pores and micro pores in fiber bundles. The crack initiation occurred at the root of the defects under in-situ tensile load and the crack was perpendicular, parallel to the stress axis or mixed mode to propagate. At the interface scale between fiber and matrix, the crack deflection will be controlled by physical parameters such as fracture energy release rate and the modulus of elasticity. At the fiber bundle scale, the crack is easy to shear propagate along the interface between weft and warp fiber bundles due to the existence of the mechanical bonding and residual tensile stress.     

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.     

Machinability improvement in milling of SiCf/SiC composites based on laser controllable ablation pretreatment

The poor machinability of SiC_f/SiC composites greatly limits its application and promotion. The laser-induced ablation products of SiC_f/SiC composites are powdery, loose and porous. Milling of laser ablated samples demonstrated that the force and heat were almost negligible when milling ablation products. Accordingly, a laser ablation pretreatment milling (LAPM) process of SiC_f/SiC composites was proposed. Under the LAPM process, after the laser ablation treatment with controllable depth, the cutting allowance could be achieved in only one pass, which greatly improved the machining efficiency compared with the conventional milling process. The material removal rate was greatly improved on the premise of ensuring the machining quality. Taking the milling of tensile specimens as an example, compared with conventional milling, the total processing time of the specimen was reduced by 31.29 % by LAPM process. Therefore, LAPM provides a potential feasible process scheme for greatly improving the machinability and machining efficiency of SiC_f/SiC composites.     

Theoretical prediction on structure evolution and optimal properties of silicon modified hexagonal boron nitride as interphase in SiCf/SiC composite

To predict the effects of Si doping on hexagonal boron nitride (h-BN) and to achieve a balance between mechanical and oxidation properties for the interphase modification in SiC_f/SiC composites, we herein calculate and analyze the crystal structures and mechanical properties of (BN)₆₄Si_x (x = 4, 8, 16, 32) models by means of density functional theory (DFT) calculations and ab initio molecular dynamics (aiMD) simulations. The possible trends of crack deflection and self-healing ability are discussed. The modeling shows an obvious transition of (BN)₆₄Si_x from the layered crystal structure and anisotropic mechanical property to amorphous structure and isotropic mechanical property as the Si doping content up to 36.1 wt%. Regarding to the application of interphase in SiC_f/SiC composites, (BN)₆₄Si₁₆ model structure possess the highest debonding potential according to Cook and Gordon’s criteria and illustrates the higher self-healing capacity at elevated temperature.     

Insights into internal oxidation of SiC/BN/SiC composites

The article presents new observations of the physical manifestations of internal oxidation and volatilization in SiC/BN/SiC composites. The observations are made on both unbroken and broken minicomposite specimens before and after 12 h exposures at 1000°C in dry air with 10 ppm water vapor. The observations are enabled by a sample preparation method involving ion-mill sectioning and polishing. Complementary analyses of volatilization and closure of resulting gaps are also presented. The observations show that BN is generally consumed in two stages: (i) through reaction with oxygen along the interfaces with both the fiber and the matrix, producing two concentric annular pockets of borosilicate glass and an intervening annulus of progressively thinning BN; and (ii) subsequent volatilization, through the reaction of boria with trace amounts of water vapor in the environment to form borohydroxide gases. The spatial extent to which these processes proceed is governed by a competition between the outward diffusion of reaction gases through both matrix cracks and interface gaps produced by boria volatilization, and the formation of oxides on the newly exposed surfaces of fibers, matrix, and coating.     

Analysis of SiC/SiC composites for energy applications at ambient conditions

Plain weave planar and biaxially braided tubular SiC/SiC CMCs are evaluated in tension and four-point bending, respectively, at ambient conditions. Custom-designed fixtures for CMC testing are developed for each loading mode and are coupled with three-dimensional digital image correlation. Stereoscopic image correlation analysis reveals crack initiation and failure sites to provide insight into stress redistribution mechanisms. Scanning electron microscopy is performed postmortem to determine the influence of microstructural features on crack initiation and failure. Crack spacing is measured in situ by stereoscopic image correlation and confirmed by SEM measurements to relate to underlying tow-tow crossing points. Triangulated surface heights of plain weave tow architecture are used to determine that subtle differences in neighboring transverse tow angle, which vary within a range of ±4° from horizontal, have no significant effect on final fracture location. The results presented reaffirm the state of current SiC/SiC CMCs developed for energy applications and will help to further improve SiC/SiC and other CMCs.     

High temperature abradable sealing coating for SiCf/SiC ceramic matrix composites

A study of porous YSZ abradable sealing coating (ASC) plasma-sprayed onto SiC_f/SiC ceramic matrix composites (CMC) through the compatibility of intermediate layers is reported. The multilayer Si/Yb₂Si₂O₇/LaMgAl₁₁O₁₉ thermal-environmental barrier coating (T-EBC) is served as intermediate layers in consideration of its ability to protect the CMC from recession and ease the misfit of the thermal expansivity. Isothermal exposure and thermal shock tests were conducted at 1200°C and led to the decomposition of t'-ZrO₂ phase to t-ZrO₂ and c-ZrO₂ phases in YSZ topcoat, the formation of mud-cracks throughout the entire coating structure and thermally grown oxide (SiO₂), with following an Yb₂Si₂O₇ reaction layer. The measured bond strength of the coated samples was 5.47 ± 0.85 MPa, and the fracture position mainly happened inside the CMC substrate. The Superficial Rockwell Hardness (HR15Y) considered to be an important factor in abradability increased by only 1.34% after 1200°C isothermal exposure for 100 h, showing excellent high temperature hardness stability. The abradability of the ASC was investigated by a sliding wear test, the fatigue wear mainly occurred in worn scar when encountering Si₃N₄ ceramic ball with high hardness and low thermal conductivity, while adhesive wear occurred when GCr15 steel ball with low hardness and high thermal conductivity are encountered.     

Fabrication of tough SiCf/SiC composites by electrophoretic deposition using a fabric coated with FeO-catalyzed phenolic resin

A hybrid processing route based on vacuum infiltration, electrophoretic deposition, and hot-pressing was adopted to fabricate dense and tough SiC_f/SiC composites. The as-received Tyranno SiC fabric preform was infiltrated with phenolic resin containing 5 wt.% FeO and SiC powders followed by pyrolysis at 1700 °C for 4 h to form an interphase. Electrophoretic deposition was performed to infiltrate the SiC-based matrix into the SiC preforms. Finally, SiC green tapes were sandwiched between the SiC fabrics to control the volume fraction of the matrix. Densification close to 95% ρ_theo was achieved by incorporating 10 wt.% Al₂O₃-Sc₂O₃ sintering additive to facilitate liquid phase sintering at 1750 °C and 20 MPa for 2 h. X-ray diffraction and Raman analyses confirmed the catalytic utility of FeO by the formation of a pyrolytic carbon phase. The flexural response was explained in terms of the extensive fractography results and observed energy dissipating modes.     

Investigations on continuous-wave laser and pulsed laser induced controllable ablation of SiCf/SiC composites

To lay a foundation for the feasibility exploration of laser-induced ablation-assisted machining for SiC_f/SiC composites, combined with numerical simulation and experiments, the laser-induced ablation mechanism of SiC_f/SiC composites was studied, and the relationship between laser parameters and ablation depth was analyzed. The laser-induced ablation products of SiC_f/SiC composites mainly consisted of recrystallized 3C-SiC and amorphous SiO₂, which were powdery and porous. According to the stratification characteristic, the ablation products were divided into attached smoke dust layer, sublimate recrystallization layer, heat-affected layer, and unaffected layer from the surface to the inside of the material. By adjusting the laser parameters (significant factors were the scanning speed and the scanning spacing), the depth of laser-induced ablation was adjustable and controllable. The ablation depth was greater in continuous-wave (CW) mode due to the continuous energy input. Therefore, CW laser is more suitable for generating larger and various ablation depths to match various cutting allowances.     

Surface engineering of SiCf/SiC composites by selective thermal removal

Surface engineering based on the Selective Thermal Removal (STR) of SiC fibers from SiC_f/SiC composites was used to obtain a brush‐like surface in view of joining processes. As observed through 3D confocal microscopy, the thermal treatment led to a selective removal of the surface fibers so that the specific surface increased. Wetting tests were performed using a Ag–Cu–Ti brazing alloy. The STR led to a negligible increase in the contact angles, which ranged from 16° to 21° for as‐received composites and increased to 28° for composites after STR. Microstructural observations showed that the brazing alloy perfectly adhered to the brush‐like surfaces were giving a mechanical interlocking expected to enhance the strength of the joint.     

In situ characterization of residual stress evolution during heat treatment of SiC/SiC ceramic matrix composites using high-energy X-ray diffraction

Volumetric strains were measured in silicon carbide/silicon carbide melt-infiltrated ceramic matrix composites (CMCs) at ambient and high temperatures using high-energy synchrotron X-ray diffraction (XRD). Both silicon and silicon carbide constituents were interrogated utilizing a broad spectrum of diffracting planes that would be largely inaccessible to common laboratory XRD equipment. Residual room-temperature principal strains in the melt-infiltrated silicon phase were found to be approximately 1100 με in compression, corresponding to stresses of approximately 300 MPa using simplifying constitutive assumptions. Residual room-temperature principal strains in silicon carbide particles found throughout the matrix were approximately 500 με in tension, corresponding to approximately 300 MPa. Residual strains were found to decrease considerably as temperatures increased from ambient temperature to 1250°C. Residual strains returned to approximately preheat treatment values after cool-down to ambient temperature. Strain measurements in the silicon phase were found to be significantly affected by dissolved boron dopant levels causing contraction of the silicon lattice. This contraction must be accounted for in high-temperature experiments for accurate calculation of stresses in the silicon phase.