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.     

Joining oxide ceramic matrix composites by ionotropic gelation

The production of complex-shaped all-oxide ceramic matrix composites (Ox-CMC) is somewhat restricted by their current processing methods, as well as by the lack of applicable joining techniques. Thus, we present a new method for joining Ox-CMCs based on the gelation of slurries with the polysaccharide polymer alginate. For this investigation, Nextel 610/alumina-zirconia composites were produced using alginate as binder and aluminum acetate as gelling agent. The joining capabilities of this technique were investigated with microstructural analyses and single-lap compression shear tests. For that, a slurry-containing alginate was used to join two composite plates at different stages of the processing: gel state, dried green body and after sintering. Joining composites plates in their gel or green state was successful as the joints showed shear strength values similar to the interlaminar shear strength of the composites plates. The quality of the joints was attributed to the interactions between the alginate chains of the composite plates and the joint. We also show that even the joining of already sintered Ox-CMCs is feasible. However, densification cracks and lower shear strength are observed for such cases.     

The excellent protection effects of silicon/ytterbium silicate bilayer environmental barrier coatings on SiCf/SiC composites

The protection effects of an environmental barrier coating (EBC) consisting of silicon bond coat and mixed ytterbium monosilicate and ytterbium disilicate composite topcoat are directly evaluated by measuring the strength retention rate of SiC_f/SiC composites completely wrapped up by the previous EBCs after soaking in a mixed oxygen and water vapor environment at 1300°C for up to 200 h. The results show that the mixed topcoat exhibits not only extremely excellent phase stability but also fantastic protection effects toward composites. After 200 h of corrosion, the fully protected composites are unveiled to present not only dramatically reduced weight gain ratios, less than .6%, compared to ∼10% for those unprotected ones, but also extremely higher strength retention rates, more than 90%, compared to only 10%–15% for those unprotected ones. Further, the fully protected composites show a quasi-ductile load versus displacement curve, suggesting the retention of the oxidation-prone pyrolytic carbon interphase of current composites.     

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。     

Improved thermal conductivity and mechanical properties of SiC/SiC composites using pitch-based carbon fibers

Pitch-based carbon fibers were assembled in horizontal and thickness directions of SiC/SiC composites to form three-dimensional heat conduction networks. The effects of heat conduction networks on microstructures, mechanics, and thermal conductivities were investigated. The results revealed the benefit of introducing heat conduction networks in the densification of composites. The maximum bending strength and interlaminar shear strength of the modified composites reached 568.67 MPa and 68.48 MPa, respectively. These values were equivalent to 18.6% and 69.4% increase compared to those of composites without channels. However, channels in thickness direction destroyed the continuity of fibers and matrix, creating numerous defects. As the volume fraction of heat conduction channels rose, the pinning strengthening effect of channels and influence of defects competed with each other to result in first enhanced mechanical properties followed by a decline. The in-plane thermal conductivity was found anisotropic with a maximum value reaching 86.20 W/(m·K) after introducing pitch-based carbon unidirectional tapes. The thermal conductivity in thickness direction increased with volume fraction of pitch-based carbon fibers and reached 19.13 W/(m·K) at 3.87 vol% pitch-based carbon fibers in the thickness direction. This value was 90.75% higher than that of composites without channels.     

Enhancing thermal conductivity of C/SiC composites containing heat transfer channels

In this study, CNTs/SiC micro-pillars at controlled content ratios were introduced into C/SiC composites as heat transfer channels to improve the thermal conductivity in the thickness direction. The thermal conductivities and bending strengths before and after heat treatment at 1650 °C were investigated and the results were discussed. The theoretical calculations and finite element analyses confirmed that CNTs/SiC micro-pillars successfully worked as heat transfer channels. The theoretical thermal conductivity calculated by effective medium theory (EMT) model was 19.25 W/m⋅k and agreed-well with the experimental value. The measured thermal conductivity was estimated to 20.69 W/m⋅k and improved to 22.36 W/m⋅k after heat treatment. The latter was 3.56-fold higher than that of traditional C/SiC and attributed to increased grain growth during heat treatment. The optimal bending strength before heat treatment was recorded as 324.5 ± 23.74 MPa due to microstructure evolution caused by CNTs. After heat treatment, the bending strength improved by 138 % with ductile fracture mode attributed to ordered layer structure of PyC interphase and complex phase composition of the composites. These features benefited the abundant propagation of cracks and energy consumption. In sum, introduction of heat transfer channels into C/SiC composites provided a new way to improve the thermal conductivity in thickness direction of ceramic matrix composites.     

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.     

Characteristics of SiCf/SiC hybrid composites fabricated by hot pressing and spark plasma sintering

Abstract

Abstract

SiC fibre reinforced SiC–matrix ceramic composites were fabricated by electrophoretic deposition (EPD) combined with ultrasonication. Fine β-SiC powder and Tyranno-SA fabrics were used as the matrix and fibre for reinforcement, respectively. Different amounts of fine Al₂O₃–Y₂O₃ were added for liquid phase assisted sintering. For EPD, highly dispersed slurry was prepared by adjusting the zeta potentials of the constituent particles to ?+40 mV for homogeneous deposition. The composite properties were compared after using two different consolidation methods: hot pressing for 2 h at 20 MPa and spark plasma sintering (SPS) for 3 min at 45 MPa at 1750°C to minimise the damage to the SiC fibre. The maximum flexural strength and density for the 45 vol.-% fibre content composites were 482 MPa and 98% after hot pressing, respectively, whereas those for SPS were 561 MPa and 99·5%, indicating the effectiveness of SPS.     

Influence of boron nitride nanotubes on the damage evolution of SiCf/SiC composites

As-grown and BN-coated boron nitride nanotubes (BNNTs) were incorporated into SiC_f/SiC composites to produce nanotube-based hierarchical composites. In-depth studies on damage evolution reveal that early damage development are delayed owing to the restriction effects on crack propagations from as-grown and BN-coated BNNTs. Moreover, this delay effect is more pronounced from BN-coated BNNTs because BN-coated BNNTs/matrix interfacial bonding strength is low. Final failure of composites with as-grown BNNTs still comes much earlier compared with virgin composite due to strong fibers/matrix bonding enhanced by as-grown BNNTs. This premature final failure is remedied in large part in composites with BN-coated BNNTs because fibers/matrix bonding enhanced by as-grown BNNTs is weaken after the deposition of an interphase on nanotube surface. Additionally, the type, the number and the released energy level of damage mechanisms during the whole damage evolution after the incorporation of as-grown and BN-coated BNNTs were also discussed elaborately compared with virgin composite.     

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.     

Phase-field simulation of microscale crack propagation/deflection in SiCf/SiC composites with weak interphase

To understand the microscale toughening mechanism, the crack propagation, and stress–strain response of unidirectional SiC_f/SiC composites with h-BN interphase under transverse and longitudinal tension are investigated by a promising micromechanical phase field (PF) method along with representative volume element. Of much interest, the calculation results are well consistent with the available experimental results. With a strong dependence on the interphase strength, the toughening mechanisms during crack propagation are well presented, for example, fiber pull-out, crack deflection, and interphase debonding. Furthermore, the longitudinal tensile strength of SiC_f/SiC composites increases with decreasing the interphase strength, where only a weak enough interphase can result in a significant crack deflection by its cracking. In particular, the ratio of the interphase strength along fibers to the matrix strength should be less than 1.254 to ensure crack deflection in the interphase and fiber pull-out. Moreover, the transverse tensile strength of SiC_f/SiC composites reaches a maximum with increasing the interphase thickness into the range of 0.25–0.5 µm.     

Mechanical,thermal, and dielectric properties of SiCf/SiC composites reinforced with electrospun SiC fibers by PIP

Electrospun unidirectional SiC fibers reinforced SiC_f/SiC composites (e-SiC_f/SiC) were prepared with ∼10% volume fraction by polymer infiltration and pyrolysis (PIP) process. Pyrolysis temperature was varied to investigate the changes in microstructures, mechanical, thermal, and dielectric properties of e-SiC_f/SiC composites. The composites prepared at 1100 °C exhibit the highest flexural strength of 286.0 ± 33.9 MPa, then reduced at 1300 °C, mainly due to the degradation of electrospun SiC fibers, increased porosity, and reaction-controlled interfacial bonding. The thermal conductivity of e-SiC_f/SiC prepared at 1300 °C reached 2.663 W/(m∙K). The dielectric properties of e-SiC_f/SiC composites were also investigated and the complex permittivities increase with raising pyrolysis temperature. The e-SiC_f/SiC composites prepared at 1300 °C exhibited EMI shielding effectiveness exceeding 24 dB over the whole X band. The electrospun SiC fibers reinforced SiC_f/SiC composites can serve as a potential material for structural components and EMI shielding applications in the future.     

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.     

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.     

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.     

Effect of interface types on the heat-resistance of Cansas-II SiCf /SiC composites

The heat-resistance of the Cansas-II SiC/CVI-SiC mini-composites with a PyC and BN interface was studied in detail. The interfacial shear strength of the SiC/PyC/SiC mini-composites decreased from 15 MPa to 3 MPa after the heat treatment at 1500 °C for 50 h, while that of the SiC/BN/SiC mini-composites decreased from 248 MPa to 1 MPa, which could be mainly attributed to the improvement of the crystallization degree of the interface and the decomposition of the matrix. Aside from the above reasons, the larger declined fraction of the interfacial shear strength of the SiC/BN/SiC mini-composites might also be related to the gaps in the BN interface induced by the volatilization of B₂O₃·SiO₂ phase, leading to a significant larger declined fraction of the tensile strength of the SiC/BN/SiC mini-composites due to the obvious expansion of the critical flaws on the fiber surface. Therefore, compared with the CVI BN interface, the CVI PyC interface has better heat-resistance at high temperatures up to 1500 °C due to the fewer impurities in PyC.     

Study of material removal mechanisms in grinding of C/SiC composites via single-abrasive scratch tests

As one of the ceramic matrix composites (CMCs), carbon fiber-reinforced silicon carbide matrix (C/SiC) composites are promising materials used in various engineering applications owing to their superior properties. Precision surface grinding has been widely applied in the machining of CMC composites; however, the material removal mechanisms of C/SiC composites have not been fully elucidated yet. To reveal the material removal mechanisms in the grinding of chemical vapor infiltration-fabricated C/SiC composites, novel single-abrasive scratch tests were designed and conducted in two typical cutting directions. The experimental parameters, especially the cutting speed, conformed to the actual grinding process. The results show that the grinding parameters (feed rate, spindle speed, depth of cut, and cutting direction) have significant influences on the grinding forces, surface integrity, and affected subsurface region. The tangential force is in general larger than the normal force at the same cutting depth. Furthermore, both the tangential and normal forces in the longitudinal cutting direction are larger than those in the transverse cutting direction. The impacts and abrasive actions at the tool tip mainly caused the material removal. The predominant material removal mode is brittle fracture in the grinding of unidirectional C/SiC composites, because the damage behaviors of the C/SiC composites are mainly the syntheses of matrix cracking, fiber breakage, and fiber/matrix interfacial debonding. These results are rationalized based on the composite properties and microstructural damage features.     

基于核应用下碳化硅陶瓷及其复合材料的连接研究进展

SiC陶瓷及其复合材料凭借其自身固有的核辐射下的稳定性而有望成为新一代核裂变以及未来核聚变反应堆中重要的结构材料.能否满足核应用环境下各种苛刻条件而实现完美连接是其能够得到最终应用的关键.本文综述了目前国际上基于核应用上SiC陶瓷及其复合材料的几种连接工艺的发展情况.     

Effect of SiC coating and heat treatment on the thermal radiation properties of C/SiC composites

The effects of SiC coating and heat treatment on the emissivity were investigated for 2D C/SiC composites prepared by CVI in the 6–16 μm range. SiC coating had an obvious effect on the spectral emissivity of the composites but caused just 5% difference in the total emissivity. A radiation transport model was applied to explain those changes caused by SiC coating. Heat treatment affected the thermal radiation properties of the composites through the microstructure evolution. Base on the complementary analytical techniques, the changes in the emissivity were attributed to a good graphitization degree of carbon phases, large β-SiC grain sizes and high α-SiC content resulting in high emissivity.     

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.