The role of TiO2 incorporation in the preparation of B4C/Al laminated composites with high strength and toughness

We prepared B₄C/Al laminated composites via ice-templating and gas-aided pressure infiltration and investigated the effects of TiO₂ addition on the microstructures and mechanical properties of the composites. The incorporation of TiO₂ led to the formation of TiB₂ after sintering, reduced the formation of harmful phases and increased the strength of ceramic architectures. However, its excessive addition resulted in the cracking of ceramic layers and the formation of metal strips after Al infiltration. The bending strength, fracture toughness and work of fracture of the composites first increased and then decreased with increasing initial TiO₂ content, reaching maxima of 420?±?20?MPa, 44?±?2?MPa?m^1/2 and 5002?±?175?J?m^?2, respectively. The specific strength and toughness are comparable to those of titanium alloys. Furthermore, fracture modes and toughening mechanisms were thoroughly addressed by analyzing crack propagation paths and fracture surface morphologies. Crack deflection and metal bridging are two primary extrinsic toughening mechanisms.     

Developing high-performance laminated Cu/TiC composites through melt infiltration of Ni-doped freeze-cast preforms

Nacre-inspired laminated composites have been proven to possess a unique combination of strength and toughness. In this study, we fabricated nacre-mimetic Cu/TiC composites via unidirectional freezing of aqueous TiC slurries containing different amounts of NiO additives, followed by ice sublimation, carbothermal reduction of NiO to Ni during sintering and then gas-pressure infiltration of the Cu melt. The introduction of Ni greatly facilitated the densification of ceramic lamellae and enhanced the interfacial bonding between Cu and TiC. The resultant composites displayed outstanding damage tolerance and anisotropic electrical conductivities. Specifically, for an ～31?vol% TiC–Cu composite containing 24?wt% Ni in the ceramic lamellae (based on the TiC content), a fracture toughness (K_Jc) of 72.5?±?1.0?MPa·m^1/2, work of fracture of 53.4?±?3.5?kJ/m², bending strength of 725?±?11?MPa and longitudinal electrical conductivity of 22.7?MS/m (～60% of the Cu matrix) were achieved, which were approx. 81%, 536%, 122% and 97% higher than those of the Ni-free composite, respectively. Noticeable toughening was demonstrated to be a consequence of multiple cracking, plastic deformation and uncracked-ligament bridging of the metal layers, as well as crack deflection and blunting. On the other hand, significant strengthening resulted from tailoring the microstructures in the ceramic layers and at the Cu/TiC interface as a result of Ni doping. We believe that the facile strategy adopted herein provides an effective way to solve the problems of wetting and bonding related to metal infiltration and can be readily extended to the preparation of other nacre-inspired metal?ceramic composites.     

Effects of post-sintering annealing on the microstructure and toughness of hot-pressed SiCf/SiC composites with Al2O3-Y2O3 additions

This study examined the effects of post-sintering heat treatment on enhancing the toughness of SiC_f/SiC composites. Commercially available Tyranno^® SiC fabrics with contiguous dual ‘PyC (inner)-SiC (outer)’ coatings deposited on the SiC fibers were infiltrated with a SiC + 10 wt% Al₂O₃-Y₂O₃ slurry by electrophoretic deposition. SiC green tapes were stacked between the slurry-infiltrated fabrics to control the matrix volume fraction. Densification of approximately 94% ρ_theo was achieved by hot pressing at 1750 °C, 20 MPa for 2 h in an Ar atmosphere. Sintered composites were then subjected to isothermal annealing treatment at 1100, 1250, 1350, and 1750 °C for 5 h in Ar. The correlation between the flexural behavior and microstructure was explained in terms of the in situ-toughened matrix, phase evolution in the sintering additive, role of dual interphases and observed fracture mechanisms. Extensive fractography analysis revealed interfacial debonding at the hybrid interfaces and matrix cracking as the key fracture modes, which were responsible for the toughening behavior in the annealed SiC_f/SiC composites.     

Preparation and fracture behavior of bionic layered SiCp/Al composites by tape casting and pressure infiltration

In this study, the bioinspired laminated composites with alternating soft Al layers and hard SiCp/Al were fabricated through the tape casting followed by pressure infiltration. In-situ bending and digital image correlation technology (DIC) analysis were carried out on the laminated composites. The results showed that the uniform layers of SiCp/Al and Al were obtained with the thickness of 30 μm and 10 μm, respectively. The interfaces between layers had an intimated combination. The bending deformation process of the laminated composites could be divided into three stages, i.e., crack initiation, crack stable diffusion and crack propagation instability. During deformation, the laminated structure changed the state of strain and strain distribution, further restricted the development of the crack, and the whole materials presented a stepped fracture. This study provides support for preparation and fracture process analysis of biomimetic layered composites prepared by tape casting.     

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.     

Fabrication of 3D-SiC/aluminum alloy interpenetrating composites by DIW and pressureless infiltration

A novel method combining direct ink writing (DIW) and pressureless infiltration is proposed for fabricating 3D-SiC/Al composites. Chopped carbon fiber was added to DIW ink to serve as a pore-forming agent and facilitate pyrolysis to provide infiltration channels during the preoxidation process. The effects of SiC particle size and carbon fiber content on mechanical properties and the infiltration process were investigated. The thickness of the oxide films produced at different preoxidation temperatures was studied using a transmission electron microscope. The interfacial and interpenetrating phase compositions of 3D-SiC/Al were examined using scanning electron microscopy, an energy dispersive spectrometer, and X-ray diffraction. The results showed that carbon fiber can improve the infiltration effect, with SiO₂ layers of differing thickness affecting the infiltration process to different degrees. The final sample exhibited good mechanical properties with a bending strength of 330.3 MPa.     

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.     

Microstructure and flexural strength of C/HfC-ZrC-SiC composites prepared by reactive melt infiltration method

C/HfC-ZrC-SiC composites were fabricated via reactive melt infiltration (RMI) of the mixed HfSi₂ and ZrSi₂ alloys. The microstructure, infiltration behavior of the hybrid silicide alloys infiltrating C/C composites, and flexural strength of C/HfC-ZrC-SiC composites was studied. Inside composites, there were more Hf-rich (Hf, Zr)C phases distributed in the exterior region, while more SiC and Zr-rich (Zr, Hf)Si₂ in the interior region. There was compositional segregation in (Hf, Zr)C, with the HfC content decreasing from the exterior region to interior region. The RMI process was performed at different temperatures to investigate the structural evolution, and a model for the reactive melt infiltration of the mixed HfSi₂ and ZrSi₂ alloys into C/C composites was established. Compared with C/HfC-SiC and C/ZrC-SiC prepared by same process, C/HfC-ZrC-SiC had the highest flexural strength of 247Mpa and 213Mpa after oxidation at 1200 ℃ for 15 min. Both the unoxidized and oxidized samples presented a pseudo-plastic fracture behavior.     

Compressive strength and wear properties of SiC/Al6061 composites reinforced with high contents of SiC fabricated by pressure-assisted infiltration

Pressure-assisted infiltration was used to synthesize SiC/Al 6061 composites containing high weight percentages of SiC. A combination of PEG and glass water was used to fabricate SiC preforms and the effect of the presence of glass water on the microstructure and mechanical properties of the preforms was evaluated by performing compression tests on the preforms. Also, the compressive strength and the hardness of the SiC/Al composites were investigated. The results revealed that the glass water improved the compressive strength of the preforms by about five times. The microstructural characterization of the composites showed that the penetration of the aluminum melt into the preforms was completed and almost no porosity could be seen in the microstructures of the composites. Moreover, the composite containing 75 wt% SiC exhibited the highest compressive strength as well as the maximum hardness. The results of the wear tests showed that increasing the SiC content reduces the wear rate so that the Al-75 wt% SiC composite has a lower wear rate and a lower coefficient of friction than those of Al-67 wt% SiC composite. This indicated higher wear resistance in these composites than the Al alloy due to the formation of a tribological layer on the surface of the composites.     

Direct ink writing of chopped carbon fibers reinforced polymer-derived SiC composites with low shrinkage and high strength

The chopped carbon fiber reinforced SiC (C_f/SiC) composite has been regarded as one of the excellent high-temperature structural materials for applications in aerospace and military fields. This paper presented a novel printing strategy using direct ink writing (DIW) of chopped fibers reinforced polymer-derived ceramics (PDCs) with polymer infiltration and pyrolysis (PIP) process for the fabrication of C_f/SiC composites with high strength and low shrinkage. Five types of PDCs printing inks with different C_f contents were prepared, their rheological properties and alignment of carbon fiber in the printing filament were studied. The 3D scaffold structures and bending test samples of C_f/SiC composites were fabricated with different C_f contents. The results found that the C_f/SiC composite with 30 wt% C_f content has high bending strength (～ 7.09 MPa) and negligible linear shrinkage (～ 0.48%). After the PIP process, the defects on the C_f/SiC composite structures were sufficiently filled, and the bending strength of C_f/SiC composite can reach up to about 100 MPa, which was about 30 times greater than that of the pure SiC matrix without C_f. This work demonstrated that the printed C_f/SiC composites by using this method is beneficial to the development of the precision and complex high-temperature structural members.     

Additive manufacturing of continuous carbon fiber reinforced high entropy ceramic matrix composites via paper laminating,direct slurry writing,and precursor infiltration and pyrolysis

In this study, continuous carbon reinforced C_f/(Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C–SiC high entropy ceramic matrix composites were additively manufactured through paper laminating (PL), direct slurry writing (DSW), and precursor infiltration and pyrolysis (PIP). (Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C high entropy ceramic (HEC) powders were synthesized by pressureless sintering and ball milling. A certain proportion of HEC powder, SiC powder, water, binder, and dispersant were mixed to prepare the HEC-SiC slurry. Meanwhile, BN coating was prepared on the 2D fiber cloth surface by the boric acid-urea method and then the cloth was cut into required shape. Additive manufacturing were conducted subsequently. Firstly, one piece of the as-treated carbon fiber cloth was auto-placed on the workbench by paper laminating (PL). Then, the HEC-SiC slurry was extruded onto the surface of the cloth by direct slurry writing (DSW). PL and DSW process were repeated, and a C_f/HEC-SiC preform was obtained after 3 cycles. At last, the preform was densified by precursor infiltration and pyrolysis (PIP) and the final C_f/HEC-SiC composite was prepared. The open porosity of the C_f/HEC-SiC composites, with the HEC volume fractions of 15, 30 and 45%, were 7.7, 10.6, and 11.3%, respectively. And the density of the C_f/HEC-SiC composites, with the HEC volume fractions of 15, 30 and 45%, were 2.9, 2.7 and 2.3 g/cm³, respectively. The mechanical properties of the C_f/HEC-SiC composites increased firstly and then decreased with the HEC content increase, reaching the maximum value when the HEC volume fraction was 30%. The mechanical properties of the C_f/HEC-SiC composites containing 45, 30 and 15% HEC were as follows: flexural strength (180.4 ± 14 MPa, 183.7 ± 4 MPa, and 173.9 ± 4 MPa), fracture toughness (11.9 ± 0.17 MPa m^1/2, 14.6 ± 2.89 MPa m^1/2, and 11.3 ± 1.88 MPa m^1/2), and tensile strength (71.5 ± 4.9 MPa, 98.4 ± 12.2 MPa, and 73.4 ± 8.5 MPa). From this study, the additive manufacturing of continuous carbon fiber reinforced high entropy ceramic matrix composites was achieved, opening a new insight into the manufacturing of ceramic matrix composites.     

Influence of graphitization treatment on microstructure and flexural strength of C/C-ZrC-SiC composites fabricated via reactive melt infiltration

C/C-ZrC-SiC composites were prepared by chemical vapor infiltration (CVI) and molten salt assisted reactive melt infiltration (RMI). The microstructure of low density and high density C/C composites without graphitization (LC/HC) and graphitization at 2000 °C (LCG/HCG) were compared. Moreover, the effects of graphitization of LC and HC on the microstructure and flexural strength of C/C-ZrC-SiC composites were investigated in detail. The composites prepared by infiltration of LC and LCG had lower flexural strength, 220.01 ± 21.18 MPa and 197.94 ± 19.05 MPa, respectively. However, the composites prepared by HC and HCG presented higher flexural strength, 308.76 ± 12.35 MPa and 289.62 ± 8.70 MPa, respectively. This was due to the phenomenon of fiber erosion in both LC and LCG during the RMI process. After graphitization, the flexural strength of C/C-ZrC-SiC composites prepared by RMI decreased, but the fracture behavior of the composites tends to be more mild. The decreased strength of the composites were caused by the increased matrix cracks, fiber damage in high temperature and the weak interfacial bonding. The improve of failure behavior of the composites was due to interface debonding between the fiber and matrix, and composites can consume the fracture energy through fiber pull-out.     

Compressive strength and damage mechanisms of 2D-C/SiC composites at high temperatures

Compressive strength of 2D-C/SiC composite was investigated from room temperature(RT) to 1600?°C at present work. Damage evolution was investigated by conducting loading/unloading tests at RT and the damage mechanisms were elucidated by observing the fracture morphology. It is found that compressive strength of 2D-C/SiC was retained until 1200?°C and then decreased with increasing temperature. The variation of compressive strength is closely related to the degradation in matrix modulus. The compressive damage of 2D-C/SiC starts at the buckling of 0° fiber and is followed by opening and closing of original pores, initiation and growth of longitudinal interbundle cracks, separation of 90° fiber bundles by longitudinal cracks, matrix cracking from intrabundle pores, propagation of matrix cracks into 0° fiber bundles, connection of cracks in 0° fiber bundles and longitudinal cracks in 90° fiber bundles.     

Simultaneous improvement in strength,toughness, and thermal stability of epoxy/halloysite nanotubes composites by interfacial modification

This work investigated the effect of silane modification of halloysite nanotubes (HNTs) on the mechanical properties of epoxy/HNTs nanocomposites. Three kinds of silane coupling agents, including 3‐(2‐aminoethyl)‐aminopropyltrimethoxysilane (AEAPS), (3‐glycidyloxypropyl)‐trimethoxysilane (GPTMS), and octyltriethoxysilane (OTES), were employed. It was shown that the modified HNTs exhibited a better dispersion in the epoxy matrix compared with pristine one. Because of strong interfacial interaction between AEAPS modified HNTs and the epoxy matrix, the nanocomposites exhibited the highest glass transition temperature and modulus among all the samples. On the other hand, AEAPS and GPTMS modified HNTs/epoxy nanocomposites showed enhanced tensile strength and toughness. The toughing mechanisms were identified by the SEM micrographs of the fracture surfaces of the different kinds of samples. In this study, simultaneous enhancement of strength, toughness, and thermal stability of epoxy by the modified HNTs provides a novel approach to produce high‐performance thermosets. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43249.     

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.     

Investigating the strength of Ti/TiB interfaces at multiple scales using density functional theory,molecular dynamics,and cohesive zone modeling

Titanium/titanium boride (Ti/TiB) composites are interesting technological materials with prospective applications in the aerospace, automotive, and biomedical industries. However, not much has been studied about the failure mechanisms of these composites. This article thoroughly investigates the adhesion and strength of two well-known Ti/TiB interface variants formed during the production of Ti/TiB composites below and above 910 °C, respectively. The studies were carried out using different theoretical methods at multiple scales, including density functional theory (DFT), molecular dynamics (MD), cohesive zone modeling (CZM), and the finite element method (FEM). First, we employed DFT to investigate the interfacial adhesion and strength of the selected planes. Then, MD simulations were utilized to study the misfit dislocation networks and derive interfacial CZMs for FEM modeling and simulation of composites. Our FEM simulations showed that the Ti/TiB interface has sufficient strength to transfer the shear load from Ti to TiB without debonding at room temperature. The results have confirmed the same phenomenon observed in some experimental studies and interpreted this phenomenon from a multiscale point of view. The research findings can be used in quantifying the failure stress of TiB whiskers directly from tension tests on Ti/TiB composites by ruling out the possibility of interface debonding.     

Multifunctional epoxy resin/polyacrylonitrile‐lithium trifluoromethanesulfonate composites films with very high transparency,high dielectric permittivity,breakdown strength and mechanical properties

Multifunctional transparent composite films with high dielectric permittivity (high‐k), breakdown strength, and mechanical properties are urgently required by cutting‐edge fields. Herein, novel multifunctional films were facilely prepared through building unique cross‐linked structure based on epoxy resin (EP) and polyacrylonitrile (PAN)‐lithium trifluoromethane sulfonate (LiTf) complex. Compared with high‐k materials reported previously, EP/(PAN‐LiTf) films simultaneously show very high transparency, good flexibility, high tensile, and breakdown strengths. For 0.22EP/(PAN‐LiTf) film with 22 wt % EP, its average transmittance and elongation at break are as high as 91% (600–800 nm) and 12.7%, respectively; moreover, its dielectric permittivity, AC breakdown strength and the maximum energy density are severally about 4.9, 1.8, and 15.2 times of those of EP resin, completely overcoming the sticky problems in conductor/polymer composites. The origin behind these attractive properties is intensively discussed, and believed to be attributed to the unique structure of EP/(PAN‐LiTf) films. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45218.     

Preparation,structures and properties of interpenetrating network structure-type Phosphate/PEEK composites with enhanced compressive strength and high temperature resistance

Phosphate/polyether ether ketone (PEEK) composites were successfully prepared by molding method and thermal treating at the temperature of 360 °C. The structures and compositions of phosphate/PEEK composites were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, differential scanning calorimetry and scanning electron microscopy. The mechanical properties thermal resistance and dielectric properties were strictly evaluated by the mechanical testing, thermogravimetric analysis and dielectric constant analysis. As the results, the interpenetrating network structure (IPNS) of Al₂O₃-phosphates was completely formed in PEEK matrix. And the phosphate/PEEK composite with 40% Al₂O₃-phosphate showed a 15.9% increasing for tensile strength and 74.5% increasing for compressive strength at room temperature. Besides, the phosphate/PEEK composite with 80 wt% Al₂O₃-phosphate dispalyed a dielectric constant of 4.0, a dielectric loss of 0.0601 and a Shore hardness of 91 HD. As the structural materials, these composites would exhibited the potential applications in aviation, aerospace and other fields.