Processing and mechanical performance of 3D Cf/SiCN composites prepared by polymer impregnation and pyrolysis

The processing of 3D carbon fiber reinforced SiCN ceramic matrix composites prepared by polymer impregnation and pyrolysis (PIP) route was improved, and factors that determined the mechanical performance of the resulting composites were discussed. 3D C_f/SiCN composites with a relative density of ∼81% and uniform microstructure were obtained after 6 PIP cycles. The optimum bending strength, Young's modulus and fracture toughness of the composites were 75.2 MPa, 66.3 GPa and 1.65 MPa m^1/2, respectively. The residual strength retention rate of the as-pyrolyzed composites was 93.3% after thermal shock test at ΔT = 780 °C. It further degraded to 14.6% when the thermal shock temperature difference reached to 1180 °C. The bending strength of the composites was 35.6 MPa after annealing at 1000 °C in static air. The deterioration of the bending strength should be attributed to the strength degradation of carbon fibers and decomposition of interfacial structure.     

Microstructure,Mechanical, and Thermal Properties of (ZrB2 + ZrC)/Zr3[Al(Si)]4C6 Composite

The microstructure, mechanical, and thermal properties of in situ hot‐pressed 30 vol% (ZrB₂+ZrC)/Zr₃[Al(Si)]₄C₆ composite have been investigated and compared with monolithic Zr₃[Al(Si)]₄C₆ ceramic. The composite is composed of ZrB₂ and ZrC grains embedded in a Zr₃[Al(Si)]₄C₆ matrix. The composite shows superior hardness (Vickers hardness of 16.4 GPa), stiffness (Young's modulus of 415 GPa), strength (bending strength of 621 MPa), and toughness (fracture toughness of 7.37 MPa·m^1/2) compared with monolithic Zr₃[Al(Si)]₄C₆. The composite retains high modulus of 357 GPa at 1430°C (86% of that at ambient temperature) due to clean grain boundaries with no glassy phase. In addition, the composite exhibits higher specific heat capacity and thermal conductivity but slightly lower coefficient of thermal expansion compared with monolithic Zr₃[Al(Si)]₄C₆. The calculation of the thermal stress fracture resistance parameter (R) predicts a much improved thermal shock resistance of the composite. Based on these results, (ZrB₂+ZrC)/Zr₃[Al(Si)]₄C₆ composites show promising potential for high‐temperature and ultra high‐temperature applications.     

Pressure-less joining of SiCf/SiC composites by Y2O3–Al2O3–SiO2 glass: Microstructure and properties

In this study, Y₂O₃–Al₂O₃–SiO₂ (YAS) glass was prepared from Y₂O₃, Al₂O₃, and SiO₂ micron powders. Thermal expansion coefficient of as-obtained YAS glass was about 3.9 × 10⁻⁶, matching-well with that of SiC_f/SiC composites. SiC_f/SiC composites were then brazed under pressure-less state by YAS glass and effects of brazing temperature on microstructures and properties of resulting joints were investigated. The results showed that glass powder in brazed seam sintered and precipitated yttrium disilicate, cristobalite, and mullite crystals after heat treatment. With the increase in temperature, joint layer gradually densified and got tightly bonded to SiC_f/SiC composite. The optimal brazing parameter was recorded as 1400 °C/30 min and shear strength of the joint was 51.7 MPa. Formation mechanism of glass-ceramic joints was proposed based on combined analysis of microstructure and fracture morphology of joints brazed at different temperatures. Thermal shock resistance testing of joints was also carried out, which depicted decline in shear strength with the increase of thermal shock times. The strength of the joint after three successive thermal shock cycles at 1200 °C was 35.6 MPa, equivalent to 69% of that without thermal shock.     

Plastic deformation-induced improved mechanical and thermal properties in hot-forged SiC-TiC composite

A novel SiC-20 vol% TiC composite prepared via a two-step sintering technique using 6.5 vol% Y₂O₃-Sc₂O₃-MgO exhibited high deformation (60 %) on hot forging attributed to the high-temperature plasticity of TiC (ductile to brittle transition temperature ～800 °C) and fine-grained microstructure (～276 nm). The newly developed SiC-TiC composite exhibited a ～2-fold increase in nominal strain as compared to that of monolithic SiC. The plastic deformation caused by grain-boundary sliding in monolithic SiC was supplemented by the plastic deformation of TiC in the SiC-TiC composite. The hot-forged composite exhibited anisotropy in its microstructure and mechanical and thermal properties due to the preferred alignment of α-SiC platelets formed in situ. The relative density, flexural strength, fracture toughness, and thermal conductivity of the composite increased from 98.4 %, 608 MPa, 5.1 MPa?m^1/2, and 34.6 Wm^?1 K^?1 in the as-sintered specimen to 99.9 %, 718–777 MPa, 6.9–7.8 MPa?m^1/2, and 54.8–74.7 Wm^?1 K^?1, respectively, on hot forging.     

Tough and wear-resistant carbon fiber reinforced TiC-based composite prepared by alloyed melt infiltration at low temperatures

To improve the toughness and friction properties of carbon fiber reinforced ceramic matrix composite, a Cu alloy modified carbon fiber reinforced TiC based ceramic matrix composite was designed and prepared by TiCu alloy melt infiltration at low temperatures up to 1100 °C. The as-produced composite was mainly composed of carbon, TiC, Ti₃Cu₄, TiCu₄ and Cu phases. Due to the ductile Cu alloy introduced into the matrix, the composite showed good mechanical performance especially the fracture toughness. The flexural strength reached about 248.36 MPa while the fracture toughness was up to 15.78 MPa·m^1/2. The high toughness of the composite was mainly attributed to the fiber bridging, fiber pull-out, interface debonding, crack propagation and deflection. The tribological performance of the as-produced composite was measured using SiC and 440C stainless steel balls as counterparts, respectively. The as-prepared composite exhibited good wear resistance and the wear mechanism was discussed based on the microstructural observations.     

Effect of intermediate heat treatment on mechanical properties of SiCf/SiC composites with BN interphase prepared by ICVI

SiC_f/SiC composites with BN interface were prepared through isothermal-isobaric chemical vapour infiltration process. Room temperature mechanical properties such as tensile, flexural, inter-laminar shear strength and fracture toughness (K_IC) were studied for the composites. The tensile strength of the SiC_f/SiC composites with stabilised BN interface was almost 3.5 times higher than that of SiC_f/SiC composites with un-stabilised BN interphase. The fracture toughness is similarly enhanced to 23 MPa m^1/2 by stabilisation treatment. Fibre push-through test results showed that the interfacial bond strength between fibre and matrix for the composite with un-stabilised BN interface was too strong (>48 MPa) and it has been modified to a weaker bond (10 MPa) due to intermediate heat treatment. In the case of composite in which BN interface was subjected to thermal treatment soon after the interface coating, the interfacial bond strength between fibre and matrix was relatively stronger (29 MPa) and facilitated limited fibre pull-out.     

Strengthening and toughening of Ti5Si3 by TiC-coated short carbon fiber: Fabrication,interfacial control,and mechanism of reinforcement

Composites of C_f/Ti₅Si₃ were prepared by spark plasma sintering a mixture of TiC-coated short carbon fiber and pre-synthesized Ti₅Si₃ powder. The TiC coating protects the C_f and mediates a mild interdiffusion process between C_f and Ti₅Si₃, rather than an exothermic reaction. Compared with traditional in-situ fabrication, the use of a pre-synthesized Ti₅Si₃ powder as a raw material mitigated heat release from the Ti-Si reaction and consequent grain overgrowth. The spark plasma sintering process was completed within 15 min and the relative density of the product reached 99.2 %. The C_f/Ti₅Si₃ composite achieved a high fracture toughness of 7.57 MPa m^1/2 and a flexural strength of 518.3 MPa, which reflected increases of 255 % and 270 %, respectively, compared with those properties of monolithic Ti₅Si₃. These improvements are attributable to the effects of the carbon fiber reinforcement, the TiC protective coating on the C_f, inhibition of grain overgrowth, and control of interfacial reaction.     

Joining of SiCf/SiC using a layered Ti3SiC2-SiCw and TiC gradient filler

A layered filler consisting of Ti₃SiC₂-SiC whiskers and TiC transition layer was used to join SiC_f/SiC. The effects of SiC_w reinforcement in Ti₃SiC₂ filler were examined after joining at 1400 or 1500 °C in terms of the microstructural evolution, joining strength, and oxidation/chemical resistances. The TiC transition layer formed by an in-situ reaction of Ti coating resulted in a decrease in thermal expansion mismatch between SiC_f/SiC and Ti₃SiC₂, revealing a sound joint without cracks formation. However, SiC_f/SiC joint without TiC layer showed formation of cracks and low joining strength. The incorporation of SiC_w in Ti₃SiC₂ filler showed an increase in joining strength, oxidation, and chemical etching resistance due to the strengthening effect. The Ti₃SiC₂ filler containing 10 wt.% SiC_w along with the formation of TiC was the optimal condition for joining of SiC_f/SiC at 1400 °C, showing the highest joining strength of 198 MPa as well as improved oxidation and chemical resistance.     

SiC/Si3N4 nano/micro-composite — processing,RT and HT mechanical properties

Two SiC/Si₃N₄ nano/micro composites were prepared from a starting mixture of crystalline α-Si₃N₄, amorphous SiNC, Y₂O₃ and/or Al₂O₃. The composite material for room temperature (RT) application has high strength of 1200 MPa, Weibull modulus of 19 and moderate fracture toughness of 7 MPa m^1/2. The composite for high temperature (HT) application, without Al₂O₃ has RT strength of 710 MPa and is able to keep 60% of its RT strength up to 1300°C. The creep resistance of composite material is approx. 1 order higher compared to relative monolith up to 1400°C.     

Co-enhancement of oxidation resistance and mechanical properties of Cf/LAS composites: The effects of h-BN addition

Carbon fiber reinforced lithium aluminosilicate glass-ceramic composites have been extensively studied and widely used in industry applications, because of its good mechanical properties and low thermal expansion coefficient. However, further investigation is also need to improve its oxidation resistance and mechanical performance to meet higher requirements. In this work, C_f/LAS glass-ceramic composites were fabricated by a slurry impregnation and hot-pressing method with different amounts of h-BN. Results indicate that composites with 2 wt.% h-BN addition exhibit excellent flexural strength and fracture toughness, reaching 910 ± 22 MPa and 21 ± 1 MPa·m^1/2, respectively, and that after oxidation at 600, 800 and 1000 °C for 1 h, their strength residual ratio can reach 47%, 35% and 32%, respectively. TEM analyses suggest the improvement of oxidation resistance and mechanical properties should be attributed to the unique interface of composites caused by h-BN addition.     

Microstructures and mechanical properties of TiB2 composite ceramics with co-addition of Ti and TiC fabricated by SPS

TiB₂ composite ceramics containing different amounts of Ti and TiC were fabricated via spark plasma sintering (SPS), and effects of their addition contents on the microstructure and mechanical properties were discussed. The newly formed phases of TiB with a cubic lattice structure in the composite ceramics were observed. At a relatively low temperature of 1510 °C, pressure of 50 MPa, and holding time of 5 min, the TiB₂ composite ceramic with 30 wt% TiC and 10 wt% Ti additions acquired an excellent strength of 727 MPa and a high toughness of 7.62 MPa m^1/2. The improvement in strength and toughness was attributed to the mixed fracture mode, second phase strengthening, and increased energy consumption for crack propagation caused by the newly formed phases and fine TiC particles. In addition, the significant effects of the Ti and TiC addition contents on the densification temperature and mechanical properties of the composite ceramics were determined using analysis of variance (ANOVA).     

Fabrication and properties of three-directional orthogonal aluminosilicate fiber fabric-reinforced mullite composite

In this study, a three-directional orthogonal aluminosilicate fiber fabric-reinforced mullite composite with excellent properties was prepared by the precursor impregnation and pyrolysis (PIP) method. The influence of the number of PIP cycles on the microstructure and mechanical properties of the composite was studied. The density and mechanical properties of the composite enhanced with increasing number of PIP cycles. After the 6th PIP cycle, the density of the composite increased by only 0.8%, and the flexural strength and fracture toughness of the composite reached 130.1 MPa and 4.91 MPa m^1/2, respectively. Moreover, the thermal shock resistance of the composite was investigated by the high-low temperature (from 1300 °C to room temperature) thermal treatment and water quenching method. The strength retention rate of the composite after 10 high-low temperature thermal cycles was 90.1%; the retention rate dropped to 79.5% after 15 thermal cycles. The composite with the critical thermal shock temperature difference 843.9 °C displayed excellent thermal shock resistance.     

ZrO2f-coated Cf hybrid fibrous reinforcements and properties of their reinforced ceramicizable phenolic resin matrix composites

Carbon fiber-reinforced ceramicizable phenolic resin matrix composites have been widely used in the field of thermal protection materials. In this paper, the ZrO_2f-coated C_f (ZrO_2f/C_f) hybrid fibrous reinforcements were designed to improve oxidation resistance of carbon fiber and ceramicizable composites reinforced by ZrO_2f/C_f hybrid fibrous reinforcements were prepared to investigated oxidation resistance and mechanical properties of the composites at high temperature. The results show that ZrO_2f/C_f hybrid fibrous reinforcements have good thermal stability and high oxidation resistance, and its ceramicizable composites have good bending strength at high temperature. Weight loss rate of the composites is only 21 %, and bending strength can be as high as 39 MPa when ablation time was 12 min at 1400 °C.     

High-temperature fracture toughness of SiC–Mo5(Si,Al)3C composites

The fracture toughness (K_1C) of melt-infiltrated SiC–Mo₅(Si,Al)₃C composites was measured from room temperature to 1400°C using the indentation strength method at 1 atm argon atmosphere. The fracture toughness was found to increase from 3.6 MPa·m^1/2 at room temperature to 7.7 MPa·m^1/2 at 1400°C. This increase was mainly attributed to the plastic deformation of the infiltrated Mo₅(Si,Al)₃C phases at high temperatures, which act as ductile toughening inclusions. The influence of annealing temperatures and atmospheres on K_1C was studied. The effect of indentation load on K_1C was also analyzed.     

Enhanced mechanical properties and thermal shock resistance of Cf/ZrB2-SiC composite via an efficient slurry injection combined with vibration-assisted vacuum infiltration

An efficient slurry injection combined with vibration-assisted vacuum infiltration process has been developed to fabricate 3D continuous carbon fiber reinforced ZrB₂-SiC ceramics. Homogenous distribution between carbon fiber and ceramic was achieved successfully, leading to an enhancement in mechanical properties. The C_f-PyC/ZrB₂-SiC composite exhibited a typical non-brittle fracture mode with a superior fracture toughness of 6.72 ± 0.21 MPa·m^1/2 and an extraordinary work of fracture of 2270 J/m², respectively, increasing by nearly 14.8 % and 36 % as compared with those of a parent composite fabricated by only slurry injection and slurry infiltration. The enhancement in fracture toughness and work of fracture were attributed to multiple toughening mechanism including crack deflection, PyC coated fiber bundles pull-out and fiber bridging. Moreover, a critical thermal shock temperature difference of 814 °C was achieved, higher than that of traditional ZrB₂-based ceramics. This work presents an efficient approach to fabricate high-performance C_f/UHTCs with uniform architecture.     

Effects of ZrC content on the synthesis of MAX phase and mechanical properties of Cf-C-SiC-Ti3SiC2-ZrC composites

In this research synthesis of Ti₃SiC₂ nano-laminate, effects of Al and ZrC on the amount and morphology of the synthesized MAX phase and mechanical properties of the C_f-C-SiC, C_f-C-SiC-Ti₃SiC₂ and C_f-C-SiC-Ti₃SiC₂-ZrC composites, fabricated by LSI method, were investigated. The infiltration process was conducted at 1500?°C for 30?min and then the samples were annealed at 1350?°C. X-ray diffraction (XRD) technique and scanning electron microscopy (SEM) were utilized in order to investigate the phase composition and microstructure of the samples, respectively. The results showed that the sample containing Al, had the largest amount of synthesized MAX phase and also addition of ZrC led to the decrease of intensities of MAX phase peaks. Among the samples, C_f-C-SiC-Ti₃Si(Al)C₂ had the best mechanical properties compared to the others. Bending strength, interlaminar shear strength and fracture toughness of this sample were 505?MPa, 34?MPa and 19.1?MPa?m^1/2 respectively. The results confirmed that the mechanical properties were decreased by addition of ZrC. Among ZrC-containing samples, the sample containing 10?vol% ZrC has shown the least decrease properties including the bending strength of 369.11?MPa, interlaminar shear strength of 26?MPa and fracture toughness of 16.9?MPa?m^1/2. Addition of ZrC phase caused pseudo-plastic behavior appearance in the force-displacement curve and led to fibers pull-out and also displacement enhancement. Microstructural observations confirmed the plate-like morphology of synthesized MAX phases. Furthermore, the distance between layers decreased and MAX phase size increased respectively by addition of Al. Also MAX phase size decreased by increasing the ZrC content. It was confirmed that the MAX phase-containing samples can tolerate various micro-deformation mechanisms including: crack deflection, bending and delamination of lamellae, kink boundary and laminate fracture. These mechanisms led to the toughening of the composites.     

Preceramic paper-derived Ti3Al(Si)C2-based composites obtained by spark plasma sintering

The paper describes the structure and properties of preceramic paper-derived Ti₃Al(Si)C₂-based composites fabricated by spark plasma sintering. The effect of sintering temperature and pressure on microstructure and mechanical properties of the composites was studied. The microstructure and phase composition were analyzed by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. It was found that at 1150 °C the sintering of materials with the MAX-phase content above 84 vol% leads to nearly dense composites. The partial decomposition of the Ti₃Al(Si)C₂ phase becomes stronger with the temperature increase from 1150 to 1350 °C. In this case, composite materials with more than 20 vol% of TiC were obtained. The paper-derived Ti₃Al(Si)C₂-based composites with the flexural strength > 900 MPa and fracture toughness of >5 MPa m^1/2 were sintered at 1150 °C. The high values of flexural strength were attributed to fine microstructure and strengthening effect by secondary TiC and Al₂O₃ phases. The flexural strength and fracture toughness decrease with increase of the sintering temperature that is caused by phase composition and porosity of the composites. The hardness of composites increases from ~9.7 GPa (at 1150 °C) to ~11.2 GPa (at 1350 °C) due to higher content of TiC and Al₂O₃ phases.     

Effect of short carbon fibre concentration on microstructure and mechanical properties of TiCN-based cermets

Short carbon fibre (C_f) reinforced TiCN-based cermets (C_f/TiCN composites) were produced by powder metallurgy method with pressureless sintering technology. The phase evolution, microstructure and fracture morphology of C_f/TiCN composites were investigated. The results showed that TiC, TiN, WC, Cr₃C₂ and Mo phases disappeared gradually and diffused into core and rim phases by dissolution–reprecipitation process, finally formed new hard TiCN core phases and complex compound (Cr, W, Mo, Ti)(CN) rim phases, with the sintering temperature increasing. The added C_f did not change the ‘core–rim’ microstructure but improved the mechanical properties of TiCN-based cermets. The C_f/TiCN composite containing 3?wt-% C_f achieved the best comprehensive mechanical properties, with fracture toughness and bending strength increasing by about 14.4% and 30.8%, respectively, when compared with the composite without C_f. Toughening and strengthening mechanisms of C_f/TiCN composite were concluded as crack deflection and branch, as well as the pull-out, fracture and bridging of carbon fibres.     

Fabrication and characterization of carbon fiber reinforced SiC ceramic matrix composites based on 3D printing technology

A novel method has been developed to fabricate carbon fiber reinforced SiC (C_f/SiC) composites by combining 3D printing and liquid silicon infiltration process. Green parts are firstly fabricated through 3D printing from a starting phenolic resin coated carbon fiber composite powder; then the green parts are subjected to vacuum resin infiltration and pyrolysis successively to generate carbon fiber/carbon (C_f/C) preforms; finally, the C_f/C preforms are infiltrated with liquid silicon to obtain C_f/SiC composites. The 3D printing processing parameters show significant effects on the physical properties of the green parts and also the resultant C_f/C preforms, consequently greatly affecting the microstructures and mechanical performances of the final C_f/SiC composites. The overall linear shrinkage of the C_f/SiC composites is less than 3%, and the maximum density, flexural strength and fracture toughness are 2.83?±?0.03?g/cm³, 249?±?17.0?MPa and 3.48?±?0.24?MPa m^1/2, respectively. It demonstrates the capability of making near net-shape C_f/SiC composite parts with complex structures.     

SiC–AlN Particulate Composite

A SiC–AlN composite was fabricated by mechanical mixing of SiC and AlN powders, hot pressed under 40 MPa at 1950°C in Ar atmosphere. The object of this attempt was to achieve full density and a little solid solution formation. Fine microstructure and crack deflection behaviour are to improve the mechanical properties of the SiC–AlN composite. The bending strength and fracture toughness were achieved 800 MPa and 7·6 MPa m^1/2 at room temperature, respectively. The fracture toughness of the SiC–AlN composite shows minimal change between room temperature and 1400°C. Post-HIP improves the surface densification of the SiC–AlN composite resulting in an increase of the strength and the ability to resist oxidization. The bending strength of SiC–AlN composite increases from 800 to 1170 MPa after HIP treatment for 1 h under 187 MPa at 1700°C in N₂ atmosphere.