Mechanical properties and microstructure evolution of 3D Cf/SiBCN composites at elevated temperatures

3D C_f/SiBCN composites were fabricated by an efficient polymer impregnation and pyrolysis (PIP) method using liquid poly(methylvinyl)borosilazanes as precursor. Mechanical properties and microstructure evolution of the prepared 3D C_f/SiBCN composites at elevated temperatures in the range of 1500‐1700°C were investigated. As temperature increased from room temperature (371 ± 31 MPa, 31 ± 2 GPa) to 1500°C (316 ± 29 MPa, 27 ± 3 GPa), strength and elastic modulus of the composite decreased slightly, which degraded seriously as temperature further increased to 1600°C (92 ± 15 MPa, 12 ± 2 GPa) and 1700°C (84 ± 12 MPa, 11 ± 2GPa). To clarify the conversion of failure mechanisms, interfacial shear strength (IFSS) and microstructure evolution of the 3D C_f/SiBCN composites at different temperatures were investigated in detail. It reveals that the declines of the strength and changes of the IFSS of the composites are strongly related to the defects and SiC nano‐crystals formed in the composites at elevated temperatures.     

Mechanical and thermal shock properties of Cf/SiBCN composite: Effect of sintering densification and fiber coating

In this work, resin-derived carbon coating was prepared on carbon fibers by polymer impregnation pyrolysis method, then silicoboron carbonitride powder was prepared by mechanical alloying, and finally carbon fiber-reinforced silicoboron carbonitride composites were prepared by hot-pressing process. The effects of sintering densification and fiber coating on microstructure, mechanical properties, thermal shock resistance, and failure mechanisms of the composites were studied. Fiber bridging hinders the sintering densification, causing more defects in fiber-dense area and lower strength. However, higher sintering temperature (1800–2000°C) can improve mechanical properties significantly, including bending strength, vickers hardness, and elastic module, because further sintering densification enhances matrix strength and fiber/matrix bonding strength, while the change of fracture toughness is not obvious (2.24–2.38 MPa·m^1/2) due to counteraction of higher debonding resistance and less pull-out length. However, fiber coating improves fracture toughness greatly via protecting carbon fibers from chemical corrosion and damage of thermal stress and external stress. Due to lower coefficient of thermal expansion, lower fiber loading ratio, less stress concentration at the fiber/matrix interface, and better defect healing effect, lower sintering temperature favors thermal shock resistance of composites, and thermal shock recession mechanisms are the damage of interface.     

Ablation behavior and mechanism of Cf/SiBCN composites in plasma ablation flame

In this work, C_f/SiBCN composites are fabricated by an improved precursor infiltration and pyrolysis (PIP) approach. Ablation behavior of the C_f/SiBCN composites is investigated in plasma ablation flame at a heat flux of 4.02 MW m⁻², which provides a quasi-real hypersonic service environment at a temperature up to 2200°C. After ablation, the ablated surface is covered with oxidation products in the form of oxide layer, fibrous residues, or bubbles, which effectively isolates the sample surface from the plasma flame and inhibits the scouring of high-speed flame to the composites. As a result, the C_f/SiBCN composites present an excellent ablation-resistant property, with linear and mass recession rates as low as 0.0030 mm s⁻¹ and 0.0539 mg mm⁻² s⁻¹, respectively. It is also revealed that the material at ablation center undergoes crystallization and oxidation processes during ablation, while the ablation behavior at transition area and ablation fringe only contains oxidation process due to the local temperature difference. Si₃N₄ and SiC grains are precipitated from amorphous SiBCN matrix during the crystallization process, and the oxidation process mainly involves the oxidation of carbon fiber and SiBCN matrix, etc.     

碳纤维增韧增强氮化硅陶瓷基复合材料力学性能的数值模拟

基于Tanake-Mori基体平均应力以及Eshlby等效夹杂法，提出了1种求连续相材料的应力和应变的近似理论，由此可精确评估两相和3相复合材料的力学性能。本文利用计算机模拟对碳纤维增韧的氮化硅复合材料（Cf/Si3n4)的弹性模量、剪切模量和泊松比进行理论计算，从其内部微观结构出发，探讨了不同相含量、气孔的含量以及形状等复合材料力学性能的影响。     

Influence of sol-gel derived ZrB2 additions on microstructure and mechanical properties of SiBCN composites

A simple method for introducing ZrB₂ using sol-gel processing into a SiBCN matrix is presented in this paper. Zirconium n-propoxide (ZNP), boric acid and furfuryl alcohol (C₅H₆O₂) (FA) were added as the precursors of zirconia, boron oxide and carbon forming ZrB₂ dispersed in a SiBCN matrix. SiBCN/ZrB₂ composites with different contents of ZrB₂ (5, 10, 15, and 20 wt%) were formed at 2000 °C for 5 min by spark plasma sintering (SPS). The microstructures were carefully studied. TEM analysis showed that the as formed ZrB₂ grains were typically 100–500 nm in size and had uniform distribution. HRTEM revealed clean grain boundaries between ZrB₂ and SiC, however, a separation of C near the SiC boundary was observed. The flexural strength, fracture toughness, Young's modulus and Vicker's hardness of composites all improved with the ZrB₂ contents and SiBCN matrix containing 20 wt% of ZrB₂ could reach 351±18 MPa, 4.5±0.2 MPa m^1/2, 172±8 GPa and 7.2±0.2 GPa, respectively. The improvement in fracture toughness can be attributed to the tortuous crack paths due to the presence of reinforcing particles.     

High-temperature electromagnetic wave absorption properties of Cf/SiCNFs/Si3N4 composites

Carbon fibers reinforced Si₃N₄ composites with SiC nanofiber interphase (C_f/SiCNFs/Si₃N₄) were prepared by combining catalysis chemical vapor deposition and gel-casting process. Microstructures, mechanical properties, and electromagnetic wave absorption properties within X-band at 25°C-800°C of C_f/SiCNFs/Si₃N₄ composites were investigated. Results show that SiC nanofibers are combined well with Si₃N₄ matrix and carbon fibers, the fracture toughness is thus increased more than double from 3.51 MPa·m^1/2 of the Si₃N₄ ceramic to 7.23 MPa·m^1/2 of the as-prepared composites. As the temperature increases from 25°C to 800°C, C_f/SiCNFs/Si₃N₄ composites show a temperature-dependent complex permittivity, attenuation constant, and impedance. The relatively high attenuation capability of C_f/SiCNFs/Si₃N₄ composites at elevated temperature results in a great minimum reflection loss of −20.3 dB at 800°C with a thin thickness of 2.0 mm. The superior electromagnetic wave absorption performance mainly originates from conductive loss, multi-reflection, and strong polarization formed by the combined effects of carbon fibers and SiC nanofibers.     

Effects of heat treatment temperatures on microstructures and mechanical properties of the chopped carbon fibres SiC composites

ABSTRACT

A simple wet papermaking technique was used to fabricate chopped carbon fibre paper (C_sf-paper) with random fibre orientation and self-supporting network structures in this work. The C_sf-papers were laminated layer by layer and further infiltrated with PyC interface and SiC matrix via chemical vapour infiltration (CVI) to obtain C_sf/SiC composites. The effects of heat treatment temperatures on microstructures, phase composition, and mechanical properties were investigated. Results showed that the C_sf-paper has played a good self-supporting role and its fibres form a completely random fibre orientation in 2D plane. The fibres almost remained undamaged and unbroken during the CVI. Proper heat treatment could improve the mechanical properties. At 1200°C, the maximum values of flexural strength and Young's modulus reached about 306 MPa and 196.5 GPa, respectively. Meanwhile, compared with tape casting, reaction sintering and spark plasma sintering, composites fabricated by wet papermaking and CVI can improve the mechanical properties.     

Synthesis of coatings on SiC fibers and their effects on microstructure and mechanical properties of SiCf/SiBCN composites

In this study, the amorphous C, ZrB₂, and BN single-layer coatings as well as C/BN, C/ZrB₂, ZrB₂/BN, and C/ZrB₂/BN composite coatings were prepared on SiC fibers (SiC_f) by an in situ synthesis and solution impregnation–pyrolysis method. Subsequently, SiC_f/SiBCN composites were fabricated by hot-pressing sintering at 1900℃/60 MPa/30 min to explore the influence of different coatings on the microstructure and mechanical performance of resulting composites. After the preparation of single-layer-coated SiC_f, the SiC_f(BN) or SiC_f(ZrB₂) tended to be overlapped with each other, whereas the dispersion of amorphous C–coated SiC_f was satisfying. Besides, some uneven areas and attached particles have appeared on fiber surfaces of the SiC_f(BN) or SiC_f(ZrB₂), whereas smooth and dense surfaces of amorphous C–coated SiC_f were observed. Because the uniformity of ZrB₂ coatings can be partially damaged by the subsequent coating process of BN, the composite coatings of ZrB₂/BN and C/ZrB₂/BN were thereby not suitable for strengthening SiBCN matrix. The SiC_f/SiBCN composites with C/ZrB₂ coatings have desirable comprehensive mechanical properties. Nevertheless, the conventional toughening mechanisms such as fiber pull-out and bridging, and crack deflection are not available for these composites because the serious crystallization of SiC_f leading to great strength loss, resulting in catastrophic brittle fracture.     

Microstructures and mechanical properties of Cf/LAS composite and Ti60 alloy joints brazed with TiZrNiCu + Cf mixed powders

In this paper, carbon fiber reinforced lithium aluminosilicate (LAS) glass-ceramics matrix composites (C_f/LAS composites) are joined to Ti60 alloy using TiZrNiCu + C_f mixed powders by proper process parameters. The carbon fibers distribute uniformly in the brazing interlayer and react with Ti, Zr elements in the brazing alloy to form (Ti, Zr)C thin reactive layers, which are between the carbon fibers and the Ti, Zr elements. The effect of C_f content on the mechanical properties and microstructure of brazed joints are investigated. The microstructure of brazed joints varied obviously with the increasing of C_f content. The thickness of reactive layer between interlayer and C_f/LAS composites and Ti solid solution (Ti (s.s)) decrease gradually, and the volume of eutectic structure (Ti(s,s) + (Ti,Zr)₂(Ni,Cu)) decrease gradually. The obtained brazed joints exhibit a maximum shear strength of 73.5 MPa at room temperature using TiZrNiCu + 0.3 wt% C_f mixed powders. The enhanced shear strength can be attributed to the reduction in thermal stress and the reinforcing effect originated from the carbon fiber addition.     

Additive manufacturing of high mechanical strength continuous Cf/SiC composites using a 3D extrusion technique and polycarbosilane-coated carbon fibers

A novel additive manufacturing approach is herein reported for manufacturing high mechanical strength continuous carbon fiber-reinforced silicon carbide (C_f/SiC) composite materials. Continuous carbon fibers were coated with polycarbosilane (PCS) using a colloidal evaporative deposition process and then coextruded with high solid content SiC ink. The zeta potential of the SiC ink was adjusted to optimize the printing ability of the suspension. During sintering, small SiC grains and whiskers were generated in the gaps in and around the PCS-coated carbon fibers, which led to the improved flexural strength and density of the composites. Meanwhile, the PCS coating on the surface of the carbon fibers prevented the carbon fibers from reacting with SiO gas generated by reactions between the SiC matrix and SiO₂ and sintering additives (Al₂O₃ and Y₂O₃), effectively preserving the structural integrity of the carbon fibers. Compared to the SiC specimens containing uncoated carbon fibers, the density of the specimens fabricated with coated carbon fibers was increased from 2.51 to 2.85 g/cm³, and the strength was increased from 190 to 232 MPa.     

Enhanced mechanical and dielectric properties of SiCf/SiC composites with silicon oxycarbide interphase

SiC_f/SiC composites with silicon oxycarbide (SiOC) interphase were successfully prepared using silicone resin as interphase precursor for dip-coating process and polycarbosilane as matrix precursor for PIP process assisted with hot mold pressing. The effects of SiOC interphase on mechanical and dielectric properties were investigated. XRD and Raman spectrum results show that SiOC interphase is composed of silicon oxycarbide and free carbon with a relatively low crystalline degree. The surface morphology of SiC fibers with SiOC interphase is smooth and homogeneous observed by SEM. The flexural strength and failure displacement of SiC_f/SiC composites with SiOC interphase vary with the thickness of interphase and the maximum value of flexural strength is 289 MPa with a failure displacement of 0.39 mm when the thickness of SiOC interphase is 0.25 µm. The complex permittivity of the composites increases from 8.8-i5.7 to 9.8-i8.3 with the interphase thicker.     

High-temperature properties and interface evolution of C/SiBCN composites prepared by precursor infiltration and pyrolysis

C/SiBCN composites with a density of 1.64 g/cm³ were prepared via precursor infiltration and pyrolysis and the bending strength and modulus at room temperature was 305 MPa and 53.5 GPa. The precursor derived SiBCN ceramics showed good thermal stability at 1600 °C and the SiC and Si₃N₄ crystals appeared above 1700 °C. The bending strength of the composites was 180 MPa after heat treatment at 1500 °C, and maintained at 40 MPa-50 MPa after heat treatment for 2 h at 1600 °C–1900 °C. In C/SiBCN composites, SiBCN matrix could retain amorphous up to 1500 °C and SiC grains appeared at 1600 °C but without Si₃N₄. The reason for no detection of Si₃N₄ was that the carbon fiber reacted with Si₃N₄ to form an interface layer (composed of SiC and unreacted C) and a polycrystalline transition layer (composed of B and C elements), leading to the degradation of the mechanical properties.     

Preparation,microstructures, and mechanical properties of directionally solidified Al2O3/Lu3Al5O12 eutectic ceramics

Al₂O₃/Lu₃Al₅O₁₂ (LuAG) directionally solidified eutectic (DSE) ceramics with two solidification rates were prepared utilizing optical floating zone (OFZ) technique. The microstructures (eutectic morphology, preferred growth direction and interface orientation) of Al₂O₃/LuAG were characterized, and the mechanical properties (Vickers hardness and fracture toughness) were compared with those of Al₂O₃/REAG (RE = Y, Er, and Yb). Results show that Al₂O₃/LuAG with solidification rate of 30 mm/h has established preferred growth direction in both Al₂O₃ and LuAG phases with cellular eutectic structures. While Al₂O₃/LuAG with solidification rate of 10 mm/h only shows preferred growth direction in Al₂O₃ phase and presents degenerate irregular eutectic microstructures. Besides, Al₂O₃/LuAG exhibits higher hardness compared with Al₂O₃/REAG (RE = Y, Er, and Yb). In addition, a special attention is focused on the relations among rare earth ionic radius, eutectic microstructures, and mechanical properties of these DSE ceramics. It is demonstrated that a smaller rare earth ionic radius could lead to larger eutectic interspacing as well as higher Vickers hardness of DSE Al₂O₃/REAG, revealing the possibility and feasibility of microstructure control and mechanical properties optimization for DSE Al₂O₃/REAG ceramics by tailoring the rare earth elements.     

Microstructures and tribological behaviors of Cf/C-SiC composites tailored by Cu and Fe-Si matrices

Ternary Cu-Fe-Si alloy were applied to modify tribological behavior of carbon fiber/carbon-silicon carbide (C_f/C-SiC) composites by reactive melt infiltration. Microstructures, physical properties and tribological properties on a full-scale train brake test rig of the modified composites were studied. Results indicate that both Cu and Fe-Si alloy as matrices lead to significantly enhanced thermal conductivity and compressive strength for C_f/C-SiC composites. Moreover, the average friction coefficient of the modified composites is between 0.25 and 0.55, which is higher than that of copper metal matrix composites. In addition, the average volume wear rate of the modified composites is only 0.168 cm³/MJ. The C_f/C-SiC composites modified by Cu and Fe-Si alloy with improved physical properties and tribological properties meet the technical requirement and show high application potential in express train brake systems.     

Effect of ZrC amount and distribution on the thermomechanical properties of Cf/SiC-ZrC composites

C_f/SiC-ZrC composites with different amounts and distributions of ZrC were fabricated by polymer impregnation and pyrolysis. The effects of the ZrC amount and distribution on the microstructural, mechanical, and ablation properties of C_f/SiC-ZrC composites were investigated. C_f/SiC-ZrC composites obtained by the alternating infiltration of ZrC organic precursors and polycarbosilane groups exhibit good tensile strength (240 ± 17.7 MPa) because the ZrC and SiC matrix can mix evenly. However, C_f/SiC-ZrC composites using only ZrC organic precursor infiltration show a low tensile strength (191 ± 16.6 MPa) because more defects can be introduced into the composites. Ablation characterization by a 30 kW plasma wind tunnel for 60 seconds showed that the C_f/SiC-ZrC composites with the highest amount of ZrC matrix (67.8 wt.%) possessed the lowest linear erosion rate of 4 μm/s because liquid SiO₂ could fill the porous ZrO₂ to form a homogenous protective layer. Nevertheless, the C_f/SiC-ZrC composites with a relatively high ZrC amount (55.3 wt.%) exhibited a poorer ablation performance compared to that of C_f/SiC-ZrC composites with a low ZrC amount (38.7 wt.%).     

Loading rate effects on mechanical properties of polymer composites at ultralow temperatures

E‐glass fibers of 55, 60, and 65 weight percentages were reinforced with epoxy matrix to prepare the laminated composites. They were exposed to ?40, ?60, and ?80°C temperatures for different times. The 3‐piont bend test was conducted on the conditioned samples at those temperatures. Mechanical test was carried out at 2 mm/min and 500 mm/min crosshead speeds. The main emphasis of the investigation was to evaluate the roles of percentage matrix phase and interfacial areas on the interlaminar shear failure mechanism of glass/epoxy composites at ultralow temperatures for different loading speeds. The mechanical performances of the laminated specimens at low temperatures were compared with room temperature property. The loading rate sensitivity of the polymer composites appeared to be inconsistent and contradictory at some points of conditioning time and as well as at a temperature of conditioning. This Phenomenon may be attributed to low‐temperature hardening, matrix cracking, misfit strain due to differential thermal coefficient of the constituent phases, and also to enhanced mechanical keying factor by compressive residual stresses at low temperatures. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 100: 2289–2292, 2006     

Mechanical and electrical properties of 3Y-TZP/TiSi2 composites sintered at different temperatures

Various amounts of TiSi₂ (30, 40, and 50 wt.%) were added to 3 mol% yttria stabilized tetragonal zirconia polycrystals (3Y-TZP) to fabricate 3Y-TZP/TiSi₂ composites by vacuum sintering. The effects of the TiSi₂ added amount, as well as the sintering temperature on the microstructure, mechanical, and electrical characteristics of the 3Y-TZP/TiSi₂ composites were examined. The sintered samples consisted of three phases: tetragonal (t-ZrO₂), TiSi₂, and reaction product Ti₅Si₃. The maximum bending strength and relative density of the composites, reaching 501.20 MPa and 98.59% respectively, were achieved at a TiSi₂ content of 30 wt.% and sintering temperature of 1500°C. The resistivity of 3Y-TZP/TiSi₂ composites showed a nonlinear decrease with increasing TiSi₂ content. These results indicated that 3Y-TZP/TiSi₂ composites had a typical percolation threshold phenomenon due to the different TiSi₂ content and a conductivity model of 3Y-TZP/TiSi₂ composites at room temperature was founded on the generalized effective medium equation. The resistivity of the composites could optionally adjust between 10² and 10⁻⁴Ω·cm with 30–50 wt.% TiSi₂ under room temperature. Overall, the 3Y-TZP/TiSi₂ composites show great potential for applications in the heat-not-burn tobacco field.     

High-temperature oxidation behavior and oxidation mechanism of C/SiBCN composites in static air

On account of the excellent oxidation resistance of precursor-derived SiBCN ceramics, carbon-fiber-reinforced SiBCN (C/SiBCN) composites are increasingly being used in high-temperature aerospace applications. However, very few studies have investigated the high-temperature oxidation behavior of C/SiBCN composites for their application to high-heat engines. Herein, C/SiBCN composites prepared by precursor infiltration and pyrolysis were tested in static air up to an oxidation temperature of 1700 °C. The composites’ structural evolution after oxidation and their potential oxidation mechanisms were investigated in detail. The carbon fibers were preferentially oxidized at temperatures in the range of 1200–1500 °C and completely oxidized at 1500 °C. The oxidation of the fibers at 1500 °C resulted in the formation of abundant oxygen channels and consequently a high oxide scale growth rate of 5–7 μm² h⁻¹ and a large mass loss of 54.6 wt%. At elevated temperatures in the range of 1600–1700 °C, a dense SiO₂ oxide layer was formed by the sacrificial oxidation of the SiBCN matrix. The oxidation rate of the composites was therefore controlled by the diffusion rate of oxygen through the protective SiO₂ oxide layer and the weight loss of the composites decreased to 28.6% after oxidation at 1600 °C for 60 min. The structural integrity of the composites was maintained after long-term oxidation at 1600 °C.     

Effects of SiC/HfC ratios on the ablation and mechanical properties of 3D Cf/HfC-SiC composites

Effects of SiC/HfC ratios on the ablation and mechanical properties of 3D C_f/HfC–SiC composites by precursor impregnation and pyrolysis (PIP) process were investigated systematically. Both strength (flexural and compressive strength) and modulus increase as the SiC/HfC ratio are improved. The compact and stiff HfC-SiC matrix in addition to the carbon fiber and PyC interphase with less reaction damage accounts for the improved mechanical properties of C_f/HfC-SiC with higher SiC/HfC ratios. Meanwhile, both weight loss and erosion depth of C_f/HfC-SiC are improved with the increased SiC/HfC ratios. Therefore, in order to balance the ablation and mechanical properties, an appropriate SiC/HfC ratio should be considered.     

Carbon content-dependent microstructures,surface characteristics and thermal stability of mechanical alloying derived SiBCN powders

Three types of SiBCN: carbon-lean, -moderate and -rich powders with the same Si/B/N mole ratio were subjected to high-energy ball milling to yield an amorphous structure. The effects of carbon content on microstructures, solid-state amorphization, surface characteristics and thermal stability of the as-milled powders were studied in detail. Results showed that the increases in carbon content can drive solid-state amorphization accompanied by strain-induced, crystallite refinement-induced and/or chemical composition-induced nucleation of nano-SiC from an amorphous body. The specific surface area increases as carbon content increases. The amorphous networks of Si–C, C–B/C–C, C–N, B–N and C–B–N bonds that compose the amorphous nature, but the species and contents of the chemical bonds are carbon content-dependent. Carbon-moderate powders possess satisfying thermal stability while carbon-rich ones perform the worst. Mechanical alloying derived SiBCN powders have outstanding oxidation resistance below 800 °C; however only carbon-moderate powders show desirable anti-oxidation ability at higher temperatures. Thus, mechanical alloying of SiBCN appears a suitable technique for developing amorphous matrix materials for practical applications.