Effect of pyrolysis temperature on the mechanical evolution of SiCf/SiC composites fabricated by PIP

Three types of SiC_f/SiC composites with a four-step three-dimensional SiC fibre preform and pyrocarbon interface fabricated via precursor infiltration and pyrolysis at 1100 °C, 1300 °C, and 1500 °C were heat-treated at 1300 °C under argon atmosphere for 50 h. The effects of the pyrolysis temperature on the microstructural and mechanical properties of the SiC_f/SiC composites were studied. With an increase in the pyrolysis temperature, the SiC crystallite size of the as-fabricated composites increased from 3.4 to 6.4 nm, and the flexural strength decreased from 742 ± 45 to 467 ± 38 MPa. After heat treatment, all the samples exhibited lower mechanical properties, accompanied by grain growth, mass loss, and the formation of open pores. The degree of mechanical degradation decreased with an increase in the pyrolysis temperature. The composites fabricated at 1500 °C exhibited the highest property retention rates with 90% flexural strength and 98% flexural modulus retained. The mechanism of the mechanical evolution after heat treatment was revealed, which suggested that the thermal stability of the mechanical properties is enhanced by the high crystallinity of the SiC matrix after pyrolysis at higher temperatures.     

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.     

Thermal transport characteristics in diamond/SiC composites via molten Si infiltration

Heat dissipation remains a critical challenge in optical and electronic devices and diamond/SiC composite is the premiere material solution because of its outstanding thermal and mechanical properties. Si liquid infiltration is one of the most promising techniques to fabricate fully dense diamond/SiC composites with desired phase structures and exceptional properties. In this study, the thermal conductivity from room temperature to 1000 °C was investigated for the diamond/SiC composites fabricated by a liquid Si infiltration method. The experimental thermal measurement shows a good agreement with the computational solution obtained by solving the Boltzmann transport equation. The results suggest a strong correlation between the composite thermal conductivity and diamond volume percentage. A level-off of the thermal conductivity at high diamond content reflects increased thermal resistance. In addition, the annealing effect on the composite thermal conductivity as well as the thermal stability were evaluated.     

Effect of thermal residual stress on the tensile properties and damage process of C/SiC composites at high temperatures

Due to the mismatch of the thermal expansion coefficients between the matrix and yarns, thermal residual stress will appear in C/SiC composites. In this paper, a progressive damage model was used to predict the thermal-mechanical behavior of C/SiC composites and reveal the failure mechanism. Firstly, the properties of the composites under tensile load were tested at three different temperatures in vacuum. Then, the elastic-plastic progressive damage constitutive laws were used and implemented by a user-defined subroutine UMAT in ABAQUS. The thermal residual stress evolution in the cooling and heating processes was characterized. Finally, the stress-strain curves of the composites under tensile load at different temperatures were studied. The effects of thermal residual stress on the tensile properties and progressive damage process of C/SiC composites were revealed sequentially. This work can give design guidance for strengthening of C/SiC composites.     

Effect of oxidation and residual stress on mechanical properties of SiC seal coated C/SiC composite

The effect of oxidation and thermal residual stress on mechanical properties of SiC seal coated C/SiC composite at ambient temperature and high temperature were studied. The oxidation of SiC seal coated C/SiC composite at 1300 and 1500 °C resulted in carbon fibres burn area near through thickness micro cracks in the SiC seal coating. With the increase in exposure time, the formation of SiO₂ layer in SiC matrix near carbon fibres burns area was found. Residual mechanical properties of SiC seal coated C/SiC composite after exposure in air show significant degradation. First time, a continuous measurement of Young's modulus with temperature of C/SiC composite was carried out using an impulse excitation technique. The effect of relaxation of thermal residual stress on mechanical properties was observed with the help of continuous measurement of Young's modulus as a function of temperature in an inert atmosphere.     

Evaluation of mechanical properties of a dense SiC/SiCN composite produced via PIP process

The material behavior of Polymer Infiltration and Pyrolysis based SiC/SiCN composites is studied and the characteristic thermal and mechanical properties in on- (0/90 °) and off-axis (±45 °) direction are summarized. The tensile properties are determined at room temperature and 1300 °C. Based on the ratio of Young’s modulus and strength between on- and off-axis loading, a new approach for the classification of Weak Matrix Composites (WMC) and Weak Interface Composites (WIC) is proposed, which seems to be reasonable for various CMCs. Even without fibre coating mechanical behavior of SiC/SiCN is similar to that of WIC. In order to explain this, a microstructure model is developed and confirmed by analysis of fracture surface. The effect of temperature on the tensile properties is investigated through analysis of residual thermal stresses. Even though at 1300 °C the strength is slightly lower, the fracture strain increased significantly from RT to 1300 °C.     

High temperature bending properties and failure mechanism of 3D needled C/SiC composites up to 2000 ℃

Three-dimensional (3D) needled C/SiC composites were prepared and subjected to three-point bending tests from room temperature (RT) to 2000 ℃ under vacuum. The results show that the flexural strength and modulus increase in the range of RT to 800 °C due to the release of thermal residual stress (TRS). At 800–1700 °C, the modulus further increases for the further release of TRS, while the destruction of the pyrolytic carbon (PyC) coating reduces the flexural strength. Up to 2000 ℃, the thermal mismatch stress in the composites cause fiber slippage and matrix crack deflection to be zigzag, which increase the fracture strength. The change of components properties mediated by high temperature and the release of TRS play a leading role in the flexural strength and fracture mode. The results provide important support for the mechanical behavior of 3D needled C/SiC composites at ultra-high temperature.     

Flexural modulus of SiC/SiC composites sintered by microwave and conventional heating

To deeply study the variation mechanisms of mechanical properties, flexural modulus of SiC fibers reinforced SiC matrix (SiC/SiC) composites prepared by conventional and microwave heating at 800?°C–1100?°C was discussed in detail. The elastic modulus of fibers and matrix, interface bonding strength and porosity of SiC/SiC composites were considered together to analyze the changing tendencies and differences in their flexural modulus. The elastic modulus of fiber and matrix was determined by nanoindentation technique and interface characteristics applying fiber push-out test. The porosity and microstructure examinations were characterized by mercury intrusion method, X-ray Diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). Moreover, two conflicts between the changing trends of elastic modulus and chemical compositions of composite components were focused and explained. Results indicate that three factors played different roles in the flexural modulus of SiC/SiC composites and residual tensile stress in composite components led to the conflicts between their elastic modulus and chemical compositions.     

XCT damage evaluation and analysis of SiC/SiC turbine guide vanes after thermal shocks

In this paper, the two-dimensional (2D) (0°/90°) plain-woven Amosic-3 SiC/SiC turbine guide vane (TGV) was fabricated using the chemical vapor infiltration method. Thermal and stress analysis of the TGV was conducted using the finite element method analysis. Multiple thermal shock tests at T = 1250, 1350, 1400, 1420, 1450, 1470, and 1480°C were conducted for N = 100, 100, 400, 300, 200, 200, and 700 cycles. After thermal shock tests, the surface damage of the TGV was observed visually, and the micro damage mechanism was analyzed using the scanning electronic microscopy. Micro X-ray computed tomography was adopted to characterize the internal damages in the SiC/SiC guide vanes. The delamination occurred at the positions approaching internal hollow, due to the weak binding force along the thickness direction and the high thermal shock stress caused by the temperature change. The diameter, area, volume, and sphericity distributions of the pores inside of the guide vanes were also obtained.     

Effects of fabrication processes on the properties of SiC/SiC composites

Precursor infiltration and pyrolysis (PIP) and chemical vapor infiltration (CVI) were used to fabricate SiC/SiC composites on a four-step 3D SiC fibre preform deposited with a pyrolytic carbon interface. The effects of fabrication processes on the microstructure and mechanical properties of the SiC/SiC composites were studied. Results showed the presence of irregular cracks in the matrix of the SiC/SiC composites prepared through PIP, and the crystal structure was amorphous. The room temperature flexural strength and modulus were 873.62 MPa and 98.16 GPa, respectively. The matrix of the SiC/SiC composites prepared through CVI was tightly bonded without cracks, the crystal structure had high crystallinity, and the room temperature bending strength and modulus were 790.79 MPa and 150.32 GPa, respectively. After heat treatment at 1300 °C for 50 h, the flexural strength and modulus retention rate of the SiC/SiC composites prepared through PIP were 50.01% and 61.87%, and those of the composites prepared through CVI were 99.24% and 96.18%, respectively. The mechanism of the evolution of the mechanical properties after heat treatment was examined, and the analysis revealed that it was caused by the different fabrication processes of the SiC matrix. After heat treatment, the SiC crystallites prepared through PIP greatly increased, and the SiOxCy in the matrix decomposed to produce volatile gases SiO and/or CO, ultimately leading to an increase in the number of cracks and porosity in the material and a decrease in the material load-bearing capacity. However, the size of the SiC crystallites prepared through CVI hardly changed, the SiC matrix was tightly bonded without cracks, and the load-bearing capacity only slightly changed.     

Torsion and flexural-torsional coupled mechanical properties of different C/SiC torque tubes at room and elevated temperatures

In this paper, the torsion and flexural-torsional coupled mechanical properties of different C/SiC torque tubes were investigated for the testing condition at room and elevated temperatures. Effects of fiber types, fiber preforms, and small hole during fabrication process on torsion mechanical properties were investigated. Flexural-torsional coupled mechanical tests for C/SiC torque tubes with different external diameter and wall thickness were conducted at room and elevated temperatures. The torsion and flexural moments and corresponding shear and flexural strength were obtained. The fracture surface and cracks propagation path were observed and analyzed. The torque and shear strength in T300™-3k torque tube were much higher than those of T300™-1k torque tube. Among 3D needled (3DN), 2D plain-woven [0°/90°] and [±45°] C/SiC torque tubes, the density, torque, and shear strength of 3DN-C/SiC torque tube were the highest. For the C/SiC torque tubes with small hole, the small hole not only increased the densification and uniformity (axial and radial) of the torque tube, but also has the potential to make the damage cracks more zigzag, which improved the fracture toughness of the torque tubes.     

The effects of preparation temperature on the SiCf/SiC 3D4d woven composite

Continuous silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites have promising applications in aero-engine due to their unique advantages, such as low density, high modulus and strength, outstanding high temperature resistance and oxidation resistance. As SiC fibers are main reinforcements in SiC_f/SiC composites, the crystallization rate and initial damage degree of SiC fibers are seriously influenced by preparation temperatures of SiC_f/SiC composites, namely mechanical properties of SiC fibers and SiC_f/SiC composites are influenced by preparation temperatures. In this paper, KD-II SiC fibers were woven into 3D4d preforms and SiC matrix was fabricated by PIP process at 1100 °C, 1200 °C, 1400 °C and 1600 °C. Digital image correlation (DIC) method was adopted to measure the uniaxial tensile properties of these SiC_f/SiC composites. In addition, finite element method (FEM) based on representative volume element (RVE) was adopted to predict the mechanical properties of SiC_f/SiC composites. The good agreements between numerical results and experimental results of uniaxial tensile tests verified the validity of the RVE. In last, the transverse tensile, transverse shear, uniaxial shear properties were predicted by this method. The predicted results illustrated that axial tensile, transverse tensile and axial shear properties were greatly influenced by the preparation temperatures of SiC_f/SiC composites while transverse shear properties were not significantly various. And the mechanical properties of SiC_f/SiC composites peaked at 1200 °C among these four temperatures while their values reached their lowest points at 1600 °C because of thermal damage and brittle failure of SiC_f/SiC composites.     

Study of dynamic compressive behaviors of 2D C/SiC composites at elevated temperatures based on in-situ observation

Dynamic and quasi-static compressive behaviors of 2D C/SiC composites were examined from room temperature to 1600 °C based on in-situ observation, under the environment of air and argon. Tests were conducted respectively on a high temperature universal test machine and an improved high temperature split Hopkinson pressure bar. The improvement of the interface strength and the nucleation of multiple cracks influence the compressive strength under dynamic conditions. As the influence of thermal residual stress, the failure angles and compressive strength of the specimen increased with the increase of temperature in the argon environment. Owing to the competition between oxidation and thermal residual stress, the compressive strength of the specimen increased slightly with increasing temperature, and then dropped sharply for temperature above 700 °C in air. The strain rate sensitivity factor of 2D C/SiC composites increased significantly as the temperature increased in the air environment, but decreased in the argon environment.     

Measuring the effects of heat treatment on SiC/SiC ceramic matrix composites using Raman spectroscopy

The evolution of residual stresses found within a silicon carbide/silicon carbide (SiC/SiC) ceramic matrix composite through thermal treatments was investigated using Raman microspectroscopy. Constituent stress states were measured before, during, and after exposures ranging from 900 to 1300°C for varying times between 1 and 60 minutes. Silicon carbide particles in the as-received condition exhibited average hydrostatic tensile stresses of approximately 300 MPa when measured at room temperature before and after heat treatment. The room temperature Raman profile of the silicon matrix was altered in both shape and location with heat treatment cycles due to increasing activation of boron within the silicon lattice as heat treatment temperatures increased. By accounting for boron activation in the silicon–boron system, little to no permanent change of any constituent stresses were observed, and the silicon matrix subsequently exhibited a complimentary average hydrostatic compressive stress of approximately 300 MPa at room temperature, measured before and after heat treatment. This result builds upon previous literature and offers increased insight into boron activation phenomena measured through Raman spectroscopy methods.     

Dynamic oxidation resistance and residual mechanical strength of ZrB2-CrSi2-SiC-Si/SiC coated C/C composites

To improve oxidation resistance of carbon/carbon (C/C) composites, a multiphase double-layer ZrB₂-CrSi₂-SiC-Si/SiC coating was prepared on the surface of C/C composites by pack cementation. Thermogravimetry analysis showed that the as-prepared coating could provide effective oxidative protection for C/C composites from room temperature to 1490 °C. After thermal cycling between 1500 °C and room temperature, the fracture behaviors of the as-prepared specimens changed and their residual flexural strengths decreased as thermal cycles increased. The specimen after 20 thermal cycles presented pseudo-plastic fracture characteristics and relatively high residual flexural strength (83.1%), while the specimen after 30 thermal cycles failed catastrophically without fiber pullout due to the severe oxidation damage of C/C substrate especially the brittleness of the reinforcement fibers.     

Elevated Temperature Strength Enhancement of ZrB2–30 vol% SiC Ceramics by Postsintering Thermal Annealing

The mechanical properties of dense, hot‐pressed ZrB₂–30 vol% SiC ceramics were characterized from room temperature up to 1600°C in air. Specimens were tested as hot‐pressed or after hot‐pressing followed by heat treatment at 1400°C, 1500°C, 1600°C, or 1800°C for 10 h. Annealing at 1400°C resulted in the largest increases in flexure strengths at the highest test temperatures, with strengths of 470 MPa at 1400°C, 385 MPa at 1500°C, and 425 MPa at 1600°C, corresponding to increases of 7%, 8%, and 12% compared to as hot‐pressed ZrB₂–SiC tested at the same temperatures. Thermal treatment at 1500°C resulted in the largest increase in elastic modulus, with values of 270 GPa at 1400°C, 240 GPa at 1500°C, and 120 GPa at 1600°C, which were increases of 6%, 12%, and 18% compared to as hot‐pressed ZrB₂–SiC. Neither ZrB₂ grain size nor SiC cluster size changed for these heat‐treatment temperatures. Microstructural analysis suggested additional phases may have formed during heat treatment and/or dislocation density may have changed. This study demonstrated that thermal annealing may be a useful method for improving the elevated temperature mechanical properties of ZrB₂‐based ceramics.     

Spherical indentations on hafnium carbide- and silicon-carbide-coated carbon–carbon composites after thermal shock test in air

In this study, high-temperature oxidations and indentations on silicon carbide (SiC)- and hafnium carbide (HfC)-coated carbon–carbon (C/C) composites were investigated to prevent the oxidation of C/C composites in air. The SiC and HfC layers were coated to protect the composite from oxidizing in air at a high temperature. High-temperature oxidation tests were performed at 500 °C, 1,000 °C, 1,350 °C, and 1,500 °C for 1 h in air and then cooled to room temperature by thermal shock. This cycle was repeated until the coating layer was damaged. As a result of measuring the weight change according to the thermal cycle and observing the fiber damage in the C/C composites, the oxidation resistance of HfC was evaluated to be superior to that of SiC. The change of the mechanical behavior was investigated using an indentation test with a tungsten carbide ball with a radius of either 3.18 or 7.93 mm before and after the high-temperature oxidation test by thermal shock. The relative elastic modulus was predicted based on the slope of the indentation load–displacement curve during loading or that of the curve during unloading. The relative hardness was also analyzed based on residual displacement after indentation. The hardness and elastic modulus of the HfC and SiC coating were higher than those of C/C composites and the mechanical properties of the HfC-coated C/C composite were relatively good compared with those of the SiC-coated composites prior to the thermal shock test. In particular, in this study, it was found that the mechanical behaviors of HfC-coated C/C composites exposed to temperatures >1,000 °C in air were transferred from elastic to quasi-plastic. The quasi-plasticity of the HfC coating layer was evaluated to be excellent regarding its resistance to mechanical damage as the coating layer was not easily delaminated or damaged even by oxidation.     

Fabrication of biomorphic SiC composites using wood preforms with different structures

Biomorphic SiC composites were fabricated from wood, including high-density compressed cedar, high-density fiberboard (HDF) and low-density paulownia followed by the fabrication of a preform and liquid silicon infiltration (LSI) process. The degree of molten silicon infiltration was strongly dependent on the cell wall thickness and pore size of the carbon preform. The mechanical properties of the biomorphic SiC composites were characterized by compressive tests at room temperature, 1000 °C and 1200 °C, and the relationship between the mechanical properties and the microstructural characteristics was analyzed. The compressive strength of the biomorphic composites was found to be strongly dependent on their bulk density and decreased as the test temperature increased to 1200 °C. Strength reduction in the biomorphic SiC composites occurred due to the deformation of the remaining Si at elevated temperatures under ambient atmospheric conditions.     

The effect of heat treatment on tensile properties of 2D C/SiC composites

Two-dimensional (2D) carbon fiber reinforced silicon carbide (C/SiC) composites with different initial strength were prepared by chemical vapor infiltration (CVI). After tensile property testing, results exhibited that as the heat-treatment temperature (HTT) increases to 1900°C, the tensile strength and toughness of the low strength specimen (LSS) increased by 110% and 530%, while the high strength specimen (HSS) increased by 5.4% and 550%, respectively. As observed from morphologies, the heat treatment increases the graphitization of the amorphous PyC interphase, which leads to the weakening of interfacial bonding strength (IBS). Meanwhile, the defects arising from heat treatment cause thermal residual stress relaxation. Therefore, the tensile strength and toughness of LSS with relatively high initial IBS increase significantly as HTT increases. For HSS with moderate initial IBS, the heat treatment slightly improves the tensile strength, but significantly improves the toughness. Consequently, the post-heat-treatment tensile properties of 2D C/SiC composites can be regulated by varying HTTs and different initial strength.     

Tensile creep properties and damage mechanisms of 2D-SiCf/SiC composites reinforced with low-oxygen high-carbon type SiC fiber

Tensile creep properties of 2D-SiC_f/SiC composites reinforced with low-oxygen high-carbon type SiC fibers were studied in vacuum at 1300°C∼1430°C. The fracture morphology was observed by scanning electron microscopy and the damage of fiber in 2D-SiC_f/SiC composites was characterized by nanoindentation. Moreover, the microstructure of the composite was investigated by high-resolution transmission electron microscopy. The results show that rupture time is much shortened and steady-state creep rate increase three orders of magnitude when creep temperature is higher than 1400°C. There are two different creep damage mechanisms due to the decrease of interfacial bonding strength at high temperature. The amorphous SiO_xC_y phase in the fibers can crystallize into SiC and C and the SiC grain grows in the fiber. The microstructural changes lead to the decrease of fiber strength and degrade the creep properties of the composite above 1400°C.