Experimental evaluation and theoretical prediction of elastic properties and failure of C/C-SiC composite

The paper presents experimental characterization and theoretical predictions of elastic and failure properties of continuous carbon fiber reinforced silicon carbide (C/C-SiC) composite fabricated by Liquid Silicon Infiltration (LSI). Its mechanical properties were determined under uniaxial tensile, compression, and pure shear loads in two sets of principal coordinate systems, 0°–90° and ±45°, respectively. The properties measured in the 0°–90° coordinate system were employed as the input data to predict their counterparts in the ±45° coordinate system. Through coordinate transformations of stress and strain tensors, the elastic constants and stress-strain behaviors were predicted and found to be in good agreement with the experimental results. In the same way, three different failure criteria, maximum stress, Tsai-Wu, and maximum strain, have been selected for the evaluation of the failure of C/C-SiC as a type of genuinely orthotropic material. Based on the comparisons with experimental results, supported by necessary practical justifications, the Tsai-Wu criterion was found to offer a reasonable prediction of the strengths, which can be assisted by the maximum stress criterion to obtain an indicative prediction of the respective failure modes.     

Effect of carbon nanotubes on the strength of adhesive lap joints of C/C and C/C-SiC ceramic fibre composites

Similar substrates of carbon/carbon (C/C) and carbon/carbon-silicon carbide (C/CSiC) composites were bonded with pure epoxy resin and the one containing 3% multiwall carbon nanotubes (MWCNTs). The results show that MWCNT/filled epoxy resin bonded C/CC/C and C/CSiCC/CSiC substrates have a higher adhesive joint strength than those bonded with epoxy resin alone. MWCNTs increase the toughness and strength of the epoxy resin, which increases the interface bond strength between two similar matching surfaces.     

Effect of high-temperature heat treatment on the microstructure and mechanical behavior of PIP-based C/C-SiC composites with SiC filler

C/C-SiC composites were fabricated by a combined process of chemical vapor deposition (CVD), slurry infiltration(SI), and precursor infiltration and pyrolysis (PIP). The microstructure and mechanical behavior were investigated for the dense C/C-SiC composites before and after high-temperature heat treatment. The results indicated that the sintering of the SiC matrix and the migration of the SiC matrix/fiber bundles weak interface occurred after high-temperature heat treatment at 1900 ℃. The SiC sintering resulted in an increase in the flexural strength of the C/C-SiC composites from 298.9 ± 35.0 MPa to 411.1 ± 57.3 MPa. The migration of the weak interface changed the direction of crack propagation, making the fracture toughness of the C/C-SiC composites decrease from 13.3 ± 1.7 MPa⋅m ^1/2 to 9.02 ± 1.5 MPa⋅m ^1/2.     

Evaluation of the moulding process for production of short-fibre-reinforced C/C-SiC composites

For the production of C/C-SiC brake discs via the liquid silicon infiltration method (LSI), the hot pressing process is the state of art technique for the moulding of the CFRP composites. This technique consists of several manual steps which increase production cost. The overall cost can be reduced by implementing injection moulding process.In this paper the influence of the moulding process (hot pressing, injection moulding) on the properties of semi-finished and final products during the production of short-fibre-reinforced C/C-SiC composites by means of the LSI process are examined. The starting polymer is chemically characterised. Carbon-fibre-reinforced plastic (CFRP) composites are fabricated by hot pressing, as well as injection moulding process. The CFRP composites are converted into porous C/C composites by pyrolysis. Liquid silicon is infiltrated to form dense C/C-SiC composites, which are further investigated during the course of this paper. Significant differences in properties of the composites are discussed.     

Microstructure and ablation properties of La2O3 modified C/C-SiC composites prepared via precursor infiltration pyrolysis

Effects of La₂O₃ modification on the microstructure, mechanical and ablation properties of C/C-SiC composites were investigated. Experimental results show that a new La₁₀(SiO₄)₆O₃ phase was generated during heat treatment process. The presence of the La-compounds, namely La₂O₃ and La₁₀(SiO₄)₆O₃, had an important impact on the structure of reinforced skeleton and the molten oxide film, and thus strongly affected the mechanical and ablation properties of the composites. Excessive La addition induced the structural damage of the reinforced skeleton, resulting in weakened mechanical and ablation properties. The C/C-SiC composites with 25.65 wt.% La₂O₃ addition displayed better mechanical properties and the best ablation resistance. The La₁₀(SiO₄)₆O₃ phase could react with molten silica to form a viscous glass during ablation. The transformation of La-compounds into La₂Si₂O₇ can reduce the ablation of SiO₂ and enhance the glass film, so as to protect the composites from further ablation.     

Key technologies for laser-assisted precision grinding of 3D C/C-SiC composites

Due to their exceptional and distinctive qualities, 3D C/C-SiC composites are widely utilized in producing high-end equipment and the aerospace national defense industries. However, the hard and pseudo plastic nature of the material and its anisotropies make it challenging to process. To improve the processing quality of 3D C/C-SiC composites, laser-assisted precision grinding technology is introduced in this paper, which innovatively controls the depth of the thermally induced damage layer by adjusting the laser process parameters to reduce the hard brittleness of the material, and then the surface is created by precision grinding with a grinding wheel on this basis. Experiments on laser-induced damage, laser-assisted grinding, and diamond scratching were carried out to investigate the effect of laser parameters on material damage and the effect of laser-assisted grinding processes, with an emphasis on revealing the mechanism of material removal. The results show that laser irradiation causes complex reactions such as sublimation, decomposition, and oxidation of 3D C/C-SiC composites, resulting in SiO2 and Si and recondensed SiC, causing surface/subsurface damage. A maximum reduction in normal grinding force, tangential grinding force, specific grinding energy, and surface roughness of 35.6%, 43.6%, 43.58%, and 24.22%, respectively, compared to conventional grinding processes with laser-assisted grinding. After laser irradiation, the degree of brittle fracture in the precision grinding of workpieces is significantly reduced due to the degradation of matrix and fiber damage caused by laser irradiation, which reduces the hard and pseudo plastic properties of the material. The removal mechanism shows a trend of ductile domain removal in the grinding of thermally damaged layers, which reduces the grinding force and improves the surface quality.     

Strength evolution of cyclic loaded LSI-based C/C-SiC composites

An experimental investigation was performed to study the influence of fatigue damage introduced by different loading cycles on the residual tensile strength (RTS) of plain-weave reinforced C_f/C-SiC composites (2D C/C-SiC). The specimens were subjected to the fatigue stress of 57 MPa for the preselected numbers of cycles as follows: 10², 10⁴ and 10⁵, respectively, before the static tensile test. The microstructures and fractured surfaces after the tensile test were examined by optical and scanning electron microscopy, respectively. The results showed that the RTS of the specimens after the preselected fatigue cycles numbers of 10², 10⁴ and 10⁵ increase to 89.8, 94.1 and 82.4 MPa, respectively, which are somewhat higher compared to the virgin samples (79.7 MPa). Additionally, we found that the linear part of the tensile stress-strain curve is independent on the fatigue cycles. Finally, the increased fatigue damage in C/C-SiC composites could determine a reduction of elastic modulus in all cases of fatigue tests.     

炭/陶复合材料的抗热震性能研究

对含石墨的炭／陶复合材料优良的抗热震性能进行了讨论。这种性质与石墨的导热系数大、断裂功高、热膨胀和弹性模量小密切相关。     

The effects of high-temperature annealing on microstructure and performance of Cf/C-SiC composites modified by FeSi2

FeSi₂ modified C/C-SiC composites (C/C-SiC-FeSi₂) are fabricated by chemical vapor infiltration (CVI) combined with reactive melt infiltration (RMI) with FeSi75 alloy. The effects of high-temperature annealing (1600?°C, 1650?°C, 1700?°C) on the microstructure and performance of C/C-SiC-FeSi₂ are investigated. With the elevation of annealing temperature, the porosity of the composites and the content of SiC increase due to the evaporation of liquid Si and the further reaction of Si and C. The mechanical performance gradually decreases due to the catalytic graphitization of the carbon fiber, the high porosity and the thermal residual stress (TRS) caused by thermal mismatch of different phases. The coefficient of thermal expansion and thermal diffusivity slightly decrease with increasing annealing temperature for the increase of porosity. However, the friction performance of the heat treated materials at high braking speed are greatly improved attributing to the increase of SiC content and the capturing and storage function of pores on hard particles.     

Shear properties of C/C-SiC sandwich structures

Carbon fiber reinforced carbon-silicon carbide (C/C-SiC) sandwich structures have been developed using the Liquid Silicon Infiltration process and the in situ joining method. They offer high mass-specific stiffness, low thermal expansion, and high environmental stability. Potential application areas are highly precise satellite structures, like optical benches. In this study, sandwich samples were manufactured using prepregs based on 2D carbon fibre fabrics and a phenolic resin precursor. Carbon fibre reinforced polymer preforms for folded and grid-cores, as well as for the skin panels were manufactured using autoclave technique. In the second step, the sandwich components were pyrolyzed, leading to C/C preforms. For the build-up of the sandwich samples, two skin panels were joined to a core structure and subsequently, the resulting C/C sandwich preform was siliconized. C/C-SiC sandwich samples were tested under shear load. Shear strength, modulus, and fracture strain were determined and compared to the results obtained by analytical calculation. The shear properties were dependent on the fiber orientation in the core structure as well as on the core type and orientation. The sandwich shear stiffness obtained in the tests was close to the expected theoretical values, calculated on the basis of the material properties and the core geometry.     

Influence of graphitization temperature on microstructure and mechanical property of C/C-SiC composites with highly textured pyrolytic carbon

C/C-SiC composites with highly textured pyrolytic carbon (HT PyC) were prepared by a combining chemical vapor infiltration and liquid silicon infiltration. The effect of HT PyC graphitization before and after 2327 and 2723 K on C/C-SiC composites was investigated. The mechanical properties decreased with increasing graphitization temperature, but graphitization treatment changed the fracture behavior from brittle like to pseudo-ductile. The decrease in bending strength from 306.21 to 243.69 MPa resulted from the weak interfacial bonding between HT PyC and fiber, and the good orientation of graphite layers. The crack at border of fiber bundle and longitudinal crack in HT PyC shortened the path of crack propagation, resulting in fracture toughness decrease from 21.11 to 14.72 MPa·m^1/2. A more pseudo-ductile behavior was due to the longer pull-out of fibers, the better orientation of graphite layers, the sliding of sublayers, and the deflection and propagation caused by the transverse cracks.     

Preparation,ablation behavior and mechanism of C/C-ZrC-SiC and C/C-SiC composites

ZrC precursor was synthesized by a solution approach using ZrOCl₂·8H₂O, acetylacetonate, glycerol and boron-modified phenolic resin. A ZrC yield of ~ 40.56 wt% was obtained at 1500 °C in the C/Zr molar ratio of 1:1. C/C-ZrC-SiC composites were fabricated by a combined processes of chemical vapor infiltration (CVI) and precursor infiltration and pyrolysis (PIP) using the synthesized ZrC precursor. For comparison, C/C-SiC composites were prepared by CVI. Thermogravimetric analysis showed that C/C-ZrC-SiC composites exhibited better oxidation resistance than C/C-SiC composites. After oxyacetylene torch ablation, the mass ablation rate of C/C-ZrC-SiC composites was 9.23% lower than that of C/C-SiC composites. The porous ZrO₂ skeleton in the ablation center was prone to be peeled off by the flame flow, resulting in the higher linear ablation rate of C/C-ZrC-SiC composites. The oxide layers of ZrO₂ and SiO₂ were formed on the transition and brim region of C/C-ZrC-SiC composites and acted as effective heat and oxygen barriers. For C/C-SiC composites, the C-SiC matrix was severely depleted in the ablation center and the formed SiO₂ layer in the brim region could protect the matrix against further ablation.     

Tribological performance of B4C modified C/C-SiC brake materials under dry air and wet conditions

In this work, boron carbide (B₄C) was selected as additive to improve the tribological performance of C/C-SiC brake materials. It contained four phases (C, B₄C, Si and SiC) in B₄C modified C/C-SiC (C/C-B₄C-SiC) brake materials. Its wear rates were much less than that of C/C-SiC, especially at high braking speeds. The introduction of B₄C particles could reduce the braking temperature. During the braking process, B₄C in the material can be oxidized to B₂O₃. The flow of B₂O₃ could cover the interface of carbon fiber and PyC to prevent them from oxidation and thereby reduce the oxidative wear of the brake materials. Under wet conditions, the braking property of C/C-B₄C-SiC brake materials did not degrade, whereas the braking process was found to be stable.     

Fabrication of C/C-SiC composites using high-char-yield resin

Carbon fiber reinforced ceramic matrix composites (C/C-SiC composites) were fabricated using a type of high-char-yield phenolic resin with the char yield of 81.17 wt.%. Firstly, the fabric prepreg was prepared by spreading the phenolic resin solution onto the two dimensional carbon fiber plain weave fabric and dried consequently. Afterward, the resin was cured and then the carbon fiber reinforced polymer (CFRP) was pyrolyzed to get amorphous carbon. Finally, C/C-SiC composites were obtained through liquid silicon infiltration (LSI) process. SEM micrographs showed that the Si/SiC area was homogeneously dispersed in the matrix, and during the siliconization process, a layer of SiC was formed along the surface of carbon fibers or carbon matrix. The fiber volume of CFRP was about 40 vol.%, which was much lower than other studies. XRD result indicated that only β-SiC type was formed. The result of X-ray computed tomography clearly showed the structure changes before and after the melt infiltration process. Mechanical property test showed that the composites had fracture strength of 186 ± 23 MPa, and a flexural modulus of 106 ± 8 GPa.     

Fatigue behavior and oxidation resistance of carbon/ceramic composites reinforced with continuous carbon fibers

The aim of this work was to compare fatigue behavior and oxidation resistance of pitch-derived CC (carbon) composite with CC/ceramic (carbon/ceramic) composites obtained by impregnation of CC composite with polysiloxane-based preceram and their subsequent heat treatment. Two types of CC/ceramic composites were studied; CC/SiCO composite obtained at 1000 °C, and CC/SiC composite obtained at 1700 °C. Both types of composites show much better fatigue mechanical performance in comparison to pure CC composite. CC/SiCO composite had 3 times better fatigue properties, and CC/SiC composite 4.5 times better fatigue properties than the reference CC composite. After a fatigue test composites partially retain their mechanical properties, and normalized residual modulus in the direction perpendicular to laminates exceeds 50% for CC and CC/SiCO composites. In the other directions normalized residual modulus is higher than 80% for all composites. Oxidative tests led at 600 °C in air atmosphere indicated oxidation resistance of CC/SiC composites.     

Influence of h-BN as additive on microstructure and oxidation mechanism of C/C-SiC composite

Due to the favorable self-healing performance, hexagonal boron nitride (h-BN) as additive in the matrix can significantly influence the oxidation behavior and the kinetic characteristics of C/C-SiC composites. In this work, C/C-SiC composites modified by h-BN (C/C-BN-SiC) were prepared by low-temperature compression molding (LTCM), pyrolysis and liquid silicon infiltration (LSI). Microstructure, oxidation behavior and kinetic characteristics of the C/C-BN-SiC composites were investigated compared with the C/C-SiC composite. Because h-BN is non-wetted by liquid silicon, the h-BN flakes in the matrix can obstruct and prolong the flow path of silicon, and protect the carbon fibers from corrosion to a certain extent. The oxidation kinetics of composites occur in low and high temperature domains, with different oxidation-controlling mechanisms, and the addition of h-BN can hinder the inward diffusion and lead to the decline of carbon recession and apparent activation energy.     

Manufacture and thermomechanical characterization of wet filament wound C/C-SiC composites

The paper presents manufacture of C/C-SiC composite materials by wet filament winding of C fibers with a water-based phenolic resin with subsequent curing via autoclave as well as pyrolysis and liquid silicon infiltration (LSI). Almost dense C/C-SiC composite materials with different winding angles ranging from ±15° to ±75° could be obtained with porosities lower than 3% and densities in the range of 2 g/cm³. Thermomechanical characterization via tensile testing at room temperature and at 1300°C revealed higher tensile strength at elevated temperature than at room temperature. Thus, C/C-SiC material obtained by wet filament winding and LSI-processing has excellent high-temperature strength for high-temperature applications. Crack patterns during pyrolysis, microstructure after siliconization, and tensile strength strongly depend on the fiber/matrix interface strength and winding angle. Moreover, calculation tools for composites, such as classical laminate and inverse laminate theory, can be applied for structural evaluation and prediction of mechanical performance of C/C-SiC structures.     

Microstructure and anti-oxidation properties of multi-composition ceramic coatings for carbon/carbon composites

To protect carbon/carbon (C/C) composites from oxidation at elevated temperature, an effective WSi₂-CrSi₂-Si ceramic coating was deposited on the surface of SiC coated C/C composites by a simple and low-cost slurry method. The microstructures of the double-layer coatings were characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy analyses. The coating exhibited excellent oxidation resistance and thermal shock resistance. It could protect C/C composites from oxidation in air at 1773 K for 300 h with only 0.1 wt.% mass gain and endure the thermal shock for 30 cycles between 1773 K and room temperature. The excellent anti-oxidation ability of the double-layer WSi₂-CrSi₂-Si/SiC coating is mainly attributed to the dense structure of the coating and the formation of stable vitreous composition including SiO₂ and Cr₂O₃ produced during oxidation.     

Size effect of carbon fiber-reinforced silicon carbide composites (C/C-SiC): Part 2 - tensile testing with alignment device

The appropriate assessment of mechanical properties is essential to design ceramic matrix composites. The size effect of strength plays a key role for the material understanding and the transfer from lab-scale samples to components. In order to investigate the size effect for carbon fiber-reinforced silicon carbon (C/C-SiC) under tensile load, a tensile testing with a minimum of deviation from the pure tensile loading is necessary. Hence, a hybrid edge/face-loading test device for self-alignment and centering of C/C-SiC tensile samples was developed, evaluated and proved to ensure pure tensile load. The mechanical analysis of more than 190 samples with two different cross-sections fabricated from the same material population revealed no significant difference in tensile strength. Although the volume under load was increased from 129 to 154 mm³, the tensile strengths of 162 ± 7 and 164 ± 6 MPa did not change. These results are discussed regarding the weakest link and energetic size effect approaches.