Effect of Al addition on the single and cyclic ablation properties of C/C–SiC composites

This article focuses on the damage behavior and mechanism of aluminum addition on reactive melt infiltrated C/C–SiC composites in single and cyclic ablation environments. Plasma ablation tests were performed on C/C–SiC composites containing 20 wt % and 40 wt % aluminum respectively. Coupled with TMA, XRD, SEM and EDS, the results showed that composites with 40 wt % Al had better ablation resistance during the cyclic ablation, while the composites with 20 wt % Al had excellent ablation damage resistance during a single ablation. This difference was due to higher number of microcracks formed inside the composites containing 40 wt % Al than 20 wt % Al, the lower specimen surface temperature during ablation, and the thermal stresses can be released by pore crack expansion during gas reciprocal loading. While in the single continuous loading of gas, the 20 wt % Al composite formed a protective oxide layer with smaller pores and fewer gas and oxygen entry channels, resulting in good resistance to ablation.     

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.     

Steam oxidation of ytterbium disilicate environmental barrier coatings with and without a silicon bond coat

The current generation of multilayer Si/Yb₂Si₂O₇ environmental barrier coatings (EBCs) are temperature limited by the melting point of Si, 1414°C. To investigate higher temperature EBCs, the cyclic steam oxidation of EBCs comprised of a single layer of ytterbium disilicate (YbDS) was compared to multilayered Si/YbDS EBCs, both deposited on SiC substrates using atmospheric plasma spray. After 500 1-h cycles at 1300°C in 90 vol%H₂O-10 vol%air with a gas velocity of 1.5 cm/s, both multilayer Si/YbDS and single layer YbDS grew thinner silica scales than bare SiC, with the single layer YbDS forming the thinnest scale. Both coatings remained fully adherent and showed no signs of delamination. Silica scales formed on the single layer coating were significantly more homogeneous and possessed a markedly lower degree of cracking compared to the multilayered EBC. The single layer EBC also was exposed at 1425°C in steam with a gas velocity of 14 cm/s in an alumina reaction tube. The EBC reduced specimen mass loss compared to bare SiC but formed an extensive 2nd phase aluminosilicate reaction product. A similar reaction product was observed to form on some regions of the bare SiC specimen and appeared to partially inhibit silica volatilization. The 1425°C steam exposures were repeated with a SiC reaction tube and no 2nd phase reaction product was observed to form on the single layer EBC or bare SiC.     

Study on interfacial debonding stress and damage mechanisms of C/SiC composites using acoustic emission

Among ceramic matrix composites (CMCs), carbon fiber-reinforced silicon carbide matrix (C/SiC) composites are widely used in numerous high-temperature structural applications because of their superior properties. The fiber–matrix (FM) interface is a decisive constituent to ensure material integrity and efficient crack deflection. Therefore, there is a critical need to study the mechanical properties of the FM interface in applications of C/SiC composites. In this study, tensile tests were conducted to evaluate the interfacial debonding stress on unidirectional C/SiC composites with fibers oriented perpendicularly to the loading direction in order to perfectly open the interfaces. The characteristics of the material damage behaviors in the tensile tests were successfully detected and distinguished using the acoustic emission (AE) technique. The relationships between the damage behaviors and features of AE signals were investigated. The results showed that there were obviously three damage stages, including the initiation and growth of cracks, FM interfacial debonding, and large-scale development and bridging of cracks, which finally resulted in material failure in the transverse tensile tests of unidirectional C/SiC composites. The frequency components distributed around 92.5 kHz were dominated by matrix damage and failure, and the high-frequency components distributed around 175.5 kHz were dominated by FM interfacial debonding. Based on the stress and strain versus time curves, the average interfacial debonding stress of the unidirectional C/SiC composites was approximately 1.91 MPa. Furthermore, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDXS) were used to observe the morphologies and analyze the chemical compositions of the fractured surfaces. The results confirmed that the fiber was completely debonded from a matrix on the fractured surface. The damage behaviors of the C/SiC composites were mainly the syntheses of matrix cracking, fiber breakage, and FM interfacial debonding.     

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.     

Evaluation of elastic constants and high temperature tensile behaviour with damage assessment of the SiC seal-coated 2.5D Cf/SiC composites having multilayered interphase and Si-B-C added matrix

Elastic constants and tensile behaviour of chemical vapour infiltration processed 2.5D C_f/SiC composites possessing multilayered (PyC/SiC)_n=4 interphase, Si-B-C containing matrix and SiC seal-coating have been evaluated with microstructural examination and damage assessment. The strength obtained as ～187 ± 2 MPa in tensile tests at 27 °C is increased by ～18% and ～22% at 1000 °C and 1250 °C, respectively due to reduced thermal stress and increased strength of load-sharing C-fibres, which are protected from oxidation till failure by a self-healing borosilicate layer. The damage evolving during tension tests has been quantified by relating it to decrease of stress-strain slope with strain. Higher (6–8 times) elastic constants measured along fibre-axes than that obtained transversely, indicate significant anisotropy. Owing to matrix cracking with fibre-debonding and pull-out, the fibre-oriented elastic constants of tensile-fractured samples are significantly lower than those of as-received composites, and the difference scales with temperature, whereas negligible change is observed perpendicular to the fibre axes.     

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.     

Fracture behavior of a melt-infiltration-processed SiC/Si composite at 900 °C in argon,air, and steam

The fracture behavior of a melt-infiltration-processed SiC/Si composite, used to mimic the matrices of industrial fiber-reinforced ceramic composites, was examined in different atmospheres and temperatures. Specimens tested in four-point bending at 900 °C in oxygen-gettered argon, dry air, or steam-rich atmospheres exhibited higher average fracture strengths than specimens tested at 25 °C. Higher mean fracture strength values were obtained for specimens tested in dry air or in a steam-rich atmosphere at 900 °C than for specimens tested in high-purity, oxygen-gettered argon at this temperature. The increased fracture strengths obtained in air and in steam-rich atmospheres coincided with increased specimen oxidation and apparent oxide filling and blunting of flaws in these composites. A transition in the location of catastrophic failure, from sites of preexisting damage created by Vickers indentations for tests in argon to other locations for tests in air or steam-rich atmospheres, was also consistent with such apparent oxide filling/blunting of indentation-induced flaws.     

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.     

Oxidation resistance of SiC nanowires reinforced SiC coating prepared by a CVD process on SiC‐coated C/C composites

Oxidation protective SiC nanowires‐reinforced SiC (SiCNWs‐SiC) coating was prepared on pack cementation (PC) SiC‐coated carbon/carbon (C/C) composites by a simple chemical vapor deposition (CVD) process. This double‐layer SiCNWs‐SiC/PC SiC‐coating system on C/C composites not only has the advantages of SiC buffer layer but also has the toughening effects of SiCNWs. The microstructure and phase composition of the nanowires and the coatings were examined by SEM, TEM, and XRD. The single‐crystalline β‐SiC nanowires with twins and stacking faults were deposited uniformly and oriented randomly with diameter of 50‐200 nm and length ranging from several to tens micrometers. The dense SiCNWs‐SiC coating with some closed pores was obtained by SiC nanocrystals stacked tightly with each other on the surface of SiCNWs. After introducing SiCNWs in the coating system, the oxidation resistance is effectively improved. The oxidation test results showed that the weight loss of the SiCNWs‐SiC/PC SiC‐coated samples was 4.91% and 1.61% after oxidation at 1073 K for 8 hours and at 1473 K for 276 hours, respectively. No matter oxidation at which temperature, the SiCNWs‐SiC/PC SiC‐coating system has better anti‐oxidation property than the single‐layer PC SiC coating or the double‐layer CVD SiC/PC SiC coating without SiCNWs.     

Processing and impact behavior of Al/SiCp composites fabricated by the pressureless melt infiltration method

In the current investigation, pressureless melt infiltration was applied to fabricate the Al/SiC composites based on the SiC porous preforms. The process was conducted by introducing the aluminum melt into the SiC preforms at 950 °C under the nitrogen atmosphere, without the aid of pressure. To explore development of melt infiltration, initial preforms were produced with variable SiC fractions (40, 50, and 60 vol.%) using three different SiC powders with the mean particle size of 20, 50, and 90 μm. While the infiltration of aluminum melt into the preforms with 40 vol.% initial SiC volume fraction (SiC particle size of 90 μm) resulted to the composites with final density of 0.94 theoretical density (TD), this value drops down to ～0.9 TD for the composites produced by preforms with the SiC (90 μm) volume fraction of 60 vol.%. On the other hand, composites fabricated by 50 μm SiC powder (SiC volume fraction of 40 vol.%) demonstrated the final density of ～0.91 TD. The impact resistance tests performed on the composites demonstrated an enhancement in the value of impact energy with an increase of SiC powder particle size. Results, additionally, revealed a significant superiority of impact energy for the composites fabricated by a combined melt infiltration and sintering (MIS) procedure compared to those produced by infiltration at 950 and 1350 °C.     

Ablation behavior of thin-blade co-deposited C/Cx-SiCy composites under the influence of the complex fluid conditions of the oxyacetylene torch

This paper offers a new way of testing the ablation property of material under an oxyacetylene torch using a thin-blade specimen, which costs much less time to reach the maximum temperature and provides a harsh turbulence fluid field that's closer to reality. The thin-blade specimen experiences a higher turbulent intensity than the traditional disk-like specimen, leading to more efficient heat exchange. The fluid field simulation agrees with the testing results. In addition, we manage to synthesize the C/Cx-SiCy composites with the co-deposition chemical vapor infiltration (CVI) method. The C/Cx-SiCy composites exhibit a similar anti-ablation property as C/C composites and consist of enough SiC phase simultaneously, combining the advantages of both C/C composites and C/SiC composites. The thin-blade C/Cx-SiCy composites show a lower linear ablation rate (1.6 μm/s) than C/C composites (4.1 μm/s) and C/SiC composites (19.6 μm/s) during the oxyacetylene test. The glass layer formed on the surface of C/Cx-SiCy could cling to the bulk material instead of peeling off due to the high PyC content in the matrix could protect the SiO₂ from blowing away.     

Fabrication of 2D C/C-SiC composites using PIP based hybrid process and investigation of mechanical properties degradation under cyclic heating

2D C/C-SiC composites were fabricated using PIP process by repeated impregnations of porous C/C composite preforms with polycarbosilane followed by pyrolysis. Effect of cyclic heating on flexural and shear strength of these composites was studied by exposing the test specimens to oxyacetylene flame for 20 s and cooling by a blast of air. The cyclic heating tests were repeated up to five times. Average flexural and shear strength of the as fabricated composites were about 330 MPa and 14.5 MPa respectively. After five heating and cooling cycles, average flexural and shear strength were reduced to 120 MPa and 5.5 MPa respectively. SEM, XRD, EDAX and XPS studies were also carried out to investigate the causes of strength reduction. Oxidation started preferentially at carbon matrix through the cut ends of the weft fibers. Oxidative damage due to repeatedly heating cooling was found to be much smaller in through-thickness direction due to passive oxidation of SiC matrix while severe damage was observed parallel to the fabric layers.     

Oxidation and ablation behaviours of a SiCnw@SiC–Si coating fabricated for carbon-fibre-reinforced carbon-matrix composites via thermal evaporation and gaseous silicon infiltration

A SiC-nanowire-modified SiC–Si (SiC_nw@SiC–Si) coating was prepared for carbon-fibre-reinforced carbon-matrix (C/C) composites using a two-step method based on thermal evaporation and gaseous silicon infiltration, and the effects of SiC nanowires on the oxidation and ablation behaviours of the coated samples were studied. Oxidation tests conducted at 1500 °C revealed that the weight loss of the SiC–Si-coated C/C composite was 15.85% after 6 h, whereas the SiC_nw@SiC–Si-coated C/C composite experienced a significantly lower weight loss of 1.27% after 50 h. Ablation tests suggested that the mass and linear ablation rates of the SiC_nw@SiC–Si-coated C/C composite were 0.05 mg/s and 0.09 μm/s, respectively; they were reduced by 78.26 and 92.74%, respectively, compared with those of the SiC–Si-coated C/C composite. Careful characterisation suggested that the network structure of the SiC nanowires in the SiC–Si phase can suppress crack propagation and firmly attach to the coating surface to enhance the interfacial adhesion between the coating and substrate, leading to improved anti-oxidation and anti-ablation properties. The SiC_nw@SiC–Si coating could offer a technological foundation for preventing the oxidation and ablation of C/C composites in aerospace engineering.     

Joining of C/SiC composites by spark plasma sintering technique

CVD–SiC coated C/SiC composites (C/SiC) were joined by spark plasma sintering (SPS) by direct bonding with and without the aid of joining materials. A calcia-alumina based glass–ceramic (CA), a SiC + 5 wt% B₄C mixture and pure Ti foils were used as joining materials in the non-direct bonding processes. Morphological and compositional analyses were performed on each joined sample. The shear strength of joined C/SiC was measured by a single lap test and found comparable to that of C/SiC.     

Tension–tension fatigue behavior and residual strength evolution of SiC/(PyC/SiC)2/SiC minicomposites prepared by CVI+MI and CVI+PIP processes

The residual tensile strength (RTS) evolution of SiC/(PyC/SiC)₂/SiC samples, prepared by chemical vapor impregnation (CVI) combined with either melting reaction sintering (MI) or polymer impregnation and pyrolysis (PIP), was investigated after 10⁶ cycles as the pre-fatigue stress increased. The fatigue limits of the two tested specimen types, CVI + MI and CVI + PIP, were 760 and 660 MPa, respectively, corresponding to 95% and 75% of the tensile strength, respectively. Although the RTS of the two specimen types first increased and then decreased, it was interesting that after pre-fatigue, the maximum RTS of the CVI + PIP-prepared sample at 680 MPa, was 16 MPa higher than that of the CVI + MI-prepared sample at 590 MPa. The nanoindentation results indicate that the matrix prepared by CVI could protect the fiber from heavy damage in subsequent preparation, and the matrix modulus and hardness were higher in samples prepared by PIP than those prepared by MI. According to the microstructure observations and hysteresis characteristics, it was concluded that the differences mainly came from the internal stress state, matrix, and fiber properties.     

Effect of co-deposited SiC nanowires and carbon nanotubes on oxidation resistance for SiC-coated C/C composites

To protect carbon/carbon composites (C/Cs) against oxidation, SiC coating toughened by SiC nanowires (SiCNWs) and carbon nanotubes (CNTs) hybrid nano-reinforcements was prepared on C/Cs by a two-step technique involving electrophoretic co-deposition and reactive melt infiltration. Co-deposited SiCNWs and CNTs with different shapes including straight-line, fusiform, curved and bamboo dispersed uniformly on the surface of C/Cs forming three-dimensional networks, which efficiently refined the SiC grains and meanwhile suppressed the cracking deflection of the coating during the fabrication process. The presence of SiCNWs and CNTs contributed to the formation of continuous glass layer during oxidation, while toughed the coating by introducing toughing methods such as bridging effect, crack deflection and nanowire pull out. Results showed that after oxidation for 45 h at 1773 K, the weight loss percentage of SiC coated specimen was 1.35%, while the weight gain percentage of the SiCNWs/CNTs reinforced SiC coating was 0.03052% due to the formation of continuous glass layer. After being exposed for 100 h, the weight loss percentage of the SiCNWs/CNTs reinforced SiC coating was 1.08%, which is relatively low.     

Electrical and Thermal Properties of SiC Ceramics Sintered with Yttria and Nitrides

The electrical and thermal properties of SiC ceramics containing 1 vol% nitrides (BN, AlN or TiN) were investigated with 2 vol% Y₂O₃ addition as a sintering additive. The AlN‐added SiC specimen exhibited an electrical resistivity (3.8 × 10¹ Ω·cm) that is larger by a factor of ~10² compared to that (1.3 × 10^?1 Ω·cm) of a baseline specimen sintered with Y₂O₃ only. On the other hand, BN‐ or TiN‐added SiC specimens exhibited resistivity that is lower than that of the baseline specimen by a factor of 10^?1. The addition of 1 vol% BN or AlN led to a decrease in the thermal conductivity of SiC from 178 W/m·K (baseline) to 99 W/m·K or 133 W/m·K, respectively. The electrical resistivity and thermal conductivity of the TiN‐added SiC specimen were 1.6 × 10^?2 Ω·cm and 211 W/m·K at room temperature, respectively. The present results suggest that the electrical and thermal properties of SiC ceramics are controllable by adding a small amount of nitrides.     

Preparing the SiC coated C/C composites with excellent mechanical and antioxidative properties using a buffer layer

The preparation of SiC coating on C/C composites via a pack cementation method would cause serious mechanical damage to C/C substrate due to the siliconization corrosion by molten silicon during the ultra-high-temperature preparation process (2173–2373 K). In order to prepare SiC coated C/C composites with excellent mechanical and antioxidative properties, we applied a buffer layer on the surface of C/C to inhibit siliconization corrosion and densify coating. Results showed that the siliconized area ratio of the C/C substrate was decreased from 60.9% to 24.8%, and its bending strength was increased from 36.9 MPa to 60.6 MPa. Moreover, the mass loss of the modified SiC coated C/C sample has reduced by ~4.14 times after oxidation for 144 h in air at 1773 K and decreased from 2.44% to ? 0.15% after suffering 50 thermal cycles between room temperature and 1773 K.     

Comparison of hydrothermal corrosion behavior of SiC with Al2O3 and Al2O3 + Y2O3 sintering additives

Fully dense SiC bulks with Al₂O₃ and Al₂O₃ + Y₂O₃ sintering additives were prepared by spark plasma sintering and the effect of sintering additives on the hydrothermal corrosion behavior of SiC bulks was investigated in the static autoclave at 400°C/10.3 MPa. The SiC specimen with Al₂O₃ sintering additive exhibited a higher weight loss and followed a linear law. However, the SiC specimen with Al₂O₃ + Y₂O₃ additive exhibited a lower weight loss and followed a parabolic law, indicating that the corrosion kinetic and mechanism were different for these two SiC bulks. Further examination revealed that, a deposited layer was formed on the surface of SiC specimen with Al₂O₃ + Y₂O₃ sintering additive after corrosion, which can effectively protect the SiC specimen from further corrosion, and thereby improved the corrosion resistance of the SiC specimen with Al₂O₃ + Y₂O₃ sintering additive.