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Long-term oxidation performance of SiCf/SiC composites manufactured at 1200 °C in air atmosphere by PIP and hybrid CVI/PIP techniques

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... The detailed EDS analyses of the cauliflower-like particles reveal that they are rich in Si and O, but there is still some C, as shown in Figure 11a-d. According to recent studies [50][51][52], these particles could be the oxides of SiC, possibly a mixture of SiC, SiO2, and SiO phases. SiC acts as the core of small particles, and its outer layer consists of SiO2 and SiO phases. ...
... The EDS analyses of the peeled SiC fiber reveal that it is mainly composed of Si The detailed EDS analyses of the cauliflower-like particles reveal that they are rich in Si and O, but there is still some C, as shown in Figure 11a-d. According to recent studies [50][51][52], these particles could be the oxides of SiC, possibly a mixture of SiC, SiO 2 , and SiO phases. SiC acts as the core of small particles, and its outer layer consists of SiO 2 and SiO phases. ...
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SiCf/SiC ceramic matrix composite (CMC), a hard and brittle material, faces significant challenges in efficient and high-quality processing of small-sized shapes. To address these challenges, the nanosecond laser was used to process micro-holes in the SiCf/SiC CMC using a two-step drilling method, including laser pre-drilling in air and laser final-drilling with a water jet. The results of the single-parameter variation and optimized orthogonal experiments reveal that the optimal parameters for laser pre-drilling in air to process micro-holes are as follows: 1000 processing cycles, 0.7 mJ single-pulse energy, −4 mm defocus, 15 kHz pulse-repetition frequency, and 85% overlap rate. With these settings, a micro-hole with an entrance diameter of 343 μm and a taper angle of 1.19° can be processed in 100 s, demonstrating high processing efficiency. However, the entrance region exhibits spattering slags with oxidation, while the sidewall is covered by the recast layer with a wrinkled morphology and attached oxides. These effects are primarily attributed to the presence of oxygen, which enhances processing efficiency but promotes oxidation. For the laser final-drilling with a water jet, the balanced parameters for micro-hole processing are as follows: 2000 processing cycles, 0.6 mJ single-pulse energy, −4 mm defocus, 10 kHz pulse-repetition frequency, 85% overlap rate, and a 4.03 m/s water jet velocity. Using these parameters, the pre-drilled micro-hole can be finally processed in 96 s, yielding an entrance diameter of 423 μm and a taper angle of 0.36°. Due to the effective elimination of spattering slags and oxides by the water jet, the final micro-hole exhibits a clean sidewall with microgrooves, indicating high-quality micro-hole processing. The sidewall morphology could be ascribed to the different physical properties of SiC fiber and matrix, with steam explosion and cavitation erosion. This two-step laser drilling may provide new insights into the high-quality and efficient processing of SiCf/SiC CMC with small-sized holes.
... This drastic decrease in the flexural strength is attributed the oxidation of the composite. 40 In contrast, all oxide composite Al 2 O 3 fibers and an Al 2 O 3 matrix made by the PIP process led to flexural strengths of approximately 405 and 369 MPa after 0 and 100 h at 1200 • C, respectively, with limited degradation due to the presence of an oxidized matrix. 41 The aim of this work was to develop a GMCs with high temperature resistance (above 1150 • C). ...
... The next fold is simply superposed to the already preparated fold in order to match 0/90 • textile orientation. Once all folds were superposed, the whole composite is consolidated in a heat chamber (1 atm) or a heating textile press (6 MPa) for different times (0.083, 0.3, 2, 6, 24, and 168 h) and different temperatures (20,40,60,80, 120, and 200 • C). The pressure of 6 MPa is performed by a heating textile press which could heat the composites by both its surface plates from 20 to 200 • C. Once consolidated, the weight and thickness of the composite geopolymer were measured. ...
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Geopolymer matrix composites (GMCs) are actively being developed for high‐temperature applications. In this work, we investigated different composite preparation parameters, such as the elaboration conditions (time, temperature and pressure) and composite dimensions (number of folds and surface area). In addition, we studied the effect of alkali cations (NaK or K), on metakaolin based geopolymer matrix composition, and textile type (N312, N610) of the composites on fiber–matrix interactions in high‐temperature geopolymer composites and their flexural behavior. The process we ultimately selected was as follows: an 8.5‐fold composite of surface area 100 cm² was pressed for 2 h at 120°C. After thermal treatment at 1150°C, composites containing the N312 textile with B2O3 showed greater heterogeneity, viscous flow and lower flexural strength (7 MPa) due to fiber–matrix interactions. In contrast, above 1150°C, composites with the N610 textile had no fiber–matrix interactions and showed greater flexural strength (51 MPa). The specific flexural strength correlated well with the overmodifying element ratio based on the composite composition. In fact, the presence of viscous flow suggested that boron and some aluminum atoms could act as network modifiers. Thus, the two ratios were nSigeo+nAlgeonMgeonSigeo+nAlgeonMgeo \frac{{n\mathrm{Si}}_{\mathrm{geo}}+n{\mathrm{Al}}_{\mathrm{geo}}}{{n\mathrm{M}}_{\mathrm{geo}}} or nSigeo+N312+nAlgeo×0.5+nAlN312nMgeo+nBN312+nAlgeo×0.5nSigeo+N312+nAlgeo×0.5+nAlN312nMgeo+nBN312+nAlgeo×0.5 \frac{{n\mathrm{Si}}_{\mathrm{geo}+\mathrm{N}312}+n{\mathrm{Al}}_{\mathrm{geo}}\times 0.5+{n\mathrm{Al}}_{\mathrm{N}312}}{{n\mathrm{M}}_{\mathrm{geo}}+{n\mathrm{B}}_{\mathrm{N}312}+{n\mathrm{Al}}_{\mathrm{geo}}\times 0.5} depending on the presence of viscous flow.
... This hybrid technique fully exploits the merits of both CVI and PIP techniques, and its produced composites have distinctive features such as high density, brilliant antioxidation property, good microstructural homogeneity, small mechanical property deviations as well as dramatically reduced fabrication durations, and so on. 17 It is worth pointing out that the processing temperature of both CVI and PIP processes is rather low, with the former ranging from 1000 to 1100 • C whilst the latter ranging from 1000 to 1200 • C. 18,19 Apparently, this manufacturing temperature is fiber friendly, but is much lower than the target application temperature of SiC f /SiC composites, which is 1300-1400 • C or even higher. A higher application than manufacturing temperature suggests that the composition, microstructure and thus properties of as-made composites might change during service, which perhaps could bring in some unexpected problems or even compromise the durability and reliability of SiC f /SiC composite parts, particularly for those PIP-derived matrix. ...
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The mechanical and thermophysical properties of KD‐SA SiCf/SiC composites manufactured by the hybrid chemical vapor infiltration (CVI)–precursor impregnation and pyrolysis (PIP) technique were systematically studied at 1400, 1600, and 1800°C, respectively, under argon atmosphere for 1 h. The results show that Si element in SiC fiber escapes and diffuses to pyrolytic carbon (PyC) interphase after 1400°C heat treatment, forming a Si‐rich line in PyC interphase. With a further increase of heat treatment temperature, the Si sublimation in the Si‐rich line leads to the cracking of the PyC interphase as well as the increase of the order degree of the PyC interphase, resulting in a significant decrease in the interfacial shear strength of the composite. Due to the decomposition of PIP SiC matrix and Si sublimation of SiC fiber, the flexural strength of the composite decreases after heat treatment at 1400°C. When the heat treatment temperature increases to 1600 and 1800°C, the flexural strength of the composite is slightly increased compared with 1400°C. Moreover, the thermal conductivity of the composites has been improved significantly by raising temperatures due to an increase of the crystallinity of the PIP SiC matrix.
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The cristobalite, transformed from amorphous silica basically, is ubiquitous in the thermodynamic stable region of quartz or tridymite. This formation mechanism of cristobalite metastability may be explained by the Ostwald's stage rule which is an experiential dynamic principle. The key factor which results in that the rate constant is higher in the process of the amorphous silica to transform to cristobalite than that in cristobalite to quartz or tridymite greatly is the similarity between the local intermediate range order structure for amorphous silica and the dynamic disorder structure of β-cristobalite. This statistical similarity leads to the increase of β-cristobalite valid nucleation rate greatly during the amorphous silica crystallization, and results in the formation of the metastabe cristobalite ultimately. The impure components in amorphous silica are propitious to decreasing the formation temperature of cristobalite and accelerating the reaction of amorphous silica to cristobalite. However, they are useless to formation of metastable cristobalite unless these impure components are in favor of stability of cristobalite structure.
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Three-dimensional carbon fiber zirconium carbide–silicon carbide composite (3D Cf/ZrC–SiC) was prepared by precursor infiltration and pyrolysis (PIP) with reactive melt infiltration (RMI) process. The 3D Cf/C–SiC substrate with open porosity of 20% and density of 1.35 g/cm3 was designed to be infiltrated by Zr0.912Si0.088 intermetallic compound. Thermodynamics calculations revealed that C could react with liquid Zr0.912Si0.088 to form ZrC at 1600 °C. Composites were prepared by heating the two materials to 1600 °C for 1 h in vacuum. The micro-structural, mechanical and ablative properties of the 3D Cf/ZrC–SiC composite were studied. ZrC and SiC were identified to be the main constituents. The flexural strength of the composite was 101.5±8.16 MPa and the elastic modulus was 35.18±9.58 GPa. The mass loss rate and linear recession rate of the 3D Cf/ZrC–SiC composite during oxyacetylene torch test were 0.013 g/s and 0.022 mm/s, respectively. The formation of ZrO2 melt on the surface of the composite contributed mainly to the excellent ablative property.
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The thermal oxidation of Si using H(2)zO=O(2) and H(2)O=N(2) ambients has been studied with an automated ellipsometer which can observe the oxidation in situ. The oxidations were carried out in the temperature range of 780 degrees 980 degrees C on < 100 > oriented single crystal Si. The resulting SiO(2) film growth data was analyzed according to a linear-parabolic oxidation model. The parabolic rate constant was found to increase abruptly with small additions of H(2)O to O(2) while the linear rate constant increased gradually over the range of added H(2)O (0- 2000 ppm). The over-all increase in the rate of oxidation due to H(2)O in O(2) was found to be greater than predicted based on the independent diffusion and reaction of O(2) and H(2)O related oxidant species. These effects of H(2)oO were found to be reversible. Therefore, the kinetic role of HO H(2)O on the oxidation of silicon is essentially twofold. The H(2)O acts both as an additional source of oxidaht and as an accelerator for the oxidation process involving O(2). It is postulated that this latter effect occurs because the H(2)O modifies the SiO(2) network thereby enhancing diffusion of the primary oxidant through the SiO(2) film.
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C/SiC and SiC/SiC composites are tough ceramics when the fiber–matrix bonding is properly optimized, usually through a thin layer of an interfacial material referred to as the interphase. These composites can be fabricated by a variety of techniques that are briefly described and compared. The design of the interphase, matrix, and coating at the nanometer scale, in order to promote microcrack deflection and to enhance the oxidation resistance is discussed. Selected properties of the composites are presented and discussed. Examples of application in engines, heat shields, braking systems, and high-temperature nuclear reactors are shown to illustrate the potential of these materials and the key points that still require research and development.
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SiC-based ceramic matrix composites, consisting of carbon or SiC fibers embedded in a SiC-matrix, are tough ceramics when the fiber/matrix bonding is properly optimized through the use of a thin interphase. They are fabricated according to different processing routes (chemical vapor infiltration, polymer impregnation/pyrolysis, liquid silicon infiltration or slurry impregnation/hot pressing) each of them displaying advantages and drawbacks which are briefly discussed. SiC-matrix composites are highly tailorable materials in terms of fiber-type (carbon fibers of SiC-based fibers such as Si–C–O, SiC+C or quasi-stoichiometric SiC reinforcements), interphase (pyrocarbon or hexagonal BN, as well as (PyC–SiC)n or (BN–SiC)n multilayered interphases), matrix (simple SiC or matrices with improved oxidation resistance, such as self-healing matrices) and coatings (SiC or engineered multilayered coatings). The potential of SiC-matrix composites for application in advanced aerojet engines (after-burner hot section), gas turbine of electrical power/steam cogeneration (combustion chamber) and inner wall of the plasma chamber of nuclear fusion reaction, all of them corresponding to very severe conditions is discussed.
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The oxidation behaviour of one-dimensional and two-dimensional SiC fibre reinforced SiC was investigated up to 1520°C in air, as well as in water vapour saturated air and argon by calorimetry, DTA and TGA. The oxidation process takes place in three steps: (1) oxidation of free carbon in the carbon coated composites between 530 and 690°C with mass losses up to 7.5%; (2) a fast exothermal process associated with mass gain starting at 800°C and terminated below 1500°C within 1 h; (3) the diffusion controlled oxidation of bulk SiC. The processes follow a logarithmic rate law between 875 and 985°C with an effective activation energy Q = 84 kJ/mol. The amorphous reaction product Si02 transforms to cristobalite at (930 ± 50)°C. The oxidation kinetics follows a quadratic rate law above 1000°C with rate constants k = 3.5 × 10−7g2/cm4h for 1D SiC/SiC and k = 5 × 10−8g2/cm4h for 2D SiC/SiC at 1520°C in air. The rate constants are up to three orders of magnitude higher than that for high density monolithic SiC which is explained by the high porosity of the SiC matrix.
Preparation of cristobalite and its thermal characteristics
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The study of crystallization process of high-purity silica at high temperature
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