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Combination of PIP and LSI processes for SiC/SiC ceramic matrix composites
Abstract
Silicon carbide fiber-reinforced silicon carbide matrix composites (SiC/SiC CMCs) are promising candidates for components in the hot gas section of jet engines, as they exhibit high temperature resistance and low density compared to their metal alloy counterparts. Three common manufacturing routes are chemical vapor infiltration, reactive melt infiltration (RMI) and polymer infiltration and pyrolysis (PIP). This work describes a new approach of a combined PIP and RMI process. A combination of the processes seems attractive: the remaining porosity after PIP process can be closed by subsequent siliconization, resulting in a dense material. SiC/SiC CMCs were manufactured by PIP process using Hi-Nicalon Type S fibers. Generally, the processing of SiC/SiC, produced solely by PIP route, is rather time-consuming and the composites show a certain residual porosity. In order to obtain a dense matrix and to reduce the processing time, an additional RMI with silicon alloy is carried out after a reduced number of PIP cycles. To protect the fibers during the siliconization, a CVD fiber coating was applied. Microstructure was examined via microCT, SEM and EDS. Bending strength was determined to 433 MPa; strain to failure was 0.60%. The overall processing time was reduced by 55% compared to standard PIP route. The hybrid material contained 70% less unreacted carbon than material produced by LSI process alone.
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.
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.
Research efforts on Ceramic Matrix Composites (CMCs) are aimed to increase the operating temperature in oxidizing environments by adding Ultra-High Temperature Ceramic (UHTC) phases to the matrix. The structural performances of UHTC-enriched CMCs are generally investigated through bending test because it requires simple fixture and specimen geometry with small quantity of plate material. However, there are hardly any scientific studies which bring out what bending test conditions are required to determine reliable flexural strength of these composites. In this study, the effect of span length and specimen orientation on the flexural strength of UHTC-enriched SICARBON™ material, produced by Airbus, was comprehensively evaluated and reported. Transition of the failure mode was obtained by tilting the specimens with horizontal build direction instead of lay-up configuration (vertical build direction). The tilted configuration allowed to get a valid flexural strength of 370 MPa even with small specimens of about 30 mm. To assess failure mode in different test configurations, virtual microstructure was generated on the base of cumulative distribution functions of observed microstructural features. Tsai-Wu failure criterion was extended in order to evaluate direction dependent failure indices for different lay-up configurations.
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