ZrB2–SiC laminated ceramic composites

The oxidation behavior for ZrB₂–20 vol% SiC (ZS20) and ZrB₂–30 vol% SiC (ZS30) ceramics at 1500 °C was evaluated by weight gain measurements and cross-sectional microstructure analysis. Based on the oxidation results, laminated ZrB₂–30 vol% SiC (ZS30)/ZrB₂–25 vol% SiC (ZS25)/ZrB₂–30 vol% SiC (ZS30) symmetric structure with ZS30 as the outer layer were prepared. The influence of thermal residual stress and the layer thickness ratio of outer and inner layer on the mechanical properties of ZS30/ZS25/ZS30 composites were studied. It was found that higher surface compressive stress resulted in higher flexural strength. The fracture toughness of ZS30/ZS25/ZS30 laminates was found to reach to 10.73 MPa m^1/2 at the layer thickness ratio of 0.5, which was almost 2 times that of ZS30 monolithic ceramics.     

Manufacturing of ceramic composites reinforced with layered woven fabrics by CVI of SiC from dichlorodimethylsilane

Manufacturing of ceramic/ceramic composites by chemical vapor infiltration of SiC from dichlorodimethylsilane (DDS) in 2and 4-ply woven carbon fabrics has been studied. Dense deposition was obtained at a low reaction pressure such as 10 torr, as expected. However, little deposition was occurred at low DDS concentration such as 4%. Spaces between plies were left void with little deposition. The amount of deposition was proportional to the pressure and the DDS concentration. From the experimental data of the amount of deposition, the first order deposition rate constant of 40 cm/min was estimated. This value was bigger than our previous value. The tendencies for 4-ply sample were similar to those of 2-ply sample. Scanning electron microphotographs and pore size distribution analysis showed the same results.     

Fabrication of CNT-SiC/SiC composites by electrophoretic deposition

Due to the outstanding mechanical and thermal properties of carbon nanotubes (CNTs), they are considered suitable reinforcement for structural materials. In this study, for the first time, electrophoretic deposition (EPD) was used to deposit (multi-walled) CNTs onto SiC fibres (SiC_f) to form an effective CNT interphase layer for SiC_f/SiC composites. This deposition was followed by electrophoretic infiltration of the CNT-coated SiC fibre mats with SiC powder to fabricate a new CNT-SiC-fibre-reinforced SiC-matrix (SiC_f/SiC) composite for fusion applications. In these EPD experiments, a commercial aqueous suspension of negatively charged CNTs and an optimized aqueous suspension of negatively charged SiC particles were used. The CNT-coatings on the SiC fibres were firm and homogenous, and uniformly distributed nanotubes were observed on the fibre surfaces. In a following step of EPD, a thick SiC layer was formed on the fibre mat when the CNT-coated SiC fibres were in contact with the positive electrode of the EPD cell; however, spaces between the fibres were not fully filled with SiC. Conversely, when CNT-coated SiC fibres were isolated from the electrode, the SiC particles were able to gradually fill the fibre mat resulting in relatively high infiltration, which leads to dense composites.     

Microstructure control of SiCw/SiC composites based on SLS technology

The preparation of SiC_w/SiC materials was realized by SLS technology. The effect of SiC powder size on the number and size of SiC whisker formation was investigated. The tortuosity and diameter of open pores are introduced to modify the classical molecular collision model, and the relationship model between the growth rate of SiC whisker and porosity was established. The influence mechanism of powder size on the number of whisker growth was revealed. According to the model, the number of in-situ whisker growth in powder can be calculated, and the calculated results by using this model agreed with the test results. So it is suitable for in-situ whisker microstructure control under SLS technology, and also suitable for other 3D printed whisker in-situ reinforced ceramic material systems. This is of great significance to expand the application of 3D printing ceramic matrix composites.     

Fabrication and mechanical properties of SiC composites toughened by buckypaper and carbon fiber fabrics alternately laminated

SiC ceramics, for the first time, were toughened with nano scale carbon nanotubes (CNTs) buckypapers and micro scale carbon fibers within this work. The CNTs buckypapers were alternately laminated with carbon fiber fabrics (C_fb) to a preform by needle punched in Z-direction. Afterwards, the buckypaper-C_fb/SiC composites were obtained by infiltrating of SiC into the as-laminated preform via chemical vapor infiltration (CVI). Some effects of different lamination thickness and CVI times on the mechanical properties of the composites were investigated. Results showed that the maximum flexural strength and work of fracture of the buckypaper-C_fb/SiC composites reached 262.4 MPa and 4.15 kJ m⁻², respectively, when the thickness reached about 3.50 mm. Compared to C_fb/SiC composites without buckypapers, the strength and work of fracture of the buckypaper-C_fb/SiC composites increased by 19.8% and 111.7%, respectively. Densified composites can be obtained after CVI for 8 times. A main factor affecting the mechanical properties of buckypaper-C_fb/SiC composites is the degree of densification. Introducing nano scale CNTs and micro scale carbon fibers reaches a multiscale co-toughening effect. Meanwhile, a sandwich structure ceramic matrix composite with high-CNT concentration was obtained in this work.     

Fabrication of carbon/carbon composites by an electrified preform heating CVI method

Carbon/carbon composites are manufactured using the electrified preform producing directly heat CVI process. The preforms are prepared by laminating the carbon fiber felts with crossply reinforcement, and infiltrated with carbon using natural gas or propylene as a reactant, with nitrogen as diluent at atmospheric pressure. The relations between the resistivity of samples and infiltration time are determined under the operating conditions. The results indicate that the preforms have gained a high infiltration rate by this technology, and the samples have higher densities using natural gas rather than propylene. Their highest average bulk densities are up to 1.71 g/cm³ after the preforms of 1100×500×35 mm size have been densified for 80 h using natural gas. The carbon fibres in the preforms have not been damaged by this technology as yet, and the composites prepared have sufficiently high flexural properties. As the brake angular velocity is increased with the constant brake moment inertia and specific pressure, the average coefficient of friction for the composites prepared using natural gas is linearly and greatly decreased, but the variations of the brake moment inertia have a slight influence on the average coefficient of the friction when the brake angular velocity and specific pressure are kept constant. Their average thickness wear is 13×10⁻⁴ mm/surface per stop.     

Fabrication of Ti3SiC2-based ceramic matrix composites by a powder-free SHS technique

A powder-free technique for fabrication of Ti₃SiC₂-based composite ceramics via self-propagating high-temperature synthesis (SHS) is developed. The essence of the method is that the SHS-compaction of a multilayer stack comprised alternating layers of titanium foils and polymer films filled with either microsized silicon carbide particles or microsized silicon carbide particles mixed with charcoal particles. It is shown that SHS-compaction of non-powder materials can be used to synthesize dense particulate-reinforced ceramic matrix composites of Ti₃SiC₂TiSi₂SiC_p. Effects of the initial reactant composition and the synthesis conditions on the microstructure of the prepared materials are discussed.     

Subcritical crack growth processes in SiC/SiC ceramic matrix composites

Ceramic matrix composites have the potential to operate at high temperatures and are, therefore being considered for a variety of advanced energy technologies such as combustor liners in land-based gas turbo/generators, heat exchangers and advanced fission and fusion reactors. Ceramic matrix composites exhibit a range of crack growth mechanisms driven by a range of environmental and nuclear conditions. The crack growth mechanisms include: (1) fiber relaxation by thermal (FR) and irradiation (FIR) processes, (2) fiber stress-rupture (SR), (3) interface removal (IR) by oxidation, and (4) oxidation embrittlement (OE) resulting from glass formation including effects of glass viscosity. Analysis of these crack growth processes has been accomplished with a combination experimental/modeling effort. Dynamic, high-temperature, in situ crack growth measurements have been made in variable Ar + O₂ environments while a Pacific Northwest National Laboratory (PNNL) developed model has been used to extrapolate this data and to add radiation effects. In addition to the modeling effort, a map showing these mechanisms as a function of environmental parameters was developed. This mechanism map is an effective tool for identifying operating regimes and predicting behavior. The process used to develop the crack growth mechanism map was to: (1) hypothesize and experimentally verify the operative mechanisms, (2) develop an analytical model for each mechanism, and (3) define the operating regime and boundary conditions for each mechanism. A map for SiC/SiC composites has been developed for chemical and nuclear environments as a function of temperature and time.     

Fabrication and mechanical properties of carbon fibers/lithium aluminosilicate ceramic matrix composites reinforced by in-situ growth SiC nanowires

To improve the mechanical properties of carbon fibers/lithium aluminosilicate (C_f/LAS) composites, C_f/LAS with in-situ grown SiC nanowires (SiC_nw-C_f/LAS) were prepared by chemical vapor phase reaction, precursor impregnation, and hot press sintering, consecutively. The effect of multi-scaled reinforcements (micro-scaled C_f and nano-scaled SiC_nw) on the mechanical properties was investigated. The phase composition, microstructure and fracture surface of the composites were characterized by XRD, Raman Spectrum, SEM, and TEM. The morphology of SiC_nw has a close relation with the content of Si. Microstructure analysis suggests that the growth of SiC nanowires depends on the VLS mechanism. The multi-scale reinforcement formed by C_f and SiC_nw can significantly improve the mechanical properties of C_f/LAS. The bending strength of SiC_nw-C_f/LAS reaches to 597 MPa, achieving an increase of 19% to C_f/LAS. Moreover, the samples show a maximum fracture toughness of 11.01 MPa m^1/2, achieving an increase of 46.4% to C_f/LAS. Through analysis of the fracture surface, the improved mechanical properties could be attributed to the multi-scaled reinforcements by the pull-out and debonding of C_f and SiC_nw from the composites.     

Interaction of fiber matrix bonding in SiC/SiC ceramic matrix composites

Non-oxide ceramic matrix composites (CMC) based on SiC fibers with SiC matrix were fabricated by polymer infiltration and pyrolysis (PIP) and characterized regarding their microstructural features and their mechanical properties. The fiber preform was made using winding technology. During the winding process, the SiC fiber roving was impregnated by a slurry containing SiC powder and sintering additives (Y₂O_3, Al₂O₃ and SiO₂). This already helped to achieve a partial matrix formation during the preform fabrication. In this way, the number of PIP cycles to achieve composites with less than 10% open porosity could be reduced significantly. Additionally, damage-tolerant properties of the composites were obtained by an optimal design of the matrix properties although only uncoated fibers were used. Finally, composites with a strength level of about 500 MPa and a damage-tolerant fracture behavior with about 0.4% strain to failure were obtained.     

Modeling environmentally induced property degradation of SiC/BN/SiC ceramic matrix composites

The degradation of SiC‐based ceramic matrix composites (CMCs) in conditions typical of gas turbine engine operation proceeds via the stress rupture of fiber bundles. The degradation is accelerated when oxygen and water invade the composite through matrix microcracks and react with fiber coatings and the fibers themselves. We review micromechanical models of the main rate‐determining phenomena involved, including the diffusion of gases and reaction products through matrix microcracks, oxidation of SiC (in both matrix and fibers) leading to the loss of stiffness and strength in exposed fibers, the formation of oxide scale on SiC fiber and along matrix crack surfaces that cause the partial closure of microcracks, and the concomitant and synergistic loss of BN fiber coatings. The micromechanical models could be formulated as time‐dependent coupled differential equations in time, which must be solved dynamically, e.g., as an iterated user‐defined material element, within a finite element simulation. A paradigm is thus established for incorporating the time‐dependent evolution of local material properties according to the local environmental and stress conditions that exist within a material, in a simulation of the damage evolution of a composite component. We exemplify the calibration of typical micromechanical degradation models using thermodynamic data for the oxidation and/or volatilization of BN and SiC by oxygen and water, mechanical test data for the rate of stress rupture of SiC fibers, and kinetic data for the processes involved in gas permeation through microcracks. We discuss approaches for validating computational simulations that include the micromechanical models of environmental degradation. A special challenge is achieving validated predictions of trends with temperature, which are expected to vary in a complex manner during use.     

Thermal conductivity studies on Si/SiC ceramic composites

Ceramic heat exchangers are increasingly used in many nuclear power plants. Silicon carbide has been treated as a promising material for heat exchanger application since it has good thermal conductivity and corrosion resistance. In this work, four different types of Si/SiC ceramic composites were prepared by liquid silicon infiltration technique. Thermal conductivities of these ceramic composites at different temperatures are measured by the laser flash thermal conductivity method. Results show that the presence of free carbon and voids are notably affecting the thermal conductivity of these materials.     

Multiple ballistic damage of segmented SiC/BN laminated ceramic composite armor

This article investigated the structure of the laminated ceramics to improve the multiple ballistic performance of segmented ceramic composite armors. The multiple ballistic experiments were conducted with 5.8 mm caliber steel core bullets at the impact velocity of about 920 m/s. The experiments verified that two laminated SiC/BN structures (GLC and ULC) exhibit higher residual ballistic performances than the monolithic SiC structure (MC). Moreover, through damage evolution analysis, two laminated SiC/BN structures (GLC and ULC) exhibit less sensitivity to the multiple ballistic impacts damages, and possess more energy absorption mechanisms than the monolithic ceramics. The structure design of the laminated of ceramics is beneficial for improving the multiple ballistic performances of composite armors and reducing the crater deformation.     

Application of the pack cementation process on SiC/SiC ceramic matrix composites

The potentials and limitations of a halide-activated pack cementation process on SiC/SiC Ceramic Matrix Composites for the development of bond coats as part of environmental barrier coating (EBCs) systems were investigated. Different pack compositions using chromium, aluminum and alloys of these elements were tested and the kinetics of coating formation were examined in addition to their microstructure. The results and their analogy to diffusion couples were discussed and it was shown that coating elements which form silicides and carbides are promising candidates for coatings deposited on SiC/SiC via pack cementation. Based on such considerations a two-step pack cementation was proposed, which used chromium, one of the suitable elements, in a first step, to finally achieve an alumina-forming coating. The oxidation resistance of the developed coating was tested via thermogravimetric analysis and compared to the uncoated material. The coating protected the fiber-matrix interface of the SiC/SiC Ceramic Matrix Composites from oxidation.     

Elastic-Property Measurements on CVI SiC/SiC Minicomposites by Acoustic Microscopy

In situ elastic properties of the fiber and matrix in composites obtained via chemical vapor infiltration/chemical vapor deposition (CVI-CVD) have been determined using acoustic microscopy. An unusually high frequency was used to attain the resolution that was required by the structure and small size of the constituents in these nonhomogeneous materials. A coupling liquid was prepared with acoustic properties that were chosen with consideration of the high frequency and the material characteristics. Local measurements on the fibers and matrix were achieved by studying the acoustic signature that was processed on very small areas. The elastic modulus of the fibers and matrices was deduced from the velocity measurements.     

Fabrication of SiC whisker-reinforced SiC ceramic matrix composites based on 3D printing and chemical vapor infiltration technology

Spray drying, binder jetting and chemical vapor infiltration (CVI) were used in combination for the first time to fabricate SiC whisker-reinforced SiC ceramic matrix composites (SiC_W/SiC). Granulated needle-shaped SiC_W was spray dried into SiC_W spherical particles to increase flowability and thereby increase printability. Then, binder jetting was employed to print a novel SiC_W preform with two-stage pores using the SiC_W spherical particles. The subsequent CVI technology produced pure, dense, and continuous SiC matrix with high modulus and strength. Consequently, SiC_W/SiC with appropriate mechanical properties was obtained. Finally, the challenges of the novel method and the ways to improve the mechanical properties of SiC_W/SiC are discussed.     

Stereolithography-based additive manufacturing of polymer-derived SiOC/SiC ceramic composites

In order to overcome challenges typically encountered during additive manufacturing of ceramics via the polymer precursor route, a novel polymer-derived SiOC/SiC composite system suitable for advanced geometric designs achievable by lithography-based ceramic manufacturing was established. The photoreactive resin system filled with 20 wt% SiC exhibits suitable viscosity characteristics, adequate stability against sedimentation, and a fast photocuring behavior. After printing and pyrolytic conversion, SiC particulates were well-dispersed within the polymer-derived SiOC matrix. A direct comparison with the unfilled polysiloxane-based resin system showed that the addition of particulate SiC increases handleability, reduces shrinkage, and significantly increases critical wall thicknesses up to 5 mm. The biaxial Ball-on-Three-Balls testing methodology yielded a characteristic strength of 325 MPa for SiOC/SiC composites. The results highlight the high potential of particle-filled preceramic polymer systems toward the fabrication of high-performance SiC-based materials by lithography-based additive manufacturing.     

Fabrication of Ti3SiC2-Ti4SiC3-SiC ceramic composites through carbosilicothermic reduction of TiO2

Dense Ti₃SiC₂-SiC, Ti₄SiC₃-SiC, and Ti₃SiC₂-Ti₄SiC₃-SiC ceramic composites were fabricated through carbosilicothermic reduction of TiO₂ under vacuum, followed by hot pressing of the as-synthesized products under 25 MPa at 1600°C. In the reduction step, SiC either alone or in combination with elemental Si was used as a reductant. A one-third excess of SiC was added in the reaction mixtures in order to ensure the presence of approximately 30 vol.% SiC in the products of synthesis. During the hot pressing step, the samples that contained Ti₃SiC₂ showed better densification compared to those containing Ti₄SiC₃. The obtained composites exhibited the strength properties typical of coarse-grained MAX-phase ceramics. The flexural strength values of 424 and 321 MPa were achieved in Ti₃SiC₂-SiC, and Ti₃SiC₂-Ti₄SiC₃-SiC composites, respectively. The fracture toughness values were 5.7 MPa·m^1/2.     

Fabrication of ZrB2-SiC ceramic composites by optimized gel-casting method

The ZrB₂-SiC ceramics with homogenous microstructures were successfully fabricated by the optimized gel-casting method and pressureless sintering. The effects of the processing parameters, including the monomer content, cross-linker/monomer ratios, initiator addition, catalyst concentration and polymerization temperature, on the final gel properties were systematically investigated. The rheological behavior and stability of ZrB₂-SiC suspensions were evaluated, and the microstructures and mechanical properties of sintered ceramics were also analyzed. The homogenous gel networks containing low monomer content (4 wt%) and without catalysts had been successfully obtained, which could be mainly attributed to the homogeneous distribution of crosslinking points and temperature-induced gelation. The crack-free and complex-shaped ZrB₂-SiC ceramic composites were achieved by the optimized gel-casting, which could reach the highest relative density of 97.2% and the flexural strength of 402 ± 57 MPa, respectively. This study provides an optimized gel-casting process for fabricating ZrB₂-SiC ceramics with excellent properties by low colloidal additives and without catalysts.