Effects of oxidation temperature on microstructure and EMI shielding performance of layered SiC/PyC porous ceramics

Herein, the influence of oxidation temperature on the oxidation behavior, microstructure and electromagnetic shielding performance of layered porous ceramics has been systematically investigated. Layered SiC/PyC porous ceramics were prepared by using low-pressure chemical vapor infiltration (LPCVI) method. The oxidized SiC/PyC layered porous ceramics exhibited a negligible mass reduction of 11.94 mg·cm^?3, which indicates the excellent high-temperature oxidation resistance of porous ceramics. The electromagnetic shielding performance of SiC/PyC porous ceramics did not exhibit any obvious change even after oxidation at high temperature from 900 to 1300 °C for 10 h. The SE_T of the layered SiC/PyC porous ceramics was 24.1, 20.0, 19.5, 19.0, 19.8 dB after oxidation at 25 °C, 900 °C, 1000 °C, 1100 °C and 1300 °C, which corresponds to a decrease of 17.01%, 19.09%, 21.16% and 17.84%, respectively. The high-temperature oxidation has rendered a more significant influence on the reflection efficiency of the layered SiC/PyC porous ceramics.     

Large-scale synthesis of SiC/PyC core-shell structure nanowires via chemical liquid-vapor deposition

In carbon/carbon (C/C) composites, SiC/PyC core-shell structure nanowires were successfully fabricated via chemical liquid-vapor deposition (CLVD). The influences of heat-treatment temperature on the microstructure and composition of SiC nanowires were studied, and meanwhile the growth mechanism of SiC nanowires was discussed. Additionally, the microstructure and morphology of SiC/PyC core-shell structure nanowires were also investigated. The results displayed that the low heat-treatment temperature could not meet the requirements of SiC nanowires growth, but the too high temperature made the nanowires appear agglomerate easily. Only when the heat-treatment temperature was 1800 °C, SiC nanowires possessed a uniform distribution. The diameter of SiC nanowire was about 300 nm, and there was a SiO₂ layer with the thickness of about 1 nm existing on the surface of SiC nanowire. The growth behavior of SiC nanowire was governed by vapor-solid (V–S) mechanism. After the PyC deposition, SiC/PyC core-shell structure nanowires were constructed, and the nanowires were about 450 nm in diameter. These nanowires displayed a core-shell structure with three layers, which were SiC nanowire core, SiO₂ interlayer and PyC shell, respectively. Meanwhile, SiC/PyC core-shell structure nanowires connected the matrices with each other, and the core-shell structure nanowires generated a stable network.     

Fabrication process and growth mechanism of novel micro-stack PyC interphase with different textures

Pyrolytic carbon (PyC) interphase plays a crucial role in the mechanical properties of fiber-reinforced ceramic matrix composites. In this research, a novel micro-stack PyC interphase with different PyC textures was designed and fabricated by changing the deposition parameters during the chemical vapor infiltration process. The growth mechanism of the micro-stack PyC interphase with different texture were also studied by experimental characterizations and kinetic calculations, and the results show that the content ratio of (C₂H₂ + C₂H₄) to C₆H₆ gas intermediate is a key parameter to control the texture types of PyC interphase. Furthermore, the value of orientation angle (OA) value, thickness, and modulus of the micro-stack PyC interphase were further characterized by high resolution TEM (HRTEM), scanning electronic microscopy, and nanoindentation. Finally, the tensile testing of mini-C_f/PyC/SiC composites was conducted, and the results showed that the tensile strength of mini-C_f/PyC/SiC composites with micro-stack PyC interphase is approximately 40% higher than that containing single high texture PyC interphase. The improvements on the tensile strength of C_f/PyC/SiC composites prove the significant advantages of micro-stack PyC interphase.     

Fabrication and properties of SiCnw-reinforced SiC composites by reactive melt infiltration with BN and PyC interface

To tailor the fiber–matrix interface of SiC nanowires-reinforced SiC (SiC_nw/SiC) ceramic matrix composites (CMCs) for improved mechanical properties, SiC nanowires were coated with BN and pyrolytic carbon (PyC) compound coatings prepared by the dip-coating process in boric acid and urea solution and the pyrolysis of phenolic resin. SiC_nw/SiC CMC with PyC/BN interfaces were fabricated by reactive melt infiltration (RMI) at 1680°C for 1 h. The influences of phenolic resin content on the microstructure and mechanical properties of the CMC were investigated. The results showed that the flexural strength and fracture toughness reach the maximum values of 294 MPa and 4.74 MPa m^1/2 as the phenolic resin content was 16 and 12 wt%, respectively. The displacement–load curve of the sample exhibited a gradient drop with increasing phenolic resin content up to 12 wt%. The results demonstrated that the PyC/BN compound coatings could play the role of protecting the SiC_nw from degradation as well as improving the more moderate interfacial bonding strengths during the RMI.     

Mechanical properties of SiCf/SiC composites with alternating PyC/BN multilayer interfaces

Alternating pyrolytic carbon/boron nitride (PyC/BN)_n multilayer coatings were applied to the KD–II silicon carbide (SiC) fibres by chemical vapour deposition technique to fabricate continuous SiC fibre-reinforced SiC matrix (SiC_f/SiC) composites with improved flexural strength and fracture toughness. Three-dimensional SiC_f/SiC composites with different interfaces were fabricated by polymer infiltration and pyrolysis process. The microstructure of the coating was characterised by scanning electron microscopy, X–photoelectron spectroscopy and transmission electron microscopy. The interfacial shear strength was determined by the single-fibre push-out test. Single-edge notched beam (SENB) test and three-point bending test were used to evaluate the influence of multilayer interfaces on the mechanical properties of SiC_f/SiC composites. The results indicated that the (PyC/BN)_n multilayer interface led to optimum flexural strength and fracture toughness of 566.0?MPa and 21.5?MPa?m^1/2, respectively, thus the fracture toughness of the composites was significantly improved.     

Microstructure and damage evolution of SiCf/PyC/SiC and SiCf/BN/SiC mini-composites: A synchrotron X-ray computed microtomography study

SiC_f/PyC/SiC and SiC_f/BN/SiC mini-composites comprising single tow SiC fibre-reinforced SiC with chemical vapor deposited PyC or BN interface layers are fabricated. The microstructure evolutions of the mini-composite samples as the oxidation temperature increases (oxidation at 1000, 1200, 1400, and 1600?°C in air for 2?h) are observed by scanning electron microscopy, energy dispersive spectrometry, and X-ray diffraction characterization methods. The damage evolution for each component of the as-fabricated SiC_f/SiC composites (SiC fibre, PyC/BN interface, SiC matrix, and mesophase) is mapped as a three-dimensional (3D) image and quantified with X-ray computed tomography. The mechanical performance of the composites is investigated via tensile tests.The results reveal that tensile failure occurs after the delamination and fibre pull-out in the SiC_f/PyC/SiC composites due to the volatilization of the PyC interface at high temperatures in the air environment. Meanwhile, the gaps between the fibres and matrix lead to rapid oxidation and crack propagation from the SiC matrix to SiC fibre, resulting in the failure of the SiC_f/PyC/SiC composites as the oxidation temperature increases to 1600?°C. On the other hand, the oxidation products of B₂O₃ molten compounds (reacted from the BN interface) fill up the fracture, cracks, and voids in the SiC matrix, providing excellent strength retention at elevated oxidation temperatures. Moreover, under the protection of B₂O₃, the SiC_f/BN/SiC mini-composites show a nearly intact microstructure of the SiC fibre, a low void growth rate from the matrix to fibre, and inhibition of new void formation and the SiO₂ grain growth from room to high temperatures. This work provides guidance for predicting the service life of SiC_f/PyC/SiC and SiC_f/BN/SiC composite materials, and is fundamental for establishing multiscale damage models on a local scale.     

Effects of porosity on electrical and thermal conductivities of porous SiC ceramics

The effects of porosity on the electrical and thermal conductivities of porous SiC ceramics, containing Y₂O₃–AlN additives, were investigated. The porosity of the porous SiC ceramic could be controlled in the range of 28–64 % by adjusting the sacrificial template (polymer microbead) content (0–30 wt%) and sintering temperature (1800–2000 °C). Both electrical and thermal conductivities of the porous SiC ceramics decreased, from 7.7 to 1.7 Ω⁻¹ cm⁻¹ and from 37.9 to 5.8 W/(m·K), respectively, with the increase in porosity from 30 to 63 %. The porous SiC ceramic with a coarser microstructure exhibited higher electrical and thermal conductivities than those of the ceramic with a finer microstructure at the equivalent porosity because of the smaller number of grain boundaries per unit volume. The decoupling of the electrical conductivity from the thermal conductivity was possible to some extent by adjusting the sintering temperature, i.e., microstructure, of the porous SiC ceramic.     

PyC interphase growth mechanism and control models of C/SiC composites

To better understand the pyrocarbon (PyC) interphase growth mechanism, a series of experiments was conducted on the PyC deposited on T-300™ and T-700™ carbon fibers by the chemical vapor infiltration (CVI) method. Nine groups of fabrication parameters were used to analyze the effects of deposition temperature, pressure, and residence time on the PyC interphase growth mechanism. Atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), Raman spectroscopy, and nanoindentation tests were performed to characterize the microstructures of carbon fibers and PyC interphase. The PyC interphase growth mechanism was discussed, and the relationships between the fabrication parameters, R (C₂/C₆) value, texture type, and interphase thickness were established through numerical simulations. The hardness and modulus of PyC for T-300™ and T-700™ carbon fibers were measured. The tensile behaviors of C/SiC minicomposites with medium and high textures PyC interphases were analyzed. The C/SiC composite with the medium texture PyC interphase possessed the higher fracture strength and failure strain with a longer fiber pullout length at the fracture surface.     

Electromagnetic shielding performance of SiC/graphitic carbon-SiCN porous ceramic nanocomposites derived from catalyst assisted single-source-precursors

In this work, SiC nanowires and graphitic carbon (GC) including 2D reduced graphene oxide and graphene-liked ribbons modified polymer derived SiCN (SiC/GC-SiCN) porous ceramic monoliths were prepared via catalyst assisted single-source-precursor derived ceramic route. The inclusion of absorbents (e.g. graphitic carbon and SiC nanowires) significantly improved the electrical conductivity of the materials from 1.77 × 10^?8 S/cm (pristine SiCN) to 0.56 S/cm. In turn, the electromagnetic interference shielding effectiveness (EMI SE) of the ceramic increased significantly from 4.0 dB to 19.2 dB. At the highest absorbent content, the SiC/GC-SiCN ceramics exhibit a high absorption power of 0.3 nW and an SE of 48.5 dB at thickness of 2 mm, which means more than 99.998 % of the EM wave is blocked. This work finds new avenue for the design of advanced electromagnetic shielding materials possessing strong absorption capability.     

The improvement of mechanical properties of SiC/SiC composites by in situ introducing vertically aligned carbon nanotubes on the PyC interface

In order to improve the mechanical properties, vertically aligned carbon nanotubes (VACNTs) were in situ introduced on the pyrocarbon (PyC) interfaces of the multilayer preform via chemical vapor deposition (CVD) process under tailored parameters. Chemical vapor infiltration (CVI) process was then employed to densify the multilayer preform to acquire SiC/SiC composites. The results show that the growth of VACNTs on PyC interface is highly dependent to the deposition temperature, time and constituent of gas during CVD process. The preferred orientation and high graphitization of VACNTs were obtained when temperature is 800?℃ and C₂H₄/H₂ ratio is 1:3. The bending strength and fracture toughness of SiC/SiC composites with PyC and PyC-VACNTs interfaces were compared. Compared to the SiC/SiC composite with PyC interface, the bending strength and fracture toughness increase 1.298 and 1.359 times, respectively after the introduction of PyC-VACNTs interface to the SiC/SiC composites. It is also demonstrated that the modification of PyC interface with VACNTs enhances the mechanical properties of SiC/SiC composites due to the occurrence of more fiber pull-outs, interfacial debonding, crack branching and deflection     

Using PyC coated short chopped carbon fiber to tackle the dilemma between toughness and strength of ZrC-SiC

Graceful toughness and high strength are mutually exclusive in engineering ZrC-SiC ceramic, which are hard to be possessed simultaneously. Here, the pyrolytic carbon (PyC) coated short chopped carbon fibers were utilized to toughen ZrC-SiC ceramic, tackling the dilemma between toughness and strength. Through the uniform incorporation of PyC coated short chopped carbon fibers, the penetration crack mode of ZrC-SiC was changed into an obviously deflecting propagation path with closed phenomenon. The PyC coating brought about a relatively weak interface bonding and guided the crack propagate along the weak interface, consequently resulting in a more flexuous crack propagation instead of passing through the fibers directly. Meanwhile, the fibers received effective protection of coating inhibiting from performance degradation. The PyC coated C_f/ZrC-SiC obtained a fracture toughness highly reaching 7.57?±?0.33?MPa?m^1/2 with a rivaling flexural strength at 268?±?16?MPa. Moreover, the graceful load-displacement curve is illustrated with a smoothly extended displacement of 0.12?mm and increased load to 83?N, which forms an obvious yield plateau. To some degree, this work provided an effective solution to tackling the dilemma between toughness and strength of engineering ZrC-SiC ceramic.     

Mechanical Behavior and Electromagnetic Interference Shielding Properties of C/SiC–Ti3Si(Al)C2

In this paper, a low‐temperature densification process of Al–Si alloy infiltration was developed to fabricate C/SiC–Ti₃Si(Al)C₂, and then the microstructure, mechanical, and electromagnetic interference (EMI) shielding properties were studied compared with those of C/SiC–Ti₃SiC₂ and C/SiC–Si. The interbundle matrix of C/SiC–Ti₃Si(Al)C₂ is mainly composed of Ti₃Si(Al)C₂, which can bring various microdeformation mechanisms, high damage tolerance, and electrical conductivity, leading to the high effective volume fraction of loading fibers and electrical conductivity of C/SiC–Ti₃Si(Al)C₂. Therefore, C/SiC–Ti₃Si(Al)C₂ shows excellent bending strength of 556 MPa, fracture toughness 21.6 MPa·m^1/2, and EMI shielding effectiveness of 43.9 dB over the frequency of 8.2–12.4 GHz. Compared with C/SiC–Si and C/SiC–Ti₃SiC₂, both the improvement of mechanical properties and EMI shielding effectiveness can be obtained by the introduction of Ti₃Si(Al)C₂ into C/SiC, revealing great potential as structural and functional materials.     

Improved thermal shock resistance of SiCnw/PyC core-shell structure-toughened CVD-SiC coating

In-situ SiC nanowire (SiCnw)/pyrolytic carbon (PyC) core-shell structures were introduced to mainly improve the thermal shock performance of chemical vapor deposition (CVD)-SiC coating on carbon/carbon (C/C) composites. The microstructure, phase composition, and mechanical properties of the CVD-SiC coating toughened by SiCnw/PyC core-shell structures were studied as well. The results show that the introduction of SiCnw/PyC core-shell structures can effectively alleviate the mismatch of coefficient of thermal expansion (CTE) between SiC coating and C/C substrate, thus enhancing the thermal shock resistance of the coating. Furthermore, the increased numbers of interfaces in the SiC coating owing to the addition of core-shell structures are beneficial to the mechanical properties of the coating after thermal shock test.     

In situ growth of one-dimensional carbon-rich SiC nanowires in porous Sc2Si2O7 ceramics with excellent microwave absorption properties

For enhancing the absorption ability of dielectric and electromagnetic wave (EMW), C-rich SiC NWs /Sc₂Si₂O₇ ceramics are successfully fabricated through in-situ growth of SiC nanowires (NWs) into porous Sc₂Si₂O₇ ceramics by precursor infiltration and pyrolysis (PIP) at 1400?°C in Ar. SiC NWs are in-situ formed in the pore channels via a vapor-liquid-solid (VLS) mechanism, the relative complex permittivity increases notably with the content of absorber (C-rich SiC NWs), which tune the microstructure and dielectric property of C-rich SiC NWs/Sc₂Si₂O₇ ceramics. Meanwhile, the minimum reflection coefficient (RC) of C-rich SiC NWs/Sc₂Si₂O₇ ceramic decreases from ?9.5?dB to ??35.5?dB at 11?GHz with a thickness of 2.75?mm, and the effective absorption bandwidth (EAB) covers the whole X band (8.2–12.4?GHz) when the content of absorber is 24.5?wt%. The results indicate that Sc₂Si₂O₇ ceramics decorated with SiC NWs and nanosized carbon have a superior microwave-absorbing ability, which can be contributed to the Debye relaxation, interfacial polarization and conductivity loss enhanced by in-situ formed SiC NWs and nanosized carbon phases. The C-rich SiC NWs /Sc₂Si₂O₇ ceramics can be a promising microwave absorbing materials within a broad bandwidth.     

Electromagnetic interference shielding and dielectric properties of SiCf/SiC composites containing pyrolytic carbon interphase

The SiC_f/SiC composites containing various thickness of pyrolytic carbon (PyC) interphase were prepared and their properties were investigated for electromagnetic interference (EMI) shielding applications in the frequency of 8.2–12.4 GHz. The composites containing 310 nm thickness (3.3 vol%) PyC interphase show an about 25 dB shielding effectiveness in the whole frequency band. Interestingly, the contribution of reflection to the EMI shielding effectiveness increases and the contribution of absorption decreases as the PyC interphase thickness increases.     

Ablative and mechanical properties of C/C-SiC-ZrC composites modified with PyC/SiC and PyC/BN interface layers

Two kinds of novel modified C/C-SiC-ZrC composites were prepared via precursor infiltration and pyrolysis, as pyrocarbon (PyC)/silicon carbide (SiC) and PyC/boron nitride (BN) dual-layer interphases were separately structured on the fibers by means of chemical vapor infiltration. Data analysis and conclusions are served for investigating the effects of these two interface layers on mechanical and anti-ablative properties. On the mechanical property hand, both PyC/BN and PyC/SiC interphase layers play positive roles, resting with the reduction of fiber damage during the fabrication process. Compared with BN, SiC shows better enhancement as the flexural strength of PyC/BN and PyC/SiC interphase-modified composites are 214.9 and 229.2 MPa, respectively. On the ablative property hand, after oxyacetylene flame ablation for 60 s, the mass and linear ablation rates of the composites modified by PyC/SiC interface were 2.2 mg/s and 9.7 μm/s, which is much lower than that modified by PyC/BN. The inferior ablation properties of PyC/BN-CSZ were attributed to the vaporization of the B₂O₃ gas that destroys the integrity of the oxide film and oxygen erosion on the substrate through the damaged BN interface.     

Fabricating porous ceramic materials via phase separations in blends of cellulose acetate and ceramic nanoparticles

As applications of porous ceramic materials have gradually expanded, the novel technologies for the fabrication of porous ceramic materials with a delicate and controllable structure are still attractive. In this work, three types of porous monolithic ceramic materials, including Al₂O₃–SiO₂, TiO₂, and SiC, have been fabricated by thermally impacted and non-solvent-induced phase separations in blends of cellulose acetate and ceramic nanoparticles. These materials possessed three-dimensional interconnected porous structures with low densities, high porosities, and hierarchical pores ranging from 5 nm to 6 μm. The relationships between microstructures and phase separations were systematically investigated. Furthermore, electromagnetic shielding effectiveness of 20 dB from 5 to 18 GHz in porous SiC materials has been achieved, revealing that those materials have potential applications in the electromagnetic shielding. This work provides a powerful and general approach to fabricate porous monolithic ceramic materials with a wide range of various ceramic nanoparticles.     

Improved electromagnetic absorbing properties of Si3N4–SiC/SiO2 composite ceramics with multi-shell microstructure

Porous Si₃N₄–SiC composite ceramic was fabricated by infiltrating SiC coating with nano-scale crystals into porous β-Si₃N₄ ceramic via chemical vapor infiltration (CVI). Silica (SiO₂) film was formed on the surface of rod-like Si₃N₄–SiC grains during oxidation at 1100 °C in air. The as-received Si₃N₄–SiC/SiO₂ composite ceramic attains a multi-shell microstructure, and exhibits reduced impedance mismatch, leading to excellent electromagnetic (EM) absorbing properties. The Si₃N₄–SiC/SiO₂ fabricated by oxidation of Si₃N₄–SiC for 10 h in air can achieve a reflection loss of ?30 dB (>99.9% absorption) at 8.7 GHz when the sample thickness is 3.8 mm. When the sample thickness is 3.5 mm, reflection loss of Si₃N₄–SiC/SiO₂ is lower than ?10 dB (>90% absorption) in the frequency range 8.3–12.4 GHz, the effective absorption bandwidth is 4.1 GHz.     

Ice-templated assembly strategy to construct oriented porous Ti3SiC2 ceramics for thermal management and electromagnetic interference shielding in harsh thermal environments

Given the electromagnetic interference (EMI) and heat aggregation issue faced by electronic components, an urgent need exists to integrate EMI shielding and thermal conductivity in one material. Herein, a novel lightweight porous Ti₃SiC₂ ceramic with ordered structural arrangement was fabricated by using budget-friendly raw materials through ice template design and in-situ reaction synthesis. Leveraging the excellent conductivity and thermal conductivity of Ti₃SiC₂, a dual-functional advanced material with efficient EMI shielding and thermal management capabilities was obtained. At room temperature, porous Ti₃SiC₂ ceramics can achieve a shielding effectiveness of 35.44 dB and a thermal conductivity of 12.17 W/mK, with performance that can be tuned by porosity. In further, the porous Ti₃SiC₂ ceramic can work stably in thermal environments from room temperature to 700 °C or in corrosive environments rich in acid, alkali, and salts due to its excellent high temperature oxidation resistance and corrosion resistance. In view of the dual-functional characteristics and the stability of operation in harsh thermal environments, ordered porous Ti₃SiC₂ ceramics are promising for modern maritime and aerospace applications.     

Thermophysical properties of carbon fiber reinforced multilayered (PyC–SiC)n matrix composites

Three kinds of carbon fiber reinforced multilayered (PyC–SiC)_n matrix (C/(PyC–SiC)_n) composites (n = 1, 2 and 4) were prepared by means of layer-by-layer deposition of PyC and SiC via chemical vapor infiltration. Thermal expansion behaviors in the temperature range of 800–2500 °C and thermal conductivity from room temperature to 1900 °C of C/(PyC–SiC)_n composites with various microstructures were investigated. The results show that with increasing PyC–SiC sequences number (n), the coefficients of thermal expansion of the composites decrease due to the increase of interfacial delamination, providing room for thermal expansion. The thermal diffusivity and thermal conductivity also decrease with the increase of sequences number, which are attributed to the enhancement of phonon-interface scattering resulted from the increasing number of interfaces. Modified parallel and series models considering the interfacial thermal resistance are proposed to elaborate thermal conductivity of the composites, which is in accordance with the experimental results.