Effect of the pyrolytic carbon (PyC) content on the dielectric and electromagnetic interference shielding properties of layered SiC/PyC porous ceramics

A novel layered SiC/pyrolytic carbon (PyC) porous ceramic was synthesized from a nickel foam substrate via low-pressure chemical vapor infiltration (LPCVI) with SiCl₃CH₃-NH₃-BCl₃-H₂-Ar. The microstructure and phase composition of the PyC deposited via Ni catalysis were investigated. In addition, the effect of the PyC content on the microstructure, conductivity, and electromagnetic shielding effectiveness of a two-layered SiC/PyC porous ceramic were discussed. Both the electrical conductivity (from 0.090 to 0.319?S/cm) and the total shielding effectiveness (from 19.2 to 29.0?dB) of the two-layer SiC/PyC porous ceramic (pore size: 200–400?µm) increased with the PyC content. The high-temperature shielding effectiveness of the sample showed an outstanding stability with temperature and remained nearly unchanged (only 2?dB variation) over the 25–600?°C temperature range.     

Microstructural evolution and microwave transmission/absorption transition in polymer-derived SiOC ceramics

Herein, we present the structural evolution of polymer-derived SiOC ceramics with the pyrolysis temperature and the corresponding change in their microwave dielectric properties. The structure of the SiOC ceramics pyrolyzed at a temperature lower than 1200 °C is amorphous, and the corresponding microwave complex permittivity is pretty low; thus, the ceramics exhibit wave transmission properties. The Structural arrangement of free carbon in the SiOC ceramics mainly happens in the temperature range of 1200 °C-1300 °C due to the separation from the Si–O–C network and graphitization, while the structural arrangement of the Si-based matrix mainly occurs in the range of 1300 °C-1400 °C owing to the separation of SiC₄ from the Si–O–C network to form nanocrystalline SiC. In pyrolysis temperature range of 1200 °C-1400 °C, the microwave permittivity of SiOC shows negligible change. At a pyrolysis temperature exceeding 1400 °C, the carbothermal reaction of free carbon and the Si–O backbone becomes significant, leading to the formation of crystalline SiC. The as-formed SiC and residual defective carbon improve the polarization loss of SiOC ceramics. In this case, the SiOC ceramics show significantly increased complex permittivity, exhibiting electromagnetic absorption characteristics. These characteristics promote the application of polymer-derived SiOC ceramics to high-temperature electromagnetic absorption materials.     

Low-temperature preparation of porous SiC ceramics using phosphoric acid as a pore-forming agent and a binder

Porous SiC ceramics combine the properties of both SiC ceramics and porous materials. Herein, we design a facile method via pressureless sintering at relatively low temperatures for the synthesis of porous SiC ceramics. In the synthesis process, phosphoric acid was used as the sintering additive that reacted with SiO₂ on the surface of SiC to form phosphates. The formed phosphates acted as a binder to connect the SiC particles. At a fixed temperature, the phosphates were partially decomposed and released a large amount of gas. This changed the pore structure of the ceramics and greatly improved their porosity. Finally, we obtained the porous SiC ceramics with high porosity and high strength. We investigate the effects of H₃PO₄ content on the phase composition, microstructure, porosity, mechanical properties and thermal expansion coefficient of the prepared porous SiC ceramics. It was shown that at the sintering temperature of 1200 °C, the highest porosity of the samples can reach 70.42% when the H₃PO₄ content is 25 wt%, and their bending strength reaches 36.11 MPa at room temperature when the H₃PO₄ content is 15 wt%. In addition, the porous SiC ceramics show good high-temperature stability with a bending strength of 42.05 MPa at 1000 °C and the thermal expansion coefficient of 3.966 × 10⁻⁶/°C.     

Fabrication and properties of SiC porous ceramics using a polyurethane preparation process

SiC porous ceramics can be prepared by introducing the polyurethane preparation method into the production process of ceramic biscuits, followed by sintering at 1300?°C for 2?h under N₂ flux after the cross-linking of polycarbosilane at 220?°C for 4?h in air. The microstructures, mechanical properties and infiltrations of the SiC porous ceramics are investigated in detail. The best dispersal effect comes from the SiC slurry with xylene as the solvent and a mixture of Silok®7096 (1?wt%) and Anjeka®6041 (4?wt%) as the dispersant. The compressive strength of SiC porous ceramics with high porosity (69.53%) reaches 16.9?MPa. The heat treatment can increase infiltration, the rate of which (4.296?×?10^?7 mm²) after the heat treatment at 750?°C in air is approximately two times faster than that before the heat treatment. The SiC porous ceramics fabricated in this study will have potential application in active thermal protection systems.     

SiC encapsulated Fe@CNT ultra-high absorptive shielding material for high temperature resistant EMI shielding

Carbon nanotubes (CNTs) decorated with ferromagnetic materials have promising potential in electromagnetic interference (EMI) shielding applications. In this work, CNT sponges with increasing density were fabricated by filling them with magnetic Fe nanowires of mutative filling ratios via chemical vapor deposition (CVD). Results indicated that Fe@CNT composites with the highest density endowed the most remarkable average SE_T value of 70.01 dB (more than 99.99999% absorption), showing an ultra-high EMI shielding performance. However, the susceptibility to oxidation of carbon materials has restricted its further development in high-temperature EMI shielding applications. Therefore, the Fe@CNT composites were encapsulated by silicon carbide (SiC) with satisfactory oxidation resistance. Thereafter, the average SE_T value of SiC encapsulated a higher density Fe@CNT sponge decreased to an adequate value of 36.48 dB due to the huge loss of electrical conductivity. However, the SE_T value of it only dropped by about 1.20 as the temperature went up from 25 to 600 °C, demonstrating an excellent stability under high temperature conditions. As a proof of concept, the Fe@CNT/SiC composites with adequate EMI shielding performance and satisfactory oxidation resistance suggest its prospect in high temperature resistant EMI shielding.     

Oxidation of 3D-printed SiC in air and steam environments

The high-temperature oxidation of additively manufactured and chemically vapor infiltrated (3D-printed SiC) has been compared to chemical vapor deposited (CVD) SiC. 100-h isothermal exposures were conducted at 1425° and 1300°C at 1 atm under both dry air and steam environments. A SiC reaction tube was utilized to reduce silica volatility. After steam oxidation at 1425° and 1300°C, on the 3D-printed SiC surface, which was intrinsically rougher than the CVD surface, scales were 70%–90% thicker at the convex regions compared to concave/flat regions. In the convex regions, large cracks perpendicular to the oxidizing interface were observed. After dry air oxidation, scale thicknesses were comparable between 3D-printed SiC and CVD SiC, regardless of geometry. Finite element modeling, conducted to elucidate the relationship between SiC geometry and ß- to α-cristobalite transformation stress, determined cristobalite transformation tensile stresses to be on the order of 10³ MPa during cool down, assuming a 6 vol% reduction. Compared to flat SiC substrates, tensile transformation stresses were elevated at concave regions and relaxed at convex regions. Combined with specimen mass gain (accounting for the rougher surface) of 3D-printed SiC being 15%–32% higher for 3D-printed SiC after 1300°C and 1425°C steam oxidation, the work presented concludes that the increased oxidation of 3D-printed SiC is primarily caused by tensile hoop stresses driven by oxidation volume expansion. Lastly, the efficacy of the 3D-printing method is demonstrated through the production of tristructural isotropic imbedded 3D-printed SiC fuel forms.     

Facile preparation of morph-genetic SiC/C porous ceramic at low temperature by processed bio-template

A porous morph-genetic SiC/C ceramic material was fabricated using biomass-derived C template, Si powder, and Fe(NO₃)₃·9H₂O as the starting materials. The effects of heating temperature, and catalyst/Si mole ratio on the formation of SiC/C ceramic were investigated. In addition, the pore size distribution was obtained through pore size analysis, and the determination of oxidation resistance of SiC/C ceramics and C template was carried out by thermogravimetric analysis. The results show that copious amounts of SiC nanowires, which were distributed on the surfaces and interiors of the C template holes, were formed at 1300 °C with 4 wt% Fe as catalyst. The SiC nanowires significantly affected the oxidation resistance and microporous structures of the prepared materials. Moreover, a possible formation mechanism for the porous SiC/C ceramic was determined.     

Influence of bonding phases on properties of in-situ bonded porous SiC membrane supports

Porous SiC ceramic membrane supports are widely employed in a wide variety of high-temperature applications, such as hot flue gas filtration, porous burners and molten metal filters. Herein, SiC supports, with a porosity of ~37%, were prepared by using low-temperature bonding techniques and the influence of different bonding phases, such as mullite, cordierite and glass, on ambient-temperature flexural strength, hot modulus of rupture (HMOR), thermal shock resistance and oxidation resistance were systematically investigated. The results reveal that the glass-bonded SiC (GBSC) support exhibited the highest ambient-temperature flexural strength of 33.6 MPa, whereas the flexural strength of mullite-bonded SiC (MBSC) and cordierite-bonded SiC (CBSC) supports ranged from 22 to 25 MPa. However, the presence of glass phase deteriorated the high-temperature properties of the support. MBSC support rendered superior mechanical strength at high temperature and self-strengthening in a certain temperature range, such as HMOR improved 47.5% at 900 °C, but HMOR of glass-bonded support was only 57.4% of the ambient-temperature strength. Moreover, MBSC and CBSC supports exhibited better thermal shock resistance than GBSC supports and the critical temperature difference of water quenching for MBSC supports was ~200 °C higher than GBSC supports. In addition, MBSC support rendered superior oxidation resistance and exhibited a weight gain rate of ~0.1% at 1150 °C for 24 h, which is 54.4% and 42.2% lower than CBSC and GBSC supports, respectively.     

Significant improvement of high-temperature oxidation resistance of HfC/SiC ceramic nanocomposites with the incorporation of a small amount of boron

Oxidation behavior of boron-containing HfC/SiC nanocomposites (SHBC) at temperatures up to 1500 °C and with exposure time up to 100 h was investigated. Two strategies to improve the oxidation resistance of the HfC/SiC ceramics are proposed. First concept involves the incorporation of a small amount of boron (ca. 0.6 wt.%) into the nanocomposite via a single-source-precursor approach, which contributes significantly to the enhancement of its oxidation resistance. Parabolic oxidation rate constants of 10⁻³ to 10^-4 mg²/(cm⁴ h) at 1300−1500 °C were measured for SHBC and were several orders of magnitude lower than those recorded for boron-free HfC/SiC. The second improvement concept is realized via passivation of the samples upon short-term oxidation at 1400 °C, providing an excellent oxidation resistance over a wide temperature range. This is a crucial step especially when considering the poor oxidation behavior of HfC and the sluggish formation of protective silica scale at moderate temperatures.     

Processing and properties of porous SiC ceramics prepared by yttrium aluminum garnet infiltration

Oxide bonded porous SiC ceramics were synthesized by infiltrating a liquid precursor of yttrium aluminum garnet into porous powder compact of SiC followed by sintering at 1300‐1500°C in air. Infiltration rate was estimated using weight gain by the liquid precursor sol into porous SiC powder compact as a function of time and was explained by Darcy's and Ficks's laws. The effects of SiC particle sizes and sintering temperatures on the formation of bonding phases, microstructure, SiC oxidation degree, flexural strength, porosity, and pore size distribution of porous SiC ceramics were studied. Various crystalline oxide phases were detected by XRD analysis. Depending on the starting SiC powder sizes and sintering temperatures, the porosity of the final ceramics varied nearly in the range of ~29‐41 vol. % with the variation of average pore diameter between ~5 and 30 μm. Flexural strength varied from 41 to 8 MPa depending on porosity. The effect of corrosion on oxide bond phases was investigated in strong acidic and basic medium at 90°C. The ceramics showed better corrosion resistance in acidic medium compared to basic medium. In basic medium, significant reduction in flexural strength (~42%) was arisen.     

Influence of additive contents on the properties of SiC ceramic membranes and their performance in oil-water separation

The high processing cost is the key challenge for the economic industrial use of SiC membrane The aim of this research was to fabricate mullite bonded porous SiC ceramic membrane at low temperature from novel combinations of fly ash and alumina (FA) in weight ratio 44.5:55.5 as sintering additives. The influences of FA and pore former content on the porosity, morphology, crystalline phase composition, mechanical performance, permeability properties were investigated. The membrane prepared at 1300°C using 20 wt% FA showed pure water permeability 3690 Lm⁻²h⁻¹bar⁻¹ and exhibited high oil removal efficiency of ∼ 98% from the synthetic oil-water emulsion having oil concentration of 1000 mg/L. The corrosion behaviour of silicon carbide membrane in the strong acid and alkali solution and its mechanism were investigated. The utilization of fly ash successfully reduced the raw material cost and sintering temperature and the use of alumina reduced the amount of oxidation of SiC as well as increased the amount of mullite bond phase which resulted excellent mechanical strength to the final ceramics.     

Temperature-dependent mechanical and oxidation behavior of in situ formed ZrN/ZrO2-containing Si3N4-based composite

In this work, Si₃N₄ and Zr(NO₃)₄ were used as raw materials to prepare ZrN/ZrO₂-containing Si₃N₄-based ceramic composite. The processing, phase composition, and microstructure of the composite were investigated. Hardness and fracture toughness of the ceramics were evaluated via Vickers indentation in Ar at 25°C, 300°C, 600°C, and 900°C. During spark plasma sintering, Zr(NO₃)₄ was transformed into tetragonal ZrO₂, which further reacted with Si₃N₄, resulting in the formation of ZrN. The introduction of ZrN enhanced the high-temperature mechanical properties of the composite, and its hardness and fracture toughness reached 13.4 GPa and 6.1 MPa·m^1/2 at 900°C, respectively. The oxidation experiment was carried out in air at 1000°C, 1300°C, and 1500°C for 5 h. It was shown that high-temperature oxidation promoted the formation and growth of porous oxide layers. The microstructure and phase composition of the formed oxide layers were investigated in detail. Finally, it was identified that the obtained composite exhibited a higher thermal diffusivity than that of monolithic Si₃N₄ in the temperature range of 100°C–1000°C.     

Spheroidization of SiC powders and their improvement on the properties of SiC porous ceramics

Spherical SiC powders were prepared at high temperature using commercial SiC powders (4.52 µm) with irregular morphology. The influence of spherical SiC powders on the properties of SiC porous ceramics was investigated. In comparison with the as-received powders, the spheroidized SiC powders exhibited a relatively narrow particle size distribution and better flowability. The spheroidization mechanism of irregular SiC powder is surface diffusion. SiC porous ceramics prepared from spheroidized SiC powders showed more uniform pore size distribution and higher bending strength than that from as-received SiC powders. The improvement in the performance of SiC porous ceramics from spheroidized powder was attributed to tighter stacking of spherical SiC particles. After sintering at 1800 °C, the open porosity, average pore diameter, and bending strength of SiC porous ceramics prepared from spheroidized SiC powder were 39%, 2803.4 nm, and 66.89 MPa, respectively. Hence, SiC porous ceramics prepared from spheroidized SiC powder could be used as membrane for micro-filtration or as support of membrane for ultra/nano-filtration.     

Efficient fabrication of carbon/silicon carbide composite for electromagnetic interference shielding applications

Ceramic matrix composites are typically prepared by a costly, time-consuming process under severe conditions. Herein, a cost-effective C/SiC composite was fabricated from a silicon gel-derived source by Joule heating. The β-SiC phase was generated via carbothermal reduction, and the carbon fabric showed a well-developed graphitic structure, promoting its thermal and anti-oxidation stabilities. Owing to the excellent dielectric loss in carbon fabric, SiC and SiO₂ as well as the micropore structure of the ceramic matrix, the absolute electromagnetic interference shielding (EMI) effectiveness (SSE/t) reached 948.18 dB?cm²?g^-1 in the X-band, exhibiting an excellent EMI SE. After oxidation at 1000 °C for 10 h in the air, the SSE/t of the composite was only reduced to 846.02 dB?cm²?g^-1. The C/SiC composite promises the efficient fabrication of high-temperature resistant materials for electromagnetic shielding applications.     

Mechanical,thermal, and dielectric properties of SiCf/SiC composites reinforced with electrospun SiC fibers by PIP

Electrospun unidirectional SiC fibers reinforced SiC_f/SiC composites (e-SiC_f/SiC) were prepared with ∼10% volume fraction by polymer infiltration and pyrolysis (PIP) process. Pyrolysis temperature was varied to investigate the changes in microstructures, mechanical, thermal, and dielectric properties of e-SiC_f/SiC composites. The composites prepared at 1100 °C exhibit the highest flexural strength of 286.0 ± 33.9 MPa, then reduced at 1300 °C, mainly due to the degradation of electrospun SiC fibers, increased porosity, and reaction-controlled interfacial bonding. The thermal conductivity of e-SiC_f/SiC prepared at 1300 °C reached 2.663 W/(m∙K). The dielectric properties of e-SiC_f/SiC composites were also investigated and the complex permittivities increase with raising pyrolysis temperature. The e-SiC_f/SiC composites prepared at 1300 °C exhibited EMI shielding effectiveness exceeding 24 dB over the whole X band. The electrospun SiC fibers reinforced SiC_f/SiC composites can serve as a potential material for structural components and EMI shielding applications in the future.     

Effect of carbon content on electrical,thermal, and mechanical properties of porous SiC ceramics with B4C and C additives

The electrical, thermal, and mechanical properties of porous SiC ceramics with B₄C-C additives were investigated as functions of C content and sintering temperature. The electrical resistivity of porous SiC ceramics decreased with increases in C content and sintering temperature. A minimal electrical resistivity of 4.6 × 10^?2 Ω·cm was obtained in porous SiC ceramics with 1 wt% B₄C and 10 wt% C. The thermal conductivity and flexural strength increased with increasing sintering temperature and showed maxima at 4 wt% C addition when sintered at 2000 °C and 2100 °C. The thermal conductivity and flexural strength of porous SiC ceramics can be tuned independently from the porosity by controlling C content and sintering temperature. Typical electrical resistivity, thermal conductivity, and flexural strength of porous SiC ceramics with 1 wt% B₄C-4 wt% C sintered at 2100 °C were 1.3 × 10^?1 Ω·cm, 76.0 W/(m·K), and 110.3 MPa, respectively.     

Processing and properties of cordierite-silica bonded porous SiC ceramics

Cordierite-silica bonded porous SiC ceramics were fabricated by infiltrating a porous powder compact of SiC with cordierite sol followed by sintering at 1300–1400 °C in air. The porosity, average pore diameter and flexural strength of the ceramics varied 30–36 vol%, ~ 4–22 µm and ~ 13–38 MPa respectively with variation of sintering temperature and SiC particle sizes. In the final ceramics SiC particles were bonded by the oxidation-derived SiO₂ and sol-gel derived cordierite. The corrosion behaviour of sintered SiC ceramics was studied in acidic and alkaline medium. The porous SiC ceramics were observed to exhibit better corrosion resistance in acid solution.     

Electromagnetic wave absorbing properties of glucose-derived carbon-rich SiOC ceramics annealed at different temperatures

A kind of glucose-derived carbon-rich silicon oxycarbide (glucose-SiOC) nanocomposite with excellent electromagnetic wave absorbing performance is obtained via solvothermal method, and then pyrolyzed at high temperature (1300°C and 1400°C) under argon atmosphere. The structural evolutions and the electromagnetic wave absorbing capabilities of the nanocomposites have been systematically investigated. The resultant 3 mol/L glucose-SiOC ceramic exhibits a heterostructure, in which nanosized glucose-derived carbon and SiC particles decorate on amorphous SiOC network. Benefitting from the nanosized carbon, SiC particles and the heterostructure attributes, the 3 mol/L glucose-SiOC ceramic displays a strong electromagnetic wave-absorbing property. The minimum reflection coefficient of the 3 mol/L glucose-SiOC ceramic pyrolyzed at 1400°C reaches −27.6 dB at 13.8 GHz. The widest effective absorption bandwidth attains 3.5 GHz in Kμ-band. This work opens up a novel and simple route to fabricate polymer-derived ceramics with excellent electromagnetic wave-absorbing performance.     

Microstructure,thermophysical properties and oxidation resistance of SiCf/SiC–YSi2–Si composite fabricated through reactive melt infiltration

As an ideal component material for advanced aeroengines, SiC composite faces severe challenges of high temperatures and oxidation. Here, a high-densification SiC_f/SiC–YSi₂–Si composite was prepared through combining PIP with RMI of Si–13 at% Y alloy to achieve enhanced performance at high temperatures. Based on the analysis of the microstructure and thermophysical properties, it found that the introduction of the highly crystalline Si–Y alloy can improve the high-temperature thermal conductivity of the composite through phonon and electron conduction. In addition, Y migrates to the surface and forms yttrium silicate with increasing oxidation temperature, which facilitates the excellent long-term oxidation resistance of the composite at 1200–1300 °C. Thus, the composite retained its high strength (89.15% and 86.84%) after oxidation at 1200 °C and 1300 °C for 100 h. The experimental results clearly demonstrate that the introduction of the Si–Y alloy is an effective way of preparing high-performance SiC composites.     

Effect of fluorine-containing additive on the synthesis and sintering of compositions from natural raw materials in the “cordierite –mullite” system

The influence of the small addition of topaz on the processes of mineral formation in the “mullite–cordierite” system with a variable ratio of cordierite and mullite has been investigated. For this purpose, a series of experiments with different compositions of the initial mixtures, that is, with predominance of cordierite over mullite (KM mixtures) and predominance of mullite over cordierite (MK mixtures), has been performed. The addition of topaz in the form of topaz concentrate has been introduced in the amount of 1% by the weight of the investigated mixtures. The samples have been fired at various temperatures, that is, samples from KM mixtures (at a temperature of 1100–1300?°C) and samples from MK mixtures (at a temperature of 1400–1550?°C. The activating effect of topaz on mineral formation and sintering processes is determined by complex influence of fluoride products of topaz thermal decomposition. These reactively gaseous fluorides partially activate the solid-phase mass transfer processes and then reduce the viscosity of high-temperature melt formed during firing that intensifies the processes of ceramic matrix consolidation.Porous polycrystalline cordierite–mullitе–corundum ceramics from the KM mixtures, which contains 70%–87% cordierite, 3%–12% mullite, and 4%–11% corundum with water absorption of 3.5%–8% and bulk density of 2.10%–2.12?g/cm³ at the firing temperature of 1300?°C, has been developed. Mullite ceramics with notably corundum content (not more than 8%) from the MK mixtures with various density degrees at the firing temperature of 1500–1550?°C, porous ceramics with water absorption of 3%–11%, and dense ceramics with water absorption of less than 1% have been produced.