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.     

Improving the electrical and microwave absorbing properties of Si3N4 ceramics with carbon nanotube fibers

Carbon nanotube fibers (CNTFs) reinforced Si₃N₄ ceramics has been prepared by incorporating CNTF preforms into ceramic precursor and followed by the sintering process. A SiC interface layer is formed due to the chemical reaction between Si and CNTs, leading to a good bonding between CNTs and Si₃N₄ matrix. Due to the ceramic deposition, the oxidation resistance is increased of 200 °C. Furthermore, the CNTs have well orientation and high-volume distribution (7 wt%) in the hybrid composites. Obvious improvements of the electrical conductivity (up to 103 S/m) and the microwave absorbing performance (up to 6 dB at 15 GHz) are obtained for the composites containing CNTFs. Our work provides a meaningful way to fabricate multifunctional ceramics possessing high electrical and microwave absorbind properties.     

Microstructures,dielectric response and microwave absorption properties of polycarbosilane derived SiC powders

Carbon-rich SiC powders with high dielectric loss were prepared via pyrolysis of polycarbosilane (PCS). The effects of pyrolysis temperature on microstructures, dielectric response and microwave absorption properties in X-band (8.2–12.4 GHz) of PCS-derived SiC powders were investigated. The PCS-derived SiC powders are mainly composed of SiC nanocrystal, turbostratic carbon and amorphous phase (SiC and/or C). The size of SiC nanocrystals and the graphitization degree of carbon both increase with the elevation of pyrolysis temperature. Furthermore, the residual carbon is transformed from amorphous into turbostratic structure with a phenomenon of regional enrichment. Moreover, the relative complex permittivity increases notably with the higher pyrolysis temperature. Meanwhile, the dielectric loss tangent increases from 0.19 to 0.57, while the microwave impedance decreases from 73.20 to 53.58. The optimal reflection loss of ?35 dB for PCS-derived SiC powders is obtained when the pyrolysis temperature is 1500 °C, which exhibits a great application prospect in microwave absorbing materials.     

Dielectric and microwave absorption properties of polymer derived SiCN ceramics annealed in N2 atmosphere

Porous SiCN ceramics were successfully fabricated by pyrolysis of a kind of polysilazane. The effects of annealing temperature on the microstructure evolution, direct-current electrical conductivity, dielectric properties, and microwave absorption properties of SiCN in the frequency range 8.2–12.4 GHz (X-band) were investigated. With the increase of annealing temperature, SiC, Si₃N₄ and free carbon nanodomains are gradually formed in the SiCN. Both the SiC and free carbon nanodomains lead to the increases of the complex relative permittivity and loss tangent of SiCN. With the increase of the annealing temperature, the average real permittivity, imaginary permittivity and loss tangent increase from 4.4, 0.2 and 0.05 to 13.8, 6.3 and 0.46, respectively. The minimum reflection coefficient and the frequency bandwidth below −10 dB for SiCN annealed at 1500 °C are −53 dB and 3.02 GHz, indicating good microwave absorption properties.     

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.     

Influence of different matrices on the mechanical and microwave absorption properties of SiC fiber-reinforced oxide matrix composites

Fiber-reinforced ceramic matrix composites have excellent mechanical and microwave absorption properties, but still present considerable challenges. We prepared a SiC_f/mullite-SiO₂ composite (composite A) and a SiC_f/Al₂O₃-SiO₂ composite (composite B) by a precursor infiltration and sintering (PIS) process. Compared with the composite B, the composite A was easily densified. The flexural strength of the composite A reached 216 MPa, whereas that of the composite B was 159 MPa. The imaginary part of permittivity for composites A and B, which was determined by the contents of matrix and porosity, varied in the range of 2.5–3.5 and 3.6–5, respectively. The microwave absorption properties of the composite A were significantly enhanced in the range of 8.2–12.4 GHz. The results indicate that an optimal reflection loss of ?44 dB was reached at 12 GHz with a thickness of 2.9 mm for the composite A. These SiC fiber-reinforced oxide matrix materials have promising applications in microwave absorption, especially at high temperatures.     

Effect of SiBCN content on the dielectric and EMW absorbing properties of SiBCN-Si3N4 composite ceramics

Siliconboron carbonitride ceramics (SiBCN) were introduced into porous Si₃N₄ substrates via low pressure chemical vapor deposition and infiltration from SiCl₃CH₃-NH₃-BCl₃-H₂-Ar system. To improve the electromagnetic wave(EMW) absorbing properties, the molar ratio, n_CH3SiCl3/(n_NH3 + n_BCl3), was increased based on thermodynamics analysis. The results show that nanosized silicon carbide crystals and free carbon dispersed uniformly in the amorphous SiBCN phase, resulting in suitable dielectric properties and improved absorption capabilities of SiBCN-Si₃N₄ ceramics. Additionally, with increasing SiBCN ceramics loading, the amount of nanocrystals and interface between nanocrystals and amorphous SiBCN phase increased, leading to enhanced polarization and dielectric loss of the composite ceramics. When SiBCN content was up to 3.64 wt%, the electromagnetic reflection coefficient (RC) of SiBCN-Si₃N₄ composite ceramics reached ?40 dB (>99.97% absorbing) with the effective electromagnetic absorbing bandwidth of 3.64 GHz in the X-band. This study makes it possible to fabricate SiBCN-based composite materials with excellent EMW absorbing properties at a low temperature.     

Dielectric,electromagnetic absorption and interference shielding properties of porous yttria-stabilized zirconia/silicon carbide composites

SiC was infiltrated into porous yttria-stabilized zirconia (YSZ) felt by chemical vapor infiltration (CVI), and continuous SiC matrix layer was formed around YSZ fibre. When 86.9 wt.% SiC is introduced into the porous YSZ felt, the mean values of the real part of the permittivity and dielectric loss tangent of porous YSZ felt increase from 1.16 and 0.007 to 8.2 and 1.31, respectively. The electromagnetic interference (EMI) shielding efficiency (SE) increases from 0.069 dB to 16.2 dB over the frequencies ranging from 8.2 GHz to 12.4 GHz. The reflection loss of the composites with a thickness of 5 mm at 8–18 GHz is smaller than ?6.5 dB, and the bandwidth below ?10 dB is 5 GHz at room temperature, which increases to 5.9 GHz at 800 °C. The considerable increases in EMI SE and microwave absorption properties are attributed to the formation of continuous SiC matrix layer composed of SiC nanocrystals in the porous YSZ felt, which is beneficial for the production of induced electric current and the enhancement of dielectric loss.     

Low-temperature preparation of Si3N4 whiskers bonded/reinforced SiC porous ceramics via foam-gelcasting combined with catalytic nitridation

Porous α-Si₃N₄ whiskers bonded/reinforced SiC (Si₃N_4(w)/SiC) ceramics were successfully prepared at as low as 1473 K for 2 h, via a combined foam-gelcasting and catalytic nitridation route using commercial Si and SiC powders containing some Fe impurity as the main raw materials. Small pores (0.03–5 μm) left by the packing of raw material particles and interlocking of in-situ formed Si₃N₄ whiskers coexisted with large ones (8–400 μm) resultant mainly from the foaming process. The impurity Fe from the raw materials Si and SiC acted as an internal catalyst, accelerating the nitridation of Si by increasing the bond length and weakening the bond strength in the N₂ molecules adsorbed on it. As-prepared Si₃N_4(w)/SiC porous ceramics contained 71.53% porosity and had flexural and compressive strengths of 5.60 ± 0.69 MPa and 12.37 ± 1.05 MPa, respectively.     

Porous SiC ceramics with dendritic pore structures by freeze casting from chemical cross-linked polycarbosilane

In this study, a commercial polycarbosilane (PCS) and divinylbenzene (DVB) were used as the preceramic polymer precursor and crosslinking agent, respectively to form porous silicon carbide (SiC) ceramics by freeze casting DVB/camphene/PCS solutions. Porous silicon carbide (SiC) with a dendritic pore structure and connecting bridges was obtained after pyrolysis at 1200 °C. The effects of DVB and PCS content on the rheological properties of the solution and the morphological characteristics and the compressive strengths of SiC ceramics were investigated. The use of DVB and the resulting chemical cross-linking yielded modified pore characteristics and much lower oxygen content in pyrolyzed SiC compared to the conventional thermal curing method. A compressive strength of 18.7 MPa was obtained for pyrolyzed SiC prepared with 20 wt% PCS and a 0.2 DVB/PCS mass ratio.     

Dielectric properties of Si3N4–SiCN composite ceramics in X-band

Si₃N₄–SiCN composite ceramics were successfully fabricated through precursor infiltration pyrolysis (PIP) method using polysilazane as precursor and porous Si₃N₄ as preform. After annealed at temperatures varying from 900 °C to 1400 °C, the phase composition of SiCN ceramics, electrical conductivity and dielectric properties of Si₃N₄–SiCN composite ceramics over the frequency range of 8.2–12.4 GHz (X-band) were investigated. With the increase of annealing temperature, the content of amorphous SiCN decreases and that of N-doped SiC nano-crystals increases, which leads to the increase of electrical conductivity. After annealed at 1400 °C, the average real and imaginary permittivities of Si₃N₄–SiCN composite ceramics are increased from 3.7 and 4.68 × 10^?3 to 8.9 and 1.8, respectively. The permittivities of Si₃N₄–SiCN composite ceramics show a typical ternary polarization relaxation, which are ascribed to the electric dipole and grain boundary relaxation of N-doped SiC nano-crystals, and dielectric polarization relaxation of the in situ formed graphite. The Si₃N₄–SiCN composite ceramics exhibit a promising prospect as microwave absorbing materials.     

Electrical conductivity,dielectric and microwave absorption properties of graphene nanosheets/magnesia composites

Herein, a novel microwave absorbing material with Graphene nanosheets (GNSs) as microwave absorbing filler and magnesia (MgO) as matrix were prepared by hot-pressing sintering. The composites were highly dense with a homogeneous distribution of GNSs. Electrical conductivity, dielectric and microwave absorption properties in X-band were investigated. The results revealed that the electrical conductivity of the GNSs/MgO composites showed a typical percolation-type behavior with a percolation threshold of 3.34 vol%. With GNSs content increased to 3 vol%, the real permittivity, imaginary permittivity and dielectric loss tangent of the composites increased from ～9, ～0 and ～0 to 26–43, 23–28 and 0.55–0.96, respectively. By adjusting the GNSs content, thickness and frequency, the 2.5 vol% GNSs/MgO composite shows the minimum reflection loss of ?36.5 dB at 10.7 GHz and the reflection loss below ?10 dB (90% absorption) ranges from 9.4 to 11.4 GHz with 1.5 mm thickness, exhibiting excellent microwave absorption properties.     

Synthesis and microwave absorption properties of SiC nanowires reinforced SiOC ceramic

Silicon carbide nanowires (SiC NWs) reinforced SiOC ceramics were fabricated through in situ growth of SiC NWs in SiOC ceramics by pyrolysis of polysiloxane. SiC NWs were in situ formed by the addition of ferrocene, the content of SiC NWs increased with the increases of annealing temperature and ferrocene content. Due to the formation of SiC NWs in the inter-particle pores of SiOC ceramics, the SiOC particles were bridged by SiC NWs, which led to the increase of electrical conductivity. With the increase of SiC NWs content, the real permittivity and the imaginary permittivity increased from 3.63 and 0.14 to 10.72 and 12.17, respectively, and the minimum reflection coefficient decreased from −1.22 dB to −20.01 dB, demonstrating the SiOC ceramics with SiC NWs had a superior microwave-absorbing ability.     

The dielectric and microwave absorption properties of polymer-derived SiCN ceramics

The polymer-derived SiCN ceramics were synthesized at different annealing temperature (900 ～ 1400 °C). The XRD, SEM, FT-IR, Raman and XPS were used to analyze the phase composition and microstructure. The result indicated that the crystallization degree and content of free carbon gradually improved with the increase of annealing temperature. The resistivity, dielectric and microwave absorption properties of the samples were studied at 2 ～ 18 GHz. The resistivity decreased gradually as the annealing temperature rose. The dielectric constant of sample decreased with the increase of frequency in 1 ～ 5 MHz. The existence of free carbon could improve the dielectric properties of polymer-derived SiCN ceramics at high frequency. The reflectance of the sample synthesized at 1100 °C was below ?10 dB (> 90% absorption) in a wide frequency range of 6 ～ 16 GHz and the maximum value of dielectric loss angle tangent was about 0.6 at 16 GHz.     

Microwave dielectric properties of low-temperature sinterable α-MoO3

The α-MoO₃ ceramics were prepared by uniaxial pressing and sintering of MoO₃ powder at 650 °C and their structure, microstructure, densification and sintering and microwave dielectric properties were investigated. The sintering temperature of α-MoO₃ was optimized based on the best densification and microwave dielectric properties. After sintering at 650 °C the relative permittivity was found to be 6.6 and the quality factor was 41,000 GHz at 11.3 GHz. The full-width half-maximum of the A_1g Raman mode of bulk α-MoO₃ at different sintering temperatures correlated well with the Qf values. Moreover, the sintered samples showed a temperature coefficient of the resonant frequency of ?25 ppm/°C in the temperature range from ?40 to 85 °C and they exhibited a very low coefficient of thermal expansion of ±4 ppm/°C. These microwave dielectric properties of α-MoO₃ will be of great benefit in future MoO₃ based materials and their applications.     

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.     

Corrosion behavior of porous silicon nitride ceramics in different atmospheres

The corrosion behavior of silicon nitride (Si₃N₄) ceramics with a porosity of 46% at 1200–1500 °C under different conditions including dry O₂, O₂ containing 20 vol% H₂O and Ar containing 20 vol% H₂O is compared. The results show that porous Si₃N₄ ceramics exhibit good oxidation resistance up to 1200 °C. Their corrosion behavior varies depending on the temperature and atmosphere. Water vapor can obviously affect the morphology of the reaction product and thus accelerate the corrosion rate due to its specific inward diffusion mechanism and devitrified effect at high temperature. In view of the reaction kinetics, it proceeds in a diffusion-controlled manner in dry O₂ while follows the parabolic-linear law at water-containing atmosphere. Furthermore, a new model considering both oxidation and volatilization reactions is established. These provide a baseline for expanding the application fields of non-oxide porous ceramics such as Si₃N₄ and silicon carbide (SiC) etc.     

Effect of pre-oxidation on the microstructure,mechanical and dielectric properties of highly porous silicon nitride ceramics

Highly porous Si₃N₄ ceramics have been fabricated via freeze casting and sintering. The as-sintered samples were pre-oxidized at 1200–1400 °C for 15 min. The effect of pre-oxidation temperature on the microstructure, flexural strength, and dielectric properties of porous Si₃N₄ ceramics were investigated. As the pre-oxidation temperature increased from 1200 °C to 1400 °C, firstly, the flexural strength of the pre-oxidized specimens remained almost constant at 1200 °C, and then decreased to 14.2 MPa at 1300 °C, but finally increased to 25.6 MPa at 1400 °C, while the dielectric constant decreased gradually over the frequencies ranging from 8.2 GHz to 12.4 GHz. This simple process allows porous Si₃N₄ ceramics to have ultra-low dielectric constant and moderate strength, which will be feasible in broadband radome applications at high temperatures.     

Co2O3 substitution effects on the structure and microwave dielectric properties of low-firing (Zn0.9Mg0.1)TiO3 ceramics

Low-firing (Zn_0.9Mg_0.1)_1?xCo_xTiO₃ (x = 0.02–0.10) (ZMC_xT) microwave dielectric ceramics with high temperature stability were synthesized via conventional solid-state reaction. The influences of Co₂O₃ substitution on the phase composition, microstructure and microwave dielectric properties of ZMC_xT ceramics were discussed. Rietveld refinement results show the coexistence of ZnTiO₃ and ZnB₂O₄ phases at x = 0.02–0.10. (Zn_0.9Mg_0.1)_1?xCo_xTiO₃ ceramic with x = 0.06 (ZMC_0.06T) obtains the best combination microwave dielectric properties of: ε_r = 21.58, Q × f = 53,948 GHz, τ_f = ? 54.38 ppm/°C. For expanding its application in LTCC field, 3 wt% ZnO-B₂O₃-SiO₂ (ZBS) and 9 wt% TiO₂ was added into ZMC_0.06T ceramic, great microwave dielectric properties were achieved at 900 °C for 4 h: ε_r = 26.03, Q × f = 34,830 GHz, τ_f = ? 4 ppm/°C, making the composite ceramic a promising candidate for LTCC industry.     

Process-tolerant pressureless-sintered silicon carbide ceramics with alumina-yttria-calcia-strontia

Process-tolerant SiC ceramics were prepared by pressureless sintering at 1850–1950 °C for 2 h in an argon atmosphere with a new quaternary additive (Al₂O₃-Y₂O₃-CaO-SrO). The SiC ceramics can be sintered to a > 94% theoretical density at 1800–1950 °C by pressureless sintering. Toughened microstructures consisting of relatively large platelet grains and small equiaxed grains were obtained when SiC ceramics were sintered at 1850–1950 °C. The presently fabricated SiC ceramics showed little variability of the microstructure and mechanical properties with sintering within the temperature range of 1850–1950 °C, demonstrating process-tolerant behavior. The thermal conductivity of the SiC ceramics increased with increasing sintering temperature from 1800 °C to 1900 °C due to decreases of the lattice oxygen content of the SiC grains and residual porosity. The flexural strength, fracture toughness, and thermal conductivity of the SiC ceramics sintered at 1850–1950 °C were in the ranges of 444–457 MPa, 4.9–5.0 MPa m^1/2, and 76–82 Wm^?1 K^?1, respectively.