研究目的
To investigate the effects of porosity and immersion-pyrolysis times on the microstructures and dielectric properties of porous SiC/Si3N4 ceramics for microwave absorbing applications.
研究成果
The immersion-pyrolysis method successfully synthesized SiC nanotubes on porous Si3N4 matrices, increasing β-SiC and free C contents with dipping times. This led to vibration and loss peaks in dielectric properties at specific frequencies (e.g., 12.9 GHz and 14.7 GHz), with reflectivity values of -7 dB to -10 dB indicating 80%-90% electromagnetic wave attenuation. Ceramics with 40 wt% benzoic acid exhibited the best dielectric properties, including high loss tangent, low reflectivity, and wide absorbing band, making them suitable for efficient microwave absorbing applications. Future studies could focus on optimizing porosity and pyrolysis conditions for enhanced performance.
研究不足
The study is limited to specific porosity ranges (up to 48.7%) and immersion-pyrolysis cycles (maximum of three times). The formation of SiC nanotubes was noted to be possibly due to uneven heating during pyrolysis, which may not be fully controlled. The dielectric properties were measured only up to 18 GHz, and the effects of higher frequencies or other environmental conditions were not explored. Optimization of process parameters for industrial scalability may require further investigation.
1:Experimental Design and Method Selection:
The study used polysilazane immersion-pyrolysis to synthesize SiC nanotubes on porous Si3N4 matrices. The method involved vacuum immersion of porous Si3N4 matrices in polysilazane followed by pyrolysis at 1100°C, with up to three immersion-pyrolysis cycles. The design aimed to adjust impedance mismatch and enhance absorbing properties by introducing SiC grains into the porous ceramics matrix.
2:Sample Selection and Data Sources:
Porous Si3N4 matrices were prepared using α-Si3N4 powder, Y2O3, Al2O3, and benzoic acid as a pore-forming agent (0–50 wt%). Samples were formed by isostatic pressing and sintered at 1700°C under nitrogen atmosphere. Dielectric properties were measured in the frequency range of 2–18 GHz.
3:List of Experimental Equipment and Materials:
Materials included α-Si3N4 powder (0.5 μm particle size, purity >93%), Y2O3 (purity >99%), Al2O3 (purity >99%), benzoic acid (purity >99%), polysilazane (liquid), paraffin wax (as binder), Si3N4 grinding balls, and absolute methanol. Equipment included ball mill, drying oven, isostatic press, sintering furnace, XRD (EVO-18, CARL ZEISS SMT Ltd), SEM (JSM-6380LA), TEM (JEM-1200EX), and vector network analyzer (VNA, 5244A).
4:5 μm particle size, purity >93%), Y2O3 (purity >99%), Al2O3 (purity >99%), benzoic acid (purity >99%), polysilazane (liquid), paraffin wax (as binder), Si3N4 grinding balls, and absolute methanol. Equipment included ball mill, drying oven, isostatic press, sintering furnace, XRD (EVO-18, CARL ZEISS SMT Ltd), SEM (JSM-6380LA), TEM (JEM-1200EX), and vector network analyzer (VNA, 5244A). Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Mixed powders were ball-milled for 15 min, dried, and formed into green specimens by isostatic pressing under 80 MPa for 200 s. Pore-forming agent was removed at 200°C before sintering at 1700°C for 120 min under nitrogen. Porous matrices were immersed in polysilazane under vacuum for 30 min and pyrolyzed at 1100°C, with up to three cycles. Porosity was measured by Archimedes' method, phases identified by XRD, microstructures observed by SEM and TEM, and dielectric properties measured using VNA with samples mixed with paraffin wax (weight ratio 5:2).
5:2). Data Analysis Methods:
5. Data Analysis Methods: Dielectric properties were analyzed using complex dielectric constant (ε = ε′ - jε″), loss tangent (tan ξ = ε″/ε′), reflectivity (R) calculated from transmission line theory, and electromagnetic attenuation coefficient (α) derived from equations based on Debye theory. XRD patterns were compared to JCPDS standards for phase identification.
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X-Ray Diffraction
EVO-18
CARL ZEISS SMT Ltd
Used to identify the phases in the ceramic samples by analyzing diffraction patterns.
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Scanning Electron Microscope
JSM-6380LA
Used to observe the microstructures of the ceramic specimens on fracture surfaces.
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Transmission Electron Microscopy
JEM-1200EX
Used for detailed microstructural analysis, including observation of SiC nanotubes.
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Vector Network Analyzer
5244A
Used to measure dielectric properties at frequencies from 2 to 18 GHz using coaxial transmission reflection method.
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Polysilazane
Guangzhou Honghai Chemical Technology Co.
Used as a precursor for synthesizing SiC nanotubes through immersion and pyrolysis.
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α-Si3N4 powder
Shanghai Macklin Biochemical Technology Co., Ltd
Used as the main matrix material for preparing porous Si3N4 ceramics.
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Y2O3
Shanghai Macklin Biochemical Technology Co., Ltd
Used as a sintering aid to enhance the sintering process and form Y-Si-O-N compounds.
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Al2O3
Shanghai Macklin Biochemical Technology Co., Ltd
Used as a sintering aid in the ceramic matrix preparation.
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Benzoic acid
Sinopharm Chemical Reagent Co., Ltd
Used as a pore-forming agent to create porosity in the Si3N4 matrices.
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Paraffin wax
Used as a binder in dielectric property measurements to hold samples and act as a wave-transparent material.
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