研究目的
Investigating the electrochemical synthesis of SiC with the aims of optimizing precursor composition, understanding the cathodic reactions, and correlating product morphology with process conditions. A further goal has been to examine the nitridation behavior of the electrochemically prepared SiC and to identify the composition and morphology of the product.
研究成果
Silicon carbide with nanowire morphology was successfully synthesized from SiO2/graphite mixtures in a CaCl2 melt. The process requires an optimized combination of precursor composition, applied voltage, and polarization duration. The electrochemically made SiC can be nitrided to form Si2N2O with retained nanowire morphology, indicating potential applications in energy and other sectors.
研究不足
The process requires optimization of precursor composition, applied voltage, and duration of polarization to achieve pure SiC. Deviations from optimal conditions lead to incomplete reaction or formation of by-products.
1:Experimental Design and Method Selection:
The FFC-Cambridge process was applied for the synthesis of SiC from mixtures of SiO2 and graphite. Porous disks were prepared by sintering in inert atmosphere and subjected to electro-deoxidation in molten CaCl2 at 1173 K under a range of experimental conditions.
2:Sample Selection and Data Sources:
Powders of SiO2 and graphite were mixed in molar ratios of 1:
3:5,
1, and 1:1.5. The mixtures were made into slurries, ground in a ball mill, dried, pressed into disks, and sintered.
4:The mixtures were made into slurries, ground in a ball mill, dried, pressed into disks, and sintered. List of Experimental Equipment and Materials:
3. List of Experimental Equipment and Materials: Anhydrous CaCl2, high-density graphite rod as anode, Ni coil as cathode, Ni/NiO assembly for potential monitoring, X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), hot extraction method for residual oxygen content determination.
5:Experimental Procedures and Operational Workflow:
Electro-deoxidation was carried out at different applied voltages and durations. The products were rinsed with distilled water and dried. The crystallographic phases, microstructures, and elemental compositions were identified.
6:Data Analysis Methods:
XRD, SEM, EDX, TEM, and hot extraction method were used for data analysis.
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Scanning electron microscope
FEI Nova NanoSem 450
FEI
Microstructure analysis
-
Energy-dispersive X-ray spectrometer
Bruker X Flash 6I100
Bruker
Elemental composition analysis
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Transmission electron microscope
FEI Tecnai G2-F20
FEI
Nanostructure analysis
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SiO2
99% purity, 0.5–5 μm
Sigma Aldrich
Precursor material for SiC synthesis
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Graphite
<20 μm
Sigma Aldrich
Precursor material for SiC synthesis
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CaCl2
Sigma Aldrich
Molten salt electrolyte
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High-density graphite rod
Tokai Carbon, UK
Anode in electrolytic cell
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X-ray diffraction analyzer
Philips PW 1830
Philips
Identification of crystallographic phases
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Hot extraction analyzer
ELTRA ONH 2000
ELTRA
Residual oxygen content determination
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Thermogravimetric and differential scanning calorimetric analyzer
SDT Q600
TA Instruments
Thermokinetic behavior analysis
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