研究目的
To explore the Joule heating action at the inter-particle region of a ceramic green pellet by introducing carbon nanotubes (CNTs) into samaria-doped ceria (SDC) to enhance electric current percolation, Joule heating, and densification during flash sintering.
研究成果
The addition of carbon nanotubes to SDC green pellets enhances densification and electrical conductivity during flash sintering due to improved electric current percolation and increased Joule heating. This results in higher shrinkage, larger grain sizes, and reduced grain boundary resistivity, suggesting a promising method for densifying electroceramics at lower temperatures.
研究不足
The study is limited to specific compositions (10 vol% CNT in SDC) and sintering conditions (850°C, 210 V/cm, 1A current). The mechanisms of flash sintering, particularly the role of CNTs, are not fully elucidated and require further experimental work. The presence of CNTs leads to their oxidation and removal during heating, which might affect reproducibility and scalability.
1:Experimental Design and Method Selection:
The study used flash sintering (electric field-assisted sintering) to densify SDC-CNT composites, focusing on the role of CNTs in enhancing Joule heating and electrical conductivity.
2:Sample Selection and Data Sources:
SDC powder (CeO2: 20 mol% Sm2O3) from Fuel Cell Materials, USA, and multiwalled CNTs synthesized by catalytic chemical vapor deposition were used. Composites with 10 vol% CNT were prepared.
3:List of Experimental Equipment and Materials:
Attrition mill with Teflon-lined jar, zirconia-yttria spheres, isopropyl alcohol, uniaxial and isostatic presses, dilatometer (Unitherm model 1161), AC power supply, multimeters (Fluke 8050A), impedance analyzer (Hewlett Packard 4192A), scanning electron microscope (JEOL JSM 6701F), thermogravimetric analyzer (Simultaneous Thermal Analysis 409E Netzsch), mass spectrometer (Thermostar GSD 320T1 Pfeiffer), X-ray diffractometer (Bruker-AXS D8 Advance).
4:Experimental Procedures and Operational Workflow:
Powders were attrition milled, pressed into pellets, and sintered in a dilatometer with AC electric fields at 850°C, current limited to 1A. Shrinkage, voltage, and current were monitored. Post-sintering, density was measured by Archimedes method, microstructure by SEM, and electrical properties by impedance spectroscopy.
5:1A. Shrinkage, voltage, and current were monitored. Post-sintering, density was measured by Archimedes method, microstructure by SEM, and electrical properties by impedance spectroscopy. Data Analysis Methods:
5. Data Analysis Methods: Impedance data were analyzed with special software for deconvolution; shrinkage and electrical resistance data were collected and compared between samples with and without CNTs.
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multimeter
Fluke 8050A
Fluke
Measured voltage and current during sintering.
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scanning electron microscope
JEOL JSM 6701F
JEOL
Observed microstructures of sintered specimens.
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X-ray diffractometer
Bruker-AXS D8 Advance
Bruker
Performed X-ray diffraction to check for phase changes.
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dilatometer
Unitherm model 1161
Anter
Used for measuring shrinkage/expansion during sintering and applying electric fields.
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power supply
custom-made AC power supply
Applied AC electric fields for flash sintering.
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impedance analyzer
Hewlett Packard 4192A
Hewlett Packard
Used for impedance spectroscopy to analyze electrical properties.
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simultaneous thermal analyzer
Simultaneous Thermal Analysis 409E
Netzsch
Conducted thermogravimetric analysis.
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mass spectrometer
Thermostar GSD 320T1
Pfeiffer
Analyzed gases evolved during thermal analysis.
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attrition mill
custom-made
Used for milling the powder mixtures.
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isostatic press
National Forge Co
Used for pressing pellets isostatically.
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zirconia-yttria spheres
1 mm diameter
Tosoh
Used as grinding media in attrition milling.
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platinum paste
ESL
Deposited on pellet surfaces for electrical measurements.
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