研究目的
To develop a new method for mass production of high-quality vertically oriented graphene nanostructures doped with nitrogen or silicon using ICP CVD combined with roll-to-roll technology, and to investigate the effects of various technological parameters on their morphology and composition.
研究成果
The ICP CVD roll-to-roll technology successfully enables mass production of high-quality VOG doped with nitrogen or silicon at lower temperatures. Key findings include the influence of deposition time and gas pressure on morphology, with nitrogen doping leading to tighter packing and silicon doping resulting in smoother surfaces. This method has potential applications in catalysis, Li-ion batteries, and supercapacitors.
研究不足
The study is limited to copper foil substrates and specific gas mixtures. The growth mechanism is complex and not fully understood, with challenges in controlling defects and uniformity over large areas. The technology may not be directly applicable to other substrates without optimization.
1：Experimental Design and Method Selection:
The study uses a novel ICP CVD system coupled with roll-to-roll technology for in-situ growth and doping of VOG on a moving copper foil substrate. Propane is used as the carbon precursor, with nitrogen or silane as dopants. Parameters like deposition time, gas partial pressure, and heating conditions are varied to study growth and doping mechanisms.
2：Sample Selection and Data Sources:
A copper foil substrate (99.8%, 35 μm thickness) is used. Gases include propane, argon, nitrogen, and silane from specified suppliers. Samples are prepared with different parameters as listed in Table
3：8%, 35 μm thickness) is used. Gases include propane, argon, nitrogen, and silane from specified suppliers. Samples are prepared with different parameters as listed in Table List of Experimental Equipment and Materials:
1. 3. List of Experimental Equipment and Materials: ICP CVD system with RF generator and matching block, roll-to-roll apparatus, heater, turbomolecular pump, gases (propane, argon, nitrogen, silane), copper foil. Characterization equipment: FE-SEM (MIRA III, Tescan Brno), EDX spectrometer (SEM S-4800, Hitachi), confocal Raman microscope (Confotec NR500, SOL Instruments Ltd.).
4：Experimental Procedures and Operational Workflow:
The copper foil is heated to 350-500°C in a vacuum chamber. Plasma is generated using RF induction. Gases are introduced at controlled flow rates and pressures. Deposition times range from 1 to 30 min. After deposition, samples are characterized using FE-SEM, EDX, and Raman spectroscopy.
5：Data Analysis Methods:
Raman spectra are analyzed for D and G bands to assess defect density and carbon hybridization. FE-SEM images are used to measure coating height and morphology. EDX provides elemental composition. Crystallite size is calculated using the IntD/IntG ratio from Raman data.
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SEM microscope
S-4800
Hitachi
Equipped with EDX spectrometer for elemental composition analysis
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Confocal Raman microscope
Confotec NR500
SOL Instruments Ltd.
Recording Raman spectra of samples
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FE-SEM microscope
MIRA III
Tescan Brno
Analyzing the morphology of VOG materials
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Turbomolecular pump
STP-iXA3306
Edwards
High vacuum pumping in the ICP CVD system
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Mechanical pump
E2M40
Edwards
Coupled with turbomolecular pump for vacuum
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RF generator
Generating radio frequency for plasma process
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Matching block
Matching output resistance of RF generator with load impedance
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Mass flow controller
Pneucleus Technologies LLC
Controlling gas flow rates
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Heater
Heating the copper foil substrate
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K-type thermocouple
Measuring temperature on sample surface
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