研究目的
To develop a facile and green process for synthesizing high-quality few-layer graphene (FLG) and investigate its use in conductive adhesives for potential applications in electronics.
研究成果
The liquid exfoliation process successfully produced high-quality FLG with minimal defects, as evidenced by characterizations. FLG/PVDF composites showed superior electrical conductivity compared to graphite/PVDF, enhanced further by sintering, and exhibited excellent flexibility and mechanical strength, making them promising for conductive adhesive applications in flexible electronics.
研究不足
The process may have limitations in scaling up for mass production, and the electrical conductivity, while improved, might not match that of metal-based adhesives in all applications. The environmental impact of using NMP and other chemicals should be considered, and long-term stability of the composites under various conditions was not extensively tested.
1：Experimental Design and Method Selection:
A liquid exfoliation process using a low-temperature, high-pressure continuous flow cell disrupter was employed to synthesize FLG from graphite. This method is chosen for its simplicity, scalability, and environmental friendliness without toxic chemicals.
2：Sample Selection and Data Sources:
Natural flake graphite with an average diameter of 500 μm was used as the feed material. Dispersions were prepared with N-Methyl-2-pyrrolidone (NMP) and polyvinylidene fluoride (PVDF) as dispersing agent and binder, respectively.
3：List of Experimental Equipment and Materials:
Equipment includes a low-temperature, ultra-high-pressure continuous flow cell disrupter (LTHPD, JNBIO, JN 10C), vacuum oven, stirrers, coating tools, atomic force microscopy (AFM, Bruker Dimension Icon), scanning electron microscopy (SEM, Hitachi S-4100), high-resolution transmission electron microscopy (HR-TEM, JEOL-JEM2000FXII), micro Raman spectroscopy system with 532 nm laser, and resistivity meter (KeithLink TG2). Materials include graphite, NMP, PVDF, de-ionized water, mica wafer, silica wafer, glass slides, and PET film.
4：2). Materials include graphite, NMP, PVDF, de-ionized water, mica wafer, silica wafer, glass slides, and PET film. Experimental Procedures and Operational Workflow:
4. Experimental Procedures and Operational Workflow: Graphite was dispersed in DI water and fed into the LTHPD at 1800 bar and 14-16°C to exfoliate into FLG. The product was dried in a vacuum oven. Slurries with various FLG:PVDF ratios were prepared by stirring in NMP, coated onto substrates, and dried. Characterizations involved SEM, TEM, AFM, Raman spectroscopy, and electrical conductivity measurements using a four-point probe. Sintering tests were conducted by heating samples on a hot plate.
5：Data Analysis Methods:
AFM was used to measure flake thickness and distribution. Raman spectra analyzed D/G ratios. Electrical conductivity was measured directly with the resistivity meter, and data were compared between different composites and conditions.
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Atomic Force Microscopy
Dimension Icon
Bruker
Used to measure the height profile and thickness distribution of the synthesized few-layer graphene.
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Scanning Electron Microscopy
S-4100
Hitachi
Used to analyze the morphologies of graphite and few-layer graphene samples.
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High-Resolution Transmission Electron Microscopy
JEM2000FXII
JEOL
Used for high-resolution imaging of the few-layer graphene to observe its structure.
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Low-Temperature, Ultra-High-Pressure Continuous Flow Cell Disrupter
JN 10C
JNBIO
Used for the liquid exfoliation process to synthesize few-layer graphene from graphite.
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Resistivity Meter
TG2
KeithLink
Used to measure the electrical conductivity of the composite films using a four-point probe.
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Micro Raman Spectroscopy System
Used to carry out Raman spectra analysis with a 532 nm laser as the excitation source.
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Vacuum Oven
Used to dry the synthesized few-layer graphene and composite slurries.
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Hot Plate
Used for the sintering process to heat the composite films and measure resistance variations with temperature.
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