High-conductivity graphene material with low-temperature gas-phase reduction and preparation method thereof

A graphene, high-conductivity technology, applied in the field of graphene material preparation, can solve problems such as high cost, damage to graphene structure, environmental pollution, etc., and achieve the effects of high-efficiency reduction, good mechanical strength and flexibility

Active Publication Date: 2013-09-18
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] In the face of the above-mentioned problems in the prior art, the inventor realized that under low temperature conditions, the oxygen-containing functional groups in graphene oxide can be effectively captured by a gas phase reaction using a non-toxic solid or commonly used gaseous reducing agent, and a relatively low temperature can be achieved. Rapid and efficient reduction at low temperature can prepare graphene with excellent conductivity and light transmission, and solve the problems of environmental pollution, high cost and damage to graphene structure that are easily caused by high temperature treatment or low temperature liquid phase chemical reduction technology

Method used

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  • High-conductivity graphene material with low-temperature gas-phase reduction and preparation method thereof
  • High-conductivity graphene material with low-temperature gas-phase reduction and preparation method thereof
  • High-conductivity graphene material with low-temperature gas-phase reduction and preparation method thereof

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preparation example Construction

[0032] The preparation method of the low-temperature gas-phase reduction high-conductivity graphene material of the present invention specifically comprises: adopting multi-temperature zone heating furnace equipment, placing the raw material graphene oxide at the low-temperature end, and placing the solid-phase reducing agent at the high-temperature end or from the high-temperature end Introduce a gas-phase reducing agent; use a mechanical pump to extract the background vacuum to a certain level, for example, to 0.5Pa-10Pa, stop vacuuming, and seal; then start to heat the two ends of the heating furnace in the multi-temperature zone to the required temperature, for example, The low temperature zone is heated to 50-500°C, and the high temperature zone is heated to 400-1200°C. After a certain period of time, the heating is stopped, and it is naturally cooled to room temperature to obtain a highly conductive graphene material. The reaction holding time can be 30-600min.

[0033]T...

Embodiment 1

[0050] The sample to be reduced is graphene oxide paper that has been vacuum filtered, with a thickness of 5 microns and a density of 1.8g / cm 3 , 10cm in diameter. The reducing agent is high-purity Al powder; the raw material graphene oxide paper is placed at the low-temperature end of the multi-temperature zone heating furnace, and the high-purity Al powder is placed at the high-temperature end. The temperature at the high-temperature end is 700°C, and the temperature at the low-temperature end is 100°C. Use a mechanical pump to extract the background vacuum to about 1Pa, stop vacuuming, and seal. Start to heat the two ends of the heating furnace in the multi-temperature zone to the required temperature respectively, keep the heat for 3 hours, stop heating, and let the furnace cool naturally.

[0051] Morphology and structure characterization of graphene

[0052] The graphene structure was characterized by Raman spectroscopy (Renishaw invia Raman Microscope, excitation wave...

Embodiment 2

[0055] The sample to be reduced is graphene oxide paper that has been vacuum filtered, with a thickness range of 5 microns and a density range of 1.8 g / cm 3 , 10cm in diameter. The reducing agent is high-purity Al powder; the raw material graphene oxide paper is placed at the low-temperature end of the multi-temperature zone heating furnace, and the high-purity Al powder is placed at the high-temperature end. The temperature at the high-temperature end is 700°C, and the temperature at the low-temperature end is 200°C. Use a mechanical pump to extract the background vacuum to about 1Pa, stop vacuuming, and seal. Start to heat the two ends of the heating furnace in the multi-temperature zone to the required temperature respectively, keep the heat for 3 hours, stop heating, and let the furnace cool naturally.

[0056] The X-ray diffraction and Raman spectra of the reduced graphene are still shown in figure 1 and figure 2 . As shown in the figure, compared with Example 1, the...

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Abstract

The invention provides a preparation method of high-conductivity graphene material with low-temperature gas-phase reduction. The preparation method comprises the following steps of: heating a low-temperature zone with graphene oxide and a high-temperature zone with a reducing agent to a certain temperature by utilizing multi-temperature zone heating equipment with the high-temperature zone and the low-temperature zone, and reducing out high-conductivity graphene. The preparation method provided by the utility model has the advantages that under the low-temperature condition, fast and high-efficiency reduction of the graphene oxide is realized, and low-temperature gas-phase reaction maintains the more complete structure of the graphene oxide, so that high-conductivity graphene powder or graphene paper and a high-transmittance and high-conductivity graphene film is prepared. The prepared graphene material has the advantages that the conductivity, the mechanical strength and the flexibility are good, and the bottleneck problem that the existing high-temperature heat treatment or low-temperature liquid-phase chemical reduction method damages the graphene structure can be effectively solved.

Description

technical field [0001] The invention relates to the technical field of preparation of graphene materials, in particular to a low-temperature gas-phase reduction high-conductivity graphene material and a preparation method thereof. Background technique [0002] Graphene is a new carbonaceous material that is densely packed into a two-dimensional honeycomb lattice structure by a single layer of carbon atoms. the basic unit of . Due to its unique two-dimensional structure and perfect crystal structure, graphene contains rich and novel physical phenomena, which provides an ideal platform for the study of quantum electrodynamic phenomena and has important theoretical research value; at the same time, graphene has Atomic-level thickness, excellent electrical properties, excellent chemical stability and thermodynamic stability are expected to be widely used in high-performance nanoelectronic devices, sensors, nanocomposites, batteries and supercapacitors, field emission materials ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/04C01B32/184
Inventor 万冬云黄富强杨重寅林天全
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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