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Method for preparing graphene powder and graphene transparent conductive film by oxyhydrogen flame method

A technology of transparent conductive film and graphene powder, which is applied in the direction of graphene, nano-carbon, etc., can solve the problems of destroying the quality of graphene, reducing the quality of graphene, and low controllability

Inactive Publication Date: 2013-07-24
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although there are many methods for preparing graphene, and the output and quality of graphene have been greatly improved, how to realize the macro-controlled preparation of graphene for different applications, and how to regulate its quality and structure still remain It is an important challenge in the field of graphene research
In the current preparation method of graphene, the micro-mechanical exfoliation method can prepare graphene of micron size, but its controllability is low, and it is difficult to synthesize on a large scale (K.S. Novoselov et al., "Science (Science) "2004, 306, 666); although SiC epitaxially grown graphene can be directly made into electronic devices through photolithography, the surface structure of SiC crystals is prone to reconstruction during high-temperature heating, resulting in complex surface structures and difficult Obtain graphene with large area and uniform thickness (C. Berger et al. (C.Berger), "Science (Science)" 2006,312,1191); CVD is considered to be a good method for preparing large-area graphene, but its The growth substrate removal process will destroy the quality of graphene (K. Kim et al. (K.Kim) "Nature (Nature)" 2009, 457, 706); although chemical exfoliation method can prepare graphene in large quantities, its violent oxidation The reduction process will destroy the carbon skeleton of the graphene plane and produce defects, resulting in a decline in the quality of the graphene obtained, which seriously restricts the popularization and application of graphene (D. Li et al. (D.Li) "Nat.Nanotech. )》2008, 3, 101)

Method used

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  • Method for preparing graphene powder and graphene transparent conductive film by oxyhydrogen flame method
  • Method for preparing graphene powder and graphene transparent conductive film by oxyhydrogen flame method
  • Method for preparing graphene powder and graphene transparent conductive film by oxyhydrogen flame method

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Embodiment 1

[0058] Direct growth of graphene powder on h-BN insulating substrate

[0059] Implementation process such as figure 1 As shown, 2 L of anisole solution of PMMA with a mass fraction of 6% was first prepared for later use.

[0060] Take 100 mL of 6% PMMA anisole solution and 5 g of h-BN powder, stir for 30 minutes, place in an oven at 120° C. for 2 hours to fully evaporate the solvent, and obtain PMMA-coated h-BN. The aforementioned PMMA-coated h-BN was packed into a quartz tube with a size of φ25×2mm. Evacuate to 100Pa, and quickly heat the quartz tube with a hydrogen-oxygen flame for 20 seconds. Afterwards, the oxyhydrogen flame was removed and the quartz tube was allowed to cool rapidly to room temperature. The samples were taken out to obtain h-BN / graphene composites.

[0061] Conductivity test of graphene grown directly on h-BN insulating substrate

[0062] Conductivity is an important index to characterize the quality of graphene. In order to measure the conductivity...

Embodiment 2

[0069] Preparation of Freestanding Graphene

[0070] In order to obtain pure graphene, on the basis of Example 1, the present invention puts 6.7 g of the obtained h-BN / graphene composite into 400 mL of ethanol, and obtains a turbid solution after ultrasonication at 300 w for 15 minutes. . After centrifugation at 1000 rpm for 5 minutes, 1.5 g of pure unsupported graphene samples were obtained.

[0071] The unsupported graphene obtained by the present embodiment is modulated into a conductive paste, scraped into a 10 μm film according to the method in Example 1, and silver paste is applied to test that its average sheet resistance is 31Ωsq (ohm / square).

[0072] Characterization of Morphological and Structural Properties

[0073] The morphology of the obtained unsupported graphene observed with a transmission electron microscope, such as Figure 7 shown. It can be seen from the figure that the obtained graphene has a size of 200 nm. Observing the graphene boundary with a hi...

Embodiment 3

[0086] Prepare 2 L of anisole solution of PMMA with a mass fraction of 4% for later use.

[0087] Take 200 mL of 4% PMMA anisole solution and 5 g of h-BN powder, stir for 20 minutes, place in an oven at 120° C. for 3 hours to fully evaporate the solvent, and obtain PMMA-coated h-BN. The aforementioned PMMA-coated h-BN was packed into a quartz tube with a size of φ25×2mm. Evacuate to 100Pa, and quickly heat the quartz tube with a hydrogen-oxygen flame for 15 seconds. Afterwards, the oxyhydrogen flame was removed and the quartz tube was allowed to cool rapidly to room temperature. The samples were taken out to obtain h-BN / graphene composites.

[0088] In order to obtain pure graphene, on the basis of the above-mentioned h-BN / graphene composite, 7.1 g of the obtained h-BN / graphene composite was placed in 800 mL of ethanol, and after ultrasonication at 400 w for 15 minutes A cloudy solution was obtained. After centrifugation at 1000 rpm for 5 minutes, 1.7 g of pure unsupported...

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Abstract

The invention discloses a method for preparing high-quality graphene powder and a graphene transparent conductive film. The method comprises that through an oxyhydrogen flame rapid heating method, organics are decomposed into high-activity carbon atoms; and the high-activity carbon atoms are re-configurated into graphene on an insulating substrate or a catalyst substrate. Through the method, high-quality graphene can directly grow on the insulating substrate, and through an ultrasonic method, high-quality graphene powder without a support substrate is obtained. Compared with the traditional chemical stripping method for preparing graphene, the method has simple processes, a low cost, less defects and good conductivity and can produce high-quality graphene. The method can be used for preparing the graphene transparent conductive film on a catalyst film substrate. The graphene transparent conductive film has quality and conductivity approximate to the optimal values of a graphene transparent conductive film obtained by the traditional CVD method. Graphene obtained by the method has wide application prospects in fields of photoelectric devices such as copper indium gallium diselenide, cadmium telluride and dye-sensitized solar cells, panel displays, super capacitors, field emission materials, and lithium ion batteries.

Description

technical field [0001] The invention relates to a method for preparing high-quality graphene powder and graphene transparent conductive film by a hydrogen-oxygen flame method. technical background [0002] Graphene is a two-dimensional material composed of a single layer of carbon atoms tightly packed. Due to the unique two-dimensional structural characteristics and excellent crystallographic quality, it not only contains rich and novel physical phenomena, and has important theoretical research value, but also its unique structure and excellent properties may make it possible to be used in many fields. Obtain significant practical applications and provide new powerful growth points for future economic and social development. For example, graphene has high light transmittance in the visible-near-infrared region (R. Nair et al. (R. Nair) "Science (Science)" 2008, 320, 1308), which avoids the traditional transparent conductive oxidation The light absorption of matter in the n...

Claims

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Application Information

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IPC IPC(8): C01B31/04C04B41/50C01B32/184
Inventor 黄富强林天全
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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