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Preparation method for few-layer graphene

A technology of graphene and a few layers, which is applied in the field of graphene prepared by ultrasonic-assisted supercritical carbon dioxide technology combined with micro-spraying, which can solve the problem of low graphene production

Active Publication Date: 2017-05-31
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of graphene within five layers obtained by this method is low, and 70% is 5-8 layers

Method used

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  • Preparation method for few-layer graphene
  • Preparation method for few-layer graphene
  • Preparation method for few-layer graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Weigh 1g of high-temperature pyrolytic graphite powder and place it in a 200ml autoclave 5;

[0026] (2) In the autoclave 5, the material is heated to 80°C, and the CO 2 Inject into the autoclave 5, when the pressure in the autoclave 5 reaches 16 MPa, the ultrasonic probe 4 starts to work under a power of 100 W, and at the same time, the stirring device 8 is turned on to start stirring.

[0027] (3) After the ultrasonic and stirring time in the autoclave 5 reaches 120 minutes, open the valve between the autoclave 5 and the micro-jet stripping device 9. After the high-pressure material comes out of the autoclave 5, it is sprayed into the micro-jet stripping device 9 A rapid pressure relief process is performed in the atmospheric receiving tank 10 to obtain a graphene product.

[0028] Through testing and characterization, the sample has less than 3 layers of graphene accounting for 88%, of which single-layer graphene accounts for 41%. See image 3 .

Embodiment 2

[0030] (1) Weigh 0.5g of natural graphite powder and place it in a 200ml autoclave 5;

[0031] (2) In the autoclave 5, the materials are heated to 60℃, and the CO 2 Inject into the autoclave 5, when the pressure in the autoclave 5 reaches 8Mpa, the ultrasonic probe 4 starts to work at a power of 300W, and at the same time, the stirring device 8 is turned on to start stirring.

[0032] (3) After the ultrasonic and stirring time in the autoclave 5 reaches 60 minutes, open the valve between the autoclave 5 and the micro-jet stripping device 9. After the high-pressure material comes out of the autoclave 5, it is sprayed into the normal temperature through the micro-jet stripping device 9 A rapid pressure relief process is performed in the pressure receiving tank 10 to obtain a graphene product.

[0033] Through testing and characterization, the sample has less than 3 layers of graphene accounting for 94%, of which single-layer graphene accounts for 45%. Figure 4 .

Embodiment 3

[0035] (1) Weigh 0.2g of expanded graphite powder and place it in a 200ml autoclave 5;

[0036] (2) In the autoclave 5, the materials are heated to 40℃, and the CO 2 Inject into the autoclave 5, when the pressure in the autoclave 5 reaches 13Mpa, the ultrasonic probe 4 starts to work under 1000W power, and at the same time the stirring device 8 is turned on to start stirring.

[0037] (3) After the ultrasonic and stirring time in the autoclave 5 reaches 30 minutes, open the valve between the autoclave 5 and the micro-jet stripping device 9. After the high-pressure material comes out of the autoclave 5, it is sprayed into the normal temperature through the micro-jet stripping device 9 The pressure in the pressure receiving tank 10 is quickly released to obtain a graphene product.

[0038] Through testing and characterization, the sample has less than 3 layers of graphene accounting for 91%, of which single-layer graphene accounts for 43%, see Figure 5 .

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Abstract

The invention discloses a method for preparing graphene by combining an ultrasonic-assisted supercritical carbon dioxide technique with micro-jetting. The method comprises the following steps: performing supercritical carbon dioxide intercalation ultrasonic treatment on a material; quickly putting into a micro-jetting stripping device; violently high-speed moving the fluid and quickly jetting into a normal-pressure receiving tank, thereby acquiring a graphene product. Compared with the prior art, the method has the advantages that high-quality graphene can be prepared; 88-94% of graphene is in the layer quantity being less than three; more than 40% of graphene is in single-layer; the method disclosed by the invention is environment-friendly; the process flow is simple; a new method is supplied for cleanly preparing the high-quality graphene on a large scale.

Description

Technical field [0001] The invention relates to the technical field of preparation of a nano two-dimensional material, and specifically relates to a method for preparing graphene by combining ultrasonic assisted supercritical carbon dioxide technology with micro-jetting. Background technique [0002] Graphene is a kind of sp 2 The hybrid composition constitutes a hexagonal two-dimensional crystal material with a honeycomb structure. The unique structure of graphene gives it excellent thermal, electrical and mechanical properties. Since it was discovered in 2004 by Professor Geim of the University of Manchester, UK, due to its peculiar properties and broad market application prospects, it has attracted relevant scholars from all over the world. Great attention. [0003] The preparation of graphene is a prerequisite for basic research and the key to commercial applications. Therefore, how to obtain large quantities of high-quality graphene becomes the key. At present, the methods ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/19B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B2204/02C01B2204/04C01B2204/30C01P2004/03C01P2004/04C01P2004/20Y02P20/54
Inventor 郑艳梅尚天宇李清彪吴秋杰
Owner XIAMEN UNIV
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