Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation

A carbon dioxide and supercritical technology, applied in the production of graphene, nano-carbon, bulk chemicals, etc., can solve the problems of high pressure, high toxicity of organic solvents, low output, etc., to increase the number of boost and step-down, and widely used Prospects, effects of huge economic benefits

Active Publication Date: 2012-06-27
上海利物盛纳米科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But this method output is extremely low, has no production value; Oxidation-reduction method is the method that uses more at present, and Chinese patent (application number: 200910099595.x) discloses " a kind of solution phase preparation method of graphene " although this method can Graphene with a large area is prepared, but this method will introduce a large number of defects due to the oxidation process, which cannot be completely repaired during reduction, which seriously affects the electrical properties of graphene; epitaxial growth and chemical vapor deposition can be obtained. High-quality bulk graphene monoliths are currently the main means of preparing high-quality graphene
However, the preparation conditions of these two methods are harsh, the yield is not high, and the preparation cost is very high; Mix and heat to high temperature (200°C-700°C) and high pressure (10-100MPa), and then prepare graphene through cooling and depressurization process
The organic solvent used in this method is highly toxic, and the preparation process has high temperature (up to 700°C) and high pressure (up to 100MPa), and the steps are complicated, so it is not suitable for large-scale preparation of graphene.

Method used

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  • Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation
  • Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation
  • Method for preparing large-scale graphene through supercritical carbon dioxide exfoliation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A certain amount of sodium lauryl sulfate is mixed with graphite powder, and the weight ratio of graphite powder and sodium lauryl sulfate is 1:5, and is added in the autoclave 4. The autoclave temperature was set at 65°C, and the control temperature was 40°C. The carbon dioxide is pumped into the autoclave 4 by the pump 3, and the pressure in the still is controlled at 18MPa. The material stays in the autoclave 4 for 120 minutes. Through testing and characterization, graphene with less than 10 layers in the product accounts for 42%.

Embodiment 2

[0025] A certain amount of sodium dodecylbenzenesulfonate is mixed with graphite powder, and the weight ratio of graphite powder and sodium dodecylbenzenesulfonate is 1:6, and is added in the autoclave 4 . The material in the autoclave 4 is heated, and the temperature is controlled to 45°C. Carbon dioxide is pumped into the autoclave 4 by the pump 3, and the pressure in the still is controlled at 10MPa. The material stays in the autoclave 4 for 60 minutes. After a quick depressurization, the carbon dioxide is pumped in again through the pump 3. Repeat the pressurization and depressurization process three times. Through testing and characterization, graphene with less than 10 layers in the product accounts for 63%.

Embodiment 3

[0027] Ethanol was used as co-solvent. A certain amount of ethanol is mixed with graphite powder and added to the autoclave 4. The material in the autoclave 4 is heated, and the temperature is controlled to 55°C. Carbon dioxide is pumped in the autoclave 4 by the pump 3, and the pressure in the control kettle is at 12MPa. The material stays in the autoclave 4 for 30 minutes. After a quick depressurization, the carbon dioxide is pumped in again through the pump 3. Repeat the pressurization and depressurization process three times. A certain amount of ethanol is added to the pressure relief tank 7, and the valve is opened to quickly relieve the pressure. According to the test and characterization, the graphene with less than 10 layers in the product accounts for 81%.

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Abstract

The invention relates to a method for preparing large-scale graphene through supercritical carbon dioxide exfoliation. Supercritical carbon dioxide is adopted as an exfoliant, a surfactant is adopted as a dispersant, graphite powder and the dispersant are put in an autoclave, the carbon dioxide is pumped in the autoclave and circularly flows in a supercritical state, and then the pressure is reduced quickly to be normal pressure; the process is repeated so that the materials undergo pressure increment and pressure reduction several times; and the layers of the graphene is controlled by controlling the times of pressure increment and pressure reduction, so as to prepare the large scale graphene. Compared with the prior art, the invention has the advantages as follows: large-scale (hundreds of micrometers) high-quality graphene can be prepared; the method belongs to physical exfoliation, the treatment conditions are mild, and the quality of the graphene cannot be damaged; besides, the carbon dioxide used in the method is nontoxic, cheap and easy to obtain, and the technology is simple.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional materials, and in particular relates to a method for preparing large-scale graphene by exfoliating supercritical carbon dioxide. Background technique [0002] Graphene is a two-dimensional crystal composed of carbon atoms, in which the carbon atoms are sp 2 Hybridization forms a honeycomb hexagonal planar structure. Graphene has excellent mechanical and electrical properties, and has broad application prospects in electronics, magnetism, optics, biology, etc. Since it was discovered by scientists from the University of Manchester in 2004, it has attracted extensive attention from researchers in the fields of physics, materials and chemistry, especially after the discoverer of graphene won the Nobel Prize in 2010, the preparation and properties of graphene And the research on application and other aspects has become a hot spot concerned by scholars from all over the world. [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
CPCY02P20/54
Inventor 王武聪赵亚平王燕金鹤阳李思宁
Owner 上海利物盛纳米科技有限公司
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