Preparation method of single-layer graphene

A graphene and monolayer technology, applied in the field of monolayer graphene preparation, can solve problems such as difficulty in preparing large-sized graphene, high price of SiC wafers, unfavorable large-scale application, etc., and achieve low cost of raw materials and production steps. Less and easy to operate

Inactive Publication Date: 2010-04-14
TIANJIN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The British scientists who first prepared graphene used the micromechanical mechanical exfoliation method. This method can only produce a small amount of products, which is only suitable for laboratory research and is not conducive to large-scale industrial application.
The epitaxial growth method generally uses high-temperature processing of SiC wafers. This method requires relatively harsh conditions, and the SiC wafers used are expensive, and it is not easy to prepare large-scale graphene.
Now many researchers use chemical methods to reduce graphene oxide with hydrazine reducing agent to prepare graphene, but because hydrazine is an extremely toxic reagent, it is not conducive to the application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] First prepare graphene oxide: take 20g of 325 mesh natural flake graphite particles and 460mL of concentrated H with a mass concentration of 98%. 2 SO 4 Place in a three-necked flask, slowly add 60g KMnO in a water bath at 0°C 4 , the control temperature cannot be higher than 20°C. Add 920mL of deionized water into the three-necked flask, and keep the reaction at 35±3°C for 2h. Finally, add 2.8L of deionized water and 50mL of H 2 o 2 , the mixture changed from tan to bright yellow, and the reaction was terminated after 15 min. Wash and filter the above reaction product with 5 L of 1:10 HCl solution to remove some metal ions. Put the graphite oxide washed with dilute hydrochloric acid into a dialysis bag, and perform dialysis in deionized water. 2 Solution inspection filtrate without SO 4 2- , and with AgNO 3 Solution test without Cl - until. Filter and dry to obtain graphite oxide. Take this graphite oxide and prepare a 1 mg / mL graphite oxide aqueous dispers...

Embodiment 2

[0016] Graphene oxide preparation method is identical with embodiment example 1.

[0017] Take 20 mL of the 1 mg / mL graphene oxide aqueous dispersion prepared in Example 1, place it in a conical flask, add 54 g of deionized water, then place the conical flask in an ice-water bath, and slowly dropwise add a mass fraction of 98% 100mL of concentrated sulfuric acid was prepared into a reaction solution with a sulfuric acid mass concentration of 70%. After the dropwise addition, the triangular flask was placed in a constant temperature blast drying oven at 80°C and reacted at a constant temperature for 24 hours. After the reaction was completed, the reaction mixture was slowly poured into 1 L of deionized water, and cooled to room temperature. Filter with a solvent filter, wash the filter cake 3 times with 500 mL of deionized water, and finally wash with BaCl 2 No white precipitate was formed in the solution test filtrate. The obtained filter cake was transferred to a vacuum ove...

Embodiment 3

[0019] Graphene oxide preparation method is identical with embodiment example 1.

[0020] Get 16 mL of the 1 mg / mL graphene oxide aqueous dispersion prepared in Example 1, place it in an Erlenmeyer flask, place the Erlenmeyer flask in an ice-water bath, slowly add 100 mL of concentrated sulfuric acid with a mass fraction of 98%, and prepare The sulfuric acid mass concentration is 90% reaction liquid, after dropwise addition, this triangular flask is put into 60 ℃ constant temperature blast drying box, constant temperature reaction 24 hours. After the reaction was completed, the reaction mixture was slowly poured into 1 L of deionized water and cooled to room temperature. Filter with a solvent filter, wash the filter cake 4 times with 500 mL of deionized water, and finally wash with BaCl 2 No white precipitate was formed in the solution test filtrate. The obtained filter cake was transferred to a vacuum oven, and dried at 75° C. for 8 hours to obtain a black graphene film. T...

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Abstract

The invention relates to a preparation method of single-layer grapheme and belongs to the technical field of grapheme preparation. Single-layer graphene oxide is used as raw materials, and the invention comprises the following steps: dropwise adding concentrated sulfuric acid according to volume ratio in single-layer graphene oxide water dispersion liquid under the condition of an ice-water bath to prepare reaction liquid with sulfuric acid mass concentration of 70%-90%; reacting at 60 DEG C-100 DEG C, and then diluting with deionized water, cooling to room temperature and filtering; washing a filter cake with the deionized water, placing the filter cake in a vacuum dryer and drying at 65 DEG C-75 DEG C to obtain black grapheme. The invention has the advantages of low raw material cost, no poisons or damages and simple operation and is suitable for mass production. The prepared single-layer grapheme can be used in micro electronic elements, lithium ion batteries, fuel batteries, nano reinforced composites and other fields and has wide application prospects.

Description

technical field [0001] The invention relates to a preparation method of single-layer graphene, which belongs to the preparation technology of graphene. Background technique [0002] Since British scientists successfully prepared single-layer graphene in the laboratory in 2004, graphene has rapidly become a research hotspot in the field of nanoscience. Graphene is a new type of carbonaceous material with the thickness of a single layer of carbon atoms and arranged in a two-dimensional honeycomb lattice structure. It is considered to be the basic unit of all other dimensional carbonaceous materials. It can be wrapped into zero-dimensional fullerenes, rolled into one-dimensional carbon nanotubes, and stacked into three-dimensional graphite. In theory, people have studied graphene for more than 60 years. Early studies believed that two-dimensional graphene sheets are thermodynamically unstable, so they cannot exist alone in nature. However, in 2004, British scientists successf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 王宇新杨伟张洁婧许莉
Owner TIANJIN UNIV
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