Method for rapidly preparing graphene in large quantities by utilizing graphite oxides

A graphene and graphite technology, which is applied in the field of preparation of rapid and large-scale acquisition of graphene, can solve the problems of inability to achieve rapid and large-scale acquisition, high equipment dependence, complex process, etc., achieves small thickness, simple and fast process, and promotes solution the effect of

Inactive Publication Date: 2012-06-20
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, using this method, the cycle is long. After the graphite oxide is obtained, it needs to be pickled and reduced with reducing agents such as hydrazine hydrate or sodium borohydride. In terms of products with low (especially single-layer graphene), there are

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0045] Take by weighing 15 grams of natural flake graphite and 5g sodium nitrate (NaNO 3 ) solid mixture, add slowly and soak in 200ml concentrated nitric acid (HNO 3 ) for 24 hours, then slowly add 20g of potassium permanganate (KMnO 4 ). Then the graphite powder soaked in an ice bath was stirred for 8 hours at 25-30°C. Use deionized water and hydrochloric acid to clean and filter the oxidized graphite in sequence until the filtrate is clear and transparent to remove metal ions and unreacted sulfate (SO 4 2– )Wait. Gained graphite oxide was then air-dried at 60° C. for 3 hours.

[0046] Put the obtained dried graphite oxide into a 1000ml alumina crucible, cover the crucible lid, seal it with adhesive tape (with a gap connecting to the outside), and place it in the center of the microwave vacuum sintering furnace cavity. After closing the furnace door, evacuate to 0.01MPa, add microwaves, rapidly increase the power to 8kW, and irradiate for 5 seconds. Then turn off the ...

Embodiment 2

[0049] Take by weighing 5 grams of natural flake graphite and 2 g sodium nitrate (NaNO 3 ) solid mixture, slowly added and soaked in 250ml concentrated sulfuric acid (H 2 SO 4 ) for 5 hours, then slowly add 8g of potassium permanganate (KMnO 4 ). Then the graphite powder soaked in ice bath was stirred at 28±2°C for 1 hour. Use deionized water and hydrochloric acid to clean and filter the oxidized graphite in sequence until the filtrate is clear and transparent to remove metal ions and unreacted sulfate (SO 4 2– )Wait. Gained graphite oxide was then air-dried at 70° C. for 2 hours.

[0050] Put the dried graphite oxide into a 500ml quartz tube, seal the quartz tube with a quartz glass sheet and adhesive tape, but keep a small amount of gaps. Place the quartz tube at the center of the cavity of the microwave vacuum sintering furnace. After closing the furnace door, evacuate to 0.02MPa, add microwaves, rapidly increase the power to 6kW, and irradiate for 3 seconds. Then ...

Embodiment 3

[0053] Weigh 5 grams of natural flake graphite and 1 g of sodium nitrate (NaNO 3 ) solid mixture, slowly added and soaked in 250ml concentrated sulfuric acid (H 2 SO 4 ) for 15 hours, then slowly add 10g of potassium dichromate (K 2 Cr 2 o 7 ). Then the graphite powder after the ice-bath immersion was stirred at about 30° C. for 2 hours. Use deionized water and hydrochloric acid to clean and filter the oxidized graphite in sequence until the filtrate is clear and transparent to remove metal ions and unreacted sulfate (SO 4 2– )Wait. Gained graphite oxide was then air-dried at 70° C. for 2 hours.

[0054] The obtained dried graphite oxide is put into a 1000ml alumina crucible, and the crucible is sealed with a quartz glass sheet and adhesive tape, but a small amount of gaps are reserved. Place the alumina crucible in the center of the cavity of the microwave vacuum sintering furnace. After closing the furnace door, evacuate to 0.02MPa, add microwaves, rapidly increase...

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Abstract

The invention aims at providing a preparation method for rapidly obtaining graphene in large quantities. On the basis of obtaining graphite oxides, the molecular thermodynamic movement of groups such as hydroxyl groups (-OH), carboxylic groups (-COOH) and the like which are generated on the surfaces of graphite oxide layers through oxidization can be induced and stimulated through microwave treatment so as to produce a momentary unsteady state, so that Van der Waals binding force between graphite layers is damaged, and graphene can be rapidly obtained in large quantities. The graphite oxides are obtained through the oxidization of metal salt such as potassium permanganate, potassium dichromate and the like as well as strong protonic acid such as concentrated sulphuric acid, concentrated nitric acid and the like, and then microwave irradiation is carried out under the conditions that the power ranges from 2 to 10 kW, the vacuum pressure ranges from 0.01 to 0.06 MPa and so on, so that microwave cleavage of the graphite oxides can be accomplished within 2 to 10 seconds, and graphene with less than ten layers can be obtained rapidly in large quantities. The preparation method can also control the layer number or the thickness of graphene products by controlling the concentration and the oxidation time of oxidizing mediums as well as the power, the degree of vacuum and the like of the microwave irradiation.

Description

technical field [0001] The invention belongs to a preparation method for rapidly obtaining graphene in large quantities by using graphite oxide as a raw material. Specifically, it refers to the use of high-frequency and high-power microwave radiation to induce and excite the thermal movement of hydroxyl groups, carboxyl groups and other groups on the graphite oxide carbon layer, and instantly destroy the van der Waals bond between graphite layers, thereby achieving rapid mass production. Get graphene. Background technique [0002] Due to the excellent properties of graphene in mechanics, electricity, optics and many other aspects, people have been attracted to carry out a very wide range of theoretical research and application practice on graphene. However, as a unique two-dimensional crystal material, its preparation has always been the focus of attention. At present, the preparation and synthesis of graphene mainly revolves around two aspects: one is to obtain perfect tw...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y40/00C01B32/19
Inventor 王继刚于娟田璇王辉
Owner SOUTHEAST UNIV
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