Method for preparing and purifying graphene by microwave radiation under vacuum

A technology of microwave radiation and graphene, applied in the field of material preparation and purification, to achieve high production efficiency, low production cost, and low microwave radiation power

Inactive Publication Date: 2011-01-19

TIANJIN UNIV

3 Cites 34 Cited by

AI-Extracted Technical Summary

Problems solved by technology

There are no literature or patent reports on the solut...

Method used

Get the graphite oxide 2g that is produced according to the method for embodiment 1, be placed in reactor. In the air atmosphere and normal pressure, adjust the microwave frequency to 2450MHz, the power to 800W, and the radiation time to 300s, and start the microwave radiation. After the reaction, the cooling water valve was opened, and after the temperature in the reactor dropped to room temperature, the water flow was stopped. Collect graphene samples. Adopt XPS and specific nitrogen surface area tester to test sample, the oxygen element atomic ratio content of the graphene that obtains is about 15%, specific surface area is about 220m2/g, the quality of the graphene that adopts this method to prepare as known by contrast is better high.

Get the graphite oxide 2g that is produced according to the method for embodiment 1, be placed in reactor....

Abstract

The invention discloses a method for preparing and purifying graphene by microwave radiation under vacuum. The method for preparing graphene is as follows: placing graphite oxide in a reactor, radiating the graphite oxide by microwaves under vacuum, and obtaining the graphene by heating and cleavage of the graphite oxide. The method for purifying graphene is as follows: placing graphene with low purity in a reactor, irradiating the graphite oxide by microwaves under vacuum, and obtaining the graphene with higher purity after impure graphene is subjected to heating and cleavage. The method is implemented under the vacuum condition, thus being favor to preventing the generated graphene from being oxidized by oxygen in the reactor, reducing the cleavage resistance of the graphite oxide, and ensuring the safety in the operation process, and the method also has the advantages of high production efficiency, low production cost, safe operation process, high product purity and the like, and can be used as one of the methods for preparing and purifying graphene massively.

Technology Topic

Cvd grapheneGraphite oxide +5

Examples

Experimental program(10)
Comparison scheme(2)

Example Embodiment

[0010] Example 1

[0011] 2g of graphite powder and 1g of sodium nitrate were uniformly mixed with 46mL of sulfuric acid with a mass concentration of 98%, stirred in an ice-water bath, slowly added 6g of potassium permanganate, reacted for 2h, and then transferred to a constant temperature water bath at 35°C for 30min. After adding 92 mL of deionized water dropwise, the temperature was raised to 98 °C and the reaction was continued for 3 h, taken out from the water bath, further diluted with deionized water, and treated with 20 mL of 30% hydrogen peroxide solution to reduce the oxidizing substances in the solution. . The impurities in the dissolved solution were washed with 5% hydrochloric acid, centrifuged while hot, and the filter cake was repeatedly washed with deionized water until the pH value of the washing solution was greater than 5, and vacuum dried at 70°C for 48 hours to obtain graphite oxide.

[0012] Take 2 g of the graphite oxide obtained in the previous step and place it in the reactor. Use a vacuum pump to evacuate, when the vacuum degree reaches 2Pa, stop evacuation, pass in argon until the air pressure is 0.1MPa, repeat the evacuation and pass argon twice, and finally use a vacuum pump to evacuate to a vacuum of 2Pa. The power microwave frequency is 2450MHz, the power is 800W, and the microwave radiation is 300s. After the reaction was completed, the temperature was lowered until the temperature in the reactor dropped to room temperature. The graphene samples were collected and tested by XPS and nitrogen specific surface area tester. The test results showed that the atomic ratio of oxygen in graphene was about 7%, and the specific surface area was about 510m. 2 /g.

Example Embodiment

[0013] Example 2

[0014] The process and conditions of this example are the same as those of Example 1, except that the power of the microwave is adjusted to 1500W, and the irradiation time is adjusted to 100s, and the graphene sample can still be obtained. The samples were tested by XPS and specific nitrogen surface area tester. The test results showed that the atomic ratio of oxygen in graphene was about 7%, and the specific surface area was about 500m. 2 /g.

Example Embodiment

[0015] Example 3

[0016] According to the preparation method of Example 1, the power of the microwave is adjusted to 2000W, the radiation time is adjusted to 2s, and other reaction conditions remain unchanged, and the graphene sample can be obtained.

PUM

Property	Measurement	Unit
Specific surface area	510.0	m²/g
Specific surface area	500.0	m²/g
Specific surface area	220.0	m²/g

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

Classification and recommendation of technical efficacy words

Increase productivity
short time consumption

Method for preparing and purifying graphene by microwave radiation under vacuum

A technology of microwave radiation and graphene, applied in the field of material preparation and purification, to achieve high production efficiency, low production cost, and low microwave radiation power

AI-Extracted Technical Summary

Problems solved by technology

Method used

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Bending device for electronic product production

Data processing method, intelligent device and intelligent processing system

Forming method of composite material winding shaft containing injection layer

Pulse modulator and drive circuit thereof

Mixing pan used for food processing

Classification and recommendation of technical efficacy words

Method and Apparatus for Service-Oriented Architecture Process Decomposition And Service Modeling

Methods and Compositions for Mammalian Cell Lines for Transfection and Protein Expression in Serum-Free Medium

Composite material of poly lactic acid / natural faric, and production method

Coffee pot with function of grinding coffee beans

Preparation method of super-retarding type polycarboxylate superplasticizer

Voltage equalizing method for modular multilevel converter

Engine assembly line and assembly method thereof

Method for optimizing route for exposing wafer

A management method for check points in cluster

Movable stacking type automatic stereoscopic warehouse