Graphene preparation method

A graphene and graphite technology, applied in the field of reducing graphene oxide aqueous solution to prepare graphene, can solve the problems of easy agglomeration of graphene, high toxicity of reducing agent, incomplete reduction, etc., and achieve sufficient reduction, less impurities and defects, and high purity. Effect

Inactive Publication Date: 2013-12-04
吴江市华诚电子有限公司
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Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of high toxicity of the reducing agent used, incomplete reduction, and easy agglomeration of graphene in the process of preparing graphene by the existing chemical reduction method, and propose a safe and efficient thiourea dioxide Or the mixed solution of carbohydrazide and soluble strong base is used as reducing agent, the method for preparing the graphene of uniform dispersion, high purity

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Examples

Experimental program
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Effect test

Embodiment 1

[0027] (1) Under the conditions of a stirring rate of 200r / min and an ice-water bath, add 3g of graphite and 1.8g of sodium nitrate to 120mL of sulfuric acid with a mass concentration of 98%, continue stirring for 30min, and use a water bath to heat the mixture to a low temperature. At 10°C, add 18g of potassium permanganate and continue to stir for 2h; heat the water bath to 40°C and react for 3h; then add 120mL of deionized water, continue to stir for 30min, then add 300mL of warm water at 35°C and 72mL of mass concentration 30% hydrogen peroxide, continue stirring for 20 min; ultrasonically disperse the above solution for 30 min, then filter, then wash 5 times with 10% hydrochloric acid and deionized water, and dry the filtered product at 70°C to obtain 4.9 g of graphite.

[0028] (2) Weigh 500 mg of graphite oxide and dissolve it in 500 mL of deionized water, and apply ultrasonic waves for 2 hours to obtain a graphene oxide aqueous solution with a concentration of 1.0 mg / m...

Embodiment 2

[0034] (1) Under the conditions of a stirring rate of 150r / min and an ice-water bath, add 2g of graphite and 1g of sodium nitrate to 70mL of sulfuric acid with a mass concentration of 98%, continue stirring for 20min, and heat the mixture to no higher than At 10°C, add 10g of potassium permanganate and continue stirring for 1.5h; heat the water bath to 35°C and react for 2h; then add 50mL of deionized water, continue stirring for 20min, add 160mL of warm water at 33°C and 35mL with a mass concentration of 25% hydrogen peroxide, continue to stir for 15 minutes; ultrasonically disperse the above solution for 20 minutes and then filter, then wash with 8% hydrochloric acid and deionized water for 5 times, and dry the filtered product at 60°C to obtain 3.3g of graphite oxide .

[0035] (2) Weigh 300 mg of graphite oxide and dissolve it in 600 mL of deionized water, and apply ultrasonic waves for 1.5 h to obtain a graphene oxide aqueous solution with a concentration of 0.5 mg / mL.

...

Embodiment 3

[0041] (1) Under the conditions of a stirring rate of 100r / min and an ice-water bath, add 1g of graphite and 0.4g of sodium nitrate to 30mL of sulfuric acid with a mass concentration of 98%, continue stirring for 15min, and use a water bath to heat up the mixture to a low temperature. At 10°C, add 4g of potassium permanganate and continue to stir for 1h; heat the water bath to 30°C and react for 1h; then add 15mL of deionized water, continue to stir for 15min, add 60mL of warm water at 30°C and 12mL with a mass concentration of 20% hydrogen peroxide, continue to stir for 10 minutes; ultrasonically disperse the above solution for 15 minutes and then filter, then wash with 5% hydrochloric acid and deionized water for 3 times, and dry the filtered product at 50°C to obtain 1.7g of graphite oxide .

[0042] (2) Weigh 100 mg of graphite oxide and dissolve it in 1 L of deionized water, and apply ultrasonic waves for 1 hour to obtain a graphene oxide aqueous solution with a concentra...

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Abstract

The invention discloses a graphene preparation method. The mixed solution of thiourea dioxide and soluable alkali or carbohydrazide and the soluable alkali is taken as a reducing agent to perform reduction-oxidation on the graphene aqueous solution, and evenly dispersed graphene powder is obtained after washing and drying. The graphene preparation method, disclosed by the invention, solves the problems that hydrazine hydrate and other existing reducing agents are high-toxic and not thorough in reduction, and the graphene is liable to gathering in the graphene preparation process. The preparation method is simple and feasible, is rapid in reaction process and moderate in reaction condition and has no special requirements to equipment, and the prepared graphene is of high quality.

Description

technical field [0001] The invention relates to the field of graphene preparation, in particular to a method for preparing graphene by reducing a graphene oxide aqueous solution by using a mixed solution of thiourea dioxide or carbohydrazide and a soluble strong base as a reducing agent. Background technique [0002] Graphene is made of sp 2 The single-layer two-dimensional material obtained by the arrangement of hybridized carbon atoms into a honeycomb lattice structure has a thickness of only 0.3554 nm and has many excellent properties. Studies have shown that the tensile strength and elastic modulus of graphene are 125 GPa and 1.1 TPa respectively, making it the material with the highest strength known so far; graphene has excellent electrical conductivity, and the carrier mobility at room temperature can reach 2×105 cm 2 / (V s), and does not decrease with temperature changes and chemical doping; the thermal conductivity of graphene at room temperature is 5×10 3 W / (m ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/19
Inventor 黄德欢石文荣邹鹏
Owner 吴江市华诚电子有限公司
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