Preparation method of graphene film

A graphene film, graphene technology, applied in the direction of graphene, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of poor composite quality, mechanical properties of composite films, influence of electrical conductivity, limited contact area, etc., to achieve bonding force Increase, improve mechanical strength and electrical and thermal conductivity, the effect of good strength

Inactive Publication Date: 2019-10-08

上海欣材科技有限公司

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Problems solved by technology

At present, the research on graphene and carbon nanotube composite materials has gradually emerged, the purpose of which is to give full play to the respective advantages of graphene and carbon nanotubes ...

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Abstract

The invention discloses a preparation method of a graphene film. The preparation method includes: preparing hydroxylated multiwalled carbon nanotubes, performing graphene surface modification, preparing a carbon nanotube-graphene compound solution, and preparing the graphene film in a spraying manner. The preparation method has the advantages that the carbon nanotubes and the graphene are integrated, and due to the fact that the graphene and the carbon nanotubes can have a synergistic effect, the mechanical strength, electric conductivity and thermal conductivity of the graphene film can be increased; by the hydroxylation of the multiwalled carbon nanotubes and the surface carboxylation of the graphene, binding force between the carbon nanotubes and the graphene is increased greatly by thereaction force between hydroxyl and carboxyl, and accordingly the graphene film is good in strength, toughness and electric conductivity.

Application Domain

Graphene

Technology Topic

Cvd grapheneCarboxylation +8

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Examples

Experimental program(2)

Example Embodiment

[0014] Example 1

[0015] A method for preparing graphene film, which is carried out according to the following steps:

[0016] (1) Preparation of hydroxylated multi-walled carbon nanotubes: Add multi-walled carbon nanotubes to a mixed solution of concentrated nitric acid and concentrated sulfuric acid. The volume ratio of concentrated nitric acid and concentrated sulfuric acid added in the mixed solution is 1:2, 60 Ultrasound at ℃ for 6h, then add deionized water to wash to pH=7, add ethylene glycol solution and potassium hydroxide solution dropwise successively, ultrasonically shake for 8h, wash and filter to pH=7, and dry to obtain surface hydroxylated multi-walled carbon Nanotubes; where the mass of multi-walled carbon nanotubes, the volume of ethylene glycol solution and the volume ratio of potassium hydroxide solution are 1g:45ml:5ml;

[0017] (2) Surface modification of graphene: Disperse graphene oxide in DMF ultrasonically, then add NaOH and succinic acid peroxide to continue ultrasonic, control the reaction temperature to 80℃, the reaction time is 2.5h, filter, wash and dry to obtain Carboxylated graphite oxide; among them, the ratio of graphene oxide, NaOH, succinic peroxide and DMF is: 1mmol:12mmol:12mmol:20ml; add surfactant to carboxylated graphite oxide, ultrasonic for 20min, then add Diazonium salt solution, add 2ml of 35-38wt% concentrated hydrochloric acid at 0-4℃, stir for 8h, then at room temperature for 6h, wash, filter, and dry to obtain surface carboxylated graphene. Among them, the carboxyl group The volume ratio of graphite oxide to diazonium salt solution is 1g:0.8ml;

[0018] (3) Preparation of carbon nanotube-graphene composite solution: After ball milling hydroxylated multi-walled carbon nanotubes, 2wt% Triton was added, and after 2 hours of dispersion under ultrasound, hydroxylated multi-walled carbon with a concentration of 4 mg/ml was obtained. Nanotube suspension; adding thionyl chloride and the surface carboxylated graphene in step (3) to the suspension, stirring continuously for 5 hours at 50°C, and filtering to obtain a carbon nanotube-graphene composite liquid; Among them, the ratio of hydroxylated multi-walled carbon nanotubes, graphene with surface carboxylation and thionyl chloride is 1g:1.2g:0.1ml;

[0019] (4) Spray the carbon nanotube-graphene composite liquid on a clean glass plate, use a film spreader to spread the film with a certain thickness, and then put it in an oven to prepare a graphene film with a stepwise temperature program, and then rewind after drying. Form a coil.

Example Embodiment

[0020] Example 2

[0021] A method for preparing graphene film, which is carried out according to the following steps:

[0022] (1) Preparation of hydroxylated multi-walled carbon nanotubes: Add multi-walled carbon nanotubes to a mixed solution of concentrated nitric acid and concentrated sulfuric acid. The volume ratio of concentrated nitric acid and concentrated sulfuric acid to the mixed solution is 1:3, 50℃ Under ultrasonic for 8h, then add deionized water to wash to pH=7, add ethylene glycol solution and potassium hydroxide solution dropwise in turn, ultrasonically shake for 5-12h, wash and filter to pH=7, and dry to obtain surface hydroxylated multi-wall Carbon nanotubes; where the mass of multi-walled carbon nanotubes, the volume of ethylene glycol solution and the volume ratio of potassium hydroxide solution are 1g:50ml:3ml;

[0023] (2) Surface modification of graphene: Disperse graphene oxide in DMF ultrasonically, then add NaOH and succinic acid peroxide to continue ultrasonic, control the reaction temperature to 75-90℃, the reaction time is 3h, filter, wash, and dry Obtain carboxylated graphite oxide; among them, the ratio of graphene oxide, NaOH, succinic peroxide and DMF is: 1mmol:10mmol:10mmol:20ml; add surfactant to carboxylated graphite oxide, ultrasonic for 15min, then Add the diazonium salt solution, add 2.5ml of 35-38wt% concentrated hydrochloric acid at 0-4°C, stir for 10h, then at room temperature for 8h, wash, filter, and dry to obtain surface carboxylated graphene. , The volume ratio of carboxylated graphite oxide to diazonium salt solution is 1g:0.9ml;

[0024] (3) Preparation of carbon nanotube-graphene composite solution: After ball milling hydroxylated multi-walled carbon nanotubes, 2wt% Triton was added, and after 2.5 hours of dispersion under ultrasound, a hydroxylated multi-walled concentration of 5mg/ml was obtained. Suspension of carbon nanotubes; adding thionyl chloride and the graphene with surface carboxylation in step (3) to the suspension, stirring for 6 hours at 60°C, and filtering to obtain a carbon nanotube-graphene composite liquid ; Among them, the ratio between hydroxylated multi-walled carbon nanotubes, surface carboxylated graphene and thionyl chloride is 1g:1.5g:0.2ml;

[0025] (4) Spray the carbon nanotube-graphene composite liquid on a clean glass plate, use a film spreader to spread the film with a certain thickness, and then put it in an oven to prepare a graphene film with a stepwise temperature program, and then rewind after drying. Form a coil.

[0026] After testing, the performance test indexes of the graphene films of Examples 1 and 2 are shown in Table 1:

[0027] Table 1

[0028]

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Classification and recommendation of technical efficacy words

Improve binding
Improve mechanical strength and electrical and thermal conductivity

Preparation method of graphene film

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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