CN106082178B - A method of preparing graphene film on insulating body - Google Patents

A method of preparing graphene film on insulating body Download PDF

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Publication number
CN106082178B
CN106082178B CN201610381337.0A CN201610381337A CN106082178B CN 106082178 B CN106082178 B CN 106082178B CN 201610381337 A CN201610381337 A CN 201610381337A CN 106082178 B CN106082178 B CN 106082178B
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China
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insulating body
acid
graphene film
graphene
graphene oxide
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CN106082178A (en
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赵崇军
王圣琪
邵肖肖
马越
赵莉
钱秀珍
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East China University of Science and Technology
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East China University of Science and Technology
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Abstract

The invention discloses a kind of methods that one-step method prepares graphene film on insulating body.By handling water-heat process of the insulating body in the graphene oxide solution containing weak acid, uniform graphene film can be obtained in matrix surface.The preparation method is simple and easy to control, at low cost without valuable instrument and equipment, process, easy to spread.Load has the insulating body of graphene film, may be used as the device of electricity or electrochemistry, there is very extensive potential using value.

Description

A method of preparing graphene film on insulating body
Technical field
The method that the present invention relates to a kind of to prepare graphene film on insulating body, and in particular to straight on insulating body The thermally grown graphene film of water receiving relates generally to the technical fields such as electricity or electrochemical device, surface modification.
Background technique
Graphene (Graphene) is a kind of new material of individual layer laminated structure being made of carbon atom, by carbon atom with Sp2 hybridized orbit forms the flat film that hexangle type is in honeycomb lattice, is the two-dimensional material of only one carbon atom thickness.Graphite Alkene has a series of performances such as excellent mechanical performance, electric conductivity, very high specific surface area.
Currently, grapheme material has obtained extensive concern and research, to become hot spot, and wherein graphene film by It is even more by favor especially in being advantageously implemented device.A kind of electrochemical deposition method is reported in preceding patent in matrix table Wheat flour for graphene method [Luo Shenglian, Liu Chengbin, Tang Yanhong, Liu Ronghua, Teng Yarong, a kind of sweet, graphene of Zhang Xilin The preparation method CN102051651A of film];Method [Ren Wencai, Gao Libo, the Malaysia of graphene are prepared using CVD method The chemical vapour deposition technique of the graphene such as roc prepares [J] novel charcoal material, 2011,26 (1): 71-80], however both Method is all only applicable to conductive matrix, and especially CVD is only applicable to a small amount of metallic matrix such as nickel and copper.In another patent In, graphene film [once outstanding, Zheng Yaxuan, Wang Han, British philosopher, Pei Songfeng, Ren Wencai, Cheng Huiming have been obtained using the method for suction filtration A kind of preparation method CN103607795A of graphene heating film], but this method is only capable of obtaining thicker film, and Large area film difficult to realize.
Summary of the invention
Based on the deficiency in first technology, the present invention proposes a kind of method that graphene film is prepared on insulating body. By introducing weak acid, graphene film can be prepared on insulating body surface, graphene conductive is deposited on insulating body Layer can change its surface conductivity.
Technical solution of the invention is as follows:
A method of it preparing graphene film on insulating body, includes the following steps:
(1) graphene oxide water solution containing weak acid is prepared;
(2) mixed solution obtained in step (1) is added in water heating kettle liner, and insulating body immersion mixing is molten In liquid, after tightening stainless steel outer sleeve, hydro-thermal process is carried out, hydrothermal temperature range is 90 °C ~ 220 °C, hydrothermal conditions For 18 ~ 30 h;
(3) hydro-thermal process terminates and takes out matrix after cooling down, and dries after cleaning, obtains surface growth graphene film Insulating body.
Further, the concentration of the graphene oxide water solution is 0.4 ~ 1 mg/mL.
Further, the weak acid be one or more of acetic acid, boric acid, phosphoric acid, salicylic acid, citric acid, lactic acid, it is weak The concentration range of acid are as follows: 0.01 ~ 0.5 mol/L.
Further, the insulating body is ceramics, glass, quartz, silica, silicon carbide, plastics, fluoropolymer resin Equal insulating materials.
Detailed description of the invention
The graphene film that Fig. 1 is handled in the graphene oxide solution that acetic acid is added
The graphene film that Fig. 2 is handled in the graphene oxide solution that citric acid is added
The graphene film that Fig. 3 is handled in the graphene oxide solution that phosphoric acid is added
Specific embodiment
The specific embodiment of graphene film is prepared on insulating body of the present invention introduced below, however it is to be noted that, this The protection scope of invention is not limited to this.
Embodiment 1
The graphene oxide (GO) for weighing 20 mg, is add to deionized water, and 1 is added into solution for ultrasound 30 minutes Then the aqueous solution that deionized water is configured to 50 mL is added in mmol acetic acid.Solution stirring is 30 minutes ultrasonic after ten minutes. Then above-mentioned mixed solution is transferred in 100 mL water heating kettles, and is put into substrate (holding is disposed vertically) and immerses in dispersion liquid, Thermal response is lauched 24 hours in 200 °C of temperature conditions, when temperature is down to room temperature, is taken out product, is cleaned and dried with deionized water Afterwards, graphene film is obtained, as a result as shown in Figure 1.
Embodiment 2
The graphene oxide (GO) for weighing 20 mg, is add to deionized water, and 1 is added into solution for ultrasound 30 minutes Then the aqueous solution that deionized water is configured to 50 mL is added in mmol acetic acid.Solution stirring is 30 minutes ultrasonic after ten minutes. Then above-mentioned mixed solution is transferred in 100 mL water heating kettles, and is put into substrate (holding is disposed vertically) and immerses in dispersion liquid, Thermal response is lauched 30 hours in 180 °C of temperature conditions, when temperature is down to room temperature, takes out product, after being cleaned with deionized water, It is placed in natural drying at room temperature and obtains the ceramic sheet matrix of growth graphene film.
Embodiment 3
The graphene oxide (GO) for weighing 20 mg, is add to deionized water, and 1 is added into solution for ultrasound 30 minutes Then the aqueous solution that deionized water is configured to 50 mL is added in mmol citric acid.Solution stirring is 30 points ultrasonic after ten minutes Clock.Then above-mentioned mixed solution is transferred in 100 mL water heating kettles, and is put into substrate (holding is disposed vertically) and immerses dispersion liquid In, thermal response is lauched 24 hours in 200 °C of temperature conditions, when temperature is down to room temperature, is taken out product, is cleaned with deionized water After drying, graphene film is obtained, as a result as shown in Figure 2.
Embodiment 4
The graphene oxide (GO) for weighing 20 mg, is add to deionized water, and 1 is added into solution for ultrasound 30 minutes Then the aqueous solution that deionized water is configured to 50 mL is added in mmol phosphoric acid.Solution stirring is 30 minutes ultrasonic after ten minutes. Then above-mentioned mixed solution is transferred in 100 mL water heating kettles, and is put into substrate (holding is disposed vertically) and immerses in dispersion liquid, Thermal response is lauched 24 hours in 200 °C of temperature conditions, when temperature is down to room temperature, is taken out product, is cleaned and dried with deionized water Afterwards, graphene film is obtained, as a result as shown in Figure 3.
Embodiment 5
The graphene oxide (GO) for weighing 20 mg, is add to deionized water, and 10 are added into solution for ultrasound 30 minutes Then the aqueous solution that deionized water is configured to 50 mL is added in mmol phosphoric acid.Solution stirring is 30 minutes ultrasonic after ten minutes. Then above-mentioned mixed solution is transferred in 100 mL water heating kettles, and is put into substrate (holding is disposed vertically) and immerses in dispersion liquid, Thermal response is lauched 24 hours in 200 °C of temperature conditions, when temperature is down to room temperature, is taken out product, is cleaned and dried with deionized water Afterwards, graphene film is obtained.

Claims (2)

1. a kind of method for growing graphene film on insulating body, it is characterised in that include the following steps:
(1) graphene oxide water solution containing weak acid is prepared, weak acid is acetic acid, boric acid, phosphoric acid, salicylic acid, citric acid, lactic acid One or more of, the concentration range of weak acid are as follows: 0.01~0.5mol/L;
(2) mixed solution obtained in step (1) is added in water heating kettle liner, and insulating body is immersed into mixed solution In, after tightening stainless steel outer sleeve, carry out hydro-thermal process, hydrothermal temperature range be 90 DEG C~220 DEG C, hydrothermal conditions be 18~ 30 hours;Insulating body is one of ceramics, glass, quartz, silica, silicon carbide, plastics;
(3) hydro-thermal process terminates and takes out matrix after cooling down, and dries after cleaning, obtains the insulation of surface growth graphene film Matrix.
2. the method according to claim 1, wherein the concentration of graphene oxide water solution is 0.4~1mg/mL.
CN201610381337.0A 2016-06-01 2016-06-01 A method of preparing graphene film on insulating body Expired - Fee Related CN106082178B (en)

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CN110117003A (en) * 2018-02-05 2019-08-13 庄鹏宇 A kind of preparation method of redox graphene film
CN108461309B (en) * 2018-04-25 2019-09-24 山西大学 A kind of preparation method of graphene film electrode material
CN109227791B (en) * 2018-08-31 2021-04-02 贵港市鼎源木业有限公司 Waterproof plywood
CN110734054A (en) * 2019-11-21 2020-01-31 泰州莱宝利复合材料科技有限公司 Preparation method of graphene films

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515144A (en) * 2011-12-23 2012-06-27 哈尔滨工业大学 Method for preparing porous carbon microspheres converted from graphene
CN104245578A (en) * 2012-03-09 2014-12-24 巴斯夫欧洲公司 Aerogel based on doped graphene

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WO2015009758A1 (en) * 2013-07-17 2015-01-22 Peerless Worldwide, Llc Process for the synthesis of graphene and graphene derivatives from so-called greenhouse gasses and other carbonaceous waste products

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102515144A (en) * 2011-12-23 2012-06-27 哈尔滨工业大学 Method for preparing porous carbon microspheres converted from graphene
CN104245578A (en) * 2012-03-09 2014-12-24 巴斯夫欧洲公司 Aerogel based on doped graphene

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