CN106082178A - A kind of method preparing graphene film on insulating body - Google Patents

A kind of method preparing graphene film on insulating body Download PDF

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Publication number
CN106082178A
CN106082178A CN201610381337.0A CN201610381337A CN106082178A CN 106082178 A CN106082178 A CN 106082178A CN 201610381337 A CN201610381337 A CN 201610381337A CN 106082178 A CN106082178 A CN 106082178A
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China
Prior art keywords
acid
insulating body
graphene film
graphene
graphene oxide
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CN201610381337.0A
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CN106082178B (en
Inventor
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 method that one-step method prepares graphene film on insulating body.By by water-heat process process in the graphene oxide solution containing weak acid for the insulating body, homogeneous graphene film can be obtained at matrix surface.This preparation method is simple and easy to control without valuable instrument and equipment, process, low cost, it is easy to promote.It is loaded with the insulating body of graphene film, can serve as the device of electricity or electrochemistry, have very extensive potential using value.

Description

A kind of method preparing graphene film on insulating body
Technical field
The present invention relates to a kind of method preparing graphene film on insulating body, be specifically related on insulating body straight The thermally grown graphene film of water receiving, relates generally to electricity or the technical field such as electrochemical device, surface modification modification.
Background technology
Graphene (Graphene) is the new material of a kind of individual layer laminated structure being made up of carbon atom, its by carbon atom with Sp2 hybridized orbit composition hexangle type is the flat film of honeycomb lattice, is the two-dimensional material of only one of which carbon atom thickness.Graphite Alkene has a series of performances such as excellent mechanical performance, electric conductivity, very high specific surface area.
At present, grapheme material has obtained extensive concern and research, thus becomes focus, and wherein graphene film by It is subject to favor especially in being advantageously implemented device especially.Report a kind of electrochemical deposition method at matrix table in front patent Face prepare Graphene method [Luo Shenglian, Liu Chengbin, Tang Yanhong, Liu Ronghua, Teng Yarong, sweet, Zhang Xilin. a kind of Graphene The preparation method of film. CN102051651A];The method utilizing CVD method to prepare Graphene [appoints literary talent, high Reeb, Malaysia Roc etc. the chemical vapour deposition technique of Graphene prepares [J]. novel charcoal material, 2011,26 (1): 71-80], but both Method is all only applicable to the matrix of conduction, and particularly CVD is only applicable to a small amount of metallic matrix such as nickel and copper.In another patent In, utilize the method for suction filtration obtained graphene film [once outstanding, Zheng Yaxuan, Wang Han, British philosopher, Pei Songfeng, appoint literary talent, Cheng Huiming. A kind of preparation method of Graphene heating film. CN103607795A], but this method is only capable of obtaining thicker film, and It is difficult to realize large area masking.
Content of the invention
Based on the deficiency in first technology, the present invention proposes a kind of method preparing graphene film on insulating body. By introducing weak acid, graphene film can be prepared on insulating body surface, deposited graphite alkene conduction on insulating body Layer can change its surface conductivity.
The technical solution of the present invention is as follows:
A kind of method preparing graphene film on insulating body, comprises the steps:
(1) graphene oxide water solution containing weak acid for the preparation;
(2) join the mixed solution preparing in step (1) in water heating kettle liner, and insulating body is immersed mixed solution In, after tightening stainless steel outer sleeve, carrying out hydro-thermal process, hydrothermal temperature scope is 90 ° of C ~ 220 ° C, and hydrothermal conditions is 18 ~ 30 h;
(3) after hydro-thermal process terminates and cools down, matrix is taken out, dry after cleaning, obtain the insulation of superficial growth graphene film Matrix.
Further, the concentration of described graphene oxide water solution is 0.4 ~ 1 mg/mL.
Further, described weak acid is acetic acid, boric acid, phosphoric acid, salicylic acid, citric acid, one or more in lactic acid, weak The concentration range of acid is: 0.01 ~ 0.5 mol/L.
Further, described insulating body is pottery, glass, quartz, silica, carborundum, plastics, fluoropolymer resin Deng insulating materials.
Brief description
Fig. 1 processes, in the graphene oxide solution adding acetic acid, the graphene film obtaining
Fig. 2 processes, in the graphene oxide solution adding citric acid, the graphene film obtaining
Fig. 3 processes, in the graphene oxide solution adding phosphoric acid, the graphene film obtaining
Detailed description of the invention
Prepare the detailed description of the invention of graphene film on insulating body of the present invention introduced below, however it is necessary that and point out, this The protection domain of invention is not limited to this.
Embodiment 1
Weigh the graphene oxide (GO) of 20 mg, join in deionized water, ultrasonic 30 minutes, in solution, add 1 mmol Acetic acid, is subsequently adding deionized water and is configured to the aqueous solution of 50 mL.This solution is stirred after 10 minutes ultrasonic 30 minutes.Subsequently Above-mentioned mixed solution is transferred in 100 mL water heating kettles, and put in substrate (holding is disposed vertically) immersion dispersion liquid, 200 Hydro-thermal reaction 24 hours under ° C temperature conditions, when temperature is down to room temperature, takes out product, after deionized water cleaning-drying, To graphene film, result is as shown in Figure 1.
Embodiment 2
Weigh the graphene oxide (GO) of 20 mg, join in deionized water, ultrasonic 30 minutes, in solution, add 1 mmol Acetic acid, is subsequently adding deionized water and is configured to the aqueous solution of 50 mL.This solution is stirred after 10 minutes ultrasonic 30 minutes.Subsequently Above-mentioned mixed solution is transferred in 100 mL water heating kettles, and put in substrate (holding is disposed vertically) immersion dispersion liquid, 180 Hydro-thermal reaction 30 hours under ° C temperature conditions, when temperature is down to room temperature, takes out product, after cleaning by deionized water, is placed in room Temperature natural drying obtains growing the potsherd matrix of graphene film.
Embodiment 3
Weigh the graphene oxide (GO) of 20 mg, join in deionized water, ultrasonic 30 minutes, in solution, add 1 mmol Citric acid, is subsequently adding deionized water and is configured to the aqueous solution of 50 mL.This solution is stirred after 10 minutes ultrasonic 30 minutes.With After transfer to above-mentioned mixed solution in 100 mL water heating kettles, and put into substrate (holding is disposed vertically) and immerse in dispersion liquid, Hydro-thermal reaction 24 hours under 200 ° of C temperature conditionss, when temperature is down to room temperature, takes out product, uses deionized water cleaning-drying After, obtaining graphene film, result is as shown in Figure 2.
Embodiment 4
Weigh the graphene oxide (GO) of 20 mg, join in deionized water, ultrasonic 30 minutes, in solution, add 1 mmol Phosphoric acid, is subsequently adding deionized water and is configured to the aqueous solution of 50 mL.This solution is stirred after 10 minutes ultrasonic 30 minutes.Subsequently Above-mentioned mixed solution is transferred in 100 mL water heating kettles, and put in substrate (holding is disposed vertically) immersion dispersion liquid, 200 Hydro-thermal reaction 24 hours under ° C temperature conditions, when temperature is down to room temperature, takes out product, after deionized water cleaning-drying, To graphene film, result is as shown in Figure 3.
Embodiment 5
Weigh the graphene oxide (GO) of 20 mg, join in deionized water, ultrasonic 30 minutes, in solution, add 10 mmol Phosphoric acid, is subsequently adding deionized water and is configured to the aqueous solution of 50 mL.This solution is stirred after 10 minutes ultrasonic 30 minutes.Subsequently Above-mentioned mixed solution is transferred in 100 mL water heating kettles, and put in substrate (holding is disposed vertically) immersion dispersion liquid, 200 Hydro-thermal reaction 24 hours under ° C temperature conditions, when temperature is down to room temperature, takes out product, after deionized water cleaning-drying, To graphene film.

Claims (4)

1. the method growing graphene film on insulating body, it is characterised in that comprise the steps:
(1) graphene oxide water solution containing weak acid for the preparation;
(2) join the mixed solution preparing in step (1) in water heating kettle liner, and insulating body is immersed mixed solution In, after tightening stainless steel outer sleeve, carrying out hydro-thermal process, hydrothermal temperature scope is 90 ° of C ~ 220 ° C, and hydrothermal conditions is 18 ~ 30 h;
(3) after hydro-thermal process terminates and cools down, matrix is taken out, dry after cleaning, obtain the insulation of superficial growth graphene film Matrix.
2. method according to claim 1, it is characterised in that the concentration of graphene oxide water solution is 0.4 ~ 1 mg/mL.
3. method according to claim 1, it is characterised in that weak acid be acetic acid, boric acid, phosphoric acid, salicylic acid, citric acid, One or more in lactic acid, the concentration range of weak acid is: 0.01 ~ 0.5 mol/L.
4. method according to claim 1, it is characterised in that described insulating body is pottery, glass, quartz, dioxy The insulating materials such as SiClx, carborundum, plastics, fluoropolymer resin.
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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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108461309A (en) * 2018-04-25 2018-08-28 山西大学 A kind of preparation method of graphene film electrode material
CN109227791A (en) * 2018-08-31 2019-01-18 徐培培 A kind of waterproof pluwood
WO2019149018A1 (en) * 2018-02-05 2019-08-08 庄鹏宇 Preparation method of reduced graphene oxide film
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 (3)

* 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
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 (3)

* 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
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

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019149018A1 (en) * 2018-02-05 2019-08-08 庄鹏宇 Preparation method of reduced graphene oxide film
CN108461309A (en) * 2018-04-25 2018-08-28 山西大学 A kind of preparation method of graphene film electrode material
CN108461309B (en) * 2018-04-25 2019-09-24 山西大学 A kind of preparation method of graphene film electrode material
CN109227791A (en) * 2018-08-31 2019-01-18 徐培培 A kind of waterproof pluwood
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

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