CN103641104A - Preparation method of graphene - Google Patents

Preparation method of graphene Download PDF

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Publication number
CN103641104A
CN103641104A CN201310592048.1A CN201310592048A CN103641104A CN 103641104 A CN103641104 A CN 103641104A CN 201310592048 A CN201310592048 A CN 201310592048A CN 103641104 A CN103641104 A CN 103641104A
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graphene
preparation
graphite
oxidized
oxidation
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CN201310592048.1A
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简玉君
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Abstract

The invention provides a preparation method of graphene, the preparation method comprises the following steps: a, graphite is oxidized into oxidized graphite by an oxidation reaction; b, oxidized graphene is formed by ultrasonic stripping of the oxidized graphite; c, then a reducing agent is added for reduction to obtain the graphene. The beneficial effects of the preparation method are that mass production of the grapheme can be achieved by a chemical oxidation and reduction method, the intermediate product oxidized graphene is good in dispersibility in water, and modification and functionalization of the grapheme are easy to realize, so that the preparation method is often used in composite materials, energy storage and other studies.

Description

The preparation method of Graphene
Technical field
The invention belongs to chemical field, particularly a kind of preparation method of Graphene.
Background technology
Graphene is the thinnest a kind of in known materials, and material is very firmly hard, and in room temperature situation, the speed of transmitting electronics is all faster than known conductor.The atomic size structure of Graphene is very special, must just can describe by quantum field theory.
Graphene is a kind of two dimensional crystal, and the common graphite of people is stacking and form by the plane carbon atom of arranging with honeycomb-patterned ordered from level to level, the interlaminar action power of graphite a little less than, be easy to peel off mutually, form very thin graphite flake.After graphite flake is shelled into individual layer, this to only have the individual layer of a carbon atom thickness be exactly Graphene.Development History.First: Graphene is the material of intensity maximum in the world up to now, if make with Graphene the film (thickness approximately 100 nanometers) that thickness is equivalent to bread and cheese plastic packaging bag thickness according to measuring and calculating, it can bear the pressure of about two tons of heavy articles so, and be unlikely to fracture; Second: Graphene is electroconductibility best material in the world.
The range of application of Graphene is wide.Ultra-thin according to Graphene, the characteristic of intensity super large, Graphene can be widely used in each field, such as ultralight flak jackets, ultra-thin and ultra-light type aircraft material etc.According to its excellent electroconductibility, make it at microelectronic, also there is huge application potential.Graphene likely can become the substitute of silicon, manufactures superminiature transistor, is used for producing following supercomputer, and the electronic mobility that carbon is higher can make following computer obtain higher speed.Grapheme material or a kind of good properties-correcting agent in addition, at new energy field as aspect ultracapacitor, lithium ion battery, due to its highly conc, high-specific surface area, applicable to appearing in laboratory as electrode materials auxiliary agent Graphene, be in 2004, at that time, two of Univ Manchester UK scientist An Delie Jim and the Ke Siteyanuowo Lip river husband that disappears found that they can obtain more and more thinner graphite flake by a kind of very simple method.They separate graphite flake from graphite, then the two sides of thin slice are bonded on a kind of special adhesive tape, tear adhesive tape, just graphite flake can be divided into two.Constantly operation like this, so thin slice is more and more thinner, last, they have obtained the thin slice only consisting of one deck carbon atom, Here it is Graphene.After this, the novel method of preparing Graphene emerges in an endless stream, and the development through 5 years, it is found that, the field of Graphene being brought into suitability for industrialized production comes within a measurable distance.Therefore, two people obtained Nobel Prize in physics in 2010.
The scientific circles that appear at of Graphene have evoked huge great waves, it is found that, Graphene has unusual conductivity, exceeds the intensity of iron and steel decades of times and fabulous light transmission, and its appearance is expected to cause one at hyundai electronics sciemtifec and technical sphere and takes turns revolution.In Graphene, electronics can move very efficiently, and traditional semi-conductor and conductor, and for example silicon and the copper Graphene that is far from puts up a good show.Collision due to electronics and atom, traditional semi-conductor and conductor have discharged some energy by hot form, general computer chips in 2013 have been wasted the electric energy of 72%-81% by this way, Graphene is different, its electron energy can not be depleted, and this makes it have the good characteristic being not of the common run.
Summary of the invention
Object of the present invention provides a kind of preparation method of Graphene, to solve the problem of prior art.
The present invention is by the following technical solutions:
A preparation method for Graphene, comprises the following steps:
A, to utilize oxidizing reaction be graphite oxide by graphite oxidation;
Graphite after b, oxidation forms graphene oxide by ultrasonic peeling off;
C, then add reductive agent to reduce, thereby obtain Graphene.
In step a, method for oxidation is: Brodie method, Staudenmaier method and Hummers method.
In step c, reductive agent is a kind of of hydrazine hydrate, NaBH and the ultrasonic reduction of highly basic
In step c, add ammoniacal liquor.
The invention has the beneficial effects as follows: by chemistry redox method, can realize the preparation in enormous quantities of Graphene, and the dispersiveness of intermediate product graphene oxide in water is better, be easy to realize the modification of Graphene and functionalization, so the method is often used in the researchs such as matrix material, energy storage.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not intended to limit the present invention.
A preparation method for Graphene, comprises the following steps:
1, utilizing oxidizing reaction is graphite oxide by graphite oxidation; By introduce oxygen-containing functional group on graphite carbon atom between layers, increase interlamellar spacing, and then weaken the interaction of interlayer; Method for oxidation is: Brodie method, Staudenmaier method and Hummers method, its principle is all first with strong acid, graphite to be processed, and then adds strong oxidizer to be oxidized.
2, the graphite after oxidation forms graphene oxide by ultrasonic peeling off,
3, then add reductive agent to reduce, thereby obtain Graphene.Reductive agent is hydrazine hydrate, NaBH and the ultrasonic reduction of highly basic etc.Because price comparison is expensive and easy residual B element, although and the ultrasonic reduction of highly basic is simple to operate and compared with environmental protection, be difficult to reduction thoroughly, after reduction, conventionally have the residual of a large amount of oxygen-containing functional groups, thereby conventionally adopt more cheap hydrazine hydrate to carry out reduction-oxidation graphite.The advantage of hydrazine hydrate reduction is reducing power by force and hydrazine hydrate is easy to volatilization, can residual impurity in product.
In step c, add ammoniacal liquor, improve on the one hand the reducing power of hydrazine hydrate, can make on the other hand the surface of Graphene mutually repel because of electronegative, and then reduce the reunion of Graphene.
By chemistry redox method, can realize the preparation in enormous quantities of Graphene, and the dispersiveness of intermediate product graphene oxide in water is better, be easy to realize the modification of Graphene and functionalization, so the method is often used in the researchs such as matrix material, energy storage.
Although above-mentioned, the specific embodiment of the present invention is described in conjunction with the embodiments; but be not limiting the scope of the invention; one of ordinary skill in the art should be understood that; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that performing creative labour can make or distortion still within protection scope of the present invention.

Claims (4)

1. a preparation method for Graphene, is characterized in that: comprise the following steps:
A, to utilize oxidizing reaction be graphite oxide by graphite oxidation;
Graphite after b, oxidation forms graphene oxide by ultrasonic peeling off;
C, then add reductive agent to reduce, thereby obtain Graphene.
2. the preparation method of Graphene as claimed in claim 1, is characterized in that: in step a, method for oxidation is: Brodie method, Staudenmaier method and Hummers method.
3. the preparation method of Graphene as claimed in claim 1, is characterized in that: in step c, reductive agent is a kind of of hydrazine hydrate, NaBH and the ultrasonic reduction of highly basic.
4. the preparation method of Graphene as claimed in claim 1, is characterized in that: in step c, add ammoniacal liquor.
CN201310592048.1A 2013-11-22 2013-11-22 Preparation method of graphene Pending CN103641104A (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103969310A (en) * 2014-05-22 2014-08-06 陕西省环境科学研究院 Graphene-modified glassy carbon electrode and application of glassy carbon electrode in determination of diosgenin content
CN104561962A (en) * 2014-12-24 2015-04-29 天津大学 Preparation method for aluminum and aluminum alloy surface coating
CN104634842A (en) * 2015-02-13 2015-05-20 西安石油大学 Method for preparing electrode modified by copper/graphene nanocomposite and application of modified electrode
CN105836855A (en) * 2016-06-13 2016-08-10 西安工业大学 Preparation method and application of graphene gas diffusion electrode
CN106037735A (en) * 2016-07-07 2016-10-26 苏州海神联合医疗器械有限公司 High-conductivity electrode applicable to electromyography-evoked potential equipment
CN108046249A (en) * 2017-12-19 2018-05-18 昆明理工大学 A kind of preparation method of graphene
CN108178939A (en) * 2018-01-31 2018-06-19 天津北方石墨烯产业研究院 It is a kind of for graphene dispersing solution of oil pipe anti-corrosive coating and preparation method thereof
CN110078063A (en) * 2019-04-25 2019-08-02 广东博智林机器人有限公司 The preparation method of redox graphene dispersion liquid and the device with graphite ene coatings
CN111892043A (en) * 2020-08-06 2020-11-06 昆明理工大学 Method for preparing reduced graphene oxide by one-pot method
CN113308172A (en) * 2021-06-08 2021-08-27 南京工程学院 Preparation and use method of composite anticorrosive paint for cable-stayed bridge inhaul cable
CN113860888A (en) * 2021-11-04 2021-12-31 四川恒力盛泰石墨烯科技有限公司 Preparation method of graphene heat dissipation film for electronic equipment

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103969310B (en) * 2014-05-22 2016-10-05 陕西省环境科学研究院 Graphene modified glass-carbon electrode and the application in measuring turmeric saponin content thereof
CN103969310A (en) * 2014-05-22 2014-08-06 陕西省环境科学研究院 Graphene-modified glassy carbon electrode and application of glassy carbon electrode in determination of diosgenin content
CN104561962A (en) * 2014-12-24 2015-04-29 天津大学 Preparation method for aluminum and aluminum alloy surface coating
CN104634842A (en) * 2015-02-13 2015-05-20 西安石油大学 Method for preparing electrode modified by copper/graphene nanocomposite and application of modified electrode
CN105836855B (en) * 2016-06-13 2019-02-15 西安工业大学 A kind of preparation method and application of graphene gas-diffusion electrode
CN105836855A (en) * 2016-06-13 2016-08-10 西安工业大学 Preparation method and application of graphene gas diffusion electrode
CN106037735A (en) * 2016-07-07 2016-10-26 苏州海神联合医疗器械有限公司 High-conductivity electrode applicable to electromyography-evoked potential equipment
CN108046249A (en) * 2017-12-19 2018-05-18 昆明理工大学 A kind of preparation method of graphene
CN108178939A (en) * 2018-01-31 2018-06-19 天津北方石墨烯产业研究院 It is a kind of for graphene dispersing solution of oil pipe anti-corrosive coating and preparation method thereof
CN110078063A (en) * 2019-04-25 2019-08-02 广东博智林机器人有限公司 The preparation method of redox graphene dispersion liquid and the device with graphite ene coatings
CN111892043A (en) * 2020-08-06 2020-11-06 昆明理工大学 Method for preparing reduced graphene oxide by one-pot method
CN113308172A (en) * 2021-06-08 2021-08-27 南京工程学院 Preparation and use method of composite anticorrosive paint for cable-stayed bridge inhaul cable
CN113860888A (en) * 2021-11-04 2021-12-31 四川恒力盛泰石墨烯科技有限公司 Preparation method of graphene heat dissipation film for electronic equipment

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