CN105084346A - Method for preparing multi-layer graphene - Google Patents
Method for preparing multi-layer graphene Download PDFInfo
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- CN105084346A CN105084346A CN201410191779.XA CN201410191779A CN105084346A CN 105084346 A CN105084346 A CN 105084346A CN 201410191779 A CN201410191779 A CN 201410191779A CN 105084346 A CN105084346 A CN 105084346A
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Abstract
The invention relates to a method for preparing multi-layer graphene. The method comprises the following steps: (a) dissolving carboxymethyl cellulose and polyethylene glycol in deionized water, and stirring the solution until the solution is clear to obtain a dispersant; (b) adding expanded graphite into the dispersant which is cooled to room temperature along with stirring to obtain a suspension; and (c) adding the suspension into a nano-grinder for grinding to obtain the multi-layer graphene. The preparation method is simple, environment-friendly, low in price and non-toxic, can be used for preparing the graphene with maintained electron structure and crystal perfection and preparing a large amount of multi-layer graphene.
Description
Technical field
The present invention relates to the preparation method of multi-layer graphene.
Background technology
Graphene is the graphite film of monoatomic layer, and its lattice is the bi-dimensional cellular structure be made up of carbon atom.Graphene is the known best material of conductivity at normal temperatures at present, and electronics movement velocity wherein reaches 1/300 of the light velocity, considerably beyond general conductor.In addition, Graphene is rigid very, and its hardness is higher than diamond, and intensity is better than iron and steel, and ideal tensile strength can reach 110GPa ~ 130GPa.Graphene, except having special structure, also has many peculiar properties, is significantly thermal conductivity and physical strength.Meanwhile, Graphene is again a kind of very excellent semiconductor material, has a lot of carrier mobility higher than silicon.Graphene also has good light transmission, is the potential substitute products of conventional I TO film.Therefore, Graphene may be used for manufacturing matrix material, battery/super capacitor, hydrogen storage material, field emmision material, hypersensor etc.
The preparation method of Graphene mainly contains chemical reduction method, micromechanics stripping method and chemical vapor infiltration, and latter two method output is lower, higher to processing requirement.Therefore mainly chemical reagent reduction method is adopted at present.Chemical reagent reduction method take graphite oxide as raw material, usually uses the reduction-oxidation graphite such as reductive agent such as dimethylhydrazine, Resorcinol and sodium borohydride thus obtains Graphene.But these reductive agent toxicity are larger or inflammable, are unfavorable for the health of operator, operation is comparatively inconvenience also, and can introduce other functional groups and affect Graphene electronic structure and perfection of crystal.
Summary of the invention
The object of this invention is to provide the preparation method of multi-layer graphene, described preparation method be more simple, environmental protection and non-toxic inexpensive, and the Graphene keeping electronic structure and perfection of crystal can be obtained, also can obtain a large amount of multi-layer graphenes.
In view of this, the invention provides a kind of preparation method of multi-layer graphene, comprising:
A) dissolve CMC (carboxymethyl cellulose) and PEG (polyoxyethylene glycol) in deionized water, stir to clarify solution, obtain dispersion agent;
B) in the dispersion agent being cooled to room temperature, adding expanded graphite with stirring, obtaining suspension liquid;
C) suspension liquid is added in nano-level grinder grind, obtain multi-layer graphene.
According to a preferred embodiment of method of the present invention, described step, a) at 40 DEG C-70 DEG C, is preferably carried out at the temperature of 55 DEG C.
According to a preferred embodiment of method of the present invention, described step a) in, in solution, the massfraction of CMC is 10-15%, and preferably the massfraction of 15%, PEG is 20-25%, preferably 25%.
According to a preferred embodiment of method of the present invention, described step a) in, the molecular weight (number-average molecular weight) of CMC is 800,000g/mol to 1,200,000g/mol, preferably 1,000,000g/mol, the molecular weight (number-average molecular weight) of PEG is 1,000,000g/mol to 1,200,000g/mol, preferably 1,200,000g/mol.
According to a preferred embodiment of method of the present invention, at described step b) in, in suspension liquid, the massfraction of expanded graphite is 1%-10%, preferably 2%.
According to a preferred embodiment of method of the present invention, at described step c) in, nano-level grinder uses zirconium ball to grind, zirconium ball is of a size of 0.3-0.6mm, rotating speed is 8m/sec-16m/sec, preferred 10m/sec, and grinding temperature is 0 DEG C-40 DEG C, preferably 35 DEG C, vacuum tightness is 0.01MPa-0.05MPa, preferred 0.05MPa, and the brand and model of nano-level grinder is gloomyly strangle SNM05, milling time is 7-10h, preferably stops grinding when being less than the D90 granularity of 500nm.
The preparation method of multi-layer graphene provided by the present invention is more simple, environmental protection and non-toxic inexpensive, and can obtain the Graphene keeping electronic structure and perfection of crystal, also can obtain a large amount of multi-layer graphenes.
Accompanying drawing explanation
The grain size distribution (Malvern 2000) of the multi-layer graphene of Fig. 1 prepared by method according to the present invention.
Scanning electron microscope (SEM) figure (Hitachi SU8010) of the multi-layer graphene of Fig. 2 prepared by method according to the present invention.
Scanning electron microscope (SEM) figure (Hitachi SU8010) of the multi-layer graphene of Fig. 3 prepared by method according to the present invention.
Embodiment
In order to understand the present invention further, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just for further illustrating the features and advantages of the present invention, instead of the restriction to protection scope of the present invention.
Embodiment 1:
A) at the temperature of 70 DEG C, add CMC (Japanese first industrial pharmaceutical) and PEG (SANYO GS changes into) in deionized water, not stopping stirring makes it dissolve, thus the dispersion agent of preparation containing 10% massfraction CMC and 25% massfraction PEG;
B) expanded graphite Guo Neng nanosecond science and technology company limited produced and the dispersant being cooled to 25 DEG C, carry out ultrasonic 0.5h with ultrasonic generator (Shanghai sound is analysed) after stirring 20min, obtain the suspension liquid that expanded graphite concentration is 2% massfraction;
C) suspension liquid is put into SNM05 (Shanghai is gloomy strangles) nano-level grinder to grind, use and be of a size of 0.3mm zirconium ball, filling ratio is 75%, and rotating speed is 15m/sec, and milling time is about 7h, obtains multi-layer graphene.
Fig. 1-3 is respectively grain size distribution and the scanning electron microscope (SEM) photograph of the multi-layer graphene prepared according to the method for embodiment 1, wherein grain size distribution (the D10:143nm of the multi-layer graphene of Fig. 1 prepared by method according to the present invention, D50:220nm, D90:359nm); The scanning electron microscope (SEM) photograph of the multi-layer graphene of Fig. 2,3 prepared by method according to the present invention.
Can find out, expanded graphite has been stripped as multi-layer graphene, can by being further separated, the better graphene product of preparation homogeneity.
By dispersion agent involved in application present method, can by the means synthesizing multilayer Graphene of grinding, the method has less energy intensive, the advantage that output is larger, is comparatively easy to carry out industry popularization.
Claims (6)
1. a preparation method for multi-layer graphene, comprising:
A) dissolve carboxymethyl cellulose and polyoxyethylene glycol in deionized water, stir to clarify solution, obtain dispersion agent;
B) in the dispersion agent being cooled to room temperature, adding expanded graphite with stirring, obtaining suspension liquid;
C) suspension liquid is added in nano-level grinder grind, obtain multi-layer graphene.
2. the preparation method of multi-layer graphene according to claim 1, described step, a) at 40 DEG C-70 DEG C, is preferably carried out at the temperature of 55 DEG C.
3. the preparation method of multi-layer graphene according to claim 1, described step a) in, in solution, the massfraction of carboxymethyl cellulose is 10-15%, preferably 15%, the massfraction of polyoxyethylene glycol is 20-25%, preferably 25%.
4. the preparation method of multi-layer graphene according to claim 1, described step a) in, the number-average molecular weight of carboxymethyl cellulose is 800,000g/mol to 1,200,000g/mol, preferably 1,000,000g/mol, the number-average molecular weight of polyoxyethylene glycol is 1,000,000g/mol to 1,200,000g/mol, preferably 1,200,000g/mol.
5. the preparation method of multi-layer graphene according to claim 1, at described step b) in, in suspension liquid, the massfraction of expanded graphite is 1%-10%, preferably 2%.
6. the preparation method of multi-layer graphene according to claim 1, at described step c) in, nano-level grinder uses zirconium ball to grind, and zirconium ball is of a size of 0.3-0.6mm, rotating speed is 8m/sec-16m/sec, preferred 10m/sec, grinding temperature is 0 DEG C-40 DEG C, preferably 35 DEG C, vacuum tightness is 0.01MPa-0.05MPa, preferred 0.05MPa, milling time is 7-10h, preferably stops grinding when being less than the D90 granularity of 500nm.
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| CN201410191779.XA CN105084346A (en) | 2014-05-08 | 2014-05-08 | Method for preparing multi-layer graphene |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073751A (en) * | 2019-12-09 | 2020-04-28 | 上海烯望材料科技有限公司 | Application of lubricating oil detergent dispersant in preparation of graphene |
| CN111847433A (en) * | 2020-06-29 | 2020-10-30 | 深圳石墨烯创新中心有限公司 | Method for preparing graphene by using three-roller grinding machine |
| WO2022045286A1 (en) * | 2020-08-28 | 2022-03-03 | 京セラ株式会社 | Graphene dispersion, graphene resin powder, and battery |
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| CN103030138A (en) * | 2012-12-17 | 2013-04-10 | 鸿纳（东莞）新材料科技有限公司 | Folding preventing less-layer graphene powder, components of composite material thereof, and application |
| CN103466608A (en) * | 2013-09-11 | 2013-12-25 | 中南大学 | Ball milling preparation method of graphene |
| CN103738955A (en) * | 2014-01-13 | 2014-04-23 | 清华大学 | Expanded graphite environment-friendly material with Kish graphite as raw material as well as preparation method and application thereof |
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| CN103030138A (en) * | 2012-12-17 | 2013-04-10 | 鸿纳（东莞）新材料科技有限公司 | Folding preventing less-layer graphene powder, components of composite material thereof, and application |
| CN103466608A (en) * | 2013-09-11 | 2013-12-25 | 中南大学 | Ball milling preparation method of graphene |
| CN103738955A (en) * | 2014-01-13 | 2014-04-23 | 清华大学 | Expanded graphite environment-friendly material with Kish graphite as raw material as well as preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111073751A (en) * | 2019-12-09 | 2020-04-28 | 上海烯望材料科技有限公司 | Application of lubricating oil detergent dispersant in preparation of graphene |
| CN111847433A (en) * | 2020-06-29 | 2020-10-30 | 深圳石墨烯创新中心有限公司 | Method for preparing graphene by using three-roller grinding machine |
| WO2022045286A1 (en) * | 2020-08-28 | 2022-03-03 | 京セラ株式会社 | Graphene dispersion, graphene resin powder, and battery |
| CN115989282A (en) * | 2020-08-28 | 2023-04-18 | 京瓷株式会社 | Graphene dispersion liquid, graphene resin powder and battery |
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