CN107539977A - The preparation method of bilayer graphene - Google Patents
The preparation method of bilayer graphene Download PDFInfo
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- CN107539977A CN107539977A CN201710953818.9A CN201710953818A CN107539977A CN 107539977 A CN107539977 A CN 107539977A CN 201710953818 A CN201710953818 A CN 201710953818A CN 107539977 A CN107539977 A CN 107539977A
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Abstract
The invention discloses a kind of preparation method of bilayer graphene, after graphite of the purity more than 70% is clayed into power, it is placed in strong oxidant solution after stirring 10min-20min repeatedly, obtain containing a large amount of Cl, MnO4, SO 2-graphite mixed emulsion I, the strong oxidizer is the one or more in the concentrated sulfuric acid, concentrated hydrochloric acid or permanganic acid, the beneficial effects of the invention are as follows：A kind of preparation method of bilayer graphene of the invention is by after the oxidation of impurities inside graphite, removed by the use being electrolysed with pellicle, it ensure that the purity for the graphene prepared, and when making, also add manganese element and titanium elements, the anti-corrosion property and toughness of graphene are greatly improved, makes the overall performance of graphene obtain further raising.
Description
Technical field
The present invention relates to the preparation method of graphene, specially a kind of preparation method of bilayer graphene.
Background technology
Graphene（It is a kind of cellular flat film formed by carbon atom with sp2 hybrid forms, is a kind of only one
The quasi- two-dimensional material of atomic layer level thickness, monoatomic layer graphite is done so being called.Univ Manchester UK physicist An De
Lie Gaimu and Constantine's Nuo Woxiao loves, graphene is isolated from graphite with micromechanics stripping method success, therefore altogether
With acquisition Nobel Prize in physics in 2010.The method of the common power production of graphene is mechanical stripping method, oxidation-reduction method,
Film production method is chemical vapour deposition technique（CVD）.Because its very good intensity, flexible, conductive, heat conduction, optics are special
Property, it is obtained for significant progress in fields such as physics, materialogy, electronic information, computer, Aero-Space.
Existing graphene preparation method, the graphene prepared is still with a small amount of Na+ and Al3+ impurity, to graphite
The purity of alkene has very big influence, reduces graphene conductive and thermal conductivity, and the graphene toughness that existing method is prepared
Still not high enough, the intensity of corrosion resistance is also inadequate.
The content of the invention
It is an object of the invention to provide a kind of preparation method of bilayer graphene and preparation method thereof, to solve the above-mentioned back of the body
The problem of being proposed in scape technology.
The purpose of the present invention is achieved by following technical proposals：A kind of preparation method of bilayer graphene, including
Following processing step：
1）The oxidation of graphite：After graphite of the purity more than 70% is clayed into power, it is placed in strong oxidant solution and stirs repeatedly
After 10min -20min, acquisition contains a large amount of Cl-, MnO4, SO42-graphite mixed emulsion I；
2）Graphite mixed emulsion I is electrolysed：By step 1）The graphite mixed emulsion I of acquisition closes magnesium, magnesium as electrolyte
Gold, zinc or kirsite are as anode, using stereotype as negative electrode, additional 220V -380V voltage, by graphite mixed emulsion I
Electrolysis, makes Cl-, MnO4, SO therein42-adsorbed through pellicle on anode, make Na+, Al3+ therein pass through semi-transparent
Film is adsorbed on negative electrode stereotype, takes the liquid of intermediate region as graphite mixed emulsion II；
3）The preparation of hydrodynamics agent：Take Mn simple substance and Ti simple substance to wear into radius to 0.2mm -0.6mm millimeter powder, take the powder
Last 2-4 parts by weight simultaneously mix 10min-20min with the pH value of 30-60 parts by weight in weakly acidic water, and it is strong to obtain performance
Agent；
4）Graphite mixed emulsion III preparation：Take step 2）The graphite mixed emulsion II30 parts by weight of acquisition and step 3）
The parts by weight of performance hardening agent 10 are obtained, in the environment of 50 °C -80 °C, 10min -20min is stirred, obtains graphite opalized with the mixture
Liquid III；
5）Graphene single epitaxial growth：By step 4 under UHV condition）Obtained 10-16 parts by weight of graphite mixing breast
Turbid III is passed into the transition metal substrate surface with catalytic activity, after room temperature risen to 110 °C -140 °C, stand
0.5h—1h；
6）Graphene secondary epitaxy grows：By step 5）It is true that transition metal of the substrate of acquisition with graphene is again placed in superelevation
By step 4 under empty condition）3-6 obtained parts by weight of graphite mixed emulsion III are passed into the transition metal with catalytic activity
Substrate surface, after room temperature risen to 110 °C -140 °C, stand 0.5h -1h, make graphene completely cover and transition metal
Substrate, form complete bilayer graphene film.
The strong oxidizer is the one or more in the concentrated sulfuric acid or permanganic acid.
The step 2）Used in pellicle aperture in below 200nm.
The step 6）In UHV condition under vacuum between 0.03~-0.1MPa.
The step 1）In the powdered graphite diameter worn between 0.03mm -0.06mm.
The transition metal is one kind in cobalt, nickel, copper and zinc.
The beneficial effects of the invention are as follows：A kind of preparation method of bilayer graphene of the invention is by the oxidation of impurities inside graphite
Afterwards, removed by the use being electrolysed with pellicle, when ensure that the purity for the graphene prepared, and making, also add manganese member
Element and titanium elements, greatly improve the anti-corrosion property and toughness of graphene, make the overall performance of graphene obtain further
Improve.
Embodiment
With reference to embodiment further instruction, but following detailed description should not be done and be managed
Solve the limitation to invent body.Those of ordinary skill in the art can apparently make various on the basis of the present invention
Change and change, it should within the scope of invention.
A kind of preparation method of bilayer graphene, is comprised the technical steps that：
1）The oxidation of graphite：After graphite of the purity more than 70% is clayed into power, it is placed in strong oxidant solution and stirs repeatedly
After 10min -20min, acquisition contains a large amount of Cl-, MnO4, SO42-graphite mixed emulsion I, after graphite is milled
Oxidation reinforced dose by Na the and Al elements in graphite it is fully oxidized be in ion；
2）Graphite mixed emulsion I is electrolysed：By step 1）The graphite mixed emulsion I of acquisition closes magnesium, magnesium as electrolyte
Gold, zinc or kirsite are as anode, using stereotype as negative electrode, additional 220V -380V voltage, by graphite mixed emulsion I
Electrolysis, makes Cl-, MnO4, SO therein42-adsorbed through pellicle on anode, make Na+, Al3+ therein pass through semi-transparent
Film is adsorbed on negative electrode stereotype, the liquid of intermediate region is taken as graphite mixed emulsion II, by being electrolysed graphite mixing breast
Turbid I, by its interior Cl-, MnO4, SO42-, separated between Na+ and Al3+ and graphite；
3）The preparation of hydrodynamics agent：Take Mn simple substance and Mn simple substance to wear into radius to 0.2mm -0.6mm millimeter powder, take the powder
Last 2-4 parts by weight simultaneously mix 10min-20min with the pH value of 30-60 parts by weight in weakly acidic water, and it is strong to obtain performance
Agent；
4）Graphite mixed emulsion III preparation：Take step 2）The graphite mixed emulsion II30 parts by weight of acquisition and step 3）
The parts by weight of performance hardening agent 10 are obtained, in the environment of 50 °C -80 °C, 10min -20min is stirred, obtains graphite opalized with the mixture
Liquid III, the pliability of a small amount of Mn raisings graphene is added by hydrodynamics agent into graphite, and addition Ti improves the anti-of graphene
Corruption；
5）Graphene single epitaxial growth：By step 4 under UHV condition）Obtained 10-16 parts by weight of graphite mixing breast
Turbid III is passed into the transition metal substrate surface with catalytic activity, after room temperature risen to 110 °C -140 °C, stand
0.5h—1h；
6）Graphene secondary epitaxy grows：By step 5）It is true that transition metal of the substrate of acquisition with graphene is again placed in superelevation
By step 4 under empty condition）3-6 obtained parts by weight of graphite mixed emulsion III are passed into the transition metal with catalytic activity
Substrate surface, after room temperature risen to 110 °C -140 °C, stand 0.5h -1h, make graphene completely cover and transition metal
Substrate, form complete bilayer graphene film.
The strong oxidizer is the one or more in the concentrated sulfuric acid or permanganic acid.
The step 2）Used in pellicle aperture in below 200nm.
The step 6）In UHV condition under vacuum between 0.03~-0.1MPa.
The step 1）In the powdered graphite diameter worn between 0.03mm -0.06mm.
The transition metal is one kind in cobalt, nickel, copper and zinc.
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.People in the art
Member should be appreciated that invention scope involved in the application, however it is not limited to the technology that the particular combination of above-mentioned technical characteristic forms
Scheme, while should also cover in the case where not departing from the inventive concept, carried out by above-mentioned technical characteristic or its equivalent feature
The other technical schemes for being combined and being formed.Such as features described above has similar work(with (but not limited to) disclosed herein
The technical scheme that the technical characteristic of energy is replaced mutually and formed.
Claims (6)
- A kind of 1. preparation method of bilayer graphene, it is characterised in that：Comprise the technical steps that：1）The oxidation of graphite：After graphite of the purity more than 70% is clayed into power, it is placed in strong oxidant solution and stirs repeatedly After 10min -20min, acquisition contains a large amount of Cl-, MnO4, SO42-graphite mixed emulsion I；2）Graphite mixed emulsion I is electrolysed：By step 1）The graphite mixed emulsion I of acquisition closes magnesium, magnesium as electrolyte Gold, zinc or kirsite are as anode, using stereotype as negative electrode, additional 220V -380V voltage, by graphite mixed emulsion I Electrolysis, makes Cl-, MnO4, SO therein42-adsorbed through pellicle on anode, make Na+, Al3+ therein pass through semi-transparent Film is adsorbed on negative electrode stereotype, takes the liquid of intermediate region as graphite mixed emulsion II；3）The preparation of hydrodynamics agent：Take Mn simple substance and Ti simple substance to wear into radius to 0.2mm -0.6mm millimeter powder, take the powder Last 2-4 parts by weight simultaneously mix 10min-20min with the pH value of 30-60 parts by weight in weakly acidic water, and it is strong to obtain performance Agent；4）Graphite mixed emulsion III preparation：Take step 2）The graphite mixed emulsion II30 parts by weight of acquisition and step 3） The parts by weight of performance hardening agent 10 are obtained, in the environment of 50 °C -80 °C, 10min -20min is stirred, obtains graphite opalized with the mixture Liquid III；5）Graphene single epitaxial growth：By step 4 under UHV condition）Obtained 10-16 parts by weight of graphite mixing breast Turbid III is passed into the transition metal substrate surface with catalytic activity, after room temperature risen to 110 °C -140 °C, stand 0.5h—1h；6）Graphene secondary epitaxy grows：By step 5）It is true that transition metal of the substrate of acquisition with graphene is again placed in superelevation By step 4 under empty condition）3-6 obtained parts by weight of graphite mixed emulsion III are passed into the transition metal with catalytic activity Substrate surface, after room temperature risen to 110 °C -140 °C, stand 0.5h -1h, make graphene completely cover and transition metal Substrate, form complete bilayer graphene film.
- A kind of 2. preparation method of bilayer graphene according to claim 1, it is characterised in that：The strong oxidizer is dense One or more in sulfuric acid or permanganic acid.
- A kind of 3. preparation method of bilayer graphene according to claim 1, it is characterised in that：The step 2）It is middle to be made The aperture of pellicle is in below 200nm.
- A kind of 4. preparation method of bilayer graphene according to claim 1, it is characterised in that：The step 6）In it is super Vacuum under high vacuum condition is between 0.03~-0.1MPa.
- A kind of 5. preparation method of bilayer graphene according to claim 1, it is characterised in that：The step 1）In wear into Powdered graphite diameter between 0.03mm -0.06mm.
- A kind of 6. preparation method of bilayer graphene according to claim 1, it is characterised in that：The transition metal is One kind in cobalt, nickel, copper and zinc.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877109A (en) * | 2012-09-19 | 2013-01-16 | 四川大学 | Method for preparing grapheme transparent conducting films by electrophoretic deposition |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN104477892A (en) * | 2014-12-12 | 2015-04-01 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of flake graphene and flake graphene device prepared by same |
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2017
- 2017-10-13 CN CN201710953818.9A patent/CN107539977A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102877109A (en) * | 2012-09-19 | 2013-01-16 | 四川大学 | Method for preparing grapheme transparent conducting films by electrophoretic deposition |
| CN103466603A (en) * | 2013-08-09 | 2013-12-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of graphene dispersion liquid, and preparation method of graphene film |
| CN104477892A (en) * | 2014-12-12 | 2015-04-01 | 盐城市新能源化学储能与动力电源研究中心 | Preparation method of flake graphene and flake graphene device prepared by same |
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Application publication date: 20180105 |