CN106865534A - A kind of method and device for preparing Graphene - Google Patents
A kind of method and device for preparing Graphene Download PDFInfo
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- CN106865534A CN106865534A CN201710206111.1A CN201710206111A CN106865534A CN 106865534 A CN106865534 A CN 106865534A CN 201710206111 A CN201710206111 A CN 201710206111A CN 106865534 A CN106865534 A CN 106865534A
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- conductive metal
- reaction vessel
- graphene
- expanded graphite
- weak acid
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
Abstract
The present invention relates to a kind of device for preparing Graphene, described device includes reaction vessel, expanded graphite cake, conductive metal mesh, conductive metal sheet, weak acid electrolyte and power supply, weak acid electrolyte is full of in reaction vessel, expanded graphite cake is inlaid in the bottom of reaction vessel, the outer surface of expanded graphite cake is welded with conductive metal mesh, and power supply is connected by wire with conductive metal mesh and conductive metal sheet respectively.The present invention mainly make use of the principle of electrolysis, and expanded graphite as one end of conductive electrode is electrolysed so that expanded graphite is successively peeled off in the electrolytic solution in access circuit, then filters cleaning, drying and has just obtained required Graphene.Invention mainly make use of the principle of electrolysis, and the proportion that single-layer graphene is accounted for is very big.
Description
Technical field
The invention belongs to technical field of graphene preparation, and in particular to a kind of method that utilization expanded graphite prepares Graphene
And device.
Background technology
Native graphite alkene is the two dimensional crystal for being stripped out from graphite material, being made up of carbon atom.Graphene is both
Most thin material, is also most tough material, 200 times more taller than best steel of fracture strength.It has well again simultaneously
Elasticity, stretch range can reach the 20% of own dimensions.It is that current nature is most thin, intensity highest material, Graphene mesh
Preceding most potential application is the substitute for turning into silicon, manufactures ultra micro transistor npn npn, for producing the supercomputer in future.With
Graphene replaces silicon, and the speed of service of computer processor will hundreds times soon.In addition, Graphene is almost fully transparent,
Only absorb 2.3% light.On the other hand, it is very fine and close, even the gas atom (helium atom) of minimum cannot also be penetrated.This
A little features cause that it is highly suitable as the raw material of transparent electron product, such as transparent touch display screen, luminescent screen and solar energy
Cell panel.As the most strong a kind of novel nano-material of the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, Graphene
It is referred to as " dark fund ", is " king of new material ", scientist even foretells that Graphene " will thoroughly change 21 century ".
In the prior art, the synthetic method of Graphene mainly has two kinds：Mechanical means and chemical method.Mechanical means includes
The method of mechanical phonograph recorder separation, epitaxy method and heating SiC, it is chemical reduction method and chemical dissociation method that chemical method is mainly.
Most common is micromechanics partition method, and directly graphene platelet is cut down from larger crystal.2004
Novoselovt etc. has prepared single-layer graphene in this way, it is possible to the stable existence under external environment.It is prepared by typical case
Method is that the pyrolytic graphite of or introducing defect expanded with another material is rubbed, and the surface of body phase graphite can produce wadding
The crystal of sheet, the Graphene containing individual layer in the crystal of these flocculus shapes.But have the disadvantage that this method is using the graphite table that rubs
The thin slice that face obtains filters out the graphene platelet of individual layer, and its size is difficult to control, it is impossible to which reliably factory length is supplied enough
Graphite flake sample.
Epitaxy method is to go out Graphene using growth substrate atomic structure " kind ", allows carbon atom to be oozed at 1150 DEG C first
Enter ruthenium, then cool down, after being cooled to 850 DEG C, a large amount of carbon atoms for absorbing before will float to ruthenium surface, the individual layer of lens shape
Carbon atom " isolated island " be covered with whole stromal surface, it is final they can grow up to a complete layer graphene.Ground floor is covered
After 80%, the second layer starts growth.The Graphene of bottom can produce strong reciprocation with ruthenium, and after the second layer just almost with
Ruthenium is kept completely separate, only remaining light current coupling, and the single-layer graphene thin slice performance for obtaining is satisfactory.But produce in this way
Graphene platelet it is often in uneven thickness, and bonding between Graphene and matrix can influence the characteristic of carbon-coating.
Chemical reduction method is to mix graphite oxide and water with the ratio of 1mg/mL, with supersonic oscillations to the clear nothing of solution
Particulate material, adds appropriate hydrazine in 100 DEG C of backflow 24h, produces black particle shape precipitation, filtering, drying Graphene.Change
It is the method that graphite oxide is prepared Graphene by the method for thermal reduction, the oxygen-containing functional group of graphite oxide interlayer to learn dissociation method
React at a certain temperature.
Wherein, electrolysis be it is the most frequently used prepare the method for Graphene, but have that Graphene yield is too low, purity is not high
Problem.
The content of the invention
The invention aims in solving existing graphene preparation technology, Graphene yield is too low, and purity is not high
Problem, and then a kind of device and method for preparing Graphene is provided.
The technical scheme is that：The present invention includes a kind of device for preparing above-mentioned Graphene, and device includes that reaction is held
Device 1, expanded graphite cake 2, conductive metal mesh 3, conductive metal sheet 4, weak acid electrolyte 5 and power supply 6, conductive metal sheet 4 are arranged on
Weak acid electrolyte 5 is full of in the top of reaction vessel 1, reaction vessel 1, expanded graphite cake 2 is placed in the bottom of reaction vessel 1, swollen
The outer surface of swollen graphite cake 2 is welded with conductive metal mesh 3, and power supply 6 is respectively by wire and conductive metal mesh 3 and conductive metal sheet 4
Connection.
Further, the suspension bracket of the conductive metal sheet 4 is placed in the top of reaction vessel 1.
Further, glue sticking is used between the expanded graphite cake 2 and reaction vessel 1.
Further, weak acid electrolyte 5 is the weak acid such as dilute oxalic acid or dilute sulfuric acid.
Further, the material of reaction vessel 1 is non-conductive.
Further, the material of conductive metal mesh 3 and conductive metal sheet 4 is copper, iron or aluminium.
The invention further relates to a kind of preparation method of Graphene, comprise the following steps：Expanded graphite cake 2 is inlaid in reaction
The bottom of container 1, then weak acid electrolyte 5 is full of reaction vessel 1, conductive metal sheet 4 is then placed in the upper of reaction vessel 1
Side, power supply 6 is connected by wire with conductive metal mesh 3 and conductive metal sheet 4 respectively, turns on the power 6 switches to expanded graphite cake 2
It is electrolysed, fully after electrolysis, the mixture of Graphene and electrolyte is taken out into cleaning, filtered after ultrasonication, then dried, i.e.,
Obtain required Graphene.
Further, the voltage of power supply 6 is preferably 8 to 30 volts.
The present invention has the advantages that：The present invention mainly make use of the principle of electrolysis, using expanded graphite as conduction
One end of electrode, is electrolysed so that expanded graphite is successively peeled off in the electrolytic solution in access electric current, and then filtering cleaning is dried
It is dry just to have obtained required Graphene.And in the Graphene for obtaining, the proportion that single-layer graphene is accounted for is very big.This kind of method is simple
It is easy, it is low to device requirement, it is not necessary to which that complicated operational means can be completed, and be worthy to be popularized.
Brief description of the drawings
Fig. 1 is the schematic diagram of the device that electrolysis of the present invention prepares Graphene；
Fig. 2 is the top view of the conductive metal mesh of the device that electrolysis of the present invention prepares Graphene.
Specific embodiment
With reference to specific embodiment, the present invention will be further described：
With reference to Fig. 1 and Fig. 2 explanation present embodiments, present embodiment includes that device includes reaction vessel 1, expanded graphite cake
2nd, conductive metal mesh 3, conductive metal sheet 4, weak acid electrolyte 5 and power supply 6, conductive metal sheet 4 are arranged on the top of reaction vessel 1
Weak acid electrolyte 5 is full of in portion, reaction vessel 1, expanded graphite cake 2 is placed in the bottom of reaction vessel 1, outside expanded graphite cake 2
Surface is welded with conductive metal mesh 3, and power supply 6 is connected by wire with conductive metal mesh 3 and conductive metal sheet 4 respectively.
Glue sticking is used between expanded graphite cake 2 and reaction vessel 1, the suspension bracket of conductive metal sheet 4 is placed on reaction vessel 1
Side.It is easy to be repeatedly opened and takes liquid.
Weak acid electrolyte 5 is preferably phosphoric acid,diluted or watery hydrochloric acid.The material of reaction vessel 1 is non-conductive, it may be preferred to glass
Container.The common cheap metals such as the preferred copper of material of conductive metal mesh 3 and conductive metal sheet 4, iron or aluminium.The voltage of power supply 6
Preferably 8 to 10 volts.
The preparation method of expanded graphite cake 2 is as follows：
Natural flake graphite is taken, in the mixed acid solution of sulfuric acid and nitric acid is added under being stirred continuously, Gao Meng is added
Sour potassium, controls uniform temperature, then adds ferric trichloride, stirs, and after reaction certain hour, dilute alkaline soln is used in centrifugation
Embathe, be washed to acidity, drying carries out high temperature puffing again after dehydration, you can obtain expanded graphite worm.Further according to device need by
It is that can be used into different shape that expanded graphite is tightly compacted.
Also a kind of preparation method of Graphene of the present invention, comprises the following steps：Expanded graphite cake 2 is inlaid in reaction vessel
1 bottom, then weak acid electrolyte 5 is full of reaction vessel 1, then conductive metal sheet 4 is placed in the top of reaction vessel 1, electricity
Source 6 is connected by wire with conductive metal mesh 3 and conductive metal sheet 4 respectively, and turn on the power 6 switches is carried out to expanded graphite cake 2
After electrolysis, fully electrolysis, the mixture of Graphene and electrolyte is taken out into cleaning, filtered after ultrasonication, then dried, that is, obtained
Required Graphene.
The principle of present embodiment：Power supply 6 leads to 8 to 30 volt voltages, and conductive metal mesh 3 can be electrolysed expanded graphite cake after being powered
2, Graphene is peeled off into, the mixture of weak acid electrolyte 5 and Graphene is poured out from reaction vessel 1, using filter
Mixture is filtered, ultrasonication cleaning is carried out to the Graphene for leaching using Ultrasound Instrument, using dryer to Graphene
Dried, obtained required Graphene.
The above is only presently preferred embodiments of the present invention, is not intended to limit embodiment of the present invention, and this area is general
Logical technical staff's central scope of the invention and spirit, can very easily carry out corresponding flexible or modification, therefore originally
The protection domain of invention should be defined by the protection domain required by claims.
Claims (9)
1. a kind of device for preparing Graphene, it is characterised in that described device include reaction vessel (1), expanded graphite cake (2),
Conductive metal mesh (3), conductive metal sheet (4), weak acid electrolyte (5) and power supply (6), conductive metal sheet (4) hold installed in reaction
Weak acid electrolyte (5) is full of in the top of device (1), reaction vessel (1), expanded graphite cake (2) is placed in the bottom of reaction vessel (1)
Portion, the outer surface of expanded graphite cake (2) is welded with conductive metal mesh (3), and power supply (6) is respectively by wire and conductive metal mesh (3)
Connected with conductive metal sheet (4).
2. a kind of device for preparing Graphene according to claim 1, it is characterised in that the conductive metal sheet (4) is used
Suspension bracket is placed in reaction vessel (1) top.
3. a kind of device for preparing Graphene according to claim 1, it is characterised in that：The expanded graphite cake (2) with
Reaction vessel uses glue sticking between (1).
4. a kind of device for preparing Graphene according to claim 1, it is characterised in that weak acid electrolyte (5) is dilute grass
The weak acid such as acid or dilute sulfuric acid.
5. a kind of device for preparing Graphene according to claim 1, it is characterised in that the material of reaction vessel (1) is not
It is conductive.
6. a kind of device for preparing Graphene according to claim 1, it is characterised in that conductive metal mesh (3) and conduction
The material of metallic plate (4) is copper, iron or aluminium.
7. a kind of method that any one of utilization the claims 1 to 6 prepares Graphene, it is characterised in that comprise the following steps：
Expanded graphite cake (2) is inlaid in the bottom of reaction vessel (1), then by weak acid electrolyte (5) full of reaction vessel (1), then
Conductive metal sheet (4) is placed in the top of reaction vessel (1), power supply (6) is respectively by wire and conductive metal mesh (3) and conduction
Metallic plate (4) is connected, and turns on the power (6) switch and expanded graphite cake (2) is electrolysed, fully after electrolysis, by Graphene and electricity
The mixture for solving liquid takes out cleaning, is filtered after ultrasonication, then dries, that is, obtain required Graphene.
8. the method that a kind of electrolysis according to claim 7 prepares Graphene, it is characterised in that weak acid electrolyte (5)
It is the weak acid such as dilute oxalic acid or dilute sulfuric acid.
9. the method that a kind of electrolysis according to claim 8 prepares Graphene, it is characterised in that the voltage of power supply (6)
It is 8 to 30 volts.
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Cited By (3)
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| EP3650585A1 (en) * | 2018-11-12 | 2020-05-13 | Fundació Institut Català de Nanociència i Nanotecnologia | Electrolytic cell and procedure for the preparation of graphene by means of electrochemical exfoliation |
| WO2021048089A1 (en) * | 2019-09-12 | 2021-03-18 | Avadain, LLC | Method and apparatus for the expansion of graphite |
| CN115010122A (en) * | 2022-06-17 | 2022-09-06 | 中钢集团南京新材料研究院有限公司 | Preparation device, preparation method and application of high-oxidation graphene |
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| CN115010122B (en) * | 2022-06-17 | 2023-07-14 | 中钢集团南京新材料研究院有限公司 | Method for preparing high-oxidation graphene |
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Application publication date: 20170620 |