CN106894039B - A kind of method and device preparing graphene - Google Patents
A kind of method and device preparing graphene Download PDFInfo
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- CN106894039B CN106894039B CN201710205344.XA CN201710205344A CN106894039B CN 106894039 B CN106894039 B CN 106894039B CN 201710205344 A CN201710205344 A CN 201710205344A CN 106894039 B CN106894039 B CN 106894039B
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- graphene
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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
Abstract
The present invention relates to a kind of device for preparing graphene, described device includes weak acid electrolyte, power supply, container, several expanded graphite cakes, several conductive metal mesh and metal plate, and container bottom end plate is equipped with metal plate, is full of weak acid electrolyte in container.The principle of electrolysis is mainly utilized in the present invention, using expanded graphite as one end of conductive electrode, accesses in circuit and is electrolysed, so that expanded graphite is successively removed in the electrolytic solution, has then just obtained required graphene after cleaning, ultrasound removing, filtering drying.And in obtained graphene, the specific gravity that single-layer graphene accounts for is very big.
Description
Technical field
The invention belongs to technical field of graphene preparation, and in particular to a method of graphene is prepared using expanded graphite
And device.
Background technique
Natural graphite alkene is the two dimensional crystal for being stripped out from graphite material, being made of carbon atom.Graphene is both
Most thin material, and most tough material, 200 times more taller than best steel of breaking strength.It has well again simultaneously
Elasticity, stretch range can reach the 20% of own dimensions.It is that current nature is most thin, the highest material of intensity, graphene mesh
Preceding most potential application is the substitute as silicon, manufactures ultra micro transistor npn npn, for producing following supercomputer.With
Graphene replaces silicon, and the speed of service of computer processor will be hundreds times fast.In addition, graphene be almost it is fully transparent,
Only absorb 2.3% light.On the other hand, it is very fine and close, even the smallest gas atom (helium atom) can not also penetrate.This
A little features make it be highly suitable as the raw material of transparent electron product, such as transparent touch display screen, luminescent screen and solar energy
Solar panel.As presently found most thin, maximum intensity, a kind of strongest novel nano-material of electrical and thermal conductivity performance, graphene
Referred to as " dark fund " is " king of new material ", and scientist even foretells that graphene " will thoroughly change 21 century ".
In the prior art, there are mainly two types of the synthetic methods of graphene: mechanical means and chemical method.Mechanical means includes
Mechanical phonograph recorder separation, epitaxy method and the method for heating SiC, chemical method are chemical reduction method and chemical dissociation method.
Most common is micromechanics partition method, directly cuts down graphene platelet from biggish crystal.2004
Novoselovt etc. has prepared single-layer graphene in this way, and can be stabilized under external environment.Typical case's preparation
Method is rubbed with the pyrolytic graphite of another material extruding or introducing defect, and the surface of body phase graphite can generate wadding
The crystal of sheet contains the graphene of single layer in the crystal of these flocculus shapes.But the disadvantage is that this method is to utilize friction graphite table
The thin slice that face obtains filters out the graphene platelet of single layer, and size is not easy to control, can not reliably supply enough factory length
Graphite flake sample.
Epitaxy method is to go out graphene using growth substrate atomic structure " kind ", and carbon atom is allowed to seep at 1150 DEG C first
Enter ruthenium, then cool down, after being cooled to 850 DEG C, a large amount of carbon atoms absorbed before will float to ruthenium surface, the single layer of lens shape
Carbon atom " isolated island " be covered with entire stromal surface, it is final they can grow up to complete one layer of graphene.First layer covering
After 80%, the second layer starts to grow.The graphene of bottom can generate strong reciprocation with ruthenium, and after the second layer just almost with
Ruthenium is kept completely separate, only remaining light current coupling, and obtained single-layer graphene thin slice performance is satisfactory.But it produces in this way
Graphene platelet it is often in uneven thickness, and the bonding between graphene and matrix will affect 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 is added appropriate hydrazine and flows back at 100 DEG C for 24 hours, generates black particle shape precipitating, filtering, graphene obtained by drying.
Chemical dissociation method is the method that graphite oxide is prepared graphene by the method heat-treated, the oxygen-containing function of graphite oxide interlayer
Group reacts at a certain temperature.
Wherein, can extract graphene purity is high, the minimum method of cost is exactly mechanical phonograph recorder separation, but there are low output,
High, the halfway problem of graphite separation is required operation technique.
Summary of the invention
The purpose of the present invention is to solve in existing graphene preparation technology, there are at high cost, complicated for operation, purity is low
The problem of, and then a kind of method for preparing graphene is provided.
The technical scheme is that a kind of device for preparing graphene, described device includes weak acid electrolyte 5, power supply
6, the bottom end plate of container 7, several expanded graphite cakes 8, several conductive metal mesh 9 and metal plate 10, container 7 is equipped with metal plate
10, container 7 is interior to be full of weak acid electrolyte 5, and several expanded graphite cakes 8 are mounted on hanger, and multiple conductive metal mesh 9 are respectively welded
On the outer surface of expanded graphite cake 8, power supply 6 is connect by conducting wire with multiple conductive metal mesh 9 and metal plate 10 respectively.
Further, the expanded graphite cake 8 is evenly distributed on 7 top of container with hanger.
Further, glue sticking is used between the metal plate 10 and container 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 5 is non-conductive.
Further, the material of conductive metal mesh 9 and metal plate 10 is copper, iron or aluminium.
The invention further relates to a kind of methods for preparing graphene using above-mentioned apparatus, comprising the following steps: by metal plate 10
It is inlaid in the bottom of reaction vessel 7, then weak acid electrolyte 5 is full of reaction vessel 7, then by several expanded graphite cakes 8 with hanging
Frame is evenly distributed on 7 top of container, and power supply 6 is connect by conducting wire with conductive metal mesh 9 and conductive metal sheet 10 respectively, opens electricity
The switch of source 6 is electrolysed expanded graphite cake 8, sufficiently after electrolysis, cleans after the mixture of graphene and electrolyte is taken out super
Sound removing filtering, then dry to get required graphene is arrived.
Further, weak acid electrolyte 5 is the weak acid such as dilute oxalic acid or dilute sulfuric acid.
Further, the voltage of power supply 6 is preferably 8 to 30 volts.
The invention has the following beneficial effects: the principles of the invention that electrolysis is mainly utilized, using expanded graphite as conduction
One end of electrode is accessed in electric current and is electrolysed, so that expanded graphite is successively removed in the electrolytic solution, then cleaning, ultrasound
Removing filtering drying has just obtained required graphene.And in obtained graphene, the specific gravity that single-layer graphene accounts for is very big.This
Kind method is simple and easy, low to device requirement, and not needing complicated operational means can be completed, and is worthy to be popularized.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for preparing the device of graphene；
Fig. 2 is the cross-sectional view for preparing the device of graphene.
Specific embodiment
The present invention will be further described combined with specific embodiments below:
Specific embodiment 4: illustrate present embodiment in conjunction with 1 and Fig. 2, present embodiment includes a kind of preparing graphene
Device, described device includes weak acid electrolyte 5, power supply 6, container 7, several expanded graphite cakes 8,9 and of several conductive metal mesh
Several metal plates 10, the bottom end plate of container 7 are equipped with metal plate 10, are full of weak acid electrolyte 5, several expansion stones in container 7
Black cake 8 is mounted on hanger, and multiple conductive metal mesh 9 are respectively welded on the outer surface of expanded graphite cake 8, and power supply 6 leads to respectively
Conducting wire is crossed to connect with multiple conductive metal mesh 9 and metal plate 10.
Expanded graphite cake 8 is evenly distributed on 7 top of container with hanger.Glue sticking is used between metal plate 10 and container 1.
Weak acid electrolyte 5 is preferably dilute oxalic acid or dilute sulfuric acid.The material of reaction vessel 1 is non-conductive, can preferred glass
Container.The common cheap metals such as the preferred copper of the material of conductive metal mesh 3 and conductive metal sheet 4, iron or aluminium.The voltage of power supply 6
Preferably 8 to 30 volts.
Expanded graphite cake 2 the preparation method is as follows:
Natural flake graphite is taken, is added into the mixed acid solution of sulfuric acid and nitric acid under constant stirring, adds Gao Meng
Sour potassium controls certain temperature, then adds ferric trichloride, stirs, and after a certain period of time, dilute alkaline soln is used in centrifuge separation for reaction
It embathes, is washed to acidity, drying can obtain expanded graphite after dehydration.It is needed further according to device expanded graphite is tightly compacted at not
Similar shape can be used.
The invention further relates to a kind of methods for preparing graphene using above-mentioned apparatus, comprising the following steps: by metal plate 10
It is inlaid in the bottom of reaction vessel 7, then weak acid electrolyte 5 is full of reaction vessel 7, then by several expanded graphite cakes 8 with hanging
Frame is evenly distributed on 7 top of container, and power supply 6 is connect by conducting wire with conductive metal mesh 9 and conductive metal sheet 10 respectively, opens electricity
The switch of source 6 is electrolysed expanded graphite cake 8, sufficiently after electrolysis, cleans after the mixture of graphene and electrolyte is taken out super
Sound removing filtering, then dry to get required graphene is arrived.
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
8, graphene is removed into, the mixture of weak acid electrolyte 5 Yu graphene is poured out from reaction vessel 7, then cleaning, ultrasound
Required graphene has just been obtained after removing, filtering drying.
Above content is only presently preferred embodiments of the present invention, is not intended to limit embodiment of the present invention, and this field is general
Logical technical staff's central scope according to the present invention and spirit can very easily carry out corresponding flexible or modification, therefore originally
The protection scope of invention should be subject to protection scope required by claims.
Claims (9)
1. a kind of device for preparing graphene, it is characterised in that: described device includes weak acid electrolyte (5), power supply (6), container
(7), the bottom end plate of several expanded graphite cakes (8), several conductive metal mesh (9) and metal plate (10), container (7) is equipped with gold
Belong to plate (10), be full of weak acid electrolyte (5) in container (7), several expanded graphite cakes (8) are mounted on hanger, multiple conductive golds
Belong to net (9) to be respectively welded on the outer surface of expanded graphite cake (8), power supply (6) passes through conducting wire and multiple conductive metal mesh respectively
(9) it is connected with metal plate (10).
2. the device that a kind of electrolysis method according to claim 1 prepares graphene, it is characterised in that: the expanded graphite cake
(8) it is evenly distributed on above container (7) with hanger.
3. the device that a kind of electrolysis method according to claim 1 prepares graphene, it is characterised in that: the metal plate (10)
Glue sticking is used between container (7).
4. a kind of device for preparing graphene according to claim 1, which is characterized in that weak acid electrolyte (5) is dilute grass
Acid.
5. a kind of device for preparing graphene according to claim 1, which is characterized in that the material of reaction vessel (7) is not
It is conductive.
6. a kind of device for preparing graphene according to claim 1, which is characterized in that conductive metal mesh (9) and metal
The material of plate (10) is copper, iron or aluminium.
7. a kind of method for preparing graphene using any one of the claims 1 to 6 described device, which is characterized in that including
Following steps: metal plate (10) is inlaid in the bottom of reaction vessel (7), then weak acid electrolyte (5) are full of reaction vessel
(7), then several expanded graphite cakes (8) are mounted on hanger, power supply (6) respectively by conducting wire and conductive metal mesh (9) and
Conductive metal sheet (10) connection is opened power supply (6) switch and is electrolysed to expanded graphite cake (8), sufficiently after electrolysis, by graphene
It filters, then is dried to get required graphene is arrived with ultrasound removing is cleaned after the mixture taking-up of electrolyte.
8. the method according to claim 7 for preparing graphene, which is characterized in that weak acid electrolyte (5) is dilute oxalic acid.
9. the method according to claim 8 for preparing graphene, which is characterized in that the voltage of power supply (6) is preferably 8 to 30
Volt.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534643A (en) * | 2012-01-16 | 2012-07-04 | 清华大学深圳研究生院 | Method for regenerating waste battery carbon rods into graphene |
| CN103451670A (en) * | 2013-09-11 | 2013-12-18 | 中南大学 | Electrochemical preparation method of graphene |
| CN106498428A (en) * | 2016-10-14 | 2017-03-15 | 电子科技大学 | The method for preparing grapheme material co-producing hydrogen |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8524067B2 (en) * | 2007-07-27 | 2013-09-03 | Nanotek Instruments, Inc. | Electrochemical method of producing nano-scaled graphene platelets |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534643A (en) * | 2012-01-16 | 2012-07-04 | 清华大学深圳研究生院 | Method for regenerating waste battery carbon rods into graphene |
| CN103451670A (en) * | 2013-09-11 | 2013-12-18 | 中南大学 | Electrochemical preparation method of graphene |
| CN106498428A (en) * | 2016-10-14 | 2017-03-15 | 电子科技大学 | The method for preparing grapheme material co-producing hydrogen |
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