CN106865532A - A kind of utilization platinum filament and graphite cake prepare the device of Graphene - Google Patents
A kind of utilization platinum filament and graphite cake prepare the device of Graphene Download PDFInfo
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- CN106865532A CN106865532A CN201710199499.7A CN201710199499A CN106865532A CN 106865532 A CN106865532 A CN 106865532A CN 201710199499 A CN201710199499 A CN 201710199499A CN 106865532 A CN106865532 A CN 106865532A
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- graphene
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- 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 the device that a kind of utilization platinum filament and graphite cake prepare Graphene, including container, platinum filament fixed plate, expanded graphite worm cake, weak acid electrolyte, power supply, conductive metal mesh and some platinum filaments, expanded graphite worm cake is inlaid in the bottom of container, weak acid electrolyte is full of in container, the inner surface of platinum filament fixed plate is welded with some platinum filaments vertically.The present invention mainly make use of the principle of electrolysis, continuous electrolysis by conductive metal mesh to expanded graphite worm cake, so that expanded graphite is successively peeled off in the electrolytic solution, again by the continuous electrolysis of platinum filament, expanded graphite worm has been obtained sufficient electrolysis stripping, filtering drying is cleaned after the completion of electrolysis and has just obtained required Graphene.
Description
Technical field
The invention belongs to technical field of graphene preparation, and in particular to a kind of utilization platinum filament prepares device and the side of Graphene
Method.
Background technology
Graphene is the two dimensional crystal for being stripped out from natural 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 preparation method of native graphite alkene mainly has two kinds：Mechanical means and chemical method.Mechanical means
Method including mechanical phonograph recorder separation, epitaxy method and heating SiC, it is that chemical reduction method dissociates with chemistry that chemical method is mainly
Method.
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..
Chemical dissociation method is the method that graphite oxide is prepared Graphene by the method for thermal reduction, the oxygen-containing function of graphite oxide interlayer
Group reacts 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, complex manufacturing, Graphene purity compared with
Low problem, and then a kind of device and method for preparing Graphene is provided.
The technical scheme is that：A kind of utilization platinum filament and graphite cake prepare the device of Graphene, and described device includes
Container 1, platinum filament fixed plate 2, expanded graphite worm cake 4, weak acid electrolyte 5, power supply 6, conductive metal mesh 8 and some platinum filaments 3, it is swollen
Swollen graphite worm cake 4 is inlaid in and weak acid electrolyte 5 is full of in the bottom of container 1, container 1, and the inner surface of platinum filament fixed plate 2 is vertical
Some platinum filaments 3 are welded with, conductive metal mesh 8 is horizontally placed in weak acid electrolyte 5, expanded graphite worm cake 4 and platinum filament fixed plate 2 are equal
Positive pole with power supply 6 is connected, and conductive metal mesh 8 is connected with the negative pole of power supply 6.
Further, the suspension bracket of platinum filament fixed plate 2 is placed in the top of container 1.
Further, gluing connection is used between the expanded graphite worm cake 4 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 container 1 is non-conductive.
Further, the one end of conductive metal mesh 8 is fixed on the side wall of container 1 by support, and the other end is passed through by support
The side wall of container 1 accesses power supply 6.
The invention further relates to a kind of method that utilization said apparatus prepare Graphene, comprise the following steps：By expanded graphite
Worm cake 4 is inlaid in the bottom of reaction vessel 1, then weak acid electrolyte 5 is full of into reaction vessel 1, then uses platinum filament fixed plate 2
Suspension bracket is fixed on the top of reaction vessel 1, and conductive metal mesh 8 is horizontally placed in weak acid electrolyte 5, by the He of expanded graphite worm cake 4
Platinum filament fixed plate 2 is connected with the positive pole of power supply 6, and conductive metal mesh 8 is connected with the negative pole of power supply 6, turns on the power 6 switches to expansion
Graphite worm cake 2 is electrolysed, fully after electrolysis, cleaning filtering after the mixture of Graphene and electrolyte is taken out, then incited somebody to action
The Graphene that filter is obtained carries out ultrasonication drying, that is, obtain required Graphene.
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 3 to 30 volts.
The present invention has the advantages that：The present invention mainly make use of the principle of electrolysis, by conductive metal mesh to swollen
The continuous electrolysis of swollen graphite worm cake so that expanded graphite is successively peeled off in the electrolytic solution, then by the continuous electrolysis of platinum filament,
Expanded graphite worm has been obtained sufficient electrolysis stripping, filtering drying is cleaned after the completion of electrolysis and has just obtained required graphite
Alkene.
By adding conductive metal mesh, can be in expanded graphite worm cake and liquid the abundant graphite worm peeled off simultaneously
It is electrolysed twice, is strengthened electrolytic efficiency.In the Graphene for obtaining, the ratio that single-layer graphene is accounted for is great, and the method work
Skill is simply easy to install.
Brief description of the drawings
Fig. 1 is structural representation of the invention.
Specific embodiment
With reference to specific embodiment, the present invention will be further described：
Refering to Fig. 1, the device of present embodiment includes container 1, platinum filament fixed plate 2, expanded graphite worm cake 4, weak acid electricity
Solution liquid 5, power supply 6, conductive metal mesh 8 and some platinum filaments 3, expanded graphite worm cake 4 are inlaid in the bottom of container 1, container 1 and fill
Full weak acid electrolyte 5, the inner surface of platinum filament fixed plate 2 is welded with some platinum filaments 3 vertically, and conductive metal mesh 8 is horizontally placed at weak acid electricity
In solution liquid 5, the positive pole of expanded graphite worm cake 4 and platinum filament fixed plate 2 with power supply 6 be connected, conductive metal mesh 8 and power supply 6
Negative pole is connected.
The suspension bracket of platinum filament fixed plate 2 is placed in the top of container 1.Gluing connection is used between expanded graphite worm cake 4 and container 1.
The one end of conductive metal mesh 8 is fixed on the side wall of container 1 by support, and the other end accesses electricity by support through the side wall of container 1
Source 6.
Weak acid electrolyte 5 is preferably the weak acid such as dilute oxalic acid or dilute sulfuric acid.The material of reaction vessel 1 is non-conductive, can be with excellent
Select glass container.The voltage of power supply 6 is preferably 8 to 30 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, high temperature drying can obtain expanded graphite worm cake after dehydration.
Present invention additionally comprises a kind of method for preparing Graphene using upper device, comprise the following steps：Expanded graphite is compacted
Worm cake 4 is inlaid in the bottom of reaction vessel 1, then weak acid electrolyte 5 is full of into reaction vessel 1, then by platinum filament fixed plate 2 with hanging
Frame is fixed on the top of reaction vessel 1, and conductive metal mesh 8 is horizontally placed in weak acid electrolyte 5, by expanded graphite worm cake 4 and platinum
Silk fixed plate 2 is connected with the positive pole of power supply 6, and conductive metal mesh 8 is connected with the negative pole of power supply 6, turns on the power 6 switches to expansion stone
Black worm cake 2 is electrolysed, and fully after electrolysis, filtering is cleaned after the mixture of Graphene and electrolyte is taken out, then will filtering
The Graphene for obtaining carries out ultrasonication drying, that is, obtain required Graphene.
The principle of present embodiment：After logical 3 to the 30 volt voltages of power supply 6, the energization of platinum filament 3 can make the expanded graphite in electrolyte
Worm cake 7 is electrolysed, and by adding conductive metal mesh, expanded graphite worm cake can be electrolysed twice simultaneously, is shelled
From into Graphene.Then the mixture of weak acid electrolyte 5 and Graphene is poured out from container 1, using filter to mixture
Filtered, ultrasound is carried out to the Graphene for leaching using ultrasonic wave, Graphene is dried using dryer, completed graphite
The electrolytic preparation of alkene.The method is simple and easy to apply and single-layer graphene accounting is very high.
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 utilization platinum filament and graphite cake prepare the device of Graphene, it is characterised in that：Described device includes container (1), platinum
Silk fixed plate (2), expanded graphite worm cake (4), weak acid electrolyte (5), power supply (6), conductive metal mesh (8) and some platinum filaments
(3), expanded graphite worm cake (4) is inlaid in and weak acid electrolyte (5) is full of in the bottom of container (1), container (1), and platinum filament is fixed
The inner surface of plate (2) is welded with some platinum filaments (3) vertically, and conductive metal mesh (8) is horizontally placed in weak acid electrolyte (5), expands stone
The positive pole of black worm cake (4) and platinum filament fixed plate (2) with power supply (6) is connected, the negative pole of conductive metal mesh (8) and power supply (6)
Connection.
2. a kind of utilization platinum filament according to claim 1 and graphite cake prepare the device of Graphene, it is characterised in that：It is described
Platinum filament fixed plate (2) suspension bracket is placed in container (1) top.
3. a kind of utilization platinum filament according to claim 1 and 2 and graphite cake prepare the device of Graphene, it is characterised in that：
Gluing connection is used between the expanded graphite worm cake (4) and container (1).
4. a kind of utilization platinum filament according to claim 1 and graphite cake prepare the device of Graphene, it is characterised in that weak acid
Electrolyte (5) is the weak acid such as dilute oxalic acid or dilute sulfuric acid.
5. a kind of utilization platinum filament according to claim 1 and graphite cake prepare the device of Graphene, it is characterised in that container
(1) material is non-conductive.
6. a kind of utilization platinum filament according to claim 1 and graphite cake prepare the device of Graphene, it is characterised in that conductive
Wire netting (8) one end is fixed on the side wall of container (1) by support, and the other end is accessed by support through the side wall of container (1)
Power supply (6).
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 worm cake (4) is inlaid in the bottom of reaction vessel (1), then by weak acid electrolyte (5) full of reaction vessel (1),
Then platinum filament fixed plate (2) is fixed on reaction vessel (1) top with suspension bracket, conductive metal mesh (8) is horizontally placed at weak acid electrolysis
In liquid (5), expanded graphite worm cake (4) and platinum filament fixed plate (2) are connected with the positive pole of power supply (6), conductive metal mesh (8) with
The negative pole connection of power supply (6), turns on the power (6) switch and expanded graphite worm cake (2) is electrolysed, fully after electrolysis, by stone
Black alkene cleans filtering after being taken out with the mixture of electrolyte, then the Graphene that will be filtrated to get carries out ultrasonication drying, obtains final product
To 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)
Preferably 3 to 30 volts.
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| CN201710199499.7A CN106865532B (en) | 2017-03-25 | 2017-03-25 | A kind of device preparing graphene using platinum filament and graphite cake |
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| CN201710199499.7A CN106865532B (en) | 2017-03-25 | 2017-03-25 | A kind of device preparing graphene using platinum filament and graphite cake |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109205600A (en) * | 2017-07-07 | 2019-01-15 | 哈尔滨摆渡新材料有限公司 | A kind of device and method preparing graphene using galvanized wire |
| CN111032568A (en) * | 2017-08-11 | 2020-04-17 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
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| 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 |
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| KR20120103987A (en) * | 2011-03-11 | 2012-09-20 | 인하대학교 산학협력단 | Method of manufacturing graphene using electronic decomposition |
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| CN103204494A (en) * | 2012-01-16 | 2013-07-17 | 中央研究院 | Device and method used for scale production of graphene and graphene oxide |
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| CN109205600A (en) * | 2017-07-07 | 2019-01-15 | 哈尔滨摆渡新材料有限公司 | A kind of device and method preparing graphene using galvanized wire |
| CN111032568A (en) * | 2017-08-11 | 2020-04-17 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
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| CN106865532B (en) | 2019-06-04 |
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