CN106865533A - A kind of utilization platinum filament prepares the device and method of Graphene - Google Patents
A kind of utilization platinum filament prepares the device and method of Graphene Download PDFInfo
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- CN106865533A CN106865533A CN201710205345.4A CN201710205345A CN106865533A CN 106865533 A CN106865533 A CN 106865533A CN 201710205345 A CN201710205345 A CN 201710205345A CN 106865533 A CN106865533 A CN 106865533A
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- graphene
- platinum filament
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- 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 the device that a kind of utilization platinum filament prepares Graphene, described device includes closed container, platinum filament fixed plate, metallic plate, weak acid electrolyte, power supply, expanded graphite and some platinum filaments, metallic plate is inlaid in the bottom of container, mixed liquor full of weak acid electrolyte and expanded graphite 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, expanded graphite worm is added in electrolyte, electric current is passed through again to be electrolysed expanded graphite worm, continuous electrolysis by platinum filament to expanded graphite, so that expanded graphite is successively peeled off in the electrolytic solution, then filter cleaning, drying and just obtained required Graphene.In the Graphene for obtaining, the ratio that single-layer graphene is accounted for is great, and the method is simple for process.
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.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, 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 prepares the device of Graphene, including a kind of using platinum filament preparation
The device of Graphene, described device includes container 1, platinum filament fixed plate 2, metallic plate 4, weak acid electrolyte 5, power supply 6, expanded graphite
Worm 7 and some platinum filaments 3, metallic plate 4 are inlaid in compacted full of weak acid electrolyte 5 and expanded graphite in the bottom of container 1, container 1
The mixed liquor of worm 7, the inner surface of platinum filament fixed plate 2 is welded with some platinum filaments 3 vertically, and the positive pole of power supply 6 is consolidated by wire with platinum filament
Fixed board 2 is connected, and the negative pole of power supply 6 is connected by wire with metallic plate 4.
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 metallic plate 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.
The invention further relates to a kind of method that utilization said apparatus prepare Graphene, comprise the following steps：Metallic plate 4 is embedding
Mounted in the bottom of reaction vessel 1, then weak acid electrolyte 5 is full of reaction vessel 1, fixes platinum filament after adding expanded graphite worm
Plate 2 is placed in the top of reaction vessel 1, and the positive pole of power supply 6 is connected by wire with platinum filament fixed plate 2, and the negative pole of power supply 6 passes through wire
It is connected with metallic plate 4, turns on the power 6 switches and expanded graphite worm 2 is electrolysed, fully after electrolysis, by Graphene and electrolysis
The mixture of liquid cleans filtering after taking out, then the Graphene that will be filtrated to get carries out ultrasonication drying, that is, obtain required graphite
Alkene.
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 present invention has the advantages that：The present invention mainly make use of the principle of electrolysis, and expanded graphite is added into electricity
In solution liquid, then access and be electrolysed in circuit, the continuous electrolysis by platinum filament to expanded graphite worm so that expanded graphite worm
Successively peeled off in the electrolytic solution, then filter cleaning, drying and just obtained required Graphene.It is single in the Graphene for obtaining
The ratio that layer graphene is accounted for is great, and the method process is simple is 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, present embodiment includes container 1, platinum filament fixed plate 2, metallic plate 4, weak acid electrolyte 5, power supply 6, swollen
Swollen graphite worm 7 and some platinum filaments 3, metallic plate 4 are inlaid in the bottom of container 1, container 1 full of weak acid electrolyte 5 and expansion
Graphite worm 7, the suspension bracket of platinum filament fixed plate 2 is placed in the top of container 1, and the inner surface of platinum filament fixed plate 2 is welded with some platinum vertically
Silk 3, the positive pole of power supply 6 is connected by wire with platinum filament fixed plate 2, and the negative pole of power supply 6 is by wire and circle metallic plate 4.Platinum filament
The material of fixed plate 2 is metal.Glue sticking is used between conductive metal sheet 4 and reaction vessel 1.
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 after dehydration.
Present invention additionally comprises a kind of method for preparing Graphene using upper device, comprise the following steps：Metallic plate 4 is embedded in
In the bottom of reaction vessel 1, then weak acid electrolyte 5 is full of reaction vessel 1, by platinum filament fixed plate after addition expanded graphite worm
2 are fixed on the top of reaction vessel 1, and the positive pole of power supply 6 is connected by wire with platinum filament fixed plate 2, and the negative pole of power supply 6 passes through wire
It is connected with metallic plate 4, turns on the power 6 switches and expanded graphite cake 2 is electrolysed, fully after electrolysis, by Graphene and electrolyte
Mixture take out after clean filtering, then the Graphene that will be filtrated to get carries out ultrasonication drying, that is, obtain required Graphene.
The principle of present embodiment：After logical 8 to the 30 volt voltages of power supply 6, the energization of platinum filament 3 can make the expanded graphite in electrolyte
Worm 7 is electrolysed, and is peeled off into Graphene, and the mixture of weak acid electrolyte 5 and Graphene is then poured out from container 1,
Mixture is filtered using filter, ultrasound is carried out to the Graphene for leaching using ultrasonic wave, using dryer to stone
Black alkene is dried, and completes the electrolytic preparation of Graphene.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 (8)
1. a kind of utilization platinum filament prepares the device of Graphene, it is characterised in that：Described device includes container (1), platinum filament fixed plate
(2), metallic plate (4), weak acid electrolyte (5), power supply (6), expanded graphite worm (7) and some platinum filaments (3), metallic plate (4) are embedding
The mixed liquor full of weak acid electrolyte (5) and expanded graphite worm (7) in the bottom of container (1), container (1), platinum filament is solid
The inner surface of fixed board (2) is welded with some platinum filaments (3) vertically, and the positive pole of power supply (6) is connected by wire with platinum filament fixed plate (2),
The negative pole of power supply (6) is connected by wire with metallic plate (4).
2. a kind of utilization platinum filament according to claim 1 prepares the device of Graphene, it is characterised in that：The platinum filament is fixed
Plate (2) suspension bracket is placed in container (1) top.
3. a kind of utilization platinum filament according to claim 1 and 2 prepares the device of Graphene, it is characterised in that：The metal
Gluing connection is used between plate (4) and container (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 container (1) is non-conductive.
6. a kind of method that any one of utilization the claims 1 to 5 prepares Graphene, it is characterised in that comprise the following steps：
Metallic plate (4) is inlaid in the bottom of reaction vessel (1), then by weak acid electrolyte (5) full of reaction vessel (1), adds expansion
Platinum filament fixed plate (2) is placed in reaction vessel (1) top after graphite worm, the positive pole of power supply (6) is fixed by wire with platinum filament
Plate (2) is connected, and the negative pole of power supply (6) is connected by wire with metallic plate (4), turns on the power (6) switch to expanded graphite worm
(2) be electrolysed, fully after electrolysis, will Graphene and electrolyte mixture take out after clean filtering, then will be filtrated to get
Graphene carries out ultrasonication drying, that is, obtain required Graphene.
7. the method that a kind of electrolysis according to claim 6 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.
8. the method that a kind of electrolysis according to claim 7 prepares Graphene, it is characterised in that the voltage of power supply (6)
It is 8 to 30 volts.
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| CN201710205345.4A CN106865533B (en) | 2017-03-25 | 2017-03-25 | A kind of device and method preparing graphene using platinum filament |
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| CN201710205345.4A CN106865533B (en) | 2017-03-25 | 2017-03-25 | A kind of device and method preparing graphene using platinum filament |
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| CN106865533A true CN106865533A (en) | 2017-06-20 |
| CN106865533B CN106865533B (en) | 2019-06-04 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111032568A (en) * | 2017-08-11 | 2020-04-17 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
| CN112938950A (en) * | 2021-03-19 | 2021-06-11 | 西安理工大学 | Graphene quantum dot solution prepared by electrochemical method and method |
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| KR20120103987A (en) * | 2011-03-11 | 2012-09-20 | 인하대학교 산학협력단 | Method of manufacturing graphene using electronic decomposition |
| CN103245104A (en) * | 2012-02-08 | 2013-08-14 | 宓玉敏 | Split type solar water heater inner machine |
| 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 |
| CN103991862A (en) * | 2013-12-27 | 2014-08-20 | 杭州金马能源科技有限公司 | Method for preparing high-quality graphene through electrochemical high-efficiency exfoliation |
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| KR20120103987A (en) * | 2011-03-11 | 2012-09-20 | 인하대학교 산학협력단 | Method of manufacturing graphene using electronic decomposition |
| 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 |
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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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| CN111032568A (en) * | 2017-08-11 | 2020-04-17 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
| CN112938950A (en) * | 2021-03-19 | 2021-06-11 | 西安理工大学 | Graphene quantum dot solution prepared by electrochemical method and method |
| CN112938950B (en) * | 2021-03-19 | 2022-12-02 | 西安理工大学 | Graphene quantum dot solution prepared by electrochemical method and method |
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| CN106865533B (en) | 2019-06-04 |
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