CN106865533B - A kind of device and method preparing graphene using platinum filament - Google Patents
A kind of device and method preparing graphene using platinum filament Download PDFInfo
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- CN106865533B CN106865533B CN201710205345.4A CN201710205345A CN106865533B CN 106865533 B CN106865533 B CN 106865533B CN 201710205345 A CN201710205345 A CN 201710205345A CN 106865533 B CN106865533 B CN 106865533B
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- platinum filament
- expanded graphite
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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 devices that graphene is prepared using platinum filament, described device includes closed container, platinum filament fixed plate, metal plate, weak acid electrolyte, power supply, expanded graphite and several platinum filaments, metal plate is inlaid in the bottom of container, the mixed liquor of weak acid electrolyte and expanded graphite is full of in container, the inner surface of platinum filament fixed plate is welded with several platinum filaments vertically.The principle of electrolysis is mainly utilized in the present invention, 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 removed in the electrolytic solution, then filters cleaning, drying and just obtained required graphene.In obtained graphene, the ratio that single-layer graphene accounts for is great, and this method is simple for process.
Description
Technical field
The invention belongs to technical field of graphene preparation, and in particular to a kind of device and side that graphene is prepared using platinum filament
Method.
Background technique
Graphene is the two dimensional crystal for being stripped out from natural 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 preparation methods of natural graphite alkene: mechanical means and chemical method.Mechanical means
Including mechanical phonograph recorder separation, epitaxy method and the method for heating SiC, chemical method is that chemical reduction method and chemistry dissociate
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.Change
Learning dissociation method is the method that graphite oxide is prepared graphene by the method heat-treated, the oxygen-containing functional group of graphite oxide interlayer
It reacts at a certain temperature.
Wherein, electrolysis method is the most common method for preparing graphene, but there are graphene yield is too low, purity is not high
The problem of.
Summary of the invention
The purpose of the present invention is to solve in existing graphene preparation technology, production technology is complicated, graphene purity compared with
Low problem, and then a kind of device and method for preparing graphene is provided.
The technical scheme is that prepared by a kind of device for being prepared graphene using platinum filament, including a kind of utilization platinum filament
The device of graphene, described device include container 1, platinum filament fixed plate 2, metal plate 4, weak acid electrolyte 5, power supply 6, expanded graphite
Worm 7 and several platinum filaments 3, metal plate 4 are inlaid in the bottom of container 1, are full of weak acid electrolyte 5 in container 1 and expanded graphite is compacted
The mixed liquor of worm 7, the inner surface of platinum filament fixed plate 2 are welded with several platinum filaments 3 vertically, and the anode of power supply 6 is solid by conducting wire and platinum filament
Fixed board 2 connects, and the cathode of power supply 6 is connect by conducting wire with metal plate 4.
Further, the platinum filament fixed plate 2 is placed in 1 top of container with hanger.
Further, it is connected between the metal plate 4 and container 1 with gluing.
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 methods for preparing graphene using above-mentioned apparatus, comprising the following steps: metal plate 4 is embedding
It is full of container 1 mounted in the bottom of container 1, then by weak acid electrolyte 5, is placed in platinum filament fixed plate 2 after expanded graphite worm is added
1 top of container, the anode of power supply 6 are connect by conducting wire with platinum filament fixed plate 2, and the cathode of power supply 6 is connected by conducting wire and metal plate 4
It connects, opens the switch of power supply 6 and expanded graphite worm 2 is electrolysed, sufficiently after electrolysis, the mixture of graphene and electrolyte is taken
Filtering is cleaned after out, then the graphene being obtained by filtration is subjected to ultrasonication drying 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, and expanded graphite is added to electricity
It solves in liquid, then accesses in circuit and be electrolysed, the continuous electrolysis by platinum filament to expanded graphite worm, so that expanded graphite worm
It is successively removed in the electrolytic solution, then filters cleaning, drying and just obtained required graphene.It is single in obtained graphene
The ratio that layer graphene accounts for is great, and this method simple process is easy to install.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Specific embodiment
The present invention will be further described combined with specific embodiments below:
Refering to fig. 1, present embodiment include container 1, it is platinum filament fixed plate 2, metal plate 4, weak acid electrolyte 5, power supply 6, swollen
Swollen graphite worm 7 and several platinum filaments 3, metal plate 4 are inlaid in the bottom of container 1, are full of weak acid electrolyte 5 and expansion in container 1
Graphite worm 7, platinum filament fixed plate 2 are placed in the top of container 1 with hanger, and the inner surface of platinum filament fixed plate 2 is welded with several platinum vertically
The anode of silk 3, power supply 6 is connect by conducting wire with platinum filament fixed plate 2, and the cathode of power supply 6 passes through conducting wire and circle metal plate 4.Platinum filament
The material of fixed plate 2 is metal.Glue sticking is used between conductive metal sheet 4 and container 1.
Weak acid electrolyte 5 is preferably the weak acid such as dilute oxalic acid or dilute sulfuric acid.The material of container 1 is non-conductive, can preferred glass
Glass container.The voltage of power supply 6 is 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, high temperature drying can obtain expanded graphite worm after dehydration.
The invention also includes a kind of methods for preparing graphene using upper device, comprising the following steps: is embedded in metal plate 4
It is full of container 1 in the bottom of container 1, then by weak acid electrolyte 5, is fixed on platinum filament fixed plate 2 after expanded graphite worm is added
1 top of container, the anode of power supply 6 are connect by conducting wire with platinum filament fixed plate 2, and the cathode of power supply 6 is connected by conducting wire and metal plate 4
It connects, opens the switch of power supply 6 and expanded graphite cake 2 is electrolysed, sufficiently after electrolysis, the mixture of graphene and electrolyte is taken out
Cleaning filtering afterwards, then the graphene being obtained by filtration is subjected to ultrasonication drying to get required graphene is arrived.
The principle of present embodiment: after power supply 6 leads to 8 to 30 volt voltages, the energization of platinum filament 3 can make the expanded graphite in electrolyte
Worm 7 is electrolysed, and is removed into graphene, and the mixture of weak acid electrolyte 5 Yu graphene is then poured out from container 1,
Mixture is filtered using filter device, ultrasound is carried out to the graphene filtered out using ultrasonic wave, using dryer to stone
Black alkene is dried, and the electrolytic preparation of graphene is completed.The method is simple and easy and single-layer graphene accounting is very high.
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 (8)
1. a kind of device for preparing graphene using platinum filament, it is characterised in that: described device includes container (1), platinum filament fixed plate
(2), metal plate (4), weak acid electrolyte (5), power supply (6), expanded graphite worm (7) and several platinum filaments (3), metal plate (4) are embedding
The mixed liquor of weak acid electrolyte (5) and expanded graphite worm (7) is full of in the bottom of container (1), container (1), platinum filament is solid
The inner surface of fixed board (2) is welded with several platinum filaments (3) vertically, and the anode of power supply (6) is connect by conducting wire with platinum filament fixed plate (2),
The cathode of power supply (6) is connect by conducting wire with metal plate (4).
2. a kind of device for preparing graphene using platinum filament according to claim 1, it is characterised in that: the platinum filament is fixed
Plate (2) is placed in above container (1) with hanger.
3. a kind of device for preparing graphene using platinum filament according to claim 1 or 2, it is characterised in that: the metal
It is connect between plate (4) and container (1) with gluing.
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 or dilute sulfuric acid.
5. a kind of device for preparing graphene according to claim 1, which is characterized in that the material of container (1) is non-conductive.
6. a kind of method for preparing graphene using any one of the claims 1 to 5, which comprises the following steps:
Metal plate (4) is inlaid in the bottom of container (1), then weak acid electrolyte (5) are full of container (1), expanded graphite worm is added
Platinum filament fixed plate (2) is placed in above container (1) afterwards, the anode of power supply (6) is connect by conducting wire with platinum filament fixed plate (2), electricity
The cathode in source (6) is connect by conducting wire with metal plate (4), is opened power supply (6) switch and is electrolysed to expanded graphite worm, sufficiently
It after electrolysis, cleans and filters after the mixture of graphene and electrolyte is taken out, then the graphene being obtained by filtration progress ultrasound is broken
It is broken to dry to get required graphene is arrived.
7. the method that a kind of electrolysis method according to claim 6 prepares graphene, which is characterized in that weak acid electrolyte (5)
For dilute oxalic acid or dilute sulfuric acid.
8. the method that a kind of electrolysis method according to claim 7 prepares graphene, which is characterized in that the voltage of power supply (6)
For 8 to 30 volts.
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| CN106865533B true CN106865533B (en) | 2019-06-04 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111032568B (en) * | 2017-08-11 | 2023-04-25 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
| 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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| 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 |
| 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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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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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