CN106865532B - A kind of device preparing graphene using platinum filament and graphite cake - Google Patents
A kind of device preparing graphene using platinum filament and graphite cake Download PDFInfo
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- CN106865532B CN106865532B CN201710199499.7A CN201710199499A CN106865532B CN 106865532 B CN106865532 B CN 106865532B CN 201710199499 A CN201710199499 A CN 201710199499A CN 106865532 B CN106865532 B CN 106865532B
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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 and graphite cake, including container, platinum filament fixed plate, expanded graphite worm cake, weak acid electrolyte, power supply, conductive metal mesh and several 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 several platinum filaments vertically.The principle of electrolysis is mainly utilized in the present invention, continuous electrolysis by conductive metal mesh to expanded graphite worm cake, so that expanded graphite is successively removed in the electrolytic solution, using the continuous electrolysis of platinum filament, expanded graphite worm is set to have obtained sufficient electrolysis stripping, cleaning filtering drying has just obtained required graphene after the completion of electrolysis.
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.
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, 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 a kind of device for preparing graphene using platinum filament and graphite cake, described device include
Container 1, platinum filament fixed plate 2, expanded graphite worm cake 4, weak acid electrolyte 5, power supply 6, conductive metal mesh 8 and several platinum filaments 3, it is swollen
Swollen graphite worm cake 4 is inlaid in the bottom of container 1, is full of weak acid electrolyte 5 in container 1, the inner surface of platinum filament fixed plate 2 is vertical
Several platinum filaments 3 are welded with, conductive metal mesh 8 is horizontally placed in weak acid electrolyte 5, and expanded graphite worm cake 4 and platinum filament fixed plate 2 are equal
It is connect with the anode of power supply 6, conductive metal mesh 8 is connect with the cathode of power supply 6.
Further, the platinum filament fixed plate 2 is placed in 1 top of container with hanger.
Further, it is connected between the expanded graphite worm cake 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.
Further, 8 one end of conductive metal mesh is fixed by the bracket the side wall in container 1, and the other end is passed through by bracket
The side wall of container 1 accesses power supply 6.
The invention further relates to a kind of methods for preparing graphene using above-mentioned apparatus, comprising the following steps: by expanded graphite
Worm cake 4 is inlaid in the bottom of container 1, then weak acid electrolyte 5 is full of anti-device 1, then fixes platinum filament fixed plate 2 with hanger
Above container 1, conductive metal mesh 8 is horizontally placed in weak acid electrolyte 5, by expanded graphite worm cake 4 and platinum filament fixed plate 2 with
The anode connection of power supply 6, conductive metal mesh 8 connect with the cathode of power supply 6, opening power supply 6 switch to expanded graphite worm cake 2 into
Row electrolysis sufficiently after electrolysis, is cleaned after the mixture of graphene and electrolyte is taken out and is filtered, then the graphene that will be obtained by filtration
Ultrasonication drying is carried out 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 3 to 30 volts.
The invention has the following beneficial effects: the principles of the invention that electrolysis is mainly utilized, by conductive metal mesh to swollen
The continuous electrolysis of swollen graphite worm cake, so that expanded graphite is successively removed in the electrolytic solution, using the continuous electrolysis of platinum filament,
Expanded graphite worm is set to have obtained sufficient electrolysis stripping, cleaning filtering drying has just obtained required graphite after the completion of electrolysis
Alkene.
By the way that conductive metal mesh is added, can be in expanded graphite worm cake and liquid the graphite worm sufficiently removed simultaneously
It is electrolysed twice, strengthens electrolytic efficiency.In obtained graphene, the ratio that single-layer graphene accounts for is great, and this method work
Skill is simply 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, 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 several platinum filaments 3, expanded graphite worm cake 4 are inlaid in the bottom of container 1, fill in container 1
Full weak acid electrolyte 5, the inner surface of platinum filament fixed plate 2 are welded with several platinum filaments 3 vertically, and conductive metal mesh 8 is horizontally placed at weak acid electricity
It solves in liquid 5, expanded graphite worm cake 4 and platinum filament fixed plate 2 are connect with the anode of power supply 6, conductive metal mesh 8 and power supply 6
Cathode connection.
Platinum filament fixed plate 2 is placed in 1 top of container with hanger.It is connected between expanded graphite worm cake 4 and container 1 with gluing.
8 one end of conductive metal mesh is fixed by the bracket the side wall in container 1, and the other end accesses electricity by the side wall that bracket passes through 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 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 cake after dehydration.
The invention also includes a kind of methods for preparing graphene using upper device, comprising the following steps: expanded graphite is compacted
Worm cake 4 is inlaid in the bottom of container 1, then weak acid electrolyte 5 is full of container 1, is then fixed on platinum filament fixed plate 2 with hanger
1 top of container, conductive metal mesh 8 are horizontally placed in weak acid electrolyte 5, by expanded graphite worm cake 4 and platinum filament fixed plate 2 and electricity
The anode connection in source 6, conductive metal mesh 8 are connect with the cathode of power supply 6, are opened the switch of power supply 6 and are carried out to expanded graphite worm cake 2
Electrolysis, sufficiently electrolysis after, will the mixture of graphene and electrolyte take out after clean filtering, then by the graphene being obtained by filtration into
Row ultrasonication dries to arrive required graphene.
The principle of present embodiment: after power supply 6 leads to 3 to 30 volt voltages, the energization of platinum filament 3 can make the expanded graphite in electrolyte
Worm cake 7 is electrolysed, and by the way that conductive metal mesh is added, can be electrolysed twice, be shelled simultaneously to expanded graphite worm cake
From at graphene.Then the mixture that weak acid electrolyte 5 Yu graphene are poured out from container 1, using filter device to mixture
It is filtered, ultrasound is carried out to the graphene filtered out using ultrasonic wave, graphene is dried using dryer, completes graphite
The electrolytic preparation of alkene.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 (9)
1. a kind of device for preparing graphene using platinum filament and graphite cake, 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 several platinum filaments
(3), expanded graphite worm cake (4) is inlaid in the bottom of container (1), is full of weak acid electrolyte (5) in container (1), platinum filament is fixed
The inner surface of plate (2) is welded with several platinum filaments (3) vertically, and conductive metal mesh (8) is horizontally placed in weak acid electrolyte (5), expands stone
Black worm cake (4) and platinum filament fixed plate (2) are connect with the anode of power supply (6), the cathode of conductive metal mesh (8) and power supply (6)
Connection.
2. a kind of device for preparing graphene using platinum filament and graphite cake according to claim 1, it is characterised in that: described
Platinum filament fixed plate (2) is placed in above container (1) with hanger.
3. a kind of device for preparing graphene using platinum filament and graphite cake according to claim 1 or 2, it is characterised in that:
It is connect between the expanded graphite worm cake (4) and container (1) with gluing.
4. a kind of device for preparing graphene using platinum filament and graphite cake according to claim 1, which is characterized in that weak acid
Electrolyte (5) is dilute oxalic acid or dilute sulfuric acid.
5. a kind of device for preparing graphene using platinum filament and graphite cake according to claim 1, which is characterized in that container
(1) material is non-conductive.
6. a kind of device for preparing graphene using platinum filament and graphite cake according to claim 1, which is characterized in that conductive
Metal mesh (8) one end is fixed by the bracket the side wall in container (1), and the other end is accessed by the side wall that bracket passes through container (1)
Power supply (6).
7. a kind of method for preparing graphene using any one of the claims 1 to 6, which comprises the following steps:
Expanded graphite worm cake (4) is inlaid in the bottom of container (1), then weak acid electrolyte (5) are full of container (1), then by platinum
Silk fixed plate (2) is fixed on above container (1) with hanger, and conductive metal mesh (8) is horizontally placed in weak acid electrolyte (5), will be swollen
Swollen graphite worm cake (4) and platinum filament fixed plate (2) are connect with the anode of power supply (6), and conductive metal mesh (8) is negative with power supply (6)
Pole connection is opened power supply (6) switch and is electrolysed to expanded graphite worm cake, sufficiently after electrolysis, by graphene and electrolyte
Mixture cleans filtering after taking out, then the graphene being obtained by filtration is carried out ultrasonication drying to get required graphene is arrived.
8. the method that a kind of electrolysis method according to claim 7 prepares graphene, which is characterized in that weak acid electrolyte (5)
For dilute oxalic acid or dilute sulfuric acid.
9. the method that a kind of electrolysis method according to claim 8 prepares graphene, which is characterized 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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| CN106865532B true CN106865532B (en) | 2019-06-04 |
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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 |
| CN111032568B (en) * | 2017-08-11 | 2023-04-25 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
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| KR20120103987A (en) * | 2011-03-11 | 2012-09-20 | 인하대학교 산학협력단 | Method of manufacturing graphene using electronic decomposition |
| 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 |
| 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 |
| 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 |
| 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 |
| 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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