CN106865535B - 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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- CN106865535B CN106865535B CN201710212527.4A CN201710212527A CN106865535B CN 106865535 B CN106865535 B CN 106865535B CN 201710212527 A CN201710212527 A CN 201710212527A CN 106865535 B CN106865535 B CN 106865535B
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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
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Abstract
The present invention relates to a kind of devices that graphene is prepared using platinum filament, described device includes container, platinum filament fixed plate, metal plate, weak acid electrolyte, power supply, expanded graphite worm and several platinum filaments, the mixed liquor of weak acid electrolyte and expanded graphite worm is full of in container, platinum filament fixed plate is inlaid in the bottom of container, and 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, and 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
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 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, described device includes container 1, platinum
Silk 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 placed in container 1
Top, the mixed liquor of weak acid electrolyte 5 and expanded graphite worm 7 is full of in container 1, platinum filament fixed plate 2 is inlaid in container 1
Bottom, 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 connected by conducting wire and platinum filament fixed plate 2
It connects, the cathode of power supply 6 is connect by conducting wire with metal plate 4.
Further, glue sticking is used between the platinum filament fixed plate 2 and container 1.
Further, the metal plate 4 is placed in 1 top of container with hanger.
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 also includes a kind of methods for preparing graphene using above-mentioned preparation, comprising the following steps: fixes platinum filament
Plate 2 is inlaid in the bottom of container 1, then weak acid electrolyte 5 is full of container 1, fixes metal plate 4 after expanded graphite worm is added
On 1 top of container, the anode of 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 metal plate 4
Connection is opened the switch of power supply 6 and is electrolysed to expanded graphite worm cake 2, sufficiently after electrolysis, by the mixed of graphene and electrolyte
It closes and cleans filtering after object takes 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 8 to 30 volts.
The invention has the following beneficial effects: the principles of the invention that electrolysis is mainly utilized, and expanded graphite worm is added
Into electrolyte, then accesses in circuit and be electrolysed, the continuous electrolysis by platinum filament to expanded graphite worm, so that expanded graphite
Worm is successively removed in the electrolytic solution, is then filtered cleaning, drying and has just been obtained required graphene.In obtained graphene
In, the ratio that single-layer graphene accounts for is great, and this method is simple for process.
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 includes container 1, platinum filament fixed plate 2, metal plate 4, weak acid electrolyte 5, power supply 6, stone
Ink 7 and several platinum filaments 3, metal plate 4 are inlaid in the top of cylindrical container 1, are full of weak acid electrolyte 5 and graphite 7, platinum in container 1
Silk fixed plate 2 is mounted on the bottom of cylindrical container 1, and the inner surface of platinum filament fixed plate 2 is welded with several platinum filaments 3 vertically, and power supply 6 is just
Pole 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.The material of platinum filament fixed plate 2
For metal.Glue sticking is used between platinum filament fixed plate 2 and container 1, conductive metal sheet 4 is placed in 1 top of container with hanger.It designs in this way
Liquid is taken convenient for being repeatedly opened.
The preferably weak acid such as dilute oxalic acid or dilute sulfuric acid of weak acid electrolyte 5.The material of container 1 is non-conductive, can be with
It is preferred that 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: by platinum filament fixed plate 2
It is inlaid in the bottom of container 1, then weak acid electrolyte 5 is full of container 1, is placed at metal plate 4 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 cake 2 is electrolysed, sufficiently after electrolysis, by the mixture of graphene and electrolyte
Filtering is cleaned after taking-up, 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 10 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 Ultrasound Instrument, 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 set
In the top of container (1), the mixed liquor of weak acid electrolyte (5) and expanded graphite worm (7) is full of in container (1), platinum filament is fixed
Plate (2) is inlaid in the bottom of container (1), and the inner surface of platinum filament fixed plate (2) is welded with several platinum filaments (3) vertically, and power supply (6) is just
Pole is connect by conducting wire with platinum filament fixed plate (2), and 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
Glue sticking is used between plate (2) and container (1).
3. a kind of device for preparing graphene using platinum filament according to claim 1 or 2, it is characterised in that: the metal
Plate (4) is placed in above container (1) with hanger.
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:
Platinum filament fixed plate (2) is inlaid in the bottom of container (1), then weak acid electrolyte (5) are full of container (1), expanded graphite is added
Metal plate (4) is placed above container (1) after worm, 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), is opened power supply (6) switch and is electrolysed to expanded graphite worm cake,
Sufficiently after electrolysis, cleans and filter after the mixture of graphene and electrolyte is taken out, then the graphene being obtained by filtration is surpassed
Sound crushing drying to get arrive required graphene.
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 8 of power supply (6)
To 30 volts.
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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 |
WO2019028803A1 (en) * | 2017-08-11 | 2019-02-14 | 徐海波 | Method and device for electrochemically preparing graphene oxide |
CN115403036B (en) * | 2022-08-30 | 2023-07-25 | 中钢天源股份有限公司 | Device, method and application for continuous electrochemical stripping |
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US4400451A (en) * | 1981-05-04 | 1983-08-23 | Diamond Shamrock Corporation | Solar energy converter |
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 |
CN102807213B (en) * | 2012-08-30 | 2015-09-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electrochemistry prepares the method for 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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Patent Citations (4)
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US4400451A (en) * | 1981-05-04 | 1983-08-23 | Diamond Shamrock Corporation | Solar energy converter |
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 |
CN102807213B (en) * | 2012-08-30 | 2015-09-09 | 中国科学院苏州纳米技术与纳米仿生研究所 | Electrochemistry prepares the method for Graphene |
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