CN106904602A - Graphene mass production equipment and its manufacture method - Google Patents
Graphene mass production equipment and its manufacture method Download PDFInfo
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- CN106904602A CN106904602A CN201510955588.0A CN201510955588A CN106904602A CN 106904602 A CN106904602 A CN 106904602A CN 201510955588 A CN201510955588 A CN 201510955588A CN 106904602 A CN106904602 A CN 106904602A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The present invention provides a kind of Graphene mass production equipment and its manufacture method, and its manufacture method includes：(1) first electrode and a second electrode are set in the electrolyte of an electrolytic cell, the first electrode is a positive pole, and second electrode is a negative pole, and the first electrode is to be located at one to have in the roller of screen cloth, and the roller has been built into plural graphite scrap；(2) apply under one first bias, and the roller is rolled under first bias, the graphite scrap is carried out ion Embedded step；(3) continue in rollers roll and apply one second bias, carry out the graphite scrap tears a layer strip step open；(4) graphite scrap forms at least one of which plural number Graphene fragment after tearing layer strip step open；(5) bottom that the plural Graphene fragment passes through the screen deposition of the roller electrolytic cell；Accordingly, the shortcoming of existing Graphene electrochemical stripping method manufacture can be solved, makes the exploitativeness with mass production, and facilitated the collection of Graphene, take, and then reach the splendid economic benefit of Graphene manufacture production.
Description
Technical field
Electrochemistry side is utilized the present invention relates to a kind of mass production technology of Graphene, more particularly to one kind
Formula and can largely produce Graphene and be easy to the collection of Graphene manufactured goods obtain Graphene mass production set
Standby and its manufacture method.
Background technology
Graphite is the crystal structure being made up of multi-layer graphene, and Graphene (graphene) is a kind of single
With sp between the graphite-structure of layer, each carbon atom2Crystalline texture and three adjacent carbon atom shapes
Into bond, and cellular hexagonal two-dimensional structure is extended into, current Graphene is widely used
In the fields such as semiconductor, contact panel or solar cell, and it is more expected be widely used in photoelectricity,
The development of many industrial fields such as green energy generates electricity, environment life doctor sensing, plyability functional material.
The manufacture method of existing Graphene includes：Mechanical stripping method (mechanical exfoliation),
Epitaxy flop-in method (Epitaxial growth), chemical gaseous phase depositing method (chemical vapor
Deposition, CVD), chemical stripping method (chemical exfoliation) and electrochemical stripping method
Methods such as (electrochemical exfoliation).As shown in figure 1, the top is by three individual layers
The graphite-structure schematic diagram that Graphene is combined into weak van der waals forces, middle graph is designated as with electrochemistry
Electrolysis makes Graphene and illustrates with coated graphite rod electrrode, is a kind of existing electrochemistry for manufacturing Graphene
Stripping method, its equipment includes an electrolytic cell 90, the electrolytic cell 90 be built-in with electrolyte 901 and
One positive electrode 91, negative electrode 92, wherein, the positive electrode 91 is a graphite material, and the negative electricity
Pole 92 is a metal or graphite material, is to carry out positive electrode stone using one first bias in its processing procedure
Insertion (intercalation) step of ink material, makes the anion in electrolyte 901 pass through voltage difference
And be intercalated between the adjacent two-layer graphite linings of positive electrode (barred body graphite material) and or its grain boundary
On (grain boundary), peeled off after the layer of tearing open that this graphite material is carried out using one second bias
(exfoliation) step, and Graphene 93 produced after peeling off will be deposited on the electrolytic cell 90
Bottom, that is, complete the generation manufacture of laboratory Graphene.Because Graphene 93 is a kind of monoatomic layer
Body, the Graphene 93A of its enlarged diagram lower section as shown, Graphene 93A may be provided in a base
On material 95, it is used to change the interaction property of the base material 95, such as electric conductivity, thermal conductivity, penetrance
Or structural strength etc..
The equipment and manufacture of the foregoing existing Graphene electrochemical stripping method, though it can manufacture life
Graphene is produced, but still with the presence of its shortcoming, for example：The existing Graphene electrochemical stripping method sets
Standby and manufacture, it is carried out without the static mode under suitably auxiliary external force is acted on, in production
During will also cause because of the non-coaxial symmetric design of electrode shape electric field between electrodes be distributed, electrolyte
The uneven phenomenons such as Pressure, Concentration, Temperature distribution, the effective lasting manufacture production of unfavorable Graphene, show
The manufacture method of non-ideal volume production.
Therefore, equipment and manufacture of the present inventor in view of existing Graphene electrochemical stripping method
Its volume production uses the fact that upper shortcoming and its global design are preferable to the greatest extent, that is, set about research and development and conceive it
Solution, it would be desirable to which developing one kind can have production, collect and take convenience and economic benefit
The Graphene mass production equipment and its manufacture method of property, to promote the development of this industry, then through it is many when
Conceive and have generation of the invention.
The content of the invention
The purpose of the present invention is to provide a kind of Graphene mass production equipment and its manufacture method, its energy
The shortcoming of existing Graphene electrochemical stripping method manufacture is solved, makes the exploitativeness with mass production,
And facilitate the collection of Graphene, take, and then reach the splendid economic benefit of Graphene manufacture production.
Another object of the present invention be providing a kind of Graphene mass production equipment and its manufacture method,
It can utilize rollers roll circulation power-assisted and coaxial-symmetrical electrode design make to put on be embedded into
The Electric Field Distribution for tearing the object of layer open is uniform, promote the insertion of graphite and strip step more efficiency,
Uniformity, and electrolyte is not produced the thermograde of inequality, and more conducively electrochemical stripping method
Manufacture production Graphene.
In order to reach above-mentioned purpose, its technological means for being used is included the present invention：One electrolytic cell,
It is built-in with a first electrode, the second electrode that electrolyte and leaching are located in the electrolyte；One roller
Device, the plural graphite scrap for including a roller and being located in the roller, the roller is that leaching is located at
In the electrolyte and be used to house the first electrode, the roller be by an interlinked mechanism interlock and rotate,
The screen cloth of plurality of through holes is provided with the barrel of the roller, the perforation of the screen cloth is greater than being shelled through tearing layer open
Graphene fragment after step, plural graphite scrap is that leaching is located in the electrolyte before this tears layer open,
The electrochemical step be used to be embedded in, peeling off and output Graphene fragment.
Aforementioned structure, the wherein first electrode are a positive pole, and the second electrode is a negative pole.
Aforementioned structure, it has further included a collection apparatus, and the collection apparatus are to be connected in the electricity
Solve the bottom of groove.
Aforementioned structure, the wherein collection apparatus are to include a pipeline and collecting tank, and the pipeline is to connect
An electric access slot outlet of the bottom of electrolytic tank is connected to, the collecting tank is to connect the pipeline, the collecting tank
Bottom is provided with the screened outlet that a tool plural number penetrates pore, and the pore that penetrates of the screened outlet is small
The Graphene chip size after this tears layer open.
Aforementioned structure, the wherein pipeline are to have further included one first pipeline, the second pipeline and
Three pipelines, first pipeline is connected between the electrolytic cell and the collecting tank, in first pipeline
The screen section of tool plural number screen cloth mesh perforation is provided with, the screen cloth mesh perforation of the screen section is big
In the size of the Graphene fragment.
Aforementioned structure, wherein second pipeline are the screened outlets for being connected to the collecting tank；One control
Groove processed, the control flume is to be connected to another end of second pipeline with respect to the collecting tank, and the control flume is
It is used to detect, adjusts concentration, acid-base value, the constituent for controlling the electrolyte.
Aforementioned structure, wherein the 3rd pipeline are to connect the control flume, and the 3rd pipeline is that have one
Go out geat, the electrolyte of the outflow control flume is reinjected the electrolytic cell.
Aforementioned structure, it has further included a supply tank, and the supply tank is connected with one the 4th pipeline
An interface of the 3rd pipeline is connect, is to be equipped with new electrolyte in the supply tank, the new electrolyte is through
Four pipelines are injected in the 3rd pipeline.
Manufacture method of the invention is included：(1) first electrode and a second electrode are set in an electricity
Solve groove electrolyte in, the first electrode be a positive pole, second electrode be a negative pole, and this first
Electrode is to be located at one to have in the roller of screen cloth, and the roller has been built into plural graphite scrap, the sieve
Net is provided with perforation of the plural number more than Graphene fragment, and the electrolyte is to perforate to pass in and out the rolling by the grade
Cylinder；(2) apply under one first bias, and the roller is rolled under first bias, make this
Graphite scrap carries out ion insertion (intercalation) step when electrode is contacted；(3) in rollers roll
In continue and apply one second and bias, the stripping for carrying out the graphite scrap tears layer (exfoliation) step open；(4)
The grade graphite scrap is stripped to tear formation at least one of which plural number Graphene fragment after layer step open；(5) this is answered
The bottom that number Graphene fragment passes through the screen deposition of the roller electrolytic cell.
It is to continue the plural Graphene fragment with electrolyte after preceding method, the wherein step (5)
The electrolytic cell is flowed out to be collected the operation of taking-up.
To make more have further understanding to technology of the invention, method characteristic and the effect reached
With understanding, careful assistant is with preferred embodiment figure and coordinates detailed description, illustrates as after.
Brief description of the drawings
Fig. 1 is that the electrochemistry of existing manufacture Graphene tears a layer stripping method schematic diagram open；
Fig. 2 is the schematic side view of present device；
Fig. 3 is the schematic perspective view of present device；
Fig. 4 is the running schematic side view of present device；
Fig. 5 is the schematic perspective view of another embodiment of present device；
Fig. 6 takes out structural representation for the collection of present device；
Fig. 7 is manufacturing method thereof schematic flow sheet of the invention.
Description of reference numerals：10- electrolytic cells；12- second electrodes；14- first electrodes；16- electrolyte；
18- hollow spaces；20- drum apparatus；21- rollers；211- screen clothes；212- electrolyzer outlets；22-
Graphite scrap；30- Graphene fragments；40- collection apparatus；41- pipelines；42- collecting tanks；421- is sieved
Net outlet；The pipelines of 43- first；431- screen sections；The pipelines of 44- second；441- interfaces；45- the 3rd
Pipeline；451- goes out geat；46- control flumes；47- supply tanks；The pipelines of 471- the 4th；S11- sets one
In the electrolyte of an electrolytic cell, the first electrode is a positive pole for first electrode and a second electrode,
Second electrode is a negative pole, and the first electrode is to be located at one to have in the roller of screen cloth, the screen cloth
It is provided with plural number and tears the perforation that layer dials the Graphene fragment produced from step, the electrolyte open more than through one
It is to perforate to pass in and out the roller by the grade；S12- is built into graphite scrap in the roller；S13- applies
Under one first bias, and the roller is rolled under first bias, enter the graphite scrap
Row ion Embedded step；S14- continues applying one second in rollers roll and biases, and carries out the graphite broken
The layer of tearing open of piece peels off (exfoliation) step；The S15- grade graphite scraps through tear open layer peel off after formed to
Few one layer of plural Graphene fragment；The perforation that the S16- plural Graphene fragments pass through the roller screen cloth
It is deposited on the bottom of the electrolytic cell；The S17- plural Graphene fragments flow out the electrolysis with electrolyte
Groove is being collected the operation of taking-up；S18- will collect the Graphene fragment for taking out with high temperature furnace or micro-
Wave heating or spray dried form or freeze-drying are dried.
Specific embodiment
Fig. 2, Fig. 3 and Fig. 4 are referred to, is Graphene mass production equipment of the present invention and its manufacture method
Preferred embodiment, those schemas are the schematic diagram to convenient illustrations, and it is only in a schematic way
Basic structure of the invention is illustrated, and shown structure is drawn not limit and is same as actual implementation
When shape and dimension scale, its it is actual implement when shape and dimension scale be a kind of selective
Design.As illustrated, Graphene mass production equipment of the present invention is to include an electrolytic cell 10 and roller
Device 20, the electrolytic cell 10 is built-in with the first electrode 14 of electrolyte 16 and one, second electrode 12,
The first electrode 14, second electrode 12 are that leaching is located in the electrolyte 16；Wherein, the electrolyte
16 composition is the solution with electrolyte, and electrolyte can include hydrochloric acid (HCl), sulfuric acid (H2SO4)
Or hydrogen bromide (HBr) etc. (in a certain embodiment, be the sulfuric acid using 0.024g/ml concentration), should
The scope of the pH-value (pH) of electrolyte 16, also can be in the electrolyte 16 between 1 to 10
(such as potassium hydroxide etc. is to use weight percent in a certain embodiment to add other additives
The potassium hydroxide of concentration 30%), quality preferably Graphene is obtained during in the hope of electrolysis.First electricity
Pole 14 is a positive pole, and the second electrode 12 is a negative pole, and the first electrode 14 is placed in roller,
Its material can be a graphite material or be a metal or alloy；The second electrode 12 is placed in roller
Outward, its material be alternatively a graphite material or be a metal alloy or its etc. it is made compound
Material, and the graphite material used by the electrode is in addition to comprising graphite (graphite), or square
Tropism graphite (highly oriented pyrolytic graphite, HOPG), pitch graphite (PAN-based
Graphite, pitch-based graphite) etc., and the metal used by the electrode is for one is difficult to be changed
Learn the precious metal of etching, for example, platinum (Pt), silver-colored (Ag), golden (Au), iridium (Ir), osmium (Os), palladium
(Pd), rhodium (Rh) or ruthenium (Ru) etc. or associated alloys.And due to the main material of Graphene output of the present invention
Self-electrode, therefore the first electrode 14, second electrode 12 are not come in material source such as prior art
Can mainly be connect with tearing the graphite scrap that is opposite in roller in layer processing procedure open and produce as electrochemical intercalation
The carrying out of conducting function is touched, its material is not limited with its polarity.
The drum apparatus 20 are the plural graphite scraps 22 for including a roller 21 and being placed in roller,
The roller 21 is that leaching is located in the electrolyte 16, and is used to house the first electrode 14, i.e., this
One electrode 14 is located in the roller 21, and the sieve of plurality of through holes is provided with the barrel of the roller 21
Net 211, the perforation of the screen cloth 211 is less than being placed in the graphite scrap in roller but more than through electrification
Tear the Graphene chip size after layer strip step open, and the electrolyte can be perforated by the grade and pass in and out rolling
Cylinder, the size of the screen cloth 211 can be between 18 to 1000 mesh mesh (mesh), preferably 35
The broken compared with coarse grain footpath graphite of layer stripping is not torn open between 300 mesh mesh (mesh), being used to filter keep here
Sheet material, and the individual layer peeled off or few layer graphene fragment is somebody's turn to do by passing through in the roller 21
Screen cloth 211 is dropped out outside cylinder；And the plural graphite scrap 22 is located in the roller 21, meanwhile,
The plural graphite scrap 22 also soaks and is located in the electrolyte 16.The roller 21 is one company of drive connection
Motivation structure (not shown), the i.e. roller 21 be by the interlinked mechanism interlock and in the electrolytic cell 10 (electricity
Solution liquid 16) in rotated, the roller 21 rotate when then drive the graphite scrap 22 in it to be turned over
It is dynamic.
Wherein, the graphite scrap 22 is：Native graphite (nature graphite), artificial synthesized graphite
(synthetic graphite), graphited carbon black (carbon black), graphited furnace black (furnace black),
Be situated between steady phase carbosphere (mesocarbon microbead write a Chinese character in simplified form MCMB) or directionality graphite (highly
Oriented graphite sheet, write a Chinese character in simplified form HOGS) or more several combinations with arbitrary proportion.
As shown in figure 4, when Graphene mass production equipment of the present invention is operated, the graphite in the roller 21
Fragment 22 fully will produce reciprocation with the electrolyte 16, be inclined using one first in its processing procedure
Pressure, and the roller 21 is carried out the (stone of graphite scrap 22 in being rolled under first bias
Ink material) insertion (intercalation) step, make anion such as sulfate radical in the electrolyte 16,
Nitrate ion etc. is intercalated into the graphite scrap 22 its two adjacent layer graphene by voltage difference
Between layer and/or on its grain boundary (grain boundary), first bias is between+0.5 volt
Between to+12 volts, and about 1 to 25 minute action time.It is sharp after continuing in the rolling of roller 21
The layer of tearing open that the graphite scrap 22 is carried out with one second bias peels off (exfoliation) step, wherein
Second bias is greater than the first bias, and between+12 volts to+36 volts, during its effect
Between about 1 to 45 minute.Separately, in processing procedure one the 3rd bias also can again be applied after second bias
Or the positive voltage of impulse waveform carries out strip step, not limited.
The graphite scrap 22 will produce plural graphite in electrolyte 16 after tearing layer strip step open
Alkene fragment 30, the thickness of the Graphene fragment 30 is less than 5nm, and lateral dimensions (lateral size) is
Between 1 to 50 μm, after the Graphene fragment 30 by by the screen cloth 211 of the roller 21
Drop out outside the roller 21 and deposit or be suspended in the bottom of the electrolytic cell 10 or electrolyte, due to
Graphene fragment 30 is water insoluble, thus in solid suspended state plural Graphene fragment 30 then
Follow-up collection can be carried out and take out operation.
Wherein, the Graphene fragment 30 is Graphene or 2~5 layers of Graphene of individual layer or more two
Plant with the combination of arbitrary proportion；The major part of Graphene fragment 30 that the inventive method is produced is high-quality
The single-layer graphene of amount.
The output plural Graphene fragment 30 is peeled off being electrochemically reacted to tear layer open due to the present invention
When, the roller 21 is, in rotation status, the graphite scrap 22 and the electrolyte in it can be made at any time
16 are sufficiently mixed, can so make that second electrode 12 applies in the roller 21 (electrolytic cell 10) the
The Electric Field Distribution of one electrode 14 is uniform, promotes the insertion of graphite and strip step more efficiency,
Even property, and the electrolyte 16 will not be produced the temperature and concentration gradient of inequality simultaneously, and it is more conducive to
Electrochemistry tears the manufacture production Graphene fragment 30 of layer stripping method open.
Fig. 5 is referred to, is another embodiment of Graphene mass production equipment of the present invention, with Fig. 3 realities
It is that the second electrode 12 is tubulose, in the tubulose of the second electrode 12 to apply the different place of example
And having a hollow space 18, the drum apparatus 20 are disposed on the hollow space 18, so knot
Structure, enables to when the roller 21 is in rotation status, and the second electrode 12 puts on the roller
The Electric Field Distribution of first electrode 14 is more uniformly distributed in 21, and is more beneficial for electrochemistry and tears a layer stripping method open
Manufacture production Graphene fragment 30.
Fig. 6 is referred to, Graphene mass production equipment of the present invention is to have further included a collection apparatus
40, the collection apparatus 40 are the bottoms for being connected in the electrolytic cell 10；The collection apparatus 40 are to include
There are a pipeline 41 and collecting tank 42, the pipeline 41 is the electricity for being connected to the bottom of electrolytic cell 10
Solution groove outlet 212, the collecting tank 42 is to connect the pipeline 41, and the bottom of collecting tank 42 is provided with
One tool plural number penetrates the screened outlet 421 of pore, and the pore that penetrates of the screened outlet 421 is less than
The size of the Graphene fragment 30, its size can be in 200 × 200nm2(nanometer square) extremely
1200×1200nm2Between (nanometer square), preferably in 300 × 300nm2(nanometer square) extremely
800×800nm2Between (nanometer square).In this way, being deposited on the Graphene fragment of the bottom of electrolytic cell 10
30 will flow out the electrolyzer outlet 212 and enter the pipeline 41 with electrolyte 16, after by this
Pipeline 41 and enter the collecting tank 42 in, you can make the Graphene fragment 30 concentrate sieve stay in the receipts
In collection groove 42, taken out with convenient collection, and the electrolyte 16 in the collecting tank 42 is then by the sieve
Net outlet 421 is flowed out outside the collecting tank 42.
In appropriate implementation method, the pipeline 41 be can further include one first pipeline 43,
Second pipeline 44 and the 3rd pipeline 45, first pipeline 43 are to be connected to the electrolytic cell 10 and be somebody's turn to do
Between collecting tank 42, the sieving of tool plural number screen cloth mesh perforation is provided with first pipeline 43
Portion 431, the screen cloth mesh perforation of the screen section 431 is greater than Graphene fragment 30, and its size can
Between 18 to 1000 mesh (mesh), preferably between 35 to 300 mesh (mesh), make graphite
Alkene fragment 30 is able to be left by the screen section 431 and filter the impurity of other greater particle sizes；This second
Pipeline 44 is the screened outlet 421 for being connected to the collecting tank 42, is used to accept and flows out the collecting tank
42 electrolyte 16；Separately, a control flume 46, the control flume 46 is to be connected to second pipeline 44
Its with respect to the collecting tank 42 another end, the control flume 46 be detect, adjust control the electrolysis
Concentration, acid-base value, constituent of liquid 16 etc.；3rd pipeline 45 is to connect the control flume 46,
3rd pipeline 45 is that have one to go out geat 451, the electrolyte of the outflow control flume 46 is noted again
Enter in the electrolytic cell 10, reach the effect of the recycling of electrolyte 16；Furthermore, a supply tank 47,
The supply tank 47 is the interface 441 that the 3rd pipeline 45 is connected with the 4th pipeline 471, should
It is to be equipped with new electrolyte in supply tank 47, the new electrolyte is managed through the injection of the 4th pipeline 471 the 3rd
In road 45, it is used to supplement the electrolyte 16 being lost in processing procedure of the present invention.
Also referring to Fig. 7, based on foregoing equipment, processing procedure, Graphene mass production system of the present invention
The method of making is to include：(1) first electrode and a second electrode are set in the electrolyte of an electrolytic cell
In, the first electrode is a positive pole, and second electrode is a negative pole, and the first electrode is to be located at one
In roller with screen cloth, the screen cloth is provided with plural number and is more than the produced graphite after tearing layer strip step open
The perforation of alkene fragment 30, the electrolyte is to perforate to pass in and out roller S11 by the grade；(2) in the rolling
Cylinder is built into plural graphite scrap S12；(3) apply under one first bias, and make the roller in this
Rolled under one bias, the graphite scrap 22 is carried out ion insertion (intercalation) step
S13；(4) continue in rollers roll and apply one second bias, carry out the graphite scrap 22 tears layer stripping open
From (exfoliation) step S14；(5) the grade graphite scrap 22 forms at least one of which plural number Graphene
The step S15 of fragment 30；(6) the plural Graphene fragment 30 is deposited by the perforation of the roller screen cloth
In the bottom step S16 of the electrolytic cell；(7) the plural Graphene fragment 30 is somebody's turn to do as electrolyte flows out
Electrolytic cell is being collected the operating procedure S17 of taking-up；Will collect take out Graphene fragment 30 with
The step S18 that high temperature furnace or heating using microwave or spray dried form or freeze-drying are dried.
Graphene mass production equipment of the present invention and its manufacture method are designed by aforementioned structure, and it can be solved
Certainly existing Graphene electrochemistry tears a layer shortcoming for stripping method manufacture open, makes the exploitativeness with mass production,
And facilitate the collection of Graphene, take, and then reach the splendid economic benefit of Graphene manufacture production
Property, meanwhile, it can make Electric Field Distribution uniform using the circulation power-assisted of rollers roll, promote graphite
It is embedded in and tears layer strip step more efficiency, uniformity open, and electrolyte is not produced inequality
Temperature and concentration gradient, and more conducively electrochemistry tears the manufacture production Graphene of layer stripping method open.
The above embodiment is only exemplary, does not constitute any limitation to the scope of the present invention.Ability
Field technique personnel should be understood that without departing from the spirit and scope of the invention can be to the technology of the present invention
The details and form of scheme are modified or are replaced, but these modifications and replacement each fall within protection model of the invention
In enclosing.
Claims (14)
1. a kind of Graphene mass production equipment, it is characterised in that including：
One electrolytic cell, it is built-in with a first electrode, that electrolyte and leaching are located in the electrolyte
Two electrodes；
One drum apparatus, the plural graphite scrap for including a roller and being located in the roller, the rolling
Cylinder is that leaching is located in the electrolyte and is used to house the first electrode, and the roller is by an interlinked mechanism
Interlock and rotate, the screen cloth of plurality of through holes is provided with the barrel of the roller, the mesh of the screen cloth is worn
Hole is greater than Graphene fragment, and the electrolyte is to perforate to pass in and out the roller, the plural stone by the grade
Black fragment is that leaching is located in the electrolyte, be used to be embedded in, tear open layer stripping electrochemical step and
Output Graphene fragment.
2. Graphene mass production equipment as claimed in claim 1, it is characterised in that first electricity
An extremely positive pole, the second electrode is a negative pole.
3. Graphene mass production equipment as claimed in claim 1, it is characterised in that second electricity
It is tubulose that pole is, the tubulose of the second electrode is interior and has a hollow space, and the drum apparatus are to set
In the hollow space.
4. Graphene mass production equipment as claimed in claim 4, it is characterised in that the graphite is broken
Piece is：Native graphite (nature graphite), artificial synthesized graphite (synthetic graphite), graphited carbon
Black (carbon black), graphited furnace black (furnace black), the steady phase carbosphere (mesocarbon of Jie
Microbead writes a Chinese character in simplified form MCMB) or directionality graphite (highly oriented graphite sheet, write a Chinese character in simplified form
) or more HOGS several combinations with arbitrary proportion.
5. Graphene mass production equipment as claimed in claim 4, it is characterised in that the Graphene
Fragment is the Graphene or 2~5 layers of Graphene of individual layer or more two kinds of combinations with arbitrary proportion.
6. Graphene mass production equipment as claimed in claim 1, it is characterised in that further bag
A collection apparatus are included, the collection apparatus are the bottoms for being connected in the electrolytic cell.
7. Graphene mass production equipment as claimed in claim 6, it is characterised in that this collects dress
It is to include a pipeline and collecting tank to put, and the pipeline is the electric access slot for being connected to the bottom of electrolytic tank
Outlet, the collecting tank is to connect the pipeline, and the collection trench bottom is provided with a tool plural number and penetrates pore
Screened outlet, the pore that penetrates of the screened outlet is less than this and tears the Graphene fragment after layer open.
8. Graphene mass production equipment as claimed in claim 7, it is characterised in that the pipeline is
One first pipeline, the second pipeline and the 3rd pipeline are further included, first pipeline is to be connected to
Between the electrolytic cell and the collecting tank, tool plural number screen cloth mesh perforation is provided with first pipeline
Screen section, the screen section screen cloth mesh perforation be greater than the Graphene fragment.
9. Graphene mass production equipment as claimed in claim 8, it is characterised in that second pipe
Road is the screened outlet for being connected to the collecting tank；One control flume, the control flume be connected to this
Two pipelines with respect to the collecting tank another end, the control flume be detect, adjust control the electrolyte
Concentration, acid-base value, constituent.
10. Graphene mass production equipment as claimed in claim 8, it is characterised in that the 3rd pipe
Road is to connect the control flume, and the 3rd pipeline is that have one to go out geat, makes the electricity of the outflow control flume
Solution liquid reinjects the electrolytic cell.
11. Graphene mass production equipment as claimed in claim 10, it is characterised in that further
A supply tank is included, the supply tank is the interface that the 3rd pipeline is connected with one the 4th pipeline,
It is to be equipped with new electrolyte in the supply tank, the new electrolyte is injected in the 3rd pipeline through the 4th pipeline.
A kind of 12. Graphene mass production manufacture methods, it is characterised in that including：
Step 1：One first electrode and a second electrode are set in the electrolyte of an electrolytic cell, are somebody's turn to do
First electrode is a positive pole, and second electrode is a negative pole, and the first electrode is to be located at one to have sieve
In the roller of net, the roller has been built into plural graphite scrap, and the screen cloth is provided with plural number more than graphite
The perforation of alkene fragment, the electrolyte is to perforate to pass in and out the roller by the grade；
Step 2：Apply under one first bias, and the roller is rolled under first bias,
The graphite scrap is set to carry out ion insertion (intercalation) step；
Step 3：Continue in rollers roll and apply one second bias, carry out the graphite scrap tears layer open
Peel off (exfoliation) step；
Step 4：The grade graphite scrap forms at least one of which plural number Graphene fragment；
Step 5：The bottom that the plural Graphene fragment passes through the screen deposition of the roller electrolytic cell.
13. Graphene mass production manufacture methods as claimed in claim 12, it is characterised in that should
It is to continue to flow out the electrolytic cell to be received with electrolyte by the plural Graphene fragment after step 5
Collect the operation taken out.
14. Graphene mass production manufacture methods as claimed in claim 13, it is characterised in that will
The operation that the Graphene garbage collection takes out be with high temperature furnace or heating using microwave or spray dried form or
Freeze-drying is dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510955588.0A CN106904602B (en) | 2015-12-17 | 2015-12-17 | Graphene mass production equipment and its manufacturing method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109350045A (en) * | 2018-09-07 | 2019-02-19 | 东南大学 | A kind of manufacturing method of electrocardio flexible sensor |
| CN109704314A (en) * | 2019-02-28 | 2019-05-03 | 嘉兴学院 | A method of continuously preparing graphene |
| WO2020248462A1 (en) * | 2019-06-11 | 2020-12-17 | 中国科学院上海微系统与信息技术研究所 | Method for preparing high-quality graphene material |
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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 |
| CN203754427U (en) * | 2014-01-08 | 2014-08-06 | 奈创科技股份有限公司 | Graphene generating device |
| CN104609413A (en) * | 2015-02-11 | 2015-05-13 | 合肥微晶材料科技有限公司 | Machine-like stripping device for ton-scale production of graphene and production method of machine-like stripping device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN203754427U (en) * | 2014-01-08 | 2014-08-06 | 奈创科技股份有限公司 | Graphene generating device |
| CN104609413A (en) * | 2015-02-11 | 2015-05-13 | 合肥微晶材料科技有限公司 | Machine-like stripping device for ton-scale production of graphene and production method of machine-like stripping device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109350045A (en) * | 2018-09-07 | 2019-02-19 | 东南大学 | A kind of manufacturing method of electrocardio flexible sensor |
| CN109350045B (en) * | 2018-09-07 | 2022-02-11 | 东南大学 | Manufacturing method of electrocardio flexible sensor |
| CN109704314A (en) * | 2019-02-28 | 2019-05-03 | 嘉兴学院 | A method of continuously preparing graphene |
| WO2020248462A1 (en) * | 2019-06-11 | 2020-12-17 | 中国科学院上海微系统与信息技术研究所 | Method for preparing high-quality graphene material |
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