CN107117604B - A kind of method for preparing graphene using electrostatic accelerating medium stream stripping - Google Patents
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 199
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 51
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 92
- 239000010439 graphite Substances 0.000 claims abstract description 92
- 239000002002 slurry Substances 0.000 claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002360 preparation method Methods 0.000 claims abstract description 19
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 18
- 238000013019 agitation Methods 0.000 claims abstract description 14
- 239000007770 graphite material Substances 0.000 claims abstract description 11
- 239000011229 interlayer Substances 0.000 claims abstract description 11
- 230000009881 electrostatic interaction Effects 0.000 claims abstract description 10
- 238000004220 aggregation Methods 0.000 claims abstract description 5
- 230000002776 aggregation Effects 0.000 claims abstract description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 22
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 11
- 238000000889 atomisation Methods 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 2
- 239000003595 mist Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 235000002639 sodium chloride Nutrition 0.000 claims description 2
- 239000001509 sodium citrate Substances 0.000 claims description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims 1
- -1 graphite alkene Chemical class 0.000 claims 1
- 229910001415 sodium ion Inorganic materials 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 10
- 238000002604 ultrasonography Methods 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002356 single layer Substances 0.000 abstract description 4
- 239000007921 spray Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 24
- 230000000694 effects Effects 0.000 description 6
- 239000012141 concentrate Substances 0.000 description 5
- 239000000725 suspension Substances 0.000 description 5
- 150000001721 carbon Chemical group 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 238000009830 intercalation Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
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- 230000006641 stabilisation Effects 0.000 description 1
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- 239000010959 steel Substances 0.000 description 1
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- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- 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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The invention belongs to grapheme material fabricating technology field, and in particular to a kind of method for preparing graphene using electrostatic accelerating medium stream stripping.Laminated crystalline graphite material, sodium salt, water are mixed into graphite slurry in the presence of mechanical agitation adds ultrasound;By graphite slurry by setting the high-pressure fog mouth of sophisticated corona unit to spray, form small misty liquid droplets, vaporific slurry particles are by corona simultaneously, negative electrical charge rapid aggregation is on graphite particulate surface, small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, the interlayer spacings that electrostatic repulsion between electric charge exceedes graphite particulate further increase, and turn into expansible graphite particle and powered;It is graphene further to accelerate to peel off by graphite using the medium flow field that electrostatic accelerator accelerates.The present invention avoids oxidation processes, is peeled off graphite into single-layer graphene with high yield, and compared with other graphenes preparation technology, the single-layer graphene defect of this method production is less, electric property, mechanical property are higher.
Description
Technical field
The invention belongs to grapheme material fabricating technology field, and in particular to one kind is shelled using electrostatic accelerating medium stream
From the method for preparing graphene.
Background technology
Carbon material be material more universal and special on a kind of earth it can form the larger diamond of hardness, can also
Softer graphite is formed, in the past 20 years, carbon nanomaterial is always the Disciplinary Frontiers of scientific and technical innovation, the fullerene found in 1985
Huge repercussion is caused with the CNT found in 1991, has risen research boom, Manchester universities in 2004
Geim groups New Two Dimensional atomic crystal-graphene of individual layer or thin layer is obtained with mechanical stripping method first.Graphene
It was found that having enriched carbon material family, the fullerene from zero dimension, one-dimensional CNTs, the Buddha's warrior attendant of two-dimentional graphene to three-dimensional are formd
The integral framework of stone and graphite.
Graphene is the individual layer two-dimension plane structure by regular hexagon close-packed arrays into honeycomb crystal lattice by carbon atom.Graphite
Alkene structure is highly stable, and the connection between each carbon atom is very flexible, and when applying external mechanical force, carbon atom face just bends change
Shape so that carbon atom need not be rearranged to adapt to external force and holding structure it is stable.The lattice structure of this stabilization makes carbon former
Son has outstanding thermal conductivity 3000W/ (m*K).The maximum characteristic of graphene is that the movement velocity of its electronics has reached the light velocity
1/300, it is that to be currently known electronics conduction velocity in material most fast considerably beyond movement velocity of the electronics in general conductor
, its electron mobility at room temperature is up to 15000cm2/ (V* s).Graphene also shows perfect quantum tunneling effect
Should, the half-integer quantum hall effect of the dirac fermion behavior of zero mass and exception.Graphene or mankind's known strength
Highest material, also harder than diamond, intensity is more than 100 times of steel best in the world.In addition, single-layer graphene have it is non-
Often big specific surface area, up to 2600m2/g.Graphene possesses that translucency is good, thermal conductivity factor is high, electron mobility is high, resistance
The performance that numerous common materials such as rate is low, mechanical strength is high do not possess, future be expected to electrode, battery, transistor, touch-screen,
The various fields extensive use such as solar energy, sensor, super light material, medical treatment, desalinization, be most promising advanced material it
One.
The preparation method of graphene mainly includes micromechanics stripping method, electronation graphene oxide method, CNT
Axially cutting method, electrochemical reducing, chemical vapour deposition technique, microwave method, solvent-thermal method, arc discharge method, epitaxial growth method,
Liquid phase peels off graphite method etc..Wherein chemical vapour deposition technique can obtain the graphene of high quality, but low yield, will to substrate
Ask high, transfer exists greatly difficult;Electronation graphene oxide method can realize batch production graphene, but due to
The structure of graphene is destroyed in oxidizing process, it is difficult to obtains the graphene product of high quality;Liquid phase stripping method is suitable
Solvent in, graphite flake layer is dissociated using ultrasonic energy, however, solvent stripping method prepare graphene exist be difficult to remove
The problem of residual solvent, and solvent peels off yield and is generally less than 10%.This means 90% raw material (graphite) is not shelled yet
From, and only 10% or less raw material is reclaimed with graphene platelet, each includes one or more layers graphene.These are low
The problem of yield process is the multiple steps of their needs and is used to be processed further to produce enough products, and including will not
Tediously long multiple steps that release liner and release liner separate.Mechanical stripping method is that one kind can prepare high quality with low cost
The simple and easy method of graphene, but usually introduce organic solvent in order to improve peeling effect during mechanical stripping and insert
Layer, though intercalation efficiency and control distribution of particles can be improved to a certain extent, the solvent residues in graphene are not easy
Remove, easily cause contamination of products.And existing machinery charge stripping efficiency is low;In addition, the crunch of abrasive media can cause graphite
Rotating fields become even closer can cause peeling effect to reduce on the contrary, cause milling time length, cost very high;Furthermore mesh
Preceding grinding production graphene belongs to batch (-type), and while being peeled off to graphite, the graphene peeled off can not be sieved in time
Select, thus be difficult to the volume production of continuous-stable, it is difficult to carry out large-scale industrialized production.
The content of the invention
The present invention proposes a kind of method for preparing graphene using electrostatic accelerating medium stream stripping, avoids oxidation-treated
Journey, graphite is peeled off into single-layer graphene with high yield.Compared with other graphenes preparation technology, this method passes through spray points electricity
Dizzy processing makes graphite powered, the ionized gas for triggering generation powered is further conveyed using electrostatic accelerator, as medium flow field
It is graphene that graphite, which is peeled off,.
To achieve the above object, adopt the following technical scheme that:
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, by laminated crystalline graphite material, sodium salt, water
Graphite slurry is mixed into the presence of mechanical agitation plus ultrasound;High pressure spray by graphite slurry by the sophisticated corona unit of setting
Mist mouth sprays, and forms small misty liquid droplets, while vaporific slurry particles, by corona, negative electrical charge rapid aggregation is in graphite particulate table
Face, small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, and it is micro- that the electrostatic repulsion between electric charge exceedes graphite
The interlayer spacings of grain further increase, and turn into expansible graphite particle and powered;Jie further accelerated using electrostatic accelerator
It is graphene that graphite is accelerated to peel off by mass flow.
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its specific preparation method are:
(1)Prepare graphite slurry
By the dissolving of sodium salt mechanical agitation in deionized water, laminated crystalline graphite material is added, opens Vltrasonic device, ultrasound
Time is 0.5 ~ 6 hour;Layered kish material is in terms of carbon, and for sodium salt to receive ionometer, the mol ratio of the two is 1:
0.05~0.5;
(2)Peel off graphene
Sprayer unit is opened, atomisation pressure is 2 ~ 6MPa, and corona unit is powered, voltage is arranged to 5 ~ 10kv, opens charging
Device is by step(1)The high-pressure fog at the needle point mouth of corona unit of the graphite slurry of preparation, forms small misty liquid droplets, simultaneously
Vaporific slurry particles are by corona, and for negative electrical charge rapid aggregation on graphite particulate surface, small misty liquid droplets are final under electrostatic interaction
It is split into single graphite particle, the interlayer spacings that the electrostatic repulsion between electric charge exceedes graphite particulate further increase, and turning into can be swollen
Swollen graphite particle;It is graphene further to accelerate to peel off by graphite using the medium flow field that electrostatic accelerator accelerates, electron energy control
System is in 0.5 ~ 0.9M eV;
(3)Separation, the washing of graphene
By step(2)The graphene mixture of preparation is separated, and solvent input is continuing with for the first time, then uses deionization
Water cleans 3 ~ 6 times, and acquisition is scattered in graphene.
The yield of test analysis, individual layer and few layer graphene is 81 ~ 97%, and graphene lateral dimension is 20 ~ 300nm.
Layered kish material includes one kind in native graphite, synthetic graphite, highly oriented pyrolytic graphite, particle
Size is less than 10 μm.
The sodium salt is in sodium acid carbonate, sodium carbonate, sodium fluoride, sodium nitrate, sodium chloride, sodium tert-butoxide, sodium citrate
At least one.
The electrostatic accelerator is 0.6MeV electron electrostatic accelerators, and the medium flow field is accelerated electronics.
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its mechanism are:Laminated crystalline graphite material
Under sodium salt environment, charge density is higher, and under electrostatic repulsion effect, carbon-coating (or being graphite interlayer) layer gap is necessarily expanded
Greatly, in the presence of ultrasound, the less cation of radius, anion diffuse into carbon-coating (or being graphite interlayer) layer gap, this
Both samples interact, and the graphene layer gap spacing for being is increased to more than 0.6nm from 0.335nm, and Van der Waals force weakens, but logical
The electrostatic interaction crossed in ion insertion and solution only allows graphite material to be expanded.Slurry is dispersed into by high-pressure fog small
Particle, under the sophisticated corona unit corona at needle point mouth, the increase of fine particles surface charge accumulation, fine particle is further
More fine particle is divided into, surface is ultimately become and carries High Density Charge, the expansion stone of a large amount of intercalating ions is contained inside layer gap
Black particle, but it is unstripped into graphene.Next electrostatic accelerating medium stream effect under, expanded graphite particles be decomposed into individual layer or
Few layer graphene.Experiment shows, in general, and Electron energy control is in 0.5 ~ 0.9MeV, and too low peeling effect is undesirable, too high meeting
Graphene is caused to produce a large amount of defects.
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping of the present invention, it is compared with prior art, described
Based on the electrostatic repulsion method that continuously stripping prepares graphene, its advantage is:
1st, this process do not suffer from aoxidize route in the case of by graphite directly using needle-tip corona, electrostatic accelerating medium
Stream stripping prepares graphene.
2nd, this method equipment is simple, easily controllable, can scale, stable stripping graphene.
3rd, compared with oxide graphene, this method production graphene platelet the defects of it is controllable, electric conductivity is higher.
Brief description of the drawings
Further to explicitly use the method that electrostatic accelerating medium stream stripping prepares graphene, illustrated by accompanying drawing.
Fig. 1:A kind of process flow diagram for the method that graphene is prepared using electrostatic accelerating medium stream stripping.
Embodiment
Below by way of embodiment, the present invention is described in further detail, but this should not be interpreted as to the present invention
Scope be only limitted to following example.In the case where not departing from above method thought of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its detailed process flow are:It is first existing by sodium
Salt mechanical agitation dissolves in deionized water, adds laminated crystalline graphite material, mechanical agitation, after ultrasonic certain time, carbon dust
Even suspension forms graphite slurry in the solution;Sprayer unit and feeding device is opened again to fill the graphite slurry of preparation in corona
High-pressure fog above placing electrodes, forms small misty liquid droplets, while vaporific slurry particles are fast by corona, negative electrical charge in needle point mouth
Speed is gathered in graphite particulate surface, and small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, between electric charge
The interlayer spacings that electrostatic repulsion exceedes graphite particulate further increase, and turn into expansible graphite particle.Further added using electrostatic
It is graphene that the medium flow field that fast device accelerates, which peels off graphite,;Finally, the graphene mixture of preparation is separated, solvent input
It is continuing with, then is cleaned with deionized water for the first time, obtains the graphene being dispersed in water.
Wherein, the graphite slurry laminate kish material is in terms of carbon, layered kish material in terms of carbon,
For sodium salt to receive ionometer, the mol ratio of the two is 1:0.05;
Wherein, the graphite slurry ultrasound plus churned mechanically time are 0.5 hour;
Wherein, the sprayer unit, its atomisation pressure are 2MPa, and the corona unit leads to, and its operating voltage is arranged to
5kv;
Wherein, the electrostatic accelerator, its Electron energy control is in 0.5MeV;
Wherein, it is 81%% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 20nm.
Embodiment 2
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its detailed process flow such as Fig. 1:First now will
Sodium salt mechanical agitation dissolves in deionized water, adds laminated crystalline graphite material, mechanical agitation, after ultrasonic certain time, carbon
Powder even suspension forms graphite slurry in the solution;Sprayer unit and feeding device are opened again by the graphite slurry of preparation in corona
High-pressure fog above device discharge electrode, forms small misty liquid droplets, while vaporific slurry particles are by corona, negative electrical charge in needle point mouth
For rapid aggregation on graphite particulate surface, small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, between electric charge
Electrostatic repulsion exceed graphite particulate interlayer spacings further increase, turn into expansible graphite particle.Further utilize electrostatic
It is graphene that the medium flow field that accelerator accelerates, which peels off graphite,;Finally, the graphene mixture of preparation is separated, solvent is thrown
Enter and be continuing with for the first time, then cleaned with deionized water, obtain the graphene being dispersed in water.
Wherein, the graphite slurry laminate kish material is in terms of carbon, layered kish material in terms of carbon,
For sodium salt to receive ionometer, the mol ratio of the two is 1:0.3;
Wherein, the graphite slurry ultrasound plus churned mechanically time are 6 hours;
Wherein, the sprayer unit, its atomisation pressure are 4MPa, and the corona unit leads to, and its operating voltage is arranged to
10kv;
Wherein, the electrostatic accelerator, its Electron energy control is in 0.7MeV;
Wherein, it is 89%% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 300nm.
Embodiment 3
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its detailed process flow are:It is first existing by sodium
Salt mechanical agitation dissolves in deionized water, adds laminated crystalline graphite material, mechanical agitation, after ultrasonic certain time, carbon dust
Even suspension forms graphite slurry in the solution;Sprayer unit and feeding device is opened again to fill the graphite slurry of preparation in corona
High-pressure fog above placing electrodes, forms small misty liquid droplets, while vaporific slurry particles are fast by corona, negative electrical charge in needle point mouth
Speed is gathered in graphite particulate surface, and small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, between electric charge
The interlayer spacings that electrostatic repulsion exceedes graphite particulate further increase, and turn into expansible graphite particle.Further added using electrostatic
It is graphene that the medium flow field that fast device accelerates, which peels off graphite,;Finally, the graphene mixture of preparation is separated, solvent input
It is continuing with, then is cleaned with deionized water for the first time, obtains the graphene being dispersed in water.
Wherein, the graphite slurry laminate kish material is in terms of carbon, layered kish material in terms of carbon,
For sodium salt to receive ionometer, the mol ratio of the two is 1:0.5,;
Wherein, the graphite slurry ultrasound plus churned mechanically time are 2 hours;
Wherein, the sprayer unit, its atomisation pressure are 6MPa, and the corona unit leads to, and its operating voltage is arranged to
8kv;
Wherein, the electrostatic accelerator, its Electron energy control is in 0.9MeV;
Wherein, it is 83%% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 100nm.
Embodiment 4
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its detailed process flow are:It is first existing by sodium
Salt mechanical agitation dissolves in deionized water, adds laminated crystalline graphite material, mechanical agitation, after ultrasonic certain time, carbon dust
Even suspension forms graphite slurry in the solution;Sprayer unit and feeding device is opened again to fill the graphite slurry of preparation in corona
High-pressure fog above placing electrodes, forms small misty liquid droplets, while vaporific slurry particles are fast by corona, negative electrical charge in needle point mouth
Speed is gathered in graphite particulate surface, and small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, between electric charge
The interlayer spacings that electrostatic repulsion exceedes graphite particulate further increase, and turn into expansible graphite particle.Further added using electrostatic
It is graphene that the medium flow field that fast device accelerates, which peels off graphite,;Finally, the graphene mixture of preparation is separated, solvent input
It is continuing with, then is cleaned with deionized water for the first time, obtains the graphene being dispersed in water.
Wherein, the graphite slurry laminate kish material is in terms of carbon, layered kish material in terms of carbon,
For sodium salt to receive ionometer, the mol ratio of the two is 1:0.35;
Wherein, the graphite slurry ultrasound plus churned mechanically time are 1 hour;
Wherein, the sprayer unit, its atomisation pressure are 2MPa, and the corona unit leads to, and its operating voltage is arranged to
6kv;
Wherein, the electrostatic accelerator, its Electron energy control is in 0.8M eV;
Wherein, it is 94%% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 120nm.
Embodiment 5
A kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its detailed process flow are:It is first existing by sodium
Salt mechanical agitation dissolves in deionized water, adds laminated crystalline graphite material, mechanical agitation, after ultrasonic certain time, carbon dust
Even suspension forms graphite slurry in the solution;Sprayer unit and feeding device is opened again to fill the graphite slurry of preparation in corona
High-pressure fog above placing electrodes, forms small misty liquid droplets, while vaporific slurry particles are fast by corona, negative electrical charge in needle point mouth
Speed is gathered in graphite particulate surface, and small misty liquid droplets are finally split into single graphite particle under electrostatic interaction, between electric charge
The interlayer spacings that electrostatic repulsion exceedes graphite particulate further increase, and turn into expansible graphite particle.Further added using electrostatic
It is graphene that the medium flow field that fast device accelerates, which peels off graphite,;Finally, the graphene mixture of preparation is separated, solvent input
It is continuing with, then is cleaned with deionized water for the first time, obtains the graphene being dispersed in water.
Wherein, the graphite slurry laminate kish material is in terms of carbon, layered kish material in terms of carbon,
For sodium salt to receive ionometer, the mol ratio of the two is 1:0.35;
Wherein, the graphite slurry ultrasound plus churned mechanically time are 2 hours;
Wherein, the sprayer unit, its atomisation pressure are 4MPa, and the corona unit leads to, and its operating voltage is arranged to
8kv;
Wherein, the electrostatic accelerator, its Electron energy control is in 0.8MeV;
Wherein, it is 97%% to prepare the individual layer of gained and the output capacity of few layer graphene, and lateral dimension concentrates on 160nm.
Claims (4)
1. a kind of method for preparing graphene using electrostatic accelerating medium stream stripping, its specific preparation method are:
(1)Prepare graphite slurry
By the dissolving of sodium salt mechanical agitation in deionized water, laminated crystalline graphite material is added, opens Vltrasonic device, ultrasonic time
For 0.5~6 hour;Layered kish material is in terms of carbon, and for sodium salt in terms of sodium ion, the mol ratio of the two is 1:0.05~
0.5;
(2)Peel off graphene
Sprayer unit is opened, atomisation pressure is 2~6MPa, and corona unit is powered, voltage is arranged to 5~10kv, opens charging dress
Put step(1)The high-pressure fog at the needle point mouth of corona unit of the graphite slurry of preparation, forms small misty liquid droplets, while mist
Shape slurry particles are finally divided by corona, negative electrical charge rapid aggregation in graphite particulate surface, small misty liquid droplets under electrostatic interaction
Split for single graphite particle, the interlayer spacings that the electrostatic repulsion between electric charge exceedes graphite particulate further increase, and turn into inflatable
Graphite particle;It is graphene further to accelerate to peel off by graphite using the medium flow field that electrostatic accelerator accelerates, Electron energy control
In 0.5~0.9MeV;
(3)Separation, the washing of graphene
By step(2)The graphene mixture of preparation is separated, and solvent input is continuing with for the first time, then clear with deionized water
Wash 3~6 times, obtain dispersed graphite alkene.
A kind of 2. method for preparing graphene using electrostatic accelerating medium stream stripping according to claim 1, it is characterised in that:
Layered kish material includes one kind in native graphite, synthetic graphite, highly oriented pyrolytic graphite, and particle size is less than
10μm。
A kind of 3. method for preparing graphene using electrostatic accelerating medium stream stripping according to claim 1, it is characterised in that:
The sodium salt in sodium acid carbonate, sodium carbonate, sodium fluoride, sodium nitrate, sodium chloride, sodium tert-butoxide, sodium citrate at least one
Kind.
A kind of 4. method for preparing graphene using electrostatic accelerating medium stream stripping according to claim 1, it is characterised in that:
The electrostatic accelerator is 0.6MeV electron electrostatic accelerators, and the medium flow field is accelerated electronics.
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