CN110078061A - A kind of preparation method and equipment of graphene powder - Google Patents
A kind of preparation method and equipment of graphene powder Download PDFInfo
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- CN110078061A CN110078061A CN201810074288.5A CN201810074288A CN110078061A CN 110078061 A CN110078061 A CN 110078061A CN 201810074288 A CN201810074288 A CN 201810074288A CN 110078061 A CN110078061 A CN 110078061A
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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
- C01B2204/04—Specific amount of layers or specific thickness
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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
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
Abstract
The present invention provides the production equipments used needed for a kind of preparation method of graphene and this preparation method.Based on the high-speed jet of using gas of the present invention or liquid, using the principle of jet stream, in the intracavitary cutting graphite raw material of device provided by the invention, to obtain forming graphene powder by graphite fine particles.It during the present invention produces graphene powder, is not polluted by other substances, speed of production is fast, can high-speed production purity is high, high-quality graphene powder.
Description
Technical field
The present invention relates to the method for the mass production graphene powder from graphite raw material, the production graphite that especially relates to
The method of the device and production graphene powder of alkene powder.
Background technique
In recent years, it is become more and more active in China in relation to the research of graphene, so that the production technology of graphene has obtained greatly
Development.Existing known graphene production method includes: supercritical methanol technology, ultrasonic stripping method, oxidation-reduction method, plasma stripping
Method, a kind of catalytic chemical vapor deposition technique, chemical vapour deposition technique, plasma method, epitaxy etc.；
In supercritical process, graphite is added in the supercritical solution of ethyl alcohol, by making the solvent point in supercritical solution
Son between each layer and from removing graphene thereon, but this method the problem is that due to supercritical solution in high temperature and
Processing under high pressure and there is big difference, and be difficult to a large amount of material of single treatment；
In ultrasonic stripping method, graphite is added in the solution, applies ultrasonic wave, to make graphene vibration removing, but this method
There is a problem of that stripping process is time-consuming, it could be also difficult to handle a large amount of material simultaneously；In oxidation-reduction method, graphite is by salt
Acid or sulfuric acid oxidation, to make graphite become thin slice, but this method has a problem that, i.e., graphene is necessarily oxidized, then
It is electrolysed or is restored with chemical reagent, still, since the complete reduction of graphene is difficult, cause the quality of graphene very low；?
In plasma stripping method, graphite is placed in a furnace, and is removed with plasma discharge, but this method there is due to
Plasma and the problem of form many holes on the surface of graphene；In alcohol catalytic chemical vapor deposition technique, ethyl alcohol and metal are urged
Agent is placed on a vacuum drying oven, and ethyl alcohol is decomposed by 1000 °C of heating furnace, to provide the crystal of graphene, but the party
Equipment used in method can very illegal huge problem, be difficult to immediately treat a large amount of material；In thermal chemical vapor deposition method,
Methane gas is introduced in vacuum drying oven, and gas is heated to 1000 °C and decomposes and form film on metallic matrix, but this
There is graphenes to obtain good crystalline problem for method；In plasma method, methane gas is introduced into vacuum drying oven,
With plasma decomposed gases, form film on metallic substrates, this method the problem is that, although treatment temperature is low,
But the crystallinity of graphene is poor, and needs to melt the substrate for taking out graphene.
Method described above is all difficult to that graphene can not be mass produced with a large amount of material of high speed processing；Can not yet
Produce high-purity pure graphene free from foreign meter.And the present invention can solve these problems, it is therefore an objective to which provide this can give birth in batches
The process units of the high-quality graphene powder of production, to produce a kind of high-purity pure graphene free from foreign meter.
Summary of the invention
The present invention is in view of the deficienciess of the prior art, provide a kind of side that can be mass high-quality graphene powder
Method and its device.
The method that the present invention produces graphene powder, the method including a kind of gas jet cracking graphite raw material；Gas packet
It containing air and other gases, is pressurizeed by gas compressor, forms ultrahigh speed gas jet, crack graphite raw material.This method
Process will not contact other impurities, so not will receive other substances pollution；Its speed of production is also very fast, can high fast-growing
Produce purity is high, high-quality graphene powder.Cracking described here is a kind of crystalline fracture parallel with specific plane, this
Mode has the attribute for being easily broken off crystal；This is because interatomic binding force is weak and the phenomenon that generate, when atom, ion or point
It when binding force between son is weaker than the cracking strength perpendicular to parallel surface, will be broken, graphene equally has from model moral
Binding force between the atom of wals force, lewis' acid, thus easily cause division.Fine grained of the present invention is finger-type
At very thin powder, not only include it is spherical, further include as slender lobule as sheet, this laminar graphene powder,
With biggish surface area, the contact area with other materials also can be larger, and electric conductivity and dispersibility can be improved in this way, this
It is a very novel technical point.
The method of another production graphene powder of the invention, the side including a kind of liquid jet cracking graphite raw material
Method, liquid include water and other solvents, are pressurizeed by force (forcing) pump, and ultrahigh speed liquid jet is formed, and crack graphite raw material.Black alkene powder
End can be obtained by the liquid after dry cracking；Separately in the case where liquid is used as useful solvent, liquid can not be dried,
The solvent containing graphene powder can be produced, is conducive to produce graphite alkene powder-product.
Method of another of the invention production graphene powder, by spraying the jet stream containing graphite raw material, make containing
The jet stream of graphite raw material is ejected into closed chamber, is collided with chamber wall and is cracked and to form tiny graphene powder.
The method of another production graphene powder of the invention, is the jet stream by least two opposite directions while flowing
Enter in device chamber, include graphite raw material in the jet stream in wherein at least one direction, graphite raw material can be because of two opposite directions
Jet stream collide and generate cracking process.
Method of another of the invention production graphene powder, is hydraulically full in the chamber device, then containing
The jet stream of graphite raw material flows into it, a cavitation effect is created, to crack graphite raw material；Cavitation effect referred herein refers to
Generate the physical phenomenon of bubble and bubble explosion, also referred to as cavitation in a short time due to the pressure difference in liquid flowing；Pressure difference
It is to be generated by jet stream influent, to generate the graphite that cracking strength is rived.
The present invention also provides the method for a kind of pair of graphene powder processing, processing method including atmospheric plasma,
Ultraviolet and ozone processing and vacuum plasma treatment method；This is a kind of modification to be carried out to graphene powder, including incite somebody to action
Dispersibility, conductivity, thermal conductivity, insulation performance, heat-radiating properties etc. assign graphene powder, it is therefore an objective to improve graphene powder
Quality.
The effluxvelocity that the present invention uses is within the scope of 100 ~ 1000 m/s；Using the diameter of jet nozzle in 0.1 ~ 1mm
In range, jet pressure is provided within the scope of 10 ~ 500 MPa, and graphene powder is made of 70% or more graphene, is cut
The length of face is 3 ~ 10000 times of thickness；About 300 layers.
Equipment of the invention includes: the raw material input device of graphite, exports the output device of jet stream, the production of enclosure space
Chamber and the output device for exporting graphene powder.Equipment of the invention includes according to characteristic described above, input unit
The first input unit of raw material and the second input unit of jet stream input unit are inputted, and controls them and enters production chamber
The pipeline in direction.According to the method for the present invention, jet stream can be gas and be also possible to liquid, so jet stream input, which is set, can use pressure
Contracting machine, pump etc. pressurize, to form ultrahigh speed jet stream.It can be the container of a sealing in the chamber of present device,
It the inside can be with gassy or liquid.
For equipment of the invention there are one processing structure, this processing structure is subjected to the graphene powder exported from chamber
Atmospheric plasma treatment, ultraviolet and ozone processing and vacuum plasma treatment, this structure is mainly to Graphene powder
Last modification, to improve the quality of graphene powder, modification includes: the dispersibility that can be taught, electric conductivity, thermally conductive
Property, insulating properties, thermal diffusivity etc..
Because being related to the jet stream of jet stream output unit output liquid, equipment of the invention also has equipment of the invention
The dry drying structure containing Graphene powder liquid, it is dry for the liquid containing graphene powder；According to the characteristic, can produce
The raw graphene powder for being free of liquid；In addition, liquid can not be dried, can be in the case where liquid is as having as solvent
The solvent containing graphene powder is produced, is conducive to produce graphite alkene powder-product.
Equipment of the invention also includes a loop structure, so that the graphene powder of output is again inputted into the chamber of equipment
Room is repeatedly cracked, to generate finer graphene powder.
The speed of equipment production graphene powder of the invention, at least 1 kg/hour or higher, because of the invention
The process that equipment produces graphite powder is mainly to obtain graphene powder by cracking graphite with jet stream, so as to improve processing
Ability.
Graphene powder produced by the invention can be used for electronic component, circuit, electronic apparatus, home electric element, automobile
In the products such as component, machine part, electrical component, pottery or native stone manufacture, paper pulp, paper；Processing paper or wood can also be used in
Product, chemical products, petroleum or coal product, plastic products and rubber product etc.；It may be also used in transparent or opaque electrode, touching
Touch screen, resistance, capacitor, transformer or composite parts, to the electrode material of double layer capacitor, rechargeable battery, be level-one or
The electrode material of secondary battery, for the electrode material of lithium ion battery, generator, motor, electric rotary machine, for being catalyzed
Fuel cell substrate, the electromechanical component of agent, dye-sensitized solar cells, flexible base board and electronic tag, sensor or biography
Sensor cell etc.；Cement, fresh concrete, concrete product, electroceramics product, laboratory or industry pottery can also be equally used in
Porcelain products, carbon electrode, carbon or graphite product, artificial bone, plastering, plastics, synthetic rubber, paint, ink, printed electronic member
Part, gelatin or adhesive, oil, lubricating oil or lubricating grease, pipeline, construction material, food package film.A kind of medical film, kitchen
Product, toy, information processing equipment chassis, household electric appliances, PET beverage bottle, mechanical part, industry adhesive, heat radiation
Lubricating grease, packaging material, engineering plastics.Furniture, tire, medical grade rubber, heat resisting gasket, vibration-proof rubber, rubber product etc..
Detailed description of the invention
Fig. 1: being a kind of structural schematic diagram using gas jet production graphene powder equipment of the present invention；
Fig. 2: figure (a) is the schematic diagram that gas jet cracks graphite raw material with (b) is schemed；
Fig. 3: being another structural schematic diagram using gas jet production graphene powder equipment of the present invention；
Fig. 4: being a kind of structural schematic diagram using liquid jet production graphene powder equipment of the present invention；
Fig. 5: figure (a) is the schematic diagram that liquid jet cracks graphite raw material with (b) is schemed；
Fig. 6: being another structural schematic diagram using liquid jet production graphene powder equipment of the present invention；
Fig. 7: figure (a) is the schematic diagram that liquid jet cracks graphite raw material with (b) is schemed；
Fig. 8: being a kind of empty structural schematic diagram using cavitation effect production graphene powder equipment of the present invention；
Fig. 9: figure (a) is the schematic diagram that graphite raw material cracks under cavitation effect with (b) is schemed；
Figure 10: it is shown that observing the obtained image of graphene powder with scanning electron microscope (SEM).；
Figure 11: the attribute schematic diagram of fine grained graphite alkene is shown in figure (a)；Scheme (b) and flake graphite alkene powder attribute is shown
Schematic diagram；
Figure 12: graphite raw material three-dimensional is cracked into fine grained by the equipment utilization cracking principle that figure (a) is shown through the invention
Schematic diagram, figure (b) be shown through the invention equipment utilization dimension cracking principle by graphite raw material two dimension crack slabbing
The schematic diagram of graphene.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited by the specific embodiments disclosed below.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.
Below will enumerate specific embodiment description the present invention production graphene powder method and apparatus, Fig. 1,3,4,6,
8 be five examples of description production graphene powder equipment production graphene and the process units of graphene powder；Fig. 1
With the example for being using gas shown by Fig. 3 as injection stream production graphene powder；It is shown by Fig. 4, Fig. 6 and Fig. 8
Use liquid as the example of injection stream production graphene powder.
The present invention produces the embodiment of graphene as shown in Figure 1, Fig. 1 is that high-speed gas jet is used to produce as injection stream
1 schematic diagram of apparatus of graphene powder, equipment has a head tank 2 and 3, for storing and inputting graphene raw material, example
Such as natural graphite, graphite powder.Raw material by pipeline 8 enter input unit 10e enter back into be input to production chamber 5 work as
In.There are one the structure compresses machines 4 as jet stream output for equipment, form high-speed gas jet for compressed gas and continue defeated
Send the device of gas jet, compression be can be with air either other gases, such as nitrogen, hydrocarbon gas, hydrogen
Deng, the jet stream discharge pressure of compressor 4 may be provided between about 10 ~ 500MPa, nozzle diameter may be set in 0.1 ~ 1mm,
It thus can control between about 100 ~ 1000 m/s of speed of jet stream, output gas jet stream is by pipeline 9, into production chamber
Room 5.Making chamber 5 is an enclosure space spherical in shape, completes cracking using ultrahigh speed gas jet in production chamber
Graphene raw material；The production chamber 5 can also block air with valve not shown in the figure, and inner atmosphere is maintained at Gao Zhen
Dummy status, jet stream of gas and raw material are input into make-up room 5 together, carry out the process of cracking graphite；Gas jet is in 9a
It is directly injected in production chamber to 9d, they can collide and crack graphite raw material 3, can also make graphite cracking not
Finished goods is collided together with the inner wall of make-up room 5 and gas jet again, is that can cause more than two times to graphite raw material in this way
Or it cracks more times；The input structure 10 that production chamber 5 shown in FIG. 1 is linked to is to input ultrahigh speed jet stream by pipeline 9
Gas jet, they have the first input channel 10a, the second input channel 10b, third input pipe for inputting gas jet
Road 10c, the 4th pipeline configuration 10d and the 5th input channel 10e, the first to the 5th input structure 10a to 10e are made of nozzle；
Figure, which is shown, has the case where there are five input structure 10, and equipment can also provide six or multiple input channels.Input structure 10
With control structure, for this control structure not shown in the figure, this control structure is to can control the input of 10a to 10e
Direction, that is, control the input direction of gas jet 9a to 9e, thus can arbitrarily control raw material input structure and
The direction of gas input jet makes them can be with multiple impacts, and control structure is not necessary component so equipment drawing does not show
Out.An equipment also deduster structure 6a makes product matter for collecting the dust of the graphene powder come out from make-up room 5
Amount is more preferable, and the technology of deduster 6a application, can also be with including the use of the gravity type (i.e. gravity settling chamber) of natural precipitation particle
It is centrifugal (i.e. the whirlwind) using centrifugal force, utilizes various filter media formulas, electrodynamic type (i.e. electric precipitator), sound wave type
(i.e. sound wave dust separator) etc..In the present embodiment, since air or other gases are used as gas, so being collected using this example
Graphene particles be dry shape.There are one the device 6b for collecting graphene powder finished product for equipment, after completing cracking, stone
Black alkene powder 7 is output in export structure 6b by 11, and 11 be a delivery nozzle, is accepted with pipeline, and output tank 6b is mainly
The Graphene powder finished product for retaining and collecting output, the graphene powder 7 exported from output tank 6b can pass through according to cutting condition
Pipeline 19 is again placed in head tank 2, is cut for repeating.
The present invention produces in this embodiment of graphene, and equipment making chamber 5 was opened before this, and equipment will make chamber
5 inside is evacuated, and by being pumped into empty process, the impurity in make-up room 5 is removed；Then, Graphene powder will be made
The raw material 3 at end is placed in head tank 2, and the raw material of head tank 2 can in the light of actual conditions be controlled to head tank 3, and raw material passes through
Head tank 3 enters the 5th input unit 10e from pipeline 8 and is input in make-up room 5 again；Compressor 4 is opened, for compressing
Gas can be air or other gases, and the gas jet after the completion of compressing is defeated with the speed of 500 m/s as ultrahigh speed jet stream
Pipeline 9 is arrived out；These ultrahigh speed jet streams pass through first to fourth input unit 10a to 10d input gas jet 9a to 9d again；?
It makes in chamber 5, the raw material 3 of the ultrahigh speed jet stream and graphite that are entered collides, and causes to crack to carry out cutting graphite
Process.In production chamber 5, the first to the 5th input unit 10a can also be controlled into 10e to the input side of make-up room 5
To, mainly control gas jet input direction, make raw material production chamber 5 inner wall collide together with gas jet so that gas
Body jet stream and raw material 3 collide, and cause more to crack, the different graphene product of output, because production chamber 5 is can
With spherical in shape, gas jet can be along the inner wall rotation of production chamber 5, and raw material 3 can generate multiple impacts with gas jet, in spy
After the cracking process for carrying out graphene raw material in the fixed time, pipeline 11 is opened, and finished product can enter deduster 6a by pipeline 11,
It is that can separate and collect the graphene particles not being inconsistent with size in deduster 6a, the graphene powder 7 for meeting demand can be stored up
In the presence of in output tank 6b, can be returned in head tank 2 again by pipeline 19 in the undesirable graphene powder of tank 6b, it can
It is repeated several times and carries out cracking process.Its cracking principle is referred to Fig. 9 description.In embodiment, Fig. 9 (a) and Fig. 9 (bB) are to retouch
State graphene powder cracking principle schematic diagram.Graphene raw material and ultrahigh speed gas jet 9a to 9d collide, and gas jet exists
Graphite layers interact, and make fracture of graphite；Graphene powder after cracking also can also generate phase with its graphite layers
Graphite is cut in interaction, and the graphite in raw material and chamber processed make the inner wall of room 5 as the flowing of gas jet can also collide,
To cut graphite.Gas jet forms air-flow in production chamber 5, makes raw material 3 and the multiple impact several times of gas jet, graphite
Alkene raw material passes through multiple cracking process, and graphite raw material is easy to be crushed in parallel in plane.According to the production method of above-mentioned technique, stone
Black alkene raw material can also add in ultrahigh speed gas jet, be mixed into production chamber 5, can also complete cracking process.Pass through
Many experiments, present invention discover that the speed of gas jet is preferably within the scope of 100 ~ 1000 m/s, when speed is less than 100 m/s,
Due to jet intensity deficiency, may crack insufficient；When speed is more than 1000 m/s, graphene is difficult control to suitable ruler
In very little fine grained.It is possible that stomata, is difficult to keep the high quality of graphene in the crystal of graphene.
The present invention produces in another embodiment of graphene as shown in figure 3, Fig. 3 is shown using gas as jet stream
Another 20 schematic diagram of graphene powder production equipment device, this process units mainly on the basis of device 1, increase benefit
The device that graphene quality is modified with atmospheric plasma.Process units 20 increases other than the structure of process units 1
Plasma processing structures 15, high voltage power supply structure 16 and gas cylinder 13.By applying high pressure, Ke Yi in high voltage power supply 16
Plasma is generated in plasma processing structures 15, plasma resonance exports in the output channel 11 from production chamber 5
Graphene powder 7 on, the end surface of graphene can be attached to, thus provide have other function graphene powder
21.Graphene powder after the modification according to the above process, make it have better dispersibility, conductivity, thermal conductivity, absolutely
Edge, heat-radiating properties etc., it is this to handle other performances that graphene powder can be improved.By plasma processing structures 15
Black alkene powder 21 afterwards is collected in deduster 6a by pipeline 18, then is stored in output magazine 6b, and exports black alkene on demand
Powder.Used post-processing can also be other modifications, such as ultraviolet and ozone processing, at still plasma
Reason.In plasma processing structures 15, atmospheric pressure plasma can produce, also can produce vacuum plasma, gas cylinder
13 output atmospheric gases, such as argon gas, nitrogen, hydrogen, ammonia and oxygen.As seen from Figure 3, device and Fig. 1 device
Component is largely identical, and same components function is same as above.Here the rear place of main description addition atmospheric plasma
Reason process.
The present invention produces another embodiment of graphene as shown in figure 4, Fig. 4 is that description uses fluid as injection stream life
Produce the process units 30 of graphene powder.In Fig. 4, it is equipped with head tank 32, used raw material can be natural graphite, graphite
The mixture of powder and powdered graphite and liquid (mixture of such as water or organic solvent)；Adding liquid is additionally provided in head tank 32
Structure 45, structure 45 is primarily used to adding liquid, and the liquid used includes water and organic solvent, (such as such as alcohols solvent
Ethyl alcohol, isopropanol, isobutanol), ketone solvent (for example, methyl ethyl ketone, methyl iso-butyl ketone (MIBK) and diketone) and ether solvent (such as second
Ether, dioxanes and dimethyl sulfoxide)；It the use of water is that can to produce pure graphene powder be without changing in the case where liquid
Property, use the graphene powder for there are other solvents that can produce other function；It can thus be formed in head tank 32
The raw material of pulpous state；Specifically, being the slurry for being floated on a liquid using graphite as raw material and forming fluid form, slurry is again by pipe
Road 38 is input in super-pressure pump 34.Device 30 has at least one export structure of super-pressure pump 34 as liquid jet,
34 be a kind of pressure for increasing liquid by pressurizeing and the device that liquid is continuously conveyed, and common super-pressure pump can be used；
Super-pressure pump 34 pressurizes slurry formation ultrahigh speed jet stream in pipeline 36 and 37, and simultaneously to two opposite directions with liquid jet
For the input of ultrahigh speed injection stream.It may be provided between about 10 ~ 500MPa from the discharge pressure of the injection stream of super-pressure pump 34, and
And jet nozzle diameter may be provided between about 0.1 ~ 1mm；The velocity interval of liquid jet about speed is 100 ~ 1000 meters/S
Between.Super-pressure pump 34 is linked to a closed space chamber as production chamber 49, and production chamber 49 can also be with one not
Valve shown in figure carrys out shroud air, and inner atmosphere, which is maintained at high vacuum state, (can extract air out or full of liquid
Body), the common rectangle production chamber used can.The fine grained for exporting graphene powder 41 is by raw material and liquid
Jet stream cracks what graphene raw material method was formed in make-up room 49.Input structure 39 has one first input unit 39a and second
Input unit 39b is respectively inputted slurry 33 with 42 and 43 two opposite directions to make-up room 49 by pipeline 36 and 37 respectively
Ultrahigh speed jetting liquid jet stream；First input unit 39a and the second input unit 39b are each made of nozzle, and input direction
Be it is opposite, in production 49 surfaces opposite to each other of chamber room, device can also use input structures as multiple for they；Separately
Outer input structure can also increase a control unit (not showing in figure), first and second input of control input unit 39a is single
First 39b thus can control the direction of input unit injection liquid jet to 49 input direction of process chamber, liquid flow in addition to
Two opposite direction injections, can be sprayed with phase processor locular wall.In make-up room 49, the phase in a manner of liquid jet of raw material 33
Mutually collision is directly to cut the cracking that graphite causes graphite, and another situation, the liquid jet containing raw material 33 can also be with system
The inner wall for making room 49 collides to crack graphite.Complete cracking after, make-up room 49 by output section 41 export graphene powder with
The form of fine particle and the mixture 40 of liquid, the mixture 40 exported from output section 41 can pass through pipeline 44 again according to demand
It is secondary to return in head tank 32, for repeating cutting process.In addition, after cracking, the mixture 40 of graphene powder is from output
The liquid that portion 41 exports can be subjected to drying process to remove liquid, to obtain pure graphene powder；If mixture
In the case that liquid in 40 is expected organic solvent, it can not dry.Fig. 4 does not show reception and reservation contains stone
The out-put container of black alkene liquid, because this is not necessary structure.
The present invention produces in the embodiment of graphene, and make-up room 49 is first hydraulically full such as water, the production opening of chamber 49, superelevation
Press pump 34 is opened.It is placed in head tank 32 by 33 and liquid of raw material of graphite powder, raw material 33 passes through in a form of slurry
Pipeline 38 is input in super-pressure pump 34.Super-pressure pump 34 in form of slurry pressurizes to raw material 33, with the speed of 300 m/s
Liquid jet is output to pipeline 36 and 37 by degree.Liquid jet is with 42 and 43 two opposite directions from first
Input unit 39a and the second input unit 39b is input to production chamber 49, in make-up room 49, the first input unit 39a and the
Two input unit 39b are split each other, and the raw material 33 of slurry form is mutually collided with liquid jet in two opposite directions, thus
Carry out the cracking process that cutting graphite is formed.In make-up room 49, there can also be a control unit to control the first input single
First 39a and the second input unit 39b enters the input direction (not being necessary structure, do not show in figure) of production chamber 49, makes liquid
Body jet stream mutually collides, alternatively, the inner wall of control liquid jet and production chamber 49 collides.As shown in figure 4, in slurry form
Raw material 33 inputs water-filled production chamber 49 by the both direction of the first input unit 39A and the second input unit 39b, when
When liquid jet mutually collides, liquid jet can cut graphite in graphite layers, form cracking process；In addition, working as liquid jet
When mutually colliding, the graphite in liquid can also be cut mutually with other graphite, form cracking process；Furthermore when liquid jet phase
Mutually when the inner wall of collision production chamber 49, graphite can be also cut, forms cracking process.This is split according to the property of graphene
Solution, graphene is easy to be broken in parallel in plane.The speed that liquid flow is penetrated be within the scope of 100 ~ 1000 m/s it is most desirable,
The case where similar to above-mentioned gas.When speed is less than 100m/s, since the intensity of jet stream is insufficient, cutting may be insufficient,
When speed is more than 1000m/s, graphene is difficult to control into the fine grained with suitable dimension, also will cause the crystal of graphene
In there may be many apertures, be thus likely difficult to guarantee graphene high quality.So injection stream together with graphite with 100 ~
The speed of 1000m/s is input to production chamber 49, is the speed of most suitable cutting graphite, can provide fine grain Graphene powder
End.After completing cracking before the deadline, the graphene powder 40 of generation can be according to cracking condition, again by pipeline 44
It is placed in head tank 32 to repeat cracking process, forms cracking loop, so as to which the cracking for carrying out graphene powder is repeated several times
Process.Until producing qualified graphene powder 40.Hereafter, can be with further progress drying process, it in the drying process, can
To remove moisture by evaporation, relevant graphene powder product is isolated.The principle of cracking process is referred to Fig. 5, and 5 (a)
It is two schematic diagrames for describing liquid jet cracking graphene raw material with 5 (b).
The present invention produces another embodiment of graphene as shown in fig. 6, Fig. 6 is also that description uses fluid as injection stream
Produce the process units 50 of graphene powder, the process units 30 of device Fig. 4 similarly as described above.Wherein marked in figure
If identical as in process units 30, the components and functionality which shows all is and 30 phase of process units symbol out
Together, the components and functionality different from process units 30 is hereafter only described.
In the manufacturing device 50 of graphene powder shown in Fig. 6, the raw material 33 of slurry form is formed in head tank 32
It is not input to super-pressure pump 34.Super-pressure pump 34 is only to liquid pressing to export on pipeline 55 and 56, and to this two sides
The liquid jet of output flowing upwards.The liquid jet of liquid passes through pipeline 55 from the first input unit 39a of production chamber 49
Input, and the raw material 33 of paddle is mixed at point 51 with the liquid jet exported from super-pressure pump 34 by pipeline 38,
And it is inputted from the second input unit 39b of production chamber 49；In production chamber 49, with 33 liquid injection of raw material containing paddle
Stream is impinging one another with opposite direction shown in 52 and 53, to carry out the cracking process that cutting graphite is formed.Raw material 33 is with slurry
Form can be input in hydraulically full make-up room 49 from the second input unit 39b, and be from first containing only liquid jet
It is inputted in input unit 39a, in this case, graphite raw material directly carries out cutting stone between liquid jet intervention graphite linings
Ink.In this embodiment, the graphene of production be entirely cracked by liquid jet, either production graphene efficiency or
The quality of production graphene can all increase.The liquid jet speed used is identical as above-mentioned example.It can also lead in this way
The cracking for crossing graphite obtains the graphene powder 54 of tiny form.It also is provided with being placed again into shape in raw material slot 32 with sampling device 50
At the structure 44 in circuit, similar to the process units 30 of graphene powder shown in Fig. 4.The cracking principle of the present embodiment can join
According to Fig. 7, Fig. 7 (a) and 7(b) it is the schematic diagram for describing graphene raw material cracking in Fig. 6 device.
The present invention produces another embodiment of graphene as shown in figure 8, Fig. 6 is also that description utilizes cavitation effect production stone
The process units 60 of black alkene powder, the process units 30 of device Fig. 4 similarly as described above.Wherein in figure labelled in symbol
Number if identical as in process units 30, the components and functionality different from process units 30 is hereafter only described.
As shown in figure 8, the process units 60 of production graphene powder is passing through existing raw material 33 in slurry form
Liquid jet stream causes to be input to production chamber 66 to a direction.It is to crack graphene raw material using cavitation effect.Raw material 33 with
Slurry form is input to super-pressure pump 34 by pipeline 38 from head tank 32 and pressurizes, and inputting liquid jet is to pass through pipeline
36 are input in production chamber 66 in the first input unit 67a, and make-up room 66 is filled with liquid and forms vacuum, works as slurry form
Existing raw material is input in production chamber 66 by the first input unit 67a in a manner of liquid jet, can be generated a sky
Change effect, the process of cracking graphite raw material is carried out using pressure difference.Pressure difference be flowed by liquid jet 61 it is hydraulically full
Chamber 66 form bubble 65, explosion can occur in a short time for bubble 65, enter graphite original using the pressure difference of cavitation effect
To graphite of riving between the bed of material, the process of cracking graphite is formed.When raw material 33 is defeated from the first input unit 67A in a form of slurry
When entering to hydraulically full process chamber 66, raw cavitation effect is formed since meeting in the process generates pressure difference, and bubble 65 exists
Explosion occurs for the short time.Resulting bubble 65 can penetrate the cracking surface of graphite, to cut graphite.Liquid jet 61
Speed is identical as the example above, this process is also the fine grained that powdered graphite 64 is obtained by the cracking of graphite, cracking
Graphene powder after process can be dried, and can also be placed again into raw material slot 32 and be formed into a loop, be similar to
The process units 30 of graphene powder shown in Fig. 4.Cracking stock is referred to Fig. 9 description, and 9 (A) and 9 (B) describe Fig. 8 device
The schematic diagram of middle graphene raw material cracking.
It may not be hydraulically full inside certain make-up room 66, can be full of other gases or vacuum, in this way
Raw material 33 in slurry form is input in vacuum from the first input unit 67A, then with the wall direct collision in make-up room 66,
The process that can be cracked, to cut graphite, cracking principle has proposition above.If using such cracking mode,
The same graphene powder that can produce small particulate form.
Graphene powder production method of the invention can be produced by five kinds of production equipments illustrated above.Furthermore, it is possible to will
Multiple devices in above-mentioned five kinds of devices combine, to carry out the cutting process comprising two or more stages.For example, graphite
Powder 40 is by that can place being split again for process units 50 to generating in 30 cutting process of graphite powder production equipment
Solution preocess, to carry out the cracking comprising two stages.In this case, graphene powder be can be as raw material
It is transferred in another process units and is formed into a loop, repeatedly recycled, substituted, form the process repeatedly cracked, can obtain
Obtain more graphene product types.
According to example above, the present invention provides used in a kind of method and this method for producing graphene powder
Device.This method is formed by jet stream cutting containing graphite raw material using process units, and the graphene of this method production is not
It can be polluted by other substances, purity is high, high-quality graphene powder can be produced.Since the present invention is former by cracking graphite
The method of material can be in be similar to leaf sheet and tiny graininess at graphene powder, graphene powder is produced, especially
It is analogous to the graphene powder of leaf sheet, obtains that surface area is larger, the contact area with other materials is increased, to mention
High conductivity and dispersibility.
Figure 10 is that the graphene powder 7 produced using process units provided by the invention passes through electron microscope (SEM)
The image observed.As shown in Figure 10, surface has the trace cracked, the graphene powder longest to graphene powder 7 on it
Part is about 990nm, and a part of thickness (perpendicular to cracking face direction) minimum (thin) is about 19.5 nm, largest portion
(thickness) is about 200 nm.Show that the long side length for cracking face is about the 50~3000 of its thickness by observing other Graphene powders
Times, graphene powder is made of 70% or more graphene powder.As graphene layer, about 300 layers of graphene list is observed
Layer.Observation by the graphene powder made to other process units finds the long side length in cracking face for Graphene powder most
30~10000 times of small thickness, graphene powder is made of 70% or more graphene powder.As graphene layer, also observe
About 300 layers of graphene single layer.
Figure 11,12 are that graphite raw material passes through the graphene product of the cracking process formation of different modes in the description present invention
And its different product attribute, it is fine grained graphite alkene product attribute schematic diagram, 11 (b) flake graphite alkene shown in 11 (a)
Product attribute schematic diagram.It is the graphene fine grained schematic diagram of the uniform shape formed by three-dimensional cracking shown in 12 (a), 12
It (b) is the flake graphite alkene schematic diagram for being cracked by two dimension and being formed shown in.Graphene raw material is former by the three-dimensional cracking crushed
Reason forms fine grained, is the biggish fine grained of thickness, graphene powder 100 as shown in FIG. 11 and 12, the application of this fine grained
When have contact area small, conductivity is small, and dispersibility is low, the small equal product attribute of specific surface area；And graphene raw material passes through two
The flake graphite alkene powder that the cracking principle that dimension crushes is formed, graphene powder 7 as shown in FIG. 11 and 12 have contact area
Greatly, conductivity is big, and dispersibility is high, the product attribute of large specific surface area etc..The specialities attribute that can use them is used in
In different purposes.
On the other hand, it is simply cut in accordance with the present production process with jet stream with process units, graphite, and it is common
Production method is compared, and graphene produced by the invention has the characteristics that high-crystallinity, high quality, is mass produced at high speed.This
It has invented and has been tested, the present invention can reach 1 ~ 10000 kg/hour of speed of production；In production method of the invention,
Wet graphene and dry graphene can also be generated, is solved the problems, such as described in background of invention.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection shall be subject to the appended claims for patent of invention.
Claims (8)
1. a kind of method for preparing graphene powder, this method includes the steps that cracking graphite raw material, with containing 100~1000
The gas jet of meter per second cracks graphite raw material, to generate tiny graphene powder.
2. a kind of device for preparing graphene powder, including head tank 2, gas jet output device 4, make-up room 5, deduster
6a, output tank 6b, it is characterised in that head tank 2 is equipped with pipeline 8 and is connected with make-up room 5, and gas jet output device 4 is equipped with pipeline
9 are connected with make-up room 5, and make-up room 5 is equipped with pipeline 11 and is connected with deduster 6a, and deduster 6a and output tank 6b connect.
3. a kind of device for preparing graphene powder, a kind of device base preparing graphene powder according to claim 2
Increase gas ions processing structure 15, high voltage power supply structure 16 and gas cylinder 13 on plinth, it is characterised in that make-up room 5 is equipped with 11 He of pipeline
Gas ions processing structure 15 is connected, and gas ions processing structure 15 is equipped with pipeline 17 and is connected with gas cylinder 13, gas ions processing structure 15
It is connected with high voltage power supply structure 16.
4. a kind of method for preparing graphene powder, this method includes the steps that cracking graphite raw material, with containing 100~1000
The liquid jet of meter per second cracks graphite raw material, to generate tiny graphene powder.
5. a kind of device for preparing graphene powder, including head tank 32, super-pressure pump 34 and make-up room 49, it is characterised in that former
Batch can 32 is equipped with pipeline 38 and is connected with super-pressure pump 34, and super-pressure pump 34 is equipped with pipeline 36,37 and is connected with make-up room 49.
6. a kind of device for preparing graphene powder, including head tank 32, super-pressure pump 34 and make-up room 66, it is characterised in that former
Batch can 32 is equipped with pipeline 38 and is connected with super-pressure pump 34, and super-pressure pump 34 is equipped with pipeline 36 and is connected with make-up room 66.
7. a kind of method for producing graphene powder, the speed of production of this method can consume minimum 1 kg/hour of raw material.
8. a kind of method for producing graphene powder, this method includes that the graphene powder obtained in the chamber is made to be again introduced into chamber
The circulation step of room.
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| CN112778729A (en) * | 2020-12-30 | 2021-05-11 | 西北大学 | Preparation method of graphene reinforced SMC composite material |
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| CN112778729A (en) * | 2020-12-30 | 2021-05-11 | 西北大学 | Preparation method of graphene reinforced SMC composite material |
| CN112778729B (en) * | 2020-12-30 | 2021-09-28 | 西北大学 | Preparation method of graphene reinforced SMC composite material |
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