CN205590299U - Generate graphene films's device - Google Patents
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- CN205590299U CN205590299U CN201521136577.1U CN201521136577U CN205590299U CN 205590299 U CN205590299 U CN 205590299U CN 201521136577 U CN201521136577 U CN 201521136577U CN 205590299 U CN205590299 U CN 205590299U
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Abstract
The utility model discloses a generate graphene films's device uses wet process stirring ball -milling to peel off graphite layer, preparation graphene films. Its characterized in that: the device by high temperature handle portion, normal position reduction portion, add medicine portion, the machinery portion of peeling off, centrifugation portion and dryer part and constitute, peel equipment includes cylindrical cavity, axis of rotation, rotation horizontal pole and ball etc. And wherein square with the axis many of axis of rotation drive are rotated horizontal poles and are driven mutual the collision and the friction of ball in the cavity at the fixed internal stirring of cylindrical cavity, rotation horizontal pole in the stirring to grind the powder, graphite material is under receiving the shear effect of frictional force, and the van der waals force in the graphite between each graphite layer disintegrates, thereby it obtains graphite alkene to make graphite peeled off the attenuate, gets into centrifugation portion. The utility model discloses the mechanical stripping off device easy operation of class of production graphite alkene, gained graphite alkene crystal structure is perfect, and can realize the high -efficient stabilization production of graphite alkene.
Description
Technical field
This utility model relates to the graphene film of a kind of efficient stable and produces equipment, particularly relates to a kind of raw
Become the device of graphene film.
Background technology
Graphene relies on one of character focus becoming investigation of materials field in recent years of its uniqueness.Initially
The two-dimension periodic honeycomb lattice structure that the Graphene found is made up of monolayer carbon hexatomic ring, can be described as this
Levying Graphene or single carbon-coating Graphene, it is prepared by adhesive tape method.It can be warped into zero dimension
Fullerene, be rolled into one-dimensional CNT or be stacked to the graphite of three-dimensional, therefore single carbon-coating Graphene
It it is the elementary cell constituting other graphite materials.As a kind of quasi-two dimensional crystal, single carbon-coating Graphene is at carbon
With or without the periodic structure that freight weight limit is multiple in plane, but in the direction being perpendicular to carbon plane, only there is nanometer chi
Degree, can be regarded as the nano material with macro-size, shows much unique character.Graphene
There are two-dimentional electricity, optics, calorifics, mechanical property and the chemical stability of brilliance, the two of its uniqueness
Dimension structure and excellent crystallography quality make its at supper-fast micro-nano opto-electronic device, radio-frequency devices, clean
The fields such as net energy source and various kinds of sensors have important practical value.Such as, electronics is abided by Graphene
Follow relativistic quantum mechanics, there is no rest mass, run with the ultraspeed of 1/300 light velocity, show
Unusual room-temperature quantum Hall effect and ballistic transport phenomenon, can prepare room temperature ballistic transport transistor, quilt
It is considered as the important foundation new material of Future Information nano-device;Graphene electric transmission speed is the 150 of silicon
Times, it is expected to prepare supper-fast computer and radio-frequency devices that speed reaches megahertz;The unimolecule of Graphene
The sensitivity of degree is expected to obtain extensively at various sensors, the such as field such as gas sensor and biosensor
Application;Graphene has the optical characteristics that 2.3% light absorbs so that it is may be used for preparing supper-fast light and visits
Survey device and mode-locked laser, on the other hand, due to extremely low optical absorption characteristics so that Graphene both can be used
In preparing opto-electronic device, such as the transparency electrode of light emitting diode and solaode etc., thus it is replaced to
This costliness, resource scarcity, the most folding transparent conducting film with indium as main component, it is also possible to
In preparing ultracapacitor and lithium ion battery;The energy conversion of solar battery based on Graphene
Efficiency is expected to reach 24%.
At present, the method predominantly organic tool stripping method of Graphene, graphite oxide reducing process, thermal decomposition are prepared
SiC method, chemical vapour deposition technique and epitaxial growth method etc..Wherein, graphite oxide reducing process relative efficiency
And cost is relatively low, and substantial amounts of graphene suspension and Graphene derivative can be prepared, but in oxidation
During reduction, the electronic structure of Graphene and perfection of crystal are easily subject to the broken of strong oxidizer
Bad, cause the structure of Graphene to there is more uncontrollable defect, and cause its part electricity, calorifics
The loss of energy;Pyrolysis SiC method also can produce uncontrollable defect and many crystalline domain structure, it is difficult to obtains preferably
Long range ordered structure, the Graphene that preparation large area has single thickness is relatively difficult;Chemical gaseous phase deposits
Although method can realize the large area deposition of graphene film, but technology controlling and process is complex;Epitaxial growth
The graphene platelet that method produces is the most in uneven thickness, and the bonding between Graphene and substrate can affect carbon
The characteristic of layer.By contrast, mechanical stripping method is a kind of to prepare high-quality graphene with low cost
Simple method.The principal element of the research of restriction grapheme material and application is at present: Graphene is difficult
It is difficult to control to quality and productivity in scale preparation and preparation process.
Utility model content
For the deficiency of prior art, the invention provides a kind of device generating graphene film, it is special
Levying and be, described device is by high-temperature process portion, in-situ reducing portion, dosing portion, mechanical stripping portion, centrifugal
Separated part and drying section are constituted;
The cylindrical chamber in described mechanical stripping portion is connected with in-situ reducing portion by the first feeding-passage, institute
The cylindrical chamber stating mechanical stripping portion is connected with dosing portion by the second feeding-passage, and rotary shaft is at cylinder
Vertical with rotating horizontal pole in shape chamber being connected, abrading-ball is placed in described cylindrical cavity indoor, described cylindrical cavity
Room is connected with centrifugation portion by discharge gate;
Wherein, described rotary shaft drives square with the axis connected rotating horizontal pole indoor at fixing cylindrical cavity
Agitation, in order in drive chamber, abrading-ball and graphite raw material mutually collide and rub in agitation.
According to a preferred implementation, described abrading-ball is diameter 50 μm~100 μm and hardness is more than
The pearl of graphite.
According to a preferred implementation, described high-temperature process portion is at 200 DEG C~1200 DEG C and nitrogen
Or under conditions of inert gas atmosphere, graphite raw material is carried out high-temperature process.
According to a preferred implementation, described in-situ reducing portion is at 200 DEG C~1200 DEG C and nitrogen hydrogen
Under conditions of mixed-gas atmosphere, graphite raw material is carried out reduction treatment.
According to a preferred implementation, for deposit the described dosing portion of surfactant additive for,
It is connected with the described mechanical stripping portion for graphite raw material is peeled off by the second feed pipe, and
Described dosing portion is for continuing the cylindrical chamber's dosing to mechanical stripping portion.
According to a preferred implementation, described mechanical stripping portion is used for receiving stone after in-situ reducing portion processes
Ink raw material the surfactant additive provided based on described dosing portion complete the described stone after high-temperature process
The mechanical stripping of ink raw material processes.
According to a preferred implementation, described centrifugation portion is for by after mechanical stripping portion processes
The mixing suspension liquid of Graphene and graphite is centrifuged separating.
According to a preferred implementation, described drying section is for doing the graphene-containing solution obtained
Dry process, obtains graphene film.
According to a preferred implementation, described high-temperature process portion is at 200 DEG C~1200 DEG C and nitrogen
Or under the conditions of inert gas atmosphere, graphite raw material is carried out high-temperature process, and it is connected with in-situ reducing portion;
Described in-situ reducing portion is under conditions of 200 DEG C~1200 DEG C and nitrogen hydrogen mixeding gas atmosphere
The graphite raw material received after described high-order process portion processes is carried out reduction treatment, and by the first charging
Pipeline is connected with mechanical stripping portion;
For depositing the described dosing portion of surfactant additive by the second feed pipe and for stone
The described mechanical stripping portion that ink raw material carries out peeling off is connected, and described dosing portion is for continuing to machinery stripping
Cylindrical chamber's dosing from portion;
Described mechanical stripping portion is used for receiving after in-situ reducing portion processes graphite raw material and based on described dosing
The surfactant additive that portion provides completes the mechanical stripping of the described graphite raw material after high-temperature process and processes;
Described centrifugation portion is for hanging the mixing of the Graphene after mechanical stripping portion processes and graphite
Turbid liquid liquid is centrifuged separating;Described drying section is for being dried place by the graphene-containing solution obtained
Reason, obtains graphene film.
According to a preferred implementation, the cylindrical chamber in described mechanical stripping portion is logical by the first charging
Road is connected with in-situ reducing portion, and the cylindrical chamber in described mechanical stripping portion passes through the second feeding-passage and adds
Medicine portion is connected, and rotary shaft vertical with rotating horizontal pole is connected cylindrical cavity is indoor, and abrading-ball is placed in described cylinder
In shape chamber, described abrading-ball is the pearl that diameter 50 μm~100 μm and hardness are more than graphite, described
The cylindrical chamber in mechanical stripping portion is connected with centrifugation portion by discharge gate, wherein, and described rotary shaft
Drive square with the axis connected rotating horizontal pole in fixing cylindrical cavity indoor agitation, in order to carry in agitation
In dynamic cavity, abrading-ball and graphite raw material mutually collide and rub.
This utility model has the advantage that
(1) abrading-ball of the present utility model is with the abrading-ball of 50 μm~100 μm as ball-milling medium, at graphite
During mechanical stripping, graphite flake layer is repeatedly peeled off number of times and is dramatically increased, and improves mechanical stripping efficiency.
(2) ball radius of the present utility model controls when 50 μm~100 μm, gained graphite flake layer
Thickness distribution is concentrated, and the graphite flake layer thickness of more than 50% is all at below 4nm.
(3) this utility model produces graphene film in the way of mechanical stripping, it is ensured that Graphene is brilliant
Body structural perfection.
Accompanying drawing explanation
Fig. 1 is device of the present utility model each portion annexation schematic diagram;With
Fig. 2 is this utility model mechanical stripping portion structural representation.
Reference numerals list
101: graphite raw material 102: high-temperature process portion 103: in-situ reducing portion
104: dosing portion 105: centrifugation portion 106: drying section
107: graphene film 200: mechanical stripping portion 201: cylindrical chamber
202: the first feeding-passage 203: the second feeding-passages 204: rotary shaft
205: rotating horizontal pole 206: abrading-ball 207: discharging channel
Detailed description of the invention
It is described in detail with embodiment below in conjunction with the accompanying drawings.
Fig. 1 shows device of the present utility model each portion annexation.As it is shown in figure 1, this utility model
A kind of device generating graphene film includes high-temperature process portion 102, in-situ reducing portion 103, dosing portion
104, mechanical stripping portion 200, centrifugation portion 105, drying section 106.Described high-temperature process portion
102 are connected with in-situ reducing portion 103, the high-temperature process portion 102 graphite raw material 101 to being added thereto
Carry out high-temperature process, and the graphite raw material 101 after processing delivers to in-situ reducing portion 103.At high temperature
Reason temperature is 200 DEG C~1200 DEG C, and processing environment remains air, vacuum, nitrogen or noble gas.
One preferred embodiment remains inert gas environment for processing environment in high-temperature process.Graphite
Raw material 101 heats 200 DEG C~1200 DEG C, under oxygen-containing functional group stability under inert gas shielding
Fall, leaves with the form such as steam, carbon dioxide.In-situ reducing portion 103 and high-temperature process portion 102
It is connected with mechanical stripping portion 200.In-situ reducing portion 103 accepts after high-temperature process portion 102 processes
Graphite raw material 101, and it is carried out reduction treatment, the graphite raw material 101 after process delivers to machinery stripping
From portion 200.In position in reduction portion 103, under 200 DEG C~1200 DEG C of temperature conditionss, add nitrogen
At least one in gas or hydrogen, as reducing medium, carries out reduction treatment to graphite raw material 101, enters one
Step removes the oxygen-containing functional group in graphite raw material 101.Dosing portion 104 is connected with mechanical stripping portion 200.
Dosing portion 104 is used for depositing surfactant additive, and former to graphite in described mechanical stripping portion 200
Material 101 carries out in stripping process, continues to mechanical stripping portion 200 dosing.Surfactant additive is
Sodium lauryl sulphate, methyl anyl alcohol, Disodium oxalate., sodium carboxymethylcellulose pyce, polyacrylamide, guar gum,
One or more in fatty acid polyethylene glycol ester.Mechanical stripping portion 200 and centrifugation portion 105 phase
Even.The mechanical stripping portion 200 graphite raw material 101 after the reduction treatment receiving in-situ reducing portion 103
The surfactant provided with dosing portion 104, and carry out stirring ball milling to the graphite raw material 101 received
Peel off, and the mixing suspension of the Graphene after lift-off processing and graphite is sent into centrifugation portion
105.Centrifugation portion 105 is connected with drying section 106.Centrifugation portion 105 is therein to entering
The mixing suspension of Graphene and graphite be centrifuged process, to Graphene suspension, and send into be dried
Portion 106.Drying section 106 is dried process to entering Graphene suspension therein, finally gives
Graphene film 107.
Fig. 2 is this utility model mechanical stripping portion structure matters figure.See shown in 2, mechanical stripping portion
200 include cylindrical chamber's the 201, first feeding-passage the 202, second feeding-passage 203, rotary shaft
204, rotating horizontal pole 205 and abrading-ball 206.The cylindrical chamber 201 in mechanical stripping portion 200 passes through
First feeding-passage 202 is connected with in-situ reducing portion 103, the cylinder in described mechanical stripping portion 200
Chamber 201 is connected with dosing portion 104 by the second feeding-passage 203, and rotary shaft 204 is in cylinder
Vertical with rotating horizontal pole 205 in chamber 201 being connected, abrading-ball 206 is placed in described cylindrical chamber 201
In, described abrading-ball 206 is the pearl that diameter 50-100 μm and hardness are more than graphite.Described machinery stripping
Cylindrical chamber 201 from portion 200 is connected with centrifugation portion 105 by discharging channel 207.Former
Reduction portion, position 103 is by first feeding-passage 202 cylindrical chamber 201 to mechanical stripping portion 200
Add graphite raw material 101.Dosing portion 104 passes through the second charging aperture 203 to mechanical stripping portion 200
Cylindrical chamber 201 adds surfactant additive.Rotary shaft 204 drives vertical with rotary shaft 204
The rotating horizontal pole 205 being connected stirs in cylindrical chamber 201.Rotating horizontal pole 205 carries in agitation
Abrading-ball 206 and graphite raw material 101 in dynamic cylindrical chamber 201 mutually collide and rub, and graphite is former
Material 101 under the shear action of described abrading-ball 206 frictional force, the Van der Waals of each graphite layers in graphite
Power is disintegrated, it is thus achieved that Graphene and the suspension of graphite.
Embodiment 1
In conjunction with Fig. 1 and Fig. 2, graphene film production process of the present utility model is described.High-temperature process portion
102 are connected with in-situ reducing portion 103, and high-temperature process portion 102 is at 1000 DEG C of high temperature and noble gas
Under processing environment, the graphite raw material 101 being added thereto is carried out 1 hour high-temperature process, and by after process
Graphite raw material 101 deliver to in-situ reducing portion 103.Graphite raw material 101 adds under inert gas shielding
Heat is to 1000 DEG C, and oxygen-containing functional group stability declines, and leaves stone with the form such as steam, carbon dioxide
Ink alkene raw material 101.In-situ reducing portion 103 is connected with high-temperature process portion 102, and by the first charging
Passage 202 is connected with the cylindrical chamber 201 in mechanical stripping portion 200.In-situ reducing portion 103 accepts
Graphite raw material 101 after high-temperature process portion 102 processes, and under 1000 DEG C of temperature conditionss, add
At least one in nitrogen or hydrogen, as reducing medium, carries out reduction treatment in 1 hour to it, after process
Graphite raw material 101 deliver to the cylindrical chamber 201 in mechanical stripping portion 200.Graphite raw material 101 enters
Row reduction treatment, will remove the oxygen-containing functional group in graphite raw material 101 further.Dosing portion 104 leads to
Cross the second feeding-passage 203 to be connected with the cylindrical chamber 201 in mechanical stripping portion 200.Dosing portion 104
For depositing surfactant additive, and in described mechanical stripping portion 200, graphite raw material 101 is carried out
In stripping process, continue to add sodium lauryl sulphate to mechanical stripping portion 200 and be made into concentration with water be
The slurry of 80.0%.The rotary shaft 204 in mechanical stripping portion 200 is in cylindrical chamber 201 and rotates
Cross bar 205 vertically connects, and abrading-ball 206 is placed in described cylindrical chamber 201, in-situ reducing portion 103
Graphite raw material is added to the cylindrical chamber 201 in mechanical stripping portion 200 by the first feeding-passage 202
101.Dosing portion 104 is by second charging aperture 203 cylindrical chamber 201 to mechanical stripping portion 200
Add surfactant additive.Rotary shaft 204 drives the rotating horizontal pole being vertically connected with rotary shaft 204
205 stir in cylindrical chamber 201.Rotating horizontal pole 205 drives cylindrical chamber 201 in agitation
Interior abrading-ball 206 and graphite raw material 101 mutually collide and rub, and graphite raw material 101 is at described abrading-ball
Under the shear action of 206 frictional force, in graphite, the Van der Waals force of each graphite layers is disintegrated, it is thus achieved that Graphene
Suspension with graphite.Described abrading-ball 206 is that diameter 50 μm~100 μm and hardness are more than graphite
Pearl.The cylindrical chamber 201 in described mechanical stripping portion 200 is divided with centrifugal by discharging channel 207
It is connected from portion 105.Mechanical stripping portion 200 passes through discharging channel 207 by the stone after lift-off processing
The mixing suspension of ink alkene and graphite sends into centrifugation portion 105.Centrifugation portion 105 and drying section
106 are connected.The mixing suspension entering Graphene therein and graphite is carried out by centrifugation portion 105
Centrifugal treating, to Graphene suspension, and send into drying section 106.Drying section 106 is to entering it
In Graphene suspension be dried process, finally give graphene film 107.
The abrading-ball 206 of the present embodiment with the abrading-ball of a diameter of 50 μm~100 μm as ball-milling medium,
During graphite mechanical stripping, for the diameter ball-milling medium more than 100 μm, graphite flake layer
Dramatically increased by repeatedly peeling off number of times, improve mechanical stripping efficiency.And gained graphite flake layer thickness divides
Cloth is concentrated, and the graphite flake layer thickness of more than 50% is all at below 4nm.
It should be noted that above-mentioned specific embodiment is exemplary, those skilled in the art can be at this
Find out various solution under the inspiration of disclosure of the invention content, and these solutions also belong to the present invention
Open scope and fall under the scope of the present invention.It will be understood by those skilled in the art that this
Bright description and accompanying drawing thereof are illustrative and not constitute limitations on claims.The protection of the present invention
Scope is limited by claim and equivalent thereof.
Claims (10)
1. the device generating graphene film, it is characterized in that, described device is made up of high-temperature process portion (102), in-situ reducing portion (103), dosing portion (104), mechanical stripping portion (200), centrifugation portion (105) and drying section (106);
The cylindrical chamber (201) of described mechanical stripping portion (200) is connected with in-situ reducing portion (103) by the first feeding-passage (202), the cylindrical chamber (201) of described mechanical stripping portion (200) is connected with dosing portion (104) by the second feeding-passage (203), rotary shaft (204) is vertical with rotating horizontal pole (205) in cylindrical chamber (201) to be connected, abrading-ball (206) is placed in described cylindrical chamber (201), described cylindrical chamber (201) is connected with centrifugation portion (105) by discharge gate;
Wherein, described rotary shaft (204) drives square with the axis connected rotating horizontal pole (205) to stir in fixing cylindrical chamber (201), in order to the mutually collision of abrading-ball (206) and graphite raw material (101) and friction in drive chamber in agitation.
A kind of device generating graphene film the most as claimed in claim 1, it is characterised in that described abrading-ball (206) is the pearl that diameter 50 μm~100 μm and hardness are more than graphite.
A kind of device generating graphene film the most as claimed in claim 1, it is characterized in that, described high-temperature process portion (102) is for carrying out high-temperature process to graphite raw material (101) under conditions of 200 DEG C~1200 DEG C and nitrogen or inert gas atmosphere.
A kind of device generating graphene film the most as claimed in claim 1, it is characterized in that, described in-situ reducing portion (103) is for carrying out reduction treatment to graphite raw material (101) under conditions of 200 DEG C~1200 DEG C and nitrogen hydrogen mixeding gas atmosphere.
A kind of device generating graphene film the most as claimed in claim 1, it is characterized in that, it is used for for depositing the described dosing portion (104) of surfactant additive, it is connected with the described mechanical stripping portion (200) for graphite raw material (101) is peeled off by the second feed pipe, and described dosing portion (104) is for continuing cylindrical chamber (201) dosing to mechanical stripping portion (200).
A kind of device generating graphene film the most as claimed in claim 1, it is characterized in that, described mechanical stripping portion (200) be used for receiving graphite raw material (101) after in-situ reducing portion (103) processes and the surfactant additive that provides based on described dosing portion (104) complete high-temperature process after the mechanical stripping of described graphite raw material (101) process.
A kind of device generating graphene film the most as claimed in claim 1, it is characterized in that, described centrifugation portion (105) is for being centrifuged separating by the mixing suspension liquid of the Graphene after mechanical stripping portion (200) process and graphite.
A kind of device generating graphene film the most as claimed in claim 1, it is characterised in that described drying section (106), for the graphene-containing solution obtained is dried process, obtains graphene film (107).
A kind of device generating graphene film the most as claimed in claim 1, it is characterized in that, described high-temperature process portion (102) for carrying out high-temperature process under the conditions of 200 DEG C~1200 DEG C and nitrogen or inert gas atmosphere to graphite raw material (101), and is connected with in-situ reducing portion (103);
Described in-situ reducing portion (103) for carrying out reduction treatment under conditions of 200 DEG C~1200 DEG C and nitrogen hydrogen mixeding gas atmosphere to the graphite raw material (101) received after described high-temperature process portion (102) processes, and is connected with mechanical stripping portion (200) by the first feed pipe;
It is connected with the described mechanical stripping portion (200) for graphite raw material (101) is peeled off by the second feed pipe for depositing the described dosing portion (104) of surfactant additive, and described dosing portion (104) is for continuing cylindrical chamber (201) dosing to mechanical stripping portion (200);
Described mechanical stripping portion (200) be used for receiving graphite raw material (101) after in-situ reducing portion (103) processes and the surfactant additive that provides based on described dosing portion (104) complete high-temperature process after the mechanical stripping of described graphite raw material (101) process;
Described centrifugation portion (105) is for being centrifuged separating by the mixing suspension liquid of the Graphene after mechanical stripping portion (200) process and graphite;Described drying section (106), for the graphene-containing solution obtained is dried process, obtains graphene film (107).
nullA kind of device generating graphene film the most as claimed in claim 1,It is characterized in that,The cylindrical chamber (201) of described mechanical stripping portion (200) is connected with in-situ reducing portion (103) by the first feeding-passage (202),The cylindrical chamber (201) of described mechanical stripping portion (200) is connected with dosing portion (104) by the second feeding-passage (203),Rotary shaft (204) is vertical with rotating horizontal pole (205) in cylindrical chamber (201) to be connected,Abrading-ball (206) is placed in described cylindrical chamber (201),Described abrading-ball (206) is the pearl that diameter 50 μm~100 μm and hardness are more than graphite,The cylindrical chamber (201) of described mechanical stripping portion (200) is connected with centrifugation portion (105) by discharge gate,Wherein,Described rotary shaft (204) drives square with the axis connected rotating horizontal pole (205) to stir in fixing cylindrical chamber (201),So that abrading-ball (206) and graphite raw material (101) mutually collide and friction in driving cavity in agitation.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107539975A (en) * | 2017-10-31 | 2018-01-05 | 南京旭羽睿材料科技有限公司 | A kind of graphene synthesizer |
CN109956499A (en) * | 2017-12-14 | 2019-07-02 | 中国科学院深圳先进技术研究院 | The stripping means of two-dimensional material |
-
2015
- 2015-12-31 CN CN201521136577.1U patent/CN205590299U/en active Active
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107539975A (en) * | 2017-10-31 | 2018-01-05 | 南京旭羽睿材料科技有限公司 | A kind of graphene synthesizer |
CN109956499A (en) * | 2017-12-14 | 2019-07-02 | 中国科学院深圳先进技术研究院 | The stripping means of two-dimensional material |
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