CN112144123B - Device for preparing graphene crystal film by electron beam scanning - Google Patents
Device for preparing graphene crystal film by electron beam scanning Download PDFInfo
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- CN112144123B CN112144123B CN202010979553.1A CN202010979553A CN112144123B CN 112144123 B CN112144123 B CN 112144123B CN 202010979553 A CN202010979553 A CN 202010979553A CN 112144123 B CN112144123 B CN 112144123B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/02—Elements
Abstract
A device for preparing a graphene crystal film by electron beam scanning comprises a vacuum chamber and an electron gun arranged at the top of the vacuum chamber, wherein a workbench is arranged inside the vacuum chamber, an insulating plate is arranged on the workbench, a metal substrate is arranged on the insulating plate, and a carbon polymer film is arranged on the metal substrate; the carbon powder adsorption cover comprises an inner layer and an outer layer, a plurality of insulating ceramic blocks are arranged between the inner layer and the outer layer, the inner layer is grounded, and the outer layer is electrically connected with a first direct current power supply so as to form a first adsorption electrostatic field between the inner layer and the outer layer, wherein the first adsorption electrostatic field is used for adsorbing carbon powder generated in the process of preparing the graphene crystal film by scanning an electron beam. The invention can adsorb the carbon powder generated in the processing process to the maximum extent through the carbon powder adsorption cover, effectively prevent the pollution of the carbon powder generated in the processing process to the electron gun and the vacuum chamber, and prolong the service life of the equipment.
Description
Technical Field
The invention relates to the technical field of graphene crystal film preparation, in particular to a device for preparing a graphene crystal film by electron beam scanning.
Background
The graphene powder and the graphene crystal film are two types of graphene accepted in the industry field at present. At present, production devices and process technologies of graphene powder are becoming mature, but the preparation technology of graphene crystal films is still in a laboratory stage. Compared with graphene powder, the graphene crystal film has more obvious application superiority in various industry fields. In the aerospace field, the graphene crystal film-based wire can replace a metal wire, or can be directly prepared on a polyimide-based composite material according to the wire layout, so that the structural weight of the aircraft can be reduced, and the overall performance of the aircraft can be effectively improved. The graphene crystal film can be made into an energy storage device, has the advantages of high energy storage capacity, high charging speed, light weight, long service life, no pollution and the like, can replace the traditional lead-acid battery and lithium battery, and can bring new revolution to the development of industries such as batteries, electric vehicles and the like. In daily life, the graphene crystal film can be made into wearable clothes.
At present, the preparation of the graphene crystal film mainly comprises a chemical vapor deposition method, an outer edge growth method, a stripping method and the like, and the methods cannot meet the requirement of large-scale batch production. In recent years, some research institutions at home and abroad begin to prepare graphene crystal films by adopting electron beam irradiation and laser scanning methods, but the requirements of large-scale high-quality graphene crystal film preparation cannot be met. When the graphene crystal film is prepared by adopting an electron beam irradiation technology, although the width and the number of layers of graphene can be controlled, the diameter of a beam spot is less than 50nm, the irradiation time needs 10-120 s, the production efficiency is too low, and the requirement of large-scale batch production cannot be met; when the graphene crystal film is prepared by adopting a laser scanning technology, the preparation is usually carried out in an atmospheric environment, carbon powder generated in the process of scanning the carbon polymer film by laser easily pollutes the surrounding environment, and the quality of the generated graphene crystal film is easily influenced by gas impurities, so that the quality is difficult to greatly improve.
Disclosure of Invention
The embodiment of the invention provides a device for preparing a graphene crystal film by electron beam scanning, which can be used for preparing the graphene crystal film in a large-scale batch manner and simultaneously improving the quality of the prepared graphene crystal film.
A device for preparing a graphene crystal film by electron beam scanning comprises a vacuum chamber and an electron gun arranged at the top of the vacuum chamber, wherein a workbench is arranged inside the vacuum chamber, an insulating plate is arranged on the workbench, a metal substrate is arranged on the insulating plate, and a carbon polymer film is arranged on the metal substrate;
the carbon polymer film outside to the regional cage of electron beam current delivery outlet at the inboard top in vacuum chamber has the carbon dust to adsorb the cover, the carbon dust adsorbs the cover and includes inlayer and skin, be equipped with a plurality of insulating ceramic blocks between inlayer and the skin, inlayer ground connection, skin and first direct current power electric connection, so that form first absorption electrostatic field between inlayer and the skin, this first absorption electrostatic field is used for adsorbing the carbon dust that electron beam scanning preparation graphite alkene crystal film in-process produced.
Furthermore, the carbon powder adsorption cover is made of a non-magnetic metal material, and the structural size of the carbon powder adsorption cover is gradually reduced from the outer side of the carbon polymer film to an electron beam output port at the top of the inner side of the vacuum chamber.
Furthermore, the inner layer and the outer layer are respectively and uniformly densely distributed with 1-3 mm first adsorption holes, and the first adsorption holes on the inner layer and the outer layer are distributed in a staggered mode.
Furthermore, the electron gun comprises a shell, wherein a cathode, a grid, an insulator, an anode fixing disc, a focusing coil, a scanning coil, a coil fixing disc and a carbon powder adsorption grid are sequentially and coaxially arranged in the shell from top to bottom;
the grid is arranged on the insulator, and the cathode is fixed on the grid through a filament seat;
a first vacuum pump interface is arranged in a cavity between the upper part of the anode fixing disc and the top of the shell and connected with a first vacuum pump set;
the focusing coil and the scanning coil are arranged on the coil fixing disc and are arranged at the lower end of the anode fixing disc, and the carbon powder adsorption grid is arranged at the lower end of the coil fixing disc;
and a second vacuum pump interface is arranged in a cavity between the lower part of the carbon powder adsorption grid and the bottom of the shell and connected with a second vacuum pump set.
Further, the carbon powder adsorption grid comprises a positive grid mesh and a grounding grid mesh, the positive grid mesh is positioned above the grounding grid mesh and connected with the grounding grid mesh through a ceramic lantern ring, and a communicated beam channel is formed among the positive grid mesh, the grounding grid mesh and the ceramic lantern ring;
the positive grid mesh is electrically connected with a second direct-current power supply, the grounding grid mesh is connected with the shell and grounded, so that a second adsorption electrostatic field is formed between the positive grid mesh and the grounding grid mesh and is used for adsorbing carbon powder which is negatively charged and flows to the position between the carbon powder adsorption grid and the bottom of the shell.
Furthermore, the diameter of the beam channel is 40-60 mm, the size of the positive grid mesh is smaller than that of the grounding grid mesh, and the distance between the positive grid mesh and the grounding grid mesh is 3-5 mm;
and the positive grid mesh and the grounding grid mesh are respectively and uniformly provided with 1mm second adsorption holes, and the second adsorption holes on the positive grid mesh and the grounding grid mesh are distributed in a staggered manner.
Furthermore, the scanning coil is electrically connected with the scanning drive circuit and the industrial personal computer in sequence to form an electron beam scanning system;
the scanning coil comprises an X-direction scanning coil and a Y-direction scanning coil, the X-direction scanning coil is electrically connected with a waveform generation card in the industrial personal computer through an X-direction scanning driving circuit, and the Y-direction scanning coil is electrically connected with the waveform generation card in the industrial personal computer through a Y-direction scanning driving circuit.
Furthermore, two ends of the cathode are electrically connected with a filament heating power supply in a high-voltage power supply through a high-voltage cable, and the grid is electrically connected with a grid power supply in the high-voltage power supply through the high-voltage cable;
the focusing coil is electrically connected with the industrial personal computer through a focusing driving circuit;
the metal substrate passes through current sensor ground connection, just current sensor with electric connection has the shaping quality sampling circuit between the metal substrate, the other end of shaping quality sampling circuit with industrial computer electric connection, the industrial computer still with PLC system electric connection.
Furthermore, the workbench is an X-Y workbench, an infrared CCD system is installed inside the carbon powder adsorption cover, and the infrared CCD system is electrically connected with a display outside the vacuum chamber.
Further, the workbench is an X workbench, a platform tool is arranged on the workbench, and a raw material installation rotating shaft and a finished product installation rotating shaft are respectively installed on two sides of the platform tool;
the insulation board is installed on the platform tool, one end of the carbon polymer film is installed on the raw material installation rotating shaft, and the other end of the carbon polymer film is tightly attached to the metal substrate and wound by the finished product installation rotating shaft.
In conclusion, compared with the prior art, the invention has the following advantages:
(1) the carbon powder adsorption cover is arranged in the area of the graphene crystal film prepared by electron beam scanning in the vacuum chamber, so that carbon powder generated in the processing process can be adsorbed to the maximum extent, the pollution of the carbon powder generated in the processing process to a vacuum pump set and the vacuum chamber can be effectively prevented, and the service life of equipment is prolonged;
(2) the first vacuum pump set is arranged at the beam source section consisting of the cathode, the grid and the anode of the electron gun, and the second vacuum pump set and the carbon powder adsorption grid are arranged near the beam output port of the electron gun, so that the pollution of carbon powder generated in the process of preparing the graphene crystal film by electron beam scanning on the beam source section and other positions of the electron gun can be effectively prevented, the occurrence of discharge phenomenon is reduced, and the stable processing process is ensured;
(3) the number of graphene layers of the graphene crystal film prepared by electron beam scanning, the width of the graphene crystal prepared by single scanning, the thickness of a carbon polymer substrate and the like can be adjusted by adjusting parameters such as working voltage, beam size, scanning frequency, focusing current and the like, so that different application requirements are met;
(4) can carry out arbitrary pattern scanning preparation graphite alkene crystal film in the work area, also can the lapping preparation graphite alkene crystal film, can satisfy laboratory scientific research work demand, can satisfy large-scale mass production demand again.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments of the present invention will be briefly described below, and it is obvious that the drawings described below are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a schematic structural diagram of an apparatus for preparing a graphene crystal thin film by electron beam scanning according to an embodiment of the present invention.
Fig. 2 is a schematic view of the structure of the electron gun of fig. 1.
Fig. 3(a) is an isometric view of the carbon powder adsorption cap of fig. 1.
Fig. 3(b) is a partial sectional view of the carbon powder adsorption cap of fig. 1.
Fig. 4(a) is a plan view of the carbon powder adsorption grid of fig. 1.
Fig. 4(b) is a sectional view of the carbon powder adsorption grid of fig. 1.
Fig. 5 is a schematic view of the electron beam scanning system of fig. 1.
Fig. 6 is a schematic structural diagram of an apparatus for preparing a graphene crystal thin film by electron beam scanning according to another embodiment of the present invention.
In the figure: 1-an electron gun; 101-a cathode; 102-a gate; 103-an insulator; 104-an anode; 105-a first vacuum pump interface; 106-focusing coil; 107-scanning coils; 107a-X direction scanning coils; 107b-Y direction scanning coils; 108-a carbon powder adsorption grid; 1081-a positive grid; 1082-a ground grid; 1083-ceramic ferrule; 1084-beam channel; 109-a second vacuum pump interface; 110-anode fixed disk; 111-coil mounting plate; 112-a first vacuum pump set; 113-a second vacuum pump set; 114-an electron beam; 2-a high voltage power supply; 3-an industrial personal computer; 301-waveform generation card; 4-vacuum chamber; 401-a third vacuum pump set; a 5-X-Y stage; 6, insulating plates; 7-a metal substrate; 8-carbon polymer films; 9-carbon powder adsorption cover; 901-inner layer cover; 902-outer cover; 903-ceramic insulating block a; 904-ceramic insulation block b; 905-ceramic insulating block c; 906-ceramic insulating block d; 10-a current sensor; 11-a PLC system; 12-a shaped mass sampling circuit; 13-a scan drive circuit; 13a-X direction scan driving circuit; 13b-Y direction scan driving circuit; 14-focus drive circuit; 15-installing a rotating shaft on the raw material; 16-installing a rotating shaft on a finished product; 17-X stage; 18-a flat plate tool; 19-a high voltage cable; 20-a first direct current power supply; 21-a second direct current power supply; 22-infrared CCD system; 221-display.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following detailed description of the embodiments and the accompanying drawings are provided to illustrate the principles of the invention and are not intended to limit the scope of the invention, i.e., the invention is not limited to the embodiments described, but covers any modifications, alterations, and improvements in the parts, components, and connections without departing from the spirit of the invention.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Referring to fig. 1 to 5, the present invention provides an apparatus for preparing a graphene crystal thin film by electron beam scanning, including a vacuum chamber 4 and an electron gun 1 disposed on the top of the vacuum chamber 4, wherein a working table is disposed inside the vacuum chamber 4, an insulating plate 6 is disposed on the working table, a metal substrate 7 is disposed on the insulating plate 6, and a carbon polymer thin film 8 is disposed on the metal substrate 7;
a carbon powder adsorption cover 9 is covered in a region from the outer side of the carbon polymer film 8 to an electron beam output port at the top of the inner side of the vacuum chamber 4, the carbon powder adsorption cover 9 comprises an inner layer 901 and an outer layer 902, a plurality of insulating ceramic blocks are arranged between the inner layer 901 and the outer layer 902, the inner layer 901 is grounded, and the outer layer 902 is electrically connected with a first direct current power supply 20, so that a first adsorption electrostatic field is formed between the inner layer 901 and the outer layer 902 and is used for adsorbing carbon powder generated by the electron gun 1 in the process of preparing the graphene crystal film by electron beam scanning.
It should be clear that, in the present invention, the first dc power supply is +24V, the electron beam 114 output by the electron gun 1 passes through the carbon powder adsorption cover and hits on the carbon polymer thin film 8, and a scanning pattern is performed according to a predetermined track under the action of the internal magnetic field of the electron gun 1, so as to prepare a graphene crystal thin film.
Referring to fig. 3(a) and 3(b), the carbon powder adsorbing cover 9 is made of a non-magnetic metal material, and the structural size of the carbon powder adsorbing cover gradually decreases from the outer side of the carbon polymer film 8 to the electron beam output port at the top of the inner side of the vacuum chamber 4.
Specifically, in this embodiment, the carbon powder adsorption cover 9 has a rectangular pyramid structure, and a ceramic insulating block a903, a ceramic insulating block b904, a ceramic insulating block c905, and a ceramic insulating block d906 are disposed between the inner layer 901 and the outer layer 902. It will be appreciated that in other embodiments the carbon powder adsorption cap 9 may have other pyramidal or conical configurations, but it is ensured that its base surrounds the carbon polymer film 8.
In a preferred embodiment of the present invention, the inner layer 901 and the outer layer 902 are respectively and uniformly densely distributed with 1-3 mm first adsorption holes, and the first adsorption holes on the inner layer 901 and the outer layer 902 are distributed in a staggered manner, so as to have a better adsorption effect.
Referring to fig. 2, the electron gun 1 includes a housing, and a cathode 101, a grid 102, an insulator 103, an anode 104, an anode fixing plate 110, a focusing coil 106, a scanning coil 107, a coil fixing plate 111, and a carbon powder adsorption grid 108 are coaxially installed in the housing from top to bottom;
the grid 102 is mounted on the insulator 103, and the cathode 101 is fixed on the grid 102 through a filament holder;
a first vacuum pump interface 105 is arranged in a cavity between the upper part of the anode fixed disk 110 and the top of the shell, and the first vacuum pump interface 105 is connected with a first vacuum pump set 112 so as to ensure the vacuum degree of a beam source excitation space formed by the cathode 101, the grid 102 and the anode 104;
the focusing coil 106 and the scanning coil 107 are mounted on the coil fixing disc 111 and are mounted at the lower end of the anode fixing disc 110, and the carbon powder adsorption grid 108 is mounted at the lower end of the coil fixing disc 111;
and a second vacuum pump interface 109 is arranged in a cavity between the lower part of the carbon powder adsorption grid 108 and the bottom of the shell, and the second vacuum pump interface 109 is connected with a second vacuum pump group 113 and used for maintaining the vacuum degree of the beam output position of the electron gun 1.
In the present invention, the carbon powder adsorption gate 108 is used for adsorbing carbon powder generated during the process of preparing the graphene crystal thin film by electron beam scanning, so as to prevent the carbon powder from drifting to the beam source excitation space of the electron gun 1, which causes the discharge phenomenon of the electron gun 1.
Referring to fig. 4(a) and 4(b), the carbon powder adsorption grid 108 includes a positive grid 1081 and a ground grid 1082, the positive grid 1081 is located above the ground grid 1082, and the two are connected by a ceramic collar 1083, and a beam passage 1084 is formed among the positive grid 1081, the ground grid 1082 and the ceramic collar 1083;
the positive grid 1081 is electrically connected to a second dc power supply 21, and the ground grid 1082 is connected to the ground of the housing, so that a second electrostatic adsorption field is formed between the positive grid 1081 and the ground grid 1082, and the second electrostatic adsorption field is used for adsorbing the carbon powder which is negatively charged and flows to the space between the carbon powder adsorption grid 108 and the bottom of the housing.
In the present invention, the second dc power supply is +12V, and the second electrostatic field can make the carbon powder flowing to the position with negative charge adsorbed by the positive grid 1081, so as not to pollute other parts of the electron gun 1.
In a preferred embodiment of the present invention, the diameter of the beam passage 1084 is 40 to 60mm, the size of the positive grid 1081 is smaller than the size of the ground grid 1082, and the distance between the positive grid 1081 and the ground grid 1082 is 3 to 5 mm;
the positive grid 1081 and the ground grid 1082 are respectively and uniformly provided with 1mm second adsorption holes, and the second adsorption holes of the positive grid 1081 and the ground grid 1082 are distributed in a staggered manner, so as to achieve a better adsorption effect.
Referring to fig. 1 and 5, the scanning coil 107 is electrically connected to the scanning driving circuit 13 and the industrial personal computer 3 in sequence to form an electron beam scanning system;
the scanning coil 107 comprises an X-direction scanning coil 107a and a Y-direction scanning coil 107b, the X-direction scanning coil 107a is electrically connected with the waveform generation card 301 in the industrial personal computer 3 through an X-direction scanning driving circuit 13a, and the Y-direction scanning coil 107b is electrically connected with the waveform generation card 301 in the industrial personal computer 3 through a Y-direction scanning driving circuit 13 b.
It should be clear that, in the present invention, the waveform generation card 301 may output at least two waveforms, wherein one of the two paths transmits one waveform to the X-direction scan driving circuit 13a, and the other path transmits one waveform to the Y-direction scan driving circuit 13 b. The X-direction scanning drive circuit 13a and the Y-direction scanning drive circuit 13b are used to amplify the weak waveform signal of the waveform generation card 301 into a strong current signal for driving the X-direction scanning coil 107a and the Y-direction scanning coil 107 b. The waveform control program of the industrial personal computer 3 may set any waveform, and the waveform is amplified by the X-direction scanning driving circuit 13a and the Y-direction scanning driving circuit 13b and then respectively transmitted to the X-direction scanning coil 107a and the Y-direction scanning coil 107b, so as to generate an interaction magnetic field in an electron beam flow channel, and enable the electron beam 114 to scan any pattern on the surface of the carbon polymer film within a certain range.
Referring to fig. 1, two ends of the cathode 101 are electrically connected to the filament heating power source in the high voltage power source 2 through the high voltage cable 19, and the grid 102 is electrically connected to the grid power source in the high voltage power source 2 through the high voltage cable 19;
the focusing coil 106 is electrically connected with the industrial personal computer 3 through a focusing drive circuit 14;
the metal substrate 7 is grounded through a current sensor 10, the current sensor 10 is electrically connected with a forming quality sampling circuit 12 between the metal substrate 7, the other end of the forming quality sampling circuit 12 is electrically connected with the industrial personal computer 3, the industrial personal computer 3 is also electrically connected with a PLC (programmable logic controller) system 11, and the PLC system 11 controls the workbench to move according to preset logic according to a main program of the industrial personal computer 3.
It is clear that in the invention, the output current range of the filament heating power supply is 0-15A and is used for heating the filament and generating electrons, and the output range of the grid power supply voltage is 0-2000V and is used for adjusting the beam current. The high-voltage cable 19 comprises two conductors for heating the cathode 101 and a conductor for connecting the grid 102, wherein the conductors are mutually insulated, and the voltage resistance between the conductors is 8000V. The focusing drive circuit 14 adjusts the current of the focusing coil 106 according to a focusing current adjusting signal given by the industrial personal computer 3, so that the focal position of the electron beam is adjusted, and the energy distribution state of the beam spot of the electron beam 114 is adjusted.
The forming quality sampling circuit 12 is used for detecting the phenomenon that the substrate of the carbon polymer film 8 is burnt out in the processing process of preparing the graphene crystal film by electron beam scanning, when the forming quality sampling circuit 12 detects that the voltage signal detected by the current sensor 10 is high, the phenomenon that the substrate of the carbon polymer film 8 is burnt out is judged to occur, the signal is transmitted to the industrial personal computer 3, and the main program of the industrial personal computer 3 adjusts an electron beam scanning strategy to avoid the phenomenon that the substrate of the carbon polymer film 8 is burnt out.
Further, the vacuum chamber 4 is connected to a third vacuum pump group 401 through a vacuum pipe, and the third vacuum pump group 401 is used for maintaining a vacuum environment in the vacuum chamber 4.
Specifically, the industrial personal computer 3 is connected with the high-voltage power supply 2, an RS485 communication interface is adopted to transmit acceleration voltage, filament heating current, a grid voltage set value and a start/stop signal to the high-voltage power supply 2, and meanwhile, the high-voltage power supply 2 feeds the acceleration voltage, the filament heating current and a beam sampling value back to the industrial personal computer 3 for a man-machine interaction system.
In conclusion, compared with the prior art, the invention has the following advantages:
(1) the carbon powder adsorption cover 9 is arranged in the area of the graphene crystal film prepared by electron beam scanning in the vacuum chamber 4, so that carbon powder generated in the processing process can be adsorbed to the maximum extent, the pollution of the carbon powder generated in the processing process to the vacuum pump set and the vacuum chamber 4 can be effectively prevented, and the service life of equipment is prolonged;
(2) a first vacuum pump set 112 is arranged at a beam source section consisting of a cathode 101, a grid 102 and an anode 104 of the electron gun 1, and a second vacuum pump set 113 and a carbon powder adsorption grid 108 are arranged near a beam output port of the electron gun 1, so that the pollution of carbon powder generated in the process of preparing a graphene crystal film by scanning an electron beam 114 to the beam source section and other positions can be effectively prevented, the occurrence of discharge phenomenon is reduced, and the stable processing process is ensured;
(3) the number of graphene layers of the graphene crystal film prepared by electron beam scanning, the width of the graphene crystal prepared by single scanning, the thickness of a carbon polymer substrate and the like can be adjusted by adjusting parameters such as working voltage, beam size, scanning frequency, focusing current and the like, so that different application requirements are met;
(4) can carry out arbitrary pattern scanning preparation graphite alkene crystal film in the work area, also can the lapping preparation graphite alkene crystal film, can satisfy laboratory scientific research work demand, can satisfy large-scale mass production demand again.
Example 1
Referring to fig. 1, the workbench is an X-Y workbench 5, an infrared CCD system 22 is installed inside the carbon powder adsorption cover 9, the infrared CCD system 22 is electrically connected to a display 221 outside the vacuum chamber 4, and the infrared CCD system 22 and the display 221 are used for observing the preparation state of the graphene crystal film and adjusting the graphene preparation work area so that an operator can observe the state of the work area.
In this embodiment, the detailed working process is as follows:
firstly, opening an X-Y workbench 5 out of a vacuum chamber 4, laying an insulating plate 6 on the X-Y workbench 5, then laying a metal substrate 7, connecting the metal substrate 7 with a current sensor 10, and covering a carbon polymer film 8 on the metal substrate 7;
step two, opening the X-Y workbench 5 on which the metal substrate 7 and the carbon polymer film 8 are laid into the vacuum chamber 4, closing the door of the vacuum chamber 4, observing the state of a processing area through the infrared CCD system 22, and adjusting the position of the X-Y workbench 5 to enable the carbon polymer film area needing to be processed to be covered in the carbon powder adsorption cover 9;
step three, starting a first vacuum pump group 112, a second vacuum pump group 113 and a third vacuum pump group 401;
detecting whether the vacuum degrees of the electron gun 1 and the vacuum chamber 4 reach the set requirement or not, and continuing to vacuumize the electron gun 1 and the vacuum chamber 4 if the vacuum degrees of the electron gun 1 and the vacuum chamber 4 do not reach the set requirement;
step five, the vacuum degrees of the electron gun 1 and the vacuum chamber 4 reach the set requirement, and the system work main program transmits the preset focusing current parameter to the focusing drive circuit 14 through the industrial personal computer 3, so that the focusing coil 106 loads the preset focusing current;
step six, a system working main program transmits the accelerating voltage, the filament heating current and the grid voltage set value to the high-voltage power supply 2 through an RS485 communication interface of the industrial personal computer 3 and the high-voltage power supply 2; the setting range of the accelerating voltage is-20 kV to-30 kV, the setting range of the heating current of the filament is 7A to 15A, and the setting value of the beam current is 2mA to 3 mA;
step seven, calling a preset scanning pattern by a system working main program, decomposing the preset scanning pattern into X-direction and Y-direction scanning waveforms, transmitting the X-direction and Y-direction scanning waveforms to the waveform generation card 301, amplifying current signals respectively by the X-direction scanning driving circuit 13a and the Y-direction scanning driving circuit 13b, and transmitting the current signals respectively to the X-direction scanning coil 107a and the Y-direction scanning coil 107 b; starting the high-voltage power supply 2 at the same time, outputting an electron beam 114 by the electron gun 1, and enabling the electron beam 114 to start scanning a pattern according to a preset track by a magnetic field generated by a scanning coil;
step eight, detecting whether the scanning pattern of the preset track is finished or not by a system working main program, not finishing continuous scanning, detecting a signal of the forming quality detection circuit 12 by the main program in the industrial personal computer 3 in the scanning process of the electron beam 114, judging that the burning loss phenomenon of the carbon polymer film 8 occurs in the scanning process of the electron beam 114 when detecting that an input signal of the forming quality detection circuit 12 is high level, and avoiding further damaging the substrate of the carbon polymer film 8 in the next scanning process by defocusing or beam current reduction;
step nine, after the scanning of the preset pattern is finished, the main program closes the output of the high-voltage power supply 2, the beam output of the electron gun 1 is turned off, and meanwhile, the input of the X-direction scanning driving circuit 13a and the input of the Y-direction scanning driving circuit 13b are both zero;
step ten, detecting whether other areas on the surface of the carbon polymer film 8 need to be processed and other areas need to be processed, controlling the X-Y workbench 5 to move by the industrial personal computer 3 through the PLC system 11 and observing through the infrared CCD system 22, so that the output position of the electron beam 114 is just opposite to the origin of coordinates of the areas needing to be scanned;
step eleven, repeating the step six to the step ten;
step twelve, when no other area on the surface of the carbon polymer film 8 needs to be processed, the system working main program sets the accelerating voltage, the filament heating current and the grid voltage to be zero through an RS485 communication interface of the industrial personal computer 3 and the high-voltage power supply 2;
step thirteen, deflating the vacuum chamber 4, opening a large door of the vacuum chamber 4, opening the X-Y workbench 5, and taking out the prepared graphene crystal film;
fourteenth, whether the graphene crystal film needs to be prepared again or not is judged, if yes, the metal substrate 7 on the X-Y workbench 5 is cleaned, and the metal substrate 7 is covered with the carbon polymer film 8; repeating the second step to the third step;
and step fifteen, otherwise, closing all the vacuum pump sets, closing the industrial personal computer 3 and other systems, and finishing the work.
Example 2
Referring to fig. 6, the workbench is an X workbench 17, a platform tool 18 is arranged on the X workbench 17, and a raw material installation rotating shaft 15 and a finished product installation rotating shaft 16 are respectively installed on two sides of the platform tool 18;
the insulation board 6 is installed on the platform tool 18, one end of the carbon polymer film 8 is installed on the raw material installation rotating shaft 15, and the other end of the carbon polymer film is tightly attached to the metal substrate 7 and wound by the finished product installation rotating shaft 16.
In this embodiment, the detailed working process is as follows:
step one, opening an X workbench 17 out of a vacuum chamber 4, installing a platform tool 18 on the X workbench 17, placing a metal substrate 7 on the platform tool 18, and connecting the metal substrate with a current sensor 10; mounting a raw material mounting rotating shaft 15 and a finished product mounting rotating shaft 16 on two sides of a platform tool 18;
secondly, mounting the wound carbon polymer film 8 on the raw material mounting rotating shaft 15, wherein the width of the wound carbon polymer film 8 is more than 200mm, the length of the wound carbon polymer film is set to be different from ten meters to tens of meters according to the process requirement, laying the wound carbon polymer film 8 close to the metal substrate 7, pre-winding the finished product mounting rotating shaft 16 for a plurality of turns, and ensuring that the carbon polymer film 8 fed by the raw material mounting rotating shaft 15 synchronously and rotatably can be wound when the finished product mounting rotating shaft 16 rotates;
step three, opening the X workbench 17 for installing the wound carbon polymer film 8 into the vacuum chamber 4, covering the carbon polymer film 8 area to be processed in the carbon powder adsorption cover 9, and closing the gate of the vacuum chamber 4;
step four, starting a first vacuum pump group 112, a second vacuum pump group 113 and a third vacuum pump group 401;
step five, detecting whether the vacuum degrees of the electron gun 1 and the vacuum chamber 4 reach the set requirement, and continuously vacuumizing the electron gun 1 and the vacuum chamber 4 when the vacuum degrees of the electron gun 1 and the vacuum chamber 4 do not reach the set requirement;
step six, the vacuum degrees of the electron gun 1 and the vacuum chamber 4 reach the set requirement, and the system work main program transmits the preset focusing current parameter to the focusing drive circuit 14 through the industrial personal computer 3, so that the focusing coil 106 loads the preset focusing current;
seventhly, transmitting an accelerating voltage, a filament heating current and a grid voltage set value to the high-voltage power supply 2 through an RS485 communication interface of the industrial personal computer 3 and the high-voltage power supply 2, wherein the accelerating voltage is set within a range of-20 kV to-30 kV, the filament heating current is set within a range of 7A to 15A, and the beam current set value is 2mA to 3 mA;
step eight, the system working main program sets the X-direction scanning waveform and the Y-direction scanning wave as sawtooth waves, the frequency of the Y-direction scanning wave is 1kHz, the Y-direction current amplitude is set according to the maximum scanning area required, the X-direction scanning period is obtained by calculation according to the Y-direction scanning frequency and the X-direction scanning length, the system working main program transmits the set X-direction scanning waveform and the set Y-direction scanning wave to a waveform generation card, and then the X-direction scanning drive circuit 13a and the Y-direction scanning drive circuit 13b respectively transmit the current signals to an X-direction scanning coil 107a and a Y-direction scanning coil 107b after amplifying the current signals; simultaneously starting the high-voltage power supply 2, outputting an electron beam 114 by the electron gun 1, and enabling the electron beam 114 to scan the surface of the carbon polymer film 8 line by line along the moving direction of the X workbench 17 by a magnetic field generated by the scanning coil 107;
step nine, a main program of system work detects whether one cycle of the X-direction scanning waveform is finished or not, continuous scanning is not finished, in the scanning process of the electron beam 114, the main program in the industrial personal computer 3 detects a signal of the forming quality detection circuit 12, when the input signal of the forming quality detection circuit 12 is detected to be high level, the burning loss phenomenon of the carbon polymer film 8 is judged to occur in the scanning process of the electron beam, and the substrate of the carbon polymer film 8 is prevented from being further damaged in the next scanning process by defocusing or beam current reduction;
step ten, when the scanning of the X-direction scanning waveform in one period is finished, the main program closes the output of the high-voltage power supply 2, the beam output of the electron gun 1 is cut off, and simultaneously the inputs of the X-direction scanning driving circuit 13a and the Y-direction scanning driving circuit 13b are both zero;
step eleven, sending a synchronous equidirectional rotating instruction of the raw material installation rotating shaft 15 and the finished product installation rotating shaft 16 to the PLC system 11 through an interface circuit of the industrial personal computer 3 and the PLC system 11 by a working main program, and controlling the finished product installation rotating shaft 16 to rotate by the PLC system 11 so as to enable the prepared graphene crystal film to be wound on the finished product installation rotating shaft 16; meanwhile, the PLC system 11 controls the raw material installation rotating shaft to rotate 15, and the carbon polymer film 8 of which the graphene crystal film needs to be prepared is laid on the metal substrate 7; the rotating speed, the action time and the size of the overlapping area of the graphene crystal thin film prepared in the two times can be obtained through early process tests;
step twelve, repeating the step eight to the step eleven;
thirteen, when the graphene crystal film wound by the finished product installation rotating shaft 16 reaches the maximum amount or no carbon polymer film which can be reprocessed is arranged on the raw material installation rotating shaft 15, the system work main program sets the accelerating voltage, the filament heating current and the grid voltage to be zero through an RS485 communication interface of the industrial personal computer 3 and the high-voltage power supply 2;
step fourteen, deflating the vacuum chamber 4, opening the gate of the vacuum chamber 4, opening the X workbench 17, and taking out the prepared graphene crystal film;
fifteenth, whether the graphene crystal film needs to be prepared again or not, if so, cleaning the metal substrate 7 on the X workbench 17, checking whether the raw material installation rotating shaft 15 needs to reload the coiled carbon polymer film or not, reloading if necessary, laying the coiled carbon polymer film close to the metal substrate 7, pre-winding the finished product installation rotating shaft 16 for several turns, and ensuring that the carbon polymer film fed by the raw material installation rotating shaft 15 in a synchronous rotating manner can be wound when the finished product installation rotating shaft 16 rotates; repeating the steps three to fourteen again.
And sixthly, otherwise, closing all the vacuum pump sets, closing the industrial personal computer 3 and other systems, and finishing the work.
It should be understood that the embodiments described herein are described in a progressive manner, and the same or similar parts in the embodiments are referred to each other, and each embodiment is described with emphasis on being different from the other embodiments. For embodiments of the method, reference is made to the description of the apparatus embodiments in part. The present invention is not limited to the specific steps and structures described above and shown in the drawings. Also, a detailed description of known process techniques is omitted herein for the sake of brevity.
The above description is only an example of the present application and is not limited to the present application. Various modifications and alterations to this application will become apparent to those skilled in the art without departing from the scope of this invention. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. A device for preparing a graphene crystal film by electron beam scanning comprises a vacuum chamber and an electron gun arranged at the top of the vacuum chamber, and is characterized in that a workbench is arranged inside the vacuum chamber, an insulating plate is arranged on the workbench, a metal substrate is arranged on the insulating plate, and a carbon polymer film is arranged on the metal substrate;
the carbon polymer film outside to the regional cage of electron beam current delivery outlet at the inboard top in vacuum chamber has the carbon dust to adsorb the cover, the carbon dust adsorbs the cover and includes inlayer and skin, be equipped with a plurality of insulating ceramic blocks between inlayer and the skin, inlayer ground connection, skin and first direct current power electric connection, so that form first absorption electrostatic field between inlayer and the skin, this first absorption electrostatic field is used for adsorbing the carbon dust that electron beam scanning preparation graphite alkene crystal film in-process produced.
2. The device for preparing the graphene crystal thin film by electron beam scanning according to claim 1, wherein the carbon powder adsorption cover is made of a non-magnetic metal material, and the structural size of the carbon powder adsorption cover is gradually reduced from the outer side of the carbon polymer thin film to an electron beam output port at the top of the inner side of the vacuum chamber.
3. The device for preparing the graphene crystal thin film by electron beam scanning according to claim 1, wherein the first adsorption holes of 1-3 mm are uniformly and densely distributed on the inner layer and the outer layer respectively, and the first adsorption holes on the inner layer and the outer layer are distributed in a staggered manner.
4. The device for preparing the graphene crystal film by electron beam scanning according to claim 1, wherein the electron gun comprises a shell, and a cathode, a grid, an insulator, an anode fixing disc, a focusing coil, a scanning coil, a coil fixing disc and a carbon powder adsorption gate are coaxially arranged in the shell from top to bottom in sequence;
the grid is arranged on the insulator, and the cathode is fixed on the grid through a filament seat;
a first vacuum pump interface is arranged in a cavity between the upper part of the anode fixing disc and the top of the shell and connected with a first vacuum pump set;
the focusing coil and the scanning coil are arranged on the coil fixing disc and are arranged at the lower end of the anode fixing disc, and the carbon powder adsorption grid is arranged at the lower end of the coil fixing disc;
and a second vacuum pump interface is arranged in a cavity between the lower part of the carbon powder adsorption grid and the bottom of the shell and connected with a second vacuum pump set.
5. The device for preparing the graphene crystal thin film by electron beam scanning according to claim 4, wherein the carbon powder adsorption grid comprises a positive grid mesh and a grounding grid mesh, the positive grid mesh is positioned above the grounding grid mesh and is connected with the grounding grid mesh through a ceramic lantern ring, and a communicated beam channel is formed among the positive grid mesh, the grounding grid mesh and the ceramic lantern ring;
the positive grid mesh is electrically connected with a second direct-current power supply, the grounding grid mesh is connected with the shell and grounded, so that a second adsorption electrostatic field is formed between the positive grid mesh and the grounding grid mesh and is used for adsorbing carbon powder which is negatively charged and flows to the position between the carbon powder adsorption grid and the bottom of the shell.
6. The device for preparing the graphene crystal thin film by electron beam scanning according to claim 5, wherein the diameter of the beam channel is 40-60 mm, the size of the positive grid is smaller than that of the grounding grid, and the distance between the positive grid and the grounding grid is 3-5 mm;
and the positive grid mesh and the grounding grid mesh are respectively and uniformly provided with 1mm second adsorption holes, and the second adsorption holes on the positive grid mesh and the grounding grid mesh are distributed in a staggered manner.
7. The device for preparing the graphene crystal film by electron beam scanning according to claim 4, wherein the scanning coil is electrically connected with a scanning driving circuit and an industrial personal computer in sequence to form an electron beam scanning system;
the scanning coil comprises an X-direction scanning coil and a Y-direction scanning coil, the X-direction scanning coil is electrically connected with a waveform generation card in the industrial personal computer through an X-direction scanning driving circuit, and the Y-direction scanning coil is electrically connected with the waveform generation card in the industrial personal computer through a Y-direction scanning driving circuit.
8. The apparatus for preparing graphene crystal thin film according to claim 7, wherein two ends of the cathode are electrically connected to a filament heating power supply in a high voltage power supply through a high voltage cable, and the grid is electrically connected to a grid power supply in the high voltage power supply through the high voltage cable;
the focusing coil is electrically connected with the industrial personal computer through a focusing driving circuit;
the metal substrate passes through current sensor ground connection, just current sensor with electric connection has the shaping quality sampling circuit between the metal substrate, the other end of shaping quality sampling circuit with industrial computer electric connection, the industrial computer still with PLC system electric connection.
9. The device for preparing the graphene crystal film by electron beam scanning according to any one of claims 1 to 8, wherein the workbench is an X-Y workbench, an infrared CCD system is installed inside the carbon powder adsorption cover, and the infrared CCD system is electrically connected with a display outside the vacuum chamber.
10. The device for preparing the graphene crystal thin film by electron beam scanning according to any one of claims 1 to 8, wherein the workbench is an X workbench, a platform tool is arranged on the workbench, and a raw material mounting rotating shaft and a finished product mounting rotating shaft are respectively mounted on two sides of the platform tool;
the insulation board is installed on the platform tool, one end of the carbon polymer film is installed on the raw material installation rotating shaft, and the other end of the carbon polymer film is tightly attached to the metal substrate and wound by the finished product installation rotating shaft.
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| CN110980704A (en) * | 2019-12-30 | 2020-04-10 | 中国科学院合肥物质科学研究院 | Electron beam induced patterned graphene and preparation method thereof |
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| CN107039123A (en) * | 2017-05-04 | 2017-08-11 | 辽宁科技大学 | A kind of electrostatic Laser Desorption graphene technology prepares carbon-coated aluminum foils device and method |
| CN109573990A (en) * | 2019-01-21 | 2019-04-05 | 广东工业大学 | A method of quickly preparing patterning doped graphene by ultraviolet laser |
| CN110838427A (en) * | 2019-11-20 | 2020-02-25 | 中国航空制造技术研究院 | Electronic gun device for fuse wire additive manufacturing |
| CN110759338A (en) * | 2019-12-04 | 2020-02-07 | 广东工业大学 | Method for preparing large-size graphene based on laser fixed-point processing |
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