CN106653520B - A kind of field emission cold-cathode and its manufacturing method - Google Patents
A kind of field emission cold-cathode and its manufacturing method Download PDFInfo
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- CN106653520B CN106653520B CN201611124177.8A CN201611124177A CN106653520B CN 106653520 B CN106653520 B CN 106653520B CN 201611124177 A CN201611124177 A CN 201611124177A CN 106653520 B CN106653520 B CN 106653520B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J19/00—Details of vacuum tubes of the types covered by group H01J21/00
- H01J19/02—Electron-emitting electrodes; Cathodes
- H01J19/24—Cold cathodes, e.g. field-emissive cathode
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J35/00—X-ray tubes
- H01J35/02—Details
- H01J35/04—Electrodes ; Mutual position thereof; Constructional adaptations therefor
- H01J35/06—Cathodes
- H01J35/065—Field emission, photo emission or secondary emission cathodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/022—Manufacture of electrodes or electrode systems of cold cathodes
- H01J9/025—Manufacture of electrodes or electrode systems of cold cathodes of field emission cathodes
Abstract
A kind of manufacturing method of field-transmitting cathode, which comprises electrically-conductive backing plate is provided；The graphene coated nanometer sheet on the electrically-conductive backing plate；Hexagonal boron nitride nanosheet is deposited on the graphene nanometer sheet surface.Pass through nanometer sheet graphene coated on electrically-conductive backing plate, hexagonal boron nitride nanosheet is deposited on the surface of the graphene nanometer sheet, so that forming stable composite nanostructure between hexagonal boron nitride nanosheet and graphene nanometer sheet, reduce the work function of graphene, increase the local electric field of graphene surface, to be substantially reduced the threshold electric field of cathode, its emission current is improved.Also, hexagonal boron nitride nanosheet part prevents graphene to be improved the launch stability of cathode by the bombardment of cation.
Description
Technical field
The invention belongs to vacuum electron device field more particularly to a kind of field emission cold-cathode and its manufacturing methods.
Background technique
Vacuum electron device, such as microwave tube, X-ray tube, electronics promote and Charge control devices, is communication, space skill
Critical component in the fields such as art, safety detection, imaging of medical.The core component of vacuum electron device is cathode, main at present
Using metal hot cathode.However, metal hot cathode body product is big, heat radiation power consumption is big, the opening time is long, material under high temperature is steamed
The defects of hair, limits vacuum electron device to micromation and integrated direction development.
In recent years, the field emission cold cathode based on various one-dimensional/two-dimension nano materials has obtained domestic and international researcher
Tunneling effect can occur under electric field action for extensive concern and research, the electronics on nanoscale tip, theoretically can be with shape
At great electric current.For example, two-dimentional carbon nanomaterial graphene has huge dimensional thickness than the edge knot with abundant prosperity
Structure can be used as effective electron emission address, along with its excellent conductive characteristic and thermal conduction characteristic and highly stable
Mechanochemistry performance, be one of very promising Flied emission nano material.Compared to hot cathode, field-transmitting cathode has room
The advantages such as warm work, quick response, low-power consumption, Miniaturized, can optimize structure applied to vacuum electron device, obtain excellent
Power and frequency characteristic.However, existing nano material field-transmitting cathode, there are emission current and current density are small, transmitting is steady
The problems such as qualitative difference, is unable to satisfy the requirement of high performance device application.
Summary of the invention
The purpose of the present invention is to provide a kind of manufacturing methods of field-transmitting cathode, to solve nano material in the prior art
Field-transmitting cathode the problems such as there are emission current and current density are small, and launch stability is poor, it is unable to satisfy high performance device application
Requirement the problem of.
In a first aspect, the embodiment of the invention provides a kind of manufacturing methods of field-transmitting cathode, which comprises
Electrically-conductive backing plate is provided；
The graphene coated nanometer sheet on the electrically-conductive backing plate；
Hexagonal boron nitride nanosheet is deposited on the graphene nanometer sheet surface.
With reference to first aspect, described to be applied on the electrically-conductive backing plate in the first possible implementation of first aspect
Covering graphene nanometer sheet step includes:
The graphene nanometer sheet is coated in the electrically-conductive backing plate by the method for electrophoretic deposition, or passes through microwave etc.
The graphene nanometer sheet is coated in the electrically-conductive backing plate by the method that gas ions increase chemical vapor deposition.
The possible implementation of with reference to first aspect the first, in second of possible implementation of first aspect, institute
It states and includes: coated in the electrically-conductive backing plate step by the graphene nanometer sheet by the method for electrophoretic deposition
It configures graphene electrophoresis liquid: graphene nanometer sheet and soluble metal inorganic salts being added in organic solvent, passed through
Ultrasonic disperser is dispersed；
It is put into the graphene electrophoresis liquid using the electrically-conductive backing plate as cathode and anode, in the cathode and anode
It is connected to power supply energization, deposits the graphene nanometer sheet in the electrically-conductive backing plate of the cathode.
The possible implementation of second with reference to first aspect, in the third possible implementation of first aspect, institute
The voltage for stating power supply is 100-200V, and the time deposited in graphene electrophoresis liquid is 1-10 minutes.
The possible implementation of with reference to first aspect the first, in the 4th kind of possible implementation of first aspect, institute
It states and the graphene nanometer sheet is coated in by the electrically-conductive backing plate by the method that microwave plasma increases chemical vapor deposition
Step specifically:
The electrically-conductive backing plate for being coated with catalyst metal layer is put into quartz container, and institute is heated under protective gas atmosphere environment
Electrically-conductive backing plate is stated to predetermined temperature and continues the first duration, then is passed through the second duration of mixed gas reaction of acetylene and hydrogen,
It is generated on the electrically-conductive backing plate and obtains graphene nanometer sheet.
The 4th kind of possible implementation with reference to first aspect, in the 5th kind of possible implementation of first aspect, institute
State catalyst metal layer be nickel layer, cobalt layers or iron layer, the catalyst metal layer with a thickness of 100-300 nanometers.
The 4th kind of possible implementation with reference to first aspect, in the 5th kind of possible implementation of first aspect, institute
Stating predetermined temperature is 700-900 degrees Celsius, and described first when is 10-30 minutes a length of, and described second when is 2-10 minutes a length of.
With reference to first aspect, described in the graphene nanometer sheet in the 5th kind of possible implementation of first aspect
Surface deposits hexagonal boron nitride nanosheet step
It disperses the hexagonal boron nitride nanosheet in alcohol solvent, by way of spin coating, spraying or dipping, in institute
State graphene nanometer sheet surface deposition hexagonal boron nitride nanosheet.
Second aspect, the embodiment of the invention provides a kind of field-transmitting cathode, the field-transmitting cathode includes:
Conductive substrate；
Graphene nanometer sheet coated on the conductive substrate surface；
And it is distributed in the hexagonal boron nitride nanosheet on the graphene nanometer sheet surface.
In conjunction with second aspect, in the first possible implementation of second aspect, the conductive substrate be iron, titanium, copper,
Chromium, cobalt, nickel, tungsten, molybdenum, gold or platinum substrate, or to be plated with the metals such as iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold, platinum
The insulating substrate of conductive coating.
In the present invention, the graphene coated nanometer sheet on electrically-conductive backing plate deposits on the surface of the graphene nanometer sheet
Hexagonal boron nitride nanosheet, so that forming stable composite Nano knot between hexagonal boron nitride nanosheet and graphene nanometer sheet
Structure reduces the work function of graphene, increases the local electric field of graphene surface, to be substantially reduced the unlatching electricity of cathode
, improve its emission current.Also, hexagonal boron nitride nanosheet part prevents graphene by the bombardment of cation, improves
The launch stability of cathode.
Detailed description of the invention
Fig. 1 is the implementation flow chart of the manufacturing method of field-transmitting cathode provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The purpose of the embodiment of the present invention is to propose a kind of new field-transmitting cathode and its manufacturing method, to solve existing skill
The field-transmitting cathode of nano material in art the problems such as there are emission current and current density are small, and launch stability is poor, Wu Faman
The requirement of sufficient high performance device application.With reference to the accompanying drawing, the present invention is further illustrated.
Fig. 1 shows the implementation process of the manufacturing method of the field-transmitting cathode of first embodiment of the invention offer, is described in detail such as
Under:
In step s101, electrically-conductive backing plate is provided.
Specifically, the electrically-conductive backing plate, it can be in the metal substrates such as iron, titanium, copper, chromium, cobalt, nickel, tungsten, molybdenum, gold, platinum
One or more, or the insulation base for the metallic conductions coating such as be plated with iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold or platinum
Plate.The electrically-conductive backing plate, can be according to the coating method of graphene nanometer sheet, really for being formed on its surface graphene nano lamella
Surely the material for the metal selected.For example it is coated according to electrophoretic deposition or microwave plasma enhanced chemical vapour deposition technique
The graphene nanometer sheet, selection ensure the metallic conduction substrate that coating method can effectively be implemented.
The insulating substrate can be one or more of glass, ceramics, silicon wafer etc..The insulating substrate surface
Metal coating, can use magnetron sputtering, electron beam evaporation, at least one of vapour deposition process or electroless plating method are plated
It covers.
In step s 102, the graphene coated nanometer sheet on the electrically-conductive backing plate.
Specifically, the coating of the graphene nanometer sheet, can use electrophoretic deposition or plasma enhanced chemical
Vapour deposition process is illustrated separately below.
1, electrophoretic deposition:
Firstly, it is necessary to graphene electrophoresis solution is prepared, it can be by graphene nanometer sheet and soluble metal inorganic salts (charge
Additive) it is added in organic solvent according to scheduled ratio, ultrasonic disperse can be carried out by supersonic generator.The ultrasound
The ultrasound works duration of wave disperser can be 1~3 hour, so as to obtain uniform and stable graphene electrophoresis solution.
Organic solvent used can be one of ethyl alcohol, acetone or isopropanol etc..Metal inorganic salt used can be nitre
Sour magnesium Mg (NO3)2, magnesium chloride Mg Cl2, aluminum nitrate Al (NO3)3, aluminium chloride AlCl3, nickel chloride NiCl2Or nickel nitrate Ni (NO3)2
Deng.
Wherein, the graphene nanometer sheet can be prepared using the method (Hummer method) of graphite oxidation reduction.Institute
Stating graphene nanometer sheet can be the graphene nanometer sheet of single-layer or multi-layer.The lateral dimension of the graphene nanometer sheet is preferably
1-10μm.The concentration of the mixed liquor of the organic solvent can be 0.1-10mg/ml, in order to improve point of graphene in the solution
Dissipate property, preferably 0.1-1mg/ml.
After obtaining graphene electrophoresis liquid, using electrically-conductive backing plate as cathode, another electrically-conductive backing plate is separately connected as anode
The electrically-conductive backing plate is put into graphene electrophoresis liquid by the cathode and anode of DC power supply, under the action of the DC voltage, positively charged
The graphene nanometer sheet of lotus is mobile to cathode direction, is deposited on electrically-conductive backing plate, obtains graphene layer.The item of the deposition process
Part is preferred are as follows: voltage 100-200V, for example can select electrophoretic voltage is 150V, 180V etc..The duration of the electrophoresis can be
1-10min, for example can select 3 minutes, 5 minutes, 8 minutes etc..
2, plasma reinforced chemical vapour deposition method:
The electrically-conductive backing plate that can be coated with catalyst metal layer is put into quartz container, such as can be in quartz ampoule.
Under protective gas atmosphere environment, such as can be under Ar plasma atmosphere environment, to heat the substrate to reaction temperature, heat preservation the
One duration.Then, it is passed through acetylene (C2H2) and hydrogen (H2) mixed gas, grow the graphene nanometer sheet that is vertically arranged.
After the second duration, reaction terminates, and can be protected down, is cooled to room temperature by argon gas.
Wherein, the catalyst metal layer can be nickel layer, Co layers of cobalt or Fe layers of iron.The catalyst metal layer
Thickness can choose as 100-300nm, for example can choose is 150 nanometers, 200 nanometers or 250 nanometers etc..
In addition, in embodiments of the present invention, the microwave power for generating Ar plasma can be 500-1000W, institute
It can be 700-900 DEG C with reaction temperature, for example can be 750 degree, 800 degree, 850 degree etc..First duration can be 10-
30min, for example be specifically as follows 15 minutes, 20 minutes or 25 minutes etc..
Wherein, the range of the ratio (H2/C2H2) of the hydrogen and acetylene can be 5-10.Such as the ratio of hydrogen and acetylene
Example can be 6 to 1,7 to 1,8 to 1 or 9 to 1 etc..Reaction pressure range in the atmosphere of the acetylene and hydrogen can be 5-
10 supports, including such as 6 supports, 7 supports, 8 supports or 9 supports.Growth time in the atmosphere of the acetylene and hydrogen can be 2-
10min, such as 5 minutes or 7 minutes etc..
In step s 103, hexagonal boron nitride nanosheet is deposited on the graphene nanometer sheet surface
Wherein, the hexagonal boron nitride nanosheet can be by way of mechanical or ultrasound, from hexagonal boron nitride crystal
Middle removing obtains.The hexagonal boron nitride nanosheet can be the hexagonal boron nitride nanosheet of single layer, or the six of multilayer
Square boron nitride nanosheet.The hexagonal boron nitride nanosheet preferentially selects hexagonal boron nitride of its lateral dimension less than 200 nanometers
Nanometer sheet.
The deposition process of the hexagonal boron nitride nanosheet includes: that hexagonal boron nitride nanosheet is well-dispersed in ethyl alcohol is molten
In agent, such as can be in such a way that ultrasonic wave disperses.Then the method for passing through spin coating, spraying or dipping, in graphene nano
Piece surface deposits hexagonal boron nitride nanosheet, forms compound field emission cathode structure.
The present invention graphene coated nanometer sheet on electrically-conductive backing plate deposits six side's nitrogen on the surface of the graphene nanometer sheet
Change boron nanometer sheet, so that forming stable composite nanostructure between hexagonal boron nitride nanosheet and graphene nanometer sheet, reduces
The work function of graphene, increases the local electric field of graphene surface, to be substantially reduced the threshold electric field of cathode, improves it
Emission current.Also, hexagonal boron nitride nanosheet part prevents graphene to be improved the hair of cathode by the bombardment of cation
Penetrate stability.
In addition, the embodiment of the invention also provides a kind of field-transmitting cathode of nano material, the field-transmitting cathode includes:
Conductive substrate；
Graphene nanometer sheet coated on the conductive substrate surface；
And it is distributed in the hexagonal boron nitride nanosheet on the graphene nanometer sheet surface.
Wherein, the conductive substrate is iron, titanium, copper, chromium, cobalt, nickel, tungsten, molybdenum, gold or platinum substrate, or is plating
There is the insulating substrate of the metallic conductions coating such as iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold, platinum.The insulating substrate, can be glass
One or more of glass, ceramics, silicon wafer etc..The metal coating on the insulating substrate surface can use magnetron sputtering, electricity
Beamlet evaporation, at least one of vapour deposition process or electroless plating method carry out plating.
The graphene nanometer sheet can be prepared using the method (Hummer method) of graphite oxidation reduction.The stone
Black alkene nanometer sheet can be the graphene nanometer sheet of single-layer or multi-layer.The lateral dimension of the graphene nanometer sheet is preferably 1-10
μm。
The hexagonal boron nitride nanosheet preferentially selects hexagonal boron nitride nanosheet of its lateral dimension less than 200 nanometers,
It specifically refers to length, width of hexagonal boron nitride nanosheet etc. and is no more than 200 nanometers.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of manufacturing method of field-transmitting cathode, which is characterized in that the described method includes:
Electrically-conductive backing plate is provided；
The graphene coated nanometer sheet on the electrically-conductive backing plate；
Hexagonal boron nitride nanosheet is deposited on the graphene nanometer sheet surface.
2. method according to claim 1, which is characterized in that the nanometer sheet step graphene coated on the electrically-conductive backing plate
Suddenly include:
The graphene nanometer sheet is coated in the electrically-conductive backing plate by the method for electrophoretic deposition, or passes through microwave plasma
The graphene nanometer sheet is coated in the electrically-conductive backing plate by the method that body increases chemical vapor deposition.
3. method according to claim 2, which is characterized in that the method by electrophoretic deposition is by the graphene nano
Piece is coated in the electrically-conductive backing plate step
It configures graphene electrophoresis liquid: graphene nanometer sheet and soluble metal inorganic salts being added in organic solvent, ultrasound is passed through
Wave disperser is dispersed；
It is put into the graphene electrophoresis liquid using the electrically-conductive backing plate as cathode and anode, is connect in the cathode with anode
It is powered to power supply, deposits the graphene nanometer sheet in the electrically-conductive backing plate of the cathode.
4. method according to claim 3, which is characterized in that the voltage of the power supply is 100-200V, in graphene electrophoresis
The time deposited in liquid is 1-10 minutes.
5. method according to claim 2, which is characterized in that described to increase chemical vapor deposition by microwave plasma
The graphene nanometer sheet is coated in the electrically-conductive backing plate step by method specifically:
The electrically-conductive backing plate for being coated with catalyst metal layer is put into quartz container, is led described in heating under protective gas atmosphere environment
Electric substrate is to predetermined temperature and continues the first duration, then is passed through the second duration of mixed gas reaction of acetylene and hydrogen, described
It is generated on electrically-conductive backing plate and obtains graphene nanometer sheet.
6. method according to claim 5, which is characterized in that the catalyst metal layer is nickel layer, cobalt layers or iron layer, institute
State catalyst metal layer with a thickness of 100-300 nanometers, the predetermined temperature is 700-900 degrees Celsius, and described first when is a length of
10-30 minutes, described second when, was 2-10 minutes a length of.
7. method according to claim 1, which is characterized in that described to deposit six sides nitridation on the graphene nanometer sheet surface
Boron nanometer sheet step includes:
It disperses the hexagonal boron nitride nanosheet in alcohol solvent, by way of spin coating, spraying or dipping, in the stone
Black alkene nanometer sheet surface deposits hexagonal boron nitride nanosheet.
8. a kind of field-transmitting cathode, which is characterized in that the field-transmitting cathode includes:
Conductive substrate；
Graphene nanometer sheet coated on the conductive substrate surface；
And it is distributed in the hexagonal boron nitride nanosheet on the graphene nanometer sheet surface.
9. field-transmitting cathode according to claim 8, which is characterized in that the conductive substrate be iron, titanium, copper, chromium, cobalt, nickel,
Tungsten, molybdenum, gold or platinum substrate, or to be plated with iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold or platinum conductive coating
Insulating substrate.
10. field-transmitting cathode according to claim 8, which is characterized in that the size of the hexagonal boron nitride nanosheet is less than
200 nanometers.
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| CN111081504B (en) * | 2019-12-10 | 2022-07-05 | 深圳先进技术研究院 | Field emission cathode and preparation method thereof |
| CN111128633B (en) * | 2019-12-10 | 2022-06-24 | 深圳先进技术研究院 | Graphene field emission cathode and preparation method thereof |
| CN111415852B (en) * | 2020-05-06 | 2024-02-09 | 上海联影医疗科技股份有限公司 | Anode assembly of X-ray tube, X-ray tube and medical imaging equipment |
| CN115851026B (en) * | 2022-12-28 | 2023-08-08 | 湖州市吴兴区核源金属新材研究院 | High-thermal-conductivity insulated electrophoretic paint and preparation method thereof |
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