CN106653520A - Field emission cold cathode and manufacturing method thereof - Google Patents
Field emission cold cathode and manufacturing method thereof Download PDFInfo
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- CN106653520A CN106653520A CN201611124177.8A CN201611124177A CN106653520A CN 106653520 A CN106653520 A CN 106653520A CN 201611124177 A CN201611124177 A CN 201611124177A CN 106653520 A CN106653520 A CN 106653520A
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- graphene
- nanometer sheet
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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
The invention provides a manufacturing method of a field emission cold cathode. The method comprises the following steps of providing a conductive substrate; coating the conductive substrate with graphene nanosheets; and depositing hexagonal boron nitride nanosheets on the surfaces of the graphene nanosheets. The graphene nanosheets coat the conductive substrates and the hexagonal boron nitride nanosheets are deposited on the surface of the graphene nanosheets, so that a stable composite nanostructure is formed between the hexagonal boron nitride nanosheets and the graphene nanosheets, the work function of graphene is reduced and the local electric field of the surface on the graphene is increased, thereby obviously reducing the turn-on field of a cathode and improving the emission current. Furthermore, the graphene is prevented from being bombarded by kations through the hexagonal boron nitride nanosheets and the emission stability of the cathode is improved.
Description
Technical field
The invention belongs to vacuum electron device field, more particularly to a kind of field emission cold-cathode and its manufacture method.
Background technology
Vacuum electron device, such as microwave tube, X-ray tube, electronics propulsion and Charge control devices, are communication, space skill
Critical component in the fields such as art, safety detection, imaging of medical.The core component of vacuum electron device is negative electrode, main at present
Using metal hot cathode.However, metal hot cathode body product is big, heat radiation power consumption is big, opening time length, material under high temperature are steamed
Send out etc. defect, limit vacuum electron device to miniaturization and integrated direction development.
In recent years, domestic and international researcher has been obtained based on the field emission cold cathode of various one-dimensional/two-dimension nano materials
Extensive concern and research, the electronics on its nanoscale tip can occur tunneling effect under electric field action, in theory can be with shape
Into great electric current.Such as, two-dimentional carbon nanomaterial Graphene has huge dimensional thickness ratio and enriches flourishing edge knot
Structure, can be 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 advantage such as warm work, quick response, low-power consumption, Miniaturized, being applied to vacuum electron device can optimize structure, obtain excellent
Power and frequency characteristic.However, existing nano material field-transmitting cathode there is emission current and current density is little, transmitting is steady
Qualitative poor the problems such as, it is impossible to meet the requirement of high performance device application.
The content of the invention
It is an object of the invention to provide a kind of manufacture method of field-transmitting cathode, to solve prior art in nano material
There is emission current in field-transmitting cathode and current density is little, launch stability difference the problems such as, it is impossible to meet high performance device application
Requirement problem.
In a first aspect, embodiments providing a kind of manufacture method of field-transmitting cathode, methods described 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.
It is described to apply on the electrically-conductive backing plate with reference in a first aspect, in the first possible implementation of first aspect
Covering graphene nanometer sheet step includes：
The graphene nanometer sheet is coated in by the electrically-conductive backing plate by the method for electrophoretic deposition, or by microwave etc.
Gas ions increase the method for chemical vapor deposition and the graphene nanometer sheet are coated in into the electrically-conductive backing plate.
With reference to the first possible implementation of first aspect, in second possible implementation of first aspect, institute
State and the graphene nanometer sheet is coated in by the electrically-conductive backing plate step by the method for electrophoretic deposition includes：
Configuration Graphene electrophoresis liquid：Graphene nanometer sheet and soluble metal inorganic salts are added in organic solvent, is passed through
Ultrasonic disperser is disperseed；
The Graphene electrophoresis liquid is put into using the electrically-conductive backing plate as negative electrode and anode, in the negative electrode and anode
Power supply energization is connected to, in the electrically-conductive backing plate of the negative electrode graphene nanometer sheet is deposited.
With reference to second possible implementation of 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.
With reference to the first possible implementation of first aspect, in the 4th kind of possible implementation of first aspect, institute
The graphene nanometer sheet is coated in the electrically-conductive backing plate by the method that state increases chemical vapor deposition by microwave plasma
Step is specially：
The electrically-conductive backing plate for being coated with catalyst metal layer is put in 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 be passed through the duration of mixed gas reaction second of acetylene and hydrogen,
Generate on the electrically-conductive backing plate and obtain graphene nanometer sheet.
With reference to the 4th kind of possible implementation of first aspect, in the 5th kind of possible implementation of first aspect, institute
It is nickel dam, cobalt layers or iron layer to state catalyst metal layer, and the thickness of the catalyst metal layer is 100-300 nanometers.
With reference to the 4th kind of possible implementation of first aspect, in the 5th kind of possible implementation of first aspect, institute
It is 700-900 degree Celsius to state predetermined temperature, a length of 10-30 minutes when described first, a length of 2-10 minutes when described second.
It is described in the graphene nanometer sheet with reference in a first aspect, in the 5th kind of possible implementation of first aspect
Surface deposition hexagonal boron nitride nanosheet step includes：
The hexagonal boron nitride nanosheet is scattered in alcohol solvent, by way of spin coating, spraying or impregnating, in institute
State graphene nanometer sheet surface deposition hexagonal boron nitride nanosheet.
Second aspect, embodiments provides a kind of field-transmitting cathode, and the field-transmitting cathode includes：
Conductive substrate；
It is coated on the graphene nanometer sheet on the conductive substrate surface；
And, it is distributed in the hexagonal boron nitride nanosheet on the graphene nanometer sheet surface.
With reference to 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 insulated 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 stable composite Nano knot is formed between hexagonal boron nitride nanosheet and graphene nanometer sheet
Structure, reduces the work function of Graphene, increased the local electric field of graphenic surface, so as to substantially reduce the unlatching electricity of negative electrode
, improve its emission current.Also, hexagonal boron nitride nanosheet part prevents Graphene to be bombarded by cation, improve
The launch stability of negative electrode.
Description of the drawings
Fig. 1 is the flowchart of the manufacture method of field-transmitting cathode provided in an embodiment of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain 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 manufacture method, to solve existing skill
There is emission current in the field-transmitting cathode of the nano material in art and current density is little, the problems such as launch stability difference, it is impossible to full
The requirement of sufficient high performance device application.Below in conjunction with the accompanying drawings, the present invention is further illustrated.
Fig. 1 shows the flow process of realizing of the manufacture method of the field-transmitting cathode that first embodiment of the invention is provided, and detailed description is such as
Under：
In step S101, there is provided electrically-conductive backing plate.
Specifically, the electrically-conductive backing plate, 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 being plated with the metallic conduction coating such as iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold or platinum
Plate.The electrically-conductive backing plate is used to form graphene nano lamella on its surface, can be according to the painting method of graphene nanometer sheet, really
The material of the fixed metal selected.Such as according to electrophoretic deposition, or the coating of microwave plasma enhanced chemical vapour deposition technique
The graphene nanometer sheet, selecting guarantees the metallic conduction substrate that painting method can effectively be implemented.
The insulated substrate, can be one or more in glass, ceramics, silicon chip etc..The insulated substrate surface
Metal coating, magnetron sputtering, electron beam evaporation can be adopted, at least one in vapour deposition process or electroless plating method be plated
Cover.
In step s 102, the graphene coated nanometer sheet on the electrically-conductive backing plate.
Specifically, the coating of the graphene nanometer sheet, can be using electrophoretic deposition or plasma enhanced chemical
Vapour deposition process, illustrates separately below.
1st, electrophoretic deposition：
Firstly, it is necessary to Graphene electrophoresis solution is prepared, can be by graphene nanometer sheet and soluble metal inorganic salts (electric charge
Additive) add in organic solvent according to predetermined ratio, ultrasonic disperse can be carried out by supersonic generator.The ultrasound
The ultrasound works duration of ripple disperser can be 1～3 hour such that it is able to obtain uniform and stable Graphene electrophoresis solution.
Organic solvent used can be the one kind in ethanol, 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 nitric acid nickel (NO3)2
Deng.
Wherein, the graphene nanometer sheet, the method (Hummer methods) that can adopt graphite oxidation reduction is prepared.Institute
State the graphene nanometer sheet that graphene nanometer sheet can be individual layer, few layer or multilayer.The lateral dimension of the graphene nanometer sheet
Preferably 1-10 μm.The concentration of the mixed liquor of the organic solvent can be 0.1-10mg/ml, in order to improve Graphene in solution
In dispersiveness, preferably 0.1-1mg/ml.
After Graphene electrophoresis liquid is obtained, using electrically-conductive backing plate as negative electrode, another electrically-conductive backing plate connects respectively as anode
The negative pole and positive pole of dc source, by the electrically-conductive backing plate Graphene electrophoresis liquid, in the presence of DC voltage, positively charged are put into
The graphene nanometer sheet of lotus to cathode direction is moved, and is deposited on electrically-conductive backing plate, obtains graphene layer.The bar of the deposition process
Part is preferably：Voltage 100-200V, such as can be 150V, 180V etc. from electrophoretic voltage.The duration of the electrophoresis can be
1-10min, such as can select 3 minutes, 5 minutes, 8 minutes etc..
2nd, plasma reinforced chemical vapour deposition method：
The electrically-conductive backing plate that catalyst metal layer can be coated with is put in quartz container, such as can be in quartz ampoule.
Under protective gas atmosphere environment, such as can be under Ar plasma atmosphere environment, plus hot substrate is to reaction temperature, insulation the
One duration.Then, it is passed through acetylene (C2H2) and hydrogen (H2) mixed gas, growth obtains the graphene nanometer sheet that is vertically arranged.
After the second duration, reaction terminates, and under being protected by argon gas, is cooled to room temperature.
Wherein, the catalyst metal layer can be nickel layer, cobalt Co layers or iron Fe layers.The catalyst metal layer
Thickness can select for 100-300nm, such as can select as 150 nanometers, 200 nanometers or 250 nanometers etc..
In addition, in embodiments of the present invention, the microwave power for generating Ar plasmas can be 500-1000W, institute
Can be 700-900 DEG C with reaction temperature, such as can be 750 degree, 800 degree, 850 degree etc..First duration can for 10-
30min, such as be specifically as follows 15 minutes, 20 minutes or 25 minutes etc..
Wherein, the scope of the ratio (H2/C2H2) of the hydrogen and acetylene can be 5-10.The ratio of such as hydrogen and acetylene
Example can be 6 to 1,7 to 1,8 to 1 or 9 to 1 etc..Reaction pressure scope 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 etc..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 machinery or ultrasound, from hexagonal boron nitride crystal
Middle stripping obtains.The hexagonal boron nitride nanosheet can be the hexagonal boron nitride nanosheet of individual layer, or the six of multilayer
Square boron nitride nanosheet.Hexagonal boron nitride nanosheet hexagonal boron nitride preferentially from its lateral dimension less than 200 nanometers
Nanometer sheet.
The deposition process of the hexagonal boron nitride nanosheet includes：Hexagonal boron nitride nanosheet is well-dispersed in into ethanol molten
In agent, such as can be by the scattered mode of ultrasonic wave.Then by spin coating, spraying or the method for impregnating, in graphene nano
Piece surface deposits hexagonal boron nitride nanosheet, forms compound field emission cathode structure.
Present invention nanometer sheet graphene coated on electrically-conductive backing plate, on the surface of the graphene nanometer sheet six side's nitrogen are deposited
Change boron nanometer sheet so that stable composite nanostructure is formed between hexagonal boron nitride nanosheet and graphene nanometer sheet, reduce
The work function of Graphene, increased the local electric field of graphenic surface, so as to substantially reduce the threshold electric field of negative electrode, improve it
Emission current.Also, hexagonal boron nitride nanosheet part prevents Graphene to be bombarded by cation, sending out for negative electrode is improve
Penetrate stability.
In addition, the embodiment of the present invention additionally provides a kind of field-transmitting cathode of nano material, the field-transmitting cathode includes：
Conductive substrate；
It is coated on the graphene nanometer sheet 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 for plating
There is the insulated substrate of the metallic conduction coating such as iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold, platinum.The insulated substrate, can be glass
One or more in glass, ceramics, silicon chip etc..The metal coating on the insulated substrate surface, can adopt magnetron sputtering, electricity
Beamlet evaporates, and at least one in vapour deposition process or electroless plating method carries out plating.
The graphene nanometer sheet, the method (Hummer methods) that can adopt graphite oxidation reduction is prepared.The stone
Black alkene nanometer sheet can be the graphene nanometer sheet of individual layer, few layer or multilayer.The lateral dimension of the graphene nanometer sheet is preferred
For 1-10 μm.
Hexagonal boron nitride nanosheet hexagonal boron nitride nanosheet preferentially from its lateral dimension less than 200 nanometers,
Specifically refer to length, width of hexagonal boron nitride nanosheet etc. and be less than 200 nanometers.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of manufacture method of field-transmitting cathode, it is characterised in that methods described 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, it is characterised in that the nanometer sheet step graphene coated on the electrically-conductive backing plate
Suddenly include：
The graphene nanometer sheet is coated in by the electrically-conductive backing plate by the method for electrophoretic deposition, or by microwave plasma
Body increases the method for chemical vapor deposition and the graphene nanometer sheet is coated in into the electrically-conductive backing plate.
3. method according to claim 2, it is characterised in that it is described by the method for electrophoretic deposition by the graphene nano
Piece is coated in the electrically-conductive backing plate step to be included：
Configuration Graphene electrophoresis liquid：Graphene nanometer sheet and soluble metal inorganic salts are added in organic solvent, by ultrasound
Ripple disperser is disperseed；
The Graphene electrophoresis liquid is put into using the electrically-conductive backing plate as negative electrode and anode, is connected with anode in the negative electrode
It is powered to power supply, in the electrically-conductive backing plate of the negative electrode graphene nanometer sheet is deposited.
4. method according to claim 3, it is characterised 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, it is characterised in that described that chemical vapor deposition is increased by microwave plasma
The graphene nanometer sheet is coated in the electrically-conductive backing plate step and is specially by method：
The electrically-conductive backing plate for being coated with catalyst metal layer is put in 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 duration of mixed gas reaction second of acetylene and hydrogen, described
Generate on electrically-conductive backing plate and obtain graphene nanometer sheet.
6. method according to claim 5, it is characterised in that the catalyst metal layer is nickel dam, cobalt layers or iron layer, institute
The thickness for stating catalyst metal layer is 100-300 nanometers, and the predetermined temperature is 700-900 degree Celsius, a length of when described first
10-30 minutes, a length of 2-10 minutes when described second.
7. method according to claim 1, it is characterised in that described to deposit six sides nitridation on the graphene nanometer sheet surface
Boron nanometer sheet step includes：
The hexagonal boron nitride nanosheet is scattered in alcohol solvent, by way of spin coating, spraying or impregnating, in the stone
Black alkene nanometer sheet surface deposits hexagonal boron nitride nanosheet.
8. a kind of field-transmitting cathode, it is characterised in that the field-transmitting cathode includes：
Conductive substrate；
It is coated on the graphene nanometer sheet 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, it is characterised in that the conductive substrate be iron, titanium, copper, chromium, cobalt, nickel,
Tungsten, molybdenum, gold or platinum substrate, or to be plated with the metallic conduction coating such as iron, titanium, nickel, cobalt, chromium, copper, tungsten, molybdenum, gold, platinum
Insulated substrate.
10. field-transmitting cathode according to claim 8, it is characterised in that the hexagonal boron nitride nanosheet is smaller in size than
200 nanometers.
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| CN201611124177.8A CN106653520B (en) | 2016-12-08 | 2016-12-08 | A kind of field emission cold-cathode and its manufacturing method |
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| 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 |
| CN115851026A (en) * | 2022-12-28 | 2023-03-28 | 湖州市吴兴区核源金属新材研究院 | High-thermal-conductivity insulating electrophoretic paint and preparation method thereof |
| 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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