CN108335955B - graphene-based field emission cold cathode and preparation method thereof - Google Patents
graphene-based field emission cold cathode and preparation method thereof Download PDFInfo
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- CN108335955B CN108335955B CN201810027577.XA CN201810027577A CN108335955B CN 108335955 B CN108335955 B CN 108335955B CN 201810027577 A CN201810027577 A CN 201810027577A CN 108335955 B CN108335955 B CN 108335955B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/30—Cold cathodes, e.g. field-emissive cathode
- H01J1/304—Field-emissive cathodes
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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
- 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 belongs to the crossing field of vacuum electronic technology and novel carbon material technology, and particularly relates to a graphene-based field emission cold cathode and a preparation method thereof.
Description
Technical Field
The invention belongs to the crossing field of vacuum electronic technology and novel carbon material technology, and particularly relates to a graphene-based field emission cold cathode and a preparation method thereof.
background
by applying an external electric field, the barrier height on the surface of the material is reduced, the width is reduced, and the electron tunneling barrier escapes from the surface of the material, which is field electron emission. The cathode capable of realizing field electron emission is called a field emission cold cathode, and the field emission cold cathode can emit electrons under a lower external electric field without providing extra energy from the outside. As an electron source with low energy consumption, excellent performance and stable work, the field emission cold cathode is applied to the fields of scanning electron microscopes, microwave tubes, X-ray tubes and the like, and particularly has important application prospect in the field electron emission display (FED) field.
To date, a number of field emission cathode materials have been studied, including velvet, carbon fiber, diamond-like carbon, one-dimensional zinc oxide nanorods/wires, carbon nanotubes, and the like. The carbon nano tube is an ideal field emission cathode material due to the unique one-dimensional nano structure, larger specific surface area and length-diameter ratio, higher mechanical strength, excellent electrical property and stable physicochemical property.
As a novel carbon nano material, graphene is formed by a single layer of carbon atoms passing through a two-dimensional planethe periodic arrangement forms a honeycomb lattice structure. Due to its unique two-dimensional structure and electronic structure, graphene has incomparable performance and unique properties with many other nanomaterials. The graphene is formed by a single layer of carbon atoms, the thickness is 0.35nm, and the theoretical specific surface area reaches 2600m2g-1thermal conductivity of 5000Wm-1K-1young's modulus of 1100GPa, and electron mobility of 2x10 at room temperature5cm2V-1s-1. The excellent electrical properties of graphene, the abundance of wrinkled protrusions, and the sharp edges only having atomic layer thickness make it an ideal electron emission material. Graphene-based cathodes exhibit the advantages of low on-field, high current density, stable and uniform emission in field electron emission. The advantages enable the graphene-based cathode to show reliable application prospects in the aspects of field emission and the like.
currently, various methods for preparing graphene-based field emission cathodes have been developed, including microwave plasma chemical vapor deposition, screen printing, electrophoretic deposition, and coating methods. The microwave plasma chemical vapor deposition method has high cost and poor controllability, and the large-area uniform growth of the graphene film is difficult to realize; the screen printing method can realize large-area preparation of the graphene film, and the uniformity is higher, but the field emission performance is reduced because the dense shielding effect of the graphene sheet layer is prominent; the electrophoretic deposition method is easy to realize, but as the deposition progresses, the uniformity of the film and the contact tightness between the sheet layers are affected; the coating method is simple and easy to implement, can realize large-area uniform preparation of the graphene film, and has low emission current density due to the agglomeration and the over-dense distribution of the graphene. Based on the above, a preparation method which has strong controllability and uniformity, is easy to realize large area and can avoid shielding effect caused by over-dense distribution of graphene on the surface layer of the film is needed for preparing the graphene-based cathode.
Disclosure of Invention
Aiming at the technical problems, the invention provides the field emission cold cathode and the preparation method thereof, which can realize the controllable preparation of the large-area, uniform and continuous cathode graphene film.
the invention is realized by the following technical scheme:
A graphene-based field emission cold cathode comprises a conductive substrate and a graphene film layer, wherein the graphene film layer is an emitter of the cathode, and the conductive substrate is in close contact with the graphene film layer.
furthermore, the thickness of the graphene film layer is 20-180 mu m, the graphene film layer is composed of micron-sized graphene clusters, and the particle size of each graphene cluster is 15-45 mu m.
Further, the bottom of the graphene film layer is formed into a graphene film by closely and continuously arranging graphene clusters, and the top of the graphene film layer is formed into an array shape by discontinuously arranging the graphene clusters.
further, the conductive substrate is used as a conductive base, can conduct electricity and is a silicon wafer or a metal sheet.
A preparation method of a graphene-based field emission cold cathode is used for preparing the cathode and is characterized in that graphene dispersion liquid is prepared, the graphene dispersion liquid is sprayed on the surface of a substrate in an atomization spraying mode, drying and solidification are carried out, then the substrate is placed in a sintering furnace for sintering, and the field emission cold cathode is obtained after annealing and furnace cooling; and adding ethyl cellulose and pine oil when the graphene dispersion liquid is prepared, wherein the ethyl cellulose and the pine oil play a role of a binder in a subsequent sintering process.
Further, the method specifically comprises the following steps:
mixing graphene and an organic solvent according to a certain proportion, uniformly dispersing by ultrasonic, adding a small amount of ethyl cellulose and terpineol, dissolving by ultrasonic dispersion, and removing excessive organic solvent by continuous stirring and heating to form a stable graphene dispersion liquid;
Removing impurities and oxides on the surface of the substrate by ultrasonic cleaning, and drying;
Carrying out ultrasonic atomization on the graphene dispersion liquid to form micron-sized graphene atomized liquid drops, and spraying the micron-sized graphene atomized liquid drops on the surface of the substrate through nitrogen gas flow;
Placing the sprayed substrate in a vacuum drying box for drying and curing;
and (3) placing the cured substrate in a sintering furnace, sintering for 0.5 ~ 1 hour at 300 ~ 500 ℃, annealing for 1 ~ 2 hours after the temperature is raised to 600 ~ 700 ℃, and cooling along with the furnace after annealing to obtain the field emission cold cathode.
further, in the preparation process of the graphene dispersion liquid, the mass ratio of the graphene to the organic solvent is controlled to be 1:30 ~ 300, the mass ratio of the terpineol to the graphene is controlled to be 1 ~ 5: 1, and the mass ratio of the ethyl cellulose to the graphene is controlled to be 2 ~ 30: 1.
Further, the organic reagent is isopropanol or ethanol.
and further, the power of ultrasonic atomization is 0.1W ~ 30W, various components in the graphene dispersion solution can be uniformly dispersed in any small volume through atomization treatment, uniform micron ~ sized graphene liquid drops can be formed under the action of ultrasonic energy, and the flow of nitrogen gas flow is controlled to be 100sccm ~ 600sccm in the process that the micron ~ sized graphene atomized liquid drops are sprayed on the surface of the substrate through the nitrogen gas flow.
further, will before the graphite alkene dispersion liquid carries out ultrasonic atomization, need with graphite alkene dispersion liquid solution is packed into the syringe in advance, injects into to the sound atomization pond through the hose and according to certain speed and accomplishes the atomizing, and this is done benefit to high atomizing of graphite alkene dispersion liquid in order to realize the control to graphite alkene dispersion liquid inlet velocity to and form the micron order graphite alkene liquid that size and density are homogeneous.
The invention has the beneficial technical effects that:
The field emission cold cathode and the preparation method provided by the invention realize the preparation of a large-area, uniform and continuous cathode graphene film, and realize the controllable preparation of the graphene cathode film on the appearance and thickness by adjusting the concentration and component ratio of a dispersion liquid, the ultrasonic atomization power, the liquid inlet speed and the spraying time; the graphene film layer prepared by the method has a stable structure and is tightly contacted with a substrate, and the surface layer of the film layer has abundant graphene folds and sharp edges, so that the requirements of serving as a field emission cold cathode are met; the surface of the thin film layer is rough and is formed by graphene clusters and distributed in an array manner, and the unique morphology avoids the condition that the distribution of the graphene emission tips is too dense, so that the shielding effect caused by the too dense distribution of the graphene can be avoided, the reduction of the starting electric field is facilitated, and the emission current is improved.
The field emission cold cathode provided by the invention has good performance advantages of low starting electric field, low threshold electric field, large emission current and the like, and can be used as an excellent electron source to be applied to the fields of Field Emission Display (FED) and the like.
Drawings
FIG. 1A is a block diagram of a field emission cold cathode according to an embodiment of the present invention;
Fig. 1B is a partially enlarged view of the graphene thin film layer in fig. 1A;
FIG. 2 is a flow chart of a method for fabricating a field emission cold cathode according to an embodiment of the present invention;
FIG. 3A is a front scanning electron micrograph of a field emission cold cathode made according to an embodiment of the present invention;
FIG. 3B is a scanning electron microscope cross-sectional view of a field emission cold cathode fabricated according to an embodiment of the present invention;
FIG. 4 is a J-E (emission current density-applied electric field) curve of a field emission cold cathode in an applied electric field according to an embodiment of the present invention.
Detailed Description
the following detailed description of the present invention, taken in conjunction with the accompanying drawings and examples, is provided to enable the invention and its various aspects and advantages to be better understood. However, the specific embodiments and examples described below are for illustrative purposes only, are not intended to limit the present invention, and do not contain all of the contents of the present invention. All other examples, which can be derived by a person skilled in the art from variations that are within the teachings of the invention, are within the scope of the invention. The term "connected", as used herein, unless otherwise expressly specified or limited, is to be construed broadly, as meaning either directly or through an intermediate connection. In the description of the present invention, it is to be understood that the directions or positional relationships indicated by the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", and the like are based on the directions or positional relationships shown in the drawings, and are only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and thus, should not be construed as limiting the present invention.
as shown in fig. 1, fig. 1A is a structural diagram of a field emission cold cathode according ~ an embodiment of the present invention, the field emission cold cathode includes a substrate 1 and an emitter, that is, a graphene thin film layer 2, the graphene thin film layer 2 is tightly attached ~ a surface of the substrate 1, the graphene thin film layer 2 is composed of graphene clusters, particle diameters of the graphene clusters are 15 μm ~ 45 μm, and thicknesses of the graphene thin film layer are 20 μm ~ 180 μm.
As shown in fig. 1B, in the field emission cold cathode of the present embodiment, the bottom 21 of the graphene thin film layer is formed by arranging graphene clusters continuously. The graphene clusters are continuously arranged to form the bottom of the compact and continuous thin film layer. The top 22 of the graphene thin film layer is formed by non-continuous arrangement of graphene clusters. At the top 22 of the graphene film layer, micron-sized graphene clusters are arranged discontinuously to form an array shape. The graphene film layer 2 is in close contact with the substrate 1 to form a cold cathode capable of performing field electron emission.
Preferably, the substrate 1 is a silicon wafer or a metal substrate. The selection of the specific substrate 1 can be determined by the staff according to the actual situation.
According to the field emission cold cathode provided by the embodiment of the invention, the graphene film layer has a stable structure, and the surface layer of the film layer has abundant graphene folds and sharp edges, so that the requirements of serving as the field emission cold cathode are met; and the surface of the thin film layer is rough, the thin film layer is formed by graphene clusters and distributed in an array manner, so that the shielding effect caused by too dense graphene distribution can be avoided, the opening electric field is favorably reduced, and the emission current is improved.
As shown in fig. 2, in another aspect, an embodiment of the present invention provides a method for preparing a field emission cold cathode, including the following steps:
S1, mixing graphene and an organic solvent according to a certain proportion, uniformly dispersing by ultrasonic, adding a small amount of ethyl cellulose and terpineol, dispersing and dissolving by ultrasonic, and removing excessive organic solvent by continuous stirring and heating to form a stable graphene dispersion liquid, wherein the mass ratio of the graphene to the organic solvent is 1 (30 ~ 300), the mass ratio of the ethyl cellulose to the graphene is (2 ~ 30): 1, and the mass ratio of the terpineol to the graphene is (1 ~ 5): 1.
And S2, removing impurities and oxides on the surface of the substrate by ultrasonic cleaning, and drying.
S3, carrying out ultrasonic atomization on the graphene dispersion liquid to form micron-sized graphene atomized liquid drops, and spraying the micron-sized graphene atomized liquid drops to the surface of the substrate through nitrogen gas flow. The ultrasonic atomization power is between 0.1W and 30W, and the flow rate of nitrogen is between 100sccm and 600 sccm.
And S4, drying the sprayed substrate in a vacuum drying oven to form the cured graphene coating.
S5, placing the solidified substrate in a sintering furnace, sintering for 0.5 ~ 1 hour at 300 ~ 500 ℃, annealing for 1 ~ 2 hours at 600 ~ 700 ℃, and cooling along with the furnace to obtain the field emission cold cathode.
According to the field emission cold cathode and the preparation method provided by the embodiment of the invention, the reduced graphene oxide is used as a raw material, and the graphene field emission cold cathode with the array surface appearance is prepared by adopting an ultrasonic atomization auxiliary spraying method. The method is low in cost, strong in controllability and uniformity and easy to realize large-area preparation, the prepared array distribution morphology solves the problem that the distribution of surface layer graphene is too dense, which is difficult to avoid by other preparation methods, and the shielding effect is reduced. The graphene-based field emission cold cathode of the present embodiment has an on-field of 1.52V/μm, a threshold field of 2.65V/μm, and an emission current density of 29.6mA/cm under an applied field of 5V/μm2Can be used as an excellent electron source for FED and the likethe field of the technology.
Example 1
The present embodiment provides a method for preparing a field emission cold cathode, which comprises the following steps:
1) Cathode substrate cleaning
Carrying out primary ultrasonic cleaning on an N-type Si sheet with the thickness of 1cmx1cm for 10 minutes by using deionized water, transferring the N-type Si sheet into a mixed solution of ammonia water, hydrogen peroxide and the deionized water for ultrasonic cleaning for 10 minutes, and then carrying out ultrasonic cleaning for 10 minutes by using the deionized water; ultrasonic cleaning the mixture in mixed solution of hydrochloric acid, hydrogen peroxide and deionized water for 10 minutes, ultrasonic cleaning with deionized water for 10 minutes, and drying with nitrogen; and transferring the mixture into absolute ethyl alcohol for ultrasonic cleaning for 10 minutes, and drying the mixture by nitrogen for later use.
2) Preparation of graphene dispersion liquid
Graphene and organic solution ethanol are mixed according to a certain mass ratio (1: 50), uniformly dispersed by ultrasonic, added with a small amount of ethyl cellulose (the mass ratio of the ethyl cellulose to the graphene is 10: 1) and terpineol (the mass ratio of the terpineol to the graphene is 2: 1), dissolved by ultrasonic dispersion, and heated to remove excessive organic solution, so as to form stable graphene dispersion liquid.
3) atomization and spraying
Placing the front side of a substrate upwards on a heating table, and heating the temperature of the heating table to 65 ℃;
filling the graphene dispersion liquid into an injector, injecting the graphene dispersion liquid into an ultrasonic atomization pool through a hose at a certain speed, and carrying out ultrasonic atomization under the power of 0.3W;
thirdly, spraying micron-sized graphene atomized liquid drops on the surface of the substrate by using nitrogen with the flow of 400 sccm.
4 substrate curing
And (3) placing the sprayed substrate in a vacuum drying oven, drying for 3 hours at 90 ℃, and removing the organic dispersing agent to form a cured graphene coating.
5 sintering and annealing treatment
And (3) placing the solidified substrate in a sintering furnace under the protection of nitrogen atmosphere, sintering for 0.5 hour at 400 ℃, raising the temperature to 600 ℃, annealing for 1 hour, and cooling along with the furnace to obtain the field emission cold cathode.
Fig. 3A is a front scanning electron microscope image of the field emission cold cathode prepared in this example, and fig. 3B is a cross-sectional scanning electron microscope image of the field emission cold cathode prepared in this example. As can be seen from the figure, the graphene field emission cold cathode prepared by the method has an array distributed surface structure, and is beneficial to field electric emission.
FIG. 4 is a J-E (emission current density-applied electric field) curve of a field emission cold cathode of an embodiment of the present invention in an applied electric field. As can be seen from the figure, the field emission cold cathode prepared by the method can realize field electron emission and has excellent field emission performance.
Example 2:
The present embodiment provides a method for preparing a field emission cold cathode, which comprises the following steps:
1) Cathode substrate cleaning
Carrying out ultrasonic cleaning on an N-type Si sheet with the thickness of 2.2cm x2.2cm by using a mixed solution of ammonia water, hydrogen peroxide and deionized water; ultrasonically cleaning the mixture by ethanol and deionized water respectively, and drying the mixture by nitrogen.
2) preparation of graphene dispersion liquid
Mixing graphene and isopropanol according to a certain mass ratio (1: 200), performing ultrasonic dispersion for 10min, adding ethyl cellulose (the mass ratio of the ethyl cellulose to the graphene is 2: 1) and terpineol (the mass ratio of the terpineol to the graphene is 1: 1), performing ultrasonic dispersion and dissolution, and continuously stirring to remove excessive organic solution to form graphene dispersion liquid.
3) Atomization and spraying
Spraying micron-sized graphene atomized liquid drops ultrasonically atomized under 6W power on the surface of a substrate fixed on a heating table at 80 ℃ by using nitrogen with the flow rate of 600sccm
4) Substrate curing
And (3) placing the sprayed substrate in a vacuum drying oven for curing, and preserving heat for 1 hour at 150 ℃.
5) Sintering and annealing treatment
And (3) placing the solidified substrate in a sintering furnace, sintering for 1 hour at 500 ℃, annealing for 2 hours at 700 ℃, and cooling along with the furnace to obtain the graphene-based field emission cold cathode.
The field emission cold cathode prepared by the embodiment can also obtain excellent field emission performance.
Example 3:
the present embodiment provides a method for preparing a field emission cold cathode, which comprises the following steps:
1) Cathode substrate cleaning
And (3) ultrasonically cleaning a metal sheet with the thickness of 0.7cm and the thickness of 0.7cm by ammonia water, ethanol, deionized water and absolute ethanol respectively, and drying by nitrogen for later use.
2) Preparation of graphene dispersion liquid
Mixing graphene and isopropanol according to a certain mass ratio (1: 300), performing ultrasonic dispersion, adding ethyl cellulose (the mass ratio of the ethyl cellulose to the graphene is 20: 1) and terpineol (the mass ratio of the terpineol to the graphene is 4: 1), performing ultrasonic dispersion and dissolution, and heating and stirring to form a graphene dispersion liquid.
3) Atomization and spraying
Filling the graphene dispersion liquid into an injector, injecting the graphene dispersion liquid into an ultrasonic atomization pool through a hose at a certain speed, and carrying out ultrasonic atomization under the power of 9W;
And secondly, spraying micron-sized graphene atomized liquid drops on the surface of the substrate by using nitrogen with the flow rate of 100 sccm.
4) substrate curing
And (3) placing the sprayed substrate in a vacuum drying oven, and drying for 2 hours at 120 ℃ to form the cured graphene coating.
5) Sintering and annealing treatment
And (3) placing the solidified substrate in a sintering furnace, sintering for 0.75 hour at 300 ℃, then raising the temperature to 650 ℃, annealing for 1 hour, and cooling along with the furnace to obtain the field emission cold cathode.
The field emission cold cathode prepared by the embodiment can also obtain excellent field emission performance
It should be noted that the above-mentioned embodiments described with reference to the drawings are only intended to illustrate the present invention and not to limit the scope of the present invention, and it should be understood by those skilled in the art that modifications and equivalent substitutions can be made without departing from the spirit and scope of the present invention. Furthermore, unless the context indicates otherwise, words that appear in the singular include the plural and vice versa. Additionally, all or a portion of any embodiment may be utilized with all or a portion of any other embodiment, unless stated otherwise.
Claims (7)
1. A graphene-based field emission cold cathode is characterized by comprising a conductive substrate and a graphene film layer, wherein the graphene film layer is an emitter of the cathode, and the conductive substrate is in close contact with the graphene film layer;
the thickness of the graphene film layer is 20-180 mu m; the graphene film layer is composed of micron-sized graphene clusters, and the particle size of each graphene cluster is 15-45 microns;
The bottom of the graphene film layer is formed into a graphene film by closely and continuously arranging graphene clusters, and the top of the graphene film layer is formed into an array shape by discontinuously arranging the graphene clusters;
the on-field of the graphene-based field emission cathode was 1.52V/μm.
2. The field emission cold cathode according to claim 1, wherein said conductive substrate is a conductive base, capable of conducting electricity, and is a silicon wafer or a metal sheet.
3. a preparation method of a graphene-based field emission cold cathode is used for preparing the field emission cold cathode as claimed in any one of claims 1-2, and is characterized in that a graphene dispersion liquid is prepared, the graphene dispersion liquid is sprayed on the surface of a substrate in an atomization spraying mode, drying and curing are carried out, then the substrate is placed in a sintering furnace for sintering, annealing and furnace cooling are carried out, and then the field emission cold cathode is obtained; wherein, when preparing the graphene dispersion liquid, ethyl cellulose and terpineol are added;
The method specifically comprises the following steps:
mixing graphene and an organic solvent according to a certain proportion, uniformly dispersing by ultrasonic, adding a small amount of ethyl cellulose and terpineol, dissolving by ultrasonic dispersion, continuously stirring and heating to form a stable graphene dispersion liquid;
Removing impurities and oxides on the surface of the substrate by ultrasonic cleaning, and drying;
carrying out ultrasonic atomization on the graphene dispersion liquid to form micron-sized graphene atomized liquid drops, and spraying the micron-sized graphene atomized liquid drops on the surface of the substrate through nitrogen gas flow;
Placing the sprayed substrate in a vacuum drying box for drying and curing;
placing the cured substrate in a sintering furnace: sintering at 300-500 ℃ for 0.5-1 hour, then annealing for 1-2 hours after the temperature is raised to 600-700 ℃, and cooling along with the furnace after annealing to obtain the field emission cold cathode.
4. The preparation method according to claim 3, wherein in the preparation of the graphene dispersion, the mass ratio of the graphene to the organic solvent is controlled to be 1: 30-300, and controlling the mass ratio of the terpineol to the graphene to be 1-5: 1, controlling the mass ratio of the ethyl cellulose to the graphene to be 2-30: 1.
5. The method according to claim 3, wherein the organic solvent is isopropyl alcohol or ethyl alcohol.
6. The preparation method according to claim 3, wherein the power of the ultrasonic atomization is 0.1W-30W; and controlling the flow of the nitrogen gas flow to be 100-600 sccm in the process of spraying the micron-sized graphene atomized liquid drops on the surface of the substrate through the nitrogen gas flow.
7. The preparation method according to claim 3, wherein before the graphene dispersion liquid is subjected to ultrasonic atomization, the graphene dispersion liquid solution is pre-filled into a syringe, and is injected into a sound atomization pool through a hose at a certain speed to complete atomization.
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