CN112053925A - Field emission cathode and preparation method thereof - Google Patents
Field emission cathode and preparation method thereof Download PDFInfo
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- CN112053925A CN112053925A CN202011075453.2A CN202011075453A CN112053925A CN 112053925 A CN112053925 A CN 112053925A CN 202011075453 A CN202011075453 A CN 202011075453A CN 112053925 A CN112053925 A CN 112053925A
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- 229910017053 inorganic salt Inorganic materials 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 229910009818 Ti3AlC2 Inorganic materials 0.000 claims description 4
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 3
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- YIXJRHPUWRPCBB-UHFFFAOYSA-N magnesium nitrate Chemical group [Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O YIXJRHPUWRPCBB-UHFFFAOYSA-N 0.000 description 2
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Images
Classifications
-
- 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
-
- 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
- H01J1/3042—Field-emissive cathodes microengineered, e.g. Spindt-type
- H01J1/3046—Edge emitters
-
- 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 field emission cathode, which comprises a conductive substrate and Ti formed on the conductive substrate3C2And the nano sheet film layer. The preparation method of the field emission cathode comprises the following steps: providing a conductive substrate; preparing Ti3C2A nanosheet dispersion; adding the Ti3C2The nanosheet dispersion is coated on the conductive substrate to form Ti on the conductive substrate3C2And the nano sheet film layer. The field emission cathode provided by the invention can better resist bombardment damage of cations to keep the structural integrity and obtain more stable emission current, and the preparation method of the field emission cathode has the advantages of simple process flow and easy realization of process conditions, and is beneficial to large-scale industrial application.
Description
Technical Field
The invention belongs to the technical field of field emission, and particularly relates to a field emission cathode and a preparation method thereof.
Background
Vacuum electronic devices have wide application in the fields of communication, space technology, security detection, medical imaging and the like. The core component of the vacuum electronic device is a cathode which is used for generating electron beam current required by the operation of the vacuum electronic device. At present, the most widely used cathode is a metal hot cathode, however, the hot cathode has the defects of large volume, large heat radiation power consumption, long starting time, material evaporation at high temperature and the like, and the development of vacuum electronic devices towards miniaturization and integration is limited.
In recent years, field emission cold cathodes based on various one-dimensional/two-dimensional nanomaterials are widely focused and researched by researchers, under a lower electric field, the nano-scale tips of the field emission cold cathodes can form a local enhancement effect, electrons can generate a tunneling effect under the action of the lower electric field, and a great emission current is formed, and typical representatives of the field emission cold cathodes are graphene and carbon nanotubes. The graphene has rich sharp edge structures, can be used as an effective electron emission address, and is an ideal field emission nanometer material due to stable mechanochemical properties and excellent electric and heat conduction characteristics. The carbon nanotube is used as a one-dimensional material, has the similar electric and heat conducting performance as graphene, has a huge length-diameter ratio, and can efficiently emit current by the end part (opening or closing) of the nanometer tube. Compared with a hot cathode, the field emission cathode has the advantages of room-temperature working, fast response (nanosecond), low power consumption, micromation and the like, and can optimize the structure and obtain excellent power and frequency characteristics when being applied to a vacuum electronic device.
However, graphene and carbon nanotubes are carbon materials, and the emission structure of graphene and carbon nanotubes is easily damaged by bombardment of cations (residual gas in vacuum is ionized by electrons to generate cations and moves to a cathode under the action of an electric field) in the field emission process, and in addition, the emission structure is also damaged by high temperature formed by joule heat generated by field emission, which causes that the emission current density of graphene and carbon nanotubes is easily attenuated or fluctuates sharply, and the emission stability is poor.
Disclosure of Invention
In view of the defects in the prior art, the invention provides a field emission cathode and a preparation method thereof, and aims to solve the problem that the existing nano-material field emission cathode has poor emission stability.
To achieve the above object, an aspect of the present invention provides a field emission cathode including a conductive substrate and Ti formed on the conductive substrate3C2And the nano sheet film layer.
Preferably, the Ti3C2The thickness of the nano-sheet film layer is 1-10 mu m.
Preferably, the conductive substrate is selected from metal substrates formed by at least one of iron, titanium, copper, chromium, cobalt, nickel, tungsten, molybdenum, tantalum and platinum as a base material; or, the conductive substrate is indium tin oxide conductive glass or silicon chip.
Another aspect of the present invention is to provide a method for preparing a field emission cathode as described above, which comprises: providing a conductive substrate; preparing Ti3C2A nanosheet dispersion; adding the Ti3C2The nanosheet dispersion is coated on the conductive substrate to form Ti on the conductive substrate3C2And the nano sheet film layer.
Preferably, the formulation Ti3C2The nanoplate dispersion comprises: providing Ti3C2Nanosheet material, the Ti3C2Adding a nanosheet raw material into a solvent, performing ultrasonic stirring, and performing centrifugal treatment to obtain the Ti3C2A nanosheet dispersion.
Preferably, the Ti3C2In the nanosheet dispersion, Ti3C2The concentration of the nano-sheet is 1 mg/mL-5 mg/mL.
Preferably, the ultrasonic power of the ultrasonic stirring is 100W-500W, and the time is 10 min-20 min.
Preferably, the Ti3C2The nano sheet raw material is prepared by the following process:
s10, under the condition of continuous stirring, adding Ti3AlC2Adding the layered material into an HF solution or a mixed solution of HCl and LiF, and etching to remove the Al intermediate layer to obtain a first intermediate product;
s20, adding the first intermediate product into deionized water and keeping the mixture in inert gasUltrasonic stripping under protection, and centrifuging to separate supernatant to obtain Ti3C2A nanosheet solution;
s30, mixing the Ti3C2Drying the nanosheet solution to obtain Ti3C2A nano-sheet powder raw material.
Preferably, the Ti is applied using an electrophoretic deposition process3C2The nanosheet dispersion is coated on the conductive substrate and includes: to the Ti3C2Adding metal inorganic salt into the nanosheet dispersion liquid to serve as a reaction solution; placing the conductive substrate as a cathode and another electrode as an anode in the reaction solution, and allowing Ti in the reaction solution to react under the action of DC voltage3C2Nanoplate deposited on the conductive substrate, forming Ti on the conductive substrate3C2And the nano sheet film layer.
Preferably, the Ti is applied using a spin coating process or a drop coating process3C2The nano-sheet dispersion liquid is coated on the conductive substrate, and Ti is formed on the conductive substrate after the nano-sheet dispersion liquid is dried to volatilize the solvent3C2And the nano sheet film layer.
The field emission cathode provided by the embodiment of the invention is Ti3C2Nanosheet being an emissive layer material, Ti3C2The nano-sheet has abundant linear edge structures, in the field emission process, the edge structures of the rest parts can still play a field emission role under the condition that one part of the edge is damaged by cation bombardment, and in addition, new edge structures can be exposed at the edge parts damaged by the cation bombardment for field emission. Thus, Ti is comparable to existing graphene or carbon nanotube materials3C2The nanosheet has richer edge structures, can better resist bombardment damage of cations and keep the structural integrity, and obtains more stable emission current.
The preparation method of the field emission cathode provided by the embodiment of the invention has the advantages of simple process flow and easy realization of process conditions, and is beneficial to large-scale industrial application.
Drawings
Fig. 1 is a schematic structural view of a field emission electrode in an embodiment of the present invention;
FIGS. 2a and 2b are Ti in examples of the present invention3C2TEM images of the nanoplates;
FIGS. 3a and 3b are Ti in examples of the present invention3C2SEM image of the nano-sheet film layer;
fig. 4a and 4b are graphs illustrating electrical tests performed on the field emission electrode in accordance with an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in detail below with reference to the accompanying drawings. Examples of these preferred embodiments are illustrated in the accompanying drawings. The embodiments of the invention shown in the drawings and described in accordance with the drawings are exemplary only, and the invention is not limited to these embodiments.
It should be noted that, in order to avoid obscuring the present invention with unnecessary details, only the structures and/or processing steps closely related to the scheme according to the present invention are shown in the drawings, and other details not so relevant to the present invention are omitted.
Embodiments of the present invention first provide a field emission cathode, as shown in fig. 1, which includes a conductive substrate 1 and Ti formed on the conductive substrate 13C2And a nanosheet film layer 2.
In this embodiment, the conductive substrate 1 is selected from ito conductive glass, Ti3C2The thickness of the nanosheet film layer 2 is 5 μm.
In some further embodiments: the conductive substrate 1 can also be selected from metal substrates formed by at least one of iron, titanium, copper, chromium, cobalt, nickel, tungsten, molybdenum, tantalum and platinum as a base material; alternatively, the conductive substrate 1 is selected to be a silicon wafer. The Ti3C2The thickness of the nanosheet thin-film layer 2 may be set within a range of 1 μm to 10 μm.
The field emission electrode provided by the above embodiment is provided with Ti3C2Nanosheet being an emissive layer material, Ti3C2The nano-sheet has abundant linear edge structures, in the field emission process, the edge structures of the rest parts can still play a field emission role under the condition that one part of the edge is damaged by cation bombardment, and in addition, new edge structures can be exposed at the edge parts damaged by the cation bombardment for field emission. Thus, Ti is comparable to existing graphene or carbon nanotube materials3C2The nanosheet has richer edge structures, can better resist bombardment damage of cations and keep the structural integrity, and obtains more stable emission current.
The embodiment of the invention also provides a preparation method of the field emission cathode, which comprises the following steps:
and S1, providing a conductive substrate.
As mentioned above, the conductive substrate 1 in this embodiment is selected from ito conductive glass.
S2, preparing Ti3C2A nanosheet dispersion.
Specifically, Ti is provided3C2Nanosheet material, the Ti3C2Adding a nanosheet raw material into a solvent, performing ultrasonic stirring, and performing centrifugal treatment to obtain the Ti3C2A nanosheet dispersion.
In this example, the solvent is selected from ethanol and Ti3C2Ti in nanosheet dispersion3C2The concentration of the nano-sheets is 2 mg/mL.
In other embodiments, the solvent may also be selected from water, Ti3C2Ti in nanosheet dispersion3C2The concentration of the nanosheets may be set within the range of 1mg/mL to 5 mg/mL.
In this example, the conditions of ultrasonic agitation were: the ultrasonic power is 100W, and the ultrasonic time is 20 min.
In other embodiments, the ultrasonic power may be set in the range of 100W to 500W, and the ultrasonic time may be set in the range of 10min to 20 min.
The true bookIn the examples, the Ti3C2The nano sheet raw material is prepared by the following process:
s10, under the condition of continuous stirring, adding Ti3AlC2And adding the layered material into an HF solution or a mixed solution of HCl and LiF, and etching to remove the Al intermediate layer to obtain a first intermediate product.
Wherein, the reaction temperature can be set within the range of 25-50 ℃ and the reaction time is set within the range of 24-48 h. Further, after the reaction is finished, washing the solid-phase product with deionized water, and performing centrifugal separation until the pH value of supernatant is 6-7 to finally obtain a first intermediate product of the solid phase.
S20, adding the first intermediate product into deionized water, carrying out ultrasonic stripping under the protection of inert gas, and after the stripping is finished, centrifugally separating out supernatant to obtain Ti3C2A nanosheet solution.
Wherein, the ultrasonic stripping is carried out at the temperature of below 25 ℃, and the time of the ultrasonic stripping can be selected within the range of 0.5 h-1 h; the speed of centrifugal separation is preferably set within the range of 4000r/min to 8000r/min, and the centrifugal time is 1h to 2 h.
S30, mixing the Ti3C2Drying the nanosheet solution to obtain Ti3C2A nano-sheet powder raw material.
Among them, the drying treatment process is preferably drying treatment under vacuum condition.
FIGS. 2a and 2b are Ti in the above examples3C2TEM images of the nanoplates at different magnifications. As can be seen from FIGS. 2a and 2b, the nanosheet structure prepared by the above process steps is rich in sharp-edged structures, indicating that Ti3AlC2The layered structure was successfully exfoliated to Ti3C2Nanosheets.
In some other embodiments, the Ti3C2The nano-sheet raw material can also be directly prepared from Ti which is obtained in the market3C2Nanosheets.
S3, mixing the Ti3C2The nano-sheet dispersion is coated on the conductive substrateForming Ti on a conductive substrate3C2And the nano sheet film layer.
In this example, the Ti was deposited by electrophoretic deposition3C2The nanosheet dispersion is coated on the conductive substrate. The method specifically comprises the following steps:
step one, adding Ti3C2Adding metal inorganic salt into the nano-sheet dispersion liquid as a reaction solution. The metal inorganic salt is selected from magnesium chloride, magnesium chloride and Ti3C2The mass ratio of the nano sheets is 1: 2.
In other embodiments, the metal inorganic salt is magnesium nitrate, and the metal inorganic salt and Ti are added3C2The mass ratio of the nanosheets can be set at 1: (1-2).
Secondly, placing the conductive substrate as a cathode and another electrode as an anode in the reaction solution, and enabling Ti in the reaction solution to be under the action of direct current voltage3C2Nanoplate deposited on the conductive substrate, forming Ti on the conductive substrate3C2And the nano sheet film layer. Wherein, the applied direct current voltage is preferably 100V-150V, and the time is 1 min-5 min.
FIGS. 3a and 3b are Ti in the above examples3C2SEM images of different magnifications of the nanosheet thin film layer. As can be seen from FIGS. 3a and 3b, Ti on the surface of the thin film layer in this example3C2The nano sheets are uniformly distributed and randomly oriented, so that uniform field emission can be realized, instability of emission current caused by failure due to over emission of local nano sheets is avoided, and the emission stability of the field emission cathode is improved.
It should be noted that in other embodiments, the Ti can be selectively applied by spin coating or drop coating3C2The nanosheet dispersion is coated onto the conductive substrate and dried (e.g., vacuum dried) to volatilize the solvent and form Ti on the conductive substrate3C2And the nano sheet film layer.
FIGS. 4a and 4b are graphs showing electrical property tests of the field emission cathode in the above embodimentsFig. 4a is a graph of voltage versus current, and fig. 4b is a graph of time versus current. As can be seen from FIG. 4a, the field emission cathode provided by the embodiment of the present invention can obtain a large emission current density (19 mA/cm) at a low voltage (4300V)2) And has good field emission I-V characteristics. As can be seen from fig. 4b, the field emission cathode provided by the embodiment of the present invention emits continuously for 250min, and the current is not substantially attenuated, so that the field emission cathode has excellent current emission stability.
In summary, the field emission electrode provided in the embodiments of the invention is made of Ti3C2The nano-sheet is an emission layer material, and has abundant linear edge structures, so that the structural integrity can be kept by better resisting the bombardment damage of cations in the field emission process, and more stable emission current and higher emission current density can be obtained.
The foregoing is directed to embodiments of the present application and it is noted that numerous modifications and adaptations may be made by those skilled in the art without departing from the principles of the present application and are intended to be within the scope of the present application.
Claims (10)
1. A field emission cathode comprising a conductive substrate and Ti formed on the conductive substrate3C2And the nano sheet film layer.
2. The field emission cathode of claim 1, wherein the Ti is3C2The thickness of the nano-sheet film layer is 1-10 mu m.
3. The field emission cathode as claimed in claim 1 or 2, wherein the conductive substrate is selected from metal substrates formed with at least one of base materials of iron, titanium, copper, chromium, cobalt, nickel, tungsten, molybdenum, tantalum, and platinum; or, the conductive substrate is indium tin oxide conductive glass or silicon chip.
4. A method of making a field emission cathode according to any of claims 1 to 3, comprising:
providing a conductive substrate;
preparing Ti3C2A nanosheet dispersion;
adding the Ti3C2The nanosheet dispersion is coated on the conductive substrate to form Ti on the conductive substrate3C2And the nano sheet film layer.
5. The method of claim 4, wherein the Ti formulation is selected from the group consisting of Ti3C2The nanoplate dispersion comprises: providing Ti3C2Nanosheet material, the Ti3C2Adding a nanosheet raw material into a solvent, performing ultrasonic stirring, and performing centrifugal treatment to obtain the Ti3C2A nanosheet dispersion.
6. The method of claim 5, wherein the Ti is selected from the group consisting of Ti, and Ti3C2In the nanosheet dispersion, Ti3C2The concentration of the nano-sheet is 1 mg/mL-5 mg/mL.
7. The method for preparing a field emission cathode of claim 5, wherein the ultrasonic power of the ultrasonic agitation is 100W-500W, and the time is 10 min-20 min.
8. The method of claim 5, wherein the Ti is selected from the group consisting of Ti, and Ti3C2The nano sheet raw material is prepared by the following process:
s10, under the condition of continuous stirring, adding Ti3AlC2Adding the layered material into an HF solution or a mixed solution of HCl and LiF, and etching to remove the Al intermediate layer to obtain a first intermediate product;
s20, adding the first intermediate product into deionized water, carrying out ultrasonic stripping under the protection of inert gas, and after the stripping is finishedSeparating the supernatant by centrifugation to obtain Ti3C2A nanosheet solution;
s30, mixing the Ti3C2Drying the nanosheet solution to obtain Ti3C2A nano-sheet powder raw material.
9. The method of any one of claims 5-8, wherein the Ti is deposited by electrophoretic deposition3C2The nanosheet dispersion is coated on the conductive substrate and includes:
to the Ti3C2Adding metal inorganic salt into the nanosheet dispersion liquid to serve as a reaction solution;
placing the conductive substrate as a cathode and another electrode as an anode in the reaction solution, and allowing Ti in the reaction solution to react under the action of DC voltage3C2Nanoplate deposited on the conductive substrate, forming Ti on the conductive substrate3C2And the nano sheet film layer.
10. The method of preparing a field emission cathode as claimed in any one of claims 5 to 8, wherein the Ti is applied by a spin coating process or a drop coating process3C2The nano-sheet dispersion liquid is coated on the conductive substrate, and Ti is formed on the conductive substrate after the nano-sheet dispersion liquid is dried to volatilize the solvent3C2And the nano sheet film layer.
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| CN1876898A (en) * | 2005-06-07 | 2006-12-13 | 东元电机股份有限公司 | Electronic emission source preparation method by batch electrophoresis deposition of carbon nanotube |
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