CN113097032B - Long-life micro-column array graphite and metal composite cathode structure and preparation method thereof - Google Patents
Long-life micro-column array graphite and metal composite cathode structure and preparation method thereof Download PDFInfo
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- CN113097032B CN113097032B CN202110443718.8A CN202110443718A CN113097032B CN 113097032 B CN113097032 B CN 113097032B CN 202110443718 A CN202110443718 A CN 202110443718A CN 113097032 B CN113097032 B CN 113097032B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J23/00—Details of transit-time tubes of the types covered by group H01J25/00
- H01J23/02—Electrodes; Magnetic control means; Screens
- H01J23/04—Cathodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J25/00—Transit-time tubes, e.g. klystrons, travelling-wave tubes, magnetrons
- H01J25/34—Travelling-wave tubes; Tubes in which a travelling wave is simulated at spaced gaps
- H01J25/42—Tubes in which an electron stream interacts with a wave travelling along a delay line or equivalent sequence of impedance elements, and with a magnet system producing an H-field crossing the E-field
- H01J25/46—Tubes in which an electron stream interacts with a wave travelling along a delay line or equivalent sequence of impedance elements, and with a magnet system producing an H-field crossing the E-field the backward travelling wave being utilised
Abstract
The invention relates to a maser, in particular to a long-service-life micropillar array graphite and metal composite cathode structure for a maser and a preparation method thereof. The invention aims to solve the technical problems that the prior micro-column graphite cathode structure has serious consumption of a convex emission structure and even completely loses the convex emission structure, so that the effect of stably emitting electron beam is lost, and the porous structure of a graphite material is easy to release gas after electron beam bombardment, so that the vacuum degree of a system is reduced, the coupling efficiency of beam waves is reduced and the insulativity of a system device is reduced. The cathode structure comprises a micropillar array graphite cathode, the micropillar array graphite cathode comprises a knife-edge-shaped annular graphite cathode matrix and a plurality of graphite micropillars arranged on the surface of the knife edge of the knife-edge-shaped annular graphite cathode matrix in an array manner, and the improvement is that: the surface of the knife-edge-shaped annular graphite cathode matrix and the top and the side wall of each graphite microcolumn are uniformly adhered with a metal coating, and the metal coating adopts refractory metal.
Description
Technical Field
The invention relates to a maser, in particular to a long-service-life micropillar array graphite and metal composite cathode structure for a maser and a preparation method thereof.
Background
The repetition frequency relativistic return wave tube is a high-power microwave source with great development potential. The cathode of the relativity back-wave tube is a key component, and is mainly used for emitting and generating a strong current electron beam under the drive of high-power pulse. With the development of high-power microwave devices towards a higher average power direction, the cathode is required to have the characteristics of large current emission density, long service life, short rise time of electron beam current, low plasma expansion speed, good stability of emitted electron beam current and the like (mentioned in the university of national defense science and technology, research on the emission and collection characteristics of high-current electron beam of carbide modified graphite materials in the school paper of 2019 years). In order to meet higher application requirements, the prior art adopts a micro-column array graphite cathode structure, the cathode surface of the structure is a columnar graphite column array structure, the diameter of a column is in the order of tens of micrometers to hundreds of micrometers (Wang Gang, su Jiancang, liu Wenyuan and the like are mentioned in "micro-column graphite cathode gas switch breakdown characteristic research" which is intensively published in the paper of south Beijing 2018 "conference on national high voltage and discharge plasma academy of sciences"). Under the drive of high-power pulse, the microcolumn structure effectively improves the stability of electron beam emitted by the cathode and shortens the rising time of the electron beam. However, since the raised points (i.e., the top ends of the micro-column structures) constructed in the micro-column graphite cathode structure are electron beam emission points, the high emission beam density thereof makes the current density at the emission points very high, so that the raised emission points in the micro-column graphite cathode structure are extremely severely consumed, and even fall off due to micro-explosion impact generated in the electron emission process, the surface of the micro-column graphite cathode is finally caused to completely lose the raised emission structure, and the effect of stabilizing the emission electron beam is lost. In addition, the porous structure of the graphite material itself makes it prone to outgassing after electron beam bombardment, resulting in a decrease in the vacuum level of the system, a decrease in the coupling efficiency of the beam waves, and a decrease in the insulation of the system devices (Tang Yunsheng, chen Changhua, and Liu Wenyuan are equivalent to those mentioned in the publication "effect of deposition temperature on the microscopic morphology and conductivity of TiC coatings" by the article "020801 in volume 11 of the journal" modern applied Physics ").
Disclosure of Invention
The invention aims to solve the technical problems that the prior micro-column graphite cathode structure has serious consumption of a convex emission structure and even completely loses the convex emission structure, so that the effect of stably emitting electron beam is lost, and the porous structure of a graphite material is easy to release gas after electron beam bombardment, so that the vacuum degree of a system is reduced, the coupling efficiency of beam waves is reduced and the insulativity of a system device is reduced.
In order to solve the technical problems, the technical solution provided by the invention is as follows:
the invention also provides a long-life micropillar array graphite and metal composite cathode structure, which comprises a micropillar array graphite cathode, wherein the micropillar array graphite cathode comprises a knife-edge-shaped annular graphite cathode matrix and a plurality of graphite micropillars arranged on the surface of the knife edge of the knife-edge-shaped annular graphite cathode matrix in an array manner; the knife edge shape is that the thickness of the ring shape is very narrow; the special feature is that:
the surface of the knife-edge-shaped annular graphite cathode matrix and the top and the side wall of each graphite microcolumn are uniformly adhered with a metal coating, and the metal coating adopts refractory metal.
Further, the material of the metal coating is one or more of Mo, W, hf, ta, zr, ti, cr, V.
Further, the thickness of the metal coating is in the range of 0.01-50 μm.
Further, the thickness of the metal coating is in the range of 1 to 10 μm.
Further, the diameter of the graphite micropillars is 5-300 mu m, and the ratio of the height to the diameter is 1: 1-20: 1, the distance between the axes of adjacent graphite micropillars is 20-500 mu m.
Further, the graphite micro-column array on the micro-column array graphite cathode is obtained by etching the surface of the knife edge-shaped annular graphite cathode matrix by ultraviolet laser.
The invention also provides a preparation method of the long-life micro-column array graphite and metal composite cathode structure, which is characterized by comprising the following steps as shown in fig. 3:
1) Processing graphite into a knife-edge annular graphite cathode matrix shown in figure 1, cleaning and drying;
2) Constructing a graphite micro-column array on the surface of a knife edge of the dried knife edge-shaped annular graphite cathode matrix by an ultraviolet laser etching mode to obtain a micro-column array graphite cathode shown in figure 2, and cleaning and drying the micro-column array graphite cathode;
3) Placing the dried micro-column array graphite cathode electrode in a chemical vapor deposition furnace, and increasing the temperature of a hearth to 300-1200 ℃ at a constant heating rate;
4) Introducing hydrogen into a hearth of the chemical vapor deposition furnace as reducing gas, and keeping the pressure of the hearth at 0.1-20 kPa;
5) Heating the metal compound of refractory metal to complete gasification, and introducing the metal compound into a hearth at a constant flow rate to perform a reduction reaction for 0.5-10 h;
6) Stopping introducing hydrogen, naturally cooling, and obtaining the long-life micro-column array graphite and metal composite cathode structure.
Further, in the step 3), the heating rate is 5-10 ℃/min;
the temperature of the hearth is raised to 500-800 ℃.
Further, in step 5), the metal compound is a metal chloride;
the metal in the metal compound is one or more of Mo, W, hf, ta, zr, ti, cr, V.
Further, in the step 5), the duration of the reduction reaction is 2-5 h.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a long-life micropillar array graphite and metal composite cathode structure and a preparation method thereof. Under the drive of high-power pulse, the electron emission positions are all at the top end of the microcolumn, and the emission process has little influence on the surface morphology of the microcolumn, and the graphite microcolumn array with the composite cathode structure can stably and uniformly emit electrons, so that the problems of random change and large fluctuation of the electron emission positions of the conventional graphite cathode are solved, and the problem of short service life of the microcolumn under the condition of high emission beam density is solved. In addition, the composite cathode structure can effectively reduce the generation of cathode surface plasmas and improve the long-time stable working capacity of a high-power microwave system.
2. The long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof adopt a preparation way of combining laser etching with a chemical vapor deposition method. Firstly, processing graphite into a graphite cathode with a required shape, then etching a micro-column array with a certain specification on the surface of the cathode by utilizing an ultraviolet laser etching method, placing the micro-column array graphite cathode in a chemical vapor deposition furnace, and preparing a metal coating under a certain condition to finally obtain the composite cathode structure of the micro-column array graphite and metal. According to the microcolumn array graphite and metal composite cathode structure prepared by the invention, under the drive of high-power pulse, each microcolumn can effectively emit electrons, the beam stability is good, the volatility is small, the uniformity is good, the beam rising time is short, the microcolumn array graphite and metal composite cathode structure has the characteristics of high toughness, high strength and high melting point of metal, and in the electron emission process, the microcolumn can effectively inhibit cracking and falling of graphite microcolumns and the outgassing of graphite materials, and the cathode can be ensured to stably operate for a long time in the high-voltage emission process.
3. The long-life micropillar array graphite and metal composite cathode structure and the preparation method thereof provided by the invention have the advantages that the metal coating is prepared by chemical vapor deposition, the bonding performance with the graphite micropillar is good, and the metal coating is not easy to fall off in the use process.
4. According to the long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof, provided by the invention, due to the deposition characteristics of a chemical vapor deposition method, the deposition rate of metal around the top of the micro-column is lower than that around the bottom of the micro-column, so that the length-diameter ratio of the graphite and metal composite micro-column is moderate, the micro-column can be effectively prevented from being broken due to a larger length-diameter ratio (the ratio of height to diameter), and the uniformity of emitted beam current is ensured.
5. The long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof provided by the invention adopt graphite and refractory metal, and the plasma expansion speed of the refractory metal is low and the mass loss is small.
6. The long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof provided by the invention have the advantages that the thickness of the metal coating is generally in the range of 0.01-50 mu m, preferably can be controlled in the range of 1-10 mu m, and the service life is longer.
Drawings
FIG. 1 is a cross-sectional view of a knife-edge annular graphite cathode substrate in accordance with the present invention, a being the knife edge;
FIG. 2 is a schematic diagram of a micropillar array graphite cathode of the present invention, showing only the micropillar array at the knife edge;
FIG. 3 is a flow chart of a method for preparing a composite cathode structure of long-life micropillar array graphite and metal of the present invention;
FIG. 4 is a scanning electron microscope image of a graphite cathode of a micro-column array obtained in example 1 of the present invention;
FIG. 5 shows a long-life micro-column array graphite and M obtained in example 1 of the present invention O Scanning electron microscope images of the composite cathode structure;
FIG. 6 shows a long-life micro-column array graphite and M obtained in example 1 of the present invention O Surface analysis EDS plot of the composite cathode structure of (c).
Detailed Description
The invention is further described below with reference to the drawings and examples.
Example 1
1) Processing graphite into a knife-edge-shaped annular graphite cathode matrix, wherein the outer diameter (namely the outer ring diameter) of the knife-edge-shaped annular graphite cathode matrix is 50mm, and the wall thickness (namely the outer ring radius minus the inner ring radius) is 1mm; ultrasonically cleaning the raw materials in ethanol, and drying the raw materials in an oven for standby;
2) By ultraviolet laser etching, a graphite micro-column array is constructed on the surface of the knife edge of the dried knife edge-shaped annular graphite cathode matrix, the diameter of the graphite micro-column is 20 mu m, and the ratio of the height to the diameter is 6:1, obtaining a micropillar array graphite cathode with the distance between the axes of adjacent graphite micropillars being 60 mu m, performing low-power ultrasonic cleaning on the micropillar array graphite cathode in ethanol to remove scraps around the graphite micropillars, and placing the micropillars in an oven for drying for later use;
3) Placing the dried micropillar array graphite cathode electrode in a chemical vapor deposition furnace, and heating the hearth temperature to 600 ℃ at a heating rate of 10 ℃/min;
4) Introducing hydrogen into a hearth of a chemical vapor deposition furnace at a flow rate of 100mL/min as a reducing gas, and keeping the pressure of the hearth at 5 kPa;
5) MoCl is added to 5 Heating to 300 ℃ to completely gasify, and introducing the mixture into a hearth at a flow rate of 30mL/min to perform reduction reaction for 3h;
6) And stopping introducing hydrogen, and naturally cooling to obtain the long-life micro-column array graphite and Mo composite cathode structure.
Fig. 4 is a scanning electron microscope image of a micro-column array graphite cathode, fig. 5 is a scanning electron microscope image of a long-life micro-column array graphite and Mo composite cathode structure, fig. 6 is a surface analysis EDS image of a long-life micro-column array graphite and Mo composite cathode structure, and tests show that: the Mo coating is uniformly adhered to the surface of the knife-edge-shaped annular graphite cathode matrix and the top and side walls of each graphite microcolumn.
Example 2
1) Processing graphite into a knife-edge-shaped annular graphite cathode matrix, wherein the outer diameter (namely the outer ring diameter) of the knife-edge-shaped annular graphite cathode matrix is 100mm, and the wall thickness (namely the outer ring radius minus the inner ring radius) is 1.5mm; ultrasonically cleaning the raw materials in ethanol, and drying the raw materials in an oven for standby;
2) By ultraviolet laser etching, a graphite micropillar array is constructed on the surface of the knife edge of the dried knife edge-shaped annular graphite cathode matrix, the diameter of the graphite micropillar is 40 mu m, and the ratio of the height to the diameter is 5:1, obtaining a micropillar array graphite cathode with the distance between the axes of adjacent graphite micropillars being 100 mu m, performing low-power ultrasonic cleaning on the micropillar array graphite cathode in ethanol to remove scraps around the graphite micropillars, and placing the micropillars in an oven for drying for later use;
3) Placing the dried micropillar array graphite cathode electrode in a chemical vapor deposition furnace, and increasing the temperature of a hearth to 700 ℃ at a heating rate of 10 ℃/min;
4) Introducing hydrogen into a hearth of a chemical vapor deposition furnace at a flow rate of 150mL/min as reducing gas, and keeping the pressure of the hearth at 1kPa;
5) WCl (WCl) 6 Heating to 350 ℃ to completely gasify, and introducing the mixture into a hearth at a flow rate of 50mL/min to perform reduction reaction for 2h;
6) Stopping introducing hydrogen, naturally cooling, and obtaining the long-life micro-column array graphite and W composite cathode structure.
Example 3
1) Processing graphite into a knife-edge-shaped annular graphite cathode matrix, wherein the outer diameter (namely the outer ring diameter) of the knife-edge-shaped annular graphite cathode matrix is 50mm, and the wall thickness (namely the outer ring radius minus the inner ring radius) is 1mm; ultrasonically cleaning the raw materials in ethanol, and drying the raw materials in an oven for standby;
2) By ultraviolet laser etching, a graphite micro-column array is constructed on the surface of the knife edge of the dried knife edge-shaped annular graphite cathode matrix, the diameter of the graphite micro-column is 5 mu m, and the ratio of the height to the diameter is 20:1, obtaining a micropillar array graphite cathode with the distance between the axes of adjacent graphite micropillars being 20 mu m, performing low-power ultrasonic cleaning on the micropillar array graphite cathode in ethanol to remove scraps around the graphite micropillars, and placing the micropillars in an oven for drying for later use;
3) Placing the dried micropillar array graphite cathode electrode in a chemical vapor deposition furnace, and increasing the temperature of a hearth to 800 ℃ at a heating rate of 5 ℃/min;
4) Introducing hydrogen into a hearth of a chemical vapor deposition furnace at a flow rate of 100mL/min as a reducing gas, and keeping the pressure of the hearth at 0.1 kPa;
5) TiCl is added to the mixture 4 Heating to complete gasification, introducing the mixture into a hearth at a flow rate of 30mL/min, and carrying out reduction reaction for 0.5h;
6) And stopping introducing hydrogen, and naturally cooling to obtain the long-life micro-column array graphite and Ti composite cathode structure.
Example 4
1) Processing graphite into a knife-edge-shaped annular graphite cathode matrix, wherein the outer diameter (namely the outer ring diameter) of the knife-edge-shaped annular graphite cathode matrix is 50mm, and the wall thickness (namely the outer ring radius minus the inner ring radius) is 1mm; ultrasonically cleaning the raw materials in ethanol, and drying the raw materials in an oven for standby;
2) By ultraviolet laser etching, a graphite micro-column array is constructed on the surface of the knife edge of the dried knife edge-shaped annular graphite cathode matrix, the diameter of the graphite micro-column is 300 mu m, and the ratio of the height to the diameter is 1:1, obtaining a micropillar array graphite cathode with the distance between the axes of adjacent graphite micropillars being 500 mu m, washing the micropillar array graphite cathode in ethanol with low-power ultrasound to remove scraps around the graphite micropillars, and placing the micropillars in an oven for drying for standby;
3) Placing the dried micropillar array graphite cathode electrode in a chemical vapor deposition furnace, and increasing the temperature of a hearth to 1200 ℃ at a heating rate of 8 ℃/min;
4) Introducing hydrogen into a hearth of a chemical vapor deposition furnace at a flow rate of 100mL/min as a reducing gas, and keeping the pressure of the hearth at 20kPa;
5) ZrCl is added to 4 Heating to complete gasification, introducing the mixture into a hearth at a flow rate of 30mL/min, and carrying out reduction reaction for 10h;
6) And stopping introducing hydrogen, and naturally cooling to obtain the long-life micro-column array graphite and Zr composite cathode structure.
Finally, it should be noted that: the foregoing embodiments are merely for illustrating the technical solutions of the present invention, and not for limiting the same, and it will be apparent to those skilled in the art that modifications may be made to the specific technical solutions described in the foregoing embodiments, or equivalents may be substituted for some of the technical features thereof, without departing from the spirit of the technical solutions protected by the present invention.
Claims (9)
1. The preparation method of the long-life micro-column array graphite and metal composite cathode structure comprises a micro-column array graphite cathode, wherein the micro-column array graphite cathode comprises a knife-edge-shaped annular graphite cathode matrix and a plurality of graphite micro-columns arranged on the surface of a knife edge of the knife edge-shaped annular graphite cathode matrix in an array manner; the surface of the knife-edge-shaped annular graphite cathode matrix and the top and the side wall of each graphite microcolumn are uniformly adhered with a metal coating, and the metal coating adopts refractory metal;
the method is characterized by comprising the following steps:
1) Processing graphite into a knife-edge annular graphite cathode matrix, cleaning and drying the graphite;
2) Constructing a graphite micro-column array on the surface of the knife edge of the dried knife edge-shaped annular graphite cathode matrix by an ultraviolet laser etching mode to obtain a micro-column array graphite cathode, and cleaning and drying the micro-column array graphite cathode;
3) Placing the dried micro-column array graphite cathode electrode in a chemical vapor deposition furnace, and increasing the temperature of a hearth to 300-1200 ℃ at a constant heating rate;
4) Introducing hydrogen into a hearth of the chemical vapor deposition furnace as reducing gas, and keeping the pressure of the hearth at 0.1-20 kPa;
5) Heating the metal compound of refractory metal to complete gasification, and introducing the metal compound into a hearth at a constant flow rate to perform a reduction reaction for 0.5-10 h;
6) Stopping introducing hydrogen, naturally cooling, and obtaining the long-life micro-column array graphite and metal composite cathode structure.
2. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 1, which is characterized in that:
in the step 3), the heating rate is 5-10 ℃/min;
the temperature of the hearth is raised to 500-800 ℃.
3. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 2, which is characterized in that:
in step 5), the metal compound is a metal chloride;
the metal in the metal compound is one or more of Mo, W, hf, ta, zr, ti, cr, V.
4. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 3, which is characterized in that:
in the step 5), the duration of the reduction reaction is 2-5 h.
5. The method for preparing the long-life micro-column array graphite and metal composite cathode structure, according to claim 4, is characterized in that:
the thickness of the metal coating is in the range of 0.01-50 mu m.
6. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 5, which is characterized in that:
the thickness of the metal coating is in the range of 1-10 mu m.
7. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to any one of claims 1 to 6, which is characterized in that:
the material of the metal coating is one or more of Mo, W, hf, ta, zr, ti, cr, V.
8. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 7, which is characterized in that:
the diameter of the graphite micro-column is 5-300 mu m, and the ratio of the height to the diameter is 1: 1-20: 1, the distance between the axes of adjacent graphite micropillars is 20-500 mu m.
9. The method for preparing the long-life micro-column array graphite and metal composite cathode structure, according to claim 8, is characterized in that:
the graphite micro-column array on the micro-column array graphite cathode is obtained by etching the surface of the knife edge-shaped annular graphite cathode matrix by ultraviolet laser.
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