CN113097032A - 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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- CN113097032A CN113097032A CN202110443718.8A CN202110443718A CN113097032A CN 113097032 A CN113097032 A CN 113097032A CN 202110443718 A CN202110443718 A CN 202110443718A CN 113097032 A CN113097032 A CN 113097032A
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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
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- 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-life micro-column 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 existing micro-column graphite cathode structure has serious consumption of a convex emission structure, even completely loses the convex emission structure, so that the effect of stably emitting electron beam current is lost, and the porous structure of a graphite material is easy to outgas after being bombarded by electron beams, so that the vacuum degree of a system is reduced, the coupling efficiency of beam waves is reduced, and the insulativity of system devices is reduced. The cathode structure comprises a micro-column array graphite cathode, the micro-column array graphite cathode comprises a knife-edge-shaped annular graphite cathode substrate and a plurality of graphite micro-columns arranged on the surface of the knife edge of the knife-edge-shaped annular graphite cathode substrate in an array manner, and the improvement is as follows: and metal coatings are uniformly adhered to the surface of the knife-edge-shaped annular graphite cathode substrate and the top end and the side wall of each graphite microcolumn, and the metal coatings are made of refractory metals.
Description
Technical Field
The invention relates to a maser, in particular to a long-life micro-column array graphite and metal composite cathode structure for a maser and a preparation method thereof.
Background
The repetition frequency relativistic backward wave tube is a high-power microwave source with great development potential. The cathode of the relativistic backward wave tube is a key component of the relativistic backward wave tube and is mainly used for emitting and generating a high-current electron beam under the driving of high-power pulse. With the development of high power microwave devices towards higher average power, the cathode is required to have the characteristics of high current emission density, long service life, short electron beam rise time, low plasma expansion speed, good stability of emitted electron beams and the like (mentioned in the research on emission and collection characteristics of high current electron beams of carbide modified graphite materials in the academic paper of 2019 of national defense science and technology university). 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, and the diameter of a column is in the order of tens of micrometers to hundreds of micrometers (the diameters of the columns are mentioned in a 'micro-column graphite cathode gas switch breakdown characteristic research' published in a paper of wanggang, soviet warehouse, liuwenyuan and the like in 2018 Nanjing, "2018 national high voltage and discharge plasma academic conference". Under the drive of high-power pulses, the microcolumn structure effectively improves the stability of the electron beam emitted by the cathode and shortens the rise time of the electron beam. However, since the protruding point (i.e. the top end of the micro-column structure) constructed in the micro-column graphite cathode structure is an electron beam emission point, the current density at the emission point is very high due to the high emission beam density, and thus the consumption of the protruding emission point in the micro-column graphite cathode structure is very serious, and even the protruding emission point falls off due to the micro-explosion impact generated in the process of emitting electrons, the surface of the micro-column graphite cathode completely loses the protruding emission structure, and the effect of stably emitting electron beams is lost. In addition, the graphite material is easy to outgas after being bombarded by electron beams due to the porous structure of the graphite material, which causes the reduction of the vacuum degree of a system, the reduction of the coupling efficiency of beam waves and the reduction of the insulation performance of system devices (mentioned in the article "influence of deposition temperature on the micro-morphology and the electric conductivity performance of the TiC coating" published in volume 11, 2, 020801 of journal of modern applied physics in the 2020, Tang Yuan, Chengchang and Liu Wen Yuan are equal to).
Disclosure of Invention
The invention aims to solve the technical problems that the existing micro-column graphite cathode structure has serious consumption of a convex emission structure, even completely loses the convex emission structure, so that the effect of stably emitting electron beam current is lost, and the porous structure of a graphite material is easy to outgas after being bombarded by electron beams, so that the vacuum degree of a system is reduced, the coupling efficiency of beam waves is reduced, and the insulativity of system devices is reduced, and provides a long-life micro-column array graphite and metal composite cathode structure and a preparation method thereof.
In order to solve the technical problems, the technical solution provided by the invention is as follows:
the invention also provides a long-life micro-column array graphite and metal composite cathode structure, which comprises a micro-column array graphite cathode, wherein the micro-column array graphite cathode comprises a knife-edge-shaped annular graphite cathode substrate and a plurality of graphite micro-columns arranged on the surface of the knife edge of the knife-edge-shaped annular graphite cathode substrate in an array manner; the knife edge shape means that the thickness of the ring shape is very narrow; it is characterized in that:
and metal coatings are uniformly adhered to the surface of the knife-edge-shaped annular graphite cathode substrate and the top end and the side wall of each graphite microcolumn, and the metal coatings are made of refractory metals.
Further, the material of the metal coating is one or more of Mo, W, Hf, Ta, Zr, Ti, Cr and V.
Further, the thickness of the metal coating is within the range of 0.01-50 mu m.
Further, the thickness of the metal coating is within the range of 1-10 mu m.
Further, the diameter of the graphite microcolumn is 5 to 300 μm, and the ratio of the height to the diameter is 1: 1-20: 1, the distance between the axes of the adjacent graphite microcolumns 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 edge-shaped annular graphite cathode substrate 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 figure 3:
1) processing graphite into a knife-edge-shaped annular graphite cathode matrix shown in figure 1, cleaning and drying the graphite cathode matrix;
2) constructing a graphite micro-column array on the surface of the dried knife-edge-shaped annular graphite cathode substrate at the knife edge a in an ultraviolet laser etching mode to obtain a micro-column array graphite cathode shown in figure 2, and cleaning and drying the graphite cathode;
3) placing the dried micro-column array graphite cathode electrode in a chemical vapor deposition furnace, and raising the temperature of a hearth to 300-1200 ℃ at a constant temperature raising rate;
4) introducing hydrogen into a hearth of the chemical vapor deposition furnace to serve as reducing gas, and keeping the pressure of the hearth at 0.1-20 kPa;
5) heating a metal compound of refractory metal until the metal compound is completely gasified, introducing the metal compound into a hearth at a constant flow rate, and carrying out reduction reaction for 0.5-10 h;
6) stopping introducing hydrogen, and naturally cooling to obtain the long-life micro-column array graphite and metal composite cathode structure.
Further, in the step 3), the heating rate is 5-10 ℃/min;
and raising the temperature of the hearth 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 and V.
Further, in the step 5), the time 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 micro-column array graphite and metal composite cathode structure and a preparation method thereof. Under the drive of high-power pulse, because the electron emission positions are all at the top end of the microcolumn, and the emission process has little influence on the surface appearance of the microcolumn, the graphite microcolumn array with the composite cathode structure can stably and uniformly emit electrons, thereby not only solving the problems of random change of the electron emission positions and large volatility of the conventional graphite cathode, but also solving the difficult problem of short service life of the microcolumn under high emission beam current density. In addition, the composite cathode structure can effectively reduce the generation of plasma on the surface of the cathode and improve the long-time stable working capability 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 approach of combining laser etching with a chemical vapor deposition method. Firstly processing graphite into a graphite cathode in a required shape, then etching a micro-column array with a certain specification on the surface of the cathode by using an ultraviolet laser etching method, then placing the graphite cathode of the micro-column array in a chemical vapor deposition furnace, preparing a metal coating under a certain condition, and finally obtaining the composite cathode structure of the graphite of the micro-column array and metal. According to the prepared micro-column array graphite and metal composite cathode structure, under the drive of high-power pulses, each micro-column can effectively emit electrons, the beam stability is good, the fluctuation is small, the uniformity is good, the beam rising time is short, and the characteristics of high toughness, high strength and high melting point of metal are achieved.
3. According to the long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof, the metal coating is prepared by a chemical vapor deposition method, has good binding performance with the graphite micro-column, and is not easy to fall off in the using process.
4. The long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof have the advantages that the deposition characteristic of a chemical vapor deposition method is benefited, 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 larger length-diameter ratio (ratio of height to diameter), and the uniformity of emission beam 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, the plasma expansion speed of the refractory metal is low, and the mass loss is small.
6. According to the long-life micro-column array graphite and metal composite cathode structure and the preparation method thereof, the thickness of the metal coating is generally in the range of 0.01-50 mu m, preferably the thickness of the coating can be controlled in the range of 1-10 mu m, and the service life can be prolonged.
Drawings
FIG. 1 is a cross-sectional view of a knife-edge-shaped annular graphite cathode substrate according to the present invention, wherein a is the knife edge;
FIG. 2 is a schematic diagram of a graphite cathode with micropillar arrays according to the present invention, showing only the micropillar arrays at the knife-edge;
FIG. 3 is a flow chart of the preparation method of the composite cathode structure of long-life micro-column array graphite and metal of the invention;
FIG. 4 is a scanning electron microscope image of a micropillar array graphite cathode obtained in example 1 of the present invention;
FIG. 5 shows the long-life microcolumn array graphite and M obtained in example 1 of the present inventionOScanning electron microscopy of the composite cathode structure of (a);
FIG. 6 shows the long-life microcolumn array graphite and M obtained in example 1 of the present inventionOEDS map of surface analysis of the composite cathode structure.
Detailed Description
The invention is further described below with reference to the figures and examples.
Example 1
1) Processing graphite into a knife-edge-shaped annular graphite cathode substrate, wherein the outer diameter (namely the diameter of an outer ring) of the knife-edge-shaped annular graphite cathode substrate is 50mm, and the wall thickness (namely the radius of the outer ring minus the radius of an inner ring) is 1 mm; ultrasonically cleaning the mixture in ethanol, and drying the mixture in an oven for later use;
2) constructing a graphite microcolumn array on the surface of the edge of the dried edge-shaped annular graphite cathode substrate in an ultraviolet laser etching mode, wherein the diameter of each graphite microcolumn is 20 microns, and the ratio of the height to the diameter is 6: 1, the distance between the axes of the adjacent graphite microcolumns is 60 mu m to obtain a microcolumn array graphite cathode, the graphite cathode is subjected to low-power ultrasonic cleaning in ethanol to remove debris around the graphite microcolumns, and the graphite cathode is placed in an oven to be dried for later use;
3) placing the dried micro-column array graphite cathode in a chemical vapor deposition furnace, and raising the temperature of a hearth to 600 ℃ at a temperature rise rate of 10 ℃/min;
4) introducing hydrogen as reducing gas into a hearth of the chemical vapor deposition furnace at a flow rate of 100mL/min, and keeping the hearth pressure at 5 kPa;
5) adding MoCl5Heating to 300 ℃ for complete gasification, and introducing into a hearth at a flow rate of 30mL/min for reduction reaction for 3 h;
6) 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 micropillar array graphite cathode, fig. 5 is a scanning electron microscope image of a long-life micropillar array graphite and Mo composite cathode structure, fig. 6 is a surface analysis EDS (electron-beam spectroscopy) image of the long-life micropillar 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 end and the side wall of each graphite microcolumn.
Example 2
1) Processing graphite into a knife-edge-shaped annular graphite cathode substrate, wherein the outer diameter (namely the diameter of an outer ring) of the knife-edge-shaped annular graphite cathode substrate is 100mm, and the wall thickness (namely the radius of the outer ring minus the radius of an inner ring) is 1.5 mm; ultrasonically cleaning the mixture in ethanol, and drying the mixture in an oven for later use;
2) constructing a graphite microcolumn array on the surface of the edge of the dried edge-shaped annular graphite cathode substrate in an ultraviolet laser etching mode, wherein the diameter of each graphite microcolumn is 40 mu m, and the ratio of the height to the diameter is 5: 1, the distance between the axes of the adjacent graphite microcolumns is 100 mu m to obtain a microcolumn array graphite cathode, the graphite cathode is subjected to low-power ultrasonic cleaning in ethanol to remove debris around the graphite microcolumns, and the graphite cathode is placed in an oven to be dried for later use;
3) placing the dried micro-column array graphite cathode in a chemical vapor deposition furnace, and raising the temperature of a hearth to 700 ℃ at a temperature rise rate of 10 ℃/min;
4) introducing hydrogen as reducing gas into a hearth of the chemical vapor deposition furnace at a flow rate of 150mL/min, and keeping the hearth pressure at 1 kPa;
5) mixing WCl6Heating to 350 ℃ for complete gasification, and introducing into a hearth at a flow rate of 50mL/min for reduction reaction for 2 h;
6) stopping introducing hydrogen, and naturally cooling to obtain 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 substrate, wherein the outer diameter (namely the diameter of an outer ring) of the knife-edge-shaped annular graphite cathode substrate is 50mm, and the wall thickness (namely the radius of the outer ring minus the radius of an inner ring) is 1 mm; ultrasonically cleaning the mixture in ethanol, and drying the mixture in an oven for later use;
2) constructing a graphite microcolumn array on the surface of the edge of the dried edge-shaped annular graphite cathode substrate in an ultraviolet laser etching mode, wherein the diameter of each graphite microcolumn is 5 microns, and the ratio of the height to the diameter is 20: 1, the distance between the axes of the adjacent graphite microcolumns is 20 mu m to obtain a microcolumn array graphite cathode, the graphite cathode is subjected to low-power ultrasonic cleaning in ethanol to remove debris around the graphite microcolumns, and the graphite cathode is placed in an oven to be dried for later use;
3) placing the dried micro-column array graphite cathode in a chemical vapor deposition furnace, and raising the temperature of a hearth to 800 ℃ at a temperature rise rate of 5 ℃/min;
4) introducing hydrogen as reducing gas into a hearth of the chemical vapor deposition furnace at a flow rate of 100mL/min, and keeping the hearth pressure at 0.1 kPa;
5) mixing TiCl4Heating to complete gasification, introducing into a hearth at a flow rate of 30mL/min, and carrying out reduction reaction for 0.5 h;
6) 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 substrate, wherein the outer diameter (namely the diameter of an outer ring) of the knife-edge-shaped annular graphite cathode substrate is 50mm, and the wall thickness (namely the radius of the outer ring minus the radius of an inner ring) is 1 mm; ultrasonically cleaning the mixture in ethanol, and drying the mixture in an oven for later use;
2) constructing a graphite microcolumn array on the surface of the edge of the dried edge-shaped annular graphite cathode substrate in an ultraviolet laser etching mode, wherein the diameter of each graphite microcolumn is 300 mu m, and the ratio of the height to the diameter is 1: 1, the distance between the axes of the adjacent graphite microcolumns is 500 mu m, so as to obtain a microcolumn array graphite cathode, ultrasonically cleaning the graphite cathode in ethanol at low power, removing debris around the graphite microcolumns, and placing the graphite cathode in an oven for drying for later use;
3) placing the dried micro-column array graphite cathode in a chemical vapor deposition furnace, and raising the temperature of a hearth to 1200 ℃ at a temperature rise rate of 8 ℃/min;
4) introducing hydrogen as reducing gas into a hearth of the chemical vapor deposition furnace at a flow rate of 100mL/min, and keeping the hearth pressure at 20 kPa;
5) reacting ZrCl4Heating to complete gasification, and introducing into a hearth at a flow rate of 30mL/min for reduction reaction for 10 h;
6) 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 above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same, and it is obvious for a person skilled in the art to modify the specific technical solutions described in the foregoing embodiments or to substitute part of the technical features, and these modifications or substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions protected by the present invention.
Claims (10)
1. A 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 substrate and a plurality of graphite micro-columns arranged on the surface of the knife edge of the knife-edge-shaped annular graphite cathode substrate in an array manner; the method is characterized in that:
and metal coatings are uniformly adhered to the surface of the knife-edge-shaped annular graphite cathode substrate and the top end and the side wall of each graphite microcolumn, and the metal coatings are made of refractory metals.
2. The long life micropillar array graphite and metal composite cathode structure of claim 1, wherein:
the thickness of the metal coating is within the range of 0.01-50 mu m.
3. The long life micropillar array graphite and metal composite cathode structure of claim 2, wherein:
the thickness of the metal coating is within the range of 1-10 mu m.
4. The long life micro-cylinder array graphite and metal composite cathode structure of claims 1 to 3, characterized in that:
the metal coating is made of one or more of Mo, W, Hf, Ta, Zr, Ti, Cr and V.
5. The long life micropillar array graphite and metal composite cathode structure of claim 4, wherein:
the diameter of the graphite microcolumn 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 the adjacent graphite microcolumns is 20-500 mu m.
6. The long life micropillar array graphite and metal composite cathode structure of claim 5, wherein:
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.
7. A preparation method of a long-life micro-column array graphite and metal composite cathode structure is characterized by comprising the following steps:
1) processing graphite into a knife-edge-shaped annular graphite cathode matrix, cleaning and drying the graphite cathode matrix;
2) constructing a graphite micro-column array on the surface of the knife-edge of the dried knife-edge-shaped annular graphite cathode substrate in 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 raising the temperature of a hearth to 300-1200 ℃ at a constant temperature raising rate;
4) introducing hydrogen into a hearth of the chemical vapor deposition furnace to serve as reducing gas, and keeping the pressure of the hearth at 0.1-20 kPa;
5) heating a metal compound of refractory metal until the metal compound is completely gasified, introducing the metal compound into a hearth at a constant flow rate, and carrying out reduction reaction for 0.5-10 h;
6) stopping introducing hydrogen, and naturally cooling to obtain the long-life micro-column array graphite and metal composite cathode structure.
8. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 5, is characterized in that:
in the step 3), the heating rate is 5-10 ℃/min;
and raising the temperature of the hearth to 500-800 ℃.
9. The method for preparing the long-life micro-column array graphite and metal composite cathode structure according to claim 7, is characterized in that:
in the 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 and V.
10. The method for preparing a composite cathode structure of graphite and metal with long service life micro-column array according to claim 9, wherein the method comprises the following steps:
in the step 5), the time of the reduction reaction is 2-5 h.
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