CN114644517A - High-performance aluminate source for terahertz traveling wave tube and preparation method thereof - Google Patents
High-performance aluminate source for terahertz traveling wave tube and preparation method thereof Download PDFInfo
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- 150000004645 aluminates Chemical class 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims abstract description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- 229910014780 CaAl2 Inorganic materials 0.000 claims abstract description 7
- 229910014779 CaAl4 Inorganic materials 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000498 ball milling Methods 0.000 claims description 20
- 229920000459 Nitrile rubber Polymers 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 239000011733 molybdenum Substances 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000012856 weighed raw material Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims 1
- WMTSAHAFZXEJBV-UHFFFAOYSA-N [Ba].[W] Chemical compound [Ba].[W] WMTSAHAFZXEJBV-UHFFFAOYSA-N 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 2
- 239000011149 active material Substances 0.000 description 3
- 238000007598 dipping method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 238000005034 decoration Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- -1 barium tungsten aluminate Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/44—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminates
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
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Abstract
The invention discloses a high-performance aluminate source for a terahertz traveling wave tube and a preparation method thereof3Al2O6、Ba3CaAl2O7、Ba5CaAl4O12And Ba2CaWO6. The invention adopts the optimal molar ratio of 4:1: 0.4-0.8 of barium carbonate, calcium carbonate and alumina powder to synthesize a multi-phase high-performance electron emission material. The cathode emission current density of the aluminate barium-tungsten prepared by the invention is more than or equal to 50A/cm2(1050 ℃), and the current density of cathode branch is 12A/cm2(1050 ℃), and the service life is more than or equal to 2000 h. Obtain an exceptionGood technical progress.
Description
Technical Field
The invention relates to an aluminate formula for a barium-tungsten cathode with high emission current density and a preparation method thereof, in particular to a preparation technology of high-performance aluminate for a terahertz travelling wave tube; the barium-tungsten cathode prepared from aluminate has high electron emission capability, and belongs to the technical field of preparation of electron emission cathode materials.
Background
The terahertz waveband traveling wave tube is continuously researched at home and abroad, and the application advantages of the vacuum electronic device in the space engineering, the communication engineering, the land-based and ship-based platforms and the like are constructed in the forms of amplifiers or microwave power modules and the like. Due to the traveling wave tube RF peak power Pout＝N×24(J/f2)4/3(Vb)13/6I.e. J ∈ f2Therefore, the high-power terahertz waveband traveling wave tube requires an electron source capable of forming electron beams with high current density, about 30A/cm2～100A/cm2. At present, three high-performance electron sources are commonly used for the terahertz traveling wave tube, and each high-performance electron source has the advantages and the disadvantages: the current density of the field emission cold cathode is large (can reach 200A/cm)2) However, the total current of the cathode is small, high-voltage ignition is easy to fail, the service life is short, and engineering application cannot be realized; large scandate hot cathode emission current density (20A/cm)2～400A/cm2) But the emitting uniformity is poor, the ion bombardment is not resisted, the service life is short, and the method is applied to corresponding high-power terahertz devices; the aluminate barium tungsten hot cathode is widely applied to various traveling wave tubes, has stable performance and long service life, but has relatively small emission current density (20A/cm)2～50A/cm2). By integrating the emission performance and reliability requirements of the electron source for the terahertz traveling wave tube, the aluminate barium tungsten hot cathode is still considered to be most suitable for the cathode of the next generation terahertz traveling wave tube. At present, the emission density level of the domestic aluminate barium-tungsten hot cathode is J more than or equal to 35A/cm2(1050 ℃), the emission density level of the foreign aluminate barium-tungsten hot cathode is J more than or equal to 50A/cm2(1050 ℃), and has a certain gap compared with the foreign advanced level.
In order to meet the engineering application requirements of the terahertz traveling wave tube, the method for improving the emission current density of the aluminate barium tungsten cathode is an effective method. At present, the aluminate formula and the preparation process are difficult to meet the requirement of the terahertz traveling-wave tube on high emission current density.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the problem of insufficient emission current density of the existing aluminate barium-tungsten cathode, and provides an aluminate formula for a high-emission-current-density barium-tungsten hot cathode for a terahertz traveling wave tube and a preparation process thereof, which can greatly improve the emission current density of the cathode, prolong the service life and reliability of the cathode and meet the requirement of the terahertz traveling wave tube on the performance of the cathode.
The technical scheme is as follows: in order to achieve the above purpose, the invention adopts the technical scheme that:
the high-performance aluminate source for the terahertz traveling wave tube is characterized by comprising Ba3Al2O6、Ba3CaAl2O7And Ba5CaAl4O12。
Preferably, the high-performance aluminate source for the terahertz travelling wave tube comprises Ba3Al2O6、Ba3CaAl2O7、Ba5CaAl4O12And Ba2CaWO6。
Preferably, the high-performance aluminate source is formed by solid dissolving CaO in Ba3Al2O6In the physical phase.
The invention provides a preparation method of a high-performance aluminate source for a terahertz traveling wave tube, which comprises the following steps of:
(1) preparation of
Weighing raw materials: weighing raw materials of barium carbonate, calcium carbonate and alumina powder according to a molar ratio;
(2) mixing
Putting the weighed raw materials into a ball milling tank, adding distilled water into the ball milling tank, simultaneously putting agate balls with different diameters, sealing and then putting the ball milling tank on a planetary ball mill for ball milling; putting the ball-milled powder into an oven, and drying;
(3) pressing
Putting the powder mixed in the step (2) into a clean nitrile rubber pipe mold, putting the nitrile rubber pipe filled with the powder into a cold isostatic press for pressing, and then taking out the aluminate rod;
(4) sintering of
And (3) putting the pressed aluminate rods into a molybdenum boat with a certain size, and sintering at high temperature in a hydrogen atmosphere.
As a preferable scheme, the preparation method of the high-performance aluminate source for the terahertz traveling wave tube comprises the following steps:
(1) preparation of
Weighing raw materials: according to a molar ratio of 4:1: weighing raw materials of barium carbonate, calcium carbonate and alumina powder 0.4-0.8;
(2) mixing of
Putting the weighed raw materials into a ball milling tank, adding 500ml of distilled water into the ball milling tank, simultaneously putting 10 agate balls with the diameter of phi 25mm and 20 agate balls with the diameter of phi 10mm, sealing, and putting the ball milling tank on a planetary ball mill for ball milling for 4-8 h, wherein the rotating speed of the ball mill is adjusted to 180 r/min; putting the ball-milled powder into an oven, and drying at 140 ℃/12 h;
(3) pressing
Putting the powder mixed in the step (2) into a clean nitrile rubber pipe mold, putting the nitrile rubber pipe filled with the powder into a cold isostatic press for pressing, applying a pressure of 100-300 MPa, maintaining for 5-8 min, and then taking out the aluminate rod;
(4) sintering
And (3) placing the pressed aluminate rods into a molybdenum boat with a certain size, and sintering at high temperature of 1400 ℃/1h in a hydrogen atmosphere.
(5) Performance testing
Preparing aluminate dipping tungsten matrix with different proportions, processing the aluminate dipping tungsten matrix into a dipping cathode with the outer diameter of 3mm, then coating a metal Os film, carrying out emission performance test, and screening out the optimal formula, wherein the formula is shown in the following table.
The invention designs a high-performance aluminate formula and a preparation process, and adopts the most preferable molar ratio of 4:1: 0.4-0.8 parts of barium carbonate, calcium carbonate and oxygenAluminum powder is synthesized into a plurality of phase high-performance electron emission materials; a certain amount of ternary substances (BaO, CaO, Al)2O3) Synthesis of Ba as main crystal phase at high temperature3Al2O6、Ba3CaAl2O7、Ba5CaAl4O12When the electron emission active material is mixed with a part of CaO being substitutionally dissolved in Ba3Al2O6In the phase of matter, the chemical stability of aluminate is improved, and excessive BaO and CaO are reacted with WO when the cathode tungsten substrate works (1000℃)2Chemically reacted to generate electron-emitting active material Ba2CaWO6This improves both the emission current density and the operational stability of the cathode. The best emission performance was demonstrated by the following screening when the molar ratio of barium carbonate, calcium carbonate and alumina powder was 4:1: 0.6. A good technical progress is obtained.
The invention can solve the defect that the emission current density of the traditional aluminate barium-tungsten cathode is relatively small, and the cathode emission current density of the optimal aluminate formula ratio is more than 50A/cm2(1050 ℃), and can meet the requirement of the terahertz frequency band traveling wave tube on high-current density electron beams. And the invention uses BaO, CaO and WO2Electron-emitting chemical reaction at high temperature to produce electron-emitting active material Ba2CaWO6Can improve electron emission, and the prepared aluminate barium tungsten cathode can work in a large current density state for a long time (taking 12A/cm)2(1050 ℃), and the service life is more than or equal to 2000 h. A good technical progress is obtained.
Drawings
FIG. 1 is a graph showing the current-voltage characteristics of the high emission current density barium tungsten aluminate cathode of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, which is to be given the full breadth of the claims appended hereto.
Example 1
1. A preparation method of a high-performance aluminate source for a terahertz traveling wave tube comprises the following steps:
(1) preparation of
Weighing raw materials: according to a molar ratio of 4:1:0.6 weighing raw materials of barium carbonate, calcium carbonate and alumina powder;
(2) mixing
Putting the weighed raw materials into a ball milling tank, adding 500ml of distilled water into the ball milling tank, simultaneously putting 10 agate balls with the diameter of phi 25mm and 20 agate balls with the diameter of phi 10mm, sealing, and putting the ball milling tank on a planetary ball mill for ball milling for 4-8 h, wherein the rotating speed of the ball mill is adjusted to 180 r/min; putting the ball-milled powder into an oven, and drying at 140 ℃/12 h;
(3) pressing
Putting the powder mixed in the step (2) into a clean nitrile rubber pipe mold, putting the nitrile rubber pipe filled with the powder into a cold isostatic press for pressing, applying a pressure of 100-300 MPa, maintaining for 5-8 min, and then taking out the aluminate rod;
(4) sintering
And (3) placing the pressed aluminate rods into a molybdenum boat with a certain size, and sintering at high temperature of 1400 ℃/1h in a hydrogen atmosphere. The aluminate source prepared comprises Ba3Al2O6、Ba3CaAl2O7、Ba5CaAl4O12And Ba2CaWO6。
2. And (3) performance detection: the cathode emission current density of the barium-tungsten cathode prepared by adopting the aluminate source is more than or equal to 50A/cm2(1050 deg.C), see FIG. 1; cathode branch current density of 12A/cm2(1050 ℃), and the service life is more than or equal to 2000 h. A very good technical progress is achieved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A high-performance aluminate source for a terahertz traveling wave tube is characterized in that,it comprises Ba3Al2O6、Ba3CaAl2O7And Ba5CaAl4O12。
2. The high performance aluminate source for terahertz traveling wave tube as set forth in claim 1, comprising Ba3Al2O6、Ba3CaAl2O7、Ba5CaAl4O12And Ba2CaWO6。
3. The high-performance aluminate source for the terahertz traveling wave tube as set forth in claim 2, wherein CaO is solid-dissolved in Ba3Al2O6In the physical phase.
4. The preparation method of the high-performance aluminate source for the terahertz traveling wave tube as claimed in any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) preparation of
Weighing raw materials: weighing raw materials of barium carbonate, calcium carbonate and alumina powder according to a molar ratio;
(2) mixing
Putting the weighed raw materials into a ball milling tank, adding distilled water into the ball milling tank, simultaneously putting agate balls with different diameters, sealing, and then putting the ball milling tank on a planetary ball mill for ball milling; putting the ball-milled powder into an oven, and drying;
(3) pressing
Filling the powder mixed in the step (2) into a clean nitrile rubber tube mold, putting the nitrile rubber tube filled with the powder into a cold isostatic press for pressing, and then taking out the aluminate rod;
(4) sintering of
And (3) putting the pressed aluminate rod into a molybdenum boat with a certain size, and sintering at high temperature in a hydrogen atmosphere.
5. The preparation method of the high-performance aluminate source for the terahertz traveling-wave tube as claimed in claim 4, is characterized by comprising the following steps:
(1) preparation of
Weighing raw materials: according to a molar ratio of 4:1: weighing raw materials of barium carbonate, calcium carbonate and alumina powder 0.4-0.8;
(2) mixing of
Putting the weighed raw materials into a ball milling tank, adding 500ml of distilled water into the ball milling tank, simultaneously putting 10 agate balls with the diameter of phi 25mm and 20 agate balls with the diameter of phi 10mm, sealing, and putting the ball milling tank on a planetary ball mill for ball milling for 4-8 h, wherein the rotating speed of the ball mill is adjusted to 180 r/min; putting the ball-milled powder into an oven, and drying at 140 ℃/12 h;
(3) pressing
Putting the powder mixed in the step (2) into a clean nitrile rubber pipe mold, putting the nitrile rubber pipe filled with the powder into a cold isostatic press for pressing, applying a pressure of 100-300 MPa, maintaining for 5-8 min, and then taking out the aluminate rod;
(4) sintering of
And (3) placing the pressed aluminate rods into a molybdenum boat with a certain size, and sintering at high temperature of 1400 ℃/1h in a hydrogen atmosphere.
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