CN102637567A - Cathode salt, preparation method of cathode salt, barium tungsten cathode comprising cathode salt and preparation method of barium tungsten cathode - Google Patents
Cathode salt, preparation method of cathode salt, barium tungsten cathode comprising cathode salt and preparation method of barium tungsten cathode Download PDFInfo
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- CN102637567A CN102637567A CN2012100908489A CN201210090848A CN102637567A CN 102637567 A CN102637567 A CN 102637567A CN 2012100908489 A CN2012100908489 A CN 2012100908489A CN 201210090848 A CN201210090848 A CN 201210090848A CN 102637567 A CN102637567 A CN 102637567A
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- negative electrode
- salt
- preparation
- cathode
- barium
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- 150000003839 salts Chemical class 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 38
- WMTSAHAFZXEJBV-UHFFFAOYSA-N [Ba].[W] Chemical compound [Ba].[W] WMTSAHAFZXEJBV-UHFFFAOYSA-N 0.000 title claims abstract description 25
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 48
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000005303 weighing Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 34
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 23
- 239000004411 aluminium Substances 0.000 claims description 23
- 229910052782 aluminium Inorganic materials 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000000992 sputter etching Methods 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 230000002045 lasting effect Effects 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 238000005530 etching Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 2
- 239000011149 active material Substances 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- Powder Metallurgy (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses cathode salt, a preparation method of the cathode salt, a barium tungsten cathode comprising the cathode salt and a preparation method of the barium tungsten cathode. The cathode salt includes components, by weight, 3-4 parts of barium carbonate, 0.3-0.8 part of calcium carbonate and 1.5-2.5 parts of aluminum powder. The preparation method of the cathode salt includes weighing, ball milling, drying and synthesizing. The barium tungsten cathode prepared by the cathode salt has high emitting power which can be up to hundreds of amperes and meets the requirements of high-power and high-frequency development of microwave devices.
Description
Technical field
The present invention relates to the microwave device technical field, be specifically related to a kind of negative electrode salt and preparation method thereof, contain barium-tungsten dispense cathode of this negative electrode salt and preparation method thereof.
Background technology
" heart " as the modern national defense equipment; Microwave device is towards development high-power, high-frequency direction; Like this, to electron source as microwave device---negative electrode has just proposed test, especially get into millimere-wave band, terahertz wave band after; The current density requirements that microwave device is annotated electronics is very big, needs the stable current density that every square centimeter of dozens or even hundreds of ampere is provided of negative electrode ability.The active material of barium-tungsten dispense cathode emitting electrons---negative electrode salt has determined the emissivities of negative electrode to a great extent.The negative electrode salt that traditional barium-tungsten dispense cathode uses can only provide 10A/cm under stable operating state
2About electric current, emission current is less, is difficult to satisfy microwave device to needs high-power, that the high-frequency direction develops.
Summary of the invention
In order to overcome the deficiency of above-mentioned prior art; The present invention provides a kind of negative electrode salt and preparation method thereof, contains barium-tungsten dispense cathode of this negative electrode salt and preparation method thereof; Use the negative electrode of this negative electrode salt manufacturing to possess the high emission ability; Can reach up to a hundred amperes emissivities, be applied in the platinotron, satisfy the demand that microwave device is high-power, high-frequency develops.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of negative electrode salt, its raw material components amount of substance ratio is: brium carbonate 3～4, calcium carbonate 0.3～0.8, aluminium powder 1.5～2.5, preferably the amount of its component materials ratio is: brium carbonate 3.5, calcium carbonate 0.5, aluminium powder 2.
A kind of negative electrode salt preparation method may further comprise the steps:
1), take by weighing dry brium carbonate, calcium carbonate, aluminium powder by formula ratio and carry out ball milling, make it to mix;
2), the powder behind the ball milling is dried in baking oven;
3), negative electrode salt is synthetic, process conditions be in dry hydrogen atmosphere 1200 ℃～1300 ℃, are incubated 7～12min.
A kind of barium-tungsten dispense cathode, said barium-tungsten dispense cathode contain the as above negative electrode salt of preparation method's preparation.
A kind of preparation method of barium-tungsten dispense cathode may further comprise the steps:
A, negative electrode salt and the negative electrode of negative electrode salt to be impregnated of preparation placed steeper, in dry hydrogen atmosphere, be rapidly heated to 1700 ℃～1800 ℃ insulation 30s～90s;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing, the facing amount is greater than 0.2mm;
D, the target surface of emission carry out ion etching and cleaning, etching depth 7 μ m～9 μ m.
The preparation method of said barium-tungsten dispense cathode also can accomplish the synthetic dipping with negative electrode of negative electrode salt synchronously; Negative electrode salt that will soon synthesize after the ball milling drying and negative electrode to be impregnated place steeper; Be warming up to 1200 ℃～1300 ℃, insulation 7～12min, and then be rapidly heated to 1700 ℃～1800 ℃; Insulation 30s～90s reduces to normal temperature subsequently.
The present invention is through a large amount of tests; Through using aluminium powder to replace aluminium oxide; Carry out rational proportion with brium carbonate, calcium carbonate, react synthetic special aluminate down, use the barium-tungsten dispense cathode emissivities of this negative electrode salt preparation high through high temperature; Overcome the less deficiency of the emission current of traditional barium-tungsten dispense cathode under stable operating state, satisfied the demand that microwave device is high-power, high-frequency develops.
Embodiment
Embodiment 1
A kind of negative electrode salt, its raw material components amount of substance ratio is: brium carbonate 3, calcium carbonate 0.3, aluminium powder 1.5.
A kind of negative electrode salt preparation method may further comprise the steps:
1), brium carbonate, calcium carbonate, aluminium powder (purity all >=99%) dried, brium carbonate, calcium carbonate, aluminium powder are toasted 8h under 120 ℃ of temperature in baking oven;
2), take by weighing dried brium carbonate 592g, calcium carbonate 30g, aluminium powder 40.5g by formula ratio and pour in the agate jar, and in the agate jar, add agate ball and pure water, according to powder: ball: the weight ratio of water=1: 0.8: 1, carry out ball milling, fully mix;
3), the powder behind the ball milling is toasted lasting 15h under 120 ℃ of temperature in baking oven;
4), negative electrode salt is synthetic, process conditions be in dry hydrogen atmosphere 1200 ℃, are incubated 12min.
A kind of preparation method of barium-tungsten dispense cathode may further comprise the steps:
A, negative electrode salt and the negative electrode of negative electrode salt to be impregnated of preparation placed steeper, in dry hydrogen atmosphere, be warming up to 1700 ℃ in the 2min, insulation 90s;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing, facing amount 0.3mm;
D, the target surface of emission carry out ion etching and cleaning, etching depth 7 μ m.
Embodiment 2
A kind of negative electrode salt of using, its raw material components amount of substance ratio is: brium carbonate 3.5, calcium carbonate 0.5, aluminium powder 2.
A kind of negative electrode salt preparation method may further comprise the steps:
1), brium carbonate, calcium carbonate, aluminium powder dried, brium carbonate, calcium carbonate, aluminium powder are toasted 7h under 140 ℃ of temperature in baking oven;
2), take by weighing dried brium carbonate 690.7g, calcium carbonate 50g, aluminium powder 54g by formula ratio and pour in the agate jar, and in the agate jar, add agate ball and pure water, press powder: ball: the weight ratio of water=1: 1: 1.2, carry out ball milling, fully mix;
3), the powder behind the ball milling is toasted lasting 12h under 130 ℃ of temperature in baking oven;
4), negative electrode salt is synthetic, process conditions be in dry hydrogen atmosphere 1250 ℃, are incubated 10min.
A kind of preparation method of barium-tungsten dispense cathode may further comprise the steps:
A, negative electrode salt and the negative electrode of negative electrode salt to be impregnated of preparation placed steeper, in dry hydrogen atmosphere, be rapidly heated to 1750 ℃ insulation 60s;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing, facing amount 3.5mm;
D, the target surface of emission carry out ion etching and cleaning, etching depth 8 μ m.
Embodiment 3
A kind of negative electrode salt, its raw material components amount of substance ratio is: brium carbonate 4, calcium carbonate 0.8, aluminium powder 2.5.
A kind of negative electrode salt preparation method may further comprise the steps:
1), brium carbonate, calcium carbonate, aluminium powder dried, brium carbonate, calcium carbonate, aluminium powder are toasted 8h under 150 ℃ of temperature in baking oven;
2), taking by weighing dried brium carbonate 789.4g, calcium carbonate 80.1g, aluminium powder 67.5g by formula ratio pours in the agate jar; And in the agate jar, add agate ball and pure water; Press powder: ball: the weight ratio of water=1: 1.2: 1.4, carry out ball milling, fully mix;
3), the powder behind the ball milling is toasted lasting 8h under 150 ℃ of temperature in baking oven;
4), negative electrode salt is synthetic, process conditions be in dry hydrogen atmosphere 1300 ℃, are incubated 7min.
A kind of preparation method of barium-tungsten dispense cathode may further comprise the steps:
A, negative electrode salt and the negative electrode of negative electrode salt to be impregnated of preparation placed steeper, in dry hydrogen atmosphere, be rapidly heated to 1800 ℃ insulation 30s;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing, facing amount 0.3mm;
D, the target surface of emission carry out ion etching and cleaning, etching depth 9 μ m.
Embodiment 4
A kind of negative electrode salt, its raw material components amount of substance ratio is: brium carbonate 3.5, calcium carbonate 0.5, aluminium powder 2.
A kind of negative electrode salt preparation method may further comprise the steps:
1), brium carbonate, calcium carbonate, aluminium powder dried, brium carbonate, calcium carbonate, aluminium powder are toasted 7h under 140 ℃ of temperature in baking oven;
2), take by weighing dried brium carbonate 690.7g, calcium carbonate 50g, aluminium powder 54g by formula ratio and pour in the agate jar, and in the agate jar, add agate ball and pure water, press powder: ball: the weight ratio of water=1: 1: 1.2, carry out ball milling, fully mix;
3), the powder behind the ball milling is toasted lasting 12h under 130 ℃ of temperature in baking oven;
4), negative electrode salt is synthetic, process conditions be in dry hydrogen atmosphere 1250 ℃, are incubated 10min.
A kind of preparation method of barium-tungsten dispense cathode may further comprise the steps:
A, the negative electrode salt synthetic after the ball milling drying and the negative electrode of negative electrode salt to be impregnated are placed steeper, insulation 10min 1250 ℃ the time is rapidly heated to 1750 ℃ insulation 60s then in dry hydrogen atmosphere;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing, facing amount 0.3mm;
D, the target surface of emission carry out ion etching and cleaning, etching depth 8 μ m.
Table 1 is the barium-tungsten dispense cathode emission test data of embodiment 1～4 preparation.
Table 1
| Embodiment | Emission (A/cm 2) |
| 1 | 68 |
| 2 | 102 |
| 3 | 71 |
| 4 | 86 |
Claims (8)
1. negative electrode salt, its raw material components amount of substance ratio is: brium carbonate 3～4, calcium carbonate 0.3～0.8, aluminium powder 1.5～2.5.
2. negative electrode salt as claimed in claim 1 is characterized in that: its raw material components amount of substance ratio is: brium carbonate 3.5, calcium carbonate 0.5, aluminium powder 2.
3. the preparation method of a negative electrode salt may further comprise the steps:
1), takes by weighing dry brium carbonate, calcium carbonate, aluminium powder and carry out ball milling after mixing by formula ratio;
2), the powder behind the ball milling is dried;
3), negative electrode salt is synthetic, process conditions be in dry hydrogen atmosphere 1200 ℃～1300 ℃, are incubated 7～12min.
4. preparation method as claimed in claim 4 is characterized in that: ball milling condition is pressed powder for adding agate ball and pure water in the agate jar in the step 1): ball: the weight ratio of water=1: 0.8～1.2: 1～1.4, carry out ball milling, and fully mix; Step 2) drying condition is in baking oven, to toast lasting 8h～15h under 120 ℃～150 ℃ temperature.
5. barium-tungsten dispense cathode, said barium-tungsten dispense cathode contain the negative electrode salt just like claim 3 or 4 described preparation methods' preparations.
6. the preparation method of a barium-tungsten dispense cathode may further comprise the steps:
A, negative electrode salt and the negative electrode of negative electrode salt to be impregnated of preparation placed steeper, in dry hydrogen atmosphere, be rapidly heated to 1700 ℃～1800 ℃ insulation 30s～90s;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing;
D, the target surface of emission carry out ion etching and cleaning.
7. the preparation method of a barium-tungsten dispense cathode may further comprise the steps:
A, negative electrode salt synthetic after the ball milling drying and negative electrode to be impregnated are placed steeper, be warming up to 1200 ℃～1300 ℃, insulation 7～12min, and then be rapidly heated to 1700 ℃～1800 ℃ insulation 30s～90s;
B, reduce to normal temperature and take out;
C, removal remained on surface salt, and Vehicle Processing;
D, the target surface of emission carry out ion etching and cleaning.
8. like claim 6 or 7 described preparation methods, it is characterized in that: said step D intermediate ion etching depth is 7 μ m～9 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210090848.9A CN102637567B (en) | 2012-03-30 | 2012-03-30 | Cathode salt, preparation method of cathode salt, barium tungsten cathode comprising cathode salt and preparation method of barium tungsten cathode |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210090848.9A CN102637567B (en) | 2012-03-30 | 2012-03-30 | Cathode salt, preparation method of cathode salt, barium tungsten cathode comprising cathode salt and preparation method of barium tungsten cathode |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103700561A (en) * | 2013-12-27 | 2014-04-02 | 安徽华东光电技术研究所 | Active composition for barium-tungsten cathode, preparation method thereof and preparation method of barium-tungsten cathode |
| CN103878378A (en) * | 2014-04-04 | 2014-06-25 | 安徽华东光电技术研究所 | Preparation method and application of tungsten powder for cathode |
| CN104485269A (en) * | 2014-11-11 | 2015-04-01 | 安徽华东光电技术研究所 | Multi-beam cathode rhenium powder treatment method |
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| JPH06168661A (en) * | 1992-09-29 | 1994-06-14 | Nec Kansai Ltd | Manufacture of impregnation type cathode |
| CN101145490A (en) * | 2007-08-03 | 2008-03-19 | 安徽华东光电技术研究所 | TWT impregnated Ba-W cathode and its preparation method |
| CN101834106A (en) * | 2010-05-12 | 2010-09-15 | 安徽华东光电技术研究所 | Tungsten-based impregnated cathode and preparation method thereof |
| CN102241412A (en) * | 2011-04-12 | 2011-11-16 | 南京三乐电子信息产业集团有限公司 | Aluminate for assembling barium-tungsten cathode of diode and preparation method thereof |
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2012
- 2012-03-30 CN CN201210090848.9A patent/CN102637567B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS5190561A (en) * | 1975-02-06 | 1976-08-09 | REIINKYOKUHODENKAN | |
| JPH06168661A (en) * | 1992-09-29 | 1994-06-14 | Nec Kansai Ltd | Manufacture of impregnation type cathode |
| CN101145490A (en) * | 2007-08-03 | 2008-03-19 | 安徽华东光电技术研究所 | TWT impregnated Ba-W cathode and its preparation method |
| CN101834106A (en) * | 2010-05-12 | 2010-09-15 | 安徽华东光电技术研究所 | Tungsten-based impregnated cathode and preparation method thereof |
| CN102241412A (en) * | 2011-04-12 | 2011-11-16 | 南京三乐电子信息产业集团有限公司 | Aluminate for assembling barium-tungsten cathode of diode and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103700561A (en) * | 2013-12-27 | 2014-04-02 | 安徽华东光电技术研究所 | Active composition for barium-tungsten cathode, preparation method thereof and preparation method of barium-tungsten cathode |
| CN103700561B (en) * | 2013-12-27 | 2016-05-25 | 安徽华东光电技术研究所 | Active composition for barium-tungsten cathode, preparation method thereof and preparation method of barium-tungsten cathode |
| CN103878378A (en) * | 2014-04-04 | 2014-06-25 | 安徽华东光电技术研究所 | Preparation method and application of tungsten powder for cathode |
| CN103878378B (en) * | 2014-04-04 | 2016-09-07 | 安徽华东光电技术研究所 | Preparation method and application of tungsten powder for cathode |
| CN104485269A (en) * | 2014-11-11 | 2015-04-01 | 安徽华东光电技术研究所 | Multi-beam cathode rhenium powder treatment method |
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| CN102637567B (en) | 2015-01-28 |
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