CN102468092B - Method for preparing heat element for heated cathode - Google Patents
Method for preparing heat element for heated cathode Download PDFInfo
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- CN102468092B CN102468092B CN201010534602.7A CN201010534602A CN102468092B CN 102468092 B CN102468092 B CN 102468092B CN 201010534602 A CN201010534602 A CN 201010534602A CN 102468092 B CN102468092 B CN 102468092B
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- heater
- molybdenum
- tungsten
- scolder
- straddle
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- 238000000034 method Methods 0.000 title claims abstract description 22
- 229910000679 solder Inorganic materials 0.000 claims abstract description 20
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 20
- 239000010937 tungsten Substances 0.000 claims abstract description 20
- 238000005516 engineering process Methods 0.000 claims abstract description 11
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical group [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 27
- 229910052750 molybdenum Inorganic materials 0.000 claims description 21
- 238000002360 preparation method Methods 0.000 claims description 21
- 239000011733 molybdenum Substances 0.000 claims description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 13
- 229910001080 W alloy Inorganic materials 0.000 claims description 13
- 239000001257 hydrogen Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 238000006396 nitration reaction Methods 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000007769 metal material Substances 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- 238000004804 winding Methods 0.000 claims description 4
- 239000000020 Nitrocellulose Substances 0.000 claims description 3
- FJWGYAHXMCUOOM-QHOUIDNNSA-N [(2s,3r,4s,5r,6r)-2-[(2r,3r,4s,5r,6s)-4,5-dinitrooxy-2-(nitrooxymethyl)-6-[(2r,3r,4s,5r,6s)-4,5,6-trinitrooxy-2-(nitrooxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-3,5-dinitrooxy-6-(nitrooxymethyl)oxan-4-yl] nitrate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O)O[C@H]1[C@@H]([C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@@H](CO[N+]([O-])=O)O1)O[N+]([O-])=O)CO[N+](=O)[O-])[C@@H]1[C@@H](CO[N+]([O-])=O)O[C@@H](O[N+]([O-])=O)[C@H](O[N+]([O-])=O)[C@H]1O[N+]([O-])=O FJWGYAHXMCUOOM-QHOUIDNNSA-N 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- OUFGXIPMNQFUES-UHFFFAOYSA-N molybdenum ruthenium Chemical compound [Mo].[Ru] OUFGXIPMNQFUES-UHFFFAOYSA-N 0.000 claims description 3
- 229920001220 nitrocellulos Polymers 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims 2
- 238000002485 combustion reaction Methods 0.000 claims 1
- 230000035939 shock Effects 0.000 abstract description 7
- 238000003466 welding Methods 0.000 abstract description 3
- 238000011982 device technology Methods 0.000 abstract 1
- 238000011161 development Methods 0.000 description 6
- 238000007796 conventional method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- JPNWDVUTVSTKMV-UHFFFAOYSA-N cobalt tungsten Chemical compound [Co].[W] JPNWDVUTVSTKMV-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- -1 W-Re Chemical compound 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 238000005094 computer simulation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
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- Microwave Tubes (AREA)
Abstract
The invention discloses a method for preparing a heat element for a heated cathode and relates to a microwave device technology. The method is used for preparing the heat element for the heated cathode. According to the method, a tungsten spiral heat element is welded with a heat element inserting leg by a high-temperature solder welding technology, so that the connecting strength of the tungsten spiral heat element and the heat element inserting leg is enhanced. The method is simple and practicable. The prepared heat element has the advantages of small contact resistance, no damage, high shock resistance, high thermal shock resistance, high finished product ratio, high reliability and the like.
Description
Technical field
The present invention relates to microwave device technical field, is the preparation method of heater for a kind of hot cathode, for the heater preparation of hot cathode.
Background technology
In electron tube, the part of heated cathode, is called heater.
Microwave vacuum electronic technology be one with a long history, dynamic, and the huge research field of development potentiality.Meanwhile, microwave vacuum electronic technology is a kind of comprehensive extremely strong research field that comprises the subjects such as microwave electronics, cathode electronics, Theory of Electromagnetic Field, material technology, vacuum technique, numerical computation technology and computer simulation emulation technology.Developing history shows, a national comprehensive strength is depended in the development of microwave vacuum electronic device and correlation technique, and determines the development level of the microwave vacuum electronic device of Zhe Gai state.Therefore, only have at present the strong big country of comprehensive scientific and technological strength such as the U.S., Russia, Britain, France, Japan, Germany, China just to there is the ability of high performance microwave vacuum electron device research and production application.
Microwave vacuum electronic device is widely used in the aspects such as high power microwave weapon in radar, satellite communication, electron accelerator, global location, controllable thermonuclear fusion and following military forward position, the function that it is unique and superior performance,, the in the situation that of high-power and high band, be particularly that other devices can not replace.Go through the development of many decades, although the theory of conventional microwave vacuum electronic device and correlation technique be mature on the whole, yet Modern High-Tech's microwave device constantly proposes new growth requirement to operating characteristic such as the power of microwave signal, frequency, bandwidth.These demands are mainly manifested in the higher frequency of requirement, larger power, wider frequency band, higher efficiency and new operating characteristic, thereby the development of microwave vacuum electronic device and correlation technique has been proposed to new challenge and opportunity to develop.And take on the hot cathode of electron emission and heater, be the part of core the most in microwave vacuum electronic device, heater performance quality will directly affect output performance and the life-span of microwave source, and then affects performance and the life-span of satellite and High-Power Microwave device.Therefore study the highly reliable heater of hot cathode, for the development tool that promotes the technology such as satellite communication and High-Power Microwave device, be of great significance.
Heater material is generally selected tungsten or tungsten alloy, as tungsten, W-Re, tungsten aluminium etc.The heater preparation method of general heater structure is:
1. wrapping wire: heater silk used is tungsten or tungsten alloy filament.The core silk of wrapping wire is molybdenum filament, utilizes spiral filament forming machine by tungsten or tungsten alloy filament continuously or be interrupted on the silk that is molybdenum around core silk.
2. clean: the taenidium winding is boiled with the 20%NaOH aqueous solution, with supersonic wave cleaning machine, clean, until tungsten filament surface aquadag is cleaned, then with running water, rinse well, then with distillation poach twice, through absolute ethyl alcohol dehydration post-drying.
3. annealing: the taenidium after washing and drying is put into hydrogen stove, rising heating voltage to 1000 ℃
b, maintain 10 minutes, after power-off cool to room temperature, take out.
4. be shaped: the taenidium of having annealed is sheared to Len req, and on heater particular manufacturing craft, coiling is shaped.
5. setting: heater is put on setting bar after being shaped, curved good leg soaks more than 2 hours with acetone in culture dish, and acetone soln is poured out, and after electricity consumption dries up, setting bar is placed in molybdenum boat together with heater, puts into hydrogen stove heating voltage and is raised to 1400 ℃
b, take out after power-off cool to room temperature after maintaining 10 minutes.
6. molten core: the heater having formalized is taken off from setting bar, and (nitration mixture is joined 50%HNO with nitration mixture
3+ 30%H
2sO
4+ 20%H
2o) dissolve molybdenum core silk.
7. straddle: shear the molybdenum filament of required length, straddle.Molybdenum filament will be inserted into the root of leg screw, and leg screw part will be stepped up with pliers, avoids molybdenum filament to come off.
8. clean: ready-made heater is boiled with the 20%NaOH aqueous solution, then with running water, rinse well, then with distilling poach 2 times, through absolute ethyl alcohol dehydration post-drying.
9. degas: heater is put into hydrogen stove, and heating voltage is raised to 900 ℃
b, maintain 10 minutes, after power-off cool to room temperature, take out.
10. check: by the cold resistance of resistance meter calorimetric, see and whether meet the requirements, if do not meet discarded.
But the preparation method of this traditional heater has a shortcoming: in the 7th step, molybdenum filament will be inserted into the root of leg screw, and leg screw part will be stepped up with pliers, avoids molybdenum filament to come off.In the process that leg screw part is stepped up with pliers, can cause the tungsten of leg screw part or tungsten alloy filament to pulverize (waste product accounts for 50-70%) or occur damage that (qualified product account for 30-50%.The heater leg screw that has as seen from Figure 3 crackle), thus cause between heater leg screw and straddle, have that contact resistance is large, vibration resistance poor performance, the shortcoming such as thermal shock resistance is poor and reliability is low.This heater, after electrophoresis and after use a period of time, there will be insulation to cause waste product (accounting for 20% left and right) between molybdenum straddle and leg screw in addition.
Summary of the invention
The object of the invention is in order to overcome traditional heater preparation method's shortcoming, the preparation method of a kind of hot cathode with heater is provided, can avoid tungsten or the tungsten alloy filament of leg screw part to occur damage, thereby prepare, have that between leg screw and straddle, contact resistance is little, vibration resistance performance is good, thermal shock resistance is good and the hot cathode heater of high reliability.
For achieving the above object, technical solution of the present invention is:
A preparation method for heater for hot cathode, it welds together tungsten spiral heater and heater straddle by high-temperature solder solder technology, comprises step:
(1) utilize on the silk that spiral filament forming machine is molybdenum by tungsten or tungsten alloy filament around core silk;
(2) taenidium winding is boiled with the 20%NaOH aqueous solution, with supersonic wave cleaning machine, clean;
(3) clean taenidium is put into hydrogen stove, rising heating voltage is to≤1000 ℃
b, maintain≤10 minutes, after power-off cool to room temperature, take out;
(4) taenidium of having annealed is sheared to Len req, on heater particular manufacturing craft, coiling is shaped;
(5) heater after being shaped is put on to setting bar, curved good leg, puts into hydrogen stove, heating voltage is raised to≤1400 ℃
b, maintain≤after 10 minutes, after power-off cool to room temperature, take out;
(6) heater having formalized is dissolved to molybdenum core silk with nitration mixture;
(7) molybdenum straddle is inserted to leg screw, and it is clean to put it in acetone soln ultrasonic cleaning;
(8) at the leg screw that inserts molybdenum core silk, be partly coated with and spread the solder paste mixing up with organic solvent;
(9) heater of coating solder paste is put into hydrogen stove, heating voltage is raised to scolder fusing point, maintains≤1 minute, after power-off cool to room temperature, takes out; Temperature retention time can not be oversize or too short, and the time, oversize heater was easily crisp, and too short scolder of time does not melt completely;
(10) check: whether, by the cold resistance of resistance meter calorimetric, see and meet the requirements, satisfactory is finished product, if do not meet discarded.
Described preparation method, the nitration mixture described in it in (6) step, its formula is: 50%HNO
3+ 30%H
2sO
4+ 20%H
2o.
Described preparation method, the organic solvent described in it in (8) step, is the organic solutions such as guncotton or glycerine.
Described preparation method, scolder, scolder fusing point described in it in (8), (9) step, scolder is high-temperature solder, scolder fusing point is at 1600 ℃
b-2000 ℃
bbetween, and the metal or alloy material that all infiltrates of scolder and molybdenum straddle and tungsten or tungsten alloy leg screw.
Described preparation method, metal or alloy material described in it, is platinum, molybdenum-ruthenium or tungsten-cobalt etc.
The inventive method, simple, the heater of preparation has and between taenidium and straddle, has that contact resistance is little, vibration resistance performance is good, thermal shock resistance is good and high reliability.
Accompanying drawing explanation
Fig. 1 is the taenidium prepared of traditional heater preparation method and the stereoscan photograph of straddle;
Fig. 2 is the taenidium that adopts method of the present invention and prepare and the stereoscan photograph of straddle;
The heating voltage that Fig. 3 is the heater that adopts method of the present invention and prepare is schematic diagram over time.
Embodiment
Shortcoming for fear of traditional heater preparation method, the preparation method of highly reliable heater for hot cathode of the present invention, be to utilize high-temperature solder solder technology that taenidium and straddle are welded together, thereby make between the taenidium of heater and straddle that tool gets an electric shock, resistance is little, vibration resistance performance is good, thermal shock resistance is good and high reliability.This high-temperature solder must possess following feature simultaneously: the first, and it must all infiltrate with molybdenum straddle and tungsten or tungsten alloy leg screw, like this guarantee firm welding.The second, its fusing point must be higher than (general 1100 ℃ of heater working temperatures
b-1400 ℃
babout), otherwise heater causes the evaporation of scolder in the course of the work.The 3rd, its molten some temperature must be higher than sintering temperature (general 1600 ℃ of the sintering temperature of the sintering insulated material of heater
b-1800 ℃
b) otherwise in sintering process, cause the evaporation of scolder, and then cause the adhesion between molybdenum straddle and tungsten or tungsten alloy leg screw to decline, and the performance that affects microwave device.The 4th, the fusing point of high-temperature solder can not be too high, and the too high meeting of welding temperature causes heater material to become fragile, and causes heater vibration resistance poor performance.In sum, high-temperature solder should select fusing point at 1600 ℃
b-2000 ℃
bbetween the metal or alloy material (as platinum, molybdenum-ruthenium, tungsten-cobalt etc.) all infiltrating with molybdenum straddle and tungsten or tungsten alloy leg screw.
Embodiment:
A preparation method for heater for hot cathode, comprises the following steps:
1. utilize on the silk that spiral filament forming machine is molybdenum by tungsten or tungsten alloy filament around core silk.
2. the taenidium winding is boiled with the 20%NaOH aqueous solution, with supersonic wave cleaning machine, clean.
3. clean taenidium is put into hydrogen stove, rising heating voltage to 1000 ℃
b, maintain 10 minutes, after power-off cool to room temperature, take out.
4. the taenidium of having annealed is sheared to Len req, on heater particular manufacturing craft, coiling is shaped.
5. the heater after being shaped is put on to setting bar, curved good leg, puts into hydrogen stove heating voltage and is raised to 1400 ℃
b, take out after power-off cool to room temperature after maintaining 10 minutes.
6. by (the nitration mixture formula: 50%HNO of nitration mixture for heater having formalized
3+ 30%H
2sO
4+ 20%H
2o) dissolve molybdenum core silk.
7. molybdenum straddle is inserted to leg screw, and it is clean to put it in acetone soln ultrasonic cleaning.
8. at the leg screw that inserts molybdenum core silk, be partly coated with and spread the solder paste (60%Mo+40%Ru) mixing up with organic solvent (as guncotton, glycerine etc.).
9. the heater of coating solder paste is put into hydrogen stove, heating voltage is raised to (1920 ℃ of scolder fusing points
b), maintain 1 minute, after power-off cool to room temperature, take out.
10. check: whether, by the cold resistance of resistance meter calorimetric, see and meet the requirements, satisfactory is finished product, if do not meet discarded.
Taenidium prepared by employing the present invention and the stereoscan photograph of straddle are shown in Fig. 2.From scheming, can find out that scolder welds together taenidium and straddle securely, on taenidium without any crackle, qualification rate 100%.Table 1 and table 2 have provided the resistance that adopts heater prepared by conventional method and the present invention.By two tables, can find out that the heater resistance that adopts heater resistance ratio conventional method prepared by the present invention to prepare is little by 10%, the heater that this explanation adopts the inventive method to prepare, has that contact resistance is little, not damaged, vibration resistance performance is good, thermal shock resistance is good, rate of finished products is high and high reliability.Fig. 3 is for the heater that adopts method of the present invention and prepare is at 1100 ℃
btime heater voltage curve over time, at high temperature the life-span surpasses and within 3000 hours, does not occur breaking phenomena to adopt as can be seen from Figure 3 heater prepared by method of the present invention.At present more than 150, only on various microwave tubes, used the heater that adopts method of the present invention to prepare, do not occurred that one is opened circuit.
Heater prepared by the inventive method is compared with the heater of preparing by conventional method, and its resistance value is as shown in table 1, table 2.The resistance that table 1 is the heater that adopts conventional method and prepare, the resistance that table 2 is the heater that adopts the inventive method and prepare.
The resistance of heater prepared by table 1 employing conventional method
The resistance of heater prepared by table 2 employing the inventive method
Claims (4)
1. the preparation method of heater for a hot cathode, it is characterized in that, the method is to adopt high-temperature solder solder technology that tungsten spiral heater and heater straddle are welded together, first at the leg screw of the after-combustion heater with straddle, be partly coated with and spread the high-temperature solder slurry being in harmonious proportion with organic bond, then the heater of coating high-temperature solder slurry is put into hydrogen high temperature furnace or high-temperature vacuum furnace, heating voltage is raised to scolder fusing point, maintain about 1 minute, after power-off cool to room temperature, take out, specifically comprise the following steps:
1) utilize on the silk that spiral filament forming machine is molybdenum by tungsten or tungsten alloy filament around core silk;
2) taenidium winding is boiled with the 20%NaOH aqueous solution, with supersonic wave cleaning machine, clean;
3) clean taenidium is put into hydrogen stove, rising heating voltage is to≤1000 ℃
b, maintain≤10 minutes, after power-off cool to room temperature, take out;
4) taenidium of having annealed is sheared to Len req, on heater particular manufacturing craft, coiling is shaped;
5) heater after being shaped is put on to setting bar, curved good leg, puts into hydrogen stove, heating voltage is raised to≤1400 ℃
b, maintain≤after 10 minutes, after power-off cool to room temperature, take out;
6) heater having formalized is dissolved to molybdenum core silk with nitration mixture;
7) molybdenum straddle is inserted to leg screw, and it is clean to put it in acetone soln ultrasonic cleaning;
8) at the leg screw that inserts molybdenum core silk, be partly coated with and spread the solder paste mixing up with organic solvent;
9) heater of coating solder paste is put into hydrogen stove, heating voltage is raised to scolder fusing point, maintains≤1 minute, after power-off cool to room temperature, takes out;
10) check: whether, by the cold resistance of resistance meter calorimetric, see and meet the requirements, satisfactory is finished product, if do not meet discarded.
2. preparation method as claimed in claim 1, is characterized in that, described 8) organic solvent in step, is guncotton or glycerine.
3. preparation method as claimed in claim 1, is characterized in that, described 8), 9) scolder, scolder fusing point in step, scolder is high-temperature solder, scolder fusing point is at 1600 ℃
b-2000 ℃
bbetween, and the metal or alloy material that all infiltrates of scolder and molybdenum straddle and tungsten or tungsten alloy leg screw.
4. preparation method as claimed in claim 4, is characterized in that, described metal or alloy material is platinum or molybdenum-ruthenium.
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CN103887129B (en) * | 2014-04-04 | 2016-04-27 | 安徽华东光电技术研究所 | Negative electrode filament and negative electrode lamp |
CN104480485B (en) * | 2014-11-18 | 2017-02-01 | 安徽华东光电技术研究所 | Tungsten-rhenium wire cleaning method for multi-beam cathode filament assembly |
CN104505322B (en) * | 2014-11-24 | 2017-03-15 | 安徽华东光电技术研究所 | Drawing device and drawing method of filament for cathode |
CN107393788B (en) * | 2017-07-17 | 2019-05-07 | 安徽华东光电技术研究所 | Heater structure and preparation method thereof |
CN111633293A (en) * | 2020-06-15 | 2020-09-08 | 安徽华东光电技术研究所有限公司 | Thorium-tungsten hot wire pin brazing method |
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KR880008372A (en) * | 1986-12-02 | 1988-08-31 | 미다 가쓰시게 | CRT Tube Cathode Heater |
CN1956124B (en) * | 2005-10-27 | 2010-07-21 | 中国科学院电子学研究所 | High efficient cathode assembly |
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