CN100431770C - Impregnated barium-tungsten cathode solder and method for using same - Google Patents
Impregnated barium-tungsten cathode solder and method for using same Download PDFInfo
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- CN100431770C CN100431770C CNB2005100942140A CN200510094214A CN100431770C CN 100431770 C CN100431770 C CN 100431770C CN B2005100942140 A CNB2005100942140 A CN B2005100942140A CN 200510094214 A CN200510094214 A CN 200510094214A CN 100431770 C CN100431770 C CN 100431770C
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Abstract
The invention relates to a barium tungsten cathode solder. Wherein, it is formed by palladium, molybdenum and cobalt at 1:5-40:0-90, while their purities are 95-100%. And its application comprises annealing, grinding, compressing, welding and salt emerging. The invention has low steam pressure, long service life, and stable cathode.
Description
Technical field
The present invention relates to negative electrode solder and using method thereof on a kind of electronic tube tube, belong to dipped barium-tungsten cathode and using method thereof especially.
Background technology
As electron source, barium-tungsten dispense cathode is widely used in all kinds of microwave devices.In its production technology, the welding between W base sponge and its molybdenum tube (Mo tube) of support is to finish the whole requisite operation of negative electrode.Adopt electron beam welding, expense is very high, and is very uneconomical.Also once adopted the laser beam weldering, but because the protective gas improper use, thereby cause the be full of cracks of Mo tube, embrittlement, so that come off.No matter be to utilize electron beam welding, or laser beam weldering all necessarily requires to be welded and keeps between the parent closely cooperating, otherwise the Mo tube at first melt contraction, can't weld.And also be difficult to guarantee that the W base is closely sturdy with the Mo tube after welding everywhere, although the two surface soldered is fine.All reasons that goes up cause because of welding the improper negative electrode yield rate that makes lowlyer, and made negative electrode can not adapt to complicated weather and landform simultaneously, and service life is not long.
Summary of the invention
The object of the present invention is to provide a kind of new impregnated barium-tungsten cathode solder.
Another object of the present invention is the using method of above-mentioned solder in dipped barium-tungsten cathode.
For achieving the above object, a kind of impregnated barium-tungsten cathode solder provided by the invention is made up of palladium powder, molybdenum powder, cobalt powder, and its weight ratio is that purity is converted to 100% palladium powder: purity is converted to 100% molybdenum powder: purity is converted to 100% cobalt powder=1: 5-40: 10-90.
Described palladium powder, molybdenum powder, cobalt powder purity are 95-100%.
Preferred solder weight ratio is that purity is converted to 100% palladium powder: purity is converted to 100% molybdenum powder: purity is converted to 100% cobalt powder=1: 10-30: 40-70; Described palladium powder, molybdenum powder, cobalt powder purity are 99-100%.
Effective combination of molybdenum powder, cobalt powder, permeable negative electrode cake and molybdenum tube number micron form the metal phase, thereby make its two strong bonded, and inserting of a small amount of palladium powder will enlarge the wandering face of molybdenum powder, cobalt powder, make welding quality more firm.Thereby palladium powder, molybdenum powder, cobalt powder three's combination, the preferred solder that can be used as negative electrode is used.
The using method of described solder in dipped barium-tungsten cathode:
A) molybdenum powder, palladium powder and cobalt powder are put into 500-1500 ℃ of hydrogen furnace annealing respectively;
B) get palladium powder, molybdenum powder and cobalt powder by weight, these three kinds of materials are ground to are not less than 200 orders, mixing, compacting;
C) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1200-1700 ℃ of insulation 5-120 after second, reduces to 1000-1350 ℃ again, and insulation is not less than 1 minute, cool to room temperature;
D) cathode that step c is made places the aluminate powder, hydrogen atmosphere, and 1300-2000 ℃ flooded 1-10 minute, and the floating salt behind the dipping is removed with cobalt silk flosssilk wadding group;
E) heater is installed
The purity of palladium powder, molybdenum powder, cobalt powder is high more, and prepared dipping barium cobalt negative electrode effect is just good more.
In step b, the order number of palladium powder, molybdenum powder, cobalt powder is high more, and prepared cathode performance to a certain extent can be better, but in view of cost consideration, so preferred order number is the 300-500 order.
In step c, long more 1200-1700 ℃ of temperature retention time, the not corresponding growth of prepared cathode performance is in view of the compromise consideration of negative electrode quality and efficient, so preferred temperature retention time is 5-60 second.
In steps d, temperature retention time is long more, and the not corresponding growth of prepared cathode performance descends, on the contrary in view of the compromise consideration of negative electrode quality and efficient, so preferred temperature retention time is 1-2 minute.
Described cathode diameter is 2-10mm, and thickness is 1-4mm.
The present invention compared with prior art has firm welding, little, the long service life of vapour pressure, and the cathode stabilization of preparing is very good, can adapt to the weather and the landform of various complexity, is particularly useful for the military microwave tube of annotating more.
Description of drawings
Fig. 1 is a dipped barium-tungsten cathode structural representation of the present invention.
In Fig. 1, molybdenum tube 1, solder 2, w base 3.
The specific embodiment
The prepared cathode diameter of the present invention is 3.6mm, and thickness is 2mm.
Technology 1:
1) palladium powder, molybdenum powder and cobalt powder are put into 500 ℃ of hydrogen furnace annealings respectively,, and strengthened its plasticity with thorough purification.
2) take by weighing 1 gram palladium powder, 10 gram molybdenum powders, 40 gram cobalt powders, (all having converted is 100%, and the purity of palladium powder is 95.4%, and the purity of molybdenum powder is 95%, and the purity of cobalt powder is 95.5%) is ground to 300 orders with these three kinds of materials, mixing, compacting;
3) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1600 ℃ of insulations after 120 seconds, reduces to 1000 ℃ again, is incubated 3 minutes, cool to room temperature;
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1500 ℃ flooded 10 minutes, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Examination criteria: detection of the present invention with service life of cathode as its examination criteria.
Detection method: above-mentioned sample is 2 * 10 in vacuum all
-5Pa, with cathode life testboard etc. as its detection method.
Except that palladium powder, molybdenum powder, cobalt powder purity difference, all the other are identical with technology 1.
Table 1:
| Formula number | 1-1 | 1-2 | 1-3 | 1-4 | 1-5 | 1-6 | 1-7 |
| Palladium powder purity (%) | 94.2 | 95.4 | 97.2 | 98.4 | 99.1 | 99.6 | 99.99 |
| Molybdenum powder purity (%) | 94.4 | 95 | 97.5 | 98.6 | 99.5 | 99.8 | 99.99 |
| Cobalt powder purity (%) | 93.8 | 95.5 | 96.2 | 98.7 | 99.2 | 99.6 | 99.99 |
| Life-span (hour) | 1500 | 1900 | 2300 | 2430 | 2500 | 2510 | 2520 |
Along with palladium powder, molybdenum powder, cobalt powder purity improve, the effect of preparation cathode is just good more.
Get prescription 1-7, except that the fineness of palladium powder, molybdenum powder, cobalt powder, all the other are identical with technology 1.
Table 2
| Formula number | 2-1 | 2-2 | 1-7 | 2-4 | 2-5 | 2-6 |
| Palladium powder, molybdenum powder, cobalt powder fineness (order) | 180 | 200 | 300 | 400 | 500 | 550 |
| Life-span (hour) | 1600 | 2200 | 2520 | 2530 | 2540 | 2540 |
The order number of palladium powder, molybdenum powder, cobalt powder is high more, and prepared cathode performance is good more.
Get prescription 1-7, except that palladium powder, molybdenum powder, cobalt powder weight ratio, all the other are identical with technology 1, and the palladium powder is got 1 gram.
Table 3
| Formula number | 3-1 | 3-2 | 1-7 | 3-4 | 3-5 | 3-6 | 3-7 | 3-8 |
| Molybdenum powder (being equivalent to 100% purity) gram | 4 | 5 | 10 | 20 | 30 | 35 | 40 | 45 |
| Cobalt powder (being equivalent to 100% purity) gram | 9 | 10 | 40 | 50 | 60 | 75 | 90 | 95 |
| Life-span (hour) | 1650 | 2000 | 2520 | 2530 | 2500 | 2450 | 2430 | 1780 |
Palladium powder, molybdenum powder, cobalt powder, its weight ratio are 1: 5-40: 10-90, the better performances of negative electrode.
Following process is filled a prescription with 1-7.
Technology 2:
1) palladium powder, molybdenum powder and cobalt powder are put into 700 ℃ of hydrogen furnace annealings respectively,, and strengthened its plasticity with thorough purification.
2) take by weighing three kinds of materials by formula ratio, these three kinds of materials are ground to 300 orders, mixing, compacting;
3) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1550 ℃ of insulations after 60 seconds, reduces to 1100 ℃ again, is incubated 2.5 minutes, cool to room temperature;
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1450 ℃ flooded 2 minutes, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Technology 3:
1) palladium powder, molybdenum powder and cobalt powder are put into 1000 ℃ of hydrogen furnace annealings respectively,, and strengthened its plasticity with thorough purification.
2) take by weighing three kinds of materials by formula ratio, these three kinds of materials are ground to 300 orders, mixing, compacting;
3) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1600 ℃ of insulations after 45 seconds, reduces to 1200 ℃ again, is incubated 2 minutes, cool to room temperature;
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1450 ℃ flooded 1 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Technology 4:
1) palladium powder, molybdenum powder and cobalt powder are put into 1350 ℃ of hydrogen furnace annealings respectively,, and strengthened its plasticity with thorough purification.
2) take by weighing three kinds of materials by formula ratio, these three kinds of materials are ground to 300 orders, mixing, compacting;
3) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1600 ℃ of insulations after 5 seconds, reduces to 1250 ℃ again, is incubated 1.5 minutes, cool to room temperature;
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1500 ℃ flooded 0.5 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
Technology 5:
1) palladium powder, molybdenum powder and cobalt powder are put into 1500 ℃ of hydrogen furnace annealings respectively,, and strengthened its plasticity with thorough purification.
2) take by weighing three kinds of materials by formula ratio, these three kinds of materials are ground to 300 orders, mixing, compacting;
3) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1600 ℃ of insulations after 5 seconds, reduces to 1350 ℃ again, is incubated 1 minute, cool to room temperature;
4) cathode that step 3 is made places the aluminate powder, hydrogen atmosphere, and 1500 ℃ flooded 0.5 minute, and the floating salt behind the dipping is removed with tungsten wire cotton mass.
5) heater is installed.
The sample number into spectrum of technology 2 preparations is 4-2, and the sample number into spectrum of technology 3 preparations is 4-3, and the like,
Table 4
| Numbering | Life-span (hour) |
| 1-7 | 2520 |
| 4-2 | 2480 |
| 4-3 | 2510 |
| 4-4 | 2490 |
| 4-5 | 2500 |
Technology 1-5 all can realize the present invention.
Claims (7)
1, a kind of impregnated barium-tungsten cathode solder, it is characterized in that: form by palladium powder, molybdenum powder, cobalt powder, its weight ratio is that purity is converted to 100% palladium powder: purity is converted to 100% molybdenum powder: purity is converted to 100% cobalt powder=1: 5-40: 10-90, and described palladium powder, molybdenum powder, cobalt powder purity are 95-100%.
2, a kind of impregnated barium-tungsten cathode solder according to claim 1 is characterized in that: the solder weight ratio is that purity is converted to 100% palladium powder: purity is converted to 100% molybdenum powder: purity is converted to 100% cobalt powder=1: 10-40: 40-70; Described palladium powder, molybdenum powder, cobalt powder purity are 99-100%.
3, the using method of a kind of impregnated barium-tungsten cathode solder according to claim 1 comprises the following steps:
A) molybdenum powder, palladium powder and cobalt powder are put into 500-1500 ℃ of hydrogen furnace annealing respectively;
B) get palladium powder, molybdenum powder and cobalt powder by weight, these three kinds of materials are ground to are not less than 200 orders, mixing, compacting;
C) solder is put on the intersection of non-surface of emission W base and molybdenum tube, thickness 2-3 millimeter, the negative electrode after coating is put the hydrogen stove into, is warmed up to 1200-1700 ℃ of insulation 5-120 after second, reduces to 1000-1350 ℃ again, and insulation is not less than 1 minute, cool to room temperature;
D) cathode that step c is made places the aluminate powder, hydrogen atmosphere, and 1500-2000 ℃ flooded 1-10 minute, and the floating salt behind the dipping is removed with cobalt silk flosssilk wadding group;
E) heater is installed.
4, the using method of a kind of impregnated barium-tungsten cathode solder according to claim 3 is characterized in that: the fineness that material grinds among the step b is the 300-500 order.
5, the using method of a kind of impregnated barium-tungsten cathode solder according to claim 3 is characterized in that: the temperature retention time among the step c 1200-1700 ℃ the time is 5-60 second.
6, the using method of a kind of impregnated barium-tungsten cathode solder according to claim 3 is characterized in that: the temperature retention time in steps d is 1-2 minute.
7, the using method of a kind of impregnated barium-tungsten cathode solder according to claim 3 is characterized in that: prepared cathode diameter is 2-10mm, and thickness is 1-4mm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100942140A CN100431770C (en) | 2005-08-31 | 2005-08-31 | Impregnated barium-tungsten cathode solder and method for using same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100942140A CN100431770C (en) | 2005-08-31 | 2005-08-31 | Impregnated barium-tungsten cathode solder and method for using same |
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| CN1923434A CN1923434A (en) | 2007-03-07 |
| CN100431770C true CN100431770C (en) | 2008-11-12 |
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| CNB2005100942140A Expired - Fee Related CN100431770C (en) | 2005-08-31 | 2005-08-31 | Impregnated barium-tungsten cathode solder and method for using same |
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| CN102500954A (en) * | 2011-11-23 | 2012-06-20 | 安徽华东光电技术研究所 | Alloy solder for dipping barium tungsten cathode and welding method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01307134A (en) * | 1988-06-02 | 1989-12-12 | Mitsubishi Electric Corp | Impregnated cathode |
| US4957463A (en) * | 1990-01-02 | 1990-09-18 | The United States Of America As Represented By The Secretary Of The Army | Method of making a long life high current density cathode from tungsten and iridium powders using a quaternary compound as the impregnant |
| CN1311725A (en) * | 1998-05-29 | 2001-09-05 | 联合讯号公司 | Cobalt-chromium-palladium-based brazing alloys |
| CN1538482A (en) * | 2003-04-17 | 2004-10-20 | 中国科学院电子学研究所 | Dipped barium tungsten cathode based on tungsten irridium alloy and its preparation method |
| CN1583353A (en) * | 2004-05-24 | 2005-02-23 | 西北有色金属研究院 | High-temperature brazing material for palladium-containing nickel-based multi-element alloy |
-
2005
- 2005-08-31 CN CNB2005100942140A patent/CN100431770C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01307134A (en) * | 1988-06-02 | 1989-12-12 | Mitsubishi Electric Corp | Impregnated cathode |
| US4957463A (en) * | 1990-01-02 | 1990-09-18 | The United States Of America As Represented By The Secretary Of The Army | Method of making a long life high current density cathode from tungsten and iridium powders using a quaternary compound as the impregnant |
| CN1311725A (en) * | 1998-05-29 | 2001-09-05 | 联合讯号公司 | Cobalt-chromium-palladium-based brazing alloys |
| CN1538482A (en) * | 2003-04-17 | 2004-10-20 | 中国科学院电子学研究所 | Dipped barium tungsten cathode based on tungsten irridium alloy and its preparation method |
| CN1583353A (en) * | 2004-05-24 | 2005-02-23 | 西北有色金属研究院 | High-temperature brazing material for palladium-containing nickel-based multi-element alloy |
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| CN1923434A (en) | 2007-03-07 |
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Granted publication date: 20081112 Termination date: 20130831 |