CN102768928B - Cathode salt and preparation method thereof, barium-tungsten cathode containing cathode salt and preparation method thereof - Google Patents
Cathode salt and preparation method thereof, barium-tungsten cathode containing cathode salt and preparation method thereof Download PDFInfo
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- CN102768928B CN102768928B CN201210090621.4A CN201210090621A CN102768928B CN 102768928 B CN102768928 B CN 102768928B CN 201210090621 A CN201210090621 A CN 201210090621A CN 102768928 B CN102768928 B CN 102768928B
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- 150000003839 salts Chemical class 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- WMTSAHAFZXEJBV-UHFFFAOYSA-N [Ba].[W] Chemical compound [Ba].[W] WMTSAHAFZXEJBV-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000000498 ball milling Methods 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 17
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000007598 dipping method Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 24
- 238000009413 insulation Methods 0.000 claims description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 16
- 229910052739 hydrogen Inorganic materials 0.000 claims description 16
- 239000012298 atmosphere Substances 0.000 claims description 15
- 238000000992 sputter etching Methods 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 9
- 239000004411 aluminium Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- ILNKLXHFYKXPKY-UHFFFAOYSA-N iridium osmium Chemical group [Os].[Ir] ILNKLXHFYKXPKY-UHFFFAOYSA-N 0.000 claims description 7
- 238000005530 etching Methods 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims 3
- 239000002184 metal Substances 0.000 claims 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 1
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 238000010849 ion bombardment Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 10
- 239000000463 material Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- WUAPFZMCVAUBPE-UHFFFAOYSA-N rhenium atom Chemical compound [Re] WUAPFZMCVAUBPE-UHFFFAOYSA-N 0.000 description 1
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- Solid Thermionic Cathode (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention discloses a cathode salt, a preparation method thereof and a cathode salt containing the sameThe barium-tungsten cathode of the cathode salt and the preparation method thereof, the cathode salt contained in the cathode comprises the following components by mass: BaCO34～5，CaCO30.4～0.7，Al2O31; the preparation method comprises weighing, ball milling, pressing into blocks and sintering; the preparation method of the barium-tungsten cathode containing the cathode salt comprises the steps of cathode substrate preparation, cathode salt dipping, cathode turning and cathode emission surface coating. The barium-tungsten cathode prepared by the cathode salt can resist ion bombardment, the microwave tube has long service life, and all technical indexes can meet the design requirements.
Description
Technical field
The present invention relates to microwave device technology field, be specifically related to a kind of cathode salt and preparation method thereof, barium-tungsten dispense cathode containing this cathode salt and preparation method thereof.
Background technology
In some microwave tube, due to its operation principle, in pipe work process, some ions etc. can be produced and return Hong negative electrode.Under such operational environment, cathode emissive surface needs to stand bombardment, could ensure the performance of microwave tube.Existing barium-tungsten dispense cathode is in the use procedure of pipe, after emitting surface suffers Ions Bombardment, there is the phenomenon that emission current declines, the technical indicator such as power, percent of pass, life-span of pipe does not reach requirement, there is this phenomenon, mainly the not resistance to Ions Bombardment of negative electrode, after suffering Ions Bombardment, the original normal transmission state of cathode surface is destroyed, and emitting material simple substance barium can not move timely and be supplemented to emitting surface.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of cathode salt and preparation method thereof, barium-tungsten dispense cathode containing this cathode salt and preparation method thereof, the barium-tungsten dispense cathode ability Ions Bombardment using this cathode salt to prepare, microwave tube long service life, all technical all can reach designing requirement.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of cathode salt, its raw material components amount of substance ratio is: BaCO
34 ~ 5, CaCO
30.4 ~ 0.7, Al
2o
31; Preferably its raw material components amount of substance ratio is: BaCO
34.5, CaCO
30.55, Al
2o
31; The purity level of three kinds of materials be analyze pure or analyze pure more than.
Prepare a method for this cathode salt, comprise the following steps:
1), BaCO is taken by formula ratio
3, CaCO
3, Al
2o
3, then carry out ball milling, raw material fully mixed;
2), dry;
3), briquet;
4), just compacting after block powder sinter in nitrogen atmosphere, sintering temperature 1300 DEG C ~ 1400 DEG C, insulation 1h ~ 2h.
A kind of negative electrode, the cathode salt that described negative electrode is prepared containing, for example upper preparation method.
A preparation method for negative electrode, comprises the following steps:
The preparation of A, cathode substrate: the substrate being directly compressed into 22% ~ 30% cell size with tungsten powder, preferably 25% ~ 28%, or be first pressed into the blank of cell size 30% ~ 32%, high temperature sintering in hydrogen atmosphere again, sintering temperature 1975 ± 25 DEG C, sintering time 50 ± 10min, obtains the substrate of 25% ~ 28% cell size; The particle diameter of described tungsten powder is 3 ~ 5 μm;
The preparation of B, cathode salt: take BaCO by formula ratio
3, CaCO
3, Al
2o
3, then carry out ball milling and fully mix;
Dry;
Briquet;
Block powder just after compacting sinters in nitrogen atmosphere, 1300 DEG C ~ 1400 DEG C insulation 1h ~ 2h;
The dipping of C, cathode salt: in hydrogen atmosphere, puts into the cathode salt prepared by substrate, 1650 DEG C ~ 1850 DEG C insulation 1 ~ 3min; Preferably 1750 ± 10 DEG C of insulation 2 ~ 4min;
D, cathode vehicle are processed: removed by the cathode salt of cathode outer surface remnants clean, and on demand cathode vehicle is machined to required size;
E, cathode emissive surface ion etching and overlay film: first cathode surface is carried out ion etching, etching depth 5 μm ~ 9 μm, and then carry out surface and cover metallic film, described metallic film is osmium iridium aluminium film, osmium iridium aluminium mass ratio is 49.5: 49.5: 1, and thicknesses of layers is 0.2 μm ~ 0.6 μm.
The present invention through lot of experiments, by adjustment cathode salt in BaO, CaO and Al
2o
3rational proportion, while increase BaO content, the content of adjustment CaO, simultaneously by the cell size of structure adjusting cathode substrate, that adds target surface carries out alloyed precious metal overlay film, thus the evaporation of good control cathode salt, the resistance to Ions Bombardment performance of barium-tungsten dispense cathode using this cathode salt to prepare is increased greatly, the Ions Bombardment produced in the microwave tube course of work can be resisted, after suffering Ions Bombardment, emitting material simple substance barium promptly can move and be supplemented to emitting surface, ensure the emission current of negative electrode, and due to barium content abundant in negative electrode, the life-span of negative electrode can be ensured, thus the performance of pipe can be ensured.
Embodiment
Embodiment 1
A kind of cathode salt, its raw material components amount of substance ratio is: BaCO
34, CaCO
30.4, Al
2o
31.
Prepare a method for this cathode salt, comprise the following steps:
1), the pure BaCO of analysis is taken respectively by formula ratio
378.9g, CaCO
34g, Al
2o
3three kinds of materials are put into agate tank by 10.2g, and get the agate ball of 5 diameter 15mm and 4 25mm, get pure water 0.1L, together put into agate tank and carry out ball milling 36h, fully mix;
2), by the powder mixed after ball milling take out from agate tank, in baking oven, 120 DEG C are dried 24h, are dried by powder;
3) be, 0.4T/cm by unit pressure
2pressure, powder pressing is become the bulk of thickness 12mm;
4), by the block powder after compacting sinter in the hydrogen atmosphere of drying, sintering temperature 1300 DEG C insulation 2h.Prepare negative electrode, comprise the following steps:
The preparation of A, cathode substrate: the substrate being directly compressed into 25% cell size with tungsten powder;
The dipping of B, cathode salt: in hydrogen atmosphere, puts into the cathode salt prepared by the substrate prepared, be heated to 1650 DEG C of insulation 1min;
C, cathode vehicle are processed: removed by the cathode salt of cathode outer surface remnants clean, cathode vehicle is machined to required size, cathode emission facing amount 0.3mm.
D, cathode emissive surface ion etching and overlay film: first cathode surface is carried out ion etching 7 μm, then carry out surface and be covered with osmium iridium aluminium film, thicknesses of layers 0.3 μm.
Embodiment 2
A kind of cathode salt, its raw material components amount of substance ratio is: BaO4.5, CaO0.55, Al
2o
31.
Prepare a method for this cathode salt, comprise the following steps:
1), the pure BaCO of analysis is taken respectively by formula ratio
388.8g, CaCO
35.5g, Al
2o
3three kinds of materials are put into agate tank by 10.2g, and get the agate ball of 5 diameter 15mm and 4 25mm, get pure water 0.125L, carry out ball milling 42h, fully mix; 2), by the powder mixed after ball milling take out from agate tank, in baking oven, 150 DEG C are dried 18h, are dried by powder;
3) be, by unit pressure the pressure of 0.6T/cm2, powder pressing become the bulk of thickness 11mm;
4), by the block powder after compacting sinter in the hydrogen atmosphere of drying, sintering temperature 1350 DEG C insulation 1.5h.Prepare negative electrode, comprise the following steps:
The preparation of A, cathode substrate: be directly compressed into the substrate of 28% with tungsten powder;
The dipping of B, cathode salt: in hydrogen atmosphere, puts into the cathode salt prepared by the substrate prepared, be heated to 1750 DEG C of insulation 2min;
C, cathode vehicle are processed: removed by the cathode salt of cathode outer surface remnants clean, cathode vehicle is machined to required size, cathode emission facing amount 0.35mm.
D, cathode emissive surface ion etching and overlay film: first cathode surface is carried out ion etching 7 μm, then carry out surface and be covered with osmium iridium aluminium film, thicknesses of layers 0.5 μm.
Embodiment 3
A kind of cathode salt, its raw material components amount of substance ratio is: BaCO
35, CaCO
30.7, Al
2o
31.
Prepare a method for this cathode salt, comprise the following steps:
1), the pure BaCO of analysis is taken respectively by formula ratio
398.7g, CaCO
37g, Al
2o
3three kinds of materials are put into agate tank by 10.2g, and get the agate ball of 5 diameter 15mm and 4 25mm, get pure water 0.16L, carry out ball milling 48h, fully mix;
2), by the powder mixed after ball milling take out from agate tank, in baking oven, 180 DEG C are dried 12h, are dried by powder;
3) be, by unit pressure the pressure of 0.8T/cm2, powder pressing become the bulk of thickness 10mm;
4), by the block powder after compacting sinter in the hydrogen atmosphere of drying, sintering temperature 1400 DEG C insulation 1h.
Prepare the negative electrode of resistance to Ions Bombardment, comprise the following steps:
The preparation of A, cathode substrate: the blank being first pressed into 30% cell size with tungsten powder, then through hydrogen high temperature sintering, sintering temperature 1975 DEG C, sintering time 50min, obtains the substrate of 26% cell size.
The dipping of B, cathode salt: in hydrogen atmosphere, puts into the cathode salt prepared by the substrate prepared, be heated to 1850 DEG C of insulation 1min;
C, cathode vehicle are processed: removed by the cathode salt of cathode outer surface remnants clean, cathode vehicle is machined to required size, cathode emission facing amount 0.3mm.
D, cathode emissive surface ion etching and overlay film: first cathode surface is carried out ion etching 7 μm, then be covered with osmium iridium aluminium film on surface, thicknesses of layers 0.6 μm.
Embodiment 4
A kind of cathode salt, its raw material components amount of substance ratio is: BaO4.5, CaO0.55, Al
2o
31.
Prepare a method for this cathode salt, comprise the following steps:
1), the pure BaCO of analysis is taken respectively by formula ratio
388.8g, CaCO
35.5g, Al
2o
3three kinds of materials are put into agate tank by 10.2g, and get the agate ball of 5 diameter 15mm and 4 25mm, get pure water 0.125L, carry out ball milling 42h, fully mix;
2), by the powder mixed after ball milling take out from agate tank, in baking oven, 150 DEG C are dried 18h, are dried by powder;
3) be, by unit pressure the pressure of 0.6T/cm2, powder pressing become the bulk of thickness 11mm;
4), by the block powder after compacting sinter in the hydrogen atmosphere of drying, sintering temperature 1350 DEG C insulation 1.5h.
Prepare barium-tungsten dispense cathode, comprise the following steps:
The preparation of A, cathode substrate: the substrate being directly compressed into 26% cell size with tungsten powder;
The dipping of B, cathode salt: in hydrogen atmosphere, puts into the cathode salt prepared by the substrate prepared, be heated to 1750 DEG C of insulation 2min;
C, cathode vehicle are processed: removed by the cathode salt of cathode outer surface remnants clean, cathode vehicle is machined to required size, cathode emission facing amount 0.3mm.
D, cathode emissive surface ion etching and overlay film: first cathode surface is carried out ion etching 8 μm, then carry out surface and be covered with rhenium aluminium film, thicknesses of layers 0.5 μm.
Table 1 is cathode performance data prepared by embodiment 1 ~ 4, the situation of change of condition is caused by Ions Bombardment cathode performance for cathode surface under same state.
Table 1
| Embodiment | Emission current decline degree after work 500h | Emission current decline degree after work 1000h |
| 1 | 5％ | 13％ |
| 2 | 2％ | 5％ |
| 3 | 5％ | 14％ |
| 4 | 4％ | 9％ |
Claims (8)
1. a cathode salt, its raw material components amount of substance ratio is: BaCO
34 ~ 5, CaCO
30.4 ~ 0.7, Al
2o
31;
Described cathode salt is prepared by following method:
1), BaCO is taken by formula ratio
3, CaCO
3, Al
2o
3, then carry out ball milling, fully mix;
2), dry;
3), briquet;
4), by the block powder after compacting sinter in hydrogen atmosphere, sintering temperature 1300 DEG C ~ 1400 DEG C, insulation 1h ~ 2h.
2. cathode salt as claimed in claim 1, is characterized in that: its raw material components amount of substance ratio is: BaCO
34.5, CaCO
30.55, Al
2o
31.
3. prepare a method for cathode salt, comprise the following steps:
1), BaCO is taken by formula ratio
3, CaCO
3, Al
2o
3, then carry out ball milling, fully mix;
2), dry;
3), briquet;
4), by the block powder after compacting sinter in hydrogen atmosphere, sintering temperature 1300 DEG C ~ 1400 DEG C, insulation 1h ~ 2h.
4. preparation method as claimed in claim 3, is characterized in that: step 1) in ball milling condition for carry out ball milling 36h ~ 48h in agate tank; Step 2) drying condition be 120 DEG C ~ 180 DEG C dry 12h ~ 24h; Step 3) condition of briquet is 0.4 ~ 0.8T/cm by unit pressure
2pressure, powder pressing is become block.
5. a barium-tungsten dispense cathode, the cathode salt that described barium-tungsten dispense cathode is prepared containing, for example preparation method described in claim 3 or 4.
6. a preparation method for barium-tungsten dispense cathode, comprises the following steps:
The preparation of A, cathode substrate: the substrate of making 22% ~ 30% cell size with tungsten powder;
The preparation of B, cathode salt: take BaCO by formula ratio
3, CaCO
3, Al
2o
3, then carry out ball milling and fully mix; Dry;
Briquet;
Block powder after compacting is sintered in hydrogen atmosphere, 1300 DEG C ~ 1400 DEG C insulation 1h ~ 2h;
The dipping of C, cathode salt: in hydrogen atmosphere, puts into the cathode salt prepared by cathode substrate, 1650 DEG C ~ 1850 DEG C insulation 1 ~ 3min;
D, cathode vehicle are processed: removed by the cathode salt of cathode outer surface remnants clean, and on demand cathode vehicle is machined to required size;
E, cathode emissive surface etching and overlay film: first cathode surface is carried out ion etching, and then carry out surface again and cover metal film.
7. preparation method as claimed in claim 6, is characterized in that: in steps A, tungsten powder direct pressing is used in the preparation of cathode substrate, and cell size is 25% ~ 28%; In step B, ball milling condition for carry out ball milling 36h ~ 48h in agate tank, and drying condition is 120 DEG C ~ 180 DEG C and dries 12h ~ 24h, and the condition of briquet is 0.4 ~ 0.8T/cm by unit pressure
2pressure, become by powder pressing thickness to be no more than the bulk of 12mm; In step C, heat-retaining condition is 1750 ± 10 DEG C of insulation 2min; Step e intermediate ion etching depth 5 μm ~ 9 μm, it is osmium iridium aluminium film that metal film is covered in institute, and thicknesses of layers is 0.2 μm ~ 0.6 μm.
8. preparation method as claimed in claim 6, it is characterized in that: in steps A, the preparation of cathode substrate is the blank being first pressed into 30% ~ 32% cell size with tungsten powder, high temperature sintering in hydrogen atmosphere again, obtain the substrate of 22% ~ 30% cell size, sintering temperature 1975 ± 25 DEG C, sintering time 50 ± 10min; In step B, ball milling condition for carry out ball milling 36h ~ 48h in agate tank, and drying condition is 120 DEG C ~ 180 DEG C and dries 12h ~ 24h, and the condition of briquet is 0.4 ~ 0.8T/cm by unit pressure
2pressure, become by powder pressing thickness to be no more than the bulk of 12mm; In step C, heat-retaining condition is 1750 ± 10 DEG C of insulation 2min; Step e intermediate ion etching depth 5 μm ~ 9 μm, it is osmium iridium aluminium film that metal film is covered in institute, and thicknesses of layers is 0.2 μm ~ 0.6 μm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210090621.4A CN102768928B (en) | 2012-03-30 | 2012-03-30 | Cathode salt and preparation method thereof, barium-tungsten cathode containing cathode salt and preparation method thereof |
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| 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 |
| CN105118760B (en) * | 2015-08-24 | 2017-06-16 | 中国科学院电子学研究所 | The method for preparing W-Re base barium-tungsten dispense cathode |
| CN105331840B (en) * | 2015-10-20 | 2017-06-13 | 安泰科技股份有限公司 | A kind of tungsten base electrode material and preparation method thereof |
| CN105755329A (en) * | 2016-03-31 | 2016-07-13 | 苏州睿昕汽车配件有限公司 | Preparation method of high-strength piston material of automobile diesel engine |
| CN109860000A (en) * | 2019-04-02 | 2019-06-07 | 戴连孚 | A kind of atom lamel cathode preparation method |
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| EP0831512A1 (en) * | 1995-06-09 | 1998-03-25 | Kabushiki Kaisha Toshiba | Impregnated cathode structure, cathode substrate used for the structure, electron gun structure using the cathode structure, and electron tube |
| CN102254766A (en) * | 2010-05-19 | 2011-11-23 | 中国科学院电子学研究所 | Method for preparing storage-type rare-earth oxide cathode |
| CN102315062A (en) * | 2010-07-07 | 2012-01-11 | 中国科学院电子学研究所 | Long-life filmed impregnated barium-tungsten cathode and preparation method thereof |
-
2012
- 2012-03-30 CN CN201210090621.4A patent/CN102768928B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0831512A1 (en) * | 1995-06-09 | 1998-03-25 | Kabushiki Kaisha Toshiba | Impregnated cathode structure, cathode substrate used for the structure, electron gun structure using the cathode structure, and electron tube |
| CN102254766A (en) * | 2010-05-19 | 2011-11-23 | 中国科学院电子学研究所 | Method for preparing storage-type rare-earth oxide cathode |
| CN102315062A (en) * | 2010-07-07 | 2012-01-11 | 中国科学院电子学研究所 | Long-life filmed impregnated barium-tungsten cathode and preparation method thereof |
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