CN105304436B - Directly heated cathode and preparation method thereof - Google Patents
Directly heated cathode and preparation method thereof Download PDFInfo
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- CN105304436B CN105304436B CN201510756121.3A CN201510756121A CN105304436B CN 105304436 B CN105304436 B CN 105304436B CN 201510756121 A CN201510756121 A CN 201510756121A CN 105304436 B CN105304436 B CN 105304436B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/894—Dioscoreaceae (Yam family)
- A61K36/8945—Dioscorea, e.g. yam, Chinese yam or water yam
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/42—Cucurbitaceae (Cucumber family)
- A61K36/428—Trichosanthes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/489—Sophora, e.g. necklacepod or mamani
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/70—Polygonaceae (Buckwheat family), e.g. spineflower or dock
Abstract
The invention discloses a directly heated cathode. A refractory oxide containing Y2O3 is adopted as an active substance; and the active substance is subjected to dip-coating on the surface of a pure tungsten filament cathode of which the surface is provided with a tungsten sponge layer to form the directly heated cathode. The invention further discloses a preparation method of the directly heated cathode. According to the directly heated cathode disclosed by the invention, the thermal emission current density of the pure tungsten filament cathode is greatly improved; and the working lifetime of the cathode is prolonged, so that the working lifetime of a high-power continuous wave magnetron is prolonged.
Description
Technical field
The present invention relates to electric vacuum technology field, relates more specifically to a kind of direct-heated cathode and preparation method thereof, the moon
Pole adopts Y containing rare earth oxide2O3Refractory oxides active substance, compared to pure tungsten wire cathode, can reduce the work temperature of negative electrode
Degree, improves the emission of negative electrode, extends the life-span of negative electrode.
Background technology
As magnetron develops towards high-output power direction, ordinary oxide negative electrode, barium-tungsten dispense cathode etc. are not resistant to because of which
High pressure, bombards intolerant to electronic and ionic, it is easy to which the shortcomings of electric spark occurs can hardly be applied.Therefore, at middle power (less than 3kW)
Using the thoriated tungsten cathode of carbonization in magnetron.And in the high power CW ripple magnetron pipe of high anode voltage (more than 10kV)
In general directly-heated type pure tungsten (W) wire cathode using emissive power very little, this is because pure tungsten wire cathode is compared to common oxidation
Thing negative electrode and barium-tungsten dispense cathode, good with launch stability, resistance to electronics, ion bom bardment ability are strong, the advantages of anti-toxic is strong, compare
In carbonized thoriated tungsten carthode, possess the longer life-span.But, ensureing normal output power situation in high power CW ripple magnetron
Under, its negative electrode is generally operational between 2450～2700K temperature, causes the evaporation of its cathode surface too fast, when the diameter of negative electrode it is low
When the 90% of initial diameter, that is, declare cathode life end, therefore in continuous wave magnetron the pure W wire cathodes life-span termination
It is the one of the main reasons for causing magnetron life to terminate.
The content of the invention
In view of this, it is an object of the invention to provide a kind of direct-heated cathode and preparation method thereof, to improve negative electrode
Emission, the operating temperature for reducing pure tungsten wire cathode, the life-span for extending negative electrode.
To achieve these goals, the invention provides a kind of preparation method of direct-heated cathode, it is characterised in that include
Following steps：
A, uniformly apply tungsten powder layer in tungsten filament substrate surface, be placed in high temperature hydrogen furnace at 1600 DEG C ± 50 DEG C insulation 10～
Tungsten spongy layer is formed after 15 minutes；
B, by Y2O3、Gd2O3、HfO2(45～50) % by weight percentage: (5～10) %: (45～50) % ball milling mixings
Prepared Y2O3、Gd2O3And HfO2Mixed-powder, and be pressed into bulk；
C, the block that step b is obtained is put in Muffle furnace, is sintered 2～4 hours in 1450 ± 50 DEG C, synthesis is containing Y2O3
Refractory oxides active substance；
D, by step c obtain containing Y2O3Refractory oxides block grind 2～3 hours；
E, by step d obtain containing Y2O3Refractory oxides active substance be uniformly applied to tungsten sponge layer surface and be prepared into
Required direct-heated cathode.
And, the direct-heated cathode that a kind of preparation method by above-mentioned direct-heated cathode is prepared.
Understood based on above-mentioned technical proposal, the emission current that preparation method of the invention can improve pure tungsten wire cathode is close
Degree, the operating temperature for reducing pure tungsten wire cathode, reduction cathode surface evaporation rate, prolongation cathode life.Containing Y2O3Refractory oxides
Sintering one layer of tungsten spongy layer between active material layer and pure tungsten silk substrate can not only increase the amount of storage of active substance, Er Qieneng
Enough increase the conductivity between pure tungsten silk substrate and coating layer of active substance.Using the higher HfO of fusing point2Ensure that active substance
Still there is relatively low evaporation rate at high temperature.Additionally, containing Y2O3Refractory oxides material has activity well, can make pure tungsten silk
Negative electrode just can obtain larger emission at a lower temperature, at the same time, this containing Y2O3Refractory oxides active matter
Matter has larger resistance to electronics, ion bom bardment and anti-poisoning energy compared to ordinary oxide, barium-tungsten dispense cathode and thoriated-tungsten cathode
Power, is a kind of ideal cathode material for being suitable for and being operated in high power CW ripple magnetron environment.
Description of the drawings
Fig. 1 is the preparation flow of the common pure tungsten wire cathode of high power CW ripple magnetron
Fig. 2 contains Y for the present invention2O3The preparation method flow chart of oxide active material layer tungsten cathode；
Fig. 3 is directly-heated type low temperature high current-density cathodes structural representation of the present invention；
Fig. 4 is the DC voltage current characteristic curve synoptic diagram of directly-heated type low temperature high current-density cathodes of the present invention；
Fig. 5 is the life curve schematic diagram of directly-heated type low temperature high current-density cathodes of the present invention.
Specific embodiment
For making the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in further detail.
The invention discloses a kind of direct-heated cathode, which is adopted containing rare earth oxide Y2O3Refractory oxides as work
Property material, by the active substance dip-coating surface for tungsten spongy layer pure tungsten wire cathode surface.The directly-heated type low temperature of the present invention is big
Current density cathode can be worked at low temperature, and life-span of the negative electrode at present on life-span platform alreadys exceed 3000 hours.
The invention also discloses a kind of preparation method of direct-heated cathode, comprises the following steps：
A, on tungsten filament substrate surface is uniformly sprayed after tungsten powder layer, be incubated 10 at being put into 1600 ± 50 DEG C in high temperature hydrogen furnace
The tungsten spongy layer with deposit active substance ability is formed after～15 minutes；
B, by Y2O3、Gd2O3、HfO2(45～50) % by weight percentage: (5～10) %: (45～50) % ball milling mixings
Prepared Y2O3、Gd2O3And HfO2Mixed-powder, and be pressed into bulk；
C, the block that step b is obtained is put in Muffle furnace sinters 2～4 hours in 1450 ± 50 DEG C, synthesis is containing Y2O3's
Refractory oxides active substance；
D, by step c obtain containing Y2O3Refractory oxides block grind 2～3 hours in Achatess alms bowl, be prepared into work
Property material；
E, by step d obtain containing Y2O3The uniform dip-coating of active substance of refractory oxides is prepared in tungsten sponge layer surface
To the direct-heated cathode.
Wherein, the purity of the tungsten powder in step a is 99.9%, and mean diameter is 1～3 μm.
Wherein, it is in the sintering process of the tungsten spongy layer in step a, during intensification, time-consuming linearly to rise from room temperature within 0.5～1 hour
To 1600 ± 50 DEG C, lower the temperature after being incubated 10～15 minutes at 1600 ± 50 DEG C, it is during cooling, time-consuming 2～4 hours from 1600 ± 50 DEG C
Room temperature is down to linearly.
Wherein, the ball milling in step b, is carried out in agate jar, and adds the pure anhydrous second of analysis in agate pot
Alcohol or deionized water, suppress behind mixing and ball milling≤24 hour.
Wherein, the Y in step b2O3、Gd2O3、HfO2The purity of three kinds of oxides is 99.9%, its weight percent score
Wei (45～50) %: (5～10) %: (45～50) %.
Wherein, the addition of pure analysis absolute ethyl alcohol or deionized water, be Achatess tank volume≤2/3.
Wherein, in step c, sintering atmosphere is air atmosphere or CO2Atmosphere.
Wherein, the grinding in step d, is carried out in Achatess alms bowl, mixing and ball milling≤3 hour.
Wherein, in step e dip-coating containing Y2O3The active substance thickness of refractory oxides is 10～100 μm.
Fig. 1 is the preparation flow figure of the tungsten cathode of prior art, and Fig. 2 is the present invention containing Y2O3Oxide active material
The preparation flow figure of the tungsten cathode of layer, both compare it can be seen that the inventive point of the present invention is the last two steps.As one
Preferred embodiment, the invention discloses a kind of method for preparing directly-heated type low temperature high current-density cathodes, its step is：Choose pure
Spend for Y that 99.9wt% particle mean sizes are 2～10 μm2O3、Gd2O3、HfO2It is (45～50) % by weight percentage: (5～
10) it is put in the agate pot of dribbling after %: (45～50) % mixing.Pour the pure anhydrous second of analysis of 2/3 volume in agate pot into
Alcohol or deionized water, ball milling mixing more than 24 hours, mix homogeneously on ball mill.Above-mentioned suspension is poured in weighing botle and is put
Under infrared lamp, drying obtains the powder for mixing, and powder is put in mould, with 40kgf/cm on hydraulic press2Pressure
Under be pressed into a diameter of 10mm, the pie shape of a height of 1～2mm；Cake block is put in high temperature muffle furnace, air or CO is passed through2
Gas is sintered, and sintering temperature is 1450 ± 50 DEG C, temperature retention time 2～4 hours.
As shown in figure 3, after 3 surface of tungsten filament substrate uniformly sprays tungsten powder layer, being put into 1600 ± 50 in high temperature hydrogen furnace
Tungsten spongy layer 2 is formed after 10～15 minutes are incubated at DEG C.Then, will sinter containing Y2O3Refractory oxides cake block is put into Achatess
It is ground in alms bowl more than 2 hours, till suitable particles size is ground to, obtains active substance；Will be the active substance 1 equal
It is even to spray in tungsten sponge layer surface, complete the preparation of directly-heated type low temperature high current-density cathodes.The present invention's for preparing is straight
The structure of heated cathode is as shown in Figure 3.
The tungsten cathode of the present invention is loaded in cylindrical shape anode vacuum diode, through 500 DEG C of insulations in 1～1.5 hour
Afterwards, degassing 5～10 minutes under 50～60mA high frequency electrics, degassing 2～5 minutes under 80～120mA high frequency electrics, now system
Vacuum has been better than 10-5Pa.Through degassing, activate and DC voltage current characteristic test is carried out after seasoned 10 hours or so.
Cathode temperature is measured using optical pyrometer in test.Test result is as shown in Figure 4.
It is this containing Y as can be seen from Figure 42O3Refractory oxides active substance W wire cathodes 1300 DEG C of cathode temperature, 1400
DEG C, 1500 DEG C when Cathode DC deviation point emission be respectively 0.4A/cm2、1.0A/cm2、4.0A/cm2, it is much larger than
The emission of pure W wire cathodes under the same terms.When cathode temperature be 1600 DEG C, 1700 DEG C when Cathode DC deviation point
Emission is respectively greater than 7.74A/cm2、10.5A/cm2, show that this negative electrode has powerful heat emission ability.
By the vacuum diode insertion life-span of the tungsten cathode equipped with the present invention after DC voltage current characteristic has been tested
Platform carries out life test, and test result is as shown in Figure 5.It is 1600 DEG C in brightness temperature that Fig. 5 is the negative electrode, and initial transmissions electric current is close
Degree 1.5A/cm2When life curve.As can be seen from Figure 5 to already exceed 3000 little the negative electrode life-span under these conditions
When, and current cathode life is still in proceeding, from Fig. 5 it is known that after 3000 hour life-span of negative electrode, its
Draw electric current density and be still not less than 1.5A/cm2, illustrate that the cathode life performance has reached high power magnetron to practical cloudy
The requirement in pole life-span, is a kind of new directly-heated type low temperature high current-density cathodes.Additionally, in the life span of negative electrode, it is cloudy
The operating temperature of pole is always held at 1600 DEG C or so, does not monitor that the phenomenons such as sparking occurs in the negative electrode, illustrates that the negative electrode has
There is higher job stability.
Particular embodiments described above, has been carried out to the purpose of the present invention, technical scheme and beneficial effect further in detail
Describe in detail bright, it should be understood that the foregoing is only the specific embodiment of the present invention, be not limited to the present invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc. should be included in the protection of the present invention
Within the scope of.
Claims (10)
1. a kind of preparation method of direct-heated cathode, it is characterised in that comprise the following steps：
A, uniformly apply tungsten powder layer in tungsten filament substrate surface, be placed in high temperature hydrogen furnace at 1600 DEG C ± 50 DEG C and be incubated 10～15 points
Tungsten spongy layer is formed after clock；
B, by Y2O3、Gd2O3、HfO2(45～50) % by weight percentage: (5～10) %：(45～50) % ball milling mixings are obtained
Y2O3、Gd2O3And HfO2Mixed-powder, and be pressed into bulk；
C, the block that step b is obtained is put in Muffle furnace, is sintered 2～4 hours in 1450 ± 50 DEG C, synthesis is containing Y2O3Difficulty
Molten oxide active material；
D, by step c obtain containing Y2O3Refractory oxides block grind 2～3 hours；
E, by step d obtain containing Y2O3Refractory oxides active substance be uniformly applied to needed for tungsten sponge layer surface is prepared into
Direct-heated cathode.
2. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that the tungsten powder purity in step a
For 99.9%, mean diameter is 1～3 μm.
3. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that tungsten spongy layer burns in step a
It is during knot, during intensification, time-consuming linearly to rise to 1600 DEG C ± 50 DEG C from room temperature within 0.5～1 hour, in 1600 DEG C of ± 50 DEG C of insulations 10
Lower the temperature after～15 minutes, during cooling, take from 1600 DEG C ± 50 DEG C and be linearly down to room temperature in 2～4 hours.
4. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that the ball milling in step b, be
Carry out in agate jar, and add pure analysis absolute ethyl alcohol or deionized water in agate pot, behind mixing and ball milling≤24 hour
Compacting.
5. the preparation method of direct-heated cathode as claimed in claim 4, it is characterised in that the pure analysis absolute ethyl alcohol is gone
The addition of ionized water, be Achatess tank volume≤2/3.
6. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that the Y in step b2O3、Gd2O3、
HfO2The purity of three kinds of oxides is 99.9%, and its percentage by weight is (45～50) %: (5～10) %: (45～50) %.
7. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that sintering atmosphere is in step c
Air atmosphere or CO2Atmosphere.
8. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that the grinding in step d is logical
Crossing carries out mixing and ball milling to realize in Achatess alms bowl.
9. the preparation method of direct-heated cathode as claimed in claim 1, it is characterised in that dip-coating containing Y in step e2O3
The thickness of refractory oxides active substance is 10～100 μm.
10. the directly-heated that a kind of preparation method of the direct-heated cathode by as described in claim 1 to 9 any one is prepared
Formula negative electrode.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109037007B (en) * | 2018-07-03 | 2021-07-13 | 九江学院 | Preparation method of directly-heated electron bombardment resistant cathode |
| CN110615474A (en) * | 2019-09-16 | 2019-12-27 | 九江学院 | Preparation method of hafnate electron emission active substance for hot cathode |
| CN111850524B (en) * | 2020-07-17 | 2022-08-30 | 广东威特真空电子制造有限公司 | Rare earth tungsten cathode and preparation method and application thereof |
| CN112798650B (en) * | 2020-12-30 | 2023-03-28 | 中国科学院空天信息创新研究院 | Device and method for testing electron bombardment resistance of cathode |
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| WO2003075310A1 (en) * | 2002-03-05 | 2003-09-12 | Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH | Short arc high-pressure discharge lamp- |
| CN101091987A (en) * | 2006-06-22 | 2007-12-26 | 中国科学院电子学研究所 | Method for producing spongy body of tungsten |
| CN101728181A (en) * | 2009-12-06 | 2010-06-09 | 甘肃虹光电子有限责任公司 | Manufacture method of annular barium-tungsten cathode emitter |
| CN102394208A (en) * | 2011-11-02 | 2012-03-28 | 北京工业大学 | Dipped yttrium oxide-tungsten based yttrium and scandate cathode material and manufacturing method thereof |
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2015
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3837909A (en) * | 1972-07-27 | 1974-09-24 | Itt | Coated coil emissive electrode |
| WO2003075310A1 (en) * | 2002-03-05 | 2003-09-12 | Patent-Treuhand-Gesellschaft für elektrische Glühlampen mbH | Short arc high-pressure discharge lamp- |
| CN101091987A (en) * | 2006-06-22 | 2007-12-26 | 中国科学院电子学研究所 | Method for producing spongy body of tungsten |
| CN101728181A (en) * | 2009-12-06 | 2010-06-09 | 甘肃虹光电子有限责任公司 | Manufacture method of annular barium-tungsten cathode emitter |
| CN102394208A (en) * | 2011-11-02 | 2012-03-28 | 北京工业大学 | Dipped yttrium oxide-tungsten based yttrium and scandate cathode material and manufacturing method thereof |
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