CN107331441A - A kind of cathodes heated indirectly by an el heated filament insulating packing and preparation method thereof - Google Patents
A kind of cathodes heated indirectly by an el heated filament insulating packing and preparation method thereof Download PDFInfo
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- CN107331441A CN107331441A CN201710576550.1A CN201710576550A CN107331441A CN 107331441 A CN107331441 A CN 107331441A CN 201710576550 A CN201710576550 A CN 201710576550A CN 107331441 A CN107331441 A CN 107331441A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J23/00—Details of transit-time tubes of the types covered by group H01J25/00
- H01J23/02—Electrodes; Magnetic control means; Screens
- H01J23/04—Cathodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
- H01J9/02—Manufacture of electrodes or electrode systems
- H01J9/04—Manufacture of electrodes or electrode systems of thermionic cathodes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6582—Hydrogen containing atmosphere
Abstract
The invention discloses a kind of cathodes heated indirectly by an el heated filament insulating packing and preparation method thereof, with alumina powder and oxidation yttrium powder by weight percentage (50%~70%)：(30%~50%) it is raw material, by ball milling, drying, sinter, mill, sieve after obtain cathodes heated indirectly by an el heated filament insulating packing, obtained filament assembly is filled using this cathodes heated indirectly by an el heated filament insulating packing, the insulating barrier of densification, the characteristics of insulating barrier has good insulation preformance, breakdown voltage resistant height, heat conduction efficiency is high can be obtained after high temperature sintering.
Description
Technical field
The invention belongs to vacuum microwave devices field, and in particular to a kind of cathodes heated indirectly by an el heated filament insulating packing and its preparation
Method.
Background technology
Electron source in modern high power microwave device, generally uses hot cathode, and filament assembly is used as hot cathode
Thermal source, its structure and performance are directly connected to the performance of device, life and reliability.
As microwave device constantly develops, propose higher requirement to hot cathode, i.e., big emission current ability and
Quick to start ability, negative electrode will quickly start just to be proposed accordingly to the rapidity that heated filament provides the uniformity heated and heat transfer
Requirement, traditional heated filament limited and insulating packing heat conductivility used is bad due to structure, limits what negative electrode quickly started
Ability, especially this defect seems especially prominent on large scale cathode heater, can not meet microwave device to negative electrode
The demand quickly started.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of cathodes heated indirectly by an el heated filament insulating packing and its preparation side
Method, using alumina powder and oxidation yttrium powder as raw material, by ball milling, drying, sinter, mill, sieve after to obtain cathodes heated indirectly by an el hot
Silk insulation filler, obtained filament assembly, the energy after high temperature sintering are filled using this cathodes heated indirectly by an el heated filament insulating packing
Obtain fine and close insulating barrier, the characteristics of insulating barrier has good insulation preformance, breakdown voltage resistant height, heat conduction efficiency is high.
The technical scheme that the present invention takes is：
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing is by alumina powder and oxidation yttrium powder percentage by weight
Than (50%~70%)：(30%~50%) constitute.
The alumina powder and oxidation yttrium powder particle diameter be 5~7um.
Present invention also offers a kind of preparation method of cathodes heated indirectly by an el heated filament insulating packing, the preparation method include with
Lower step：
(1) alumina powder and oxidation yttrium powder per distribution ratio by weight are added distilled water and carries out mixing and ball milling 5~7.5
Hour, (alumina powder+oxidation yttrium powder)：Distilled water=100g：(100~150) mL, and the mixture after ball milling is dried；
(2) by dried mixture compacted, it is put into hydrogen furnace and is sintered；
(3) powder is milled into after mixture of the sintering after blocking is cooled down, 200~600 eye mesh screens is crossed and is sieved, you can
Obtain cathodes heated indirectly by an el heated filament insulating packing.
The step (in 1), the drying temperature is 90~110 DEG C, and the time is 8~10 hours；Ball milling is used to agate
The mode that agate ball is added in tank is carried out, and the weight of the agate ball is the 1.5~2 of alumina powder and oxidation yttrium powder gross weight
Times, a diameter of 10~25mm of agate ball.
In the step (2), dried mixture is put into molybdenum bowl and is compacted；Wet hydrogen work is passed through in the hydrogen furnace
For protection gas；The dewpoint humidity of the wet hydrogen is 15 ± 5 DEG C, beneficial to the sintering strength and the carbon of removal residual for improving mixture
Temperature in pollutant, the hydrogen furnace is 1840~1880 DEG C, and the sintered heat insulating time is 2~4 minutes.
In the step (3), milled in corundum mortar, grinding time is 120~180 minutes.
In the step (2), when the purpose of compacting is next step high temperature sintering, alumina powder and oxidation yttrium powder being capable of shapes
Into fine and close agglomerate；And dried mixture is put into molybdenum bowl and is compacted, it is due to the temperature range ratio that molybdenum bowl can be born
It is higher, when carrying out high temperature sintering, raw material will not be polluted.When being sintered using hydrogen furnace, wet hydrogen is passed through as protection
Gas, due to containing certain vapor in wet hydrogen, can make the sintering of mixed material blocking, beneficial to the sintering for improving mixture
Intensity and the carbon pollutant for removing residual, it is ensured that the insulating properties of filler.When carrying out high temperature sintering, temperature should be controlled 1840
~1880 DEG C, if temperature is higher than 1880 DEG C, crushing of milling is not easy after mixture fusing cooling；If temperature is less than 1840 DEG C,
Filament assembly sintering temperature can be very high in follow-up application for mixture, influences heated filament performance.
In the step (3), mill and carried out in corundum mortar, the hardness of corundum mortar is higher, when being milled not
Raw material can be polluted；Screen cloth of the mixture through 200~600 mesh after milling is sieved, between screening is obtained within this range
The epigranular of heated cathode heated filament insulating packing, obtains filament assembly in follow-up filling, cause is resulted in by high temperature sintering
Close insulating barrier, if undersized or excessive, the consistency of the insulating barrier obtained when applying in the later stage is bad.
The present invention by control alumina powder and oxidation yttrium powder between proportioning, with reference to grinding, drying, sinter, mill,
The control of sieving technology parameter, has prepared cathodes heated indirectly by an el heated filament insulating packing of good performance, using between the present invention
Cathodes heated indirectly by an el filament assembly prepared by heated cathode heated filament insulating packing is with using traditional single alumina powder insulating packing
The cathodes heated indirectly by an el filament assembly of preparation is compared, and possesses higher breakdown voltage resistant, filament assembly and the negative electrode temperature difference are smaller.
Embodiment
Alumina powder and oxidation yttrium powder can be from the market sale producer be directly commercially available, both particle diameters are 5
~7um, purity is 99.9%.
Embodiment 1
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing is by alumina powder and oxidation yttrium powder percentage by weight
Than 60%：40% composition.
The preparation method of the cathodes heated indirectly by an el heated filament insulating packing is：
(1) according to percentage by weight 60%：40% ratio is put into agate after weighing alumina powder and oxidation yttrium powder respectively
In tank, distilled water is measured with graduated cylinder and pours into agate pot, alumina powder and the ratio between oxidation yttrium powder gross weight and the volume of distilled water are
100g：100ml, is then placed in alumina powder and oxidation yttrium powder gross weight agate ball 1.5 times heavy carries out ball milling, and Ball-milling Time is
7.5 hours so that alumina powder and oxidation yttrium powder are thoroughly mixed in agate jar；Mixture in agate pot is poured into beaker,
Agate ball is taken out, then beaker is put into baking oven, the drying 10 hours of 110 DEG C of temperature is controlled so that alumina powder and oxidation
Yttrium powder compound is completely dried；
(2) it will be cooled to 20~35 DEG C of drying alumina powder with ox horn spoon and oxidation yttrium powder compound load in molybdenum bowl simultaneously
It is compacted with ox horn spoon；The molybdenum bowl that will be equipped with compound is put into hydrogen furnace 1860 DEG C and is sintered, and 4 minutes is incubated, in hydrogen furnace
Be passed through dewpoint humidity be 15 ± 5 DEG C wet hydrogen as protection gas so that compound is fully sintered blocking；
(3) the mixed material block after sintering is put into corundum mortar and milled, grinding time 180 minutes, until burning
Mixed material block after knot is milled into powdered completely；The powder mixture milled with the screen cloth screening of 200 mesh, you can obtain
Cathodes heated indirectly by an el heated filament insulating packing.
Embodiment 2
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing is by alumina powder and oxidation yttrium powder percentage by weight
Than 60%：40% composition.
The preparation method of the cathodes heated indirectly by an el heated filament insulating packing is：
(1) according to percentage by weight 50%：50% ratio is put into agate after weighing alumina powder and oxidation yttrium powder respectively
In, distilled water is measured with graduated cylinder and pours into agate pot, alumina powder and the ratio between oxidation yttrium powder gross weight and the volume of distilled water are
100g：100ml, is then placed in alumina powder and oxidation yttrium powder gross weight agate ball 1.5 times heavy carries out ball milling, and Ball-milling Time is
7.5 hours so that alumina powder and oxidation yttrium powder are thoroughly mixed in agate jar；Mixture in agate pot is poured into beaker,
Agate ball is taken out, then beaker is put into baking oven, the drying 10 hours of 90 DEG C of temperature is controlled so that alumina powder and yittrium oxide
Powder compound is completely dried；
(2) it will be cooled to 20~35 DEG C of drying alumina powder with ox horn spoon and oxidation yttrium powder compound load in molybdenum bowl simultaneously
It is compacted with ox horn spoon；The molybdenum bowl that will be equipped with compound is put into hydrogen furnace 1840 DEG C and is sintered, and 4 minutes is incubated, in hydrogen furnace
Be passed through dewpoint humidity be 15 ± 5 DEG C wet hydrogen as protection gas so that compound is fully sintered blocking；
(3) the mixed material block after sintering is put into corundum mortar and milled, grinding time 180 minutes, until burning
Mixed material block after knot is milled into powdered completely；The powder mixture milled with the screen cloth screening of 400 mesh, you can obtain
Cathodes heated indirectly by an el heated filament insulating packing.
Embodiment 3
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing is by alumina powder and oxidation yttrium powder percentage by weight
Than 70%：30% composition.
The preparation method of the cathodes heated indirectly by an el heated filament insulating packing is：
(1) according to percentage by weight 70%：30% ratio is put into agate after weighing alumina powder and oxidation yttrium powder respectively
In tank, distilled water is measured with graduated cylinder and pours into agate pot, alumina powder and the ratio between oxidation yttrium powder gross weight and the volume of distilled water are
100g：140ml, is then placed in alumina powder and oxidation yttrium powder gross weight agate ball 2 times heavy carries out ball milling, and Ball-milling Time is 5
Hour so that alumina powder and oxidation yttrium powder are thoroughly mixed in agate jar；Mixture in agate pot is poured into beaker, taken out
Beaker, is then put into baking oven by agate ball, controls the drying 8 hours of 100 DEG C of temperature so that alumina powder and oxidation yttrium powder are mixed
Material is closed to be completely dried；
(2) it will be cooled to 20~35 DEG C of drying alumina powder with ox horn spoon and oxidation yttrium powder compound load in molybdenum bowl simultaneously
It is compacted with ox horn spoon；The molybdenum bowl that will be equipped with compound is put into hydrogen furnace 1880 DEG C and is sintered, and 2 minutes is incubated, in hydrogen furnace
Be passed through dewpoint humidity be 15 ± 5 DEG C wet hydrogen as protection gas so that compound is fully sintered blocking；
(3) the mixed material block after sintering is put into corundum mortar and milled, grinding time 120 minutes, until burning
Mixed material block after knot is milled into powdered completely；The powder mixture milled with the screen cloth screening of 600 mesh, you can obtain
Cathodes heated indirectly by an el heated filament insulating packing.
Comparative example 1
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing is made up of alumina powder, the cathodes heated indirectly by an el
The preparation method be the same as Example 1 of heated filament insulating packing.
Comparative example 2
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing is made up of oxidation yttrium powder, the cathodes heated indirectly by an el
The preparation method be the same as Example 1 of heated filament insulating packing.
Cathodes heated indirectly by an el heated filament group made from the cathodes heated indirectly by an el heated filament insulating packing obtained as each embodiment and comparative example
The performance of part is as shown in table 1：
The performance parameter of each embodiment of table 1 and comparative example
As can be seen from the table, the indirect-heating as made from cathodes heated indirectly by an el heated filament insulating packing disclosed by the invention is cloudy
Pole filament assembly has higher breakdown voltage resistant and higher heat conduction efficiency.
The above-mentioned detailed description carried out with reference to embodiment to cathodes heated indirectly by an el heated filament insulating packing and preparation method thereof, is to say
It is bright property rather than limited, several embodiments can be included according to limited scope, therefore it is of the invention total not departing from
Changing and modifications under body design, should belong within protection scope of the present invention.
Claims (10)
1. a kind of cathodes heated indirectly by an el heated filament insulating packing, it is characterised in that the insulating packing is by alumina powder and oxidation yttrium powder
By weight percentage (50%~70%)：(30%~50%) constitute.
2. cathodes heated indirectly by an el heated filament insulating packing according to claim 1, it is characterised in that the alumina powder and oxidation
The particle diameter of yttrium powder is 5~7um.
3. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 1, it is characterised in that the preparation
Method comprises the following steps：
(1) it is the alumina powder and oxidation yttrium powder per distribution ratio addition distilled water progress mixing and ball milling 5~7.5 by weight is small
When, (alumina powder+oxidation yttrium powder)：Distilled water=100g：(100~150) mL, and the mixture after ball milling is dried；
(2) by dried mixture compacted, it is put into hydrogen furnace and is sintered；
(3) powder is milled into after mixture of the sintering after blocking is cooled down, 200~600 eye mesh screens is crossed and is sieved, you can obtained
Cathodes heated indirectly by an el heated filament insulating packing.
4. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 3, it is characterised in that the drying
Temperature is 90~110 DEG C, and the time is 8~10 hours.
5. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 3, it is characterised in that the step
(in 1), ball milling is carried out by the way of agate ball is added into agate pot, and the weight of the agate ball is alumina powder and oxidation
1.5~2 times of yttrium powder gross weight, a diameter of 10~25mm of agate ball.
6. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 3, it is characterised in that the step
(2) in, dried mixture is put into molybdenum bowl and is compacted.
7. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 3, it is characterised in that the hydrogen
Wet hydrogen is passed through in stove as protection gas.
8. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 7, it is characterised in that the wet hydrogen
The dewpoint humidity of gas is 15 ± 5 DEG C.
9. the preparation method of the cathodes heated indirectly by an el heated filament insulating packing according to claim 3 or 6-8 any one, its feature
It is, the temperature in the hydrogen furnace is 1840~1880 DEG C, the sintered heat insulating time is 2~4 minutes.
10. according to the preparation method of the cathodes heated indirectly by an el heated filament insulating packing described in claim 3, it is characterised in that the step
(3) in, milled in corundum mortar, grinding time is 120~180 minutes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112490098A (en) * | 2020-12-09 | 2021-03-12 | 成都国光电气股份有限公司 | Mixed filling powder for hot wire component and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112490098A (en) * | 2020-12-09 | 2021-03-12 | 成都国光电气股份有限公司 | Mixed filling powder for hot wire component and preparation method thereof |
| CN112490098B (en) * | 2020-12-09 | 2023-03-14 | 成都国光电气股份有限公司 | Mixed filling powder for hot wire component and preparation method thereof |
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| CN107331441B (en) | 2019-03-12 |
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