CN107331441B - 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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- CN107331441B CN107331441B CN201710576550.1A CN201710576550A CN107331441B CN 107331441 B CN107331441 B CN 107331441B CN 201710576550 A CN201710576550 A CN 201710576550A CN 107331441 B CN107331441 B CN 107331441B
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- H—ELECTRICITY
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- 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
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- 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
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- 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
- C04B2235/658—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 packings and preparation method thereof, by weight percentage (50%~70%) with alumina powder and oxidation yttrium powder: (30%~50%) is raw material, by ball milling, drying, be sintered, mill, sieve after obtain cathodes heated indirectly by an el heated filament insulating packing, the filament assembly filled using this cathodes heated indirectly by an el heated filament insulating packing, fine and close insulating layer can be obtained after high temperature sintering, which has the characteristics that good insulation preformance, breakdown voltage resistant height, heat conduction efficiency are high.
Description
Technical field
The invention belongs to vacuum microwave devices fields, and in particular to a kind of cathodes heated indirectly by an el heated filament insulating packing and its preparation
Method.
Background technique
Electron source in modern high power microwave device, what is generallyd use is hot cathode, and filament assembly is as hot cathode
Heat source, structure and performance are directly related to the performance of device, life and reliability.
As microwave device constantly develops, to hot cathode, more stringent requirements are proposed, i.e., big emission current ability and
Quick start ability, the rapidity that cathode wants quick start just to provide heated filament the uniformity and heat transfer that heat propose accordingly
Requirement, traditional heated filament due to structure limit and insulating packing heating conduction used it is bad, limit cathode quick start
Ability, especially this defect seems especially prominent on large scale cathode heater, is no longer satisfied microwave device to cathode
The demand of quick start.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of cathodes heated indirectly by an el heated filament insulating packing and its preparation sides
Method, using alumina powder and oxidation yttrium powder as raw material, by ball milling, drying, be sintered, mill, sieve after to obtain cathodes heated indirectly by an el hot
Silk insulation filler, the filament assembly filled using this cathodes heated indirectly by an el heated filament insulating packing, the energy after high temperature sintering
Fine and close insulating layer is obtained, which has the characteristics that good insulation preformance, breakdown voltage resistant height, heat conduction efficiency are high.
The technical scheme adopted by the invention is as follows:
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%) composition.
The alumina powder and the partial size of oxidation yttrium powder are 5~7um.
The present invention also provides 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 carry 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 dry；
(2) it by the mixture compacted after drying, is put into hydrogen furnace and is sintered；
(3) by be sintered it is blocking after mixture it is cooling after be milled into powder, cross 200~600 mesh screens and sieved
Obtain cathodes heated indirectly by an el heated filament insulating packing.
The step (in 1), the drying temperature are 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 carries out, and the weight of the agate ball is the 1.5~2 of alumina powder and oxidation yttrium powder total weight
Times, the diameter of agate ball is 10~25mm.
In the step (2), the mixture after drying is put into molybdenum bowl and is compacted；Wet hydrogen work is passed through in the hydrogen furnace
To protect gas；The dewpoint humidity of the wet hydrogen is 15 ± 5 DEG C, conducive to the sintering strength for improving mixture and removes remaining carbon
Pollutant, the temperature in the hydrogen furnace are 1840~1880 DEG C, and the sintered heat insulating time is 2~4 minutes.
It in the step (3), mills 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
At fine and close agglomerate；And the mixture after drying is put into molybdenum bowl and is compacted, it is the temperature range ratio that can be born due to molybdenum bowl
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 can make the sintering of mixed material blocking, due to containing certain vapor in wet hydrogen conducive to the sintering for improving mixture
Intensity and the remaining carbon pollutant of removal, guarantee the insulation performance of filler.When carrying out high temperature sintering, temperature should be controlled 1840
~1880 DEG C, if temperature is higher than 1880 DEG C, it is not easy crushing of milling after mixture fusing is cooling；If temperature is lower than 1840 DEG C,
Filament assembly sintering temperature can be very high in subsequent application for mixture, influences heated filament performance.
In the step (3), mills and carried out in corundum mortar, the hardness of corundum mortar is higher, not when being milled
Raw material can be polluted；Mixture after milling is sieved through the sieve of 200~600 mesh, between screening obtains within this range
The epigranular of heated cathode heated filament insulating packing obtains filament assembly in subsequent filling, can be caused by high temperature sintering
Close insulating layer, if undersized or excessive, in later period application, the consistency of insulating layer obtained is bad.
The present invention is by control alumina powder and aoxidizes the proportion between yttrium powder, in conjunction with to grinding, drying, be sintered, mill,
Cathodes heated indirectly by an el heated filament insulating packing of good performance has been prepared, between of the invention in the control of sieving technology parameter
Cathodes heated indirectly by an el filament assembly and use traditional single alumina powder insulating packing prepared by heated cathode heated filament insulating packing
The cathodes heated indirectly by an el filament assembly of preparation is compared, and has higher breakdown voltage resistant, and filament assembly and the cathode temperature difference are smaller.
Specific embodiment
Alumina powder and oxidation yttrium powder can sale producer from the market be directly commercially available, the partial size of the two is 5
~7um, purity 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
It is formed than 60%:40%.
The cathodes heated indirectly by an el heated filament insulating packing the preparation method comprises the following steps:
(1) agate is put into after weighing alumina powder and oxidation yttrium powder respectively according to the ratio of weight percent 60%:40%
In tank, distilled water is measured with graduated cylinder and pours into agate pot, alumina powder and oxidation the ratio between yttrium powder total weight and the volume of distilled water are
100g:100ml, the agate ball for being then placed in 1.5 times of yttrium powder total weight heavy of alumina powder and oxidation carry 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 mixture 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 mixture be packed into molybdenum bowl simultaneously
It is compacted with ox horn spoon；Molybdenum bowl equipped with mixture is put into hydrogen furnace and is sintered for 1860 DEG C, 4 minutes are kept the temperature, in hydrogen furnace
It is passed through the wet hydrogen that dewpoint humidity is 15 ± 5 DEG C and is used as protection gas, so that mixture is fully sintered blocking；
(3) sintered mixed material block is put into corundum mortar and is milled, grinding time 180 minutes, until burning
Mixed material block after knot is milled into powdered completely；The powder mixture milled is screened with the sieve of 200 mesh, can be obtained
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
It is formed than 60%:40%.
The cathodes heated indirectly by an el heated filament insulating packing the preparation method comprises the following steps:
(1) agate is put into after weighing alumina powder and oxidation yttrium powder respectively according to the ratio of weight percent 50%:50%
In, distilled water is measured with graduated cylinder and pours into agate pot, and alumina powder and oxidation the ratio between yttrium powder total weight and the volume of distilled water are
100g:100ml, the agate ball for being then placed in 1.5 times of yttrium powder total weight heavy of alumina powder and oxidation carry 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 yttrium oxide
Powder mixture 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 mixture be packed into molybdenum bowl simultaneously
It is compacted with ox horn spoon；Molybdenum bowl equipped with mixture is put into hydrogen furnace and is sintered for 1840 DEG C, 4 minutes are kept the temperature, in hydrogen furnace
It is passed through the wet hydrogen that dewpoint humidity is 15 ± 5 DEG C and is used as protection gas, so that mixture is fully sintered blocking；
(3) sintered mixed material block is put into corundum mortar and is milled, grinding time 180 minutes, until burning
Mixed material block after knot is milled into powdered completely；The powder mixture milled is screened with the sieve of 400 mesh, can be obtained
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
It is formed than 70%:30%.
The cathodes heated indirectly by an el heated filament insulating packing the preparation method comprises the following steps:
(1) agate is put into after weighing alumina powder and oxidation yttrium powder respectively according to the ratio of weight percent 70%:30%
In tank, distilled water is measured with graduated cylinder and pours into agate pot, alumina powder and oxidation the ratio between yttrium powder total weight and the volume of distilled water are
100g:140ml, the agate ball for being then placed in 2 times of yttrium powder total weight heavy of alumina powder and oxidation carry out ball milling, Ball-milling Time 5
Hour, so that alumina powder and oxidation yttrium powder are thoroughly mixed in agate jar；Mixture in agate pot is poured into beaker, is taken out
Then beaker is put into baking oven by agate ball, control 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 mixture be packed into molybdenum bowl simultaneously
It is compacted with ox horn spoon；Molybdenum bowl equipped with mixture is put into hydrogen furnace and is sintered for 1880 DEG C, 2 minutes are kept the temperature, in hydrogen furnace
It is passed through the wet hydrogen that dewpoint humidity is 15 ± 5 DEG C and is used as protection gas, so that mixture is fully sintered blocking；
(3) sintered mixed material block is put into corundum mortar and is milled, grinding time 120 minutes, until burning
Mixed material block after knot is milled into powdered completely；The powder mixture milled is screened with the sieve of 600 mesh, can be obtained
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 are made of alumina powder, the cathodes heated indirectly by an el
The preparation method is the same as that of Example 1 for heated filament insulating packing.
Comparative example 2
A kind of cathodes heated indirectly by an el heated filament insulating packing, the insulating packing are made of oxidation yttrium powder, the cathodes heated indirectly by an el
The preparation method is the same as that of Example 1 for 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 table 1 each embodiment and comparative example
As can be seen from the table, the yin of the indirect-heating as made from cathodes heated indirectly by an el heated filament insulating packing disclosed by the invention
The with higher breakdown voltage resistant and higher heat conduction efficiency of pole filament assembly.
The above-mentioned detailed description carried out referring to embodiment to cathodes heated indirectly by an el heated filament insulating packing and preparation method thereof, is to say
Bright property without being restrictive, several embodiments can be enumerated according to limited range, therefore of the invention total not departing from
Change and modification under body design, should belong within protection scope of the present invention.
Claims (9)
1. a kind of preparation method of cathodes heated indirectly by an el heated filament insulating packing, which is characterized in that the insulating packing is by alumina powder
By weight percentage (50% ~ 70%) with oxidation yttrium powder: (30% ~ 50%) composition；
The preparation method of the cathodes heated indirectly by an el heated filament insulating packing the following steps are included:
(1) alumina powder and oxidation yttrium powder per distribution ratio by weight are added distilled water and carried out mixing and ball milling 5 ~ 7.5 hours,
(alumina powder+oxidation yttrium powder): distilled water=100g:(100 ~ 150) mL, and the mixture after ball milling is dry；
(2) it by the mixture compacted after drying, is put into hydrogen furnace and is sintered；
(3) by be sintered it is blocking after mixture it is cooling after be milled into powder, cross 200 ~ 600 mesh screens and sieved, be can be obtained
Cathodes heated indirectly by an el heated filament insulating packing.
2. preparation method according to claim 1, which is characterized in that the alumina powder and the partial size of oxidation yttrium powder are
5~7um。
3. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 1, which is characterized in that the drying
Temperature is 90 ~ 110 DEG C, and the time is 8 ~ 10 hours.
4. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 1, which is characterized in that the step
(1) in, 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 oxygen
1.5 ~ 2 times for changing yttrium powder total weight, the diameter of agate ball are 10 ~ 25mm.
5. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 1, which is characterized in that the step
(2) in, the mixture after drying is put into molybdenum bowl and is compacted.
6. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 1, which is characterized in that the hydrogen
Wet hydrogen is passed through in furnace as protection gas.
7. the preparation method of cathodes heated indirectly by an el heated filament insulating packing according to claim 6, which is characterized in that the wet hydrogen
The dewpoint humidity of gas is 15 ± 5 DEG C.
8. according to claim 1 or the preparation method of cathodes heated indirectly by an el heated filament insulating packing described in 5-7 any one, feature
It is, the temperature in the hydrogen furnace is 1840 ~ 1880 DEG C, and the sintered heat insulating time is 2 ~ 4 minutes.
9. according to the preparation method of cathodes heated indirectly by an el heated filament insulating packing described in claim 1, which is characterized in that the step
(3) it in, mills in corundum mortar, grinding time is 120 ~ 180 minutes.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576258A (en) * | 2003-07-23 | 2005-02-09 | Ge医疗***环球技术有限公司 | Preparation of rare earth ceramic garnet |
| CN1827264A (en) * | 2006-03-24 | 2006-09-06 | 自贡市天恒合金应用技术有限公司 | Method for preparing composite raw powder for the production of ultrafine hard alloy |
| CN203746784U (en) * | 2013-12-16 | 2014-07-30 | 安徽华东光电技术研究所 | Helix travelling wave tube cathode structure |
| CN105585313A (en) * | 2016-01-14 | 2016-05-18 | 深圳市商德先进陶瓷有限公司 | Alumina ceramic powder, alumina ceramic and preparation method of alumina ceramic |
| CN105931932A (en) * | 2016-04-26 | 2016-09-07 | 北京科技大学 | Preparation method of aluminum nitride insulation layer cathode hot wire |
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2017
- 2017-07-14 CN CN201710576550.1A patent/CN107331441B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1576258A (en) * | 2003-07-23 | 2005-02-09 | Ge医疗***环球技术有限公司 | Preparation of rare earth ceramic garnet |
| CN1827264A (en) * | 2006-03-24 | 2006-09-06 | 自贡市天恒合金应用技术有限公司 | Method for preparing composite raw powder for the production of ultrafine hard alloy |
| CN203746784U (en) * | 2013-12-16 | 2014-07-30 | 安徽华东光电技术研究所 | Helix travelling wave tube cathode structure |
| CN105585313A (en) * | 2016-01-14 | 2016-05-18 | 深圳市商德先进陶瓷有限公司 | Alumina ceramic powder, alumina ceramic and preparation method of alumina ceramic |
| CN105931932A (en) * | 2016-04-26 | 2016-09-07 | 北京科技大学 | Preparation method of aluminum nitride insulation layer cathode hot wire |
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