CN108878234A - A kind of ZrH2The Y of addition2O3The preparation method of-W base secondary emitters - Google Patents
A kind of ZrH2The Y of addition2O3The preparation method of-W base secondary emitters Download PDFInfo
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- CN108878234A CN108878234A CN201810615636.5A CN201810615636A CN108878234A CN 108878234 A CN108878234 A CN 108878234A CN 201810615636 A CN201810615636 A CN 201810615636A CN 108878234 A CN108878234 A CN 108878234A
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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
- H01J9/042—Manufacture, activation of the emissive part
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/13—Solid thermionic cathodes
- H01J1/14—Solid thermionic cathodes characterised by the material
- H01J1/144—Solid thermionic cathodes characterised by the material with other metal oxides as an emissive material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
- H01J1/02—Main electrodes
- H01J1/13—Solid thermionic cathodes
- H01J1/14—Solid thermionic cathodes characterised by the material
- H01J1/146—Solid thermionic cathodes characterised by the material with metals or alloys as an emissive material
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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
- H01J9/042—Manufacture, activation of the emissive part
- H01J9/045—Activation of assembled cathode
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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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Abstract
A kind of ZrH2The Y of addition2O3The preparation method of-W base secondary emitters, belongs to the preparation technical field of cathode material.With the Y being prepared2O3Based on the tungsten powder of Uniform Doped and 411 aluminates, prepare containing activator ZrH2The immersion-type Rare-Earth Tungsten base secondary cathode of addition, and its emission properties and secondary emission performance are tested.It was found that there is activator ZrH2The emission properties and secondary emission performance of the Rare-Earth Tungsten base secondary cathode of addition are the most excellent, its zero-field emission current density is no ZrH23.1-3.4 times for adding Rare-Earth Tungsten base secondary cathode, its maximum secondary emission ratio is no ZrH21.2 times for adding Rare-Earth Tungsten base secondary cathode.Activator ZrH is prepared using the method2The Y of addition2O3- W base secondary emitters have excellent emission properties and secondary emission performance, are expected to apply in high power magnetron.
Description
Technical field
A kind of ZrH2The Y of addition2O3The preparation method of-W base secondary emitters belongs to electron emitting cathode material preparation skill
Art field.
Background technique
Direction with magnetron towards high-output power is developed, anticathode emitting performance, resistance to electronic and ionic bombardment property
More stringent requirements are proposed for energy and service life.Though oxide-coated cathode emitting performance with higher, its resistance to bombardment performance
It is poor, it is easy sparking under high working voltage, oxide layer is caused to fall off.It is widely used in high power CW wave magnetron
ThO2- W has biggish heat emission, secondary emission performance and longer working life, but since Th has radioactivity, should not be again
It uses.Though alloy cathode has preferable secondary emission performance, most of preparation costs are costly, it is difficult to large-scale promotion
It uses.At present in the widely used barium-tungsten dispense cathode of magnetron, though there is preferable thermoelectron and secondary electron emissions performance, it is big
Under power continuous wave magnetron working environment, it will receive violent electronic and ionic and return Hong effect, so that cathode surface temperature is excessively high,
Quickly so as to cause BaO consumption, the service life is shorter.The rare earth of early-stage study-molybdenum ceramic cathode, secondary performance are excellent
It is different, have certain resistance to bombardment ability, launch stability is preferable, but the cathode emission properties are poor, lead to magnetron starting of oscillation
It is difficult.The working principle of high power magnetron determines that the large-scale application of above-mentioned cathode material has certain limitation.Therefore,
Require further study novel cathode material, it is desirable that it is with preferable hot-electron emission property, higher secondary electron emissions
Energy and resistance to bombardment characteristic, to meet high-power and millimeter wave magnetron further development.
Summary of the invention
A kind of ZrH2The Y of addition2O3The preparation method of-W base secondary emitters, using the method for mechanical mixture by ZrH2With
Aluminate is mixed, the cathode base that then dipping is obtained with Yttrium oxide doping tungsten powder institute compacting sintering, dipping after again into
ZrH has been obtained after row washing annealing2The Y of addition2O3- W base secondary emitters.
A kind of ZrH provided by the invention2The Y of addition2O3The preparation method of-W base secondary emitters, which is characterized in that preparation
Process includes the following steps：
A. ammonium metatungstate [(NH is selected4)6(H2W12O40)4H2O] (AMT) be the source W, yttrium nitrate (Y (NO3)3·4H2It O) is the source Y
It is dissolved in deionized water respectively, then two kinds of solution is mixed, are stirred evenly；By spray dryer by AMT and Y (NO3)3It is mixed
It closes solution and is prepared into uniformly mixed Precursor Powder；
B. the resulting Precursor Powder of step A is put into Muffle furnace and is calcined, the product obtained after calcining carries out again
It grinds and sieves；
C. the obtained Precursor Powder of step B is placed in hydrogen reducing furnace and carries out hydrogen reducing, obtained yttrium oxide and mix
Miscellaneous tungsten powder；
D. the tungsten powder of the resulting Yttrium oxide doping of step C is fitted into mold, applies certain Bidirectional pressure by hydraulic press
Simultaneously pressure maintaining for a period of time, obtains cathode green body to power, this cathode green body has certain porosity and mechanical strength；
E. the resulting cathode green body of step D is placed in tungsten net hydrogen furnace to be sintered, sintering process includes low temperature presintering
With two stages of high temperature sintering；
F. by 411 aluminate ZrH2Ball mill progress mechanical mixture is reinstated as salt activator agent one is mixed with dipping, mixing is equal
Vacuum saves stand-by after even；
G. will be in step E resulting cathode base embedment obtained the hybrids infusion salt activator agent of step F 411 salt+
ZrH2, it is placed in molybdenum boat, then puts it into tungsten net hydrogen furnace and be sintered dipping process in a hydrogen atmosphere；
H. the resulting cathode of step G is put into water deionized water, is cleaned in ultrasonic washing instrument, cleaning process
In constantly observe cathode surface, until do not observe under the microscope active salt there are until；It is de- that cathode is impregnated with alcohol again
Water is then placed in drying box and dries, and anneals again after taking-up；Activator ZrH is finally obtained2The Y of addition2O3- W base
Grade emitter.
In above method step A, the purity of selected ammonium metatungstate is 99.9%, and the amount containing Y is that 10-20wt% is (excellent
Select 15wt%).It is preferably atomizing pressure 10kp that spray dryer technological parameter, which is arranged,a, outlet temperature is 92-96 DEG C, air blast speed
Rate is 0.5m3/ min, feed rate 400ml/h.
In above method step B, the calcination temperature is 650 DEG C ± 50 DEG C, keeps the temperature 150min ± 10min.
In above method step C, reduction process is to carry out in a hydrogen atmosphere, in 550 DEG C of ± 50 DEG C of heat preservation 120min-
150min, 1150 DEG C of -1180 DEG C of heat preservation 150min-180min.
In above method step D, weighs powder prepared by 0.12-0.13g and be fitted into mold, applied by hydraulic press
The bidirection press and pressure maintaining 30s of 0.75Mpa.
In above method step E, the sintering process low temperature sintering technique keeps the temperature 20min when being 850 DEG C ± 50 DEG C,
20min is kept the temperature at 1100 DEG C ± 100 DEG C, high-sintering process is 1450-1550 DEG C, preferably 1520 DEG C, keeps the temperature 20min.
In above method step F, the mechanical mixture process is by 411 aluminates and ZrH2Machinery is carried out with ball mill
Mixing, preferably ZrH2Mass percentage is 6-19%, and preferably ratio of grinding media to material is 6:1, Ball-milling Time 4h.
In above method step G, the dipping process is first gradually to be warming up to 1450-1550 DEG C preferably 1520 DEG C, so
It is warming up to 1675 DEG C in 1-2min afterwards, after keeping the temperature 1.2min, 1500 DEG C is cooled in 1 minute, it then gradually will be to taking after room temperature
Out.
In above method H, the annealing process is 1050 DEG C, keeps the temperature 30min.
Compared with prior art, the beneficial effects of the invention are as follows：
1. pair having ZrH2The Y of addition2O3- W base secondary emitters and without ZrH2The Y of addition2O3The heat of-W base secondary emitters
Electron emission capability is tested, and discovery has ZrH2The Y of addition2O3The hot-electron emission property of-W base secondary emitters is the most
It is excellent, at 1050 DEG Cb, 1100 DEG CbWith 1150 DEG CbLocating zero field current density is respectively 3.73A/cm2, 5.27A/cm2And 7.25A/
cm2, it is no ZrH2The Y of addition2O33.1-3.4 times of the heat emission current density of-W base secondary emitters, in the activated aluminum of dipping
ZrH is added in hydrochlorate2It can larger raising Y2O3The hot-electron emission property of-W base secondary cathode.
2. pair having ZrH2The Y of addition2O3- W base secondary emitters and without ZrH2The Y of addition2O3Time of-W base secondary emitters
Grade electron emission capability is tested, and discovery has ZrH2The Y of addition2O3The hot-electron emission property of-W base secondary emitters is most
To be excellent, its maximum secondary emission ratio is no ZrH2The Y of addition2O31.2 times of-W base secondary emitters, in the work of dipping
ZrH is added in property aluminate2It can larger raising Y2O3The secondary emission performance of-W base secondary cathode.
Detailed description of the invention
The present invention has 4 attached drawings, is now respectively described below：
The SEM figure and energy spectrum analysis (a) matrix surface (b) matrix section of Fig. 1 sample after sintering
Fig. 2 cathode surface SEM schemes the cathode that (a) has activator to add without the cathode (b) that activator adds
The made cathode of Fig. 3 embodiment 1 is at 1200 DEG CbPulse Voltammetry characteristic curve after activation
The made cathode of Fig. 4 embodiment 2 is at 1200 DEG CbPulse Voltammetry characteristic curve after activation
The made cathode of Fig. 5 embodiment 3 is at 1200 DEG CbPulse Voltammetry characteristic curve after activation
δ-EP the curve of Fig. 6 difference cathode
Specific embodiment
Below with reference to embodiment, the invention will be further described, but the present invention is not limited to following embodiments.
Embodiment 1
(1) ammonium metatungstate [(NH soluble easily in water is selected4)6(H2W12O40)4H2O] (99.9%pure), (AMT) is the source W,
Yttrium nitrate (Y (NO3)3·4H2O it) is dissolved in deionized water respectively for the source Y, then two kinds of solution is mixed, are stirred evenly.Sample
In the amount containing Y be 15wt%.Setting Eyela SD-1000 type spray dryer technological parameter is atomizing pressure 10kpa, outlet temperature
Degree is 92-96 DEG C, blast rate 0.5m3/ min, feed rate 400ml/h pass through spray dryer for AMT and Y in this way
(NO3)3Mixed solution is prepared into uniformly mixed Precursor Powder.The Precursor Powder formed is collected, puts it into Muffle furnace and carries out
Calcining, calcination temperature are 650 DEG C, keep the temperature 150min, and the product obtained after calcining is ground and sieved again, are then collected true
Sky saves pending hydrogen reducing.Hydrogen reducing test is carried out in hydrogen reducing furnace, and powder is contained in homemade molybdenum boat,
Reducing process parameter is that heating rate is 10 DEG C/min, keeps the temperature 120 minutes at 550 DEG C of temperature, then heats to 1150 DEG C, is protected
Warm 150min, then furnace cooling.
(1) the tungsten powder about 0.12-0.13g that rare-earth oxidation doped yttrium is prepared is weighed, loading cavity body of mould diameter is 3mm
Mold in, 0.75Pa bidirection press and pressure maintaining 30s are applied by hydraulic press, obtain having certain porosity and mechanical strength
Cathode green body.
(2) the cathode green body suppressed placement L7520IIA type tungsten net hydrogen furnace is sintered in a hydrogen atmosphere, is burnt
The technological parameter of knot keeps the temperature 20min when being 850 DEG C；20min is kept the temperature at 1100 DEG C, 1520 DEG C, keeps the temperature 20min, it is then cold with furnace
But, cathode base is obtained.
(3) by the ZrH of 411 aluminates and 18.75% weight ratio2Progress mechanical mixture, mixed dipping salt, then
It is sintered obtained cathode base to be embedded in mixed dipping salt, be placed in L7520IIA type tungsten net hydrogen furnace in hydrogen gas
High temperature dipping is carried out under atmosphere, the technological parameter of setting is to be to slowly warm up to 1520 DEG C, is then rapidly heated to 1675 DEG C, keeps the temperature
After 1.2min, fast cooling, then gradually will be to taking out after room temperature to 1500 DEG C.
(4) cathode obtained after dipping is put into water deionized water, is cleaned in ultrasonic washing instrument, cleaned
In the process constantly observation cathode surface, until do not observe under the microscope active salt there are until.Yin is impregnated with alcohol again
Pole dehydration, is then placed in drying box and dries in 80 DEG C, anneal again after taking-up.Annealing process is 1050 DEG C, heat preservation
30min is prepared to have obtained activator ZrH2The Y of addition2O3- W base secondary emitters.
Comparative example 2
(1) spray drying process is used, ammonium metatungstate [(NH soluble easily in water is selected4)6(H2W12O40)4H2O] (99.9%
Pure), (AMT) is the source W, yttrium nitrate (Y (NO3)3·4H2O it) is dissolved in deionized water for the source Y, then mixes two kinds of solution respectively
It closes, stirs evenly.Amount in sample containing Y is 15wt%.It is atomization that Eyela SD-1000 type spray dryer technological parameter, which is arranged,
Pressure 10kpa, outlet temperature is 92-96 DEG C, blast rate 0.5m3/ min, feed rate 400ml/h, in this way by spraying
Drier is by AMT and Y (NO3)3Mixed solution is prepared into uniformly mixed Precursor Powder.The Precursor Powder formed is collected, is put
Enter in Muffle furnace and calcined, calcination temperature be 650 DEG C, keep the temperature 150min, calcining after obtain product carry out again grinding and
Then sieving collects vacuum and saves pending hydrogen reducing.Hydrogen reducing test is carried out in hydrogen reducing furnace, and powder is held
In homemade molybdenum boat, reducing process parameter is that heating rate is 10 DEG C/min, keeps the temperature 120 minutes at 550 DEG C of temperature, then
1150 DEG C are warming up to, 150min, then furnace cooling are kept the temperature.
(2) the tungsten powder about 0.12-0.13g that rare-earth oxidation doped yttrium is prepared is weighed, loading cavity body of mould diameter is 3mm
Mold in, 0.75MPa bidirection press and pressure maintaining 30s are applied by hydraulic press, obtain that there is certain porosity and mechanical strength
Cathode green body.
(3) the cathode green body suppressed placement L7520IIA type tungsten net hydrogen furnace is sintered in a hydrogen atmosphere, is burnt
20 minutes are kept the temperature when the technological parameter of knot is 850 DEG C；20min is kept the temperature at 1100 DEG C, 1520 DEG C, 20 minutes is kept the temperature, then with furnace
It is cooling, obtain cathode base.
(4) cathode base for obtaining sintering is embedded in 411 aluminates, is then placed within L7520IIA type tungsten net hydrogen furnace
In carry out high temperature dipping in a hydrogen atmosphere, the technological parameter of setting is to be to slowly warm up to 1520 DEG C, be then rapidly heated to
1675 DEG C, after keeping the temperature 1.2min, fast cooling, then gradually will be to taking out after room temperature to 1500 DEG C.
(5) cathode obtained after dipping is put into water deionized water, is cleaned in ultrasonic washing instrument, cleaned
In the process constantly observation cathode surface, until do not observe under the microscope active salt there are until.Yin is impregnated with alcohol again
Pole dehydration, is then placed in drying box and dries in 80 DEG C, anneal again after taking-up.Annealing process is 1050 DEG C, heat preservation
30min is prepared to obtain no activator ZrH2The Y of addition2O3- W base secondary emitters.
Comparative example 3
(1) ammonium metatungstate [(NH soluble easily in water is selected4)6(H2W12O40)4H2O] (99.9%pure), (AMT) is the source W,
Yttrium nitrate (Y (NO3)3·4H2O it) is dissolved in deionized water respectively for the source Y, then two kinds of solution is mixed, are stirred evenly.Sample
In the amount containing Y be 15wt%.Setting Eyela SD-1000 type spray dryer technological parameter is atomizing pressure 10kpa, outlet temperature
Degree is 92-96 DEG C, blast rate 0.5m3/ min, feed rate 400ml/h pass through spray dryer for AMT and Y in this way
(NO3)3Mixed solution is prepared into uniformly mixed Precursor Powder.The Precursor Powder formed is collected, puts it into Muffle furnace and carries out
Calcining, calcination temperature are 650 DEG C, keep the temperature 150min, and the product obtained after calcining is ground and sieved again, are then collected true
Sky saves pending hydrogen reducing.Hydrogen reducing test is carried out in hydrogen reducing furnace, and powder is contained in homemade molybdenum boat,
Reducing process parameter is that heating rate is 10 DEG C/min, keeps the temperature 120 minutes at 550 DEG C of temperature, then heats to 1150 DEG C, is protected
Warm 150min, then furnace cooling.
(2) the tungsten powder about 0.12-0.13g that rare-earth oxidation doped yttrium is prepared is weighed, loading cavity body of mould diameter is 3mm
Mold in, 0.75Pa bidirection press and pressure maintaining 30s are applied by hydraulic press, obtain having certain porosity and mechanical strength
Cathode green body.
(3) the cathode green body suppressed placement L7520IIA type tungsten net hydrogen furnace is sintered in a hydrogen atmosphere, is burnt
The technological parameter of knot keeps the temperature 20min when being 850 DEG C；20min is kept the temperature at 1100 DEG C, 1520 DEG C, keeps the temperature 20min, it is then cold with furnace
But, cathode base is obtained.
(4) by the ZrH of 411 aluminates and 6.25% weight ratio2Progress mechanical mixture, mixed dipping salt, then
It is sintered obtained cathode base to be embedded in mixed dipping salt, be placed in L7520IIA type tungsten net hydrogen furnace in hydrogen gas
High temperature dipping is carried out under atmosphere, the technological parameter of setting is to be to slowly warm up to 1520 DEG C, is then rapidly heated to 1675 DEG C, keeps the temperature
After 1.2min, fast cooling, then gradually will be to taking out after room temperature to 1500 DEG C.
(5) cathode obtained after dipping is put into water deionized water, is cleaned in ultrasonic washing instrument, cleaned
In the process constantly observation cathode surface, until do not observe under the microscope active salt there are until.Yin is impregnated with alcohol again
Pole dehydration, is then placed in drying box and dries in 80 DEG C, anneal again after taking-up.Annealing process is 1050 DEG C, heat preservation
30min is prepared to have obtained activator ZrH2The Y of addition2O3- W base secondary emitters.
The foregoing is merely main scheme for implementing said method of the invention, however the present invention is not limited to this, all not depart from this
Any modification, equivalent replacement or improvement for being made in the case where invention core etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of ZrH2The Y of addition2O3The preparation method of-W base secondary emitters, which is characterized in that preparation process includes following step
Suddenly：
A. ammonium metatungstate [(NH is selected4)6(H2W12O40)4H2O] (AMT) be the source W, yttrium nitrate (Y (NO3)3·4H2O) distinguish for the source Y
It is dissolved in deionized water, then two kinds of solution is mixed, are stirred evenly；By spray dryer by AMT and Y (NO3)3It mixes molten
Liquid is prepared into uniformly mixed Precursor Powder；
B. the resulting Precursor Powder of step A is put into Muffle furnace and is calcined, the product obtained after calcining is ground again
And sieving；
C. the obtained Precursor Powder of step B is placed in hydrogen reducing furnace and carries out hydrogen reducing, obtain Yttrium oxide doping
Tungsten powder；
D. the tungsten powder of the resulting Yttrium oxide doping of step C is fitted into mold, certain bidirection press is applied simultaneously by hydraulic press
Pressure maintaining for a period of time, obtains cathode green body, this cathode green body has certain porosity and mechanical strength；
E. the resulting cathode green body of step D is placed in tungsten net hydrogen furnace to be sintered, sintering process includes low temperature presintering and height
Temperature two stages of sintering；
F. by 411 aluminates, ZrH2Ball mill progress mechanical mixture is reinstated as salt activator agent one is mixed with dipping, after mixing
Vacuum saves stand-by；
G. by i.e. 411 salt+ZrH in the resulting cathode base embedment obtained hybrid infusion salt activator agent of step F of step E2, set
In molybdenum boat, then puts it into tungsten net hydrogen furnace and be sintered dipping process in a hydrogen atmosphere；
H. the resulting cathode of step G is put into water deionized water, is cleaned in ultrasonic washing instrument, in cleaning process not
Disconnected observation cathode surface, until do not observe under the microscope active salt there are until；Cathode dehydration is impregnated with alcohol again, so
After be put into drying box and dry, anneal again after taking-up；Activator ZrH is finally obtained2The Y of addition2O3- W base secondary emission
Body.
2. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In,
In step A, the purity of selected ammonium metatungstate is 99.9%, and the amount containing Y is 10-20wt%, preferably 15wt%.
3. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In in above method step B, the calcination temperature is 650 DEG C ± 50 DEG C, keeps the temperature 150min ± 10min.
4. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In, in above method step C, reduction process is to carry out in a hydrogen atmosphere, in 550 DEG C of ± 50 DEG C of heat preservation 120min-150min,
1150 DEG C of -1180 DEG C of heat preservation 150min-180min.
5. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In in above method step D, powder prepared by weighing 0.12-0.13g is fitted into mold, applies 0.75Mpa by hydraulic press
Bidirection press and pressure maintaining 30s.
6. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In, in above method step E, the sintering process low temperature sintering technique keeps the temperature 20min when being 850 DEG C ± 50 DEG C, and 1100
20min is kept the temperature at DEG C ± 100 DEG C, high-sintering process is 1450-1550 DEG C, preferably 1520 DEG C, keeps the temperature 20min.
7. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In in above method step F, the mechanical mixture process is by 411 aluminates and ZrH2Mechanical mixture is carried out with ball mill,
It is preferred that ZrH2Mass percentage is 6-19%, and preferably ratio of grinding media to material is 6:1, Ball-milling Time 4h.
8. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In in above method step G, the dipping process is first gradually to be warming up to 1450-1550 DEG C preferably 1520 DEG C, then 1-
It is warming up to 1675 DEG C in 2min, after keeping the temperature 1.2min, 1500 DEG C is cooled in 1 minute, it then gradually will be to taking out after room temperature.
9. a kind of ZrH described in accordance with the claim 12The Y of addition2O3The preparation method of-W base secondary emitters, feature exist
In in above method H, the annealing process is 1050 DEG C, keeps the temperature 30min.
10. according to the described in any item methods of claim 1-9, the ZrH being prepared2The Y of addition2O3- W base secondary emitters.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860000A (en) * | 2019-04-02 | 2019-06-07 | 戴连孚 | A kind of atom lamel cathode preparation method |
| RU2759154C1 (en) * | 2021-01-11 | 2021-11-09 | Акционерное общество "НПО "НИИТАЛ" | Emission material based on yttrium and lanthanum aluminates for metal-porous cathodes of high-power vacuum electronic equipment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2350364A1 (en) * | 1973-10-08 | 1975-04-24 | Interatom | Oxygen-ion conducting ceramics metallisation - by reductive sintering and thermal decompsn. of thorium, yttrium or zirconium hydride |
| CN101221869A (en) * | 2007-11-28 | 2008-07-16 | 南京工业大学 | High current density electron emitter material containing zirconium tungsten base and preparation method thereof |
| CN103526096A (en) * | 2013-10-25 | 2014-01-22 | 中国科学院合肥物质科学研究院 | Tungsten, zirconium and yttrium oxide alloy and preparation method thereof |
| CN103740994A (en) * | 2014-02-10 | 2014-04-23 | 中国科学院合肥物质科学研究院 | Nanostructure tungsten alloy and preparation method thereof |
-
2018
- 2018-06-14 CN CN201810615636.5A patent/CN108878234B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2350364A1 (en) * | 1973-10-08 | 1975-04-24 | Interatom | Oxygen-ion conducting ceramics metallisation - by reductive sintering and thermal decompsn. of thorium, yttrium or zirconium hydride |
| CN101221869A (en) * | 2007-11-28 | 2008-07-16 | 南京工业大学 | High current density electron emitter material containing zirconium tungsten base and preparation method thereof |
| CN103526096A (en) * | 2013-10-25 | 2014-01-22 | 中国科学院合肥物质科学研究院 | Tungsten, zirconium and yttrium oxide alloy and preparation method thereof |
| CN103740994A (en) * | 2014-02-10 | 2014-04-23 | 中国科学院合肥物质科学研究院 | Nanostructure tungsten alloy and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109860000A (en) * | 2019-04-02 | 2019-06-07 | 戴连孚 | A kind of atom lamel cathode preparation method |
| RU2759154C1 (en) * | 2021-01-11 | 2021-11-09 | Акционерное общество "НПО "НИИТАЛ" | Emission material based on yttrium and lanthanum aluminates for metal-porous cathodes of high-power vacuum electronic equipment |
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