CN109065422A - A kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode - Google Patents

A kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode Download PDF

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CN109065422A
CN109065422A CN201810710971.3A CN201810710971A CN109065422A CN 109065422 A CN109065422 A CN 109065422A CN 201810710971 A CN201810710971 A CN 201810710971A CN 109065422 A CN109065422 A CN 109065422A
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tungsten
rhenium alloy
directly
cathode
heated type
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CN109065422B (en
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漆世锴
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Jiujiang University
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Jiujiang University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus 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
    • H01J9/02Manufacture of electrodes or electrode systems
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J23/00Details of transit-time tubes of the types covered by group H01J25/00
    • H01J23/02Electrodes; Magnetic control means; Screens
    • H01J23/04Cathodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2209/00Apparatus and processes for manufacture of discharge tubes
    • H01J2209/02Manufacture of cathodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2223/00Details of transit-time tubes of the types covered by group H01J2225/00
    • H01J2223/02Electrodes; Magnetic control means; Screens
    • H01J2223/04Cathodes

Abstract

A kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode, this method step includes: to mix metal tungsten powder and rhenium powder, the tungsten-rhenium alloy powder being uniformly mixed;The tungsten-rhenium alloy powder is uniformly mixed with 1.5~3wt% cotton solution, mixed solution is applied to tungsten cathode substrate surface, is toasted;Tungsten wire after surface to be applied with to tungsten-rhenium alloy powder is put into high temperature hydrogen furnace, keeps the temperature 5~10 minutes at 1500 ± 50 DEG C, tungsten-rhenium alloy layer is prepared;Then, the tungsten wire that surface has been sintered tungsten-rhenium alloy layer is placed in air pressure is 10‑3~10‑1It in the benzene atmosphere of Pa, is carbonized in the case where tungsten wire temperature is 2000~2400K, carbonization time is 0.5~2 minute, that is, directly-heated type carbonization tungsten-rhenium alloy cathode is prepared.Directly-heated type carbonization tungsten-rhenium alloy cathode of the invention can be improved the emission of the effective pure tungsten wire cathode of magnetic control, the operating temperature and surface evaporation rate of pure tungsten wire cathode be reduced, to extend the service life of cathode and magnetron.

Description

A kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode
Technical field
The present invention relates to a kind of preparation methods of directly-heated type carbonization tungsten-rhenium alloy cathode.
Background technique
Magnetron just develops towards the direction of high-output power at present, and common barium-tungsten dispense cathode, oxide-coated cathode etc. are because of it Intolerant to electronics, ion bombardment, intolerant to anode high voltage, it is prone to which the disadvantages of striking sparks can hardly answer in middle high power magnetron With.Therefore, in the middle high power CW wave magnetron of high anode voltage, weaker directly-heated type pure tungsten (W) silk yin of emissive power Pole is widely applied.It is compared with ordinary oxide cathode with barium-tungsten dispense cathode, pure W wire cathode has launch stability height, resistance to electricity The advantages that son, ion bombardment ability are strong, and anti-toxicity is strong.But in normal output power, middle high power CW wave magnetic The cathode of keyholed back plate is generally operational in 2450K temperature or more, and it is too fast that excessively high cathode operating temperature will will lead to cathode surface evaporation, When the diameter of cathode is lower than the 90% of initial diameter, the cathode life of the magnetron ends.Therefore the high-power company in The termination in pure W wire cathode service life is one of the main reason for causing magnetron life to terminate in continuous wave magnetron.
Summary of the invention
Its purpose of the invention, which is that, provides a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode, solves in The problem of termination in pure W wire cathode service life causes magnetron life to terminate in high power CW wave magnetron has and improves pure W The characteristics of emission of cathode reduces the operating temperature of cathode, extends the service life of cathode.
It adopts the technical scheme that achieve the above object, a kind of preparation side of directly-heated type carbonization tungsten-rhenium alloy cathode Method, comprising steps of
A, metal tungsten powder and rhenium powder are mixed to pour into agate alms bowl and is ground sufficiently, the tungsten-rhenium alloy powder being uniformly mixed;
B, the tungsten-rhenium alloy powder is uniformly mixed with 1.5~3wt% cotton solution, mixed solution is applied to tungsten cathode Substrate surface is placed under infrared lamp and toasts;
C, the tungsten wire after surface to be applied with to tungsten-rhenium alloy powder is put into high temperature hydrogen furnace, and 5~10 are kept the temperature at 1500 ± 50 DEG C Minute, that is, tungsten-rhenium alloy layer is prepared;
D, the tungsten wire that surface has been sintered tungsten-rhenium alloy layer is placed in air pressure is 10-3~10-1In the benzene atmosphere of Pa, in tungsten wire temperature To be carbonized under 2000~2400K, carbonization time is 0.5~2 minute, that is, directly-heated type carbonization tungsten-rhenium alloy yin is prepared Pole.
Beneficial effect
The present invention has the following advantages that compared with prior art.
It is an advantage of the invention that by the way that experimental results demonstrate close to pure W, carbonization treatment tends to the fusing point of metal Re Enough improve the heat emission current density of alloy cathode;Directly-heated type carbonization tungsten-rhenium alloy cathode, which not only remains pure W cathode, has hair It is good to penetrate stability, the advantages that resistance to electronics, ion bombardment ability are strong, and anti-toxicity can be strong, but also there is biggish heat emission electricity Current density, directly-heated type of the invention carbonization tungsten-rhenium alloy cathode can be mentioned when being lower than at least 400 DEG C of pure W cathode temperature as a result, For identical heat emission current density.So directly-heated type produced by the present invention is carbonized, tungsten-rhenium alloy cathode be can be improved high-power The emission of the pure W wire cathode of continuous wave magnetron reduces the operating temperature of pure W wire cathode, reduces cathode surface and steams Hair rate, to extend the service life of cathode.
Detailed description of the invention
Below in conjunction with attached drawing, the invention will be further described.
Fig. 1 is preparation flow figure of the invention;
Fig. 2 is structural schematic diagram of the invention;
Fig. 3 is the heat emission current density contrast curve chart of the invention with pure tungsten wire cathode;
Fig. 4 is life curve schematic diagram of the invention.
Specific embodiment
A kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode, as shown in Figs 1-4, comprising steps of
A, metal tungsten powder and rhenium powder are mixed to pour into agate alms bowl and is ground sufficiently, the tungsten-rhenium alloy powder being uniformly mixed;
B, the tungsten-rhenium alloy powder is uniformly mixed with 1.5~3wt% cotton solution, mixed solution is applied to tungsten cathode Substrate surface is placed under infrared lamp and toasts;
C, the tungsten wire after surface to be applied with to tungsten-rhenium alloy powder is put into high temperature hydrogen furnace, and 5~10 are kept the temperature at 1500 ± 50 DEG C Minute, that is, tungsten-rhenium alloy layer is prepared;
D, the tungsten wire that surface has been sintered tungsten-rhenium alloy layer is placed in air pressure is 10-3~10-1In the benzene atmosphere of Pa, in tungsten wire temperature To be carbonized under 2000~2400K, carbonization time is 0.5~2 minute, that is, directly-heated type carbonization tungsten-rhenium alloy yin is prepared Pole.
It is that (90~95wt%:5~10wt% is mixed that W powder and Re powder in a step, which are according to weight percent,;W Powder, Re powder are that purity is 99.9%, and average grain diameter is 1~3 μm.
Grinding in a step carries out in agate alms bowl, and mixed grinding 24~48 hours.
Tungsten-rhenium alloy powder in the b step is mixed with 1.5~3wt% cotton solution by weight for 1:2~4, Incorporation time 0.5~2 hour.
Baking in the b step is carried out under infrared lamp, baking time >=1 hour.
Sintering process in the step c are as follows: first heat up, time-consuming linearly rises to 1500 ± 50 from room temperature in 0.5~2 hour DEG C, in heat preservation 5~cool down after ten minutes, when cooling, room temperature is linearly down within time-consuming 0.5~3 hour from 1500 ± 50 DEG C.
The tungsten-rhenium alloy layer that tungsten filament is sintered in the step c with a thickness of between 50~300 μm.
High vacuum chamber is pumped to 10 first with vacuum pump system in the Step d-7Pa connects benzene vapor afterwards, makes vacuum Degree is maintained at 10-3~10-1Pa。
The purity of benzene vapor needs >=99.8% in the Step d.
After carbonization is completed in the Step d, the operating temperature of cathode is linear from 2000K~2400K time-consuming 1~4 hour It is cooled to room temperature.
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference Attached drawing, the present invention is described in further detail.
The invention discloses a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode, alloy cathode made from this method It is used as substrate using pure metal W, one layer of tungsten-rhenium alloy layer is sintered in substrate surface, surface has then been sintered tungsten-rhenium alloy layer Tungsten wire be placed in air pressure be 10-3~10-1In the benzene atmosphere of Pa, it is carbonized, is carbonized in the case where tungsten wire temperature is 2000~2400K Time is 0.5~2 minute, that is, directly-heated type carbonization tungsten-rhenium alloy cathode is prepared.The directly-heated type is carbonized tungsten-rhenium alloy cathode can To be used for middle high power CW wave magnetron, the service life on service life platform is alreadyd exceed 2000 hours at present.
A kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode, comprising the following steps:
A, it is ground 24~48 hours after mixing metal W powder and Re powder and obtains mixed uniformly tungsten-rhenium alloy powder;
B, it after evenly mixing by mixed uniformly tungsten-rhenium alloy powder and (1.5~3) wt% cotton solution, will be mixed using spray gun Solution is sprayed in W substrate surfaces, then, baking W silk table face to cotton solution evaporating completely;
C, the W silk after surface to be sprayed to upper tungsten-rhenium alloy powder, which is put into high temperature hydrogen furnace at 1500 ± 50 DEG C, keeps the temperature 5~10 points Tungsten-rhenium alloy layer is prepared in clock;
D, the tungsten wire that surface has been sintered tungsten-rhenium alloy layer is placed in air pressure is 10-3~10-1In the benzene atmosphere of Pa, in tungsten wire temperature To be carbonized under 2000~2400K, carbonization time is 0.5~2 minute, that is, directly-heated type carbonization tungsten-rhenium alloy yin is prepared Pole.
Wherein, the purity of metal W powder and Re powder is preferably 99.9%, and average grain diameter is preferably 1~3 μm.Wherein, in a step W powder and Re powder be according to weight percent be (90~95) wt%:(5~10) wt% mixes.
Wherein, the grinding in a step is carried out in agate alms bowl, mixed grinding 24~48 hours.
Wherein, the tungsten-rhenium alloy powder in b step and (1.5~3) wt% cotton solution are by weight for 1:(2~4) it is mixed It closes, incorporation time 0.5~2 hour.
Wherein, the baking in b step is carried out under infrared lamp, baking time >=1 hour.
Wherein, the sintering process in step c are as follows: first heat up, time-consuming linearly rises to 1500 ± 50 from room temperature in 0.5~2 hour DEG C, in heat preservation 5~cool down after ten minutes, when cooling, room temperature is linearly down within time-consuming 0.5~3 hour from 1500 ± 50 DEG C.
Wherein, the tungsten-rhenium alloy layer that tungsten filament is sintered in step c with a thickness of between 50~300 μm.
Wherein, high vacuum chamber is pumped to 10 first with vacuum pump system in Step d-7Pa connects benzene vapor afterwards, makes vacuum Degree is maintained at 10-3~10-1Pa。
Wherein, the purity for the benzene vapor connected in Step d needs >=99.8%.
Wherein, after carbonization is completed in Step d, the operating temperature of cathode is linear from 2000K~2400K time-consuming 1~4 hour It is cooled to room temperature.
The preparation method flow chart of directly-heated type carbonization tungsten-rhenium alloy cathode of the invention is as shown in Figure 1, relative to existing skill The preparation method of the pure W wire cathode of art preparation, black matrix is inventive point of the invention in figure.
As a preferred embodiment, the preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode of the invention includes following step Rapid: selection purity is the metal W powder that 99.9wt% average particle size is 1~3 μm and Re powder is (90~95) wt% by weight percentage: (5~10) wt% pours into agate alms bowl ground and mixed 24~48 hours until uniformly.Then by uniformly mixed tungsten-rhenium alloy powder with (1.5~3) wt% cotton solution according to weight percent be 1:(2~4) pour into agate alms bowl mix 0.5~2 hour after pour into spray It is uniformly sprayed in rifle in W substrate surfaces, then processed tungsten wire is put under infrared lamp and is toasted 1 hour or more until guncotton Solution evaporating completely.Metal W silk after surface to be sprayed to upper tungsten-rhenium alloy powder later is put into high temperature hydrogen furnace 1500 ± 50 The preparation of the tungsten-rhenium alloy layer is completed in heat preservation for 5~10 minutes at DEG C.Finally, the tungsten wire that surface has been sintered tungsten-rhenium alloy layer is placed in Air pressure is 10-3~10-1In the benzene atmosphere of Pa, tungsten wire temperature be 2000~2400K under be carbonized, carbonization time be 0.5~ 2 minutes, that is, directly-heated type carbonization tungsten-rhenium alloy cathode is prepared.The structure for the alloy cathode of the invention being prepared such as Fig. 2 It is shown.
The alloy cathode performance of the invention being prepared is detected.By directly-heated type carbonization tungsten-rhenium alloy cathode filament dress Enter in cylinder-shaped anode vacuum diode.By vacuum diode system after 450~500 DEG C of heat preservations degassing in 0.5~2.0 hour, Again with 40~70mA high-frequency current degassing 5~20 minutes, 60~130mA high-frequency current degassing 5~10 minutes, system vacuum at this time Degree has been better than 10-5Pa.Hereafter using progress heat emission characteristic survey after the degassing of cathode high temperature, activation and seasoned 24 hours It tries, cathode temperature is measured using leucoscope in test.Test results are shown in figure 3.
Will carry out heat emission characteristic be completed after equipped with the alloy cathode silk vacuum diode insertion service life platform into The test of row cathode life.Test results are shown in figure 4 for it.
Fig. 3 show the heat emission characteristic curve graph of directly-heated type carbonization tungsten-rhenium alloy cathode, as shown in Figure 4 the alloy cathode Zero-field emission current density when operating temperature is 1700 DEG C, 1800 DEG C, 1900 DEG C, 2000 DEG C is respectively 0.11A/cm2、 0.28 A/cm2、1.02A/cm2、2.21A/cm2, and the zero-field emission current density of pure W wire cathode reaches 0.11A/cm2、 0.28A/cm2When operating temperature at least be respectively 2100 DEG C, 2200 DEG C.It is compared with pure W wire cathode, directly-heated type carbonization W-Re Alloy cathode can make pure W cathode operating temperature reduce at least 400 DEG C, show that the alloy cathode has powerful heat emission energy Power.
It is 1800 DEG C that Fig. 4, which show directly-heated type carbonization tungsten-rhenium alloy cathode in brightness temperature, and initial transmissions current density is 0.3A/cm2When life curve.As shown in Figure 4, the service life of the alloy cathode alreadys exceed 2000 hours, and the service life still after In continuous.In addition, not monitoring that the alloy cathode surface has during life experiment and significantly evapotranspiring, illustrate alloy yin It is great to have preferable high-temperature stability.
Table 1 show directly-heated type carbonization tungsten-rhenium alloy cathode of the invention and applies in 15kW continuous wave magnetron Real work situation.It is known that the application of directly-heated type carbonization tungsten-rhenium alloy cathode can be such that pure W cathode filament preheats from table 1 Electric current can reduce 2A, and operating current can reduce 1A, and it is W pure that this can all be such that magnetron reduces while guaranteeing normal output power The operating temperature of cathode, to extend service life of the cathode in pipe.
Table 1

Claims (10)

1. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode, which is characterized in that comprising steps of
A, metal tungsten powder and rhenium powder are mixed to pour into agate alms bowl and is ground sufficiently, the tungsten-rhenium alloy powder being uniformly mixed;
B, the tungsten-rhenium alloy powder is uniformly mixed with 1.5~3wt% cotton solution, mixed solution is applied to tungsten cathode Substrate surface is placed under infrared lamp and toasts;
C, the tungsten wire after surface to be applied with to tungsten-rhenium alloy powder is put into high temperature hydrogen furnace, and 5~10 are kept the temperature at 1500 ± 50 DEG C Minute, that is, tungsten-rhenium alloy layer is prepared;
D, the tungsten wire that surface has been sintered tungsten-rhenium alloy layer is placed in air pressure is 10-3~10-1In the benzene atmosphere of Pa, it is in tungsten wire temperature It is carbonized under 2000~2400K, carbonization time is 0.5~2 minute, that is, directly-heated type carbonization tungsten-rhenium alloy cathode is prepared.
2. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described It is that (90~95wt%:5~10wt% is mixed that W powder and Re powder in a step, which are according to weight percent,;W powder, Re powder are purity It is 99.9%, average grain diameter is 1~3 μm.
3. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described Grinding in a step carries out in agate alms bowl, and mixed grinding 24~48 hours.
4. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described Tungsten-rhenium alloy powder in b step is mixed with 1.5~3wt% cotton solution by weight for 1:2~4, incorporation time 0.5 ~2 hours.
5. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described Baking in b step is carried out under infrared lamp, baking time >=1 hour.
6. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described Sintering process in step c are as follows: first heat up, time-consuming linearly rises to 1500 ± 50 DEG C from room temperature in 0.5~2 hour, in heat preservation 5~10 Cool down after minute, when cooling, is linearly down to room temperature within time-consuming 0.5~3 hour from 1500 ± 50 DEG C.
7. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described The tungsten-rhenium alloy layer that tungsten filament is sintered in step c with a thickness of between 50~300 μm.
8. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described High vacuum chamber is pumped to 10 first with vacuum pump system in Step d-7Pa connects benzene vapor afterwards, and vacuum degree is made to be maintained at 10-3 ~10-1Pa。
9. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that described The purity of benzene vapor needs >=99.8% in Step d.
10. a kind of preparation method of directly-heated type carbonization tungsten-rhenium alloy cathode according to claim 1, which is characterized in that institute It states in Step d after carbonization completion, the operating temperature of cathode was linearly cooled to room temperature from 2000K~2400K time-consuming 1~4 hour.
CN201810710971.3A 2018-07-03 2018-07-03 Preparation method of directly-heated high-temperature tungsten-rhenium alloy cathode Expired - Fee Related CN109065422B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110112045A (en) * 2019-04-01 2019-08-09 九江学院 High power magnetic keyholed back plate direct-heated cathode and preparation method thereof
CN110676137A (en) * 2019-09-16 2020-01-10 九江学院 Preparation method of cathode for magnetron

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN105702542A (en) * 2015-11-09 2016-06-22 中国科学院电子学研究所 Rhenium doped tungsten-based alloy cathode and preparation method thereof

Patent Citations (1)

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Publication number Priority date Publication date Assignee Title
CN105702542A (en) * 2015-11-09 2016-06-22 中国科学院电子学研究所 Rhenium doped tungsten-based alloy cathode and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110112045A (en) * 2019-04-01 2019-08-09 九江学院 High power magnetic keyholed back plate direct-heated cathode and preparation method thereof
CN110676137A (en) * 2019-09-16 2020-01-10 九江学院 Preparation method of cathode for magnetron
CN110676137B (en) * 2019-09-16 2022-05-27 九江学院 Preparation method of cathode for magnetron

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