WO2019008738A1 - Source d'électrons du type à émission de champ et dispositif à faisceau de particules chargées - Google Patents

Source d'électrons du type à émission de champ et dispositif à faisceau de particules chargées Download PDF

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Publication number
WO2019008738A1
WO2019008738A1 PCT/JP2017/024942 JP2017024942W WO2019008738A1 WO 2019008738 A1 WO2019008738 A1 WO 2019008738A1 JP 2017024942 W JP2017024942 W JP 2017024942W WO 2019008738 A1 WO2019008738 A1 WO 2019008738A1
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WIPO (PCT)
Prior art keywords
electrode
needle electrode
source
zirconia
needle
Prior art date
Application number
PCT/JP2017/024942
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English (en)
Japanese (ja)
Inventor
亜紀 武居
創一 片桐
宗一郎 松永
源 川野
土肥 隆
Original Assignee
株式会社日立ハイテクノロジーズ
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Priority to PCT/JP2017/024942 priority Critical patent/WO2019008738A1/fr
Publication of WO2019008738A1 publication Critical patent/WO2019008738A1/fr

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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00Details 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
    • H01J1/02Main electrodes
    • H01J1/30Cold cathodes, e.g. field-emissive cathode
    • H01J1/304Field-emissive cathodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00Details 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
    • H01J1/46Control electrodes, e.g. grid; Auxiliary electrodes
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02Details
    • H01J37/04Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/06Electron sources; Electron guns
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02Details
    • H01J37/04Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/06Electron sources; Electron guns
    • H01J37/073Electron guns using field emission, photo emission, or secondary emission electron sources
    • 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

Definitions

  • the present invention relates to a field emission type electron source and a charged particle beam apparatus using the same.
  • a scanning electron microscope Scanning Electron Microscope
  • TEM Transmission Electron Microscope
  • SEM Scanning Electron Microscope
  • TEM Transmission Electron Microscope
  • An image is obtained by detecting secondary electrons or reflected electrons obtained to obtain an image
  • TEM Transmission Electron Microscope
  • a field emission electron source is generally used for the electron gun of these electron microscopes.
  • Field emission type electron sources are roughly classified into cold cathode field emission type electron sources and hot cathode field emission type electron sources.
  • the cold cathode field emission electron source applies an electric field to the tip of a needle-like electrode having a tip of a single crystal tungsten wire sharpened to emit electrons.
  • zirconia is attached to the side surface of the needle-like electrode having the tip of the single-crystal tungsten wire pointed at the tip of the single-crystal tungsten wire, and an electric field is applied to the tip of the needle in a heated state to emit electrons.
  • This hot cathode field emission electron source is also called a Schottky electron source.
  • the Schottky electron source forms a low work function region by supplying zirconium and oxygen by thermal diffusion on a tungsten crystal face (100).
  • the heating temperature is about 1600 K to 1900 K, usually 1700 K to 1800 K.
  • a crystal face (100) is provided at the tip of a tungsten needle, and a strong electric field is applied to take out thermoelectrons passing the potential barrier and electrons transmitted by tunneling.
  • a needle-like electrode whose tip is a crystal orientation (100) of single crystal tungsten is fixed by spot welding to a heating tungsten filament.
  • the needle electrode is provided with zirconia which is a diffusion source.
  • the diffusion source is molded around the needle when viewed from the tip of the needle.
  • Patent Document 1 discloses a method of forming a diffusion source by forming a solution in which zirconium hydride fine particles are mixed in an organic solvent with a brush and adhering it to the side circumference of a tungsten needle and vacuum heating for sintering.
  • U.S. Pat. No. 5,959,095 discloses using scandium oxide as the diffusion source to reduce the work function of a single crystal tungsten tip (100) surface to operate at low temperatures.
  • scandium oxide powder is mixed with an organic solvent or the like to form a slurry and to be attached or vapor deposited.
  • Patent Document 3 discloses that a practically stable life can be obtained by controlling the thickness and length of zirconia as a diffusion source.
  • Non-Patent Document 1 is trying to elucidate the structure and composition of a Schottky electron source using a surface analysis method with respect to the selective lowering mechanism of the work function due to zirconia diffusion.
  • the zirconia of the diffusion source As the zirconia of the diffusion source is heated and diffused on the surface of the single crystal tungsten wire, the work function of the tungsten crystal face (100) at the tip of the needle-like electrode is lowered from 4.5 eV to about 2.8 eV.
  • the diffusion failure of zirconia occurs during emission, the state of the crystal plane at the tip of the tungsten needle changes, and the electron emission characteristics deteriorate irregularly.
  • zirconia needs to be stably diffused to the surface of the single crystal tungsten wire.
  • Equation 1 The relationship between the surface coverage of the diffusion substance and the diffusion distance when the substance diffuses on the surface is expressed by (Equation 1).
  • k diffusion coefficient
  • K evaporation coefficient
  • C surface coverage
  • x diffusion distance
  • FIG. 2 is manufactured by changing the sintering position of zirconia of the field emission type electron source, and shows the diffusion failure rate in comparison with the conventional case (point 20). It can be seen that, as the sintering position of zirconia is closer to the tip and the diffusion distance L to the tip of the needle electrode becomes shorter, the diffusion failure decreases and stable emission characteristics can be obtained.
  • the dotted lines in the figure estimate the relationship between the diffusion distance L and the diffusion failure from these experimental results, and the diffusion source is placed closer to the tip of the needle electrode so that the diffusion distance L becomes shorter. It shows that the emission characteristics are stable.
  • FIG. 3 shows a schematic view of an electron gun mounted with a Schottky electron source.
  • the electron source 101 has a tungsten needle electrode 1, a filament 3 and a suppressor electrode 4.
  • the tungsten needle electrode 1 is fixed to the filament 3.
  • a diffusion source 2 is formed around the tungsten needle electrode 1 to supply zirconia to the tip of the tungsten needle electrode 1 during emission.
  • the filament 3 and the tungsten needle electrode 1 are covered with the suppressor electrode 4 except that the tip of the tungsten needle electrode 1 protrudes from the suppressor electrode opening 5.
  • the filament 3 is heated by a heating power source 108, and zirconia is diffused and supplied from the diffusion source 2 to the tip (emitter) of the tungsten needle electrode 1.
  • a positive voltage is applied to the extraction electrode 103 from the extraction electrode power supply 105, and the thermal electrons are extracted from the tip (emitter) of the tungsten needle-like electrode 1.
  • the extracted electrons are accelerated by the accelerating electrode 104 to which a positive voltage is applied by the accelerating electrode power supply 107.
  • a negative voltage is applied by the bias power supply 106.
  • the tip of the tungsten needle electrode 1 is disposed between the extraction electrode 103 and the suppressor electrode 4, so a strong electric field is applied near the tip of the needle electrode 1. ing.
  • the diffusion source 2 is disposed near the tip of the needle electrode 1, the diffusion source 2 is affected by this electric field.
  • the diffusion source is arranged to be contained in the suppressor electrode which is not affected by the electric field. Since the tungsten needle electrode of a general field emission electron source is configured to protrude 250 ⁇ m from the suppressor electrode, the distance from the tip of the needle to the zirconia was at least 250 ⁇ m.
  • the present invention provides a field emission electron source that can suppress the influence of an electric field and obtain stable long-term emission characteristics even when a diffusion source is disposed closer to the tip of a needle electrode, and a charged particle beam device using the same. It is to do.
  • a field emission electron source in which a suppressor electrode is disposed so as to cover the filament and the needle electrode except for the portion of the needle electrode protruding from the opening of the suppressor electrode, around the needle electrode, on the surface thereof
  • a diffusion source is formed to supply the zirconia to be diffused, the diffusion source having a thickness of at least 10 ⁇ m at least in the part covered by the suppressor electrode and 100 nm in the part protruding from the opening 5 It is formed to have the above thickness.
  • such a field emission type electron source is configured as an electron source of a charged particle beam device.
  • the diffusion of zirconia on the surface of the needle electrode of the field emission electron source becomes stable, and stable long-term emission becomes possible.
  • FIG. 2 is a view showing the shape of a diffusion source of Example 1; It is a figure which estimates consumption length of the zirconia diffusion source of the tip side of needlelike electrode 1.
  • FIG. 6 is a view showing the shape of a diffusion source of Example 2;
  • FIG. 7 is a view showing the shape of a diffusion source in Example 3; It is a figure which shows the whole structure of a scanning electron microscope.
  • FIG. 1A shows the entire configuration of a field emission type electron source 101.
  • the bottom of the needle electrode 1 is spot-welded with the tip of the single crystal tungsten rod sharpened sharply.
  • the tip 8 of the needle electrode 1 is the (100) plane of tungsten single crystal.
  • the tungsten needle electrode 1 around which the diffusion source 2 is formed is covered by a suppressor electrode 4.
  • the suppressor electrode 4 is an inverted cup-type structure with a circular opening 5 at the center of the cup bottom.
  • the tip portion of the tungsten needle-like electrode 1 is fixed so as to protrude from the opening 5.
  • a diffusion source 2 is provided which extends to the side surface of the tip portion of the tungsten needle electrode 1 which protrudes from the opening 5 of the suppressor electrode 4.
  • the zirconia of the diffusion source is heated by the tungsten filament 3 to diffuse the surface of the needle-like electrode and lower the work function of the tip 8 of the needle-like electrode 1, but the diffusion also progresses simultaneously with evaporation. Therefore, when the zirconia is depleted, the field emission electron source can not emit electrons and has a lifetime. That is, the diffusion source needs a volume (amount) according to the life.
  • FIG. 4 shows the relation between the consumption length per unit time and the consumption volume with respect to the thickness of zirconia of the diffusion source. The graph in FIG. 4 is obtained by experimentally accelerating and evaluating the consumption of zirconia of the diffusion source by heating the needle electrode to 2000 K, which is 200 K to 300 K higher than the normal use temperature.
  • the normal use temperature is measured by measuring the ratio R of the amount of gas released at the time of heating at the normal use temperature (1700 K to 1800 K) and at the time of 2000 K heating, heating time h and consumption volume ⁇ V (total volume V).
  • the consumption length per unit time increases when the thickness is thinner than 10 ⁇ m, whereas it tends to converge to a constant value when the thickness exceeds 10 ⁇ m.
  • the consumption volume per unit time increases in proportion to the thickness.
  • the thickness of the diffusion source zirconia is set to 10 ⁇ m and adjust the lifetime by the length.
  • the lifetime can be easily controlled by setting the thickness of the entire zirconia to 10 ⁇ m, but if the diffused source located in the portion protruding from the opening of the suppressor electrode has an excessive level difference or unevenness, it may cause an electric discharge. Therefore, it is desirable that the diffusion source located outside the suppressor be gradually thinner from the opening to the tip of the suppressor electrode.
  • the shape of the diffusion source of Example 1 is shown in FIG.
  • the diffusion source 9 is formed using inkjet technology.
  • the diffusion source 9 is formed by dispersing zirconia particles in a liquid of 5 to 10 pl and applying it on the side surface of the needle electrode 1 with an ink jet coater.
  • the liquid in which the zirconia particles are dispersed may be either an organic solvent or an inorganic solvent.
  • the interval and the number of times of application of the zirconia dispersion are controlled so that they can be formed smoothly and thinly.
  • the application of zirconia by inkjet is easy in controlling the thickness and is excellent in that surface irregularities can be formed less.
  • the zirconia coating start position is a position 100 ⁇ m away from the tip 8 so as not to be affected by polishing for sharpening the tip of the needle electrode 1. It should be noted that in consideration of manufacturing errors and the like, the position may be 100 ⁇ 50 ⁇ m away from the tip. If zirconia is generally thinly applied as the diffusion source 9, the diffusion source will evaporate and be depleted in a short period of time, so long-term stable emission can not be obtained. For this reason, it is desirable that the thickness be at least 10 ⁇ m at a portion sufficiently away from the tip.
  • the length of the diffusion source 9 located outside the suppressor electrode 4 is 150 ⁇ m.
  • the diffusion source 9 having a length of 150 ⁇ m is thinly applied so as not to cause unevenness.
  • the thickness of the diffusion source 9 in the portion covered by the suppressor electrode 4 is gradually increased so as to be 10 ⁇ m or more.
  • the zirconia is sintered on the side of the needle electrode 1 by heating in vacuum after application.
  • the application of zirconia by inkjet is characterized in that surface irregularities can be reduced.
  • mechanical polishing and laser annealing are used. You may process which makes the surface smooth.
  • the diffusion source located in the portion projecting from the opening 5 of the suppressor electrode 4 needs a certain thickness.
  • the amount of zirconia lost by the action of diffusion, evaporation, and the like is larger than the amount of zirconia supplied from the diffusion source at the rear (filament side). If the diffusion distance L between the tip of the source and the tip of the needle electrode is increased, the effect is reduced. For this reason, it is necessary to have a thickness that can suppress the retraction of the tip of the diffusion source to some extent.
  • FIG. 6 shows the estimation of the length of zirconia consumed on the tip end of the needle electrode during continuous emission at 1700K.
  • the thickness of the diffusion source 9 located in the portion of the suppressor electrode 4 which protrudes from the opening 5 is preferably 100 nm or more, preferably 1 ⁇ m or more.
  • the inside diameter of the opening 5 of the suppressor electrode 4 is It is designed to be at least twice as large as the diameter of the tungsten needle electrode 1.
  • Such positional relationship with the opening 5 is a factor that restricts the thickness of the diffusion source 9.
  • the field emission type electron source thus configured is installed in the electron gun shown in FIG.
  • the electron source 101 is heated to a predetermined temperature by the heating power supply 108 and a predetermined voltage is applied to the extraction electrode 103 and the suppressor electrode 4 to apply an electric field to the tip of the needle electrode 1, continuation of normal electron emission confirmed. Also, there were no protrusions or cracks that would cause the electric field to concentrate on the zirconia surface.
  • the diffusion source 9 is formed by applying zirconia to the vicinity of the tip 8 of the tungsten needle electrode 1.
  • the angle and distance of the ink jet outlet are controlled so that zirconia can be applied thinly and uniformly to the pointed portion of the tip.
  • the angle and the distance of the tungsten needle electrode 1 itself may be adjusted. Apply so as to have a gentle roundness so that there is no step due to a sudden change in thickness.
  • the portion covered by the suppressor electrode should have a thickness of 10 ⁇ m or more so that the zirconia of the diffusion source is not depleted.
  • Zirconia was applied to the tips 8 of the plurality of tungsten needle electrodes 1 and the shape of the zirconia after heating and sintering was observed. As a result, there were no protrusions or cracks that would concentrate the electric field on the surface of the zirconia. Also, the variation of the amount of sintered zirconia was within 2%. As described above, in the case of the application by the ink jet, the film thickness control can be performed with high accuracy as compared with the prior art.
  • the tip of the tungsten needle electrode 1 protrudes from the opening 5 of the suppressor electrode 4, but in the protruding part, zirconia having a smooth surface on all surfaces except for the tip 8.
  • the electron gun was set up and evaluated, and it was found that a field emission type electron source having stable diffusion can be manufactured with good reproducibility.
  • FIG. 8 Yet another form of the diffusion source is shown in FIG. 8 to illustrate the method of formation.
  • Example 3 a portion other than the tip 8 of the tungsten needle electrode 1 is covered with a zirconia thin film.
  • a zirconia thin film 10a of about 10 to 100 nm is formed on the whole by using a vacuum evaporation method on the insulator, the conductive terminal, the heating filament 3 connected thereto, and the tungsten needle electrode 1. At this time, zirconia is prevented from being formed on the tungsten crystal face (100) of the tip 8.
  • the zirconia at the tip may be removed by etching.
  • the zirconia 10b serving as a diffusion source is made 10 ⁇ m or more thick by ink jet technology or dripping dispersion.
  • the needle electrode 1 is applied to the side surface. This prevents premature depletion of the zirconia of the diffusion source.
  • the zirconia 10 b is sintered on the side of the needle electrode 1 by heating in a vacuum.
  • the tip of the tungsten needle-like electrode 1 protrudes from the opening 5 of the suppressor electrode 4, but a zirconia thin film 10a having a smooth surface deposited is present in the protruding part. .
  • a field emission type electron source whose diffusion is stable can be manufactured.
  • the electron gun 100 includes the field emission type electron source 101, the extraction electrode 103 and the acceleration electrode 104 described as the first to third embodiments. The details are as shown in FIG.
  • the electron beam 131 emitted from the electron gun 100 passes through the first condenser lens 112 and the second condenser lens 113, and is irradiated by the objective lens 116 so as to form an image on the sample 117 held on the stage 118.
  • the objective lens 116 may be an electric field lens, a magnetic field lens, or an electric field magnetic field superposition lens.
  • an aligner 111 for controlling the beam axis of the electron beam 131 is disposed at the rear stage of the electron gun 100.
  • the present invention can also be applied to reflected electrons reflected in front of the sample, backscattered electrons generated from the inside of the sample, secondary electrons and tertiary electrons generated by the reflector and the like. . And in order to detect these electrons resulting from irradiation of an electron beam, detector 121 or detector 120 can change a kind and arrangement suitably.
  • a high quality image can be stably obtained by applying an electric field emission electron source whose emission characteristics according to the present embodiment are stable over a long period of time.
  • the present invention is not limited to an embodiment, and can be variously changed in the range which does not deviate from the gist.
  • the diffusion source is not limited to zirconia, and any of compounds and oxides of metal elements selected from Ca, Sr, Ba, Sc, Y, La, Ti, Zr, Hf, and lanthanoid series groups.
  • two or more elements may be freely combined.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Electron Sources, Ion Sources (AREA)
  • Cold Cathode And The Manufacture (AREA)

Abstract

L'invention concerne : une source d'électrons du type à émission de champ avec laquelle l'influence d'un champ électrique peut être supprimée et des caractéristiques d'émission à long terme stables peuvent être obtenues même lorsqu'une source d'alimentation en diffusion est disposée à proximité de la pointe d'une électrode du type aiguille ; et un dispositif à faisceau de particules chargées l'utilisant. Selon la présente invention, une électrode de suppression (4) est disposée pour recouvrir un filament (3) et l'électrode du type aiguille (1) à l'exclusion d'une partie, de l'électrode du type aiguille (1), faisant saillie à partir d'une partie d'ouverture (5) de l'électrode de suppression (4), et une source d'alimentation en diffusion (9) permettant de fournir de la zircone qui est diffusée sur la surface de l'électrode du type aiguille (1) est formée autour de l'électrode du type aiguille (1), la source d'alimentation en diffusion (9) présentant une épaisseur de 10 µm ou plus dans au moins la partie recouverte par l'électrode de suppression (4) et présente une épaisseur de 100 nm ou plus dans la partie faisant saillie à partir de la partie d'ouverture (5).
PCT/JP2017/024942 2017-07-07 2017-07-07 Source d'électrons du type à émission de champ et dispositif à faisceau de particules chargées WO2019008738A1 (fr)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI724803B (zh) * 2019-04-18 2021-04-11 日商日立全球先端科技股份有限公司 電子源及荷電粒子束裝置
CN112786415A (zh) * 2021-03-03 2021-05-11 大束科技(北京)有限责任公司 发射针结构、热场发射电子源及电子显微镜
CN112992632A (zh) * 2021-02-05 2021-06-18 大束科技(北京)有限责任公司 发射针、电子源、电子显微镜及大半径电子束形成方法

Citations (2)

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JPH08250054A (ja) * 1995-03-14 1996-09-27 Hitachi Ltd 拡散補給型電子線源およびそれを用いた電子線装置
JP2013084550A (ja) * 2011-09-26 2013-05-09 Hitachi High-Technologies Corp 電界放出型電子源

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JPH08250054A (ja) * 1995-03-14 1996-09-27 Hitachi Ltd 拡散補給型電子線源およびそれを用いた電子線装置
JP2013084550A (ja) * 2011-09-26 2013-05-09 Hitachi High-Technologies Corp 電界放出型電子源

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI724803B (zh) * 2019-04-18 2021-04-11 日商日立全球先端科技股份有限公司 電子源及荷電粒子束裝置
CN112992632A (zh) * 2021-02-05 2021-06-18 大束科技(北京)有限责任公司 发射针、电子源、电子显微镜及大半径电子束形成方法
CN112786415A (zh) * 2021-03-03 2021-05-11 大束科技(北京)有限责任公司 发射针结构、热场发射电子源及电子显微镜

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