WO2000046830A1 - Plaque diaphragme et son procede de traitement - Google Patents

Plaque diaphragme et son procede de traitement Download PDF

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Publication number
WO2000046830A1
WO2000046830A1 PCT/JP2000/000640 JP0000640W WO0046830A1 WO 2000046830 A1 WO2000046830 A1 WO 2000046830A1 JP 0000640 W JP0000640 W JP 0000640W WO 0046830 A1 WO0046830 A1 WO 0046830A1
Authority
WO
WIPO (PCT)
Prior art keywords
coating
aperture plate
plate
osmium
cleaning
Prior art date
Application number
PCT/JP2000/000640
Other languages
English (en)
Japanese (ja)
Inventor
Hirosi Sato
Original Assignee
Daiwa Tecthno Systems Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Daiwa Tecthno Systems Co., Ltd. filed Critical Daiwa Tecthno Systems Co., Ltd.
Publication of WO2000046830A1 publication Critical patent/WO2000046830A1/fr

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Classifications

    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/26—Processing photosensitive materials; Apparatus therefor
    • G03F7/42—Stripping or agents therefor
    • G03F7/422—Stripping or agents therefor using liquids only
    • G03F7/423—Stripping or agents therefor using liquids only containing mineral acids or salts thereof, containing mineral oxidizing substances, e.g. peroxy compounds
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
    • H01J37/02—Details
    • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
    • H01J37/09—Diaphragms; Shields associated with electron or ion-optical arrangements; Compensation of disturbing fields

Definitions

  • the present invention relates to an aperture plate and a method of processing the same, and more particularly, to a high-precision aperture plate suitable for an electron beam application device such as an electron microscope and a method of processing the same.
  • an aperture plate has been used to adjust a beam diameter of an electron beam.
  • This aperture plate is, for example, a metal plate having a high melting point made of molybdenum or the like and having minute passing holes formed therein, as described in Japanese Patent Application Laid-Open No. H04-204624. The surface was coated with platinum or platinum-palladium to prevent contamination.
  • etching is used as a method of making holes in the aperture plate.
  • a resist used for etching a molybdenum metal plate is a resist used for ordinary semiconductor manufacturing and the like. Unlike the heat exchangers used, they have high heat resistance, corrosion resistance, and acid resistance.
  • the resist used at the time of etching is not completely removed and remains on the surface of the aperture plate, the surface of the residual resist, which is an insulator, may be lost when the aperture plate is mounted on an electron microscope and used.
  • the resolution is not improved due to charging, which affects the electron beam and causes problems such as contamination (impurity source).
  • An object of the present invention is to solve the above-mentioned problems of the prior art, and to provide an aperture plate capable of achieving and maintaining high resolution and a method of processing the same. Disclosure of the invention
  • the present invention is characterized by a washing step capable of completely removing the residual resist from the aperture plate, or a coating step of coating the surface of the aperture plate with osmium.
  • the residual resist of the drawing plate after the hole forming process by etching is more completely removed than in the conventional method, so that problems such as charged contamination, coating peeling, etc. are reduced. And the resolution is improved.
  • the coated osmium forms a hard bond coat layer, and a uniform conductive amorphous thin film at the molecular level is formed on the surface of the aperture plate, so that deterioration of resolution can be prevented.
  • FIG. 1 is an explanatory view showing a cleaning step of a diaphragm plate to which the present invention is applied.
  • FIG. 2 is an explanatory view showing a coating process of an aperture plate to which the present invention is applied.
  • BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described in detail.
  • mi is an explanatory view showing a part of the processing step of the aperture plate to which the present invention is applied.
  • the process of manufacturing an aperture plate for an electron microscope can be broadly divided into three processes.
  • the first step is a step of making a hole of a predetermined size by etching a molybdenum metal plate.
  • the molybdenum plate which is a material, is first baked in a vacuum furnace, finished to a predetermined thickness and surface by a rolling roller, and then heat-treated in a hydrogen furnace in a state of leaning against it. Thereafter, a hole having a predetermined diameter is formed by etching by a known method.
  • the photoresist used at this time is, for example, a mixture of xylene, ethylbenzene, cyclized polyisoprene, and the like. Unlike a resist usually used in semiconductor manufacturing, etc., heat resistance of 100 ° C. or more and corrosion resistance are used. It is highly resistant to sulfuric acid and hydrofluoric acid. Therefore, after drilling holes, the resist is removed to some extent by, for example, a well-known RI RI (reactive ion etching) apparatus, but it is insufficient as an aperture plate, and the aperture plate 10 subjected to the resist removal processing is not enough. The resist still remains on the surface.
  • RI RI reactive ion etching
  • FIG. 1 shows this washing step.
  • the cleaning step first, ten aperture plates (10) in which holes are completed are prepared. Then, 50 cc (11) of " ⁇ GR sulfuric acid” (concentration: 97%, for precision analysis) was put into a beaker, and this was heated to 80 degrees Celsius to 12 degrees by any known heating device. Heat to 0 degrees. Then, put 10 diaphragm plates in the heated UGR sulfuric acid 11 and maintain the temperature for 10 to 20 minutes.
  • ⁇ GR sulfuric acid concentration: 97%, for precision analysis
  • An EL mixture is a mixture of EL sulfuric acid (96% concentration, for electronics industry) and EL hydrogen peroxide solution (30% concentration, for electronics industry) in a ratio of 4: 1 to 6: 1. It is.
  • the beaker is set in the ultrasonic cleaning device 15 for about 40 seconds to 1 minute, and the aperture plate 13 is cleaned. Discard the EL mixture 14 after washing.
  • the distilled water 17 heated to 40 to 50 degrees Celsius is poured into a beaker containing the diaphragm plate 16 and poured and washed. This is repeated twice. Furthermore, take the squeezing plate in a net basket, put the basket in a beaker, add 15 O cc of distilled water heated to 40 to 50 degrees Celsius, and set it in the ultrasonic cleaning device 15.
  • FIG. 2 is an explanatory view showing a coating step of the present invention.
  • the gas in the vacuum vessel 21 of the coating apparatus 20 is exhausted.
  • a rotary pump is used for evacuation in a commercially available coating apparatus 20, but a rotary pump can obtain only a vacuum degree of about 10 ⁇ 2 Torr.
  • a metal diaphragm plate is coated at such a low vacuum, a uniform film thickness is formed on the surface of the diaphragm plate, unlike the film formation on the insulator surface, which is the purpose of a commercially available coating device.
  • a cleaning process as a pretreatment is sufficiently performed, and in the coating process, for example, a well-known oil diffusion (diffusion) is used as an exhaust pump. ) Use a pump to secure a vacuum of 10 minus 4 to 5 torr.
  • an inert gas such as an argon gas, a helium gas, or a nitrogen gas after the evacuation and exhausting the gas again, the concentration of oxygen and water vapor can be further reduced.
  • the injection of the inert gas and the exhaust may be repeated a plurality of times.
  • the present invention by reducing the concentration of the impurity gas by the above-described method, the occurrence of unevenness in the coating film thickness is eliminated, and uniform film formation can be stably performed.
  • Oxmium tetroxide is used as the metal to be coated.
  • the aperture plate was coated with platinum or platinum-palladium, there was a problem that the metal was crystallized (granulated) and the coating surface was not uniform and smooth.
  • the uniformity was not obtained. It becomes a hard amorphous thin film and has better conductivity than conventional metals.
  • the melting point of osmium is as high as 270 degrees Celsius, and there is no damage due to electron beam irradiation of an electron microscope.Therefore, it is possible to irradiate a sufficiently focused strong electron beam at a high accelerating voltage. The resolution can be brought out to the limit.
  • a commercially available coating device can be applied to the coating process.
  • a plasma coating device (NL-OPC80N) manufactured by Japan Laser Electronics Co., Ltd. may be applied.
  • a plasma coating device (NL-OPC80N) manufactured by Japan Laser Electronics Co., Ltd. may be applied.
  • a small amount of osmium tetroxide crystal placed in a sublimation cylinder is introduced into a small-capacity gas reactor equipped with an anode plate and a cathode plate, and a dilute sublimation gas pressure is applied.
  • a glow discharge is generated at a flowing glow discharge voltage. Then, the space between the electrodes instantly becomes a plasma state and emits light.
  • ionized osmium molecules are instantaneously adhered and deposited on the surface of the diaphragm 18 placed in the negative glo phase region on the cathode plate, and an amorphous osmium thin film is formed.
  • the film thickness to be coated is about several nanometers to several tens of nanometers.
  • the present invention may have the following modifications.
  • the combination of the cleaning step and the coating step is disclosed.However, for example, only the cleaning step or the coating step alone has an effect of improving the resolution as compared with the conventional aperture plate. It may be performed alone.
  • the holes in the aperture plate can be opened by electric discharge machining, machining, laser machining, electronic beam machining, etc., in addition to etching. In such a case, as described above, by applying an osmium coating, The effect can be expected.
  • a metal other than molybdenum as the material of the aperture plate, for example, a metal having a lower melting point than molybdenum. Even in such a case, by applying the osmium coating, the surface of the aperture plate is covered with the conductive thin film having a high melting point, so that the above-described effects can be expected.
  • the case where the aperture plate is newly manufactured is disclosed.
  • impurities adhere or the coating is peeled off.
  • both the cleaning process and the coating process of the present invention or only one of them may be performed.
  • the present invention is not limited to the aperture plate of the electron microscope, and can be applied to processing of parts of an apparatus that handles an arbitrary electron beam. is there. Industrial applicability
  • the hole by etching is obtained. Residual resist on the aperture plate after blanking is more completely removed as compared with the conventional method, so that problems such as charging / contamination and peeling of coating are reduced and resolution is improved. There is.
  • the coated osmium becomes a hard amorphous conductive film, there is an effect that deterioration of resolution can be prevented. Since osmium has a higher melting point than platinum, performance can be further improved by further coating osmium on a conventional platinum-coated drawing plate.
  • the aperture plate of the present invention can achieve high resolution and maintain the performance.

Abstract

Procédé servant à traiter une plaque diaphragme de microscope électronique, par exemple, ce qui consiste à nettoyer les résidus de résine photosensible sur ladite plaque dans laquelle on a pratiqué un orifice par attaque chimique au moyen d'acide sulfurique chaud concentré ou d'une solution aqueuse chaude de peroxyde d'hydrogène et à revêtir la plaque diaphragme d'osmium. Ce procédé permet d'enlever la résine photosensible résiduelle de façon plus efficace que les procédés classiques. De ce fait, il permet de supprimer les problèmes de charge, de contamination et de séparation du revêtement et d'améliorer la résolution. Le revêtement d'osmium sert de feuil conducteur dur non cristallin, ce qui empêche la dégradation de la résolution.
PCT/JP2000/000640 1999-02-08 2000-02-07 Plaque diaphragme et son procede de traitement WO2000046830A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
JP3036499 1999-02-08
JP11/30364 1999-02-08
JP11208534A JP3117687B2 (ja) 1999-02-08 1999-07-23 絞りプレートおよびその処理方法
JP11/208534 1999-07-23

Publications (1)

Publication Number Publication Date
WO2000046830A1 true WO2000046830A1 (fr) 2000-08-10

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2000/000640 WO2000046830A1 (fr) 1999-02-08 2000-02-07 Plaque diaphragme et son procede de traitement

Country Status (2)

Country Link
JP (1) JP3117687B2 (fr)
WO (1) WO2000046830A1 (fr)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4726048B2 (ja) * 2005-05-27 2011-07-20 株式会社日立製作所 位相回復方式の電子顕微鏡による観察方法
JP5703439B2 (ja) * 2012-12-17 2015-04-22 株式会社ユーテック 金属プレート及びオスミウム膜の成膜方法
CN104599927B (zh) * 2014-12-24 2016-11-30 西安理工大学 一种多孔光阑的制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5557246A (en) * 1978-10-23 1980-04-26 Jeol Ltd Electron-ray contracting apparatus and its manufacturing method
JPH0249338A (ja) * 1988-04-28 1990-02-19 Hitachi Ltd 荷電粒子線用絞り
JPH04206244A (ja) * 1990-11-30 1992-07-28 Hitachi Ltd 絞り装置およびその製法
JPH0963999A (ja) * 1995-08-21 1997-03-07 Nippon Telegr & Teleph Corp <Ntt> 金属製ホルダーの洗浄方法
JPH09306374A (ja) * 1996-05-20 1997-11-28 Sony Corp 陰極線管の第一制御電極からの浮遊電子放出防止方法および第一制御電極
JPH10130868A (ja) * 1996-10-24 1998-05-19 Dainippon Screen Mfg Co Ltd 金属薄板のエッチングにおける面出し方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5557246A (en) * 1978-10-23 1980-04-26 Jeol Ltd Electron-ray contracting apparatus and its manufacturing method
JPH0249338A (ja) * 1988-04-28 1990-02-19 Hitachi Ltd 荷電粒子線用絞り
JPH04206244A (ja) * 1990-11-30 1992-07-28 Hitachi Ltd 絞り装置およびその製法
JPH0963999A (ja) * 1995-08-21 1997-03-07 Nippon Telegr & Teleph Corp <Ntt> 金属製ホルダーの洗浄方法
JPH09306374A (ja) * 1996-05-20 1997-11-28 Sony Corp 陰極線管の第一制御電極からの浮遊電子放出防止方法および第一制御電極
JPH10130868A (ja) * 1996-10-24 1998-05-19 Dainippon Screen Mfg Co Ltd 金属薄板のエッチングにおける面出し方法

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JP2000299076A (ja) 2000-10-24
JP3117687B2 (ja) 2000-12-18

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