WO2019116605A1 - Dispositif d'irradiation par faisceau d'électrons et système d'analyse - Google Patents

Dispositif d'irradiation par faisceau d'électrons et système d'analyse Download PDF

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Publication number
WO2019116605A1
WO2019116605A1 PCT/JP2018/021484 JP2018021484W WO2019116605A1 WO 2019116605 A1 WO2019116605 A1 WO 2019116605A1 JP 2018021484 W JP2018021484 W JP 2018021484W WO 2019116605 A1 WO2019116605 A1 WO 2019116605A1
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WIPO (PCT)
Prior art keywords
sample
electron beam
beam irradiation
gas
irradiation apparatus
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PCT/JP2018/021484
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English (en)
Japanese (ja)
Inventor
明子 久田
祐介 大南
誠 中林
康 照井
吉江　正樹
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株式会社日立ハイテクノロジーズ
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Publication of WO2019116605A1 publication Critical patent/WO2019116605A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
    • 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
    • H01J37/16—Vessels; Containers
    • 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
    • H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
    • 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
    • H01J37/20—Means for supporting or positioning the objects or the material; Means for adjusting diaphragms or lenses associated with the support
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes

Definitions

  • the present invention relates to an electron beam irradiation apparatus for irradiating a sample with an electron beam.
  • a scanning electron microscope (SEM), a transmission electron microscope (TEM), or the like is used to observe a minute region of the object.
  • SEM scanning electron microscope
  • TEM transmission electron microscope
  • EDS energy dispersive X-ray analysis
  • the observation sample is, for example, an organic substance, it is generally difficult to identify its composition by EDS because the constituent element is C / H / O / N or the like.
  • Patent Document 1 describes a matrix-assisted laser desorption ionization method (MALDI method) in which a sample component is subjected to mass analysis using a laser.
  • Patent Documents 2 to 7 disclose a method of analyzing the mass of a sample component released by irradiating an ion beam or an electron beam to a sample.
  • Non-Patent Document 1 describes a method for desorbing a component from a sample using an electron beam by utilizing gas in the vicinity of the sample and charging of the surface of the sample.
  • Patent No. 4645197 gazette JP 09-096614 A WO 1997/019343 JP, 2012-021775, A WO2009 / 125761 JP 2017-050279 JP, 2017-026620, A
  • the present invention has been made in view of the above problems, and by irradiating a sample with an electron beam, the component separated from the sample is effectively recovered, and the component is subjected to mass analysis.
  • the electron beam irradiation apparatus recovers the components of the sample desorbed from the sample by generating a gas flow in the sample chamber.
  • the components separated from the sample can be efficiently recovered by irradiating the electron beam.
  • region can be analyzed rather than the sample detachment
  • FIG. 1 is a block diagram of an electron beam irradiation apparatus 100 according to a first embodiment.
  • FIG. 5 is a block diagram of an electron beam irradiation apparatus 100 according to a second embodiment.
  • FIG. 6 is a block diagram of an electron beam irradiation apparatus 100 according to a third embodiment.
  • This is a configuration example in which the analyzer 300 is directly connected to the gas suction port 132. It is a flowchart explaining the procedure which analyzes the sample 200 using the electron beam irradiation apparatus 100 which concerns on this invention. It is a conceptual diagram explaining each step of FIG.
  • the electron beam irradiation apparatus can apply the component desorbed from the sample by irradiating the sample with the electron beam, for example, in an analysis process such as mass spectrometry.
  • an analysis process such as mass spectrometry.
  • the components in the sample refer to atoms, molecules, ions, aggregates of molecules, molecules of molecules, and the like that constitute the sample.
  • a compound such as an oxide or a nitride is contained as a component.
  • components contained in a biological sample such as a protein or a lipid, a carbon-based compound such as a resin or a rubber, and the like are assumed to be analyzed.
  • any sample for which it is desired to analyze the recovered component can be the subject of the present invention.
  • a solid, a liquid, etc. which can be irradiated with an electron beam by an electron beam irradiation apparatus are assumed. It may be a gelled gel-like sample, or may be a sample in which liquid or solid is mixed, such as cells / bacteria / living tissue.
  • sample components refers to all methods or devices that reveal the components that constitute the sample. For example, (a) liquid chromatography to analyze after melting the recovered component into liquid, (b) gas chromatography to analyze the recovered component in the state of gas, (c) dissolve the recovered component into liquid or Ionization in the state of a gas, mass analysis that analyzes the mass and chemical structure of the component by ion trajectory control may be considered. If the recovered component is DNA, a DNA sequencer may be used. In addition, immunological detection using an antibody against the collected component, a color reaction specific to the collected component, analysis using an enzyme reaction to the collected component, and the like are also conceivable.
  • FIG. 1 is a conceptual view for explaining the principle of desorbing sample components by irradiating the sample with an electron beam. Similar to Non-Patent Document 1, FIG. 1 illustrates a method for desorbing sample components by using gas in the vicinity of the sample and charging of the sample surface.
  • the sample 1 When processing the sample 1 using the method shown in FIG. 1, the sample 1 needs to be charged, so the sample 1 needs to be an insulator.
  • the sample component to be recovered is a conductor or a semiconductor
  • the conductor or the semiconductor can be recovered as a sample component by covering it with an insulator so that charges do not escape to the periphery thereof.
  • FIG. 2 is a conceptual diagram for explaining the principle of recovering the component desorbed from the sample.
  • the component 201 separated from the sample 200 is recovered by generating a gas flow in the sample chamber containing the sample 200.
  • a gas inlet 131 and a gas suction port 132 described later are connected to the sample chamber.
  • the gas inlet 131 introduces a gas 133 such as N 2 , O 2 , H 2 , Ar, He or the like into the sample chamber.
  • the gas 133 flows from the gas inlet 131 toward the gas suction port 132 and passes near the sample 200.
  • the component 201 is recovered from the gas suction port 132 by the gas flow of gas 133.
  • the gas 133 When the sample 200 is an insulator, the gas 133 is charged by the electron beam as described in FIG. The electric field between the gas 133 and the sample 200 causes the component 201 to desorb from the sample 200. That is, the gas 133 has both the role of desorbing the component 201 and the role of recovering the component 201.
  • FIG. 3 is a conceptual view for explaining the principle of recovering the component 201.
  • the trap portion 160 is filled with, for example, a carrier that adsorbs the component 201.
  • a carrier that adsorbs the component 201.
  • a granular or crushed filler used for a solid phase column or the like can be used, or a membrane or a fiber to which the component 201 is adsorbed can be used.
  • the trap unit 160 captures the component 201.
  • the gas 133 is exhausted from the gas suction port 132 to the outside of the sample chamber.
  • FIG. 4 is a block diagram of the electron beam irradiation apparatus 100 according to the first embodiment of the present invention.
  • the electron beam irradiation apparatus 100 is an apparatus for desorbing and recovering the component 201 from the sample 200 by irradiating the sample 200 with the electron beam 112.
  • the electron beam irradiation apparatus 100 includes an electron beam irradiation unit 110, a sample chamber 120, a gas inlet 131, a gas suction port 132, a sample stage 140, a deflector 151, an objective lens 152, and an electron beam detector 153.
  • the electron beam irradiation unit 110 includes an electron beam source (not shown), and emits the electron beam 112 from the emission port 111.
  • the sample chamber 120 accommodates the sample 200.
  • the gas inlet 131 and the gas suction port 132 are the ones described in FIGS. 2 to 3 and are connected to the sample chamber 120.
  • the sample stage 140 is a stage on which the sample 200 is placed.
  • the deflector 151 adjusts the irradiation angle of the electron beam 112 to the sample 200 by deflecting the electron beam 112.
  • the objective lens 152 focuses the electron beam 112 on the surface of the sample 200.
  • the electron beam detector 153 detects an electron beam generated by irradiating the sample 200 with the electron beam 112, and outputs a detection signal.
  • the electron beam irradiation apparatus 100 is used in a low vacuum to atmospheric pressure atmosphere environment where a gas is present near the sample 200.
  • the pressure in the vicinity of the sample 200 is, for example, 10 0 Pa to 10 5 Pa.
  • the sample 200 near the pressure of when irradiating an electron beam 112 to the sample 200 is a 10 0 Pa ⁇ 10 4 Pa.
  • the moisture is relatively easy to evaporate.
  • the sample 200 contains moisture and it is not desirable to evaporate the moisture in the sample chamber 120, it is desirable to subject the sample 200 to a treatment that does not cause significant denaturation or deformation even when placed in a vacuum environment. For example, after a tissue section or a cell is attached to a supporting substrate such as a slide glass and dried, the sample 200 is introduced into the sample chamber 120.
  • the electron beam irradiation apparatus 100 desorbs the component 201 from the sample 200 by irradiating the electron beam 112 after introducing the gas 133 into the sample chamber 120. Further, the component 201 is recovered from the gas suction port 132 by the gas flow of the gas 133. By using the electron beam 112, the component 201 in a minute region on the sample 200 can be desorbed. Further, since the minute component 201 can be efficiently recovered by the gas flow of the gas 133, an analysis process such as mass spectrometry can be performed on the component 201 in the minute region of the sample 200.
  • FIG. 5 is a block diagram of an electron beam irradiation apparatus 100 according to a second embodiment of the present invention.
  • the partition wall 121 is disposed between the vicinity of the emission port 111 and the sample chamber 120.
  • the other configuration is the same as that of the first embodiment, so the difference will be mainly described below.
  • the component 201 is recovered using the air flow generated by sucking the gas 133 from the gas suction port 132.
  • the pressure in the sample chamber 120 needs to be higher than the vacuum.
  • the partition wall 121 for dividing the air pressure is disposed between the emission port 111 and the sample chamber 120. While the air pressure in the space on the side of the emission port 111 sandwiching the partition wall 121 is a vacuum, the air pressure in the vicinity of the sample 200 in the sample chamber 120 is set to a pressure at which a gas flow of the gas 133 is generated.
  • the partition wall 121 may be a film that transmits the electron beam 112, or may have a small hole that allows the electron beam 112 to pass through.
  • a thin film of silicon nitride which transmits an electron beam can be used.
  • FIG. 6 is a block diagram of an electron beam irradiation apparatus 100 according to a third embodiment of the present invention.
  • the gas suction port 132 has the trap portion 160 described in FIG.
  • the other configuration is the same as that of any one of the first and second embodiments, so the difference will be mainly described below.
  • the structure which provided the trap part 160 was shown.
  • the trap unit 160 is configured to be attachable to and detachable from the electron beam irradiation apparatus 100.
  • the user can store the trap portion 160 after the trap portion 160 captures the component 201.
  • the trap part 160 removed from the electron beam irradiation apparatus 100 can be conveyed to an analyzer, and the component 201 can be analyzed using this.
  • the component 201 adsorbed by the trap portion 160 is dissolved in a solution, and mass analysis of the component 201 is performed by a liquid chromatography analyzer.
  • the trap part 160 is arrange
  • the analyzer may be directly connected to the outside of the gas suction port 132, and the analyzer itself may be provided with the trap portion 160.
  • FIG. 7 shows a configuration example in which the analyzer 300 is directly connected to the gas suction port 132.
  • the analyzer 300 may receive the mixed gas of the gas 133 and the component 201 and analyze it in the gas state, or the trap portion 160 may be arranged in the analyzer 300 to analyze the trapped component 201. You may
  • FIG. 8 is a flow chart for explaining the procedure of analyzing the sample 200 using the electron beam irradiation apparatus 100 according to the present invention.
  • the component 201 is adsorbed to the trap unit 160 described in the third embodiment and the component 201 is analyzed by a mass spectrometer is shown.
  • the trap unit 160 is a solid phase column.
  • the electron beam irradiation apparatus 100 has a function as a scanning electron microscope (SEM). Each step of FIG. 8 will be described below.
  • Step S801 The user prepares the sample 200 in a form capable of irradiating the electron beam 112.
  • the preparation of the sample 200 may vary depending on the type of the sample 200, the type of the electron beam irradiation apparatus, and the like, but can be prepared by a conventional method in the art.
  • sample preparation cells, tissue sections and the like are adopted as the sample 200 and mounted on a slide glass.
  • Step S802 The user places the sample 200 on the sample stage 140 and acquires an SEM image of the sample 200 using the electron beam irradiation apparatus 100.
  • the electron beam irradiation apparatus 100 irradiates the sample 200 with the electron beam 112 without introducing the gas 133 into the sample chamber 120, and the electron beam detector 153 detects the generated electrons.
  • the intensity of the electron beam 112 is set to a degree suitable for SEM observation.
  • the arithmetic unit provided in the electron beam irradiation apparatus 100 generates a SEM image using the detection signal.
  • the air pressure in the sample chamber 120 may be atmospheric pressure or may be vacuumed to reduce the scattering of the electron beam 112 by the gas to obtain a clear SEM image.
  • Step S803 The user designates an area to be analyzed on the SEM image. For example, a specific site of a cell sample is designated.
  • Step S804 The user instructs the electron beam irradiation apparatus 100 to detach the designated area of the sample 200.
  • the electron beam irradiation apparatus 100 introduces a gas into the sample chamber 120 from the gas inlet 131 and sucks the gas from the gas suction port 132 to the outside of the sample chamber 120 to generate an air flow in the sample chamber 120.
  • the electron beam irradiation apparatus 100 moves the sample stage 140 so that the electron beam 112 is irradiated to the region designated in step S 803, and then irradiates the electron beam 112.
  • the strength of the electron beam 112 is such that the component 201 can be desorbed. As a result, the component 201 is desorbed from the designated region, and is adsorbed to the carrier in the trap portion 160.
  • Step S805 to S807 The user removes the trap portion 160 (solid phase column) (step S805) and elutes the component 201 adsorbed on the carrier in the column from the column by injecting a solvent such as methanol into the solid phase column (step S805) S806).
  • Step S805 Supplement
  • the electron beam irradiation apparatus 100 combines and displays the position of the selected region on the SEM image and the mass spectrometry data. Data transmission and reception between the electron beam irradiator 100 and the mass spectrometer are performed via an appropriate interface. In the case where there are a plurality of analysis areas, the mapping images of the specific component substances are displayed together. Furthermore, based on mass spectrometry data, area images of degree classification such as quantitative values and ratios of a plurality of substances are displayed together.
  • FIG. 9 is a conceptual diagram for explaining each step of FIG.
  • step S801 the user places a cell sample on a slide glass.
  • step S803 the user designates one or more analysis regions on the SEM image.
  • step S808 the electron beam irradiation apparatus 100 displays each image illustrated in FIG.
  • the present invention is not limited to the embodiments described above, but includes various modifications.
  • the above-described embodiments are described in detail in order to explain the present invention in an easy-to-understand manner, and are not necessarily limited to those having all the described configurations. Further, part of the configuration of one embodiment can be replaced with the configuration of another embodiment, and the configuration of another embodiment can be added to the configuration of one embodiment. Moreover, it is possible to add, delete, and replace other configurations for part of the configurations of the respective embodiments.
  • the following can be considered as a second principle for removing the component 201 from the sample 200.
  • the irradiated part When the electron beam 112 is irradiated to the sample 200, the irradiated part generates heat. If the thermal energy generated upon irradiation with the electron beam 112 is sufficiently larger than the binding energy of the component 201 in the sample 200, the component 201 evaporates or volatilizes from the sample 200, whereby the component 201 can be removed.
  • the following can be considered as a third principle for removing the component 201 from the sample 200.
  • a chemical reaction between the gas in the vicinity of the sample 200 and the sample 200 converts the gas into a substance which is easily desorbed.
  • H 2 O, H 2 or O 2 is present in the gas near the sample 200 and the sample 200 is a carbon material such as an organic substance.
  • the irradiation energy when the electron beam 112 is irradiated to the sample 200 can accelerate the reaction between the sample 200 and the gas in the vicinity of the sample 200, and the component 201 can be desorbed.
  • the following can be considered as the fourth principle for removing the component 201 from the sample 200.
  • a known second substance different from the sample 200 is mixed in advance in the vicinity of the sample 200, and when the second substance is desorbed from the sample 200, the sample 200 is also desorbed simultaneously by using the desorbed energy.
  • the sample 200 since the melting point or the boiling point of the component 201 is high, the sample 200 may not be able to be released by the second principle.
  • a second substance having a relatively low melting point or boiling point is interposed in the vicinity of the sample 200.
  • the second substance is irradiated with the electron beam 112
  • the second substance is desorbed according to the second principle.
  • the sample 200 can also be desorbed simultaneously.
  • the second substance that tends to be charged is mixed in advance in the vicinity of the sample 200, and the sample 200 is desorbed according to the principle described in the first embodiment, or the second substance that is chemically reactive is mixed in the vicinity of the sample 200 in advance. Let me do it. Thereby, the sample 200 can be desorbed when the second substance is desorbed using the third principle.
  • the example in which the electron beam irradiation apparatus 100 is configured as a scanning electron microscope has been described.
  • the same effect can also be exhibited by applying the present invention to other electron beam irradiation devices.
  • Electron beam detector 160 Trap portion 200: Sample 201: Component 300: Analyzer

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Electron Tubes For Measurement (AREA)

Abstract

Le but de la présente invention est de fournir un dispositif d'irradiation par faisceau d'électrons apte à collecter efficacement un composant ayant été retiré d'un échantillon en réponse à l'irradiation d'un faisceau d'électrons sur l'échantillon et grâce auquel le composant peut être fourni pour une analyse de masse. Ledit dispositif d'irradiation par faisceau d'électrons collecte un composant d'échantillon retiré d'un échantillon par la création d'un écoulement de gaz dans une chambre d'échantillon (voir FIG. 4).
PCT/JP2018/021484 2017-12-13 2018-06-05 Dispositif d'irradiation par faisceau d'électrons et système d'analyse WO2019116605A1 (fr)

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JP2017-238708 2017-12-13
JP2017238708A JP2021055996A (ja) 2017-12-13 2017-12-13 電子線照射装置、分析システム

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5713660A (en) * 1980-06-27 1982-01-23 Nippon Steel Corp Method of analysing solid local gas and its device
JPH06318446A (ja) * 1993-05-07 1994-11-15 Hitachi Ltd 分析方法および装置
JPH0963525A (ja) * 1995-08-22 1997-03-07 Nikon Corp 走査型電子顕微鏡
JPH0996614A (ja) * 1995-09-29 1997-04-08 Advantest Corp 微小領域の表面不純物の分析方法およびこの方法を実施する装置
JP2004226336A (ja) * 2003-01-27 2004-08-12 Hitachi Plant Eng & Constr Co Ltd 揮発有機物の測定方法および測定用サンプリング器具
WO2013129143A1 (fr) * 2012-02-27 2013-09-06 株式会社日立ハイテクノロジーズ Dispositif à faisceau de particules chargées

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5713660A (en) * 1980-06-27 1982-01-23 Nippon Steel Corp Method of analysing solid local gas and its device
JPH06318446A (ja) * 1993-05-07 1994-11-15 Hitachi Ltd 分析方法および装置
JPH0963525A (ja) * 1995-08-22 1997-03-07 Nikon Corp 走査型電子顕微鏡
JPH0996614A (ja) * 1995-09-29 1997-04-08 Advantest Corp 微小領域の表面不純物の分析方法およびこの方法を実施する装置
JP2004226336A (ja) * 2003-01-27 2004-08-12 Hitachi Plant Eng & Constr Co Ltd 揮発有機物の測定方法および測定用サンプリング器具
WO2013129143A1 (fr) * 2012-02-27 2013-09-06 株式会社日立ハイテクノロジーズ Dispositif à faisceau de particules chargées

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JUN-ICHI NIITSUMA ET AL.: "Nanoprocessing of Diamond Using a Variable Pressure Scanning Electron Microscope", JPN. J. APPL. PHYS., vol. 45, no. 2, 2006, pages L71 - L73, XP001245479, DOI: doi:10.1143/JJAP.45.L71 *

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