WO2013183057A1 - Système et procédé de réalisation d'analyse de matières dans un environnement non vide utilisant un microscope électronique - Google Patents

Système et procédé de réalisation d'analyse de matières dans un environnement non vide utilisant un microscope électronique Download PDF

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Publication number
WO2013183057A1
WO2013183057A1 PCT/IL2013/050489 IL2013050489W WO2013183057A1 WO 2013183057 A1 WO2013183057 A1 WO 2013183057A1 IL 2013050489 W IL2013050489 W IL 2013050489W WO 2013183057 A1 WO2013183057 A1 WO 2013183057A1
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WO
WIPO (PCT)
Prior art keywords
electron beam
scattering
vacuum environment
travel distance
electron microscope
Prior art date
Application number
PCT/IL2013/050489
Other languages
English (en)
Inventor
Dov Shachal
Rafi De Picciotto
Original Assignee
B-Nano 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 B-Nano Ltd. filed Critical B-Nano Ltd.
Priority to CN201380029748.8A priority Critical patent/CN104508460B/zh
Priority to JP2015515648A priority patent/JP6125622B2/ja
Priority to KR20147036796A priority patent/KR20150023526A/ko
Publication of WO2013183057A1 publication Critical patent/WO2013183057A1/fr

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Classifications

    • 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]
    • G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/07—Investigating materials by wave or particle radiation secondary emission
    • G01N2223/079—Investigating materials by wave or particle radiation secondary emission incident electron beam and measuring excited X-rays
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/10—Different kinds of radiation or particles
    • G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016—X-ray
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/30—Accessories, mechanical or electrical features
    • G01N2223/309—Accessories, mechanical or electrical features support of sample holder

Definitions

  • the present invention relates generally to scanning electron microscopes.
  • the present invention seeks to provide an improved scanning electron microscope.
  • a method for performing analysis of materials when present in a non- vacuum environment using an electron microscope including generating a first characteristic spectrum for a material by: directing an electron beam from the electron microscope onto the material in a first non-vacuum environment, in which a first amount of scattering of the electron beam takes place, collecting first X-rays emitted from the material and performing spectral analysis on the first X-rays, thereafter, generating a second characteristic spectrum for the material by: directing an electron beam from the electron microscope onto the material in a second non-vacuum environment, in which a second amount of scattering of the electron beam takes place, collecting second X-rays emitted from the material and performing spectral analysis on the second X-rays, comparing the first and second characteristic spectra and noting peaks whose intensity increases with increased scattering, generating a scattering- compensated characteristic spectrum for the material from at least one of the first and second characteristic spectra by eliminating
  • the scattering compensated characteristic spectrum includes at least one peak whose intensity decreases with increased scattering.
  • the first non-vacuum environment includes a first gas and the second non-vacuum environment includes a second gas, having electron beam scattering characteristics different from those of the first gas.
  • the first non-vacuum environment has a first electron beam travel distance to the material associated therewith and the second non-vacuum environment has a second electron beam travel distance to the material associated therewith, the second electron beam travel distance producing a different amount of electron beam scattering than the first electron beam travel distance.
  • a system for performing analysis of materials when present in a non-vacuum environment using an electron microscope including a characteristic spectrum generator, generating first and second characteristic spectra for a material by: directing an electron beam from the electron microscope onto the material in respective first and second non-vacuum environments, in which respective first and second amounts of scattering of the electron beam takes place, collecting X-rays emitted from the material in the first and second non-vacuum environments and performing spectral analysis on the X-rays from the material in the first and second non-vacuum environments and a scattering-compensated characteristic spectrum generator operative by: comparing the first and second characteristic spectra and noting peaks whose intensity increases with increased scattering and generating a scattering-compensated characteristic spectrum for the material from at least one of the first and second characteristic spectra by eliminating at least one peak whose intensity increases with increased scattering.
  • the scattering compensated characteristic spectrum includes least one peak whose intensity decreases with increased scattering.
  • the system for performing analysis of materials when present in a non-vacuum environment using an electron microscope also includes a gas supply controller operative to supply a first gas to the first non-vacuum environment and a second gas to the second non- vacuum environment, the second gas having electron beam scattering characteristics different from those of the first gas.
  • the system for performing analysis of materials when present in a non-vacuum environment using an electron microscope also includes a movable sample mount operative to be positioned at a first electron beam travel distance to the material in the first non- vacuum environment and to be positioned at a second electron beam travel distance to the material in the second non-vacuum environment, the second electron beam travel distance producing a different amount of electron beam scattering than the first electron beam travel distance.
  • an electron microscope-based material analysis system operative for directing an electron beam from the electron microscope onto a material in a non-vacuum environment, collecting X-rays emitted from the material and performing spectral analysis on the X-rays
  • a computerized method for performing analysis of materials when present in a non-vacuum environment using the electron microscope-based system including operating the microscope -based material analysis system for: generating a first characteristic spectrum for a material by: directing an electron beam onto a material in a first non-vacuum environment, in which a first amount of scattering of the electron beam takes place, collecting first X-rays emitted from the material and performing spectral analysis on the first X-rays, thereafter, generating a second characteristic spectrum for the material by: directing an electron beam onto a material in a second non- vacuum environment, in which a second amount of scattering of the electron beam takes place; collecting second X-rays
  • the scattering compensated characteristic spectrum includes at least one peak whose intensity decreases with increased scattering.
  • the first non-vacuum environment includes a first gas and the second non-vacuum environment includes a second gas, having electron beam scattering characteristics different from those of the first gas.
  • the first non-vacuum environment has a first electron beam travel distance to the material associated therewith and the second non-vacuum environment has a second electron beam travel distance to the material associated therewith, the second electron beam travel distance producing a different amount of electron beam scattering than the first electron beam travel distance.
  • the scattering compensated characteristic spectrum includes at least one peak whose intensity decreases with increased scattering.
  • the first non-vacuum environment includes a first gas and the second non-vacuum environment includes a second gas, having electron beam scattering characteristics different from those of the first gas.
  • the first non-vacuum environment has a first electron beam travel distance to the material associated therewith and the second non-vacuum environment has a second electron beam travel distance to the material associated therewith, the second electron beam travel distance producing a different amount of electron beam scattering than the first electron beam travel distance.
  • Fig. 1 is a simplified illustration of a system for performing analysis of materials when present in a non-vacuum environment constructed and operative in accordance with a preferred embodiment of the present invention
  • Figs. 2A and 2B are, respectively, simplified X-ray spectra obtained by directing an electron beam onto the same spot on the same sample in first and second different non-vacuum environments in which different gases are present, producing different amounts of scattering of the electron beam;
  • Fig. 2C is a scattering-compensated simplified X-ray spectrum derived from the spectra of Figs. 2A & 2B by eliminating at least one peak whose intensity increases with increased scattering;
  • Figs. 3A and 3B are respectively simplified X-ray spectra obtained by directing an electron beam onto the same spot on the same sample in first and second different non-vacuum environments in which different electron beam path lengths are present, producing different amounts of scattering of the electron beam;
  • Fig. 3C is a scattering-compensated simplified X-ray spectrum derived from the spectra of Figs. 3 A & 3B by eliminating at least one peak whose intensity increases with increased scattering.
  • the scanning electron microscope 100 includes a conventional SEM column 102, an example of which is a SEM column which forms part of a Gemini® column based SEM, commercially available from Carl Zeiss SMT GmbH, Oberkochen, Germany, having a beam aperture 104 arranged along an optical axis 106 of the SEM column 102.
  • the SEM column 102 is typically maintained under vacuum.
  • a vacuum interface 108 typically in the form of a vacuum enclosure coupled to a vacuum pump (not shown) via a conduit 109, interfaces between the interior of the SEM column 102 at the beam aperture 104 and the ambient and is formed with a vacuum retaining, beam permeable membrane 110, which is aligned with the beam aperture 104 along optical axis 106.
  • Membrane 110 is preferably a model 4104SN-BA membrane, commercially available from SPI Supplies, West Chester, PA, USA. In accordance with a preferred embodiment of the invention, the membrane 110 is not electrically grounded. It is noted that the thickness of the membrane 110 is in the nanometer range and is not shown to scale.
  • Membrane 110 is typically supported onto the vacuum interface 108 by means of a membrane holder 112, typically in the form of an apertured disc formed of an electrical conductor, such as stainless steel.
  • the membrane holder 112 sealingly underlies an electrical insulator 114, also typically in the form of an apertured disc.
  • the electrical insulator 114 is sealingly mounted onto an inner facing bottom flange portion 116 of vacuum interface 108.
  • a sample here designated by reference numeral 120, is located below and spaced from membrane 110, typically by a distance of up to 500 microns and is positioned such that an electron beam directed along optical axis 106 impinges thereon.
  • Sample 120 is preferably supported by a sample holder 122.
  • Sample holder 122 is preferably formed of an electrical conductor, such as stainless steel or aluminum, and may or may not be grounded, depending on the application.
  • sample holder 122 is supported on a movable sample mount 126, which provides movement of the sample holder in an upward-downward direction relative to SEM column 102, as shown by arrow 128. It is appreciated that movable sample mount 126 provides for multiple positioning of sample 120 relative to SEM column 102 and provides for multiple electron beam travel distances to sample 120 within the non-vacuum environment producing different amounts of electron beam scattering.
  • a gas such as helium or nitrogen
  • a gas supply controller 132 is preferably operative to select a gas for injecting from one or more of multiple gas input conduits 134, each coupled to a different gas supply (not shown). It is appreciated that different gases may provide different electron beam scattering characteristics.
  • An X-ray spectrometer 150 is operative to collect X-ray photons 152 emitted from sample 120 and generate an X-ray spectrum therefrom, which is preferably used for material analysis such as qualitative or quantitative analysis of the elements which are present in the sample 120.
  • scanning electron microscope 100 is used to generate a scattering-compensated characteristic spectrum for a material in sample 120 by comparing at least two X-ray spectra to eliminate at least one peak whose intensity increases with increased scattering.
  • a first characteristic spectrum for a material is generated by directing an electron beam from scanning electron microscope 100 along axis 106 onto a material in a first non-vacuum environment, in which a first amount of scattering of the electron beam about axis 106 takes place, collecting X-rays emitted from the material and performing spectral analysis on the X-rays.
  • a second characteristic spectrum for a material is generated by directing an electron beam from scanning electron microscope 100 along axis 106 onto a material in a second non-vacuum environment, in which a second amount of scattering of the electron beam about axis 106 takes place, collecting X-rays emitted from the material and performing spectral analysis on the X-rays.
  • the first and second spectra are then compared, noting peaks whose intensity increases with increased scattering and a scattering-compensated characteristic spectrum for the material is generated by eliminating at least one peak whose intensity increases with increased scattering.
  • the generated scattering-compensated characteristic spectrum may include at least one peak whose intensity decreases with increased scattering.
  • the first and second non-vacuum environments having different scattering characteristics include using gas supply controller 132 to introduce different gases using into the non- vacuum environment, where the different gases have different scattering characteristics.
  • the first and second non-vacuum environments having different scattering characteristics include using movable sample mount 126 to change the electron beam travel distance to the material, where the different travel distances produce different amounts of electron beam scattering.
  • the first and second non-vacuum environments having different scattering characteristics include using gas supply controller 132 to introduce different gases using into the non- vacuum environment and using movable sample mount 126 to change the electron beam travel distance to the material.
  • Figs. 2A and 2B illustrate simplified X-ray spectra obtained by directing an electron beam onto the same spot on the same sample in first and second different non-vacuum environments in which different gases are present, producing different amounts of scattering of the electron beam.
  • Fig. 2C shows a scattering-compensated simplified X-ray spectrum derived from the spectra of Figs. 2A & 2B by eliminating the peak centered at about 1.5 kEv whose intensity increases with increased scattering. As seen from a comparison of Figs.
  • the X-ray spectra also includes a peak centered at about 1.75 kEv whose intensity decreases with increased scattering, which is not eliminated in the scattering-compensated simplified X-ray spectrum shown in Fig. 2C.
  • Figs. 3A and 3B illustrate simplified X-ray spectra obtained by directing an electron beam onto the same spot on the same sample in first and second different non-vacuum environments in which different electron beam path lengths are present, producing different amounts of scattering of the electron beam.
  • Fig. 3C shows a scattering-compensated simplified X-ray spectrum derived from the spectra of Figs. 3A & 3B by eliminating a peak centered at about 1.5 kEv whose intensity increases with increased scattering. As seen from a comparison of Figs.
  • the X-ray spectra also includes a peak centered at about 1.75 kEv whose intensity decreases with increased scattering, which is not eliminated in the scattering-compensated simplified X-ray spectrum shown in Fig. 3C.

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

La présente invention porte sur un procédé de réalisation d'analyse de matières lorsqu'elles sont présentes dans un environnement non vide utilisant un microscope électronique, le procédé comprenant la génération d'un premier et d'un second spectre caractéristique pour une matière par la direction d'un faisceau électronique provenant du microscope électronique sur la matière dans des premier et second environnements non vides respectifs, dans lesquels de première et seconde quantités respectives de diffusion du faisceau électronique ont lieu, la collecte de premier et second rayons X respectifs émis par la matière et la réalisation d'une analyse spectrale sur les premier et second rayons X, la comparaison des premier et second spectres caractéristiques et l'annotation de pics dont l'intensité augmente avec une diffusion accrue, la génération d'un spectre caractéristique compensé en diffusion pour la matière à partir d'au moins l'un des premier et second spectres caractéristiques par élimination d'au moins un pic dont l'intensité augmente avec une diffusion accrue.
PCT/IL2013/050489 2012-06-05 2013-06-05 Système et procédé de réalisation d'analyse de matières dans un environnement non vide utilisant un microscope électronique WO2013183057A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201380029748.8A CN104508460B (zh) 2012-06-05 2013-06-05 使用电子显微镜对存在于非真空环境的材料进行分析的系统及方法
JP2015515648A JP6125622B2 (ja) 2012-06-05 2013-06-05 電子顕微鏡を用い非真空環境中で材料の分析を行うためのシステムおよび方法
KR20147036796A KR20150023526A (ko) 2012-06-05 2013-06-05 전자현미경을 사용하여 비진공 환경에서 재료를 분석하기 위한 시스템 및 방법

Applications Claiming Priority (2)

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US201261655567P 2012-06-05 2012-06-05
US61/655,567 2012-06-05

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WO2013183057A1 true WO2013183057A1 (fr) 2013-12-12

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US9431213B2 (en) 2008-07-03 2016-08-30 B-Nano Ltd. Scanning electron microscope, an interface and a method for observing an object within a non-vacuum environment
US9466458B2 (en) 2013-02-20 2016-10-11 B-Nano Ltd. Scanning electron microscope

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Also Published As

Publication number Publication date
JP2015520495A (ja) 2015-07-16
JP6125622B2 (ja) 2017-05-10
KR20150023526A (ko) 2015-03-05
CN104508460A (zh) 2015-04-08
CN104508460B (zh) 2017-09-12

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