WO2008060237A1 - Appareil électronique de prise de vues par rotation - Google Patents

Appareil électronique de prise de vues par rotation Download PDF

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Publication number
WO2008060237A1
WO2008060237A1 PCT/SE2007/050853 SE2007050853W WO2008060237A1 WO 2008060237 A1 WO2008060237 A1 WO 2008060237A1 SE 2007050853 W SE2007050853 W SE 2007050853W WO 2008060237 A1 WO2008060237 A1 WO 2008060237A1
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WO
WIPO (PCT)
Prior art keywords
patterns
related technique
rotation
electron
specific
Prior art date
Application number
PCT/SE2007/050853
Other languages
English (en)
Inventor
Sven HOVMÖLLER
Original Assignee
Hovmoeller Sven
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 Hovmoeller Sven filed Critical Hovmoeller Sven
Publication of WO2008060237A1 publication Critical patent/WO2008060237A1/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
    • G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • 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
    • H01J37/147—Arrangements for directing or deflecting the discharge along a desired path
    • H01J37/1478—Beam tilting means, i.e. for stereoscopy or for beam channelling
    • 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
    • H01J37/252—Tubes for spot-analysing by electron or ion beams; Microanalysers
    • H01J37/256—Tubes for spot-analysing by electron or ion beams; Microanalysers using scanning beams
    • 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
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H01J37/295—Electron or ion diffraction tubes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/15—Means for deflecting or directing discharge
    • H01J2237/1505—Rotating beam around optical axis
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/15—Means for deflecting or directing discharge
    • H01J2237/1506—Tilting or rocking beam around an axis substantially at an angle to optical axis
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/25—Tubes for localised analysis using electron or ion beams

Definitions

  • Electron diffraction 0 In many modern industrial applications it is necessary to be able to study samples in the nanometer scale. Such specimens may contain from 1 to 10 000 atoms. The only way to study such minute samples is by electrons, which interact about a million times stronger with matter. However, in the traditional mode of electron diffraction, SAED, both the electron beam and crystal are fixed, thereby5 limiting the amount of data that is recorded in any one image. In order to collect a 3D data set, it is necessary to collect a large number of diffraction patterns at different angles (see Figure 1).
  • fig. 1 there is disclosed an example of a collection of electron diffraction patterns from many directions on the same crystal. Each diffraction pattern is in ⁇ fact a section through 3D space, as illustrated by the set of five lines at the bottom left of fig, 1.
  • Electron precession Recently Paul Midgley and Roger Vincent in Bristol, UK invented the precession method for electron diffraction. Here the electron beam is tilted by a small angle, typically 1-3 degrees, and then rotated around the optical axis. In this way a volume of reciprocal space is recorded, rather than just single sections.
  • the multiple scattering is greatly reduced, since at any one moment only a small number of reflections are excited.
  • the beam tilt is accomplished by adding small currents to the lens(es) above the sample in the electron microscope.
  • the electromagnetic coils below the sample are used to descan.
  • the precession technique has recently been improved and commercialized by NanoMEGAS, protected by several patents.
  • Electron precession solves all these problems, but one important thing remains. It is very difficult, not to say impossible to collect full 3D data with the precession geometry. There will be many partially recorded reflections at the borders of the scanned space.
  • SAED Selected Area Electron Diffraction
  • precession was a standard technique until about 1975, when the oscillation or rotation method was developed by Arndt and Wonacott in Cambridge, UK.
  • the main reason for going from precession to rotation was the simplified geometry, especially the fact that one film recorded by rotation could be directly added on to the following, allowing partially recorded reflections on one film to be filled in on the next film.
  • full high-quality electron diffraction data should also be collected by a rotation method.
  • Eiectron rotation can be achieved by a device rather simiiar to the one making electron precession.
  • the main difference is that the electron beam (and its corresponding descanning unit) should not go around in a circle, but rather follow a straight line, like a pendulum.
  • This Sine can be along the x-direction, along the y- direction or along any diagonal in between.
  • each scan may have a rotation of only +/- 0.5 degrees along a line.
  • the next scan will follow on from exactly where the previous stopped, i.e. from +0.5 to +1.5 degrees, with the next one + 1.5 to +2.5 degrees etc.
  • One such series of rotation images can total up to about 6 degrees (the exact range is limited by the design of the specific model of electron microscope).
  • the diffraction patterns may be recorded on any media, including photographic film, imaging plates or CCD cameras.
  • the device and related technique described in this Patent uses a combination of specific scanning protocol of ED intensities (including beam rotation) that can be further and simultaneously scanned across a specific nanocrystai surface observed in TEM.
  • This may require the presence of a scan generator configured to control scan coils for scanning an ED pattern, said scanning generator may exist in the TEM or can be built as external device to synchronize beam displacement over the sample with simultaneous acquisition of ED patterns.
  • a computer may collect such patterns (through the frame grabber) and store them for further on-line or off-Sine analysis.
  • Such ED patterns generated at each sample point of the nanocrystai under study may reveal crystal structure details such as crystal phase and local orientation after comparison with recalculated theoretical kinematical ED patterns of known crystal phases under different crystaSlographic orientations.
  • Such ED patterns obtained under specific scanning protocols may be useful as quasi-kinematicai ED intensity fingerprints of known phases and can be used as such for search/comparison with known crystaSiographic databases (for example ICDD, FIZ, CSD or others). Such comparison can be performed visually or by image processing techniques. Rotation, oscillation and alternative scanning protocois (inciuding but not limited to beam precession) are producing ED intensities close the their ideal kinematical values, aSiowing therefore direct comparison with simulated kinematical ED patterns of known compounds without taking in account crystal thickness effects.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Crystallography & Structural 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)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

La présente invention se rapporte à un dispositif permettant d'obtenir des séquences de diffraction d'électrons par rotation (osculation) en faisant osciller un faisceau dans les directions X, Y ou dans toute direction de l'axe du cristal, pour toute plage angulaire variable conformément à un quelconque protocole spécifique d'oscillation.
PCT/SE2007/050853 2006-11-15 2007-11-15 Appareil électronique de prise de vues par rotation WO2008060237A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US85895306P 2006-11-15 2006-11-15
US60/858,953 2006-11-15

Publications (1)

Publication Number Publication Date
WO2008060237A1 true WO2008060237A1 (fr) 2008-05-22

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/SE2007/050853 WO2008060237A1 (fr) 2006-11-15 2007-11-15 Appareil électronique de prise de vues par rotation

Country Status (1)

Country Link
WO (1) WO2008060237A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010052289A1 (fr) * 2008-11-06 2010-05-14 Nanomegas Sprl Procédés et dispositifs d’analyse à haut débit d’une structure cristalline par diffraction électronique
EP2642279A1 (fr) 2012-03-19 2013-09-25 Universidad de Barcelona Procédé et système pour améliorer les signaux de pic caractéristique dans la microscopie électronique analytique
WO2021029519A1 (fr) * 2019-08-09 2021-02-18 재단법인 포항산업과학연구원 Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4160162A (en) * 1976-11-12 1979-07-03 Siemens Aktiengesellschaft Method for the pictorial display of a diffraction image in a transmission-type, scanning, corpuscular-beam microscope
US5004918A (en) * 1989-01-25 1991-04-02 Jeol Ltd. Differential phase contrast scanning transmission electron microscope
US20030006373A1 (en) * 2001-07-05 2003-01-09 Hitachi. Ltd. Observation apparatus and observation method using an electron beam
US20040061053A1 (en) * 2001-02-28 2004-04-01 Yoshifumi Taniguchi Method and apparatus for measuring physical properties of micro region
US20040183012A1 (en) * 2003-03-18 2004-09-23 Toshie Yaguchi Material characterization system
WO2005022582A1 (fr) * 2003-09-02 2005-03-10 Nanomegas Sprl Procede de mesure de modeles de diffraction a partir d'une microscopie electronique de transmission permettant de determiner des structures cristallines et procede associe
US20060151701A1 (en) * 2005-01-12 2006-07-13 Ruriko Tsuneta Scanning transmission electron microscope and scanning transmission electron microscopy

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4160162A (en) * 1976-11-12 1979-07-03 Siemens Aktiengesellschaft Method for the pictorial display of a diffraction image in a transmission-type, scanning, corpuscular-beam microscope
US5004918A (en) * 1989-01-25 1991-04-02 Jeol Ltd. Differential phase contrast scanning transmission electron microscope
US20040061053A1 (en) * 2001-02-28 2004-04-01 Yoshifumi Taniguchi Method and apparatus for measuring physical properties of micro region
US20030006373A1 (en) * 2001-07-05 2003-01-09 Hitachi. Ltd. Observation apparatus and observation method using an electron beam
US20040183012A1 (en) * 2003-03-18 2004-09-23 Toshie Yaguchi Material characterization system
WO2005022582A1 (fr) * 2003-09-02 2005-03-10 Nanomegas Sprl Procede de mesure de modeles de diffraction a partir d'une microscopie electronique de transmission permettant de determiner des structures cristallines et procede associe
US20060151701A1 (en) * 2005-01-12 2006-07-13 Ruriko Tsuneta Scanning transmission electron microscope and scanning transmission electron microscopy

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2010052289A1 (fr) * 2008-11-06 2010-05-14 Nanomegas Sprl Procédés et dispositifs d’analyse à haut débit d’une structure cristalline par diffraction électronique
US8253099B2 (en) 2008-11-06 2012-08-28 Nanomegas Sprl Methods and devices for high throughput crystal structure analysis by electron diffraction
EP2818852A1 (fr) * 2008-11-06 2014-12-31 Nanomegas SPRL Procédés et dispositifs pour l'analyse de structure cristalline à haut rendement par la diffraction d'électrons
EP2642279A1 (fr) 2012-03-19 2013-09-25 Universidad de Barcelona Procédé et système pour améliorer les signaux de pic caractéristique dans la microscopie électronique analytique
US9406496B2 (en) 2012-03-19 2016-08-02 Universitat De Barcelona Method and system for improving characteristic peak signals in analytical electron microscopy
WO2021029519A1 (fr) * 2019-08-09 2021-02-18 재단법인 포항산업과학연구원 Appareil et procédé d'analyse de la structure cristalline d'un échantillon, et support d'enregistrement lisible par ordinateur

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