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DE20307617U1 - Combination of devices for analyzing the real structure of solid bodies analyzes the luminescent properties of all materials with cathode luminescence and scanning electron microscopes. - Google Patents

Combination of devices for analyzing the real structure of solid bodies analyzes the luminescent properties of all materials with cathode luminescence and scanning electron microscopes.

Info

Publication number
DE20307617U1
DE20307617U1 DE20307617U DE20307617U DE20307617U1 DE 20307617 U1 DE20307617 U1 DE 20307617U1 DE 20307617 U DE20307617 U DE 20307617U DE 20307617 U DE20307617 U DE 20307617U DE 20307617 U1 DE20307617 U1 DE 20307617U1
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DE
Germany
Prior art keywords
devices
scanning electron
cathode luminescence
analyzing
materials
Prior art date
Legal status (The legal status 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 status listed.)
Expired - Lifetime
Application number
DE20307617U
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German (de)
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
STONEWOOD ENTWICKLUNGS und VER
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STONEWOOD ENTWICKLUNGS und VER
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Priority to DE20307617U priority Critical patent/DE20307617U1/en
Publication of DE20307617U1 publication Critical patent/DE20307617U1/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • 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
    • H01J37/244Detectors; Associated components or circuits therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/225Investigating 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
    • G01N23/2251Investigating 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]
    • G01N23/2254Measuring cathodoluminescence
    • 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
    • H01J37/22Optical, image processing or photographic arrangements associated with the tube
    • H01J37/226Optical arrangements for illuminating the object; optical arrangements for collecting light from the object
    • H01J37/228Optical arrangements for illuminating the object; optical arrangements for collecting light from the object whereby illumination or light collection take place in the same area of the discharge
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2237/00Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
    • H01J2237/26Electron or ion microscopes
    • H01J2237/28Scanning microscopes
    • H01J2237/2803Scanning microscopes characterised by the imaging method
    • H01J2237/2808Cathodoluminescence

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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)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

Cathode luminescence and scanning electron microscopes have an adapter (5) connected to a portable spectrometer unit (PSU) (7) linked via a luminous fiber cable (LFC) (6). An electron beam (1) excites a sample piece (3) in a vacuum test chamber (2) for a cathode luminescence microscope. A lens focuses resulting luminescent radiation (4) on the LFC that passes a signal to the PSU.

Description

Stonewood Entwicklungs- und
Verwertungsgesellschaft mbH & Co.KG Rothermundstraße 9
01277 Dresden
5
Stonewood Development and
Verwertungsgesellschaft mbH & Co.KG Rothermundstrasse 9
01277 Dresden
5

Gerätekombination zur Analyse der Realstruktur von FestkörpernCombination of devices for analyzing the real structure of solids

BeschreibungDescription

Bei der Erfindung handelt es sich um eine Gerätekombination, mit deren Hilfe die Realstruktur von Festkörpern analysiert werden kann. Derartige Analysen werden u.a. im Zuge des Prozesses der Verkieselung von Holz durchgeführt, um beispielsweise den Prozeß des Entstehens von Kieselsäure im Zellenaufbau des Holzes verfolgen zu können.
Insofern ermöglicht die erfinderische Gerätekombination eine sehr effiziente Analysentechnik, die ihrerseits ein hochauflösendes, optisches Verfahren zur Unterscheidung und Identifizierung von Strukturphasen bei Festkörpern bzw. von Strukturzuständen derselben darstellt.
The invention is a combination of devices that can be used to analyze the real structure of solids. Such analyses are carried out during the process of silicification of wood, for example, in order to be able to follow the process of the formation of silica in the cell structure of the wood.
In this respect, the inventive device combination enables a very efficient analysis technique, which in turn represents a high-resolution, optical method for distinguishing and identifying structural phases in solids or structural states thereof.

Im übrigen verfügt die erfinderische Gerätekombination insofern generell über ein großes Anwendungspotential im Material- und Werkstoffsektor, als dadurch beispielsweise Reinheitsprüfungen von Werkstoffen, Nachweise von Phasenumwandlungen und Diffusionsprozessen sowie Untersuchungen von nichtkristallinen Materialien möglich werden.Furthermore, the inventive device combination generally has great application potential in the materials sector, as it enables, for example, purity tests of materials, detection of phase transformations and diffusion processes, and investigations of non-crystalline materials.

Üblicherweise findet bei derartigen Analysen - unter Verwendung diesbezüglich geeigneter Elektronen-Strahlgeräte - das Verfahren der Kathodenlumines-Usually, such analyses are carried out using suitable electron beam devices, the method of cathodoluminescence

Vr.-irvi \A Vr.-irvi \A

-2--2-

zenz Anwendung.zenz application.

Als Lumineszenz bezeichnet man bekanntlich die Emission elektromagnetischer Strahlung vom ultravioletten (UV-) über den sichtbaren (VIS-) bis zum infraroten (IR-) Spektralbereich infolge einer vorangegangenen Anregung durch Energieabsorbtion. Im Falle der Kathodenlumineszenz erfolgt die Anregung über einen Elektronenstrahl. Dadurch, daß die Mineralien und Materialien sehr unterschiedliche Lumineszenzeigenschaften aufweisen, werden die vorstehend erwähnten Untersuchungen u.a. zwecks Analyse und Charakterisierung der Zusammensetzung und Struktur mineralischer Werkstoffe durchgeführt. Vom Stande der Technik her sind ähnliche Geräte bzw. Verfahren beispielsweise aus den Erfindungsschriften DE 2944019A1 und DE 3037983A1 bekannt.Luminescence is known as the emission of electromagnetic radiation from the ultraviolet (UV) through the visible (VIS) to the infrared (IR) spectral range as a result of previous excitation by energy absorption. In the case of cathode luminescence, the excitation takes place via an electron beam. Because minerals and materials have very different luminescence properties, the above-mentioned investigations are carried out, among other things, for the purpose of analyzing and characterizing the composition and structure of mineral materials. Similar devices and methods are known from the state of the art, for example from the invention documents DE 2944019A1 and DE 3037983A1.

Ziel der Erfindung ist es nun, eine Geräteanordnung zu finden, die es gestattet,The aim of the invention is to find a device arrangement that allows

- einerseits eine schnelle Obersichtsanalyse von Proben zu gewährleisten, wodurch die Erfassung "echter" Lumineszenzfarben und damit eine optimale Kontrastierung bei der Abbildung von Phasen- und Strukturunterschieden möglich ist und - andererseits eine extrem hohe Ortsauflösung (<1&mgr;&pgr;&igr;) für Detail Untersuchungen zu erzielen; - darüber hinaus sollen Messungen in verschiedenen Wellenlängenbereichen bei unterschiedlichen Temperaturen möglich werden sowie zeitaufgelöste, die Aussagekraft der Analysenergebnisse wesentlich erhöhende Messungen möglich werden.- on the one hand, to ensure a rapid overview analysis of samples, which enables the detection of "real" luminescence colors and thus optimal contrast when imaging phase and structural differences and - on the other hand, to achieve an extremely high spatial resolution (<1μπα) for detailed investigations; - in addition, measurements in different wavelength ranges at different temperatures should be possible, as well as time-resolved measurements, which significantly increase the significance of the analysis results.

Die Aufgabe der Erfindung wird nun dadurch gelöst, daß die kommerziell verfügbare, gerätetechnische Einheit eines Kathodenlumineszenzmikroskops und dieThe object of the invention is now achieved by combining the commercially available technical unit of a cathode luminescence microscope and the

-3--3-

gerätetechnische Einheit eines Rasterelektronenmikroskops in der Weise modifiziert werden, daß eine Signalauskopplung erfolgt, so daß alsdann die Ankopplung einer einheitlichen Spektrometereinheit möglich wird.The technical unit of a scanning electron microscope can be modified in such a way that a signal is coupled out, so that the coupling of a uniform spectrometer unit is then possible.

Erfindungsgemäß ist die Spektrometereinheit transportabel gestaltet, um - wechselseitig - eine Messung in beiden Grundgeräten zu gewährleisten sowie einen kurzzeitigen Umbau der Meßplätze ohne Veränderung der Grundkonfiguration zu ermöglichen.According to the invention, the spectrometer unit is designed to be portable in order to ensure - alternately - a measurement in both basic devices and to enable a short-term conversion of the measuring stations without changing the basic configuration.

Hinsichtlich der im Detail vorzunehmenden Kombination der beiden Geräteeinheiten wurde nun gefunden, daß diese durch zusätzliche Einschaltung eines Adapters modifizierten werden, so daß über ein Lichtfaserkabel eine Signalauskopplung erfolgt, die die Ankopplung der einheitlichen Spektrometereinheit ermöglicht.With regard to the detailed combination of the two device units, it has now been found that these are modified by additionally connecting an adapter so that a signal is coupled out via an optical fiber cable, which enables the coupling of the unified spectrometer unit.

Nachstehend soll die Erfindung anhand eines Ausführungsbeispiels näher erläutert werden:The invention will be explained in more detail below using an embodiment:

Fig.l zeigt die grundsätzliche Geräteanordnung gemäß Oberbegriff des Schutzanspruches. Danach wird die in die Vakuum-Probenkammer 2 eines Kathodenlumineszenzmikroskops eingebrachte Probe 3 mittels Elektronenstrahl 1 angeregt und auf diese Weise eine Lumineszenzstahlung 4 erzeugt. Mittels einer Optik wird die Lumineszenzstrahlung 4 auf das an den Adapter 5 angeschlossene Lichtfaserkabel 6 fokussiert, welches das Signal seinerseits zur transportablen Spektrometereinheit 7 leitet.Fig. 1 shows the basic device arrangement according to the generic term of the protection claim. The sample 3 introduced into the vacuum sample chamber 2 of a cathode luminescence microscope is then excited by means of an electron beam 1 and in this way a luminescence radiation 4 is generated. The luminescence radiation 4 is focused by means of an optics onto the optical fiber cable 6 connected to the adapter 5, which in turn conducts the signal to the portable spectrometer unit 7.

Sofern nun eine Untersuchung von S1O2-Phasen mittels Kathodenlumineszenz durchgeführt wird, sind folgende unterschiedliche Herangehensweisen erforderlich, die durch die Kopplung der Geräte möglich sind:If an investigation of S1O2 phases is carried out using cathodoluminescence, the following different approaches are required, which are possible by coupling the devices:

A) Da sich die SiO2-Matrix selbst gegenüber Elektronenbeschuß sehr sensibel verhält, muß eine sofortige Messung der spektralen Kathodenlumineszenz erfolgen, um ein initiales Signal zu erhalten. Diese Messungen sind aufgrund der Handhabung an einem Kathodenlumineszenzmikroskop optimal umsetzbar.A) Since the SiO 2 matrix itself is very sensitive to electron bombardment, an immediate measurement of the spectral cathodoluminescence must be carried out in order to obtain an initial signal. These measurements can be carried out optimally due to the handling on a cathodoluminescence microscope.

B) Die Analyse von Mikroeinschlüssen in der SiOj-Matrix hingegen muß aufgrund der hohen Anforderungen an die Ortsauf lösung an einem Rasterelektronenmikroskop/Kathodenelektronenmikroskop-Gerät durchgeführt werden.B) The analysis of microinclusions in the SiO2 matrix, however, has to be carried out on a scanning electron microscope/cathode electron microscope due to the high demands on spatial resolution.

Durch Kombination beider Geräte und sukzessive Messung der Probe mit einer identischen Spektrometereinheit 7 an unterschiedlichen Geräten war die Aufgabe mit der vorgesehenen Analysentechnik überhaupt realisierbar.By combining both devices and successively measuring the sample with an identical spectrometer unit 7 on different devices, the task was actually feasible with the intended analysis technology.

&bull; ··

&bull; ··

Claims (2)

1. Gerätekombination zur Analyse der Realstruktur von Festkörpern, basierend auf der Analyse der Lumineszenzeigenschaft des jeweiligen Materials, dadurch gekennzeichnet, daß die gerätetechnische Einheit eines Kathodenlumineszenzmikroskops und die gerätetechnische Einheit eines Rasterelektronenmikroskops über einen Adapter (5) verfügt, an den eine über ein Lichtfaserkabel (6) verbundene Spektrometereinheit (7) angeschlossen ist. 1. Device combination for analyzing the real structure of solids based on the analysis of the luminescence property of the respective material, characterized in that the device unit of a cathode luminescence microscope and the device unit of a scanning electron microscope have an adapter ( 5 ) to which a spectrometer unit ( 7 ) connected via an optical fiber cable ( 6 ) is connected. 2. Gerätekombination nach Anspruch 1, dadurch gekennzeichnet, daß die Spektrometereinheit (7) transportabel gestaltet ist. 2. Device combination according to claim 1, characterized in that the spectrometer unit ( 7 ) is designed to be transportable.
DE20307617U 2003-05-16 2003-05-16 Combination of devices for analyzing the real structure of solid bodies analyzes the luminescent properties of all materials with cathode luminescence and scanning electron microscopes. Expired - Lifetime DE20307617U1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008138976A1 (en) * 2007-05-15 2008-11-20 Friedrich-Alexander-Universität Erlangen-Nürnberg Object imaging method and system
US8674320B2 (en) 2010-10-01 2014-03-18 Attolight Sa Deconvolution of time-gated cathodoluminescence images
DE102013209104A1 (en) * 2013-05-16 2014-11-20 Carl Zeiss Microscopy Gmbh Apparatus and method for spectroscopic analysis

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008138976A1 (en) * 2007-05-15 2008-11-20 Friedrich-Alexander-Universität Erlangen-Nürnberg Object imaging method and system
US8674320B2 (en) 2010-10-01 2014-03-18 Attolight Sa Deconvolution of time-gated cathodoluminescence images
DE102013209104A1 (en) * 2013-05-16 2014-11-20 Carl Zeiss Microscopy Gmbh Apparatus and method for spectroscopic analysis
EP2818853A1 (en) * 2013-05-16 2014-12-31 Carl Zeiss Microscopy GmbH Device and method for spectroscopic analysis
US9927361B2 (en) 2013-05-16 2018-03-27 Carl Zeiss Microscopy Gmbh Devices and methods for spectroscopic analysis
US10436712B2 (en) 2013-05-16 2019-10-08 Carl Zeiss Microscopy Gmbh Devices and methods for spectroscopic analysis

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