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EP0475098B1 - Microscope à rayons X - Google Patents

Microscope à rayons X Download PDF

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Publication number
EP0475098B1
EP0475098B1 EP91113635A EP91113635A EP0475098B1 EP 0475098 B1 EP0475098 B1 EP 0475098B1 EP 91113635 A EP91113635 A EP 91113635A EP 91113635 A EP91113635 A EP 91113635A EP 0475098 B1 EP0475098 B1 EP 0475098B1
Authority
EP
European Patent Office
Prior art keywords
ray
microscope
radiation
source
specimen
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
EP91113635A
Other languages
German (de)
English (en)
Other versions
EP0475098A2 (fr
EP0475098A3 (en
Inventor
Jürgen Dr. Thieme
Günter Prof. Dr. Schmahl
Bastian Dr. Nieman
Dietbert Dr. Rudolph
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.)
Carl Zeiss SMT GmbH
Carl Zeiss AG
Original Assignee
Carl Zeiss SMT GmbH
Carl Zeiss AG
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 Carl Zeiss SMT GmbH, Carl Zeiss AG filed Critical Carl Zeiss SMT GmbH
Publication of EP0475098A2 publication Critical patent/EP0475098A2/fr
Publication of EP0475098A3 publication Critical patent/EP0475098A3/de
Application granted granted Critical
Publication of EP0475098B1 publication Critical patent/EP0475098B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
    • G21K7/00—Gamma- or X-ray microscopes

Definitions

  • X-ray microscopes which differ in their optical structure with respect to the beam source used, the optics for focusing the X-ray beam on the object to be examined and those for imaging the object on the imaging X-ray detector used to a greater or lesser extent.
  • X-ray microscopes have been described in which mirror optics are used to image the object on the detector, for example Wolter optics that image the object with grazing incidence of the X-rays.
  • the quality of the microscopic image generated with such microscopes is not particularly good, since the mirror optics are sometimes subject to considerable image errors.
  • image errors - in the case of mirror optics that work with grazing incidence this is, for example, the so-called angular tangent error - limit the resolution of the optics aperture, which is possible in principle and which can be achieved with the microscope.
  • zone plates are used both for focusing the X-ray radiation on the object and for imaging the object on the detector. Similar to very thin lenses, these zone plates enable a largely image-free and thus high-resolution image of the object. However, they have a significantly poorer efficiency than mirror optics. In practice, it is between 5% and 15%, i.e. only a maximum of 15% of the X-rays incident on the zone plate are used for the imaging.
  • zone plate used as a condenser not only serves to focus the X-ray radiation on the object, but also acts as a monochromator and separates the monochromatic radiation required for high-resolution imaging from the more or less extensive wavelength range emitted by the X-ray source. This is done simply by means of a suitable pinhole on the optical axis, which has the effect that only one of the monochromatic images resulting from the wavelength dependence of the focal length of the zone plate on the optical axis passes through the diaphragm.
  • the X-ray microscope described is relatively weak due to the use of zone plates with the mentioned low efficiency, so that long exposure times result, which e.g. can cause motion blur during exposure when recording live cells.
  • One is therefore dependent on X-ray sources that are as intensive as possible.
  • synchrotron radiation from electron storage rings is used almost exclusively for X-ray microscopy.
  • this has the disadvantage that the X-ray microscope is not self-sufficient, i.e. the user is bound to one of the few electron storage rings in terms of space and the measurement time available to him.
  • the so-called plasma focus source is also known as the X-ray source.
  • X-ray sources for example described in DE-OS 33 32 711, give X-rays do not emit continuously, but instead deliver individual short X-ray pulses, which are followed by a relatively long dead time, during which the capacitors of the X-ray source have to be recharged. In many cases, the X-ray energy contained in a pulse is not sufficient.
  • WO 87/00644 describes an arrangement for X-ray lithography in which the X-ray tube is imaged on a zone plate by means of a mirror condenser. At the same time, the zone plate shows the lithography mask arranged behind the mirror condenser in the beam path on the target in a reduced size.
  • the intensity of the X-rays emitted by conventional X-ray tubes is far too low for such tubes to be used in X-ray microscopes.
  • the broad radiation spectrum of the X-ray tube together with the wavelength-dependent focal length of the zone plate leads to a low signal / noise ratio in the target plane, which at least cannot be accepted in X-ray microscopy.
  • the post-published EP-A2 0 459 833 describes an X-ray microscope which has a laser plasma source for generating the X-rays, a multi-layered mirror condenser for imaging the X-ray source on the object and a zone plate for enlarged imaging of the object.
  • An X-ray film is provided as the X-ray detector.
  • the available X-ray energy is optimally used.
  • the use of mirror optics on the illumination side does not have a disadvantage, since the image errors of the mirror condenser are significantly less critical when illuminated than on the imaging side of the microscope.
  • 20 to 30 times the light gain is achieved compared to a zone plate on the lighting side
  • the mirror condenser cannot be used as a monochromator, this is also not necessary since X-ray sources such as the plasma focus already provide a sufficiently intense monochromatic line radiation.
  • the zone plate with its excellent imaging properties can be retained on the imaging side.
  • the mirror condenser can be a segment of an ellipsoid that focuses the X-ray radiation on the object with grazing incidence. It is expedient if the mirror condenser is coated with a multilayer to increase the reflectivity. As a result, the efficiency of the microscope can be further improved.
  • the zone plate used for imaging the object on the detector is expediently a phase zone plate which has a higher efficiency than an amplitude zone plate.
  • the condenser images the X-ray source directly onto the object in the manner of the so-called “critical lighting”.
  • critical lighting which is usually used in microscopy
  • the mirror condenser is replaced by one or several foils are protected, through which the X-ray beam passes.
  • the sensitive mirror surfaces can be shielded against dust and dirt from the environment, possibly also against vapors from the plasma focus source, which would otherwise be deposited on the optical surfaces of the condenser and reduce its efficiency.
  • Either a photo plate or an X-ray sensitive CCD camera can be used as the detector.
  • An image memory is expediently connected downstream of the camera, into which the images of the objects to be examined, each generated with an X-ray pulse, are then read and further processed, for example, using the known methods of image processing.
  • the x-ray source (1) denotes the x-ray source.
  • This x-ray source is a plasma focus source of the type as described in DE-OS 33 32 711.
  • This plasma focus source briefly provides a point-shaped plasma which emits X-rays with a dominant emission wavelength on the Lyman- ⁇ line of the six-fold ionized nitrogen.
  • the plasma focus source (1) is operated with a capacitor bank (2) which is electrically charged in the period between the discharges.
  • the X-ray radiation emanating from the plasma focus (1a) is applied to the one by means of a mirror condenser (3) Slide (4) focused object.
  • the mirror condenser (3) has the shape of an ellipsoid of revolution and reflects the X-rays striking its mirror surfaces under grazing incidence.
  • the mirror condenser (3) is closed at both ends by a film (15) and (16), which protects the sensitive mirror surfaces against dirt.
  • the foils are made of a material that is as weakly absorbent as possible in the spectral range of the X-rays, such as polyimide.
  • micro zone plate (5) is arranged above the object level.
  • This micro zone plate represents the actual imaging optics of the X-ray microscope. Its distance from the object plane is greatly exaggerated in the representation. In fact, the micro zone plate has a diameter of about 20 - 50 ⁇ m and is only a few tenths of a mm above the object to be examined.
  • the microzone plate (5) images the object in a greatly enlarged manner on a detector (6).
  • the detector (6) is a solid-state camera, as can be obtained, for example, from Valvo under the name NXA 1011, and is sensitized to X-rays by removing the cover glass and the photosensitive surface with a fluorescent dye, e.g. Gd2O2S: Tb was occupied.
  • the CCD camera (6) is attached to a carrier (7) which, as indicated by the arrow, can be moved along the optical axis with the aid of an adjusting device (8) for the purpose of focusing.
  • the components of the X-ray microscope described above are located in a cylindrical column (9) which is built onto the capacitor bank (2) and is under a vacuum or is filled with a gas such as helium or hydrogen which is only weakly absorbent in the area of the X-ray radiation used.
  • the signal lines of the CCD camera (6) are passed through the setting device (8) and connected to an electronic unit (10) which ensures that the image is read out from the CCD camera (6).
  • This camera electronics (10) is synchronized via a control unit (11) with the electronics (not shown) for the operation of the plasma focus source in such a way that after each x-ray pulse emitted by the plasma focus source (1) an image is drawn in and stored in an image memory (13) .
  • the images stored there can then be viewed using a monitor (12) which is also connected to the electronic unit (10).

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Transforming Light Signals Into Electric Signals (AREA)
  • Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
  • Liquid Crystal Substances (AREA)

Claims (11)

  1. Microscope à rayons X comprenant
    - une source de rayons X pulsée (1) émettant un rayonnement à spectre de raie intense à une longueur d'onde dominante,
    - un condenseur à miroirs (3) focalisant le rayonnement émis par la source de rayons X (1) sur l'objet à explorer (4),
    - et une optique à rayons X constituée par une lentille zonée (5) reproduisant l'objet (4) à plus grande échelle et avec une résolution élevée sur un détecteur de rayons X (6), où le détecteur est une caméra à semiconducteurs.
  2. Microscope à rayons X selon la revendication 1, où la surface réfléchissante du condenseur à miroirs (3) est dotée d'un revêtement multicouches qui en accroît le pouvoir réfléchissant.
  3. Microscope à rayons X selon la revendication 1, où le condenseur à miroirs (3) focalise les rayons X par incidence rasante.
  4. Microscope à rayons X selon la revendication 3, où le condenseur à miroirs (3) a la forme d'un segment d'ellipsoïde.
  5. Microscope à rayons X selon la revendication 1, où la source de rayons X (1) est constituée par une source à foyer plasma.
  6. Microscope à rayons X selon la revendication 1, où la lentille zonée (5) est une lentille zonée à effet de déphasage.
  7. Microscope à rayons X selon la revendication 1, où le condenseur à miroirs (3) est protégé par des feuilles (15, 16) laissant passer les rayons X.
  8. Microscope à rayons X selon la revendication 1, où le condenseur à miroirs (3) reproduit la source de rayons X (1a) directement sur l'objet (4).
  9. Microscope à rayons X selon la revendication 1, où une électronique (11) est prévue qui synchronise le détecteur (6) avec la source de rayons X pulsée (1), de manière à ce qu'une image captée par le détecteur soit enregistrée respectivement après chaque impulsion de rayons X.
  10. Procédé servant à générer des images microscopiques de haute résolution avec des rayons X, où
    - le rayonnement d'une source de rayons X pulsée est focalisé sur l'objet à l'aide d'un condenseur à miroirs,
    - une image de l'objet est produite respectivement à chaque déclenchement d'une impulsion de rayons X,
    - l'image de la caméra, sur laquelle la lentille zonée reproduit l'objet microscopique examiné, est enregistrée respectivement à la suite d'une impulsion de rayons X, en synchronisation avec la source de rayons X pulsée.
EP91113635A 1990-08-29 1991-08-14 Microscope à rayons X Expired - Lifetime EP0475098B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4027285 1990-08-29
DE4027285A DE4027285A1 (de) 1990-08-29 1990-08-29 Roentgenmikroskop

Publications (3)

Publication Number Publication Date
EP0475098A2 EP0475098A2 (fr) 1992-03-18
EP0475098A3 EP0475098A3 (en) 1992-07-22
EP0475098B1 true EP0475098B1 (fr) 1996-02-07

Family

ID=6413137

Family Applications (1)

Application Number Title Priority Date Filing Date
EP91113635A Expired - Lifetime EP0475098B1 (fr) 1990-08-29 1991-08-14 Microscope à rayons X

Country Status (5)

Country Link
US (1) US5222113A (fr)
EP (1) EP0475098B1 (fr)
JP (1) JP3133103B2 (fr)
AT (1) ATE134065T1 (fr)
DE (2) DE4027285A1 (fr)

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US5528646A (en) * 1992-08-27 1996-06-18 Olympus Optical Co., Ltd. Sample vessel for X-ray microscopes
JP3703483B2 (ja) * 1993-09-15 2005-10-05 カール−ツァイス−スチフツング 位相コントラスト−ｘ線顕微鏡
US6091796A (en) * 1994-11-23 2000-07-18 Thermotrex Corporation Scintillator based microscope
US5965065A (en) * 1994-12-05 1999-10-12 Powell; Stephen Forbes Method of filtering x-rays
JP3069131B2 (ja) * 1996-01-10 2000-07-24 ニーマン、バスチアン Ｘ線ビーム用のコンデンサモノクロメータ装置
DE19700880A1 (de) * 1996-01-12 1997-07-17 Bastian Dr Niemann Röntgenmikroskop mit Zonenplatten
CN1175430C (zh) * 1997-04-08 2004-11-10 Xrt有限公司 极细小物体的高分辨率x射线成像
GB9815968D0 (en) 1998-07-23 1998-09-23 Bede Scient Instr Ltd X-ray focusing apparatus
DE19956782C2 (de) * 1999-11-25 2001-11-15 Lutz Kipp Optisches Fokussierelement, Meßsystem und Apparatur mit einem solchen optischen Element und Verwendung desselben
EP1126477A3 (fr) * 2000-02-14 2003-06-18 Leica Microsystems Lithography GmbH Procédé d'examen de structures dans un substrat sémiconducteur
US6195272B1 (en) 2000-03-16 2001-02-27 Joseph E. Pascente Pulsed high voltage power supply radiography system having a one to one correspondence between low voltage input pulses and high voltage output pulses
JP4220170B2 (ja) * 2002-03-22 2009-02-04 浜松ホトニクス株式会社 Ｘ線像拡大装置
EP1446813B1 (fr) * 2002-05-10 2010-11-10 Carl Zeiss SMT AG Microscope aux rayons x reflechissant concus pour examiner des objets presentant des longueurs d' en reflexion
US7245696B2 (en) * 2002-05-29 2007-07-17 Xradia, Inc. Element-specific X-ray fluorescence microscope and method of operation
AU2003256831A1 (en) * 2002-08-02 2004-02-23 X-Ray Optical Systems, Inc. An optical device for directing x-rays having a plurality of optical crystals
US7365909B2 (en) * 2002-10-17 2008-04-29 Xradia, Inc. Fabrication methods for micro compounds optics
US7072442B1 (en) * 2002-11-20 2006-07-04 Kla-Tencor Technologies Corporation X-ray metrology using a transmissive x-ray optical element
DE10254026C5 (de) * 2002-11-20 2009-01-29 Incoatec Gmbh Reflektor für Röntgenstrahlung
US7119953B2 (en) * 2002-12-27 2006-10-10 Xradia, Inc. Phase contrast microscope for short wavelength radiation and imaging method
DE10319269A1 (de) * 2003-04-25 2004-11-25 Carl Zeiss Sms Gmbh Abbildungssystem für ein, auf extrem ultravioletter (EUV) Strahlung basierendem Mikroskop
DE10334169A1 (de) 2003-07-26 2005-02-24 Bruker Axs Gmbh Gekapselter Röntgenspiegel
US7170969B1 (en) * 2003-11-07 2007-01-30 Xradia, Inc. X-ray microscope capillary condenser system
US20050211910A1 (en) * 2004-03-29 2005-09-29 Jmar Research, Inc. Morphology and Spectroscopy of Nanoscale Regions using X-Rays Generated by Laser Produced Plasma
US7302043B2 (en) * 2004-07-27 2007-11-27 Gatan, Inc. Rotating shutter for laser-produced plasma debris mitigation
US7452820B2 (en) * 2004-08-05 2008-11-18 Gatan, Inc. Radiation-resistant zone plates and method of manufacturing thereof
US7466796B2 (en) * 2004-08-05 2008-12-16 Gatan, Inc. Condenser zone plate illumination for point X-ray sources
US7231017B2 (en) * 2005-07-27 2007-06-12 Physical Optics Corporation Lobster eye X-ray imaging system and method of fabrication thereof
CN101356589B (zh) 2005-08-01 2013-02-27 纽约州立大学研究基金会 采用点聚焦、弯曲单色光学器件的x射线成像系统
US20070108387A1 (en) * 2005-11-14 2007-05-17 Xradia, Inc. Tunable x-ray fluorescence imager for multi-element analysis
DE102005056404B4 (de) * 2005-11-23 2013-04-25 Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh Röntgenmikroskop mit Kondensor-Monochromator-Anordnung hoher spektraler Auflösung
US7499521B2 (en) * 2007-01-04 2009-03-03 Xradia, Inc. System and method for fuel cell material x-ray analysis
DE102007041939A1 (de) * 2007-09-04 2009-03-05 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Vorrichtung und Verfahren für die XUV-Mikroskopie
US9291578B2 (en) 2012-08-03 2016-03-22 David L. Adler X-ray photoemission microscope for integrated devices
US9129715B2 (en) 2012-09-05 2015-09-08 SVXR, Inc. High speed x-ray inspection microscope
US20160086681A1 (en) * 2014-09-24 2016-03-24 Carl Zeiss X-ray Microscopy, Inc. Zone Plate and Method for Fabricating Same Using Conformal Coating
DE102020207795A1 (de) 2019-06-24 2020-12-24 Ims Messsysteme Gmbh Vorrichtung und Verfahren zum Bestimmen der Werkstoffeigenschaften eines polykristallinen Produkts
DE102019124919B4 (de) * 2019-09-17 2021-08-26 Ri Research Instruments Gmbh Mikroskopisches System zur Prüfung von Strukturen und Defekten auf EUV-Lithographie-Photomasken
JP7572033B2 (ja) * 2020-10-23 2024-10-23 株式会社リガク 結像型ｘ線顕微鏡

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JP2921038B2 (ja) * 1990-06-01 1999-07-19 キヤノン株式会社 Ｘ線を用いた観察装置

Also Published As

Publication number Publication date
ATE134065T1 (de) 1996-02-15
JPH04262300A (ja) 1992-09-17
JP3133103B2 (ja) 2001-02-05
DE59107380D1 (de) 1996-03-21
EP0475098A2 (fr) 1992-03-18
US5222113A (en) 1993-06-22
EP0475098A3 (en) 1992-07-22
DE4027285A1 (de) 1992-03-05

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