EP2194375B1 - Elément optique pour rayons X et diffractomètre doté d'une fente de Soller - Google Patents

Elément optique pour rayons X et diffractomètre doté d'une fente de Soller Download PDF

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Publication number
EP2194375B1
EP2194375B1 EP09177712.8A EP09177712A EP2194375B1 EP 2194375 B1 EP2194375 B1 EP 2194375B1 EP 09177712 A EP09177712 A EP 09177712A EP 2194375 B1 EP2194375 B1 EP 2194375B1
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EP
European Patent Office
Prior art keywords
optical element
soller
ray
ray optical
soller slit
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Application number
EP09177712.8A
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German (de)
English (en)
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EP2194375A1 (fr
Inventor
Christoph Ollinger
Norbert Kuhnmünch
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Bruker AXS GmbH
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Bruker AXS GmbH
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    • 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
    • G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
    • G21K1/02—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating using diaphragms, collimators

Definitions

  • the invention relates to an X-ray optical element having a Soller aperture comprising a plurality of lamellae for collimating an X-ray beam with respect to the direction of the axis of the Soller aperture, and having a further aperture for limiting an X-ray beam, wherein the further aperture is rigidly connected to the Soller aperture during operation.
  • X-ray diffractometry can be used for a variety of analytical tasks, using different measurement geometries, e.g. Bragg-Brentano or parallel beam geometry. However, this requires different optical elements in the beam path. In order to enable a quick change between the different measuring geometries, it is desirable to keep the necessary rebuilding measures as low as possible.
  • US 6,807,251 B2 is an X-ray diffractometer with a parabolic mirror for using the diffractometer in the parallel beam geometry, and a slit diaphragm for limiting the X-ray beam in the Bragg Brentano geometry known.
  • the mirror and the slit are rigidly connected.
  • a rotatable path selection disc with a slit is disposed behind the diaphragm / mirror unit and can select by rotation the X-ray beam (parallel or divergent) required for the corresponding geometry.
  • roller blinds with which vertical and / or horizontal divergence of X-rays can be restricted is advantageous.
  • linear rollerblades are in US 6,266,392 B1 . US2005 / 0281382 A1 and US Pat. No. 6,307,917 B1 described in detail.
  • Bruker Advanced X-ray solutions "Diffraction Solutions D8 Advance" 2002 discloses an X-ray diffractometer for reflection and transmission measurements in parallel beam geometry. The X-ray emanating from the sample runs through a linear or a radial Soller aperture.
  • US Pat. No. 6,307,917 B1 discloses an X-ray apparatus with Soller aperture for collimating divergent X-rays.
  • the Soller panel is part of a monochromator unit with a monochromator panel that serves to confine the X-ray beam, which is then collimated by the Soller panel.
  • the object of the invention is to propose an X-ray optical element with a Soller aperture and another aperture, which allows automatic switching between the Soller aperture and the further aperture.
  • the X-ray bounded by the further diaphragm intersects the axis of the Soller diaphragm within the Soller diaphragm and the direction of the X-ray bounded by the further diaphragm includes an angle ⁇ ⁇ 10 ° with the axis of the Soller diaphragm.
  • An X-ray beam coming from a radiation source can thus be limited either by the Soller diaphragm or by the further diaphragm, as the case may be at which angle the soller axis is aligned with the direction of the incident x-ray beam. If the X-ray beam collapses parallel or at a small angle ( ⁇ 10 °) to the Soller axis, it passes through the Soller aperture. The greater the direction of the incident X-ray differs from the Soller axis, the more radiation passes through the further aperture.
  • the Soller diaphragm has a beam window which allows X-ray radiation to be conducted in one direction, which forms an angle ⁇ ⁇ 10 ° with the axis of the Soller diaphragm. In this way, a very compact and flexible optical element is realized.
  • the "Soller Aperture Axis” is to be understood as meaning the axis of symmetry of the Soller Aperture, which runs in the direction of the X-ray beam to be collimated by the Soller Aperture (optical axis), ie. in the case of a linear Soller panel, the Soller axis runs between an inlet opening and an outlet opening parallel to the slats of the Soller panel. In the case of a radial Soller aperture, the Soller axis extends along the mirror plane of the Soller aperture between an inlet opening and an outlet opening.
  • the optical setup of a diffractometer can be adapted to the application required by the sample or the question (for example Bragg-Brentano, powder GID, reflectometry).
  • An embodiment of the X-ray optical element according to the invention provides that the Soller aperture is a linear Soller aperture.
  • a linear roller blind includes a plurality of thin laminations (eg, metal foils) arranged parallel to each other and spaced from each other. Linear roller blinds are used in particular when using point detectors.
  • the Soller aperture is a radial Soller aperture.
  • Radial Soller covers are used in particular when using strip detectors.
  • the slats of the linear Soller diaphragm are arranged parallel to the beam direction of the X-ray bounded by the further diaphragm.
  • both the X-ray beam bounded by the further diaphragm and an X-ray beam extending in the direction of the Soller axis (in different directions) can pass through the Soller diaphragm.
  • the Soller panel has a recess perpendicular to the Soller axis.
  • the X-ray beam bounded by the further diaphragm can thus intersect the axis of the Soller diaphragm within the Soller diaphragm, irrespective of the orientation of the slats of the Soller diaphragm.
  • the Soller panel may comprise two partial panels, wherein the further panel is at least partially disposed between the two partial panels.
  • the two partial panels of the Soller panel must then be precisely adjusted.
  • the further diaphragm has at least two diaphragm jaws, wherein the diaphragm jaws are arranged on different sides of the Soller diaphragm.
  • a diaphragm jaw is arranged on the side of the Soller diaphragm, which faces the incident on the further diaphragm X-ray, and the other diaphragm jaw is arranged on the side facing away from the incident on the further diaphragm X-ray.
  • the diaphragm jaws with the axis of the Soller aperture an angle not equal to 90 °, preferably 45 °, include.
  • the further diaphragm can also be arranged completely on one side of the roller blind, in particular in one piece.
  • a pinhole can be used.
  • the further diaphragm is made of tantalum.
  • the geometry of the further diaphragm, in particular the diaphragm opening can be adjusted in the non-operating state.
  • the beam cross section of the X-ray emerging from the further diaphragm is thus well-defined.
  • a further embodiment of the X-ray optical element according to the invention provides that the further diaphragm is a linear Soller diaphragm.
  • the X-ray optical element comprises in this embodiment two Soller diaphragms whose axes are arranged at an angle ⁇ ⁇ 10 °.
  • the two Soller aperture in cross through, so that at least one of the Soller covers has a recess within which the other Soller panel is at least partially arranged.
  • the two linear roller blinds have different divergence angles, i.
  • the distances between the slats are different for the two linear roller blinds.
  • the further panel may be a radial Soller panel. This is particularly advantageous in the use of strip detectors.
  • the optical element according to the invention has two radial blind plates with different opening angles.
  • the invention also relates to a diffractometer having a source for generating a primary beam, a sample holder for arranging a sample, a detector for registering a secondary beam emanating from the sample and having an X-ray optical element described above.
  • the X-ray optical element is rotatably mounted in the diffractometer about an axis of rotation perpendicular to the axis of the Soller aperture.
  • the inlet opening of the Soller aperture can thus be driven by rotation of the beam path and at the same time the beam window of the further aperture in the beam path.
  • the incident X-ray beam does not have to be divided into two beam paths, but rather the X-ray optical element can be aligned by rotation so that optimum radiation can be realized for each geometry.
  • a motor is provided for rotating the X-ray optical element.
  • the X-ray optical element is mounted on the motor axis for this purpose.
  • the size of the opening defined by the further aperture can be varied perpendicular to the X-ray beam (clear height of the further diaphragm).
  • an automatic control of the rotation of the X-ray optical element is provided, in particular a computer control.
  • the X-ray optical element is preferably arranged on the secondary beam side, e.g. to switch between Bragg-Brentano (further aperture in the beam) and reflectometry (linear Soller aperture in the beam).
  • the X-ray optical element may be arranged on the primary beam, for example for switching between Bragg-Brentano on flat powder samples (further aperture in the beam) and reflection measurements on uneven powder samples (linear Soller aperture in the beam).
  • the sample holder is arranged at the crossing point of the Lammellenraumen of at least one radial Soller aperture of the X-ray optical element.
  • An arrangement of the sample holder at the crossing point of the Soller blades is particularly advantageous for transmission measurements on capillary samples with strip detector
  • the source is arranged in the center of at least one radial Soller aperture of the X-ray optical element.
  • An arrangement of the source at the crossing point of the Soller blades is particularly advantageous for measurements in Bragg-Brentano arrangement in which special emphasis is placed on scattered beam suppression.
  • Fig. 1a -c and Fig. 2 show a particularly preferred embodiment of an optical element 1 according to the invention with a linear Sollerblende 2 (equatorially arranged Sollerblende) and a further diaphragm, the two diaphragm jaws 3a, 3b, for example in the form of tantalum cutting comprises.
  • the diaphragm jaws 3 a, 3 b, as well as the Soller diaphragm 2 are fastened to a holder 4 , whereby the further diaphragm is rigidly connected to the Soller diaphragm 2.
  • the Soller panel 2 has a Soller axis 5 which extends parallel to the slats of the Soller panel between an inlet opening 6 and an outlet opening 7 .
  • the plane formed by the diaphragm jaws 3 a, 3 b of the further diaphragm closes with the axis 5 of Soller aperture an angle which is not equal to 90 ° and preferably> 10 °, in the case shown 45 °.
  • the distance between the diaphragm jaws 3a, 3b to each other can be changed in the non-operating state by moving the diaphragm jaws 3a, 3b.
  • the Soller panel 2 has a beam window in the form of a recess 8 through which radiation with a propagation direction that does not run along the Soller axis 5 can pass through the X-ray optical element 1 ( Fig. 1b, 1c ).
  • a beam window can also be realized that by appropriate alignment of the slats of the Soller shutter 2 of the beam path during rotation of the X-ray optical element 1 relative to the Soller axis 5 both through the slats of the Soller shutter 2 and through the further aperture extends (not shown). The slats of the Sollerblende 2 off Fig. 1a-c would then be aligned parallel to the drawing plane.
  • Fig. 1a is an alignment of the X-ray optical element according to the invention against an incident X-ray 10 ("X-ray 10" will also include radiation bundles hereinafter) shown, in which the Sollerblende 2 is arranged parallel to the X-ray beam 10. The X-ray beam 10 is then collimated by the Soller shutter 2.
  • the X-ray optical element 1 By rotation of the X-ray optical element 1 about an axis of rotation 9, the X-ray optical element 1 can be rotated relative to the incident X-ray beam 10.
  • the axis of rotation 9 of the X-ray optical element 1 is in this case in each position of the X-ray optical element 1 perpendicular to the Soller axis 5 and the incident X-ray 10.
  • the X-ray optical element 1 allows the choice between a beam path through the Soller aperture 2 or a beam path through the further aperture, without while distracting or dividing the X-ray beam 10.
  • the beam path running through the further diaphragm intersects the beam path passing through the Soller diaphragm 2 within the Soller diaphragm 2.
  • a compact embodiment of the X-ray optical element 1 is realized.
  • Fig. 1b, 1c show two different positions of the X-ray optical element 1 relative to the incident X-ray beam 10, in which the X-ray beam 10 is limited by the further aperture (dimmed).
  • the limited height (with respect to the incident X-ray beam 10) of the further diaphragm can be varied by the diaphragm jaws 3a, 3b. This is done by the Fig. 1b, 1c clear.
  • the maximum passage of the X-ray beam 10 through the further diaphragm takes place in the embodiment shown here in a 90 ° relative to the in Fig. 1a shown position (position with beam parallel to the Soller axis 5).
  • the use of the X-ray optical element according to the invention in a diffractometer allows an automatic change between a Bragg-Brentano beam path, in which the simple further aperture limits the X-ray beam 10, and a parallel beam path through the Soller aperture 2.
  • a parallel primary beam reflectometry measurements are also possible in which, for small angles of incidence, that is to say in the region of intense reflexes, a construction with a single diaphragm (for example with diaphragm jaws 3a, 3b) is selected.
  • Fig. 3 shows a schematic structure of such a diffractometer according to the invention with an X-ray source 11, a sample holder 12, a detector 13 and two inventive X-ray optical elements 1, wherein one of the X-ray optical elements primary beam side and the other secondary beam side is arranged.
  • the X-ray optical elements 1 are on a goniometer attached and rotatably arranged with respect to the X-ray source 11, the sample holder 12 and the detector 13.
  • the rotation of the X-ray optical elements 1 is realized in each case by means of a motor (not shown).
  • the optical axis (direction of the X-ray beam 10) passes through the axis of rotation of the X-ray optical element 1 or the motor. It is also possible to provide only one optical element 1, ie either primary beam side or secondary beam side.
  • X-ray optical element 1 instead of in Fig. 1a-c and Fig.2 shown X-ray optical element 1, other embodiments of the X-ray optical element according to the invention can be used in the primary beam 10a and / or in the secondary beam 10b .
  • the X-ray optical element 1 ' may comprise a radial Soller diaphragm 14 , as in FIG Fig. 4 shown.
  • This embodiment of the X-ray optical element 1 ' can be used for a change between, for example, transmission measurements with capillaries and streak detector (use of the radial Soller aperture 14) and Bragg Brentano measurements in reflection geometry (use of the further aperture with diaphragm jaws 3a, 3b).
  • the source 11, the sample holder 12 or the detector 13 may be advantageous to arrange the source 11, the sample holder 12 or the detector 13 in the center of the radial Soller aperture 14, wherein the point of intersection of the slats of the radial Soller aperture 14 with the axis 15 of the radial Soller aperture 14 is the center of the radial Soller aperture 14 is defined.
  • Fig. 5 shows a further embodiment of the X-ray optical element 1 " according to the invention , in which a linear Sollerblende 2 and a radial Sollerblende 14 are combined.
  • the axis 5 of the linear Sollerblende 2 and the axis 15 of the radial Sollerblende 14 are preferably perpendicular to each other.
  • This embodiment of the X-ray optical Element 1 " is used to adjust the beam path during the automatic change between transmission measurements and reflectance measurements in powder samples. In particular, when switching between capillary samples with strip detector (use the radial Soller aperture 2) and flat samples with point detectors (using the linear Soller aperture 14).
  • two linear roller blinds 2 can also be combined (not shown). If the lamellae of the two linear roller blinds 2 are oriented perpendicular to one another and perpendicular to the roller axis 5, such an X-ray optical element can be used for switching between applications in which the one hand is measured in the scattering plane and, on the other hand, measured out of the scattering plane.
  • All embodiments of the diffractometer according to the invention can also be used for neutron beam diffractometry.
  • a change between a Soller panel and at least one further panel without user intervention and readjustment can be done automatically.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • General Engineering & Computer Science (AREA)
  • High Energy & Nuclear Physics (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Claims (15)

  1. Élément optique pour rayons X (1, 1', 1") doté d'une fente de Soller comprenant plusieurs lamelles pour collimater un faisceau de rayons X par rapport à la direction de l'axe (5, 15) de la fente de Soller et d'une autre fente pour limiter un faisceau de rayons X (10), l'autre fente étant reliée rigidement à la fente de Soller (2, 14) pendant le fonctionnement,
    caractérisé en ce
    que le faisceau de rayons X (10) limité par l'autre fente coupe l'axe (5, 15) de la fente de Soller à l'intérieur de la fente de Soller et la direction du faisceau de rayons X (10) fait un angle α ≥ 10° avec l'axe (5, 15) de la fente de Soller.
  2. Élément optique pour rayons X (1, 1") selon la revendication 1, caractérisé en ce que la fente de Soller est une fente de Soller linéaire (2).
  3. Élément optique pour rayons X (1', 1") selon la revendication 1, caractérisé en ce que la fente de Soller est une fente de Soller radiale (14).
  4. Élément optique pour rayons X (1, 1', 1") selon l'une des revendications précédentes, caractérisé en ce que la fente de Soller présente un évidement (8) perpendiculaire à l'axe de Soller (5).
  5. Élément optique pour rayons X (1, 1') selon l'une des revendications 1 à 4, caractérisé en ce que l'autre fente présente au moins deux joues de fente (3a, 3b), lesquelles joues de fente (3a, 3b) sont disposées sur des côtés différents de la fente de Soller (2, 14).
  6. Élément optique pour rayons X (1, 1') selon la revendication 5, caractérisé en ce que les joues de fente (3a, 3b) font un angle différent de 90°, de préférence égal à 45°, avec l'axe (5, 15) de la fente de Soller (2, 14).
  7. Élément optique pour rayons X (1") selon l'une des revendications 1 à 4, caractérisé en ce que l'autre fente est une fente de Soller linéaire (2).
  8. Élément optique pour rayons X selon la revendication 7 et la revendication 2, caractérisé en ce que les deux fentes de Soller linéaires (2) présentent des angles de divergence différents.
  9. Élément optique pour rayons X (1") selon l'une des revendications 1 à 4, caractérisé en ce que l'autre fente est une fente de Soller radiale (14).
  10. Élément optique pour rayons X selon la revendication 3 et la revendication 9, caractérisé en ce que les deux fentes de Soller radiales (14) présentent des angles d'ouverture différents et/ou des angles de divergence différents.
  11. Diffractomètre comprenant une source (11) pour générer un faisceau primaire, un porte-échantillon (12) pour y disposer un échantillon, un détecteur (13) pour enregistrer un faisceau secondaire provenant de l'échantillon et un élément optique pour rayons X (1, 1', 1") selon l'une des revendications précédentes.
  12. Diffractomètre selon la revendication 11, caractérisé en ce que l'élément optique pour rayons X (1, 1', 1") est monté tournant dans le diffractomètre autour d'un axe de rotation (9) perpendiculaire à l'axe (5, 15) de la fente de Soller (2, 14).
  13. Diffractomètre selon la revendication 12, caractérisé en ce qu'une commande automatique de la rotation de l'élément optique pour rayons X (1, 1', 1") est prévue, en particulier une commande par ordinateur.
  14. Diffractomètre selon l'une des revendications 11 à 13, caractérisé en ce que l'élément optique pour rayons X (1, 1', 1") est disposé côté faisceau primaire.
  15. Diffractomètre selon l'une des revendications 11 à 13, caractérisé en ce que l'élément optique pour rayons X (1, 1', 1") est disposé côté faisceau secondaire.
EP09177712.8A 2008-12-02 2009-12-02 Elément optique pour rayons X et diffractomètre doté d'une fente de Soller Active EP2194375B1 (fr)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE102008060070A DE102008060070B4 (de) 2008-12-02 2008-12-02 Röntgenoptisches Element und Diffraktometer mit einer Sollerblende

Publications (2)

Publication Number Publication Date
EP2194375A1 EP2194375A1 (fr) 2010-06-09
EP2194375B1 true EP2194375B1 (fr) 2018-01-31

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US (1) US7983389B2 (fr)
EP (1) EP2194375B1 (fr)
DE (1) DE102008060070B4 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102021103037B3 (de) 2021-02-09 2022-03-31 Bruker Axs Gmbh Verstellbarer segmentierter Kollimator

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JP6905748B2 (ja) * 2017-10-25 2021-07-21 株式会社リガク ソーラースリット、ｘ線回折装置および方法
DE102017223228B3 (de) 2017-12-19 2018-12-27 Bruker Axs Gmbh Aufbau zur ortsaufgelösten Messung mit einem wellenlängendispersiven Röntgenspektrometer
EP3553507A1 (fr) * 2018-04-13 2019-10-16 Malvern Panalytical B.V. Appareil d'analyse à rayons x

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JP3950239B2 (ja) * 1998-09-28 2007-07-25 株式会社リガク Ｘ線装置
JP3722454B2 (ja) 1998-11-02 2005-11-30 株式会社リガク ソーラスリット及びその製造方法
NL1015740C1 (nl) * 1999-07-23 2000-09-27 Koninkl Philips Electronics Nv Stralingsanalysetoestel voorzien van een regelbare collimator.
DE10141958B4 (de) 2001-08-28 2006-06-08 Bruker Axs Gmbh Röntgen-Diffraktometer
JP3548556B2 (ja) 2001-12-28 2004-07-28 株式会社リガク Ｘ線回折装置
US7127037B2 (en) 2002-07-26 2006-10-24 Bede Scientific Instruments Ltd. Soller slit using low density materials
JP4908119B2 (ja) 2005-10-19 2012-04-04 株式会社リガク 蛍光ｘ線分析装置
JP4658003B2 (ja) 2006-08-29 2011-03-23 株式会社リガク Ｘ線分析装置
JP4860418B2 (ja) * 2006-10-10 2012-01-25 株式会社リガク Ｘ線光学系

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102021103037B3 (de) 2021-02-09 2022-03-31 Bruker Axs Gmbh Verstellbarer segmentierter Kollimator
EP4040447A2 (fr) 2021-02-09 2022-08-10 Bruker AXS GmbH Collimateur segmenté réglable
US11742104B2 (en) 2021-02-09 2023-08-29 Bruker Axs Gmbh Adjusted segmented collimator comprising a Soller slit

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DE102008060070B4 (de) 2010-10-14
DE102008060070A1 (de) 2010-06-10
US20100135460A1 (en) 2010-06-03
US7983389B2 (en) 2011-07-19
EP2194375A1 (fr) 2010-06-09

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