WO1991013344A1 - X-ray diffractometer - Google Patents

X-ray diffractometer Download PDF

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Publication number
WO1991013344A1
WO1991013344A1 PCT/DE1991/000138 DE9100138W WO9113344A1 WO 1991013344 A1 WO1991013344 A1 WO 1991013344A1 DE 9100138 W DE9100138 W DE 9100138W WO 9113344 A1 WO9113344 A1 WO 9113344A1
Authority
WO
WIPO (PCT)
Prior art keywords
goniometer
ray
detector
sample
ray diffractometer
Prior art date
Application number
PCT/DE1991/000138
Other languages
German (de)
French (fr)
Inventor
Norbert Broll
Original Assignee
Siemens Aktiengesellschaft
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 Siemens Aktiengesellschaft filed Critical Siemens Aktiengesellschaft
Publication of WO1991013344A1 publication Critical patent/WO1991013344A1/en

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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
    • G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions

Definitions

  • the invention relates to an X-ray diffractometer with an X-ray emitter, a detector and a sample holder, which are arranged in a goniometer system so as to be movable relative to one another.
  • Known diffractometers have a goniometer system with two concentric goniometer circles, the sample holder on the inner goniometer circle being pivotable about an axis passing through the sample surface and the detector attached to the outer goniometer circle being pivotable about the same axis.
  • the central axis of the radiation path of the X-ray emitter (primary beam) and the central axis of the beam path into the detector lie in the surface plane of the sample.
  • Diffractometers can be operated as 2 teta / teta diffractometers, in which the sample surface halves an angle of 2 teta between the primary beam and the beam reflected on the surface (1: 2 condition according to Bragg-Brentano), or as 2 teta / omega -Diffractometer, in which there is no fixed association between the angle 2 teta and the angular position of the samples.
  • Surface angle Omega
  • the invention solves the problem of creating an X-ray diffractometer in which heavy and / or microphonic sensitive detectors can also be used with mechanical and structural outlay that does not go beyond the usual. Only relatively minor changes to the goniometer system of a conventional X-ray diffractometer are required in order to be able to use heavy, in particular liquid-cooled semiconductor detectors.
  • FIGS. 1 and 2 show schematically an embodiment.
  • the goniometer system 1 of the X-ray diffractometer essentially consists of two concentric goniometer circles, which are plate-shaped or ring-shaped and can be rotated by means of a geared motor.
  • a sample holder 4 for the sample P is arranged in the middle of the inner gonometer circle 2 such that the axis of rotation of the goniometer system lies in the plane of the sample surface.
  • the X-ray emitter R is attached to the outer goniometer circuit 3.
  • the X-ray radiation emanating from its focal spot B falls through the aperture diaphragm 5 onto the sample surface of the specimen P, is diffracted there and passes through a diffuser diaphragm 6 and a detector diaphragm 7 into the stationary detector D, for example a semiconductor detector cooled with liquid nitrogen on a Ge or Si basis.
  • the beam direction of the X-ray emitter and the direction of incidence of the beam into the detector form an angle of 90 ".
  • Figure 3 shows a goniometer system 1, shown schematically in a view from above.
  • the detector D which is fixedly attached to the goniometer housing 9 with the aid of a flange connection 8, with a holder 10 for diaphragms, for example anti-scatter diaphragm 6 and the detector diaphragm 7.
  • the sample holder 4 with the sample P is located centrally on the inner goniometer circle, which is designed as a disk and is surrounded by the outer goniometer circuit 3 in the form of an annular disk.
  • the X-ray emitter R is attached to the outer goniometer circuit 3 with the aid of an angle flange 11, which also carries the aperture base 12 for receiving aperture diaphragms 5 or monochromators.
  • the goniometer system 1 can be operated in a manner known per se either in the 2 Teta / Teta or in the 2 Teta / Omega mode.

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth 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

In the X-ray diffractometer the detector (D), particularly a liquid-cooled semi-conductor, is rigidly mounted on the goniometer housing (9). The sample holder (4) with the sample (P) can be rotated on the inner goniometer circle (2) about a central axis going through the measuring plane in the surface of the sample. The X-ray machine (R) is secured onto the outer circle (3) of the goniometer and moves with the latter. Easy construction is possible since the relatively heavy, liquid-cooled detectors, which are sensitive to vibrations, are secured rigidly.

Description

RöntgendiffraktometerX-ray diffractometer
Die Erfindung bezieht sich auf ein Röntgendiffraktometer mit einem Röntgenstrahier, einem Detektor und einem Probenhalter, die relativ zueinander bewegbar in einem Goniometersystem an¬ geordnet sind.The invention relates to an X-ray diffractometer with an X-ray emitter, a detector and a sample holder, which are arranged in a goniometer system so as to be movable relative to one another.
Bekannte Diffrakto eter weisen ein Goniometersystem mit zwei konzentrischen Goniometerkreisen auf, wobei der Probenhalter auf dem inneren Goniometerkreis um eine durch die Probenober¬ fläche gehende Achse und der an dem äußeren Goniometerkreis befestigte Detektor um die gleiche Achse schwenkbar sind. In der Grundstellung liegen die Mittelachse des Strahleπgaπgs des Röntgenstrahlers (Primärstrahl) und die Mittelachse des Strahlengangs in den Detektor in der Oberflächeπebene der Probe.Known diffractometers have a goniometer system with two concentric goniometer circles, the sample holder on the inner goniometer circle being pivotable about an axis passing through the sample surface and the detector attached to the outer goniometer circle being pivotable about the same axis. In the basic position, the central axis of the radiation path of the X-ray emitter (primary beam) and the central axis of the beam path into the detector lie in the surface plane of the sample.
Diffraktometer können als 2 Teta/Teta-Diffraktometer betrieben werden, bei dem die Probenoberfläche jeweils einen Winkel 2 Teta zwischen Primärstrahl und auf der Oberfläche reflektier¬ tem Strahl halbiert (1 : 2-Bedingung nach Bragg-Brentano) , oder als 2 Teta/Omega-Diffraktometer, bei dem keine feste Zuordnung zwischen dem Winkel 2 Teta und der Winkelstellung der Proben- . Oberfläche (Winkel Omega) besteht.Diffractometers can be operated as 2 teta / teta diffractometers, in which the sample surface halves an angle of 2 teta between the primary beam and the beam reflected on the surface (1: 2 condition according to Bragg-Brentano), or as 2 teta / omega -Diffractometer, in which there is no fixed association between the angle 2 teta and the angular position of the samples. Surface (angle Omega) exists.
Bei der Verwendung von relativ schweren und/oder gegen Erschüt¬ terungen empfindlichen, insbesondere flüssigkeitsgekühlten Halbleiterdetektorsystemen muß für die Bewegung des Detektors ein erheblicher mechanischer Aufwand getrieben werden.When using relatively heavy and / or sensitive to vibrations, in particular liquid-cooled semiconductor detector systems, a considerable mechanical effort must be made to move the detector.
Die Erfindung, wie sie in den Ansprüchen gekennzeichnet ist, löst die Aufgabe, ein Röntgendiffraktometer zu schaffen, bei welchem bei nicht über das Übliche hinausgehendem mechanischen und konstruktiven Aufwand auch schwere und/oder gegen Mikro- phonie empfindliche Detektoren eingesetzt werden können. Es bedarf nur relativ geringfügiger Änderungen an dem Goniometersystem eines herkömmlichen Röntgeπdiffraktometers, um auch schwere, insbesondere flüssigkeitsgekühlte Halbleiter¬ detektoren einsetzen zu können.The invention, as characterized in the claims, solves the problem of creating an X-ray diffractometer in which heavy and / or microphonic sensitive detectors can also be used with mechanical and structural outlay that does not go beyond the usual. Only relatively minor changes to the goniometer system of a conventional X-ray diffractometer are required in order to be able to use heavy, in particular liquid-cooled semiconductor detectors.
Zur Erläuterung der Erfindung sind in den Figuren 1 und 2 das Aufbau- und Betriebsprinzip eines erfindungsgemäßen Röntgen- diffraktometers dargestellt. Figur 3 zeigt schematisch ein Ausführungsbeispiel.To explain the invention, the construction and operating principle of an X-ray diffractometer according to the invention are shown in FIGS. 1 and 2. Figure 3 shows schematically an embodiment.
In den Figuren sind gleiche Teile mit den gleichen Bezugs¬ zeichen versehen.In the figures, the same parts are provided with the same reference symbols.
Das Goniometersystem 1 des Röntgendiffraktometers besteht im wesentlichen aus zwei konzentrischen Goniometerkreisen, die teller- oder ringscheibenförmig ausgebildet und mittels eines Getriebemotors drehbar sind. In der Mitte des inneren Gonio¬ meterkreises 2 ist eine Probenhalterung 4 für die Probe P derart angeordnet, daß die Drehachse des Goniometersystems in der Ebene der Probenoberfläche liegt.The goniometer system 1 of the X-ray diffractometer essentially consists of two concentric goniometer circles, which are plate-shaped or ring-shaped and can be rotated by means of a geared motor. A sample holder 4 for the sample P is arranged in the middle of the inner gonometer circle 2 such that the axis of rotation of the goniometer system lies in the plane of the sample surface.
An dem äußeren Goniometerkreis 3 ist der Röntgenstrahier R befestigt. Die von dessen Brennfleck B ausgehende Röntgen¬ strahlung fällt durch die Aperturblende 5 auf die Probenober- fläche der Probe P, wird dort gebeugt und gelangt durch eine Streustrahlblende 6 und eine Detektorblende 7 in den ortsfest angeordneten Detektor D, beispielsweise einen mit flüssigem Stickstoff gekühlten Halbleiterdetektor auf Ge- oder Si- i- Basis.The X-ray emitter R is attached to the outer goniometer circuit 3. The X-ray radiation emanating from its focal spot B falls through the aperture diaphragm 5 onto the sample surface of the specimen P, is diffracted there and passes through a diffuser diaphragm 6 and a detector diaphragm 7 into the stationary detector D, for example a semiconductor detector cooled with liquid nitrogen on a Ge or Si basis.
In der in Figur 1 dargestellten Position befinden sich der Röntgenstrahier R in seiner Anfangsposition gegenüber dem orts¬ festen Detektor D (2 Teta = 0*) wie auch der Probenhalter 4 mit der Probe P (Omega = 0").In the position shown in FIG. 1, the X-ray emitter R is in its initial position in relation to the fixed detector D (2 Teta = 0 * ), as is the sample holder 4 with the sample P (Omega = 0 ").
In der Figur 2 ist die 90β-45β-Position dargestellt, d. h., der Röntgenstrahier R ist mit dem äußeren Goniometerkreis um 90* aus seiner Anfangslage gedreht (2 Teta = 90°), der Proben¬ halter 4 mit der Probe P um den halben Winkel 2 Teta, entspre- chend Omega = 45°. Strahlrichtung des Röntgenstrahlers und ■ Einfallsrichtung des Strahls in den Detektor bilden einen Winkel von 90".FIG. 2 shows the 90 β -45 β position, ie the X-ray emitter R is rotated with the outer goniometer circle by 90 * from its initial position (2 Teta = 90 °), the sample holder 4 with the sample P. half the angle 2 teta, corresponding omega = 45 °. The beam direction of the X-ray emitter and the direction of incidence of the beam into the detector form an angle of 90 ".
Figur 3 zeigt ein Goniometersystem 1, schematisch dargestellt in einer Ansicht von oben. Man erkennt den mit Hilfe einer Flanschverbindung 8 ortsfest an dem Goniometergehäuse 9 an¬ gebrachten Detektor D mit einer Halterung 10 für Blenden, bei¬ spielsweise Streustrahlblende 6 und die Detektorblende 7. Die Probenhalterung 4 mit der Probe P befindet sich zentrisch auf dem inneren Goniometerkreis, der als Scheibe ausgebildet und von dem äußeren Goniometerkreis 3 in Ringscheibenform umgeben ist. Der Röntgenstrahier R ist mit Hilfe eines Winkelflansc.hes 11 an dem äußeren Goniometerkreis 3 befestigt, welche.r auch die Blendenbasis 12 zur Aufnahme von Aperturblenden 5 oder Mono- chromatoren trägt. Diametral gegenüber dem Röntgenstrahier R ist auf dem äußeren Goniometerkreis 3 ein Gegengewicht 13 befestigt, dessen Masse der des Röntgenstrahlers R entspricht. Das Goniometersystem 1 kann in an sich bekannter Weise entweder im 2 Teta/Teta- oder im 2 Teta/Omega-Modus betrieben werden. Figure 3 shows a goniometer system 1, shown schematically in a view from above. One recognizes the detector D, which is fixedly attached to the goniometer housing 9 with the aid of a flange connection 8, with a holder 10 for diaphragms, for example anti-scatter diaphragm 6 and the detector diaphragm 7. The sample holder 4 with the sample P is located centrally on the inner goniometer circle, which is designed as a disk and is surrounded by the outer goniometer circuit 3 in the form of an annular disk. The X-ray emitter R is attached to the outer goniometer circuit 3 with the aid of an angle flange 11, which also carries the aperture base 12 for receiving aperture diaphragms 5 or monochromators. A counterweight 13, the mass of which corresponds to that of the X-ray emitter R, is fastened diametrically opposite the X-ray emitter R on the outer goniometer circuit 3. The goniometer system 1 can be operated in a manner known per se either in the 2 Teta / Teta or in the 2 Teta / Omega mode.

Claims

Patentansprüche Claims
1. Röntgendiffraktometer mit einem Röntgenstrahier, einem Detektor und einem Probenhalter, die relativ zueinander be- wegbar in einem Goniometersystem angeordnet sind, d a ¬ d u r c h g e k e n n z e i c h n e t , daß der Detektor (D) ortsfest angeordnet, der zentrisch angeordnete Proben¬ halter (4) um eine durch die Oberfläche der Probe (P) gehende Mittelachse auf einem inneren Goniometerkreis (2) drehbar und der Röntgenstrahier (R) auf einem äußeren Goniometer¬ kreis (3) schwenkbar befestigt ist.1. X-ray diffractometer with an X-ray source, a detector and a sample holder, which are arranged such that they can be moved relative to one another in a goniometer system, since ¬ characterized in that the detector (D) is arranged in a stationary manner, the centrally arranged sample holder (4) by one the surface of the sample (P), the central axis, is rotatable on an inner goniometer circuit (2) and the X-ray emitter (R) is pivotably fastened on an outer goniometer circuit (3).
2. Röntgendiffraktometer nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t , daß der Röπtgenstrahler (R) und der Probenhalter (4) unabhängig voneinander um die Mittel¬ achse des Goniometersystems drehbar sind.2. X-ray diffractometer according to claim 1, so that the X-ray emitter (R) and the sample holder (4) can be rotated independently of one another about the central axis of the goniometer system.
3. Röntgendiffraktometer nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t , daß der Röntgenstrahier (R) mit der doppelten Winkelgeschwindigkeit des Probenhalters (4) drehbar ist.3. X-ray diffractometer according to claim 1, so that the x-ray emitter (R) can be rotated at twice the angular velocity of the sample holder (4).
4. Röntgendiffraktometer nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t , daß der Röntgenstrahier (R) mit Hilfe eines Flansches (11) an der Ringscheibe des äußeren Goniometerkreises (3).und diametral gegenüber ein Gegengewicht (13) befestigt ist.4. X-ray diffractometer according to claim 1, so that the X-ray radiator (R) is attached to the ring disc of the outer goniometer circuit (3) by means of a flange (11) and diametrically opposite a counterweight (13).
5. Röntgendiffraktometer nach Anspruch 1, d a d u r c h g e k e n n z e i c h n e t , daß der Detektor (D) ein mit flüssigem Stickstoff gekühlter Halbleiterdetektor ist. 5. X-ray diffractometer according to claim 1, so that the detector (D) is a semiconductor detector cooled with liquid nitrogen.
PCT/DE1991/000138 1990-02-22 1991-02-21 X-ray diffractometer WO1991013344A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE9002130U DE9002130U1 (en) 1990-02-22 1990-02-22
DEG9002130.4U 1990-02-22

Publications (1)

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DE (1) DE9002130U1 (en)
WO (1) WO1991013344A1 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0539626A1 (en) * 1991-10-30 1993-05-05 Koninklijke Philips Electronics N.V. X-ray examination apparatus
FR2683329A1 (en) * 1991-10-30 1993-05-07 Sandoz Sa OPTICAL DEVICE FOR SUPPORTING A PHOTOREFRINGENT CRYSTAL.
DE102016224940B3 (en) * 2016-12-14 2017-08-24 Bruker Axs Gmbh X-ray device with motor torque compensation at the detector circuit of the goniometer and method for operating an X-ray device

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4137673C2 (en) * 1991-11-15 2001-08-02 Bruker Axs Analytical X Ray Sy X-ray reflectometer

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1572719A1 (en) * 1967-08-05 1970-02-12 Luecke Dr Kurt X-ray goniometer for quick determination of the texture of crystalline samples in the back and transmission area
DE1950152B2 (en) * 1969-10-04 1977-12-08 Institut Max Von Laue - Paul Langevin, Grenoble (Frankreich), Niederlassung Institut Max Von Laue - Paul Langevin, Aussenstelle Garching, 8046 Garching DEVICE FOR THE SIMULTANEOUS INTENSITY MEASUREMENT OF SEVERAL NEUTRON SINGLE CRYSTAL INTERFERENCES
GB1546060A (en) * 1977-02-08 1979-05-16 Cgr Mev Neutrontherapy apparatus using a linear accelerator of electrons
DE3103322A1 (en) * 1980-03-03 1981-12-03 Jenoptik Jena Gmbh, Ddr 6900 Jena X-ray diffractometer

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1572719A1 (en) * 1967-08-05 1970-02-12 Luecke Dr Kurt X-ray goniometer for quick determination of the texture of crystalline samples in the back and transmission area
DE1950152B2 (en) * 1969-10-04 1977-12-08 Institut Max Von Laue - Paul Langevin, Grenoble (Frankreich), Niederlassung Institut Max Von Laue - Paul Langevin, Aussenstelle Garching, 8046 Garching DEVICE FOR THE SIMULTANEOUS INTENSITY MEASUREMENT OF SEVERAL NEUTRON SINGLE CRYSTAL INTERFERENCES
GB1546060A (en) * 1977-02-08 1979-05-16 Cgr Mev Neutrontherapy apparatus using a linear accelerator of electrons
DE3103322A1 (en) * 1980-03-03 1981-12-03 Jenoptik Jena Gmbh, Ddr 6900 Jena X-ray diffractometer

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0539626A1 (en) * 1991-10-30 1993-05-05 Koninklijke Philips Electronics N.V. X-ray examination apparatus
FR2683329A1 (en) * 1991-10-30 1993-05-07 Sandoz Sa OPTICAL DEVICE FOR SUPPORTING A PHOTOREFRINGENT CRYSTAL.
US5384663A (en) * 1991-10-30 1995-01-24 Sandoz Ltd. Rotatable crystal positioning apparatus
DE102016224940B3 (en) * 2016-12-14 2017-08-24 Bruker Axs Gmbh X-ray device with motor torque compensation at the detector circuit of the goniometer and method for operating an X-ray device
US9995697B1 (en) 2016-12-14 2018-06-12 Bruker Axs Gmbh X-ray apparatus having a motor-driven torque compensation at the detector circle of the goniometer
EP3336526A1 (en) * 2016-12-14 2018-06-20 Bruker AXS GmbH X-ray device with motorized torque compensation on the detector circuit of the goniometer

Also Published As

Publication number Publication date
EP0516677A1 (en) 1992-12-09
DE9002130U1 (en) 1990-04-26

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