DE4236291A1 - Texture and stress analysis and crystal orientation determn. method - involves exposing specimen to x-rays and measuring radiation from specimen with energy resolution detector at various output angles - Google Patents

Texture and stress analysis and crystal orientation determn. method - involves exposing specimen to x-rays and measuring radiation from specimen with energy resolution detector at various output angles

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Publication number
DE4236291A1
DE4236291A1 DE19924236291 DE4236291A DE4236291A1 DE 4236291 A1 DE4236291 A1 DE 4236291A1 DE 19924236291 DE19924236291 DE 19924236291 DE 4236291 A DE4236291 A DE 4236291A DE 4236291 A1 DE4236291 A1 DE 4236291A1
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specimen
sample
radiation
texture
detector
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Dirk Meyer
Kurt Dr Richter
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RICH. SEIFERT & CO FREIBERGER PRAEZISIONSMECHANIK
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FREIBERGER PRAEZISIONSMECHANIK
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    • 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
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/606—Specific applications or type of materials texture
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00—Investigating materials by wave or particle radiation
    • G01N2223/60—Specific applications or type of materials
    • G01N2223/607—Specific applications or type of materials strain

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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

The specimen is exposed to x-radiation and the radiation emanating from the specimen is measured by an energy resolving detector at different output angles, which are varied in steps and at which the detector is arranged wrt. the specimen surface. The specimen is stepwise rotated at various rotation angles about the normal to the surface. The intensity maxima of the electrical output signals are measured. The specimen is exposed to polychromatic primary radiation, and the specimen tilt is 0 deg. for all measurements. ADVANTAGE-Ensures that region of specimen does not change during texture and stress analysis and enables essentially more rapid determination of unknown crystal orientations than conventional techniques.

Description

Die Erfindung betrifft ein Verfahren zur Messung von Textur und Spannung sowie zur Bestimmung von Kristallorientierungen.The invention relates to a method for measuring texture and voltage as well as for the determination of crystal orientations.

Bei der Textur- und Spannungsanalyse mittels Röntgenbeugung wird der Einstrahlwinkel der monochromatischen Primärstrahlung in Bezug auf die Probenoberfläche im Verlauf des Meßverfahrens variiert. Die Probenoberflächennormale wird dabei aus der Goniometerebene herausgekippt (1).For texture and stress analysis using X-ray diffraction becomes the angle of incidence of the monochromatic primary radiation in relation to the sample surface in the course of the measurement process varies. The sample surface normal is taken from the Goniometer level tilted out (1).

Damit verbunden ist eine veränderte Eindringtiefe der Röntgenstrahlung in die Probe und bei endlichem Primärstrahlquerschnitt ein verändertes bestrahltes Probengebiet, gekoppelt mit Änderungen der Breite der Beugungsreflexe. Dies ruft zum einen eine Verwischung von Textur- und Spannungsgradienten hervor, die man häufig mit zunehmendem Abstand von der Probenoberfläche zur Probenmitte hin beobachtet, zum anderen können dicht benachbarte Reflexe bei extremen Kippwinkeln durch Verbreiterung infolge Verletzung der Fokussierbedingung ineinanderlaufen, was die Auswertung erschwert.Associated with this is a changed penetration depth of the X-rays in the sample and at finite Primary beam cross section a modified irradiated Sample area, coupled with changes in the width of the Diffraction reflexes. On the one hand, this calls a blurring of Texture and tension gradients that you often use increasing distance from the sample surface to the sample center observed, on the other hand, closely adjacent reflections at extreme tilt angles due to widening Violation of the focussing condition, what the Evaluation difficult.

Eine Einkristallorientierungsbestimmung erfordert drei Winkel schrittweise zu verstellen, um bei einem Kristall unbekannter Orientierung eine bestimmte Netzebenenschar (hkl) in Reflexionsstellung zu bringen. Entsprechend hoch ist der Meßaufwand.A single crystal orientation determination requires three angles to gradually adjust to make a crystal unknown Orientation a certain network level group (hkl) in Bring reflection position. The is accordingly high Measurement effort.

Weiterhin sind Vorrichtungen bekannt, die mehrkanalig mit fest angeordneten Primärstrahlkollimatoren und energieauflösenden Detektoren unter Verwendung von harter polychromatischer Röntgenstrahlung im Durchstrahlbetrieb arbeiten. Damit wird ein über die Probendicke gemittelter Texturwert gemessen. Eine Spannungsanalyse ist nicht möglich (2, 3). Furthermore, devices are known which are multi-channel fixed arranged primary beam collimators and energy-resolving Detectors using hard polychromatic Work with X-rays in radiographic mode. So that will a texture value averaged over the sample thickness was measured. A Stress analysis is not possible (2, 3).  

In (4) wird ein Röntgendiffraktometer beschrieben, welches bei herkömmlicher Geometrie des Strahlengangs (Bragg-Brentano- Fokussierung (1)) einen energieauflösenden Detektor verwendet, um Kb-Anteile der verwendeten charakteristischen Strahlung, Fluoreszenzstrahlung von der Probe sowie die störenden Anteile des Bremsspektrums zu eliminieren, mit dem Ziel, ein verbessertes Effekt-Untergrundverhältnis für eine monochromatische Strahlung, z. B. Cu-Kα, zu erhalten bzw. um störende Kβ-Reflexe aus dem Beugungsdiagramm zu eliminieren.In (4) an X-ray diffractometer is described which, in the conventional geometry of the beam path (Bragg-Brentano focusing (1)), uses an energy-resolving detector in order to detect K b components of the characteristic radiation used, fluorescent radiation from the sample and the disruptive components of the braking spectrum to eliminate, with the aim of an improved effect-background ratio for monochromatic radiation, e.g. B. Cu-K α , or to eliminate disturbing K β reflections from the diffraction pattern.

(1) Glocker Materialprüfung mit Röntgenstrahlen, Springer- Verlag, Berlin-Heidelberg-New York, 1971
(2) DE-OS 38 25 830
(3) DE-AS 28 17 742
(4) DD 2 81 658(1) Glocker material testing with X-rays, Springer-Verlag, Berlin-Heidelberg-New York, 1971
(2) DE-OS 38 25 830
(3) DE-AS 28 17 742
(4) DD 2 81 658

Aufgabe der Erfindung ist es, ein Verfahren anzugeben, bei dem sich das Probengebiet während der Textur- und Spannungsanalyse nicht ändert und mit dem unbekannte Kristallorientierungen wesentlich rascher bestimmbar sind.The object of the invention is to provide a method in which the sample area during texture and stress analysis does not change and with the unknown crystal orientations can be determined much more quickly.

Erfindungsgemäß wird die Aufgabe dadurch gelöst, daß die Probe mit polychromatischer Primärstrahlung bestrahlt wird, die Probenkippung für alle Messungen 0° beträgt, der Einstrahlwinkel α für wenigstens eine Meßreihe, bei denen die Winkel β und Φ alle interessierenden Werte durchlaufen haben, konstant ist und die von der Probe ausgehende Strahlung mit einem energieauflösenden Detektor gemessen wird.According to the invention the object is achieved in that the sample is irradiated with polychromatic primary radiation, the Sample tilt for all measurements is 0 ° Beam angle α for at least one series of measurements in which the Angles β and Φ have passed all values of interest, is constant and the radiation emanating from the sample an energy-resolving detector is measured.

Das Verfahren hat mehrere Vorteile. Durch die konstanten Kipp- und Einfallwinkel ändert sich das bestrahlte Probengebiet während der Vielzahl von Messungen, die zu einer Analyse erforderlich sind, nicht. Die Zahl der notwendigen Winkelschrittveränderungen und damit die Zahl der Messungen wird stark reduziert. Beispielsweise ist es möglich, Polfiguren exakt desselben Probengebietes in wesentlich kürzerer Zeit aufzunehmen. Es können mehrere Polfiguren gleichzeitig aufgezeichnet werden. Der 2R-Bereich wird nicht eingeschränkt.The process has several advantages. Due to the constant tilting and the angle of incidence changes the irradiated sample area during the multitude of measurements that lead to an analysis are not required. The number of necessary Angular step changes and thus the number of measurements is greatly reduced. For example, it is possible Pole figures of exactly the same sample area in essential record less time. There can be several pole figures  can be recorded simultaneously. The 2R area will not limited.

Messungen mit sehr kleinem Einstrahlwinkel (streifender Einfall) sind möglich. Mit geringer Änderung des Einstrahlwinkels α für eine zweite oder dritte Meßreihe kann in verschiedenen oberflächennahen Schichten gemessen werden und aus der vergleichenden Analyse können Textur- und Spannungsgradienten ermittelt werden.Measurements with a very small angle of incidence (grazing Idea) are possible. With little change in Beam angle α for a second or third series of measurements can can be measured in different layers near the surface and from the comparative analysis texture and Voltage gradients are determined.

Die Intensitätsmaxima werden mittels Vielkanalanalysator und Computer ausgewertet.The intensity maxima are determined using a multi-channel analyzer and Computer evaluated.

Die Erfindung wird nachfolgend in einem Ausführungsbeispiel näher dargestellt.The invention is described below in one embodiment shown in more detail.

In den Zeichnungen zeigenShow in the drawings

Fig. 1 die Zuordnung der Winkel während der Messung, Fig. 1 shows the assignment of the angle during the measurement,

Fig. 2 ein erstes Intensitätsspektrum, Fig. 2 shows a first intensity range,

Fig. 3 ein zweites Intensitätsspektrum. Fig. 3 shows a second intensity spectrum.

Zur Durchführung des Verfahrens wird ein in der Röntgendiffraktrometrie übliches Diffraktometer mit separat ansteuerbarer ω-Achse für die Einstellung des Einstrahlwinkels α und mit einer 2R-Achse für die Einstellung des Winkels β verwendet. Die Probe wird mit einem polychromatischen Röntgenstrahl, der wie üblich in Ausdehnung und Divergenz begrenzt ist, bestrahlt. Der Probentisch wird bei allen Messungen nicht gekippt, sondern in Nullstellung gehalten. Die von der Probe ausgehende polychromatische Strahlung wird mit einem energieauflösenden Detektor, einem Elektrolumineszenz­ detektor D, unter verschiedenen Winkeln β und Φ gemessen. Für wenigstens eine Meßreihe, bei der β und Φ alle interes­ sierenden Werte durchlaufen haben, ist der Einstrahlwinkel α konstant. Das Meßsignal ist auf einen Vielkanalanalysator geschaltet. Vor dem Detektor D ist ein Kollimator K mit üblicher Funktion angeordnet. Die Probe ist auf einem Drehtisch (Φ= 360°) befestigt. Die Φ-Achse liegt in der Goniometerebene. Vom Vielkanalanalysator wird das Impulshöhenspektrum aufgenommen.To carry out the procedure, a X-ray diffractometry usual diffractometer with separately controllable ω-axis for setting the angle of incidence α and with a 2R axis for setting the angle β used. The sample is made with a polychromatic X-ray beam, as usual, in extent and divergence is irradiated. The rehearsal table is with everyone Measurements not tilted, but held in the zero position. The polychromatic radiation emanating from the sample is also an energy-resolving detector, an electroluminescence detector D, measured at different angles β and Φ. For at least one series of measurements in which β and Φ all interest have passed the values, the angle of incidence is α  constant. The measurement signal is on a multi-channel analyzer switched. A collimator K is in front of the detector D. usual function arranged. The sample is on one Rotary table (Φ = 360 °) attached. The Φ axis lies in the Goniometer level. The multi-channel analyzer does that Pulse height spectrum recorded.

In den Fig. 2 und 3 sind für zwei verschiedene Winkeleinstellungen unterschiedliche Impulsgruppen mit unterschiedlicher Lage und Intensität zu erkennen. Lage und Intensität der von der Beugung herrührenden Maxima ändern sich mit dem Winkel β und dem Drehwinkel Φ. Die in der Probe angeregte Fluoreszenzstrahlung hingegen erzeugt Intensitätsmaxima, deren Lage nicht vom Winkel β abhängt und deren Intensität bei Drehung der Probe um Φ konstant bleibt.In FIGS. 2 and 3 different pulse groups are visible to the different position and intensity for two different angle settings. The position and intensity of the maxima resulting from diffraction change with the angle β and the angle of rotation Φ. The fluorescence radiation excited in the sample, on the other hand, produces intensity maxima whose position does not depend on the angle β and whose intensity remains constant when the sample is rotated by Φ.

Die Beugungspeaks werden mit einem Computerprogramm bestimmten Netzebenenscharen (hkl) zugeordnet. Aus der integralen Intensität der Beugungspeaks wird die Häufigkeit der Kristallitorientierungen (Textur) ermittelt. Aus der Lage der Beugungspeaks werden die Netzebenenabstände d und aus deren Abweichungen vom spannungsfreien Idealwert in Abhängigkeit von β die Spannungen in der Probe errechnet. Die den einzelnen Rechenverfahren zugrundeliegenden physikalischen Formeln und Methoden sind bekannt (1).The diffraction peaks are determined using a computer program Network layers (hkl) assigned. From the integral The intensity of the diffraction peaks becomes the frequency of the Orientation of crystallites (texture) determined. From the location of the Diffraction peaks become the network plane distances d and from them Deviations from the stress-free ideal value depending on β the stresses in the sample are calculated. The individual Underlying physical formulas and Methods are known (1).

Zur Ermittlung von Textur- und Spannungsgradienten werden für dasselbe Probengebiet mehrere Meßreihen unter leicht verändertem Einstrahlwinkel α durchgeführt.To determine texture and stress gradients, for the same sample area several series of measurements under easy changed angle of incidence α performed.

Claims (1)

Verfahren zur Messung von Textur und Spannung sowie zur Bestimmung von Kristallorientierungen, bei dem die Probe mit Röntgenstrahlung bestrahlt, die von der Probe ausgehende Strahlung in einem Detektor unter verschiedenen, schrittweise geänderten Austrittswinkeln β, unter dem der Detektor gegenüber der Probenoberfläche angeordnet ist, und schrittweise geändertem Drehungswinkel Φ der Probe um die Oberflächennormale gemessen und die Intensitätsmaxima des elektronischen Ausgangssignals ausgewertet werden, gekennzeichnet dadurch, daß die Probe mit polychromatischer Primärstrahlung bestrahlt wird, die Probenkippung für alle Messungen 0° beträgt, der Einstrahlwinkel α für wenigstens eine Meßreihe, bei der die Winkel β und Φ alle interessierenden Werte durchlaufen haben, konstant ist, und die von der Probe ausgehende Strahlung mit einem energieauflösenden Detektor gemessen wird.Method for measuring texture and tension and for determining crystal orientations, in which the sample is irradiated with X-radiation, the radiation emanating from the sample in a detector at different, gradually changed exit angles β, at which the detector is arranged opposite the sample surface, and stepwise changed rotation angle Φ of the sample around the surface normal and the intensity maxima of the electronic output signal are evaluated, characterized in that the sample is irradiated with polychromatic primary radiation, the sample tilt for all measurements is 0 °, the angle of incidence α for at least one series of measurements in which the Angles β and Φ have passed all values of interest, is constant, and the radiation emanating from the sample is measured with an energy-resolving detector.
DE19924236291 1992-10-23 1992-10-23 Texture and stress analysis and crystal orientation determn. method - involves exposing specimen to x-rays and measuring radiation from specimen with energy resolution detector at various output angles Withdrawn DE4236291A1 (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE10160326A1 (en) * 2001-12-07 2003-06-26 Intax Roentgenanalysentechnik Polychromatic X-ray ice crystal probe compares scattered powers in different directions
DE19907453B4 (en) * 1999-02-22 2006-08-24 Bruker Axs Microanalysis Gmbh Method for determining the orientation of single crystals
DE102006038907A1 (en) * 2006-08-18 2008-02-21 Forschungszentrum Jülich GmbH Sample`s i.e. group three nitride, reciprocal grid point measuring method, involves producing reflex at grid point by X-ray diffraction experiment, and performing another X-ray diffraction experiment at point under same angle of incidence
EP3048442A1 (en) * 2015-01-20 2016-07-27 United Technologies Corporation X-ray topography systems and methods for analysing micro-textured regions in metal samples

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2612676A1 (en) * 1976-03-25 1977-09-29 Krause Hans Goniometer for measuring tension and crystal orientation - in which sample performs three movements
US4128762A (en) * 1976-09-08 1978-12-05 Hitachi, Ltd. Apparatus for measuring mechanical stress using white X-rays

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2612676A1 (en) * 1976-03-25 1977-09-29 Krause Hans Goniometer for measuring tension and crystal orientation - in which sample performs three movements
US4128762A (en) * 1976-09-08 1978-12-05 Hitachi, Ltd. Apparatus for measuring mechanical stress using white X-rays

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SZPUNAR, J.: Geometry of Texture Measurements for Dispersive Methods. In: Texture of Crystalline Solids, 1981, Vol.4, S.171-181 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19907453B4 (en) * 1999-02-22 2006-08-24 Bruker Axs Microanalysis Gmbh Method for determining the orientation of single crystals
DE10160326A1 (en) * 2001-12-07 2003-06-26 Intax Roentgenanalysentechnik Polychromatic X-ray ice crystal probe compares scattered powers in different directions
DE10160326B4 (en) * 2001-12-07 2006-07-20 Bruker Axs Microanalysis Gmbh Method for the X-ray orientation determination of single crystals
DE102006038907A1 (en) * 2006-08-18 2008-02-21 Forschungszentrum Jülich GmbH Sample`s i.e. group three nitride, reciprocal grid point measuring method, involves producing reflex at grid point by X-ray diffraction experiment, and performing another X-ray diffraction experiment at point under same angle of incidence
EP3048442A1 (en) * 2015-01-20 2016-07-27 United Technologies Corporation X-ray topography systems and methods for analysing micro-textured regions in metal samples
US10161887B2 (en) 2015-01-20 2018-12-25 United Technologies Corporation Systems and methods for materials analysis
US10458929B2 (en) 2015-01-20 2019-10-29 United Technologies Corporation Systems and methods for materials analysis

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