WO2006095468A1 - Analyseur de diffraction aux rayons x et procédé d’analyse - Google Patents

Analyseur de diffraction aux rayons x et procédé d’analyse Download PDF

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Publication number
WO2006095468A1
WO2006095468A1 PCT/JP2005/018063 JP2005018063W WO2006095468A1 WO 2006095468 A1 WO2006095468 A1 WO 2006095468A1 JP 2005018063 W JP2005018063 W JP 2005018063W WO 2006095468 A1 WO2006095468 A1 WO 2006095468A1
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ray
sample
rays
incident
ray tube
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PCT/JP2005/018063
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Japanese (ja)
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Kenji Sakurai
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National Institute For Materials Science
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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

Definitions

  • an X-ray diffraction pattern including local structure information of a sample having an inhomogeneous crystal structure that is fixedly held, for example, a polycrystal, a member having a strain or a defect is used as incident X-rays for illuminating the sample.
  • X-ray diffraction analyzer and X-ray diffraction device for acquisition using X-ray tubes that generate X-rays and two-dimensional position-sensitive detectors consisting of a plurality of detector elements arranged in two dimensions
  • the present invention relates to a line diffraction analysis method. Background art
  • the X-ray diffraction method is a technique for obtaining an X-ray diffraction pattern corresponding to the crystal structure of a sample by detecting diffraction X-rays generated when the crystalline sample is irradiated with X-rays.
  • X-ray diffraction patterns are known to be acquired in various formats depending on the purpose and the equipment used. For example, in an ordinary powder X-ray diffractometer, the data is acquired in the form of a combination of diffraction angle and diffraction X-ray intensity, and is represented by a graph with the diffraction angle on the horizontal axis and the diffraction X-ray intensity on the vertical axis.
  • a device such as a Devi Sierra camera, an X-ray diffraction pattern is acquired as a photograph showing the intensity of the diffracted X-ray as a shade.
  • the powder X-ray diffraction method which generally uses powder (polycrystal) as its object, aims to know the crystal structure of a sample with uniform and random orientation. Therefore, it is possible to collect multiple diffraction spots (where the diffraction X-ray intensity is strong, which appears as a peak in the diffraction X-ray intensity profile with respect to the diffraction angle) and to grasp the intensity and the geometrical positional relationship between them. is important.
  • the characteristic X-ray from the X-ray tube is typically used as the incident X-ray illuminating the sample, and the intensity of the diffracted X-ray from the sample is scanned by the so-called ⁇ / 2 ⁇ scanning of the biaxial goniometer Measure the diffraction angle dependent intensity profile.
  • an optical system that approximately satisfies the concentration method is usually used. That is, only the X-rays that diverge from the light source located on the focal circle and that have passed through the divergence slit through the parallel slit are diffracted by the plane sample in contact with the focal circle. The Diffracted X-rays are concentrated on the light receiving slit on the focal circle and detected by the detector via the parallel slit and scattering slit.
  • a so-called real sample that is not a sample made for the purpose of X-ray diffraction measurement includes, for example, a texture in which different crystal structures coexist, a texture with different orientations, a defect, and a load.
  • the crystal structure is non-uniform, such as distortion of the crystal structure, and it is important to know the local crystal structure of each part of the sample.
  • the information obtained by the above-mentioned general powder X-ray diffraction method is the average information of the region illuminated by incident X-rays in the sample, information on the difference in crystal structure depending on the site in the region is used. I can't get it.
  • the time required to obtain an X-ray diffraction pattern for one point on a sample is about 20 to 30 minutes, which is the same as the measurement time by a general powder X-ray diffraction method. If the number of measurement points on the sample is 1 0 0 X 1 0 0 1 0 0 0 0 0, the measurement will take about 5 0 0 hours, that is, about 2 0 0 days become.
  • two-axis goniometry is achieved by detecting diffraction X-ray information at different diffraction angles at each element of the detector using a one-dimensional or two-dimensional position-sensitive detector.
  • the technique that omits the evening ⁇ ⁇ 2 ⁇ scan is common.
  • it in order to obtain information on each part of the sample, it must be measured point by point, so it is not possible to obtain information on each part in a wide area of the sample.
  • the sample is supported so as to be rotatable around an axis perpendicular to the optical axis of the incident X-ray,
  • a position-sensitive detector is installed with a fixed scattering angle (20 angle) with respect to the incident X-ray, and a collimator is placed between the sample and the position-sensitive detector to measure the surface of the sample.
  • Each part in the region and each detection element of the position sensitive detector are in one-to-one correspondence, and the entire region to be measured is illuminated with monochromatic X-rays with good parallelism.
  • There is also proposed a technique for obtaining a diffraction pattern only by ⁇ scanning of a sample without scanning the measurement point on the sample by detecting with a detection element German Patent No.
  • the present invention reduces, for example, the attenuation of the intensity in the optical path until the X-ray beam emitted from the X-ray tube reaches the sample, thereby having, for example, a polycrystalline body, distortion, and defects.
  • X-ray diffraction pattern with local structure information of a sample with a non-uniform crystal structure such as a member to be observed, especially a two-dimensional distribution image of diffraction X-ray intensity when focusing on a specific crystal lattice plane, It is an object of the present invention to provide an X-ray diffraction analysis apparatus and an X-ray diffraction analysis method that can be acquired in a short time and easily at a site where a structure requiring nondestructive inspection such as residual stress measurement is installed. To do.
  • the problem is that an X-ray diffraction pattern including local structure information of a sample having a non-uniform crystal structure that is fixed and held is used as an incident X-ray that illuminates the sample.
  • an X-ray diffraction analysis apparatus for acquiring using an X-ray tube that generates an image and a two-dimensional position-sensitive detector composed of a plurality of detector elements arranged two-dimensionally, the X-ray tube is The incident X-rays can illuminate the entire measurement area to be observed on the sample surface and are fixedly held at a position close to the sample as long as they are not in contact with the sample.
  • a position sensitive detector is arranged on the surface of the sample so as to be rotatable around a rotation axis extending perpendicularly to the optical axis of the incident X-ray through the center of the region to be measured. Diffracted and emitted from each part in the measurement area Angular divergence limiting means for limiting the angular divergence of the diffracted X-ray in order to distinguish and detect the diffracted X-rays with different detection elements of the two-dimensional position sensitive detector, respectively, around the rotation axis.
  • a two-dimensional diffraction X-ray image is formed and recorded so as to rotate integrally with a three-dimensional position sensitive detector, and each pixel value is the intensity of the diffraction X-ray detected by the detection element. This is solved by the X-ray diffraction analyzer.
  • an X-ray diffraction pattern including local structure information of a sample having a non-uniform crystal structure that is fixedly held is used as an X-ray tube that generates characteristic X-rays of a predetermined element as incident X-rays that illuminate the sample.
  • an X-ray diffraction analysis method for acquisition using a two-dimensional position-sensitive detector consisting of a plurality of detector elements arranged in two; ⁇ the light is emitted from an X-ray tube placed close to the sample. Then, illuminate the entire measurement area to be observed on the sample surface with incident X-rays incident on the sample without passing through any optical element, and it is diffracted by the sample and emitted from each part in the measurement area.
  • the diffracted X-rays emitted from each part can be detected in a two-dimensional position sensitive detector. And detecting the two-dimensional position sensitive detector through the center of the measurement area around the sample surface around the rotation axis extending perpendicular to the optical axis of the X-ray.
  • a two-dimensional position sensitive detector is held at a desired angular position by rotating it, and a two-dimensional diffraction X-ray image is formed with the intensity of the diffracted X-ray detected by each detector at that position as the pixel value.
  • the sample is fixed and held, that is, the sample is not moved during the measurement, and the incident X-rays illuminate the sample with a predetermined element.
  • the X-ray tube that generates X-rays is fixed and held at a position where it can illuminate the entire measurement area of the sample and as close as possible to the sample without touching the sample. That is, the X-ray beam generated in the immediate vicinity of the sample is incident on the sample without passing through any optical element that makes the X-ray beam monochromatic or collimated, so that the X-ray beam passes through the optical element.
  • the X-ray tube for generating incident X-rays is an X-ray tube for generating an X-ray beam having a linear thin rectangular cross section, and the major axis of the rectangular cross section is the rotation. If the X-ray tube is fixed and held so that the angle extending between the sample surface and the optical axis of the incident X-ray is 0 to 3 degrees, the X-ray tube is a sample. A large area of the sample can be illuminated uniformly even when placed close to the surface.
  • the X-ray tube can be exchanged, and the X-ray tube can be selected and used from among a plurality of X-ray tubes that generate characteristic X-rays of different elements. Then, depending on the sample, use of incident X-rays with a wavelength that does not generate fluorescent X-rays, and rotation (turning) of the two-dimensional position-sensitive detector
  • the target lattice plane when the angular range is limited For example, it is possible to use incident X-rays having such a wavelength that the diffraction angle becomes an angle convenient for measurement.
  • a mechanism for adjusting the distance between the X-ray tube and the sample and the angle formed by the sample surface and the optical axis of the incident X-ray is provided.
  • Optimal illumination of the measurement area by X-rays can be realized. Also, these adjustments are made before measurement, and once the measurement starts, the sample and the X-ray tube are not moved, so the mechanism may be manually operated.
  • the X-ray extraction window of the X-ray tube is made of a filter material that absorbs K) 3 rays out of the characteristic X-rays generated in the X-ray tube
  • Diffraction X obtained by using an X-ray beam mixed with both K j3 rays (which may include X-rays of other wavelengths, but can be ignored because the intensity is weak) as incident X-rays
  • Line components can be eliminated when the line image is adversely affected.
  • the rotation angle range of the two-dimensional position sensitive detector and the angle divergence limiting means is from a position of 60 degrees to a position of 120 degrees with respect to the sample surface. Since the rotation of the two-dimensional position sensitive detector and the sample is not hindered without a large separation, the apparatus can be configured compactly. For most samples, if the diffraction pattern is acquired within this rotation angle range, the purpose of imaging the distribution of the crystal structure and imaging the residual stress distribution can be sufficiently fulfilled.
  • the rotational angle position of the two-dimensional position sensitive detector is set.
  • the X Arrangement of two-dimensional position sensitive detectors close to each other can be realized.
  • the mechanism since this distance is fixed during the rotation angle scanning of the two-dimensional position sensitive detector, the mechanism may be a manually operated mechanism.
  • FIG. 1 is a conceptual diagram of an X-ray diffraction analyzer according to the present invention.
  • BEST MODE FOR CARRYING OUT THE INVENTION is a conceptual diagram of an X-ray diffraction analyzer according to the present invention.
  • FIG. 1 shows a conceptual diagram of an X-ray diffraction analyzer according to the present invention.
  • Sample 1 is fixed and held by the sample support 2 and is not moved during the measurement.
  • a two-dimensional position sensitive detector 3 consisting of a plurality of detector elements arranged two-dimensionally has a measurement area A in the same plane as the measurement area A to be observed on the sample surface by the detector support 4. It is held so that it can rotate (swivel) around the rotation axis 5 that extends through the center of the two-dimensional position-sensitive detector 3 detector surface at any rotation position.
  • a two-dimensional surface formed by the detection surfaces of all detection elements always looks at the measurement area A. Between the sample 1 and the two-dimensional position sensitive detector 3, the angle divergence of the diffracted X-rays 6 generated from the sample 1 and emitted from each part in the measurement area A on the sample surface is limited.
  • a collimator for example, a collection of synthetic quartz filaments
  • Angular divergence limiting means 7 such as the same processing of light metal by billiplate and lithography technology is provided. The angle divergence limiting means 7 is rotated around the rotation axis 5 integrally with the two-dimensional position sensitive detector 3.
  • each detection element detects only the diffracted X-rays 6 emitted from one specific part in the measurement area A, regardless of the rotation position of the two-dimensional position sensitive detector 3. .
  • the two-dimensional position sensitive detector 3 and the angle divergence limiting means 7 may be integrated. Although not shown in FIG. 1, the two-dimensional position sensitive detector 3 generates and records a two-dimensional diffraction X-ray image having the diffraction X-ray intensity detected by each detection element as each pixel value.
  • the image forming and recording unit is provided inside or outside.
  • X-ray tube 9 that generates characteristic X-rays of a given element and has a narrow rectangular cross section (linear focal point) and emits X-ray beams as incident X-rays 8 has the long axis of the rectangular cross section of incident X-rays 8 It is fixed and held by the X-ray tube support section 10 so as to be parallel to the rotation axis 5.
  • X-rays emitted from the X-ray tube 9 are divergent light, but at the time of emission from the narrow X-ray extraction window of the X-ray tube 9, the incident X-rays are X-ray beams having a nearly rectangular thin rectangular section. is there.
  • the incident angle at which the incident X-ray 8 is incident on the sample surface is a low angle of about 0 to 3 degrees with respect to the sample surface (however, it does not necessarily have to be smaller than 3 degrees).
  • the X-ray tube 9 is fixed and held so as to obtain a thin film arrangement.
  • the X-ray tube 9 On the incident X-ray optical path between the X-ray tube 9 and the sample 1, there is no monochromator for monochromatization or optical elements for collimation. As a result, the X-ray tube 9 can be placed as close as possible to the measurement area A as long as it does not contact the sample 1 or the sample support 2. How far the X-ray tube 9 is actually placed close to the measurement area A depends on where the sample 1 or its supporting part or the two-dimensional position sensitive detector 3 physically contacts the X-ray tube 9 For example, it can be set to about 50 mm to 70 mm.
  • the use of the above-described thin film arrangement is advantageous in that even when the X-ray tube 9 is brought close to the sample 1, the entire measurement area A can be illuminated uniformly with the incident X-ray 8.
  • the X-ray tube 9 and the sample 1 very close to each other, attenuation of incident X-rays by the atmosphere can be suppressed as much as possible without introducing a vacuum path.
  • Another great advantage is that no optical element is placed on the incident X-ray optical path, thereby eliminating the intensity attenuation caused by the optical element.
  • the incident X-ray 8 remains the divergent light generated by the X-ray tube 9 because it does not go through the optical element, but the incident X-ray 8 diverges because the X-ray tube 9 is placed very close to the sample 1.
  • the influence on the diffraction X-ray pattern acquired to be light can be ignored.
  • the above-mentioned measurement area A is an area that the two-dimensional position sensitive detector 3 expects when the sample surface is viewed as a two-dimensional surface, that is, diffraction that can be detected by the two-dimensional position sensitive detector 3. This refers to the area formed by the point where the X-ray 6 is emitted.
  • the sample surface becomes a two-dimensional surface. Only the diffracted X-rays 6 emitted from any part in the measured region A when viewed are detected by the detection element of the detector 3.
  • the emission site is determined as the position where the diffracted X-ray 6 is generated. At that time, the deviation between the actual generation position and emission position in the sample on the sample surface is only an error that can be ignored with respect to the resolution of the detector.
  • the measurement area A is almost the same size as the detector surface of the two-dimensional position sensitive detector 3. That's it. For example, if the detector surface of the two-dimensional position sensitive detector 3 is 10 mm square, the area A to be measured is also approximately 10 mm square. Therefore, in this case, the incident X-ray 8 is incident so that the distance between the X-ray tube 9 and the sample 1 can be as close as possible so that the area of the 10 mm square is uniformly illuminated at once. It is necessary to determine the incident angle of the X-ray 8 with respect to the sample surface.
  • the X-ray tube support portion 10 is provided with an X-ray tube position adjusting mechanism for that purpose.
  • the X-ray tube position adjustment mechanism is not required, such as when measuring only samples of approximately the same size and shape. Since the sample is not moved during the measurement while scanning the detector position at an angle, the distance between the X-ray tube 9 and the sample 1 is also fixed during the measurement.
  • this distance is based on the position closest to the sample surface within the range in which the two-dimensional position sensitive detector 3 and the angle divergence limiting means 7 that rotates integrally with the detector 3 do not block the incident X-ray 8. In consideration of avoiding contact with other members of the apparatus, a position farther than that may be selected.
  • the X-ray diffraction analyzer is a device whose primary object is to obtain information on the distribution of different structures existing in a sample by acquiring a diffraction X-ray intensity distribution image. Focus on structures with specific lattice spacing rather than using a wide range of scattering angles to obtain diffraction angles and diffracted X-ray intensities there, as is the case with conventional powder X-ray diffraction methods. By performing continuous or step scanning of the angle near the theoretical diffraction angle position corresponding to the lattice spacing, the distribution of the structure having the lattice spacing in the sample and the theoretical diffraction angle It is more effective to observe the deviation from the actual diffraction angle. In particular, in the case of specializing in the latter usage, the rotation angle range of the two-dimensional position sensitive detector 3 can be limited, and there is an advantage that the apparatus can be downsized.
  • the latter method is used, that is, one method for acquiring a diffraction X-ray image representing the distribution of a specific crystal structure in a sample. Is as follows. First, paying attention to a specific lattice plane of the crystal structure, the scattering angle corresponding to the theoretical diffraction angle corresponding to the plane spacing of the lattice plane.
  • the two-dimensional position sensitive detector 3 is moved to the position (angle formed by the optical axis of the incident X-ray and the optical axis of the diffracted X-ray). Finding the optimal angular position while continuously scanning the rotational position (scattering angular position) of the two-dimensional position-sensitive detector 3 centered on this position with incident X-rays 8 being irradiated, and diffracting X-ray image at the optimal angular position Is obtained, the diffraction X-ray intensity distribution for the lattice plane of interest is obtained. From that image, it is possible to specify in which part of the sample 1 the crystal structure of interest is observed.
  • diffraction X-ray images are respectively obtained at a plurality of detector rotation angle positions around the detector rotation angle position corresponding to the theoretical diffraction angle. It is possible to get.
  • the reason why the scattering angle position is scanned is that the theoretical diffraction angle and the actual diffraction angle do not always coincide with each other.
  • the diffraction angle is an angle with respect to the optical axis of the incident X-ray 8, it does not coincide with the exit angle of the diffraction X-ray 6 with respect to the sample surface unless the incident angle of the incident X-ray 8 is 0 degree.
  • the sample-detector distance is determined depending on the purpose, it is necessary to perform an angle scan of the detector as described above, and the sample-detector distance during the angle scan. With this in mind, it is necessary to be careful not to make contact between parts or block incident X-rays 8 at the maximum and minimum angles of the angular scanning range.
  • the distance between the sample and the detector is when the detector surface of the two-dimensional position sensitive detector 3 faces the sample surface (the angle of emission of the diffraction X-ray 6 with respect to the sample surface is 90 degrees).
  • the incident X-ray 8 can be made closest without interfering with the members and without contact between the members, such an arrangement is the arrangement with the highest detection efficiency in the X-ray diffraction analyzer according to the present invention.
  • this arrangement can shorten the distance between the sample and the detector to about 2 to 5 mm.
  • the two-dimensional position sensitive detector 3 is rotated so that the emission angle of the diffracted X-rays 6 that can be detected from this position is increased or decreased, the distance between the sample surface and the detector surface is increased.
  • the two-dimensional position sensitive detector 3 when the two-dimensional position sensitive detector 3 is rotated approximately 30 degrees from the position facing the sample surface, the distance between the sample and the detector is approximately 12 to 15 mm. However, it does not mean that measurement cannot be performed if it is further away. Considering that the distance between the sample and the detector is not too far away, the choice to use only diffracted X-rays 6 with an exit angle in the range of 60 to 120 degrees relative to the sample surface, i.e. It is fully conceivable that the rotational angle range of the three-dimensional position sensitive detector 3 is limited to this range. A grating plane that can detect diffracted X-rays 6 within this angular range should be selected as the grating plane of interest.
  • the X-ray tube 9 Since the X-ray tube 9 is replaceable, if an X-ray tube that generates characteristic X-rays with appropriate X-ray energy (wavelength) according to the object to be measured is selected from a plurality of X-ray tubes, Even if the rotation angle range of the 2D position sensitive detector 3 is limited, it can handle a sufficiently wide range of samples.
  • chrome wire from chrome tube (5 4 1 4 e V), iron ⁇ ⁇ ray from iron tube (6 4 0 3 e V), copper ⁇ : wire from copper tube (8 0 4 7 e V) Is selected by the following two criteria.
  • the diffraction angle (incident X-rays) corresponding to the lattice spacing of interest within the rotation angle range around the rotational axis 5 around which the two-dimensional position sensitive detector 3 can move. 8 and the angle formed by diffraction X-ray 6 (that is, the scattering angle) 2005/018063 Select to detect diffracted X-rays 6.
  • the angle of emission of the diffracted X-ray 6 from the target grating surface with respect to the sample surface is 60 to 120 degrees, preferably around 90 degrees.
  • Wavelength characteristics Select an X-ray tube 9 that generates X-rays.
  • pay attention to the absorption edge of the main component in the sample so that the diffraction image is not buried in the background by X-ray fluorescence.
  • X rays include ⁇ ] 8 rays. ⁇ ⁇ If the X-ray diffraction pattern is adversely affected by including the / 3 line, it is better to eliminate the line by using a filter material that absorbs ⁇ ⁇ -ray as the extraction window of the X-ray tube 9 . At this time, in order to place the X-ray tube 9 and the sample 1 close to each other, an optical element that absorbs three rays is not provided on the optical path of the incident X-ray, but a part of the X-ray tube 9 is provided. It is important to form the X-ray extraction window with a material that absorbs ⁇ rays. As filter material, titanium is promising for chromium tubes, manganese is for iron tubes, and Niggler metal foil is for copper tubes.
  • the sample support 2 is illustrated assuming that the X-ray diffraction analyzer according to the present invention is used in the laboratory, but the role of the sample support 2 is fixed so that the sample 1 does not move. Since it is to be held, if the sample 1 is a part of a fixed structure, the sample support 2 is naturally unnecessary. In such a case, the position of the sample cannot be moved from a fixed position, so the X-ray tube 9 and the two-dimensional position sensitive detector 3 are optimally suited to the location of the measurement area to be observed. Will be placed in position. On the other hand, in the case of equipment intended for use in the laboratory, a two-dimensional position sensitive detector
  • the procedure for determining the position of the X-ray tube 9 may be taken. In an apparatus for use in the laboratory, if the apparatus is configured so that the surface of Sample 1 is horizontal, even unstable samples such as precipitates from a solution can be measured. Can be targeted.
  • the two-dimensional position sensitive detector 3 has a multi-element semiconductor ⁇ X-ray detector and X-ray detection capability.
  • a CCD camera, a CMO S image sensor, etc. can be used.
  • With a CCD camera or CMOS image sensor that can detect X-rays directly it is also possible to distinguish diffraction X-rays from fluorescent X-rays by determining the detected X-ray energy from the amount of generated charges. It becomes.
  • the detector has a scintillation area that emits light by X-rays instead of directly detecting X-rays and detects the light emission of the scintillation area, there is no problem in implementing the present invention. There is no.
  • the image forming / recording unit generally includes a computer as a part thereof, but the function of the computer can also be configured to be built in the two-dimensional position sensitive detector 3 as a microchip.

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Abstract

L’invention concerne un tube à rayons X (9) générant des rayons X caractéristiques d’un élément spécifique comme rayons X incidents (8) pour éclairer un échantillon (1) fixé à demeure à un endroit auquel les rayons X incidents (8) peuvent entièrement éclairer la zone (A) de l’échantillon (1) à mesurer et sont proches de l’échantillon (1) mais sans toucher l’échantillon (1). Ainsi, l’atténuation d’intensité d’un faisceau à rayons X émis depuis le tube à rayons X (9) dans le trajet optique jusqu’à l’échantillon est minimisée. En conséquence, il est possible d’acquérir facilement une figure de diffraction aux rayons X englobant des informations structurelles locales sur l’échantillon ayant une structure cristalline inégale en un court laps de temps dans un laboratoire ou sur le site.
PCT/JP2005/018063 2005-03-09 2005-09-22 Analyseur de diffraction aux rayons x et procédé d’analyse WO2006095468A1 (fr)

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EP2818851B1 (fr) * 2013-06-26 2023-07-26 Malvern Panalytical B.V. Imagerie de diffraction

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