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CN-116194760-B - Laboratory-based 3D scanning X-ray Laue micro diffraction System and method (Lab 3D mu XRD)

CN116194760BCN 116194760 BCN116194760 BCN 116194760BCN-116194760-B

Abstract

A laboratory-based 3D scanning X-ray scanning laue micro-diffraction system and method for crystalline material characterization includes focusing optics, a sample located at a distance from the focusing optics, a laboratory X-ray source, a stage that translates and rotates the sample, a detector arranged to detect a laue diffraction pattern that diffracts X-rays. The method includes scanning each layer of the sample by translating the sample relative to the focused beam with a different rotation to illuminate each voxel in the layer in more than one rotation and indexing each voxel in the layer in a different rotation using the recorded luer diffraction pattern. By repeating the translation and rotation for different layers of the sample, a 3D image of the grain structure of the sample is reconstructed.

Inventors

  • ZHANG YUBIN
  • Dort Jules Johnson

Assignees

  • 丹麦技术大学

Dates

Publication Date
20260508
Application Date
20210712
Priority Date
20200715

Claims (19)

  1. 1. A method for generating 3D orientation imaging of a crystalline material, comprising: focusing a polychromatic X-ray beam (3) generated by a laboratory X-ray source (2) to a spot size diameter of less than 30 μm inside a sample (7) to produce a focused beam (5), Defining a first translation axis perpendicular to said focused beam (5), Defining a second axis of translation perpendicular to said first axis of translation and to said focused beam (5), Defining one or more layers in a predetermined metering volume of the sample (7) along the second axis of translation, -Scanning each layer of the sample (7) by Translating the sample (7) along the first translation axis at specific intervals, recording the resulting diffraction pattern for each translation step, Wherein each layer of the sample (7) is scanned under a different rotation of the sample (7) so that each voxel (15) in that layer is illuminated in more than one rotation, such that the luer diffraction pattern from each voxel (15) is recorded in at least two recordings, Wherein a layer is scanned by translating the sample (7) to the next layer along the second translation axis, -Indexing the recorded luer diffraction pattern (13) to reconstruct a 3D image of the grain structure of the sample (7).
  2. 2. The method according to claim 1, wherein the translation step along the first translation axis is selected based on the focused beam and the size of the sample (7), and the range of translation covers a part of the longest side or all of the longest side of the sample when rotated.
  3. 3. The method of claim 1, wherein the interval of rotation is on the order of 1 to 90 degrees and the interval of translation has a range of 1-30 μιη corresponding to spot size.
  4. 4. The method of claim 1, wherein the interval of rotation is the same for different rotations or varies for each rotation.
  5. 5. The method of claim 4, wherein the change in rotation comprises a first 30 degrees rotation followed by a 60 degrees rotation.
  6. 6. The method of claim 1, wherein rotation is summed up to a predetermined rotation range, the predetermined rotation range comprising any one of a quarter of a week, a half of a week, or a full of a week of the sample.
  7. 7. The method of claim 1, wherein the luer diffraction pattern is detected at different time intervals to produce a 4D image of the crystalline material, wherein time is a fourth dimension.
  8. 8. The method of claim 1, wherein the index is of a type of pattern matching, dictionary indexing, deep learning.
  9. 9. Laboratory-based 3D scanning X-ray laue micro-diffraction system (1) for characterizing crystalline material by performing the method according to claim 1, comprising: Focusing optics (4), A sample (7) located at a distance from the focusing optics (4), A laboratory X-ray source (2) for generating a polychromatic X-ray beam (3), -Said focusing optics (4) arranged in the path of said X-ray beam (3) between said X-ray source (2) and said sample (7) to produce a focused beam (5) having a spot size diameter of less than 30 μm at an image point inside said sample (7), said focused beam (5) diffracting from an inner sample volume (12) within said sample (7) illuminated by said focused beam (5) to produce diffracted X-rays (8), A stage (6) for holding the sample (7), the stage (6) being adapted to rotate and translate the sample (7) at specific intervals and angles with respect to the focused beam (5), -A detector (9) arranged to detect a luer diffraction pattern (13) of said diffracted X-rays (8).
  10. 10. The system according to claim 9, wherein a beam blocker (10) for blocking a transmitted beam (11) is arranged behind the sample (7), and/or a shield (16) is arranged between the sample (7) and the X-ray source (2), the shield (16) being for blocking the X-ray beam (3) from the X-ray source (2) that does not pass through the focusing optics (4).
  11. 11. The system of claim 9, wherein the laboratory X-ray source produces a polychromatic X-ray beam having an X-ray energy in the range of 5-150 keV.
  12. 12. The system of claim 9, wherein the focusing optics (4) focus the X-ray beam to a spot size diameter of less than 20 μιη.
  13. 13. The system of claim 12, wherein the focusing optics (4) focus the X-ray beam to a spot size diameter of less than 10 μιη.
  14. 14. The system of claim 13, wherein the focusing optics (4) focus the X-ray beam to a spot size diameter of less than 5 μιη.
  15. 15. The system of claim 14, wherein the focusing optics (4) focus the X-ray beam to a spot size diameter of less than 1 μιη.
  16. 16. The system according to claim 9, wherein the detector (9) is of the photon counting, flat panel, scintillator based CCD or CMOS detector type.
  17. 17. The system of claim 9, wherein the focusing optics (4) comprise at least one of a double parabolic X-ray mirror optic, an elliptical multi-capillary optic, KIRKPATRICK-Baez mirror.
  18. 18. The system according to claim 9, wherein two or more detectors (9) are arranged at different positions in the path of the diffracted X-rays (8), the detectors (9) having non-overlapping areas on a radial plane defined by the diffracted X-rays (8).
  19. 19. The system according to claim 9, wherein the detector (9) is placed 5-10 mm to 1 meter from the sample (7) and the focusing optics (4) is placed 20-50 mm from the sample (7), measured from the end of the focusing optics (4).

Description

Laboratory-based 3D scanning X-ray Laue micro diffraction System and method (Lab 3D mu XRD) Technical Field The present invention relates to the general field of crystalline material characterization using diffraction measurements. Background Characterization of crystalline materials can help scientists in industry and academia understand the characteristics of crystalline materials and the relationships between processing/manufacturing and characteristics/properties. This is accomplished by characterizing the crystal orientation of each crystal (also referred to as a grain) in the polycrystalline material using diffraction measurements, wherein the beam diffracts from a single grain and the diffraction pattern is recorded. In order to adequately characterize the sample, imaging of the 3D distribution of grain orientation is required. The first form of 3DXRD, 3D X-ray diffraction, was invented 20 years ago, in which a monochromatic hard X-ray beam from a high-flux synchrotron source penetrated the sample to a depth of a few centimeters in the case of aluminum or a few millimeters in the case of steel. In a 3DXRD experiment, a tomographic data acquisition procedure is performed using a layer or box beam that irradiates a section or a portion of the volume of the sample, respectively. High-energy X-ray diffraction microscopy and Diffraction Contrast Tomography (DCT) are branches of 3DXRD, which can characterize grains larger than a few microns, with spatial resolution as low as about 300nm, and standard resolution of about 1 μm. Currently, it remains challenging to characterize deformed materials using 3DXRD and provide local intra-crystalline strain information. Scanning 3DXRD can be used to improve spatial resolution and characterize local strain information using a focused monochromatic beam, where the sample volume is mapped after a series of translation and rotation steps. In all these cases, when monochromatic X-rays are used, the diffraction produced is bragg diffraction. Another form of synchrotron 3D characterization is the laue micro-diffraction technique in which polychromatic X-rays are focused by a non-dispersive KIRKPATRICK-Baez mirror to a size of about 0.5 μm and directed onto a sample. Pt wire or knife edge was used as the differential aperture to resolve where the luer diffraction occurred along the beam within the sample. The 3D volume mapping is achieved after horizontal and vertical translation of the sample. In the case of the laue micro-diffraction technique, there is no need to rotate the sample. One limitation of these techniques is that they require synchrotron facilities, which are costly to build and operate, and the available beam time is limited. In order to be able to characterize more materials faster and cheaper, it is important that these systems and techniques have to accommodate X-rays from laboratory sources. So far only one such system, the LabDCT system, has been developed. LabDCT systems are disclosed in US8385503B2 and US9383324B 2. US8385503B2 and US9383324B2 or US 2015/0316493 A1 disclose a system in which white/polychromatic divergent light from a laboratory X-ray source is directed through an aperture to a sample. In this system, sample translation is performed to align the sample. The X-ray beam directed at the sample is divergent, so that a volume of the sample is irradiated. The sample is rotated only during LabDCT data acquisition, so LabDCT works by using an aperture that confines the polychromatic cone-shaped X-ray beam to the desired volume. As the sample rotates, multiple diffraction spots from different lattice planes of the same grain can be recorded on the area detector with high signal to noise ratio. These points are used for indexing of crystal directions and reconstructing the 3D sample volume. However, currently, stress cannot be measured. Although LabDCT works with laboratory X-ray sources, it has inherent limitations due to the laue focusing effect, which requires that the crystal/grain be defect free. Further, it can map 3D grains only with a spatial resolution of 5-10 μm and is applicable only to grains larger than 20-30 μm. This is not sufficient since the typical grain size of most metals is in the range of 1-25 μm. Furthermore LabDCT is not able to characterize the deformed material nor is it able to determine the local lattice strain within individual grains. WO 2009/126868 A1 discloses an X-ray generation system using focused monochromatic X-rays, or X-rays having a limited discrete energy range instead of a continuous polychromatic spectrum, as described in US9383324B2, which are considered too low for DCT. The DCT was originally designed based on monochromatic synchrotron X-ray beams. Accordingly, an improved laboratory-based diffraction system and method would be advantageous, and in particular a system and method that can characterize small grains on the order of a few μm in size and determine local lattice strain and that can operate e