Position specifying method, position specifying device, and position specifying program

Abstract

To provide a position specifying method, a position specifying device and a position specifying program capable of specifying a position of a structure causing damage such as a crack in a sample in a single crystal state from a change of an obtained diffraction image.SOLUTION: A position specifying method for specifying a position of a target structure in a sample includes a step of vertically irradiating an S1 of a sample in a single crystal state with white X-rays R10, a step of acquiring a diffracted image generated by the radiation, and a step of moving an irradiated position on the S1 of the sample.SELECTED DRAWING: Figure 1

Description

[Technical Field]

[0001] The present invention relates to a position specifying method, a position specifying device, and a position specifying program for specifying the position of a target structure within a sample. [Background technology]

[0002] X-ray diffraction is a conventional method for measuring damage in components used under high-temperature, high-load environments. Damage diagnosis methods for nickel-based superalloys have advanced rapidly in recent years, and it is now possible to perform non-destructive testing of thick metal materials, even deep within them, using high-energy X-rays.

[0003] Patent Document 1 discloses a method for diagnosing sample degradation by placing a sample so that the damage direction is parallel to the surface of the sample holder, measuring the diffraction image obtained by the reflection Laue method for the single-crystal sample with a two-dimensional detector, and calculating the full width at half maximum (FWHM) in the damage direction. This method eliminates the need for complicated work and allows measurement and analysis in a laboratory.

[0004] In response to this, Patent Document 2 discloses a method in which a single-crystal sample is irradiated with a thin beam of white X-rays, a coefficient for the variance of the intensity distribution in a specific direction in the resulting diffraction spot is calculated, and the state of damage in the sample is identified from the coefficient. This method makes it possible to measure damage in a single-crystal sample without removing a thermal barrier coating, for example, when a nickel-based superalloy, such as a turbine blade for thermal power generation, is coated with a thermal barrier coating having a thickness of 100 μm or more. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] Patent No. 7093929 [Patent Document 2] Japanese Patent Application Publication No. 2023-140749 Summary of the Invention [Problem to be solved by the invention]

[0006] The nickel-based superalloys that are the main target of the damage diagnosis methods described above are metallic materials with a single-crystal dendritic structure. For example, in the method described in Patent Document 1, a white X-ray beam is irradiated onto a sample by the Laue method, and the half-width of the diffraction peak is measured.

[0007] However, metal materials with such dendritic structures contain a mixture of multiple single-crystal grains. For example, there are regions where two large grains are separated, and regions where small, separate grains exist within a large grain. In either of these regions, if the material is left in a harsh environment for a long period of time, cracks or other damage may occur at the grain boundaries between adjacent grains.

[0008] However, although the above-mentioned analysis of transmission Laue images can determine the orientation of a single crystal, it cannot distinguish the grain boundaries that exist between those grains, and it cannot detect the presence of foreign grains in a thick material.

[0009] The present invention has been made in consideration of the above circumstances, and aims to provide a position identification method, a position identification device, and a position identification program that can identify the position of a structure that causes damage such as cracks in a single crystal sample from changes in the obtained diffraction image. [Means for solving the problem]

[0010] (1) In order to achieve the above object, the position identification method of the present invention is a position identification method for identifying the position of a target structure within a sample, and includes the steps of irradiating the surface of a single-crystal sample with white X-rays, acquiring a diffraction image generated by the irradiation, and moving the irradiation position on the surface of the sample, and is characterized in that the position of the target structure is identified based on the diffraction image acquired by scanning measurement through repetition of the series of steps from irradiation to movement.

[0011] (2) Furthermore, in the position identification method described in (1) above, the irradiation is vertical irradiation in a direction perpendicular to the surface of the sample, and the position of the target structure is a position on a plane parallel to the surface of the sample.

[0012] (3) Furthermore, in the position identification method described in (2) above, the target structure is a grain boundary, and the position of the grain boundary is identified from the deviation of the relative positional relationship of the diffraction points based on the acquired diffraction image.

[0013] (4) Furthermore, in the position identification method described in (3) above, the scanning measurement is performed twice, and in one of the two scanning measurements, the irradiation is performed as normal irradiation in a direction perpendicular to the surface of the sample, and in the other of the two scanning measurements, the irradiation is performed as oblique irradiation in a direction tilted with respect to the surface of the sample, and the position of the target structure perpendicular to the surface of the sample is identified based on the acquired diffraction image.

[0014] (5) Furthermore, in the position identification method described in (3) above, the target structure is a heterocrystalline grain, and the three-dimensional position of the target structure is identified from the overlap of diffraction points on the diffraction image of the base material.

[0015] (6) Furthermore, the position identification device of the present invention is a position identification device that identifies the position of a target structure within a sample, and is characterized by including: a diffraction image memory unit that stores the diffraction images obtained by repeatedly irradiating the surface of a single-crystal sample with white X-rays and moving the irradiation position on the surface of the sample; and a position identification unit that identifies the position of the target structure based on changes in the stored diffraction images.

[0016] (7) Furthermore, the position identification program of the present invention is a position identification program for identifying the position of a target structure within a sample, characterized in that it causes a computer to execute the following processes: obtaining a diffraction image by irradiating a surface of a single-crystal sample with white X-rays and repeatedly moving the irradiation position on the surface of the sample, thereby storing the obtained diffraction image; and identifying the position of the target structure based on changes in the stored diffraction image. [Brief explanation of the drawings]

[0017] [Figure 1] FIG. 1 is a schematic diagram showing vertical irradiation of a sample with X-rays and scanning thereof. [Figure 2] 1 is a schematic diagram showing oblique irradiation of a sample with X-rays and scanning thereof. [Figure 3] 1 is a schematic diagram showing the configuration of a position specifying system of the present invention. [Figure 4] 1 is a block diagram showing a configuration of a position specifying device according to the present invention; [Figure 5] 10 is a flowchart illustrating a method for determining location using normal illumination only. [Figure 6] 10 is a flowchart illustrating a method for determining a position using normal illumination and oblique illumination. [Figure 7] FIG. 1 is a schematic cross-sectional view of a sample used in an experiment. [Figure 8] (a) and (b) are diffraction patterns generated at specific positions within the sample. [Figure 9] 1 is a schematic diagram showing X-ray irradiation and scanning of a sample in an experiment. [Figure 10] (a) to (f) are side photographs showing the layout inside the device at y=0 to 5, respectively. [Figure 11] (a)~(f) are diffraction images at y=0~5, respectively. DETAILED DESCRIPTION OF THE INVENTION

[0018] Next, an embodiment of the present invention will be described with reference to the drawings. To facilitate understanding of the description, the same reference numerals are used to designate the same components in the drawings, and duplicated descriptions will be omitted.

[0019] [principle] In single-crystal samples, where multiple single-crystal grains are mixed in some regions, cracks and other damage may occur at the grain boundaries between adjacent grains if the sample is placed in a harsh environment. Therefore, it is important to identify the location of target structures, such as grain boundaries and deformed grains.

[0020] The term "single crystal state" refers to a state in which a material is formed of a single crystal or coarse crystal grains. In other words, the "single crystal state" refers to a state in which a sample is formed of a single crystal or coarse crystal grains in which the X-ray beam diameter can be shaped to irradiate a portion of a single crystal or a single coarse crystal grain within the material. The principle will be explained below with reference to a specific example.

[0021] (Grain boundary location) Figure 1 is a schematic diagram showing the perpendicular irradiation of X-rays onto sample S1 and the scanning of the X-rays. When it is desired to identify the orientation of crystal grain A and crystal grain B in sample S1, which is in a single crystal state, diffraction images are observed continuously within the region of interest. If there is a discrepancy in the relative positions of the diffraction points present in the two observed diffraction images, it can be inferred that a grain boundary E1 exists between the two crystal grains. Note that the term "diffraction point" is almost synonymous with the term "diffraction spot," but while the term "diffraction spot" focuses on the spread, the term "diffraction point" focuses on the peak position.

[0022] When white X-rays R11 are irradiated perpendicularly (direction D1) onto the surface F1 of a single-crystal sample S1, a diffraction pattern dependent on the orientation of the single crystal can be obtained by the transmission Laue method. High-energy white X-rays are preferable. High-energy X-rays result in a small diffraction angle, resulting in a diffraction spot detected at a low angle. High-energy X-rays allow measurement through thick metal samples. Multiple diffraction images can be obtained by moving the irradiation position parallel to the surface F1 of the sample S1 (direction G1) and scanning the diffraction image. The relative positions of the diffraction peaks in the diffraction image provide information on the positions of the diffraction peaks of grain A and grain B. Scanning measurement refers to the acquisition of diffraction image data by repeating a series of steps, from irradiation to scanning. The diameter of the irradiated X-ray beam can be varied depending on the purpose. For example, a large X-ray beam diameter can be used to simply confirm the presence of grain boundaries, while a small X-ray beam diameter can be used to precisely determine the location of grain boundaries.

[0023] In this way, it is possible to detect position information where a diffraction image containing a mixture of diffraction peaks from both crystal grains is obtained. Therefore, the position Lg where the crystal grain boundary E1 exists can be detected by analyzing the position information of the diffraction peak. In other words, based on the obtained diffraction image, the parallel position Lg of the crystal grain boundary E1 can be identified from the deviation in the relative positional relationship of the diffraction points.

[0024] Although two-dimensional scanning along the surface F1 of the sample S1 may be performed, scanning measurement using the Laue method along the detected grain boundary E1 can also efficiently detect the grain boundary E1 throughout the entire sample S1. In this way, the parallel position of the target structure (position on a plane parallel to the sample surface) can be identified based on the acquired diffraction image. In other words, the parallel position of the target structure, which is the cause of damage such as cracks in a single-crystal sample, can be identified from changes in the obtained diffraction image.

[0025] (Identifying the location of different crystal grains) Figure 2 is a schematic diagram showing oblique irradiation of X-rays onto sample S2 and the scanning of the X-rays. When it is desired to detect a relatively small deformed crystal grain C present within crystal grain B, the position of the deformed crystal grain C can be estimated if the diffraction points originating from the deformed crystal grain C are observed to overlap in the diffraction images at two observation points.

[0026] In a thick metallic material with a dendritic structure in a single crystal state, when a different crystal grain C is contained within sample S2, the diffraction image obtained by the transmission Laue method, which includes the diffraction positions of the different crystal grains, naturally includes the diffraction image from the different crystal grain C in addition to the diffraction image from the crystal grain B of the base material. Therefore, by performing scanning measurements of the diffraction image using white X-rays R21 incident perpendicularly to the surface F2 of sample S2 and scanning measurements of the diffraction image using white X-rays R22 incident obliquely, the three-dimensional diffraction positions of the different crystal grains within sample S2 can be detected. Scanning measurements refer to the acquisition of diffraction image data by repeating a series of steps from irradiation to movement.

[0027] When white X-rays are irradiated perpendicularly to the surface F2 of the sample S2 (direction D1), a diffraction pattern dependent on the orientation of the single crystal can be obtained by the transmission Laue method. Then, by moving the irradiation position parallel to the surface F2 of the sample S2 (direction G1) and scanning the diffraction image, multiple diffraction images can be obtained. By analyzing the relative diffraction peak information in the multiple diffraction images, the diffraction peak position Ld from the deformed crystal grain C can be detected. If the deformed crystal grain C is detected during the in-plane movement, the step of tilting the incident direction of the white X-rays from the direction D1 perpendicular to the surface F2 of the sample is performed.

[0028] Next, the diffraction region in sample S2 detected by the normal incidence of white X-rays is irradiated with white X-rays obliquely in a direction (D2) tilted by an angle δ from the direction D1 perpendicular to the surface F2 of sample S2, to obtain a diffraction image. Then, while maintaining the tilt angle δ, the irradiation position on sample S2 is moved (direction G2) at a constant interval and the acquisition of diffraction images is repeated, performing scanning measurement. In other words, diffraction image data is obtained by repeating a series of steps from irradiation to movement. Note that in the two measurements above, the white X-rays are incident on the same plane.

[0029] In principle, oblique irradiation is performed by tilting the surface F2 of sample S2 by an angle -δ relative to the X-ray irradiation direction. However, the tilt is relative, and the irradiation direction itself of the X-ray irradiator can also be tilted. As shown in Figure 2, the depth position D of the deformed crystal grain (perpendicular to the sample surface) can be determined from the angle δ and the oblique X-ray scanning distance Δ. The irradiation position where the diffraction spot overlaps with the diffraction image of the base material is the location of the deformed crystal grain C. By identifying the position Ld on the plane parallel to the surface F1 of sample S2 and the depth position D, it is possible to determine the location of the target structure within the plane formed by the normal and oblique X-ray incidence directions. In this way, by scanning and measuring the diffraction images of the X-rays incident on the surface F2 of sample S2 with both normal and oblique incidence, the three-dimensional position of the target structure within sample S2 can be detected.

[0030] As with the search for grain boundaries, the X-ray beam diameter may be selected depending on the purpose. If the purpose is to confirm the presence of foreign crystal grains, it is preferable to select a large X-ray beam diameter. If the three-dimensional position of foreign crystal grains is to be determined with high precision, it is preferable to select a small X-ray beam diameter. However, even when confirming the presence of foreign crystal grains, selecting a large X-ray beam diameter may result in diffraction spots from many crystal grains, making it impossible to identify the diffraction spot originating from the target crystal grain. In such cases, it is preferable to select an appropriate X-ray beam diameter depending on the sample.

[0031] [Target samples] The specimens targeted by the present invention are in a single crystal state. The present invention is particularly effective for metallic specimens, large thick specimens, plate-shaped specimens, or specimens with a combination of these characteristics. The specimen is preferably formed of a Ni-based superalloy material having a dendritic structure in a single crystal state. This increases the effectiveness when applied to, for example, turbine blades for thermal power generation.

[0032] In thermal power plants, generators are equipped with multiple turbine stages lined up depending on the purpose. Nickel-based superalloys are used for the turbine blades (moving blades) of the three to four stages, which are particularly exposed to high-temperature environments. Directionally solidified blades or single-crystal blades are particularly used for the first and second stage turbine blades. The directionally solidified material used as turbine blade material is made of nickel-based superalloys and is formed as a rod-shaped single crystal several millimeters wide, and is in a single-crystal state.

[0033] The subgrains of nickel-based superalloys are composed of a single crystal composite material consisting of a nickel solid solution matrix (γ phase (gamma phase)) and a nickel-based intermetallic compound precipitate phase (γ' phase (gamma prime phase)). The γ phase has an fcc structure with a face-centered cubic lattice of Ni atoms. The γ' phase has a cubic superlattice structure in which atoms at each corner of the face-centered cubic lattice are replaced by Al or Ti atoms.

[0034] In nickel-based superalloys, countless γ' phase clusters are regularly arranged in three dimensions, and a network-structured framework of γ phase surrounds each γ' phase cluster, forming a single crystal. Although it is a composite material consisting of different phases, the orientation of each phase is consistent. In this way, in nickel-based superalloys, the γ' phase is coherently dispersed within the γ phase, forming a single crystal state.

[0035] When white X-rays are irradiated onto a single-crystal base material, diffraction spots known as Laue spots appear. The crystal orientation is consistent within a single crystal grain, but differs between adjacent crystal grains. Furthermore, if a specific group of crystal grains contains different crystal grains, the diffraction spots of the different crystal grains will appear superimposed on the diffraction image of the basic structure. When a single-crystal base material is not deformed at all, Laue spots appear with a circular periphery, but as the material deforms, the periphery of the Laue spots changes from a circle to an ellipse, and the major axis of the ellipse elongates. Damage can be detected by the elongation of the major axis.

[0036] [Location Identification System] A system used to identify the position of a target structure will be described. FIG. 3 is a schematic diagram showing the configuration of a position identification system 100. The position identification system 100 includes an X-ray diffraction apparatus 110 and a processing device 150 (position identification device). The X-ray diffraction apparatus 110 is an apparatus used for measurements to detect diffraction patterns. The processing device 150 is an apparatus that mainly identifies the position of a target structure from the detected diffraction patterns. The X-ray diffraction apparatus 110 and the processing device 150 are preferably connected so that they can send and receive information, whether wired or wireless. The processing device 150 may also be located on the cloud.

[0037] [X-ray diffractometer] The following describes the basic configuration of the X-ray diffraction apparatus 110. The X-ray diffraction apparatus 110 includes an X-ray irradiation unit 120, a sample holder 130, a position adjustment mechanism 135, and a detector 140.

[0038] The X-ray irradiation unit 120 includes a main body 121 and a collimator 122, and generates white X-rays to irradiate the sample S0. The main body 121 includes a housing, an X-ray source, and an X-ray shielding window. The X-ray source preferably uses a finely focused X-ray target and generates a narrow beam of white X-rays. Here, "narrow beam" refers to an X-ray beam with a size equivalent to the size of the grain boundary or heterocrystalline grain to be detected. The X-rays pass through the X-ray shielding window and are emitted to the outside.

[0039] The collimator 122 has a collimator body and a shielding cover, and can form a narrow beam of X-rays. The shielding cover is preferably made of, for example, lead. It is preferable to use the collimator 122 to adjust the beam size to match the size of the subgrains of the sample. Two pieces of information, the degree of damage to the sample and the direction of the damage, can be simultaneously evaluated from the diffraction spots. The direction in which the damage occurs can be identified from the extension direction of the detected diffraction spots.

[0040] The sample holder 130 can mount a sample as a measurement target to be irradiated with white X-rays, and can be fixed by adjusting its position to the X-ray irradiation position. The sample holder 130 is configured so that its angular position can be adjusted in three axes by a position adjustment mechanism 135, as shown in Figure 7.

[0041] The position adjustment mechanism 135 makes it possible to adjust the angle of the lattice plane of the sample relative to the irradiated white X-rays. The angular position of the sample can be adjusted by a motor or the like in response to a control signal from the processing device 150. Incident X-rays R1 emitted from the X-ray irradiation unit 120 are diffracted by the sample S0 to generate diffracted X-rays R2, which generate multiple diffraction spots in space.

[0042] The position adjustment mechanism 135 can adjust the angle of the X-ray incidence axis from the X-ray irradiation unit 120 so that the diffracted X-rays are incident on the detector 140. The position adjustment mechanism 135 can adjust the tilt of the sample holder 130. The position adjustment mechanism 135 can move the sample S0 in a direction parallel to its surface in response to a control signal from the processing device 150.

[0043] The lattice planes of sample S0 are the lattice planes of the single crystal of the base material. The incident X-rays are diffracted by the sample, generating multiple diffraction spots in space. The positions of the diffraction spots are determined according to the lattice planes present in sample S0.

[0044] The detector 140 generates an electrical signal according to the intensity of the X-rays incident on the detection surface, thereby detecting the diffraction spots generated by the sample S0. The detector 140 is preferably a two-dimensional detector in order to easily detect the shape of the diffraction spots, and specifically, an imaging plate or a semiconductor detector can be used.

[0045] The position of the X-ray direct beam DB1 is 2θ = 0. The angle of the detector 140 with respect to the sample S0 is represented by β, and the angle of incidence of the X-rays with respect to the sample S0 is represented by α. The angle of incidence α and the angle β of the detector 140 are usually fixed, and during measurement, none of the X-ray irradiation unit 120, the sample holder 130, and the detector 140 are moved.

[0046] [Processing equipment] 4 is a block diagram showing the configuration of the processing device (position identification device) 150. The processing device 150 can be configured as a device equipped with a CPU and memory, such as a PC, and controls the X-ray diffraction device 110 and processes detected data by executing a program. The processing device 150 includes an input / output control unit 151, a position control unit 152, a scan control unit 153, a diffraction image storage unit 155, a diffraction image display unit 156, and a position identification unit 159.

[0047] The processing device 150 is connected to an input device 160 and an output device 170. The input device 160 is a device that accepts input from a user, such as a mouse, a touch panel, or a keyboard. The output device 170 is a device such as a display or a printer.

[0048] The processing device 150 processes data and controls the device in response to input of position information of the X-ray irradiation unit 120, the sample holder 130, and the detector 140, input of instructions from the user, and input of measurement results from the detector 140. The processing device 150 outputs the position of the target structure as a result of position identification. It may also output a diffraction image captured for each position.

[0049] The input / output control unit 151 receives instructions from the user and outputs measurement results and processing results. For example, the input / output control unit 151 receives a designation of an area in which the position of a target structure within a sample is to be identified. The initial position for irradiating X-rays and the increment width for scanning can be determined according to the designated area.

[0050] The position control unit 152 controls the arrangement of the X-ray irradiation unit 120, the sample holder 130, and the detector 140 based on the input information. The position control unit 152 can adjust the tilt of the sample holder 130 via the position adjustment mechanism 135. The position control unit 152 controls the incident direction of the white X-rays by adjusting the arrangement of the sample relative to the X-ray irradiation unit 120. This enables perpendicular irradiation, in which the incident direction of the white X-rays is perpendicular to the sample surface, or oblique irradiation, in which the incident direction is tilted at a certain angle.

[0051] The scan control unit 153 moves and stops the position where X-rays are irradiated within the region where the position of the target structure is to be identified. The movement interval is adjusted depending on the type of vertical or oblique irradiation and the size of the target structure. The start and end positions of the scan are determined depending on the specified region.

[0052] The diffraction image storage unit 155 stores the diffraction images obtained by detecting the diffraction lines generated at each irradiation position of the white X-ray. This diffraction image is obtained by obtaining a diffraction image by vertically irradiating the surface of the single-crystal sample with the white X-ray and repeatedly moving (scanning) the irradiation position on the surface of the sample. At this time, the type of irradiation, the irradiation position, and the diffraction image are stored as corresponding data.

[0053] The diffraction image display unit 156 displays the acquired diffraction image together with the irradiation position on the output device 170. Based on the display, the user can check the diffraction image obtained by scanning and specify diffraction images before and after a shift in the diffraction points occurs. The user can also specify a diffraction image in which the diffraction points of different crystal grains overlap. The user's specification is performed by the input / output control unit 151.

[0054] The position identifying unit 159 identifies the position of the target structure based on a change in the specified diffraction image. Specifically, the position of the target structure is identified based on the irradiation position at which the diffraction image with the change (shift or overlap of diffraction points) specified by the user was acquired. For example, the position between the irradiation position where the shift of the diffraction points was confirmed and the irradiation position immediately before that can be identified as the position of the grain boundary. Furthermore, the parallel position of the different crystal grains can be identified from the position of perpendicular irradiation where the overlap of the diffraction points was confirmed, and the vertical position of the different crystal grains can be identified from the position of oblique irradiation where the overlap of the diffraction points was confirmed.

[0055] (Location method) A method for locating a target structure in a sample using the location identification system 100 configured as described above will now be described. First, a method for identifying the parallel position of the sample (a position on a plane parallel to the sample surface) using only normal illumination, such as when identifying the position of a grain boundary, will be described. Figure 5 is a flowchart showing the location identification method when only normal illumination is used.

[0056] First, a single-crystal sample is placed (step S01), and the incident direction of white X-rays is adjusted so that it is perpendicular to the sample surface (step S02). The incident direction is basically adjusted by adjusting the orientation of the sample, but it may also be adjusted by adjusting the orientation of the X-ray irradiation unit.

[0057] The sample is set at the initial position of the scan, and parameters such as the step size and end position are set according to the target structure and type of irradiation to perform initialization (step S03). Then, X-rays are irradiated onto the sample, and a diffraction image is detected, acquired, and stored together with position information (step S04). Next, it is determined whether the scan has ended (step S05).

[0058] If the scan is not complete, the X-ray irradiation position is further controlled to move in increments (step S06), and the process returns to step S04. This repeats the acquisition of a diffraction image by vertical irradiation with white X-rays and the movement of the irradiation position on the sample surface.

[0059] On the other hand, if the scanning has been completed, the diffraction images detected by the scanning are displayed in the order of movement (step S07). The user specifies a diffraction image with a shifted diffraction point, and the position specifying device 150 accepts the input (step S08). Then, the position of the target structure is specified based on the input diffraction image specification (step S09), and the series of steps is completed.

[0060] Next, we will explain how to determine the parallel and vertical positions of a sample (positions on a line perpendicular to the sample surface) using normal and oblique irradiation, as in the case of determining the position of a foreign crystal grain. Figure 6 is a flowchart showing the method for determining the position when normal and oblique irradiation are used.

[0061] First, a single-crystal sample is placed (Step T01), and the incident direction of the white X-rays on the sample surface is adjusted (Step T02). In one scan, the incident direction is adjusted to be perpendicular to the sample surface, and in the other scan, the incident direction is adjusted to be tilted at a predetermined angle δ from the perpendicular direction to the sample surface.

[0062] The sample is set at the initial position of the scan, and parameters such as the step size and end position are set according to the target structure and type of irradiation to perform initialization (step T03). Then, X-rays are irradiated onto the sample, and a diffraction image is detected, acquired, and stored together with position information (step T04). Next, it is determined whether the scan has ended (step T05).

[0063] If the scan is not completed, the X-ray irradiation position is further controlled to move in increments (step T06), and the process returns to step T04. This repeats the acquisition of diffraction images by vertical or oblique irradiation of white X-rays and the movement of the irradiation position on the sample surface (scan control).

[0064] On the other hand, if the scan has ended, it is determined whether the measurement has ended (step T07). If the measurement has not ended, the process returns to step T02, the incident direction of the X-rays is adjusted (step T02), the irradiation position is moved to the initial position of the next scan, and the parameters are also set to their initial values ​​(step T03). Then, scan control (steps T04 to T05 are repeated) is performed until the scan ends.

[0065] If the measurement is completed in step T07, the process proceeds to step T08, where a series of diffraction images are displayed in order of movement, classified by the type of irradiation (step T08).

[0066] The user specifies a diffraction image with a shifted diffraction point, and the position specifying device 150 accepts the input (step T09). Then, the position of the target structure is specified based on the input diffraction image specification (step T10), and the series of steps ends. In this way, the position of the structure that causes damage such as cracks in the single crystal sample can be specified from the change in the obtained diffraction image.

[0067] In the above example, the position of the target structure is identified based on the changes in the diffraction image specified by the user after checking the displayed diffraction image. However, changes in the diffraction image can also be identified by computer processing. For example, if the crystalline structures of the base material and the target structure are known, predicted changes in the diffraction image can be set as conditions. It is also possible to identify the diffraction image and its changes using image recognition using AI.

[0068] [Example] (Example of detecting grain boundaries) Figure 7 is a schematic cross-sectional view of sample S3, the subject of the experiment. As shown in Figure 7, by irradiating white X-rays perpendicularly to sample surface F3 and scanning the transmission Laue image, it was possible to detect the diffraction images and position information for each of crystal grains A and B. By irradiating white X-rays perpendicularly to sample surface F3 and scanning the irradiation positions P31 to P34 of crystal grains A and B using the transmission Laue method, the diffraction images and position information for each of crystal grains A and B were obtained.

[0069] Figures 8(a) and (b) show diffraction images generated at specific positions within the sample. Figures 8(a) and (b) show the diffraction images of (110) crystal grain A at irradiation position P32 and (111) crystal grain B at irradiation position P33, respectively. The position information of the crystal grain boundary E3 was obtained from the differences in the relative positions of the diffraction peaks in the measured multiple transmission Laue images. Thus, it was confirmed that the position of the crystal grain boundary E3 can be identified using the method of the present invention.

[0070] (Example of detection of different crystal grains) Figure 9 is a schematic diagram showing the X-ray irradiation and scanning of sample S4 in the experiment. As shown in Figure 9, a hypothetical heterocrystalline sample S42, 1.5 mm thick and 3 mm wide, was placed on the back of base material sample S41, 1.5 mm thick and 10 mm wide. White X-rays R41 were irradiated perpendicularly to the surface F4 of sample S4 using the transmission Laue method, and a diffraction image was obtained. During the measurement, sample S4 was moved 1 mm at a time in the width direction to obtain a diffraction image.

[0071] Figures 10(a) to (f) are side photographs showing the arrangement inside the apparatus for y = 0 to 5, respectively. Figures 11(a) to (f) are diffraction images for y = 0 to 5, respectively. The diffraction images measured at the arrangements (y = 0 to 5) shown in Figures 10(a) to (f) are the diffraction images shown in Figures 11(a) to (f), respectively. X-rays are irradiated at the cross points (white dots in the photographs) where the laser beam hits in each arrangement. The white circles shown in Figures 11(c) to (e) contain diffraction peaks from the deformed crystal grains. In this way, it was confirmed that the position of the deformed crystal grains can be identified using the method of the present invention. [Explanation of symbols]

[0072] 100 Location System 110 X-ray Diffraction Equipment 120 X-ray irradiation section 121 Main body 122 Collimator 130 Sample holder 135 Position adjustment mechanism 140 detectors 150 Processing device (location identification device) 151 Input / Output Control Unit 152 Position control section 153 Scanning control section 155 Diffraction image storage unit 156 Diffraction image display unit 159 Location identification part 160 Input Devices 170 Output Device A grain B grain C Heterogeneous grain Lg, Ld, D position D1 direction DB1 Direct Beam E1 Grain boundary E3 grain boundary F1~F4 surface G1, G2 movement direction Ld diffraction peak position P31~P34 Irradiation position R1, R2, R41 X-ray S0 sample S1 Sample S2 sample S3 Sample S4 Sample Δ Scanning distance δ Predetermined angle

Claims

1. 1. A method for locating a structure of interest within a sample, comprising: irradiating a surface of a single crystal sample with white X-rays; acquiring a diffraction image produced by said irradiation; and moving the irradiation position on the surface of the sample; A position identification method, characterized in that the position of a target structure is identified based on a diffraction image acquired by scanning measurement through repetition of a series of steps from irradiation to movement.

2. the irradiation is normal irradiation in a direction perpendicular to the surface of the sample, 2. The position specifying method according to claim 1, wherein the position of the target structure is a position on a plane parallel to the surface of the sample.

3. the target structure is a grain boundary, 3. The position specifying method according to claim 2, wherein the position of the grain boundary is specified from a deviation in the relative positional relationship of diffraction points based on the acquired diffraction image.

4. The scanning measurement is performed twice, In one of the two scanning measurements, normal irradiation in a direction perpendicular to the surface of the sample is performed as the irradiation; In the other of the two scanning measurements, the irradiation is performed obliquely in a direction inclined with respect to the surface of the sample; 2. The position specifying method according to claim 1, wherein the position of the target structure perpendicular to the surface of the sample is specified based on the acquired diffraction image.

5. the target structure is a heterocrystalline grain, 5. The method for identifying a position according to claim 4, wherein the three-dimensional position of the target structure is identified from the overlap of diffraction points on a diffraction image of the base material.

6. 1. A localization device for locating a structure of interest within a sample, comprising: a diffraction image storage unit that stores the diffraction images obtained by repeatedly irradiating a surface of a single-crystal sample with white X-rays and moving the irradiation position on the surface of the sample; and a position specifying unit that specifies the position of a target structure based on a change in the stored diffraction image.

7. a location identification program for identifying a location of a target structure within a sample, a process of acquiring a diffraction image by irradiating a surface of a single-crystal sample with white X-rays and storing the acquired diffraction image by repeatedly moving the irradiation position on the surface of the sample; and a process of identifying the position of the target structure based on the change in the stored diffraction image.

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