Structure evaluation method, structure evaluation apparatus, and structure evaluation program

By using a slit to selectively pass diffracted X-rays from specific regions of a large single-crystal sample, the method addresses the challenge of evaluating damage in thick metal materials, providing precise and non-destructive structural assessment.

JP2026002046APending Publication Date: 2026-01-08RIGAKU CORP +1
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Patent Information

Application Number
JP2024099736
Authority / Receiving Office
JP · JP
Patent Type
Applications
Current Assignee / Owner
Filing Date
2024-06-20
Publication Date
2026-01-08

AI Technical Summary

Technical Problem

Existing methods for measuring damage in thick metal materials under high-temperature, high-load environments, such as turbine blades, struggle to distinguish between diffracted X-rays generated from different regions, making it difficult to evaluate the damage in specific areas accurately.

Method used

A method involving the use of a slit to selectively pass diffracted X-rays from specific regions of a large single-crystal sample, allowing for the evaluation of each region's structure by detecting and comparing diffraction spots, and calculating the damage state and life consumption rate based on the variance of intensity distribution in the diffraction spots.

Benefits of technology

Enables precise, non-destructive evaluation of the structural damage in each region of thick metal materials by distinguishing between diffracted X-rays, facilitating accurate damage assessment and life prediction.

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Abstract

To provide a structure evaluation method, a structure evaluation device, and a structure evaluation program capable of distinguishing diffracted X-rays generated for each region and evaluating each structure.SOLUTION: A structure evaluation method performed by measuring diffracted X-rays transmitted through a sample includes a step of simultaneously irradiating a plurality of regions of a S11 of a large-sized sample in a single crystal state with white X-rays R11, and a step of detecting diffracted X-rays generated by the radiation, in which measurement including a series of steps is performed a plurality of times, and in at least one of the plurality of times of measurement, a slit 11 that selectively passes only diffracted X-rays generated from a specific region among a plurality of regions C11 and C12 irradiated with X-rays is disposed on a back side of the S10 of the large-sized sample. By using the slit 11, diffracted X-rays generated in a plurality of regions C11 and C12 of the S10 of the large sample are detected, respectively, and the structure is evaluated for each region.SELECTED DRAWING: Figure 5
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Description

[Technical Field]

[0001] The present invention relates to a structure evaluation method, a structure evaluation device, and a structure evaluation program that measure diffracted X-rays transmitted through 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 spot 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 the 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 related to 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. For example, in the case of a nickel-based superalloy, such as a turbine blade for thermal power generation, that has a thermal barrier coating with a thickness of 100 μm or more formed thereon, the damage in the single-crystal sample can be measured without removing the thermal barrier coating.

[0005] Meanwhile, a technique using a slit to focus diffracted X-rays is known. Patent Document 3 discloses a method in which, since diffracted X-rays are generated from a wide range when X-rays are incident on a thin film at a small angle, a slit is provided at the center of a goniometer to block part of the diffracted X-rays and extract only the diffracted X-rays from a narrow irradiation range. By limiting the generation position of the diffracted X-rays, the generation position of the diffracted X-rays is spread, preventing the diffracted X-rays from becoming broad.

[0006] Patent Document 4 discloses a method for blocking part of the diffracted X-rays with a slit and extracting only the diffracted X-rays from a narrow irradiation range, since diffracted X-rays are generated from multiple locations during transmission measurement of a thick sample. This is also a method for preventing the diffracted X-rays from becoming broad. [Prior art documents] [Patent documents]

[0007] [Patent Document 1] Patent No. 7093929 [Patent Document 2] Japanese Patent Application Publication No. 2023-140749 [Patent Document 3] Japanese Patent Application Laid-Open No. 2017-223539 [Patent Document 4] Japanese Patent Application Laid-Open No. 2012-7935 Summary of the Invention [Problem to be solved by the invention]

[0008] As mentioned above, a method for measuring damage in components used in high-temperature, high-load environments using X-ray diffraction has been proposed. However, when obtaining a Laue image of a thick metal material using X-rays, it is difficult to determine which part of the material the diffraction spot originates from. For example, damage can spread from a specific location in the moving blades of turbine blades used in thermal power generation, making it necessary to measure the degree of damage in each region.

[0009] The present invention has been made in consideration of the above circumstances, and aims to provide a structure evaluation method, a structure evaluation device, and a structure evaluation program that can distinguish between diffracted X-rays generated in each region and evaluate each structure. [Means for solving the problem]

[0010] (1) In order to achieve the above-mentioned object, the structural evaluation method of the present invention is a structural evaluation method performed by measuring diffracted X-rays transmitted through a sample, and includes the steps of simultaneously irradiating white X-rays onto multiple regions of a large single-crystal sample and detecting the diffracted X-rays generated by the irradiation. The measurement consisting of the series of steps is performed multiple times, and in at least one of the multiple measurements, a slit is placed on the back side of the large sample that selectively passes only diffracted X-rays generated from specific regions among the multiple regions irradiated with the X-rays, and the diffracted X-rays generated in each of the multiple regions of the large sample are detected using the slit, and the structure is evaluated for each region.

[0011] (2) Furthermore, in the structural evaluation method described in (1) above, the multiple measurements are performed using multiple types of slits that each pass diffracted X-rays from different regions among the multiple regions.

[0012] (3) Furthermore, in the structural evaluation method described in (1) or (2) above, the diffraction X-ray data detected in the multiple measurements are compared to extract data on diffraction spots for each region, and the structure is evaluated for each region using the extracted data.

[0013] (4) Furthermore, in the structural evaluation method described in any one of (1) to (3) above, the damage state is identified for each region of the large sample from a coefficient related to the variance of the intensity distribution in a specific direction in the diffraction spot of the detected diffracted X-rays.

[0014] (5) Furthermore, in the structural evaluation method described in (4) above, a damage life consumption rate is calculated for each region of the large sample from the half width of the diffraction spot.

[0015] (6) Furthermore, in the structural evaluation method described in (1) or (2) above, the slit is formed in a disk or ring, and the main surface is perpendicular to the irradiation direction of the white X-rays, and the slit is positioned so that the center of the disk or ring coincides with the central axis of the white X-rays.

[0016] (7) Furthermore, in the structural evaluation method described in (6) above, the large sample is formed of a Ni-based superalloy material having a dendritic structure in a single crystal state, and the slit is characterized in that the outer diameter of the disk or the inner diameter of the ring is designed according to the diffraction angle of the diffracted X-rays.

[0017] (8) Furthermore, in the structural evaluation method described in any one of (1) to (9) above, the large sample is characterized in that it consists of an abdominal portion and a dorsal portion sandwiching a hollow portion, and the specific region is the abdominal portion or the dorsal portion.

[0018] (9) Furthermore, the structural evaluation device of the present invention is a structural evaluation device that uses measurement data of diffracted X-rays that have passed through a sample, and is equipped with a data extraction unit that extracts data on the diffraction spots for each region by comparing the diffracted X-ray data obtained by performing multiple measurements in which white X-rays are irradiated simultaneously on multiple regions of a large single-crystal sample, and a damage state identification unit that identifies the damage state for each region using the extracted data, and is characterized in that in at least one of the multiple measurements, a slit is placed on the back side of the large sample that selectively allows only diffracted X-rays generated from a specific region to pass through, among the multiple regions irradiated with the X-rays, and measurement data obtained is used.

[0019] (10) Furthermore, the structural evaluation program of the present invention is a structural evaluation program that uses measurement data of diffracted X-rays that have passed through a sample, and has a computer execute the following processes: extracting data on the diffraction spots for each region by comparing the diffracted X-ray data obtained by performing multiple measurements in which white X-rays are irradiated simultaneously on multiple regions of a large single-crystal sample; and identifying the damage state for each region using the extracted data; and is characterized in that, in at least one of the multiple measurements, measurement data obtained by placing a slit on the back side of the large sample that selectively allows only diffracted X-rays generated from a specific region among the multiple regions irradiated with the X-rays to pass through is used. [Brief explanation of the drawings]

[0020] [Figure 1] FIG. 1 is a schematic side view showing an embodiment of X-ray diffraction measurement of a large hollow sample using a disk-shaped slit. [Figure 2] 1(a) to 1(c) are enlarged views showing the diffraction region of the abdomen and the diffraction region of the dorsum, respectively, and a front view showing the disk-shaped slits. [Figure 3] FIG. 1 is a schematic side view showing an embodiment of X-ray diffraction measurement of a large hollow sample using an annular slit. [Figure 4] 10(a) to 10(c) are enlarged views showing the diffraction region of the abdomen and the diffraction region of the dorsum, respectively, and a front view showing the annular slit. [Figure 5] FIG. 1 is a schematic side view showing an aspect of X-ray diffraction measurement of a large solid sample using a large-diameter disk-shaped slit. [Figure 6] 1(a) to 1(c) are front views showing a small-diameter disk-shaped slit, a large-diameter disk-shaped slit, and a small-diameter annular slit, respectively. [Figure 7] 1 is a schematic diagram showing the configuration of a structural evaluation system according to the present invention. [Figure 8] 1 is a block diagram showing the configuration of a structural evaluation device according to the present invention. [Figure 9] 1 is a flowchart showing a structure evaluation method according to the present invention. [Figure 10]FIG. 1 is a perspective view showing the configuration of an experimental X-ray diffraction device. [Figure 11] FIG. 1 is a schematic diagram showing the diffraction region and main diffraction lines of the abdomen. [Figure 12] 10 is an image showing the diffraction pattern caused by the abdomen. [Figure 13] This is the intensity profile in the 2θ direction of a specific diffraction spot. [Figure 14] FIG. 1 is a schematic diagram showing the diffraction region and main diffraction lines on the back surface. [Figure 15] 10 is an image showing the diffraction pattern produced by the back. [Figure 16] FIG. 1 is a schematic diagram showing the ventral and dorsal diffraction regions and the main diffraction lines. [Figure 17] 10 is an image showing the diffraction patterns produced by the ventral and dorsal regions. [Figure 18] This is the intensity profile in the 2θ direction of a specific diffraction spot. [Figure 19] FIG. 1 is a schematic diagram showing the ventral and dorsal diffraction regions and the main diffraction lines. [Figure 20] FIG. 10 is an enlarged view of the ventral and dorsal diffraction regions. [Figure 21] 10 is an image showing the diffraction pattern caused by the abdomen. [Figure 22] This is the intensity profile in the 2θ direction of a specific diffraction spot. [Figure 23] Schematic diagram showing the ventral and dorsal diffraction regions, the annular slit and the main diffraction lines. [Figure 24] 10 is an enlarged view of the ventral and dorsal diffraction regions and the annular slit. [Figure 25] 10 is an image showing the diffraction pattern produced by the back. [Figure 26] FIG. 1 is a schematic diagram showing the diffraction region and main diffraction lines of the abdomen. [Figure 27] 10 is an image showing the diffraction pattern caused by the abdomen. [Figure 28] FIG. 1 is a schematic diagram showing the diffraction region and main diffraction lines on the back surface. [Figure 29]10 is an image showing the diffraction pattern produced by the back. [Figure 30] This is the intensity profile in the 2θ direction of a specific diffraction spot. [Figure 31] FIG. 1 is a schematic diagram showing the ventral and dorsal diffraction regions and the main diffraction lines. [Figure 32] 10 is an image showing the diffraction patterns produced by the ventral and dorsal regions. [Figure 33] This is the intensity profile in the 2θ direction of a specific diffraction spot. [Figure 34] Schematic diagram showing the ventral and dorsal diffraction regions, the disk-shaped slit, and the main diffraction lines. [Figure 35] 10 is an enlarged view of the ventral and dorsal diffraction regions and the disc-shaped slit. [Figure 36] 10 is an image showing the diffraction pattern caused by the abdomen. [Figure 37] Schematic diagram showing the ventral and dorsal diffraction regions, the annular slit and the main diffraction lines. [Figure 38] 10 is an enlarged view of the ventral and dorsal diffraction regions and the annular slit. [Figure 39] 10 is an image showing the diffraction pattern produced by the back. [Figure 40] This is the intensity profile in the 2θ direction of a specific diffraction spot. DETAILED DESCRIPTION OF THE INVENTION

[0021] 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.

[0022] [principle] In this invention, a special slit is placed that selectively transmits diffracted X-rays according to the diffraction region, and white X-rays are irradiated onto a large sample (e.g., a thick metal material) with a dendritic structure in a single crystal state (transmission Laue method). Within the single crystal state sample, wavelengths are selected according to the respective combinations of interplanar spacing and diffraction angle, and diffracted X-rays are generated in each diffraction region. The transmitted diffracted X-rays are either blocked by the slit or pass through the slit. The diffracted X-rays that reach the detector are then measured to identify the diffraction region that generated the diffraction spot. The detector is a two-dimensional detector.

[0023] The slit is made of a material that can adequately absorb and block diffracted X-rays, such as lead, but is not limited to lead. It is preferable to position the slit in the shape of a disk or ring, with its main surface perpendicular to the direction of white X-ray irradiation, its center aligned with the central axis of the white X-ray, and its position immediately behind the large sample. This allows for selective passage or blocking of diffracted rays from each region along the irradiation direction. Note that "immediately behind" refers to a position that is in contact with or nearly in contact with the dorsal surface of the large sample in the direction of white X-ray propagation. For convenience, the incident side of the large sample onto which the white X-rays are incident is referred to as the "ventral side," and the exit side of the transmitted X-rays is referred to as the "dorsal side."

[0024] 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.

[0025] (hollow sample) First, we will explain the case where X-ray diffraction measurement is performed using a disk-shaped slit 11. Fig. 1 is a side view schematic diagram showing an aspect of X-ray diffraction measurement of a large hollow sample S10 using a disk-shaped slit 11. Figs. 2(a) to 2(c) are enlarged views showing the diffraction region of the abdominal portion S11 and the diffraction region of the dorsal portion S12, and a front view showing the disk-shaped slit 11, respectively.

[0026] The large single-crystal sample S10 has a concave portion (belly S11) and a convex portion (back S12). The large sample S10 is oriented with the belly S11 facing the X-ray irradiation side and the back S12 facing the X-ray detection side (hereinafter, in all examples, the belly side refers to the X-ray irradiation side and the back side refers to the detector side). A space is formed inside the sample surrounded by the belly S11 and back S12. As a result, the large sample consists of S10, the belly S11, and the back S12, which sandwich the hollow portion. Either the belly S11 or the back S12 is the specific region through which the slit passes diffracted X-rays. For example, if a disk-shaped slit S11 is used, the diffracted X-rays generated in the belly S11 will pass through. Figure 1 shows a cross-section of the large sample S10.

[0027] Large sample S10 is a rotor blade sample made of a Ni-based superalloy with a hollow, single-crystal dendritic structure, and its cross section parallel to the direction of white X-ray irradiation is shown in Figure 1. Large sample S10 is positioned so that the direction of this cross section coincides with the 100 crystal plane.

[0028] When a large sample S10 is irradiated with a direct beam R11 of white X-rays, the direct beam R11 is incident on the abdominal region S11. Diffracted X-rays R14 are generated in the X-ray irradiated portion (diffraction region) of the abdominal region S11, pass through the back region S12, and are detected by the detector 140. Figure 2(a) shows an enlarged view of the diffraction region of the abdominal region S11 by enlarging the circular region C11 shown in Figure 1.

[0029] The direct beam R12 that passes through the abdomen S11 passes through the air and enters the back S12. The direct beam R13 that passes through the back S12 passes through the disk-shaped slit 11. Diffracted X-rays are also generated in the X-ray irradiated area (diffraction region) of the back S12, but the disk-shaped slit 11 blocks these diffracted X-rays. These diffracted X-rays are blocked by the disk-shaped slit 11. The dashed line in the figure indicates hypothetical diffracted X-rays V15 that would be generated if they were not blocked by the disk-shaped slit 11.

[0030] FIG. 2(b) shows an enlarged view of the circular region C12 shown in FIG. 1. As shown in FIG. 2(b), diffracted X-rays R14 pass through the disk-shaped slit 11 without hitting it, while diffracted X-rays generated in the diffraction region of the back portion S12 hit the disk-shaped slit 11 and are blocked (virtual diffracted X-rays V11). FIG. 2(c) is a front view showing the disk-shaped slit 11. The dashed circle B12 indicates the outer diameter of the annular slit 12, which will be described later. The disk-shaped slit 11 shown in FIGS. 1 and 2(b) is a side cross-sectional view. The diffracted X-rays R14 that reach the detector 140 are detected as diffraction spots.

[0031] Next, X-ray diffraction measurement is performed on the hollow large sample S10 using the annular slit 12. Fig. 3 is a side view schematic showing an aspect of X-ray diffraction measurement of the hollow large sample S10 using the annular slit 12. Figs. 4(a) to 4(c) are enlarged views showing the diffraction region of the abdominal portion S11 and the diffraction region of the dorsal portion S12, and a front view showing the annular slit 12, respectively. Fig. 3 shows a cross section of the large sample S10.

[0032] When a direct beam R11 of white X-rays is irradiated onto the large sample S10, the direct beam R11 is incident on the abdominal portion S11. Diffracted X-rays R14 are generated in the X-ray irradiated portion (diffraction region) of the abdominal portion S11, pass through the dorsal portion S12, and are detected by the detector 140. Figure 4(a) shows an enlarged view of the diffraction region of the dorsal portion S12 by enlarging the circular region C21 shown in Figure 3.

[0033] The direct beam R12 that has passed through the abdomen S11 passes through the hollow and is incident on the back S12. The direct beam R13 that has passed through the back S12 passes through the central hole 12a of the annular slit 12. Diffracted X-rays R15 are generated in the X-ray irradiated portion (diffraction region) of the back S12 and pass through the hole 12a of the annular slit 12.

[0034] FIG. 4(b) shows an enlarged view of the circular region C22 shown in FIG. 3. As shown in FIG. 4(b), diffracted X-ray R14 is blocked by the annular slit 12 (virtual diffracted X-ray V14). Diffracted X-ray R15 generated in the diffraction region of the back portion S12 passes through the annular slit 12. FIG. 4(c) is a front view showing the annular slit 12. The annular slit 12 has a hole 12a in the center. The annular slit 12 shown in FIGS. 3 and 4(b) is a side cross-sectional view. The diffracted X-ray R15 that reaches the detector 140 is detected as a diffraction spot.

[0035] As described above, the structure of the abdominal portion S11 of the hollow large-sized sample S10 can be evaluated by measuring the diffracted radiation that passed through the disk-shaped slit 11. Also, the structure of the dorsal portion S12 can be evaluated by measuring the diffracted radiation that passed through the annular slit 12. Specifically, the damage life consumption rate can be calculated for each region, and the damage state can be confirmed.

[0036] In this way, multiple measurements can be performed using multiple types of slits that allow diffracted X-rays from different regions to pass through, allowing the structure of different regions to be evaluated using the diffracted X-rays that pass through each slit.

[0037] In hollow samples, it is possible that the dorsal and ventral regions have different structures. Compared to solid samples (described later), hollow samples allow for easy separation of the diffraction lines from the dorsal and ventral regions by using a slit. This makes it possible to measure specific regions without comparing diffracted X-ray data detected in multiple measurements.

[0038] (solid sample) Next, X-ray diffraction measurement of a large solid sample S20 using various slits will be described. Fig. 5 is a side view showing a schematic diagram of X-ray diffraction measurement of a large solid sample S20 using a large-diameter disk-shaped slit 32.

[0039] The large, solid sample S20 in a single crystal state has an abdominal portion S21 forming a concave portion, a middle portion S22, and a back portion S23 forming a convex portion. In other words, there is no space between the abdominal portion S21 and the back portion S23, and the middle portion S22, which is a sample in a single crystal state, is filled in between them.

[0040] When the large sample S20 is irradiated with a direct beam R21 of white X-rays, the direct beam R21 is incident on the abdominal portion S21. Diffracted X-rays R23 are generated in the X-ray irradiated portion (diffraction region) of the abdominal portion S21. The diffracted X-rays R23 pass through the middle portion S22 and the back portion S23 and are detected by the detector 140.

[0041] The direct beam that has passed through the abdominal region S21 is incident on the middle region S22 and further on the back region S23. Diffracted X-rays are generated in the X-ray irradiated areas (diffraction regions) of the middle region S22 and the back region S23, but the disc-shaped slit 32 blocks these diffracted X-rays. The disc-shaped slit 32 shown in FIG. 5 is a side cross-sectional view. The direct beam R21 that has passed through the back region S23 is transmitted through the disc-shaped slit 32. The direct beam R22 that has passed through the disc-shaped slit 32 is detected by the detector 140.

[0042] The dashed lines in the figure indicate hypothetical diffracted X-rays V24 and V25 that are not blocked by the disk-shaped slit 32. The diffracted X-ray R23 that reaches the detector 140 is detected as a diffraction spot caused by the abdomen S23.

[0043] The large-diameter disk-shaped slit 32 is used to measure diffracted X-rays from the abdominal region S21, and similar measurements are then performed using the small-diameter disk-shaped slit 31 and the small-hole annular slit 33. The dashed circle B33 indicates the outer diameter of the annular slit 33, which will be described later. Figures 6(a) to 6(c) are front views showing the small-diameter disk-shaped slit 31, the large-diameter disk-shaped slit 32, and the small-hole annular slit 33, respectively.

[0044] In measurements using the small-diameter disk-shaped slit 31, diffracted X-rays generated in the diffraction regions of the abdominal region S21 and the middle region S22 pass through the disk-shaped slit 31 and are detected by the detector 140. At this time, diffracted X-rays generated in the diffraction region of the dorsal region S23 are absorbed and blocked by the disk-shaped slit 31.

[0045] By comparing the diffraction spots generated by the diffracted X-rays generated in the diffraction region of the abdominal portion S21 with those detected when a large-diameter disk-shaped slit 32 is used, the diffraction spots generated by the diffracted X-rays generated in the diffraction region of the intermediate portion S22 can be identified.

[0046] For example, when identifying diffraction spots in the middle part by comparison, the diffraction spots of the middle and abdomen parts are compared with the diffraction spots of only the abdomen part. Then, diffraction spots corresponding to the diffraction spots of only the abdomen part can be removed as diffraction spots of the abdomen data. In this case, only peaks with similar average half-widths of the diffraction spots can be removed.

[0047] It is also possible to compare the average half-width obtained from the diffraction peaks at the abdomen with the average half-width of the remaining diffraction peaks that do not correspond to the diffraction spots at the abdomen, and remove only diffraction spots with similar average half-widths. However, if the average half-width obtained from the diffraction peaks at the abdomen and the average half-width of the remaining diffraction spots (including the diffraction spots at the middle parts) that do not correspond to the diffraction spots at the abdomen are almost the same, the analysis results of the damage state will not be significantly affected even if the diffraction peaks at the abdomen are not removed. If there is no significant difference in the half-widths of the diffraction peaks at the abdomen and the middle parts, there is little problem in using data that includes both the data at the abdomen and the middle parts.

[0048] In measurements using the small-hole annular slit 33, diffracted X-rays generated in the diffraction region of the dorsal region S23 pass through the holes 33a of the annular slit 33 and are detected by the detector 140. On the other hand, diffracted X-rays generated in the diffraction regions of the abdominal region S21 and the middle region S22 are absorbed and blocked by the annular slit 33.

[0049] In this way, by using multiple slits, it becomes possible to independently select diffraction data from the abdominal, middle, and dorsal regions. Here, the explanation is limited to three diffraction regions, but in practice, more diffraction regions can be set and the diameter of the circular slit can be gradually increased. Similarly to the measurement of three diffraction regions, by selecting diffracted X-rays while capturing the characteristics of the diffraction region and diffraction spot, it is also possible to determine the average half-width of the diffraction spot from a specific diffraction region. In other words, two or four or more regions can be distinguished.

[0050] In addition, in the above example, three slits are used to identify the diffracted X-rays from each region, but it is also possible to identify the diffracted X-rays from each region using data measured with two slits and no slits. By comparing the diffracted X-ray data detected from multiple measurements, it is possible to extract diffraction spot data for each region and evaluate the structure of each region using the extracted data. It is also possible to identify diffraction spots occurring from specific regions and evaluate the structure of those regions using a combination of data obtained from measurements without a slit and data obtained from measurements with a slit.

[0051] In addition to the above combinations, a large annular slit can also be used, which allows the diffracted X-rays from the middle section S22 and the back section S23 to pass through. In either case, a combination of slits is used that allows the diffracted X-rays from each region to be distinguished by comparison. As described above, by using a slit in at least one measurement and comparing the diffracted X-rays detected in multiple measurements, the structure of each region can be evaluated.

[0052] In the above examples, the shape of the slit is a disk or annulus, but the shape is not limited to these as long as it passes or blocks the diffraction rays of the diffraction angle to be detected. For example, it may be a sphere or a sphere with a hole. Furthermore, the combination of slits is not limited to the above examples.

[0053] [Target samples] The large sample is preferably made of a Ni-based superalloy material with a dendritic structure in a single crystal state, and the slit's outer diameter or inner diameter of the annulus is preferably designed according to the diffraction angle of the diffracted X-rays. This method is particularly effective when applied to, for example, turbine blades for thermal power generation. It is also particularly effective when the large sample is hollow. In this case, information from the area on the X-ray irradiated side of the large sample and the area on the detector side can be efficiently separated. Note that metal materials with a dendritic structure in a single crystal state are composed of numerous dendritic subgrains with diameters of approximately several hundred micrometers.

[0054] 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 into rods several millimeters wide, in a single-crystal state.

[0055] 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.

[0056] 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.

[0057] For example, when a nickel-based superalloy is used for a turbine blade, centrifugal force causes the turbine blade to stretch in the

[0001] direction of the subgrains. This stretching direction is the damage direction. Then, in the process leading up to fracture due to damage deformation, etc., the regular arrangement of the single crystal state is disrupted. The direction and degree of this disruption of the arrangement are expressed as the damage direction and damage degree. Note that the damage state refers to the damage degree and damage direction.

[0058] When white X-rays are irradiated onto a single-crystal substrate, so-called Laue spots appear as diffraction spots. When a single-crystal substrate is not deformed at all, Laue spots appear with a circular periphery. As the substrate deforms, the periphery of the Laue spots changes from a circular shape to an ellipse, and the major axis of the ellipse elongates. For example, when evaluating damage in a nickel-based superalloy, disturbances in the crystal structure of the γ and γ' phases are observed as broadening of the diffraction peaks of the diffraction planes within the crystal. In this way, the coefficient related to the dispersion of the diffraction spots corresponds to the coefficient of damage in the nickel-based superalloy, allowing the damage state of the turbine blade to be identified and the remaining life of the turbine blade to be estimated.

[0059] [Principle of damage measurement] The sample is irradiated with white X-rays using the Laue method. The white X-rays are preferably a fine beam. A fine beam refers to a beam size equivalent to the crystal grain size (including subgrain grain size) to be irradiated with X-rays. When white X-rays are irradiated onto a damaged subgrain, diffracted X-rays are generated by crystallites with slightly wider lattice spacing due to variations in orientation within the subgrain, resulting in a diffraction peak with a large half-width.

[0060] When X-rays are incident so that the direction parallel to the intersection of the lattice plane and the diffraction plane along which the X-rays are diffracted coincides with the direction of crystal damage, the change in the half-width of the diffraction peak due to damage is greatest. Therefore, when evaluating the degree of damage in a metallic material with a dendritic structure in a single crystal state, the most efficient method is to evaluate the degree of damage based on the broadening of the diffraction spot oriented parallel to or close to the direction of damage. In single crystal or polycrystalline samples, the half-width of the diffraction spot is affected by the thickness of the sample, making it difficult to evaluate the crystallinity from the broadening of the half-width. For these reasons, it is preferable that the sample be a metallic material with a dendritic structure.

[0061] [Structural evaluation system] A system used for structural evaluation will be described. FIG. 7 is a schematic diagram showing the configuration of a structural evaluation system 100. The structural evaluation system 100 includes an X-ray diffraction device 110 and a processing device 150 (structural evaluation device). The X-ray diffraction device 110 is a device used for measurements to detect diffraction spots. The processing device 150 is a device that mainly identifies the state of damage from the detected diffraction spots. The X-ray diffraction device 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.

[0062] [X-ray diffractometer] The basic configuration of the X-ray diffraction instrument 110 will be described. The X-ray diffraction instrument 110 includes an X-ray irradiation unit 120, a sample holder 130, a position adjustment mechanism 135, and a detector 140. Although not shown in Figure 7, if a slit is used, it is installed on the rear side immediately behind the sample S0.

[0063] 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, which generates a narrow beam of white X-rays. The X-rays pass through the X-ray shielding window and are emitted to the outside.

[0064] 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.

[0065] 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.

[0066] 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.

[0067] 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 also adjust the tilt of the sample holder .

[0068] 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.

[0069] 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.

[0070] 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.

[0071] [Processing equipment] 8 is a block diagram showing the configuration of the processing device (structural evaluation 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 a position adjustment unit 151, a data extraction unit 153, a coefficient calculation unit 155, a damage state identification unit 156, and a storage unit 157.

[0072] 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.

[0073] The processing device 150 processes data and controls the device in response to input of positional 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 identified damage state in the sample as a result of the structural evaluation. It may also output an image of the captured diffraction spot and the direction in which the peak shape is to be viewed.

[0074] The position adjustment unit 151 adjusts the arrangement of the detector 140 relative to the X-ray irradiation unit 120 based on the input information. This makes it possible to adjust the angle of the incident X-rays from the X-ray irradiation unit 120 so that the diffracted X-rays are incident on the detector 140. Specifically, the position angle adjustment (φ angle, etc.) of the detector 140 and the angle of the X-ray irradiation unit 120 are adjusted.

[0075] Furthermore, the position adjustment unit 151 can adjust the tilt of the sample holder 130 via the position adjustment mechanism 135. Note that the X-ray irradiation unit 120 may be fixed and the positions of the sample holder 130 and the detector 140 may be adjusted.

[0076] The data extraction unit 153 extracts diffraction spot data for each region by comparing the diffracted X-ray data obtained by performing measurements multiple times in which white X-rays are irradiated simultaneously on multiple regions of a large single-crystal sample.

[0077] The coefficient calculation unit 155 analyzes the diffraction peak in the 2θ direction to determine the extent of the broadening of the base of the diffraction peak. Specifically, based on the detected data of the diffraction spot, it calculates a coefficient that relates to the variance of the intensity distribution in a specific direction at the diffraction spot of the detected data. From this coefficient, the damage state can be identified for each region of the large sample.

[0078] The damage state of the sample can be identified from the coefficient of dispersion of the intensity distribution in a specific direction in the diffraction spot. The coefficient of dispersion of the intensity distribution of the diffraction spot is preferably the half-width of the peak in the specific direction. The half-width means the peak width at half the height of the peak.

[0079] The damage state specifying unit 156 specifies the damage state of the sample from the calculated coefficient. In doing so, it refers to a function supplied from the storage unit 157 and uses a calibration curve of a function between the coefficient that is related to the variance of the intensity distribution in a specific direction in the diffraction spot and the damage life consumption rate. As the damage state of the sample, it is possible to calculate the damage life consumption rate calculated from the coefficient that is related to the variance of the intensity distribution of the diffraction spot.

[0080] The calibration curve is obtained by plotting the damage life consumption rate against the half-width of each peak using a sample with a known damage life consumption rate, and then drawing an approximate curve using the least squares method. This allows for accurate and precise damage evaluation of each region nondestructively. In this case, unreliable data close to fracture can be ignored, and a linear approximation can be performed using only data on damage life consumption rates between 0% and 50%, for example.

[0081] The memory unit 157 stores a coefficient related to the variance of the intensity distribution in a specific direction in a diffraction spot, which is prepared based on a standard sample, and a function of the damage life consumption rate. The memory unit 157 is referenced when evaluating damage to the sample. The memory unit 157 supplies the necessary functions as required in response to a request from the damage state specifying unit 156.

[0082] [Structural evaluation method] A method for evaluating the structure of a sample using the structure evaluation system 100 configured as described above will now be described. Fig. 9 is a flowchart showing the structure evaluation method. First, a large sample is placed on the sample holder 130, and the position of the large sample made of a single-crystalline material is adjusted so that the white X-ray beam is incident on the sample by the X-ray irradiation unit 120. A slit that passes diffracted X-rays from the target diffraction region is also placed on the detector side (back side) immediately behind the large sample (step S01).

[0083] The slit shape used depends on the purpose. Examples of slit types include disk-shaped slits and annular slits. However, depending on the purpose, measurements may be performed without a slit. In at least one of the multiple measurements, a slit is placed on the back side of the large sample to selectively pass only diffracted X-rays generated from a specific region among the multiple regions irradiated with X-rays. By using a slit, diffracted X-rays generated in multiple regions of the large sample can be detected and the structure can be evaluated for each region.

[0084] It is preferable to determine the specific specifications of the slit according to the energy of the X-rays to be transmitted. For example, when using a 150 keV X-ray source, the X-ray absorption formula I=I0e -μx Using this equation, we can determine that the thickness of lead when the X-ray intensity decreases to 1 / e is approximately 0.4 mm (= x). The X-ray absorption equation shows that when X-rays of intensity I0 pass through an absorbing plate of thickness x cm with a linear absorption coefficient μ, the X-ray intensity is I.

[0085] μ=22.8(cm at 150 keV -1), the lead thickness x can be found by setting μx = 1 (I = I0 / e). This is because the thickness of the absorbing plate when the X-ray intensity drops to 1 / e is usually set as the limit of the X-ray penetration distance. In other words, once the material is determined for a specific energy, the thickness required for X-ray absorption is determined. In addition, the diameter of the center of the slit is determined by considering the diffraction angles of the absorbed and unabsorbed diffracted rays relative to the thickness of the slit plate.

[0086] When placing a large specimen, it is preferable to align the damage direction of the specimen parallel to the surface of the specimen holder. For example, in the case of specimen S0 cut from a turbine blade, the damage direction is from the center of rotation of the turbine toward the tip of the blade.

[0087] Next, a white X-ray beam is irradiated onto a large single-crystal sample, irradiating multiple regions with the white X-ray simultaneously (step S02). Diffracted X-rays are generated from the multiple diffraction regions, and the diffraction spots are detected by detector 140 (step S03). It is preferable to select the diffraction spots to be observed on the low-angle side, where the X-ray intensity is relatively strong.

[0088] After aligning the detectors, the diffraction spots are detected while the instruments in each measurement system remain stationary. By using white X-rays, the detectors can be set at a low angle, and multiple high-intensity diffraction spots can be detected at a stationary position without rotating the instruments, regardless of the crystal orientation.

[0089] It is determined whether measurement of each region is complete (step S04), and if not, the process returns to step S01. This allows the measurement consisting of a series of steps to be performed multiple times. When performing step S01 in a loop, it may be necessary to position only the sample or the slit, as necessary. When measurement of each region is complete, diffraction spots arising from specific diffraction regions are extracted based on the obtained data (step S05). The extracted diffraction spots are then used to calculate the degree of damage to the diffraction regions from which they originate (step S06).

[0090] When calculating the degree of damage, the shape of the diffraction spot is measured, and the peak shape in the damage direction, which indicates the state of damage, is extracted from the shape, and the coefficient of dispersion is calculated by data processing. The direction in which the coefficient of dispersion is calculated is the 2θ direction. When the large sample is a turbine blade, it is preferable to measure the diffraction spot of the lattice plane parallel to its side surface.

[0091] Next, the damage assessment curve (master curve) stored in the memory unit 157 is read out, and the damage state of the sample is identified based on the coefficient related to the dispersion of the peak shape. Then, the remaining life can be estimated based on the damage state of the sample. The calculation results are output on a display, printer, etc. This completes the series of processes.

[0092] [Example] An experiment was conducted on a sample simulating an actual rotor blade. Fig. 10 is a perspective view showing the configuration of an X-ray diffraction apparatus 200 used for the experiment. The X-ray diffraction apparatus 200 includes an X-ray irradiation unit 120 and a detector 140. A sample S50 is placed between the X-ray irradiation unit 120 and the detector 140.

[0093] Sample S50 simulates a hollow sample. Sample S50 includes wood W10 and sample boards S51 and S52. Wood W10 is basically 10 mm thick and has a concave shape with an H-shaped horizontal cross section and a central thickness of 5 mm.

[0094] Sample plates S51 and S52 are Ni-based superalloy specimens in a single crystal state with damage life consumption rates of 79% and 0%, respectively. Sample plate S51 is a 2 mm x 10 mm rectangle with a thickness of 1.5 mm. Sample plate S52 is a 10 mm x 10 mm square with a thickness of 1.5 mm. Sample plates S51 and S52 are supported by adhesive bonding to a piece of wood W10. The sample plate on the X-ray irradiation side is referred to as the belly side, and the sample plate on the detector side is referred to as the back side. Sample plate S51 was subjected to a tensile test in the longitudinal direction (001 crystal orientation).

[0095] A lead block with a diameter of 3 mm and a thickness of 2 mm was used as the disk-shaped slit, and a lead plate with a square shape of 11.5 mm x 11.5 mm and a hole with a diameter of 3 mm in the center was used as the annular slit.

[0096] The experiments were carried out under four conditions: when X-rays were irradiated only on one of the samples, when the two samples were placed in series with a 10 mm gap between them, and when the two samples were swapped and measurements were taken in the same way. Diffraction images and diffraction peak profiles were obtained for each sample position.

[0097] (Embodiment 1) Samples with different damage life consumption rates (ventral side (79%) or dorsal side (0%)) (Experiment 1) (ventral side (79%) only, no slit) Sample plate S51 with a damage life consumption rate of 79% was placed on the X-ray incident side (ventral side), and the diffraction spots were measured without placing a slit. Figure 11 is a schematic diagram showing the diffraction region and main diffraction lines of the ventral side. Figure 12 is an image showing the diffraction image M1 generated by the ventral side. In the diffraction image M1, a diffraction spot SP1 unique to sample plate S51 appears. Figure 13 shows the intensity profile in the 2θ direction of a specific diffraction spot SP1. The half-width of the diffraction spot SP1 is wide.

[0098] (Experiment 2) (dorsal side (0%) only, no slit) Sample plate S52 with a damage life consumption rate of 0% was placed on the detector side (back side) and the diffraction spots were measured without a slit. Figure 14 is a schematic diagram showing the diffraction region and main diffraction lines of the back. Figure 15 is an image showing diffraction image M2 generated by the back. Diffraction spots are clearly visible in diffraction image M2.

[0099] From (Experiment 1) and (Experiment 2), it can be seen that the half-width of the diffraction spot of the sample plate with a high damage life consumption rate is larger than the half-width of the diffraction spot of the sample plate with a low damage life consumption rate.

[0100] (Embodiment 2) Ventral (79%) and dorsal (0%) samples (Experiment 3) (ventral (79%) and dorsal (0%), no slit) Sample plate S51 with a damage life consumption rate of 79% was placed on the X-ray incident side (ventral side), and sample plate S52 with a damage life consumption rate of 0% was placed on the detector side (dorsal side). Diffraction spots were measured without a slit. Figure 16 is a schematic diagram showing the diffraction regions and major diffraction lines of the ventral and dorsal regions. Figure 17 is an image showing diffraction image M3 generated by the ventral and dorsal regions. Diffraction image M3 shows diffraction spot SP3, which corresponds to diffraction spot SP1. Figure 18 shows the intensity profile in the 2θ direction of a specific diffraction spot SP3. The half-width of diffraction spot SP3 is wide.

[0101] (Experiment 4) (ventral (79%) and dorsal (0%), discoid slit) Sample plate S51 with a damage life consumption rate of 79% was placed on the X-ray incident side (ventral side), and sample plate S52 with a damage life consumption rate of 0% was placed on the detector side (dorsal side). A lead block with a diameter of 3 mm and a thickness of 2 mm was used as the disk-shaped slit 51. Figure 19 is a schematic diagram showing the diffraction regions of the ventral and dorsal regions, the disk-shaped slit 51, and the main diffraction lines. Figure 20 is an enlarged view of the diffraction regions of the ventral and dorsal regions. Figure 21 is an image showing the diffraction image M4 generated by the ventral region. In diffraction image M4, a diffraction spot SP4 corresponding to diffraction spot SP1 (or SP3) appears. Furthermore, clear diffraction spots are no longer visible. Figure 22 shows the intensity profile in the 2θ direction of a specific diffraction spot SP4. The half-width of diffraction spot SP4 is wide.

[0102] (Experiment 5) (ventral (79%) and dorsal (0%), circular slit) Sample plate S51 with a damage life consumption rate of 79% was placed on the X-ray incident side (ventral side), and sample plate S52 with a damage life consumption rate of 0% was placed on the detector side (dorsal side). An 11.5 mm × 11.5 mm square lead plate with a 3 mm diameter hole in the center was used as the annular slit 52. Figure 23 is a schematic diagram showing the diffraction regions of the ventral and dorsal regions, the annular slit, and the main diffraction lines. Figure 24 is an enlarged view of the diffraction regions of the ventral and dorsal regions and the annular slit. Figure 25 is an image showing the diffraction image M5 generated by the dorsal region. Diffraction spots are clearly visible in diffraction image M5.

[0103] In (Experiment 3), no slit was placed, so diffraction spots from both the ventral and dorsal sides were obtained. On the other hand, in (Experiment 4), a disk-shaped slit was placed, so diffraction spots with a large FWHM were detected from the ventral sample plate, which has a high damage life consumption rate. Furthermore, in (Experiment 5), a circular slit was placed, so diffraction spots with a small FWHM were detected from the dorsal sample plate, which has a low damage life consumption rate. As in (Experiment 4) and (Experiment 5), a slit may be used to extract only diffraction spots from a specific region, such as the dorsal or ventral region. Furthermore, by comparing (Experiment 3) with (Experiment 4) or (Experiment 3) with (Experiment 5), diffraction spots from specific regions may be extracted depending on the presence or absence of a single type of slit.

[0104] (Embodiment 3) Samples with different damage life consumption rates (ventral side (0%) or dorsal side (79%)) (Experiment 6) (ventral side (0%) only, no slit) The sample plate S52 with a damage life consumption rate of 0% was placed on the X-ray incident side (ventral side) and the diffraction spots were measured. Figure 26 is a schematic diagram showing the diffraction region and main diffraction lines of the abdomen. Figure 27 is an image showing the diffraction image M6 generated by the abdomen. Diffraction spots are clearly visible in the diffraction image M6.

[0105] (Experiment 7) (dorsal side (79%) only, no slit) The sample plate S51, with a damage life consumption rate of 79%, was placed on the detector side (back side) and the diffraction spots were measured. Figure 28 is a schematic diagram showing the diffraction region and main diffraction lines of the back. Figure 29 is an image showing the diffraction image M7 generated by the back. Diffraction image M7 shows a diffraction spot SP7 specific to the sample plate S51. Figure 30 shows the intensity profile in the 2θ direction of a specific diffraction spot SP8. The half-width of the diffraction spot SP7 is wide.

[0106] In (Embodiment 3), the positions of the ventral and dorsal samples were swapped compared to (Embodiment 1), and measurements were taken with the FWHM of the diffraction spot of the sample plate with a high damage life consumption rate was found to be wider than the FWHM of the diffraction spot of the sample plate with a low damage life consumption rate, even when the positions of the ventral and dorsal samples were swapped.

[0107] (Embodiment 4) Ventral (0%) and dorsal (79%) samples (Experiment 8) (ventral (0%) and dorsal (79%), no slit) Sample plate S52 with a damage life consumption rate of 0% was placed on the X-ray incident side (ventral side), and sample plate S51 with a damage life consumption rate of 79% was placed on the detector side (dorsal side). Diffraction spots were measured without a slit. Figure 31 is a schematic diagram showing the diffraction regions and major diffraction lines of the ventral and dorsal regions. Figure 32 is an image showing diffraction image M8 generated by the ventral and dorsal regions. Diffraction image M8 shows diffraction spot SP8, which corresponds to diffraction spot SP7. Figure 33 shows the intensity profile in the 2θ direction of a specific diffraction spot SP8. The half-width of diffraction spot SP8 is broad.

[0108] (Experiment 9) (ventral (0%) and dorsal (79%), discoid slits) Sample plate S52 with a damage life consumption rate of 0% was placed on the X-ray incident side (ventral side), and sample plate S51 with a damage life consumption rate of 79% was placed on the detector side (dorsal side). A lead block with a diameter of 3 mm and a thickness of 2 mm was used as the disk-shaped slit 51. Figure 34 is a schematic diagram showing the diffraction regions of the ventral and dorsal regions, the disk-shaped slit, and the main diffraction lines. Figure 35 is an enlarged view of the diffraction regions of the ventral and dorsal regions and the disk-shaped slit. Figure 36 is an image showing the diffraction image M9 generated by the ventral region. Diffraction spots are clearly visible in diffraction image M9.

[0109] (Experiment 10) (ventral (0%) and dorsal (79%), circular slit) Sample plate S52 with a damage life consumption rate of 0% was placed on the X-ray incident side (ventral side), and sample plate S51 with a damage life consumption rate of 79% was placed on the detector side (dorsal side). Figure 37 is a schematic diagram showing the diffraction regions of the ventral and dorsal regions, the annular slit, and the main diffraction lines. Figure 38 is an enlarged view of the diffraction regions of the ventral and dorsal regions and the annular slit. Figure 39 is an image showing the diffraction image M10 generated by the dorsal region. In the diffraction image M10, a diffraction spot SP10 corresponding to the diffraction spot SP7 appears. Figure 40 shows the intensity profile in the 2θ direction of a specific diffraction spot SP10. The half-width of the diffraction spot SP10 is wider.

[0110] In (Experiment 8), no slit was placed, so diffraction spots from both the ventral and dorsal sides were obtained. On the other hand, in (Experiment 9), a disk-shaped slit was placed, so diffraction spots with narrow half-widths originating from the ventral sample plate, which has a low damage life consumption rate, were detected. Furthermore, in (Experiment 10), a circular slit was placed, so diffraction spots with wide half-widths originating from the dorsal sample plate, which has a high damage life consumption rate, were detected. As such, slits can be used to extract only diffraction spots from specific regions, such as the dorsal or ventral regions, as in (Experiment 9) and (Experiment 10). Furthermore, by comparing (Experiment 8) with (Experiment 9) or (Experiment 8) with (Experiment 10), diffraction spots from specific regions can be extracted depending on the presence or absence of a single type of slit. [Explanation of symbols]

[0111] 11 Circular slit 12 Circular slit 12a hole 31 Circular slit 32 Circular slit 33 Circular slit 33a hole 51 Circular slit 52 Circular slit 100 Structural Evaluation System 110 X-ray Diffraction Equipment 120 X-ray irradiation section 121 Main body 122 Collimator 125 cabinet 126 X-ray source 127 X-ray shield window 128 Collimator body 129 Shielding Cover 130 Sample holder 135 Position adjustment mechanism 140 detectors 150 Processing equipment (structural evaluation equipment) 151 Position adjustment section 153 Data Extraction Unit 153 Data Extraction Unit 155 Coefficient calculation unit 156 Damage Identification Section 157 Memory section 160 Input Devices 170 Output Device 200 X-ray Diffractometer DB1 Direct Beam R11 Direct Beam R12 Direct Beam R13 Direct Beam R14 Diffraction X-rays R15 Diffraction X-rays R2 Diffracted X-rays R21 Direct Beam R22 Direct Beam R23 Diffraction X-rays V11 Diffracted X-rays (virtual) V14 Diffracted X-ray (virtual) V15 Diffracted X-ray (virtual) V24 Diffracted X-ray (virtual) V25 Diffracted X-ray (virtual) S0 sample S10 Large Sample S11 abdomen S12 back S20 Large Sample S21 abdomen S22 middle part S23 back S50 sample S51 Sample Plate S52 sample plate SP1 diffraction spot SP3 diffraction spot SP4 diffraction spot SP8 Diffraction Spot SP9 Diffraction Spot SP12 diffraction spot

Claims

1. A structural evaluation method performed by measuring diffracted X-rays transmitted through a sample, comprising: irradiating multiple regions of a large single-crystal sample simultaneously with white X-rays; detecting diffracted X-rays produced by said irradiation; The measurement consisting of the series of steps is carried out a plurality of times; a slit is disposed on the rear side of the large sample, which selectively passes only diffracted X-rays generated from a specific region among the plurality of regions irradiated with the X-rays in at least one of the plurality of measurements; A structural evaluation method, characterized in that the slit is used to detect diffracted X-rays generated in each of a plurality of regions of the large sample, and the structure is evaluated for each region.

2. 2. A structural evaluation method according to claim 1, wherein the measurements are performed multiple times using a plurality of types of slits that respectively pass diffracted X-rays from different regions among the plurality of regions.

3. 3. A structural evaluation method according to claim 1, wherein the diffraction X-ray data detected in the multiple measurements is compared to extract diffraction spot data for each region, and the structure is evaluated for each region using the extracted data.

4. 3. A structural evaluation method according to claim 1, wherein the damage state is identified for each region of the large sample from a coefficient related to the dispersion of the intensity distribution in a specific direction in the diffraction spot of the detected diffracted X-rays.

5. 5. A structural evaluation method according to claim 4, wherein a damage life consumption rate is calculated for each region of the large sample from the half-width of the diffraction spot.

6. The slit is formed in a disk or annulus, 3. A structural evaluation method according to claim 1, wherein the slit is arranged so that the main surface is perpendicular to the irradiation direction of the white X-ray and the center of the disk or annulus coincides with the central axis of the white X-ray.

7. The large sample is formed of a Ni-based superalloy material having a dendritic structure in a single crystal state, 7. The structural evaluation method according to claim 6, wherein the slit has an outer diameter of the disk or an inner diameter of the ring designed according to the diffraction angle of the diffracted X-rays.

8. 3. A structural evaluation method according to claim 1, wherein the large sample comprises a belly portion and a dorsal portion sandwiching a hollow portion, and the specific region is the belly portion or the dorsal portion.

9. A structural evaluation apparatus that uses measurement data of diffracted X-rays transmitted through a sample, a data extraction unit that extracts diffraction spot data for each region by comparing diffracted X-ray data obtained by performing measurements multiple times in which white X-rays are irradiated simultaneously on multiple regions of a large single-crystal sample; a damage state specifying unit that specifies a damage state for each region based on the extracted data, A structural evaluation device characterized in that, in at least one of the multiple measurements, a slit is placed on the back side of the large sample to selectively pass only diffracted X-rays generated from a specific region among the multiple regions irradiated with the X-rays, and measurement data obtained is used.

10. A structural evaluation program using measurement data of diffracted X-rays transmitted through a sample, A process of extracting diffraction spot data for each region by comparing diffracted X-ray data obtained by performing measurements multiple times in which white X-rays are irradiated simultaneously on multiple regions of a large single-crystal sample; and causing a computer to execute a process of identifying a damage state for each region using the extracted data; A structural evaluation program characterized in that, in at least one of the multiple measurements, measurement data obtained by placing a slit on the back side of the large sample that selectively passes only diffracted X-rays generated from a specific region among the multiple regions irradiated with the X-rays is used.

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