Correction amount determination device, method, recording medium, and jig

Abstract

Provided is a correction amount determination device, method, recording medium, and jig. A correction amount determination device (300) includes: a diffraction data storage section (310) that stores diffraction data obtained by irradiating a standard sample that is an aggregate of crystal particles that are isotropic and free of strain with X-rays, the diffraction data including a combination of a diffraction angle of the irradiated X-rays with respect to a sample rotation angle and a sample surface height; a correspondence relationship determination section (320) that determines a first correspondence relationship based on the diffraction data; and a correction amount determination section (330) that determines a correction amount of the sample surface height with respect to a desired sample rotation angle and diffraction angle by a first function.

Description

Technical Field

[0001] This invention relates to a calibration amount determination device, method, recording medium, and fixture for calibrating the position of a beam irradiation. Background Technology

[0002] The size of components in electronic devices such as televisions, personal computers, and mobile phones is decreasing year by year. Consequently, the analysis of minute areas is frequently performed when evaluating the functionality and performance of these electronic devices. Furthermore, components in transportation machinery such as automobiles are also trending towards miniaturization to reduce CO2 emissions or improve fuel efficiency, leading to increased analysis of minute areas.

[0003] In these analyses, X-rays are generally used. Apparatus for analyzing small areas requires high cross-axis accuracy in order to irradiate a specific point with an X-ray beam. Therefore, such apparatuses often employ vertical goniometers that fix a relatively heavy X-ray source.

[0004] However, in this case, the sample needs to be positioned on the goniometer at a 90° angle from the direction of gravity. This has drawbacks such as requiring the sample to be securely mounted on the stage and the inability to measure heavy objects. On the other hand, in recent years, horizontal goniometers with the sample mounted on a stage level with the ground have gradually become mainstream in X-ray diffraction equipment. In such a mechanism, large-scale fixation is not required, and even heavy objects are easier to measure. Furthermore, sample setup is simplified; however, this reduces the cross-precision required for analyzing small areas.

[0005] The X-ray beam position of a horizontal goniometer is less prone to shift. However, regardless of the type of goniometer used, deflection can occur due to the weight of the axis itself or machining errors caused by changes in the axis's angle, resulting in angular or positional shifts. Furthermore, the X-ray beam position or the measurement position of the sample shifts from the mechanical rotation axis. Therefore, in qualitative, quantitative, stress, or pole measurements performed over small areas, diffracted X-rays from areas outside the desired measurement region may be detected, including unwanted information in the analytical data. Additionally, shifts in the X-ray beam position or the measurement position of the sample affect the diffraction angle, reducing measurement accuracy.

[0006] In contrast, known techniques for aligning minute regions on a sample with a rotation axis (Patent Documents 1-4) exist. In the technique described in Patent Document 1, the sample is positioned with the X-ray irradiation position from the X-ray irradiation unit as the rotation axis, and the direction of the principal strain is used as the relationship between the sample's rotation angle and the diffraction angle. In the technique described in Patent Document 2, any part of the sample is positioned at an arbitrary angle on the optical path of the incident X-ray beam, and the residual stress is measured using an X-ray diffraction apparatus that rotates the sample with the optical axis of the incident X-ray beam as the rotation axis.

[0007] Furthermore, in the technology described in Patent Document 3, the rotation axis of the ψ-axis is kept on the θ-axis by adjusting the position of the fluorescent plate on the uniaxial stage and the position of the laser displacement meter's spot, corresponding to various changes in the tilt angle ψ. In the technology described in Patent Document 4, the extraction angle of the X-rays extracted from the X-ray source is changed by rotating and tilting around the rotation axis of the X-ray source, which is located separately from the tip of the X-ray incident arm, so that the X-rays incident on the sample can always irradiate the same irradiation position on the sample.

[0008] Existing technical documents

[0009] Patent documents

[0010] Patent Document 1: Japanese Patent Application Publication No. 03-269351

[0011] Patent Document 2: Japanese Patent Application Publication No. 05-288616

[0012] Patent Document 3: Japanese Patent Application Publication No. 07-260598

[0013] Patent Document 4: Japanese Patent Application Publication No. 08-94549

[0014] As mentioned above, various mechanisms have been proposed to date for aligning minute areas on a specimen with the axis of rotation. However, it has not been possible to accurately and precisely correct for the offset of the beam irradiation position caused by changes in the angle of the mechanical axis using a stable, objective method. Summary of the Invention

[0015] The present invention was made in view of this situation, and its object is to provide a calibration amount determination device, method, recording medium and fixture that can accurately and precisely correct beam irradiation position offsets that accompany changes in mechanical axis through a stable and objective method, and can irradiate X-rays at a constant position even when the sample is rotated.

[0016] (1) In order to achieve the above objective, the correction amount determination device of the present invention is a correction amount determination device for determining the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, characterized in that it comprises: a diffraction data storage unit that stores diffraction data obtained by irradiating a standard sample, which is an aggregate of isotropic and strain-free crystal particles, with X-rays, including a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height; a correspondence determination unit that determines a first correspondence based on the diffraction data; and a correction amount determination unit that determines the correction amount of the sample surface height relative to the desired sample rotation angle and the diffraction angle by means of the first correspondence.

[0017] (2) In addition, the correction amount determination device of the present invention is characterized in that the sample rotation angle is at least one of the angle χ, which is perpendicular to the scattering vector and about the X-ray travel direction, and the angle ω, which is about the axis perpendicular to the optical surface.

[0018] (3) In addition, the correction amount determination device of the present invention is characterized in that the first correspondence is a polynomial of the diffraction angle having a polynomial of the sample rotation angle as a coefficient and representing the correction amount of the sample surface height.

[0019] (4) In addition, the calibration amount determination device of the present invention is characterized in that it further comprises a sample position control unit, which controls the relative position of the sample with respect to the desired sample rotation angle and the diffraction angle by a calibration amount of the sample surface height.

[0020] (5) In addition, the correction amount determination device of the present invention is characterized in that it further comprises a reference position data storage unit, which stores reference position data in a direction parallel to the sample surface measured by a fixture after the position of the sample surface height direction has been corrected and controlled relative to the desired sample rotation angle and the diffraction angle, and the correction amount determination unit determines the correction amount in the direction parallel to the sample surface based on the reference position data through a second correspondence.

[0021] (6) In addition, the correction amount determination device of the present invention is characterized in that the second correspondence is a polynomial of the diffraction angle having a polynomial of the sample rotation angle as a coefficient and representing the correction amount of the direction parallel to the sample surface.

[0022] (7) In addition, the fixture of the present invention is a flat plate fixture for correcting the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system. It is characterized in that the light-receiving surface has adjacent first regions and second regions formed by materials with different intensities of scattered X-rays, and is mounted to the X-ray diffraction device in such a way that the irradiation position can be scanned across the boundary of the first region and the second region to measure the intensity of scattered X-rays.

[0023] (8) In addition, the clamp of the present invention is characterized in that the boundary between the first region and the second region is an orthogonal straight line.

[0024] (9) In addition, the clamp of the present invention is characterized in that the first region is formed of stainless steel and the second region is formed of Si.

[0025] (10) In addition, the fixture of the present invention is characterized in that the second region is formed by an aggregate of crystal particles.

[0026] (11) In addition, the correction amount determination method of the present invention is a correction amount determination method for determining the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, characterized in that it includes: a step of obtaining diffraction data, said diffraction data being obtained by irradiating a standard sample, which is an aggregate of isotropic and strain-free crystal particles, with X-rays, including a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height; a step of determining a first correspondence based on said diffraction data; and a step of determining a correction amount of the sample surface height relative to the desired sample rotation angle and the diffraction angle through said first correspondence.

[0027] (12) In addition, the correction amount determination procedure of the present invention is a correction amount determination procedure for determining the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system. It is characterized in that the computer performs: a process to determine a first correspondence based on diffraction data, said diffraction data being obtained by irradiating a standard sample, which is an aggregate of isotropic and strain-free crystal particles, with X-rays, including a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height; and a process to determine the correction amount of the sample surface height relative to the desired sample rotation angle and the diffraction angle through said first correspondence. Attached Figure Description

[0028] Figure 1A and Figure 1B It is a 3D diagram showing the XYZ coordinates before and after rotation around the x-axis.

[0029] Figure 2A and Figure 2B These are 3D diagrams showing the XYZ coordinates before and after rotation around the ω-axis.

[0030] Figure 3 This is a schematic diagram showing the change in the height of the sample surface and the error in the diffraction angle caused by the shift in the beam irradiation position.

[0031] Figure 4 This is a schematic diagram showing the configuration of an X-ray measurement system.

[0032] Figures 5A to 5C These are, respectively, a top view of an example fixture and a coordinate graph showing the intensity of scattered light when the beam illumination position is scanned X and Y on the fixture.

[0033] Figures 6A to 6C These are, respectively, a top view of an example fixture and a coordinate graph showing the intensity of scattered light when the beam illumination position is scanned X and Y on the fixture.

[0034] Figure 7A and Figure 7B These are, respectively, a top view of an example fixture and a coordinate graph showing the intensity of scattered light when the beam irradiation position is scanned in a certain direction on the fixture.

[0035] Figure 8A and Figure 8B These are, respectively, a top view of an example fixture and a coordinate graph showing the intensity of scattered light when the beam irradiation position is scanned in a certain direction on the fixture.

[0036] Figure 9 This is a top view showing an example of a clamp.

[0037] Figure 10 This is a block diagram showing the structure of an X-ray measurement system.

[0038] Figure 11 This is a flowchart illustrating a method for correcting the beam irradiation position.

[0039] Figure 12A and Figure 12B This is a flowchart showing the method for determining the correspondence between the correction amounts in the Z and XY directions.

[0040] Figure 13 The coordinate graph of 2θ was plotted for each change of Z in χ on the diffraction plane (111) of the Si powder sample.

[0041] Figure 14A and Figure 14B The coordinate graphs of the coefficients Aχ and Bχ of the function with respect to χ are plotted respectively.

[0042] Figure 15 It plots the coordinates of Z obtained by using functions for each χ and θ.

[0043] Figures 16A-16C The graphs are plotted for the coefficients Dχ, Eχ, and Fχ of the function with respect to χ.

[0044] Figure 17A and Figure 17B The graphs show the coordinates of X obtained by applying functions to each θ when χ = 0° and 30°.

[0045] Figure 18A and Figure 18B The graphs show the coordinates of Y obtained by applying functions to each θ when χ = 0° and 30°.

[0046] Figures 19A-19C The graphs show the coordinates of the coefficients Hχ, Iχ, and Jχ of the function with respect to χ.

[0047] Figures 20A to 20C The graphs show the coordinates of the coefficients Lχ, Mχ, and Nχ of the function with respect to χ.

[0048] Figure 21 The diffraction plane (111) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0049] Figure 22 The diffraction plane (220) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0050] Figure 23 The diffraction plane (311) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0051] Figure 24 The diffraction plane (400) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0052] Figure 25 The diffraction plane (331) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0053] Figure 26 The diffraction plane (422) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0054] Figure 27 The diffraction plane (511) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0055] Figure 28 The diffraction plane (440) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0056] Figure 29 The diffraction plane (531) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0057] Figure 30 The diffraction plane (620) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0058] Figure 31The diffraction plane (533) of the unstrained Si powder sample shows the coordinate plots of the corrected and uncorrected samples relative to sin2ψ and 2θ, respectively.

[0059] Explanation of reference numerals in the attached figures

[0060] 100 X-ray measurement system

[0061] 200 X-ray diffraction apparatus

[0062] 210 X-ray Irradiation Section

[0063] 230 Sample Stage

[0064] 232 bracket

[0065] 235 Base

[0066] 237 Head

[0067] 238 Sample Plate

[0068] 240° goniometer

[0069] 250 detectors

[0070] 300 Computer (Calibration Determination Device)

[0071] 310 Diffraction Data Storage Unit

[0072] 320 Correspondence Determination Department

[0073] 330 Correction Quantity Determination Section

[0074] 350 Reference Location Data Storage Unit

[0075] 370 Calibration Storage Unit

[0076] 380 Sample Position Control Unit

[0077] 400, 500 clamps

[0078] 410, 510, Area 1

[0079] 420, 520, Area 2

[0080] R1 Incident X-ray

[0081] R2 diffraction beam

[0082] S0 sample. Detailed Implementation

[0083] Next, embodiments of the present invention will be described with reference to the accompanying drawings. For ease of understanding, the same constituent elements in each drawing will be labeled with the same reference numerals, and repeated descriptions will be omitted.

[0084] [principle]

[0085] Ideally, when performing X-ray diffraction measurements on a small area of ​​a sample, the X-ray beam should irradiate a point specified by the user, even if the angle of the mechanical axis is changed. However, due to deflection caused by machining precision or the weight of the shaft, the irradiation position of the X-ray beam or the measurement position of the sample may shift from the reference position.

[0086] Deflection or offset of mechanical shafts can be attributed to several main factors, including the shaft's precision and torque caused by its own weight. However, existing methods, which adjust both the X-ray beam irradiation position and the sample measurement position to the mechanical rotation axis position of each shaft, cannot adjust positional offsets caused by deflection or other factors resulting from shaft displacement. Moreover, adjusting positional offsets caused by such displacements is difficult.

[0087] In this invention, instead of adjusting the X-ray beam position and the measurement position of the sample to the position of the mechanical rotation axis, the offset of the X-ray beam irradiation position or the measurement position of the sample caused by the tilt of the sample is corrected.

[0088] Figure 1A and Figure 1B This is a three-dimensional view showing the XYZ coordinates before and after rotation about the x-axis. The x-axis is parallel to the smooth surface. Furthermore, the XYZ coordinates are based on the sample S0. The Z-axis is perpendicular to the sample surface, and the X and Y axes are parallel to the sample surface. For rotation about the x-axis, the X-axis is aligned with the x-axis. The Y-axis is perpendicular to the X-axis.

[0089] When the beam irradiation position shifts due to rotation along the x-axis, 2θ remains unchanged even if there is a shift in the x-axis direction. When the beam irradiation position shifts along the y-axis due to rotation along the x-axis, the height Z of the sample surface irradiated by the X-rays changes according to the sample rotation angle χ around the x-axis, thus changing 2θ. Furthermore, the beam irradiation positions in both the x-axis and y-axis directions also shift according to χ. When the beam irradiation position shifts along the z-axis due to rotation along the x-axis, the height Z of the sample surface irradiated by the X-rays also changes, thus changing the 2θ angle. Furthermore, the beam irradiation positions in both the x-axis and y-axis directions also shift according to χ.

[0090] Figure 2A and Figure 2BThese are three-dimensional diagrams showing the XYZ coordinates before and after rotation around the ω-axis. The ω-axis is the axis perpendicular to the optical surface. The Y-axis coincides with the ω-axis. When the beam irradiation position in the X-axis direction shifts due to rotation around the ω-axis, the height Z of the sample surface irradiated by the X-rays changes, corresponding to the angle ω around the ω-axis, thus altering 2θ. Furthermore, the beam irradiation position in the X-axis direction also shifts according to ω.

[0091] When the X-rays shift towards the Y-axis due to rotation along the ω-axis, the height Z of the sample surface irradiated by the X-rays does not change with ω, and 2θ remains constant. However, when the X-rays shift towards the Z-axis due to rotation along the ω-axis, the height Z of the sample surface irradiated by the X-rays changes with ω, thus altering the 2θ angle. Furthermore, the beam irradiation position along the X-axis also shifts with ω.

[0092] Furthermore, when placing the specimen on the specimen stage, the surface of the specimen to be measured may sometimes be tilted around the ω-axis. In this case, since the goal is to measure the specimen surface with its normal perpendicular to the χ-axis, the specimen is rotated around the ω-axis to adjust its tilt, and then rotated around the χ-axis for measurement. Although this adjustment is merely an operation to align the optical axis with the reference angle, it alters the mechanical axis from its initial configuration. If there is also deflection of the mechanical axis, the beam position will shift when the specimen is not tilted around the ω-axis compared to when it is tilted around the ω-axis. Therefore, a correction considering both the χ-axis and ω-axis angular positions is required.

[0093] In the above-described case, the powder sample is moved along the Z-axis to obtain its X-ray profile in order to correct for the offset. Furthermore, the movement of the sample is relative; it can be either the movement of the sample itself or the movement of the entire goniometer, including the X-ray source and detector.

[0094] The sample is rotated at arbitrary angular intervals by varying the rotation angle χ, causing the sample surface to move to an arbitrary Z position at each χ angle, corresponding to an arbitrary 2θ angle. At this point, the X-ray irradiation position does not shift along the Z-axis at each χ position. This is because, for powder samples, shifts in the XY-axis directions do not affect the peak position of the X-ray profile. By determining the height Z at each sample rotation angle, corresponding to an arbitrary diffraction angle 2θ, using the relationship between 2θ and Z, the effects of height shifts caused by shifts in the rotation axis and beam irradiation position can be corrected.

[0095] Figure 3 This is a schematic diagram showing the change in sample surface height and the error in diffraction angle caused by the shift in the beam irradiation position. (See diagram for example.) Figure 3 As shown, due to the shift in the beam irradiation position, the height Z of the sample surface changes, thus 2θ also produces Δ2θ=tan-1 The change in (ΔL / camera length).

[0096] In such Figure 3 When the X-ray irradiation position shifts along the Y-axis, the position also changes along the Y and Z axes due to the change in the sample rotation angle χ. Furthermore, even if the χ-axis angle changes, the height position Z should remain the same, but it does change, and the 2θ angle also changes. Therefore, the sample position is adjusted to an X-ray irradiation position with an arbitrary χ angle. In such cases... Figure 3 In the event of such a shift, the shift in the X-ray irradiation position can be corrected by adjusting the goniometer, which includes the sample or X-ray source and detector, in the Z and Y axes.

[0097] To correct for the Z-axis offset, the amount of offset is determined by the tendency of the 2θ angle to change when the Z-axis is varied at each angle along the χ-axis using a powder sample. Since a strain-free powder sample is used, the diffraction angle 2θ does not change even if the sample rotation angle χ is different. Therefore, it is effective to determine the relationship between 2θ and Z using the same diffraction plane as a reference.

[0098] The rotation of the sample relative to the measurement system that produces the above-described shift in the X-ray irradiation position implies a relative rotation between the measurement system and the sample. That is, the rotation of the sample relative to the measurement system includes not only the case of sample rotation but also the case of measurement system rotation.

[0099] [First Implementation]

[0100] (The overall structure of the system)

[0101] Figure 4 This is a schematic diagram showing the configuration of an X-ray measurement system 100. The X-ray measurement system 100 includes an X-ray diffraction device 200 and a computer 300 (calibration determination device). These devices and components are connected via wired or wireless means, enabling the transmission and reception of control information, measurement data, etc. Furthermore, the computer 300 can also be located in the cloud.

[0102] (Composition of an X-ray diffraction apparatus)

[0103] The X-ray diffraction apparatus 200 includes an X-ray irradiation unit 210, a sample stage 230, and a detector 250. The X-ray diffraction apparatus 200 is used for X-ray diffraction measurements and is controlled by a computer 300. Diffraction data acquired by the X-ray diffraction apparatus 200 is transmitted to the computer 300.

[0104] The X-ray irradiation unit 210 generates X-rays and irradiates the sample with them. The X-rays generated during the generation stage can be monochromatic, or they can be filtered into monochromatic X-rays along the path until they reach the detector 250. The system is designed to detect the composition of diffraction data based on monochromatic X-rays, at least during the detection stage. By irradiating the sample with monochromatic X-rays, diffraction beams varying according to lattice plane spacing can be detected simultaneously. CuKα rays are preferably used as monochromatic X-rays. Preferably, the X-ray irradiation unit 210 is equipped with a collimator or similar device, allowing the beam size to be adjusted according to the grain size of the sample.

[0105] The sample stage 230 can hold the sample S0 and can adjust and fix the position of the X-ray irradiated object to a specific position. For example... Figure 4 As shown, the sample stage 230 can be operated by an adjustment mechanism equipped with a motor, etc., via a control signal from the computer 300. As a result, the position of the sample S0 can be adjusted by rotating along the x-axis, rotating along the ω-axis, moving along the X-axis, moving along the Y-axis, and moving along the Z-axis. Details of the adjustment mechanism will be described later. Incident X-rays R1 are emitted from the X-ray irradiation unit 210 and diffracted at the irradiation position of the sample S0 to produce a diffracted beam R2. The angle of the diffracted beam R2 relative to the incident X-ray R1 can be represented by 2θ. Furthermore, correction control can also perform equivalent movements on other axes instead of movements based on the XYZ axes.

[0106] Detector 250 generates an electrical signal based on the intensity of the X-rays incident on the detection surface. This allows for the detection of the diffracted beam generated by sample S0. From the viewpoint of ease of peak detection, a two-dimensional detector is preferred for detector 250. A semiconductor detector can be used as detector 250. The position of detector 250 can be adjusted via a control signal from computer 300.

[0107] (Adjustment of organizational structure)

[0108] The sample stage 230 includes a base 235, a head 237, and a sample plate 238. The x-axis bracket (x-axis adjustment mechanism) 232 is integrated with the base 235 and allows the entire sample stage to swing along the bracket 232. The base 235 has a z-axis adjustment mechanism and... Z-axis rotation mechanism. The Z-axis adjustment mechanism adjusts the height of the sample S0. The shaft rotation mechanism rotates the sample S0. The head 237 can be removed or replaced depending on the purpose of the measurement. The head 237 is equipped with an XY axis adjustment mechanism that allows movement parallel to the stage surface. The head 237 is configured to mount the sample plate 238 on its upper part.

[0109] Figure 4The goniometer 240 shown has an incident arm and an exit arm. The incident arm supports the X-ray irradiation unit 210, and the exit arm supports the detector 250. Furthermore, the incident arm is connected to an ω(θs) rotation system that rotates in the vertical direction (arrow ω) toward the sample surface. Additionally, the exit arm is connected to a 2θ(θd) rotation system that rotates relative to the direction perpendicular to the sample surface (arrow 2θ), and a 2θχ rotation system that rotates relative to the direction horizontal to the sample surface (arrow 2θχ). The goniometer 240 is configured, for example, to perform measurements along five axes (ω, χ, ...). Scanning of 2θ and 2θχ axis.

[0110] The ω-axis is the in-plane rotation axis (perpendicular to the surface) of the stage on which the specimen is placed. The ω-axis controls the angle of X-rays incident on the specimen surface by controlling the posture of the specimen or X-ray source. The χ-axis controls the inclination (tilt angle) of the specimen reference plane in a direction perpendicular to the direction of X-ray travel when ω is 0°.

[0111] (Composition of the clamp)

[0112] It is preferable to use a jig for correcting the beam irradiation position in the XY direction. Figures 5A to 5C The figures show a top view of an example fixture 400 and a coordinate graph showing the intensity of scattered light when the beam irradiation position is scanned X and Y on the fixture 400. The fixture 400 is formed in a flat plate shape to correct for the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system. The fixture 400 includes, for example, a first region and a recess forming a second region, in which a standard sample is filled. The fixture 400 is mounted to an X-ray diffraction apparatus in such a way that the intensity of scattered X-rays can be measured by scanning the irradiation position across the boundary between the first and second regions.

[0113] The fixture 400 has adjacent first regions 410 and second regions 420 on its light-receiving surface, formed by materials whose intensity of fluorescent X-rays differs from that of the X-rays being irradiated. Therefore, the beam irradiation position on the sample can be determined based on the position of the boundary formed by the first region 410 and the second region 420. The first region 410 forms a frame surrounding a central portion, and the second region 420 forms a square central portion.

[0114] Preferably, the boundary between the first region 410 and the second region 420 is an orthogonal straight line. This allows the boundary of the orthogonal straight line to be used as a reference position in the X and Y directions. Furthermore, it is preferable that the first region 410 is made of stainless steel and the second region 420 is made of Si. This makes it particularly easy to locate the boundary from the difference in the emission intensity of fluorescent X-rays, especially for the characteristic X-rays of Cu. Additionally, X-rays of other wavelengths can be used instead of the characteristic X-rays of Cu. Moreover, the materials of the first region 410 and the second region 420 can be any combination that allows the boundary to be identified from the difference in the emission intensity of fluorescent X-rays generated based on the wavelength of the irradiated X-rays, or they can be made of materials different from those described above.

[0115] Further preferably, the second region 420 forms a flat, light-receiving surface and is formed from an aggregate of isotropic and strain-free crystal particles. Thus, the second region 420 can be used as a standard specimen with a flat, strain-free surface and a constant diffraction angle with respect to specimen rotation.

[0116] In the example above, the first region surrounds the central part, but the first region can also be formed only on one side in the X direction and one side in the Y direction. Figures 6A to 6C These are, respectively, a top view of a fixture 500 showing an example, and a coordinate graph showing the intensity of scattered light when the beam irradiation position is scanned X and Y on the fixture.

[0117] The clamp 500 has a first region 510 and a second region 520 on its light-receiving surface, and its material or other characteristics are the same as those of the clamp 400 described above. However, the first region 510 exists only on one side in the X direction and one side in the Y direction, and is formed in an L-shape. Even with this configuration, the beam irradiation position can be corrected based on the position of the boundary formed by the first region 510 and the second region 520.

[0118] The above example of a fixture can scan in two directions with a single setup, but it can also scan in only one direction. Figure 7A and Figure 7B These are, respectively, a top view of a fixture 600 showing an example, and a coordinate graph showing the intensity of scattered light when the beam irradiation position is scanned in a certain direction on the fixture.

[0119] The clamp 600 has a first region 610 and a second region 620 on its light-receiving surface, and its material or other characteristics are the same as those of the clamp 400 described above. However, the clamp 600 is formed such that the first region 610 surrounds the rectangular second region 620. In this configuration, by scanning in the direction traversing the boundary formed by the first region 610 and the second region 620, changing the orientation of the clamp 600 by 90° and scanning again in the direction traversing the boundary, a reference position can be determined, and the beam irradiation position can be corrected based on this.

[0120] Figure 8A and Figure 8B These are, respectively, a top view showing an example of a fixture 700, and a coordinate graph showing the intensity of scattered light when the beam irradiation position is scanned in a certain direction on the fixture. The fixture 700 is formed such that a second region 720 surrounds a rectangular first region 710. The fixture 700 can be used in the same way as the fixture 600.

[0121] It can also be a clamp that simply divides a region into two parts by a boundary. Figure 9 This is a top view showing an example of a clamp 800. The clamp 800 is configured to divide the area into a first region 810 and a second region 820 by a boundary. The clamp 800 can also be used in the same way as clamps 600 and 700.

[0122] (Composition of the calibration amount determination device)

[0123] Figure 10 This is a block diagram showing the configuration of the X-ray measurement system 100. The computer (calibration determination device) 300, for example a PC, consists of a processor for executing processing, a memory for storing programs, a data storage device, a hard disk, etc. The computer 300 controls the X-ray diffraction apparatus 200 and processes the measurement data. The computer 300 accepts input from the user via an input device and outputs information to the user via an output device.

[0124] The computer 300 includes a diffraction data storage unit 310, a correspondence determination unit 320, a correction amount determination unit 330, a reference position data storage unit 350, a correction amount storage unit 370, and a sample position control unit 380, which determines the correction amount for the offset of the X-ray irradiation position caused by the rotation of the sample.

[0125] The diffraction data storage unit 310 stores diffraction data obtained by irradiating a standard sample, which is an aggregate of crystal particles, with X-rays, including a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height.

[0126] The correspondence determination unit 320 determines the correspondence between the sample rotation angle and the diffraction angle and the sample height based on diffraction data. The correspondence is preferably a function, and more preferably an approximation obtained by fitting the diffraction data. Preferably, the approximation is a polynomial with the sample rotation angle as coefficients, used to calculate the diffraction angle at the sample position. Therefore, the approximation can be easily determined through fitting. Alternatively, the correspondence can also be a correspondence between the sample rotation angle and the diffraction angle and a correction quantity obtained from measurements.

[0127] The correction amount determination unit 330 determines the sample surface height relative to the desired sample rotation angle and diffraction angle as the correction amount in the Z direction using a first correspondence. Furthermore, the sample rotation angle is either the sample rotation angle χ perpendicular to the scattering vector and about the X-ray travel direction, or the angle ω about an axis perpendicular to the optical path. The correction amount determination unit 330 preferably uses a first function expressed by a mathematical formula as the first correspondence to calculate the correction amount in the Z direction, but it can also determine the correction amount in the Z direction using measured values.

[0128] Furthermore, the correction amount determination unit 330 determines the correction amounts in the X and Y directions based on the second correspondence and the reference position data. This allows the correction amounts in the X and Y directions to be determined. The correction amount determination unit 330 preferably uses a second function expressed by a mathematical formula as the second correspondence to calculate the correction amounts in the X and Y directions, but it can also determine the correction amounts in the X and Y directions using measured values.

[0129] This allows for the correction of the sample position relative to the sample rotation angle and diffraction angle, thus enabling accurate and high-precision correction of beam irradiation position offsets using a stable and objective method. Even with sample rotation, X-rays can be irradiated at specific locations, resulting in accurate and high-precision X-ray diffraction measurements of minute areas of the sample. Furthermore, it improves the measurement accuracy of the X-ray diffraction apparatus.

[0130] The reference position data storage unit 350 stores reference position data in the X and Y directions, which are parallel to the sample surface, measured by a fixture after the Z-direction position has been corrected and controlled using a Z-direction correction amount, relative to the desired sample rotation angle and diffraction angle.

[0131] The calibration value storage unit 370 stores the calibration values ​​in each direction determined by the established correspondence. The sample position control unit 380, relative to the desired sample rotation angle and diffraction angle, drives the Z-axis adjustment mechanism of the base 235 and the XY-axis adjustment mechanism of the head 237 to control the relative position of the sample using the calibration values ​​in each direction along the X, Y, and Z axes. Thus, it is possible to accurately and precisely correct for the deviation of the beam irradiation position caused by the sample rotation angle using functions or calculated calibration values ​​in each direction.

[0132] (Method for correcting and controlling beam irradiation position)

[0133] Next, the system configured as described above can be used to correct the beam irradiation position. The following is an example illustrating the method for correcting the beam irradiation position when the sample rotation angle χ is changed. Figure 11 This is a flowchart illustrating the method for correcting the beam illumination position. First, the beam reference positions in the X and Y directions are determined (step S1).

[0134] For example, the position determined by the position determination mechanism of each device can be set as the reference position. Examples of position determination mechanisms include laser irradiation mechanisms and cameras. This confirms the offset between the fixture's position and the reference position. When performing XY direction correction, the XY position of the beam irradiation position is determined using the fixture's position. For this, it is necessary to know the offset between the fixture's position and the reference position and create a correction formula based on this offset.

[0135] However, from the user's viewpoint of operability or reproducibility, it is preferable to align the fixture position with the reference position (the reference position of the device). By using this method, which improves assembly reproducibility, the fixture position is adjusted at the time of shipment from the factory, thus eliminating the need for confirmation and input of the fixture's assembly position offset when the user makes adjustments.

[0136] Regarding the offset, the center position of the powder sample located in the center of the fixture (region 2) is determined by confirming the beam position in the XY direction. If the center position of the powder sample deviates from the beam reference position (the position irradiated by the laser or the position observed by the camera), this offset needs to be added to the correction formula.

[0137] For example, the center position of the second region of the fixture can be determined using X-rays. On the other hand, the reference position on the X-ray diffraction apparatus 200 can be determined using a camera or a laser. For example, the offset can be confirmed using a camera on the X-ray diffraction apparatus 200 and an XY stage. When using a laser, it can also be confirmed from outside the X-ray diffraction apparatus 200 using a CCD camera.

[0138] Next, the diffraction angles 2θ at multiple x-coordinates and sample surface height Z are measured on each diffraction plane (step S2). When measuring Si powder using CuKα rays, 11 diffraction angles exist within a range of approximately 2θ = 28° to 140°. The 2θ angle is determined using the 2θ / θ relationship, and since the incident angle θ varies, the measurement also reflects the change in beam position due to the deflection of the mechanical shaft.

[0139] When using a powder sample as the standard sample, the diffracted beam is detected at the same diffraction angle 2θ even when the x-axis changes. Furthermore, even when the beam's irradiation position is moved in the XY direction, the diffracted beam is still obtained at the same diffraction angle 2θ. This is because the powder sample is strain-free. When the sample rotation angle x changes on a diffraction surface, the diffraction angle 2θ changes due to x. This is because the height Z of the sample surface irradiated by the beam changes due to the deflection of the mechanical axis.

[0140] Due to the deflection of the mechanical shaft and the change in the sample surface height Z, the beam irradiation position changes from a specific XY position. However, when using a powder sample, the diffraction angle 2θ does not change due to the change in the beam irradiation position in the XY direction caused by the shift in the XY irradiation position. The diffraction angle 2θ changes due to the change in the Z direction. Therefore, the sample surface height Z for which the diffraction angle 2θ, which is specific to the diffraction surface, is measured is the sample surface height Z without the shift in the beam irradiation position caused by the deflection of the mechanical shaft, etc.

[0141] Then, the relationship between 2θ and Z is summarized along with its relationship with each χ, and these relationships are also approximated using the most suitable function (step S3). Furthermore, considering the possibility that the offset between the rotation axis and the X-ray irradiation position changes due to the variation in the diffraction angle 2θ, the above relationships are determined for multiple diffraction planes. The relationships between the coefficients of the 2θ-Z relationship and χ are determined from the relationships across all diffraction planes. Details will be described later.

[0142] Using the derived function (first correspondence), set arbitrary diffraction angles 2θ and χ, and calculate the corrected sample surface height Z at these angles. With respect to any diffraction angle 2θ (incident angle θ) and any χ, the sample surface height Z that yields the same diffraction angle 2θ will be obtained. This means that at the obtained sample surface height Z, the height of the beam irradiation position is the same. Calculate the corrected sample surface height Z at any χ at diffraction angles 2θ from low to high angles. Then, move the sample surface height to the calculated Z (step S4).

[0143] Next, the XY position is confirmed by changing χ for each 2θ / θ increment (step S5). The XY position can be confirmed using a fixture and by the intensity difference of the fluorescent X-rays from the SUS and Si powders. Since confirmation by diffraction angle is not required, 2θ / θ can be confirmed at equal intervals from low to high angles. Equal intervals are preferred to effectively approximate the relationship between 2θ / θ, χ, and the XY position in the correction of the beam irradiation position in the XY direction. Furthermore, the range of 2θ / θ from low to high angles can be within the angle range used in the actual measurement.

[0144] The beam irradiation position in the XY direction is determined at each diffraction angle 2θ and each χ point with corrected sample surface height Z. At the Z-axis position determined from the sample rotation angle χ used in the measurement and the sample's 2θ angle, the offset of the X-ray irradiation position in the X and Y axes at multiple χ points is confirmed and measured using fluorescent powder, photosensitive paper, or a fixture capable of determining the X-ray irradiation position. The relationship between the offset in the X and Y axes and χ is fitted to a function, and an approximate formula (second correspondence) is determined (step S6). The offset in the X and Y axes is then determined using this formula from any diffraction angle 2θ and the χ used in the measurement.

[0145] Furthermore, when the offset of the X-ray irradiation position changes due to variations in the diffraction angle 2θ, the offsets of the X-ray irradiation position in the X and Y axes at multiple χ points across multiple diffraction planes are identified and measured. The coefficients of the relationships between 2θ and X, and 2θ and Y, are derived from the relationships across all diffraction planes and their relation to χ. The coefficients of the relationships between 2θ and X, and 2θ and Y, are obtained using the χ point used in the measurement, and the offsets in the X and Y axes at each χ point are calculated using the 2θ angle of the measured object.

[0146] Specifically, X-ray and Y-ray scans were performed using the drive mechanism of the XY stage at each 2θ / θ and each χ point to measure the fluorescence X-ray intensity of SUS and Si powders. For fixture 400, scans were performed in the order of SUS, Si powder, SUS, across the Si powder. Then, the center position in the XY direction of the fixture was determined by finding the center of the low-intensity region. The coordinates of the XY center position of the standard sample changed when the beam was shifted. For fixture 500, scans were performed from SUS to Si powder to confirm the edge of the boundary. The distance to the edge changed when the beam irradiation position shifted, thus determining the current beam irradiation position.

[0147] Alternatively, instead of XY scanning based on X-ray intensity as described above, fluorescent powder or photosensitive paper can be used, and the X-ray irradiation position can be confirmed using a camera or similar device, then the position can be quantified through image processing or similar methods. Alternatively, a laser or similar device can be used, and the X-ray beam path can be aligned with the laser beam path beforehand, the laser irradiation position can be confirmed using a camera or similar device, then the position can be quantified through image processing or similar methods.

[0148] Then, the correction formulas for the sample surface height Z and the XY position are stored as inherent correction formulas of the device (step S7). This allows for correction of the XZ position accompanying changes in the incident angle θ, as well as correction of the rotation axis of the ω-axis and the offset of the beam irradiation position. For example, by registering the correction formulas in the software, the position of the beam or sample can be corrected to the XYZ position obtained based on the incident angle θ and sample rotation angle χ determined from the measurement conditions.

[0149] Furthermore, it is preferable that all steps be performed by the manufacturer before shipment. In this case, when the measurement system changes, the user does not need to determine the beam reference position, the fixture position, or confirm the offset of the beam reference position.

[0150] (Method for determining the correspondence in the Z direction)

[0151] Figure 12A This demonstrates the method for determining the correspondence between the correction amounts in the Z direction (equivalent to...). Figure 11 The flowchart for step S3). For each diffraction plane, a polynomial is fitted to the relationship between the diffraction angle 2θ at each x-axis and the sample surface height Z (step S31).

[0152] The function, such as a linear, quadratic, or cubic function, is selected based on the measured distribution of the offset. Automatic function selection is preferred, but it can also be set to be user-selectable. However, since the sample surface height Z is a linear change in a single-axis direction, it is conceivable that a linear or quadratic function can adequately approximate it. For each sample rotation angle χ of each diffraction plane (hkl), the relationship between the diffraction angle 2θ and the sample surface height Z holds; therefore, their slopes and intercepts become coefficients for each diffraction plane and for each χ.

[0153]

[0154] The polynomial is fitted to the relationship between the coefficients of the polynomial obtained for each diffraction plane and the sample rotation angle χ (step S32). For example, the following polynomials of χ can be fitted for the slope Aχ and the intercept Bχ, respectively.

[0155]

[0156]

[0157] Using these approximations, the sample surface height Z at any χ point near the intercept Bχhkl (diffraction angle 2θ) can be calculated to obtain the same diffraction angle 2θ.

[0158] Next, using the approximation formula for each diffraction plane, we set arbitrary diffraction angles 2θ and χ, and calculate the sample surface height Z that becomes the arbitrary diffraction angle 2θ (step S33). The following functions are obtained using equations (1) to (3).

[0159]

[0160] When the diffraction angle 2θ changes, the calculated Z will change. This is not due to the diffraction angle 2θ, but rather to the X-ray incident angle θ. For convenience, it is represented by 2θ, but strictly speaking, it can be represented by θ as follows.

[0161]

[0162] The sample surface height Z is calculated at each diffraction plane and plotted for each χ. Then, using the calculated sample surface height Z at any χ on each diffraction plane, a polynomial, such as equation (6), is fitted to the data of the relationship between the diffraction angle 2θ and the sample surface height Z for each χ (step S34). The polynomial can be a linear function, a quadratic function, or a cubic function, etc. Since the mechanical deflection of the χ axis overlaps with the mechanical deflection of the 2θ / θ axis during offset, it is impossible to make a unified judgment. Therefore, it is preferable to automatically or allow the user to select the most suitable function.

[0163] Z = D χ θ 2 +E χ θ+F χ …(6)

[0164] For the data on the relationship between the coefficients of the polynomial obtained in this way and χ, a polynomial is fitted as follows (step S35).

[0165] D χ =d D χ 3 +e D χ 2 +f D χ+g D …(7)

[0166] E χ =d E χ 3 +e E χ 2 +f E χ+g E …(8)

[0167] F χ =d E χ+e E …(9)

[0168] Using equations (6), (7), (8), and (9) above, as shown below, for any diffraction surface and any x, the sample surface height Z that will result in a constant diffraction angle 2θ is calculated (step S36). At this time, if the diffraction angle 2θ is determined, the height of the beam irradiation position is determined.

[0169] Z=(d D χ3 +e D χ 2 +f D χ+g D )θ 2 +(d E χ 3 +e E χ 2 +f E χ+g E )θ+(d g χ+e E )…(10)

[0170] (Method for determining the correspondence between the X and Y directions)

[0171] Figure 12B It is a method for showing the correspondence between the correction amounts that determine the XY directions (equivalent to...) Figure 11 The flowchart of step S6). Using the measured beam irradiation positions in the X and Y directions, the data for the relationship between the diffraction angle 2θ and the X position for each χ and the relationship between the diffraction angle 2θ and the Y position are fitted with the following polynomial (step S61).

[0172] X χ =H χ θ 2 +I χ θ+J χ …(11)

[0173] Y χ =L χ θ 2 +M χ θ+N χ …(12)

[0174] For the data relating the coefficients of the polynomial obtained as an approximation to χ, the following polynomial is used for fitting (step S62).

[0175] H χ =h H χ 3 +i H χ 2 +j H χ+k H …(13)

[0176] I χ =h I χ 3 +i I χ 2 +j I χ+k I …(14)

[0177] J χ =h J χ 3 +i J χ 2 +j J χ+k J …(15)

[0178] L χ =l L χ 3 +m L χ 2 +n L χ+o L …(16)

[0179] M χ =l M χ 3 +m M χ 2 +n M χ+o M …(17)

[0180] N x =l N χ 3 +m N χ 2 +n N χ+o N …(18)

[0181] Using the approximate formulas obtained, arbitrary diffraction angles 2θ and χ are set, and the X and Y positions at these angles are obtained as shown below. That is, equation (19) is obtained through equations (11), (13) to (15). In addition, equation (20) is obtained through equations (12), (16), (17), and (18).

[0182]

[0183]

[0184] Then, subtract the offset between the fixture position and the reference position from the calculated XY position to obtain the corrected X position and Y position respectively. That is, when the offset between the fixture position and the reference position is set as ΔX and ΔY, equations (21) and (22) are obtained.

[0185]

[0186]

[0187] (Determination Method)

[0188] Using the prepared correspondences or calculated correction values ​​as described above, X-ray diffraction measurements can be performed while simultaneously controlling the beam irradiation position. First, the user places the sample on the stage and inputs measurement conditions such as the diffraction angle or sample rotation angle. Then, the user instructs the measurement to begin.

[0189] The correction positions in each of the XYZ directions are determined by setting the diffraction angle 2θ or the sample rotation angles ω and χ in the measurement conditions. Then, the function or calculated correction value is used as a correspondence. Measurements are performed while moving the beam irradiation position to the correction positions in each of the XYZ directions.

[0190] When the measurement is performed by exposure rather than scanning, the measurement can be taken simply after moving to the calibrated position. When the measurement is performed by scanning, the XYZ direction positions need to be corrected by moving the rotation axes of each sample; therefore, the XYZ direction positions need to be shifted in conjunction with the rotation axes of each sample. In this case, feedback control is preferred. Furthermore, while multiple diffraction planes were used for correction in the above example, only one diffraction plane can also be used. For example, such a method can be used in stress measurements.

[0191] [Example]

[0192] (Verification of the correction amount)

[0193] Experiments were conducted to determine the aforementioned correction amount. An existing X-ray diffraction apparatus (Rigaku SmartLab) was operated at 9 kW, and a miniature optical system unit was used in the incident optics system. Additionally, approximately... The beam diameter of CuKα X-rays.

[0194] To determine the offset of the X-ray irradiation position along the X and Y axes, a fixture containing Si powder and SUS arranged in a direction orthogonal to the axial direction was used. The intensity of the scattered rays was scanned along each of the X and Y axes, and the offset of the X-ray irradiation position was confirmed by the difference in fluorescence X-ray intensity between the Si powder and SUS.

[0195] The offsets shown in the table below can be determined within the micro-optical system unit. This represents the offset between the center position determined by the XY-axis offset and the center position calculated using the correction formula; that is, the difference between the measured value and the calculated value of the correction formula. For The beam's X-direction offset is less than ±0.05mm, therefore it can be determined that the impact on the offset measurement is small.

[0196] X position Y position Maximum value 0.039mm 0.009mm Minimum value -0.045mm -0.008mm

[0197] Next, the beam irradiation position was aligned with the reference position, and the diffraction angle was measured by changing Z at each χ for each diffraction surface. The diffraction surfaces selected were (111), (220), (311), (400), (331), (422), (511), (440), (531), (620), and (533) (the same applies below). Additionally, the sample rotation angle χ was selected as 0°, 6°, 12°, 18°, 24°, 30°, 36°, 42°, 48°, 54°, and 60° (the same applies below).

[0198] Figure 13 The coordinates of 2θ, determined by varying Z for each χ, were plotted for the diffraction plane (111) of the Si powder sample. Such plotting was performed for each diffraction plane. Then, equation (1) was fitted to each plot.

[0199] Using the approximation determined by each diffraction plane, the coefficients Aχ and Bχ were plotted by changing the sample rotation angle χ. Figure 14A and Figure 14B The coordinate graphs of the coefficients Aχ and Bχ of the approximation for χ are plotted respectively. Moreover, equations (2) and (3) are fitted to the relationship between the coefficients Aχ and Bχ and χ.

[0200] Z was plotted for each χ and each θ using the obtained approximation, and equation (6) was fitted. Figure 15 It is a coordinate graph of Z obtained from the approximation for each χ and each θ. Moreover, the coefficients Dχ, Eχ, and Fχ of the obtained approximation are plotted for each χ. Figures 16A-16C The coordinate graphs of the coefficients Dχ, Eχ, and Fχ of the approximation for χ are plotted. Then, equations (7) to (9) are fitted to the relationship between the coefficients Dχ, Eχ, and Fχ and χ. In this way, an approximation for calculating Z for each θ and each χ can be obtained.

[0201] Next, the surface height of the powder sample was adjusted to the Z calculated for each θ and each χ, and the beam irradiation positions in the X and Y directions were determined. X and Y were plotted for each χ and each θ, and equations (11) and (12) were fitted. Figure 17A and Figure 17B The coordinate graphs of X obtained by the approximation formula were plotted for each θ at χ = ​​0° and 30° respectively. Figure 18A and Figure 18B The coordinate graphs of Y obtained by the approximation formula were plotted for each θ with respect to χ = 0° and 30° respectively.

[0202] Furthermore, for each χ, the coefficients Hχ, Iχ, Jχ and Lχ, Mχ, Nχ of the obtained approximation were plotted. Figures 19A-19C The coordinate graphs of the coefficients Hχ, Iχ, and Jχ for the approximation of χ are plotted respectively. Figures 20A to 20C The coordinate graphs of the coefficients Lχ, Mχ, and Nχ of the approximation formula for χ are plotted separately. Through the above processing, the corrected positions of X, Y, and Z can be calculated using the approximation formula for each θ and each χ.

[0203] (Verification of measurements with and without calibration)

[0204] Using the calculated results above, X-ray diffraction measurements were performed on unstrained Si powder samples while correcting for the offset by varying the x-axis. X-ray stress measurements were conducted on the Si powder samples to evaluate the change in diffraction angle 2θ when x-axis was varied in each diffraction plane.

[0205] In addition, X-ray stress measurement was performed using the sin2ψ method (tilt method). Figures 21-31 This is a graph showing the coordinates of each diffraction plane of an unstrained Si powder sample with and without correction, relative to 2θ with respect to sin²ψ. In the 2θ-sin²ψ graph, χ = ψ, and in the case of the tilt method, the horizontal axis of the graph coincides with χ.

[0206] according to Figures 21-31 Without correction, the diffraction angle 2θ changes significantly with increasing χ. With correction, the change in diffraction angle 2θ is smaller compared to the uncorrected case, exhibiting a roughly constant value.

[0207] Furthermore, this application claims priority based on Japanese Patent Application No. 2021-188118, filed on November 18, 2021, the entire contents of which are incorporated herein by reference.

Claims

1. A calibration amount determination device, which determines the calibration amount for the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, characterized in that, have: A diffraction data storage unit stores diffraction data obtained by irradiating a standard sample, which is an aggregate of isotropic and strain-free crystal particles, with X-rays, including a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height. The correspondence determination unit determines the first correspondence based on the diffraction data; and The correction amount determination unit determines the correction amount of the sample surface height relative to the desired sample rotation angle and the diffraction angle through the first correspondence.

2. The calibration amount determination device according to claim 1, characterized in that, The sample rotation angle is at least one of the angle χ, which is perpendicular to the scattering vector and about the direction of X-ray travel, and the angle ω, which is about the axis perpendicular to the direction of the light path.

3. The calibration amount determination device according to claim 1 or claim 2, characterized in that, The first correspondence is a polynomial of the diffraction angle with coefficients representing the sample rotation angle and a correction amount representing the sample surface height.

4. The calibration amount determination device according to claim 1 or claim 2, characterized in that, It also includes a sample position control unit, which controls the relative position of the sample with respect to the desired sample rotation angle and the diffraction angle by a correction amount of the sample surface height.

5. The calibration amount determination device according to claim 4, characterized in that, It also includes a reference position data storage unit, which stores reference position data in a direction parallel to the sample surface, measured by a fixture after the position in the height direction of the sample surface has been corrected and controlled, relative to the desired sample rotation angle and the diffraction angle. The correction amount determination unit determines the correction amount in the direction parallel to the sample surface through the second correspondence and based on the reference position data.

6. The calibration amount determination device according to claim 5, characterized in that, The second correspondence is a polynomial of the diffraction angle with coefficients representing the polynomial of the sample rotation angle and representing the correction amount of the direction parallel to the sample surface.

7. A clamp, a flat plate-shaped clamp for correcting the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, characterized in that, The light-receiving surface has adjacent first and second regions formed by materials with different intensities of scattered X-rays. The X-ray diffraction apparatus is mounted in such a manner that the intensity of scattered X-rays can be determined by scanning the irradiation position across the boundary between the first region and the second region.

8. The clamp according to claim 7, characterized in that, The boundary between the first region and the second region is an orthogonal straight line.

9. The clamp according to claim 7 or claim 8, characterized in that, The first region is formed of stainless steel, and the second region is formed of Si.

10. The clamp according to claim 7 or claim 8, characterized in that, The second region is formed by an aggregate of crystal particles.

11. A method for determining a correction amount, which is a method for determining a correction amount based on the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, characterized in that, Include: The step of obtaining diffraction data is to irradiate a standard sample, which is an aggregate of isotropic and strain-free crystal particles, with X-rays, including a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height. The step of determining the first correspondence based on the diffraction data; and The step of determining the correction amount of the sample surface height relative to the desired sample rotation angle and the diffraction angle through the first correspondence.

12. A recording medium, a computer-readable and non-transitory recording medium for recording programs, characterized in that, The program is a correction amount determination program for determining the offset of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, and is executed by a computer: The process of determining the first correspondence based on diffraction data, which is obtained by irradiating a standard sample as an aggregate of isotropic and strain-free crystal particles with X-rays, includes a combination of diffraction angles of the irradiated X-rays relative to the sample rotation angle and the sample surface height; and The process of determining the correction amount of the sample surface height relative to the desired sample rotation angle and diffraction angle through the first correspondence.

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