Correction amount specifying device, method, program and tool

Abstract

To provide a correction quantity specification device, method, program, and fixture capable of correcting a deviation in beam irradiation position due to change of a machine axis accurately with high precision by a stable objective technique to enable irradiation of a fixed position with X rays even if a sample rotates.SOLUTION: There is provided a correction quantity specification device 300 that specifies a correction quantity for a deviation in X-ray irradiation position caused as a sample rotates relative to a measurement system, and that comprises: a diffraction data storage part 310 which stores diffraction data consisting of a combination of an angle of sample rotation and a diffraction angle of irradiation X rays to a sample surface heigh which are obtained by irradiating a standard sample as an aggregate of isotropic strain-free crystal particles with X rays; a function determination part 320 which determines first correspondence relation based upon the diffraction data; and a correction quantity specification part 330 which specifies a correction quantity for a sample surface height to a desired sample rotation angle and diffraction angle with a first function.SELECTED DRAWING: Figure 10

Description

[Technical Field]

[0001] The present invention relates to a correction amount specifying device, method, program, and tool for correcting a beam irradiation position. [Background technology]

[0002] The components of electronic devices such as televisions, personal computers, and mobile phones are becoming smaller every year. Accordingly, microscopic analysis is becoming more common when evaluating the functions and performance of these electronic devices. Furthermore, there is a trend toward miniaturization of components for transportation machinery such as automobiles to reduce CO2 emissions and improve fuel efficiency, and microscopic analysis is becoming more common.

[0003] X-rays are generally used in these analyses. To analyze a small area, a device must have high accuracy in crossing each axis in order to irradiate the X-ray beam at a specific point. For this reason, such a device must have a relatively heavy X-ray source fixed in place. Vertical Goniometer is often adopted.

[0004] However, in this case, the sample must be placed on the goniometer at a 90° angle from the direction of gravity. This has the disadvantage of requiring the sample to be placed firmly on the stage, making it impossible to measure heavy objects. On the other hand, horizontal goniometers, in which the sample is placed on a stage level with the floor, are becoming the norm in recent X-ray diffraction instruments. This type of mechanism does not require extensive fixation, making it relatively easy to measure heavy objects. Furthermore, while sample placement is simplified, the accuracy of crosstalk required to analyze micro-areas is reduced.

[0005] The horizontal goniometer is less likely to misalign the X-ray beam irradiation position. However, regardless of which goniometer is used, angular or positional misalignment occurs due to deflection caused by the weight of the axis when the axis angle is changed or by machining errors in the machine. This causes the X-ray beam irradiation position or sample measurement position to shift from the mechanical rotation axis position. As a result, when qualitative, quantitative, stress, or pole measurement of a microscopic area is performed, diffracted X-rays from areas other than the desired measurement area are detected, and unnecessary information is included in the analysis data. Furthermore, misalignment of the X-ray beam position or sample measurement position affects the diffraction angle, reducing measurement accuracy.

[0006] In response to this, techniques for aligning a minute region on a sample with a rotation axis are known (Patent Documents 1 to 4). In the technique described in Patent Document 1, the sample is positioned so that the position of X-ray irradiation from the X-ray irradiation means becomes the rotation axis, and the direction of principal strain is detected as the relationship between the rotation angle and diffraction angle of the sample. In the technique described in Patent Document 2, an arbitrary location on the sample is positioned on the optical path of the incident X-ray beam at an arbitrary angle, and residual stress is measured using an X-ray diffraction device that rotates the sample around the optical axis of the incident X-ray beam.

[0007] In addition, in the technology described in Patent Document 3, the rotation axis of the ψ axis is always positioned on the θ axis in response to each change in the tilt angle ψ by adjusting the position of the fluorescent screen on the uniaxial stage and the spot position of the laser displacement meter. In the technology described in Patent Document 4, the take-off angle of the X-rays from the X-ray source is changed by rotating and tilting around a rotation axis including the X-ray source provided away from the tip of the X-ray injection arm, so that the X-rays incident on the sample can always be irradiated at the same irradiation position on the sample. [Prior art documents] [Patent documents]

[0008] [Patent Document 1] Japanese Patent Application Publication No. 03-269351 [Patent Document 2] Japanese Patent Application Publication No. 05-288616 [Patent Document 3] Japanese Patent Application Publication No. 07-260598 [Patent Document 4] Japanese Patent Application Publication No. 08-94549 Summary of the Invention [Problem to be solved by the invention]

[0009] As mentioned above, various mechanisms have been proposed to align a microscopic area on a sample with the rotation axis, but no stable and objective method has been achieved to accurately and precisely correct the deviation in the beam irradiation position that occurs when the angle of the mechanical axis is changed.

[0010] The present invention has been made in consideration of the above circumstances, and aims to provide a correction amount specifying device, method, program, and tool that can accurately and with high precision correct beam irradiation position deviations caused by changes in mechanical axes using a stable and objective method, and that can irradiate X-rays at a constant position even if the sample rotates. [Means for solving the problem]

[0011] (1) In order to achieve the above object, the correction amount specifying device of the present invention is a correction amount specifying device that specifies a correction amount for a shift in the X-ray irradiation position caused by rotation of a sample relative to a measurement system, and is characterized by comprising: a diffraction data storage unit that stores diffraction data obtained by irradiating X-rays onto a standard sample that is an aggregate of isotropic and distortion-free crystal grains with X-rays, the diffraction data consisting of a combination of a sample rotation angle and a sample surface height, a correspondence relationship determination unit that determines a first correspondence relationship based on the diffraction data, and a correction amount specifying unit that specifies a desired correction amount for the sample rotation angle and the sample surface height relative to the diffraction angle based on the first correspondence relationship.

[0012] (2) Furthermore, the correction amount determination device of the present invention is characterized in that the sample rotation angle is at least one of an angle χ around an axis perpendicular to the scattering vector and in the direction in which the X-rays travel, and an angle ω around an axis perpendicular to the optical path plane.

[0013] (3) Furthermore, the correction amount determination device of the present invention is characterized in that the first correspondence relationship is a polynomial of the diffraction angle that has a polynomial of the sample rotation angle as a coefficient and represents the correction amount of the sample surface height.

[0014] (4) Furthermore, the correction amount specifying device of the present invention is characterized by further comprising a sample position control unit that controls the relative position of the sample with the correction amount of the sample surface height with respect to the desired sample rotation angle and the desired diffraction angle.

[0015] (5) The correction amount specifying device of the present invention further includes a reference position data storage unit that stores reference position data in a direction parallel to the sample surface measured using a jig that is controlled to correct the position of the sample surface in the height direction with respect to the desired sample rotation angle and diffraction angle, and the correction amount specifying unit is characterized in that it specifies the correction amount in the direction parallel to the sample surface based on the reference position data using a second correspondence relationship.

[0016] (6) Furthermore, the correction amount determination device of the present invention is characterized in that the second correspondence relationship is a polynomial of the diffraction angle that has a polynomial of the sample rotation angle as a coefficient and represents the correction amount in a direction parallel to the sample surface.

[0017] (7) Furthermore, the jig of the present invention is a flat jig for correcting the deviation of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, and is characterized in that it has adjacent first and second regions on the light-receiving surface formed of materials with different scattered X-ray intensities, and is attached to an X-ray diffraction device so that the irradiation position can be scanned across the boundary between the first and second regions to measure the scattered X-ray intensity.

[0018] (8) The jig of the present invention is also characterized in that the boundary between the first region and the second region is a straight line that intersects at right angles.

[0019] (9) Furthermore, the jig of the present invention is characterized in that the first region is made of stainless steel, and the second region is made of Si.

[0020] (10) Furthermore, the jig of the present invention is characterized in that the second region is formed of an aggregate of crystal grains.

[0021] (11) A correction amount specifying method of the present invention is a correction amount specifying method for specifying a correction amount for a deviation of an X-ray irradiation position caused by rotation of a sample relative to a measurement system, the method comprising the steps of: irradiating a standard sample, which is an aggregate of isotropic and distortion-free crystal grains, with X-rays, obtaining diffraction data consisting of a combination of a sample rotation angle and a diffraction angle of the irradiated X-rays relative to the sample surface height; determining a first correspondence relationship based on the diffraction data; 1st and specifying a correction amount of the sample surface height for the desired sample rotation angle and diffraction angle based on the correspondence relationship.

[0022] (12) Furthermore, the correction amount specifying program of the present invention is a correction amount specifying program for specifying a correction amount for a deviation of an X-ray irradiation position caused by rotation of a sample relative to a measurement system, characterized in that the program causes a computer to execute the following processes: determining a first correspondence relationship based on diffraction data obtained by irradiating X-rays onto a standard sample, which is an aggregate of isotropic and distortion-free crystal grains, and the diffraction angle of the irradiated X-rays relative to the sample rotation angle and the sample surface height; and specifying a desired correction amount for the sample rotation angle and the sample surface height relative to the diffraction angle based on the first correspondence relationship. [Brief explanation of the drawings]

[0023] [Figure 1] 10A and 10B are perspective views showing XYZ coordinates before and after rotation around the χ axis, respectively. [Figure 2] 10A and 10B are perspective views showing XYZ coordinates before and after rotation around the ω axis, respectively. [Figure 3] 1 is a schematic diagram showing a change in sample surface height and an error in diffraction angle caused by a deviation in the beam irradiation position. [Figure 4] FIG. 1 is a schematic diagram showing the configuration of an X-ray measurement system. [Figure 5] 10(a) to 10(c) are plan views showing an example of a jig, and graphs showing the intensity of scattered light when the beam irradiation position on the jig is scanned in the X and Y directions. [Figure 6] 10(a) to 10(c) are plan views showing an example of a jig, and graphs showing the intensity of scattered light when the beam irradiation position on the jig is scanned in the X and Y directions. [Figure 7] 1A and 1B are a plan view showing an example of a jig, and a graph showing the intensity of scattered light when the beam irradiation position on the jig is scanned in a certain direction. [Figure 8] 1A and 1B are a plan view showing an example of a jig, and a graph showing the intensity of scattered light when the beam irradiation position on the jig is scanned in a certain direction. [Figure 9] FIG. 1 is a plan view showing an example of a jig. [Figure 10] FIG. 1 is a block diagram showing the configuration of an X-ray measurement system. [Figure 11] 10 is a flowchart showing a method for correcting a beam irradiation position. [Figure 12] 10A and 10B are flowcharts showing a method for determining a correspondence relationship for obtaining correction amounts in the Z direction and the X and Y directions, respectively. [Figure 13] This is a graph plotting 2θ measured for each χ while changing Z for the diffraction plane (111) of a Si powder sample. [Figure 14] (a) and (b) are graphs plotting the coefficients Aχ and Bχ of the functions against χ, respectively. [Figure 15] This is a graph plotting Z obtained as a function for each χ and each θ. [Figure 16] (a) to (c) are graphs plotting the coefficients of the functions Dχ, Eχ, and Fχ against χ, respectively. [Figure 17] (a) and (b) are graphs plotting the function X for each θ when χ = 0° and 30°, respectively. [Figure 18] (a) and (b) are graphs plotting the Y obtained as a function for each θ when χ = 0° and 30°, respectively. [Figure 19] (a) to (c) are graphs plotting the coefficients of the functions Hχ, Iχ, and Jχ against χ, respectively. [Figure 20] (a) to (c) are graphs plotting the coefficients of the functions Lχ, Mχ, and Nχ against χ, respectively. [Figure 21] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (111) of an unstrained Si powder sample. [Figure 22] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (220) of an unstrained Si powder sample. [Figure 23] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (311) of an unstrained Si powder sample. [Figure 24] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (400) of an unstrained Si powder sample. [Figure 25] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (331) of an unstrained Si powder sample. [Figure 26] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (422) of an unstrained Si powder sample. [Figure 27] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (511) of an unstrained Si powder sample. [Figure 28] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (440) of an unstrained Si powder sample. [Figure 29] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (531) of an unstrained Si powder sample. [Figure 30] 10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (620) of an unstrained Si powder sample. [Figure 31]10 is a graph showing 2θ versus sin2ψ with and without correction for the diffraction plane (533) of an unstrained Si powder sample. DETAILED DESCRIPTION OF THE INVENTION

[0024] 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.

[0025] [principle] When performing X-ray diffraction measurements on a microscopic region of a sample, ideally the X-ray beam should be directed at a single point specified by the user, even if the angle of the mechanical axis is changed. However, due to factors such as deflection caused by machining precision or the weight of the axis, the irradiation position of the X-ray beam or the measurement position on the sample can deviate from the reference position.

[0026] Deflection and misalignment of mechanical axes can be attributed to several factors, including the precision of the mechanical axes and moments due to their own weight. However, with conventional methods that adjust both the X-ray beam irradiation position and the sample measurement position to the mechanical rotation axis position of each axis, it is not possible to adjust for positional misalignment caused by deflection when the axes are moved. Furthermore, it is difficult to adjust for positional misalignment when both are moved.

[0027] In the present invention, instead of adjusting the X-ray beam position and the sample measurement position to the mechanical rotation axis position, the deviation of the X-ray beam irradiation position or the sample measurement position caused by the tilt of the sample is corrected.

[0028] Figures 1(a) and (b) are perspective views showing the XYZ coordinates before and after rotation around the χ axis, respectively. The χ axis is an axis parallel to the optical path plane. The XYZ coordinates are coordinates 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. When rotating around the χ axis, the X axis coincides with the χ axis. The Y axis is perpendicular to the X axis.

[0029] When the beam irradiation position shifts due to rotation around the chi-axis, 2θ does not change even if there is a shift in the X-axis direction. When there is a shift in the Y-axis direction due to rotation around the chi-axis, 2θ changes because the height Z of the sample surface where the X-rays are irradiated changes according to the sample rotation angle χ around the chi-axis. In addition, the beam irradiation position in the X-axis and Y-axis directions also shifts according to χ. When there is a shift in the Z-axis direction due to rotation around the chi-axis, the height Z of the sample surface where the X-rays are irradiated also changes, causing a change in the 2θ angle. In addition, the beam irradiation position in the X-axis and Y-axis directions also shifts according to χ.

[0030] Figures 2(a) and (b) are perspective views showing the XYZ coordinates before and after rotation around the ω axis, respectively. The ω axis is perpendicular to the optical path plane. The Y axis coincides with the ω axis. If the beam irradiation position in the X axis direction shifts due to rotation around the ω axis, the height Z of the sample surface where the X-rays are irradiated changes according to the angle ω around the ω axis, which changes 2θ. The beam irradiation position in the X axis direction also shifts according to ω.

[0031] When misalignment occurs in the Y-axis direction due to rotation around the ω axis, the height Z of the sample surface where the X-rays are irradiated does not change according to ω, and 2θ remains unchanged. When misalignment occurs in the Z-axis direction due to rotation around the ω axis, the height Z of the sample surface where the X-rays are irradiated changes according to ω, and the 2θ angle changes. In addition, the beam irradiation position in the X-axis direction also shifts according to ω.

[0032] Furthermore, when the sample is placed on the stage of the sample holder, the surface of the sample to be measured may be tilted around the ω axis. In this case, to measure the normal to the sample surface perpendicular to the χ axis, the sample is rotated around the ω axis to adjust the tilt, and then rotated around the χ axis for measurement. This adjustment is simply an operation to align the optical axis with a reference angle, but it changes the mechanical axis from its initial position. In this case, if there is deflection of the mechanical axis, the beam position will deviate when the sample is tilted around the ω axis compared to when it is not tilted, so corrections must be made taking into account the angular positions of both the χ axis and the ω axis.

[0033] In such cases, the powder sample is moved in the Z-axis direction to correct the misalignment and acquire its X-ray profile. Note that the sample movement is relative, and can be either the sample itself or the entire goniometer including the X-ray source and detector.

[0034] The sample rotation angle χ is changed at arbitrary angular intervals, and the sample surface is moved to a Z position that results in an arbitrary 2θ angle at each χ. At this time, the X-ray irradiation position at each χ will not be misaligned along the Z axis. This is because, for powder samples, misalignment in the X and Y axes does not affect the peak position of the X-ray profile. From the relationship between 2θ and Z, the height Z at which an arbitrary diffraction angle 2θ is achieved at each sample rotation angle can be calculated, allowing correction for the effects of height misalignment due to misalignment between the rotation axis and the beam irradiation position.

[0035] Figure 3 is a schematic diagram showing the change in sample surface height and the error in the diffraction angle caused by the deviation of the beam irradiation position. As shown in Figure 3, the deviation of the beam irradiation position causes the change in the sample surface height Z, which also affects 2θ, as shown by Δ2θ=tan -1 A change of (ΔL / camera length) occurs.

[0036] As shown in Figure 3, if the X-ray irradiation position is misaligned in the Y-axis direction, the X-ray irradiation position also changes in the Y-axis and Z-axis directions as the sample rotation angle χ changes. Even if the angle of the χ axis changes, the height position Z should remain the same, but this changes, resulting in a change in the 2θ angle. Therefore, the sample position is adjusted to the X-ray irradiation position irradiated at an arbitrary χ. When the X-ray irradiation position is misaligned as shown in Figure 3, the misalignment can be corrected by adjusting the sample or the goniometer, which includes the X-ray source and detector, in the Z-axis and Y-axis directions.

[0037] To correct for Z-axis misalignment, a powder sample is used, and the amount of misalignment is determined from the tendency of change in the 2θ angle when the Z axis is changed for each angle of the χ axis. Because an unstrained powder sample is used, the diffraction angle 2θ does not change even if the sample rotation angle χ changes. Therefore, it is effective to determine the relationship between 2θ and Z measured using the same diffraction plane as the reference.

[0038] The rotation of the sample relative to the measurement system, which causes the deviation of the X-ray irradiation position, refers to the relative rotation between the measurement system and the sample. In other words, the rotation of the sample relative to the measurement system includes not only the rotation of the sample but also the rotation of the measurement system.

[0039] [First embodiment] (Overall system configuration) 4 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 (correction amount specifying device). These devices and components are connected by wire or wirelessly, and are capable of transmitting and receiving control information, measurement data, and the like. The computer 300 may be placed on the cloud.

[0040] (Configuration of X-ray diffraction equipment) 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 measurement and is controlled by a computer 300. The diffraction data acquired by the X-ray diffraction apparatus 200 is transmitted to the computer 300.

[0041] The X-ray irradiation unit 210 generates X-rays and irradiates the sample with the generated X-rays. The X-rays may be monochromatic X-rays at the generation stage, or may be filtered to become monochromatic X-rays on the path before entering the detector 250. The system is configured to be able to detect diffraction data using monochromatic X-rays at least at the detection stage. By irradiating the sample with monochromatic X-rays, it is possible to simultaneously detect different diffracted beams depending on the lattice spacing. It is preferable to use CuKα rays as the monochromatic X-rays. The X-ray irradiation unit 210 is preferably equipped with a collimator or the like, and is capable of adjusting the beam size to match the size of the crystal grains of the sample.

[0042] The sample stage 230 can mount the sample S0 and fix the measurement target to be irradiated with X-rays at a specific position. As shown in Figure 4, the sample stage 230 can operate an adjustment mechanism equipped with a motor, etc., in response to a control signal from the computer 300. As a result, the position of the sample S0 can be adjusted by rotating it along the x-axis, ω-axis, and moving it along the x-axis, y-axis, and 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 generate a diffracted beam R2. The angle of the diffracted beam R2 relative to the incident X-rays R1 can be expressed as 2θ. Note that the correction control may involve equivalent movement along other axes instead of the X, Y, and Z axes.

[0043] The detector 250 generates an electrical signal according to the intensity of the X-rays incident on the detection surface. This allows the detection of the diffracted beam generated by the sample S0. The detector 250 is preferably a two-dimensional detector from the viewpoint of ease of peak detection. A semiconductor detector can be used as the detector 250. The position of the detector 250 can be adjusted by a control signal from the computer 300. (adjustment mechanism)

[0044] The sample stage 230 is composed of a base section 235, a head section 237, and a sample plate 238. The χ cradle (χ axis adjustment mechanism) 232 and the base section 235 are integrated, and the entire sample stage can be swung along the cradle 232. The base section 235 has a Z axis adjustment mechanism and a φ axis rotation mechanism. The Z axis adjustment mechanism adjusts the height of the sample S0. The φ axis rotation mechanism rotates the sample S0. The head section 237 can be removed and replaced depending on the measurement purpose. The head section 237 is equipped with an XY axis adjustment mechanism that enables movement parallel to the stage surface. The head section 237 is configured so that the sample plate 238 can be attached to its upper section.

[0045] The goniometer 240 shown in Fig. 4 has an incident-side arm and an exit-side arm. The incident-side arm supports the X-ray irradiation unit 210, and the exit-side arm supports the detector 250. Furthermore, a ω(θs) rotation system that rotates in the vertical direction (arrow ω direction) of the sample surface is connected to the incident-side arm. Furthermore, a 2θ(θd) rotation system that rotates in the vertical direction (arrow 2θ direction) of the sample surface and a 2θχ rotation system that rotates in the horizontal direction (arrow 2θχ direction) of the sample surface are connected to the exit-side arm. The goniometer 240 is configured to be capable of scanning five axes (ω, χ, φ, 2θ, and 2θχ axes) as measurement axes, for example.

[0046] The φ axis is the in-plane rotation axis (axis perpendicular to the surface) of the stage surface on which the sample is placed. The ω axis is the axis that controls the angle of the X-rays incident on the sample surface by controlling the attitude of the sample or X-ray source. The χ axis is the axis that controls the tilt (tilt) of the sample reference plane in the direction perpendicular to the direction of X-ray propagation when the ω value is 0°.

[0047] (Jig configuration) It is preferable to use a jig to correct the beam irradiation position in the X and Y directions. Figures 5(a) to 5(c) are a plan view showing an example jig 400, and a graph showing the scattered light intensity when the beam irradiation position on the jig 400 is scanned in the X and Y directions. The jig 400 is formed in a flat plate shape and is used to correct the deviation of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system. The jig 400 is composed of, for example, depressions that form a first region and a second region, and a standard sample is filled in the depression. The jig 400 is attached to an X-ray diffraction instrument so that the irradiation position can be scanned across the boundary between the first and second regions to measure the scattered X-ray intensity.

[0048] The jig 400 has adjacent first and second regions 410 and 420 on its light-receiving surface, each made of a material that produces fluorescent X-rays with different intensities relative to the irradiated X-rays. This makes it possible to determine the beam irradiation position on the sample based on the position of the boundary formed by the first and second regions 410 and 420. The first region 410 forms a frame surrounding the center, and the second region 420 forms the center of a square.

[0049] The boundary between the first region 410 and the second region 420 is preferably a straight line that intersects at right angles. This allows the boundary to be used as a reference position in the X and Y directions. The first region 410 is preferably made of stainless steel, and the second region 420 is preferably made of silicon. This makes it easy to locate the boundary based on the difference in the amount of fluorescent X-ray radiation, particularly with respect to the characteristic X-ray radiation of Cu. X-rays of other wavelengths may be irradiated instead of the characteristic X-ray radiation of Cu. The first region 410 and the second region 420 may be made of materials other than those mentioned above, as long as the combination of materials allows the boundary to be recognized based on the difference in the amount of fluorescent X-ray radiation generated depending on the wavelength of the irradiated X-rays.

[0050] It is more preferable that the second region 420 has a flat light-receiving surface and is formed of an aggregate of isotropic and strain-free crystal grains, which allows the second region 420 to be used as a standard sample with a flat surface, strain-free, and a constant diffraction angle even with sample rotation.

[0051] In the above example, the first region surrounds the central portion, but the first region may be formed only on one side in the X direction and one side in the Y direction. Figures 6(a) to 6(c) are a plan view showing an example jig 500, and a graph showing the intensity of scattered light when the beam irradiation position on the jig is scanned in the X and Y directions.

[0052] The jig 500 has a first region 510 and a second region 520 on the light receiving surface, and the material and other characteristics are the same as those of the jig 400. 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 first region510 and the second area 520 The beam irradiation position can be corrected based on the position of the boundary formed by the above.

[0053] The above jig example can scan in two directions with a single installation, but it may also be capable of scanning in only one direction. Figures 7(a) and (b) are a plan view showing an example jig 600, and a graph showing the intensity of scattered light when the beam irradiation position on the jig is scanned in a certain direction.

[0054] Jig 600 has a first region 610 and a second region 620 on its light receiving surface, and its materials and other characteristics are the same as those of jig 400. However, jig 600 is formed such that first region 610 surrounds rectangular second region 620. With this configuration, after scanning in a direction across the boundary formed by first region 610 and second region 620, the orientation of jig 600 is changed by 90° and scanning again in a direction across the boundary, thereby identifying a reference position and making it possible to correct the beam irradiation position based on this.

[0055] 8(a) and (b) are a plan view showing an example jig 700 and a graph showing the intensity of scattered light when the beam irradiation position on the jig is scanned in a certain direction. The jig 700 is formed so that a rectangular first region 710 is surrounded by a second region 720. The jig 700 can be used in the same way as the jig 600.

[0056] The jig may simply be one in which a single boundary divides the area into two. Fig. 9 is a plan view showing an example of jig 800. Jig 800 is configured such that a single boundary divides the area into a first area 810 and a second area 820. Jig 800 can be used in the same way as jigs 600 and 700.

[0057] (Configuration of the correction amount specifying device) 10 is a block diagram showing the configuration of the X-ray measurement system 100. The computer (correction amount specifying device) 300 is, for example, a PC, and is composed of a processor that executes processing and a memory or a hard disk that stores programs and data. The computer 300 controls the X-ray diffraction device 200 and processes measurement data. The computer 300 accepts input from a user via an input device and outputs information to the user via an output device.

[0058] The computer 300 is composed of a diffraction data storage unit 310, a correspondence relationship determination unit 320, a correction amount specification unit 330, a reference position data storage unit 350, a correction amount storage unit 370, and a sample position control unit 380, and specifies the correction amount for the shift in the X-ray irradiation position caused by the rotation of the sample.

[0059] The diffraction data storage unit 310 stores diffraction data obtained by irradiating a standard sample, which is an aggregate of crystal grains, with X-rays, and which is made up of a combination of the diffraction angle of the irradiated X-rays relative to the sample rotation angle and the sample surface height.

[0060] The correspondence relationship determination unit 320 determines a correspondence relationship that associates the sample rotation angle and diffraction angle with the sample height based on the diffraction data. The correspondence relationship is preferably a function, and more preferably an approximate expression obtained by fitting to the diffraction data. The approximate expression is preferably a polynomial of the diffraction angle that has coefficients that are polynomials of the sample rotation angle and that calculates the sample position. This makes it possible to easily determine the approximate expression by fitting. Note that the correspondence relationship may also be one that associates the correction amount obtained from actual measurement with the sample rotation angle and diffraction angle.

[0061] The correction amount specifying unit 330 specifies the sample surface height for the desired sample rotation angle and diffraction angle as the correction amount in the Z direction using the first correspondence relationship. The sample rotation angle is the sample rotation angle χ around an axis perpendicular to the scattering vector and in the direction in which the X-rays travel, or the angle ω around an axis perpendicular to the optical path plane. The correction amount specifying unit 330 preferably calculates the correction amount in the Z direction using a first function expressed by a mathematical formula as the first correspondence relationship, but it is also possible to specify the correction amount in the Z direction using actual measured values.

[0062] Furthermore, the correction amount specifying unit 330 specifies the correction amounts in the X and Y directions based on the reference position data using the second correspondence relationship. In this way, the correction amount specifying unit 330 can specify the correction amounts in the X and Y directions. It is preferable that the correction amount specifying unit 330 calculates the correction amounts in the X and Y directions using a second function expressed by a mathematical formula as the second correspondence relationship, but it is also possible to specify the correction amounts in the X and Y directions using actual measured values.

[0063] This ability to correct the sample position for the sample rotation angle and diffraction angle allows for accurate and highly precise correction of beam irradiation position deviations using a stable and objective method. Since X-rays can be irradiated to a specific position even when the sample is rotating, accurate and highly precise X-ray diffraction measurements can be made on a microscopic region of the sample. This also improves the measurement accuracy of the X-ray diffraction instrument.

[0064] The reference position data storage unit 350 stores the reference position data, which is corrected and controlled by the correction amount in the Z direction for the desired sample rotation angle and diffraction angle. Ta The reference position data in the X and Y directions parallel to the sample surface measured using the jig is stored.

[0065] The correction amount storage unit 370 stores the correction amount for each direction specified by the determined correspondence. The sample position control unit 380 drives the Z-axis adjustment mechanism of the base unit 235 and the XY-axis adjustment mechanism of the head unit 237 to control the relative position of the sample using the correction amounts in the X-, Y-, and Z-axis directions for the desired sample rotation angle and diffraction angle. This makes it possible to accurately and highly precisely correct the deviation of the beam irradiation position that occurs depending on the sample rotation angle using the correction amounts in each direction calculated or function for the sample to be measured.

[0066] (Method for correcting and controlling beam irradiation position) Next, the beam irradiation position can be corrected using the system configured as described above. As an example, a method for correcting the beam irradiation position when the sample rotation angle χ is changed will be described below. Figure 11 is a flowchart showing the method for correcting the beam irradiation position. First, the beam reference positions in the X and Y directions are determined (step S1).

[0067] For example, the position determined by the measurement position determination mechanism for each device can be used as the reference position. Examples of measurement position determination mechanisms include a laser irradiation mechanism and a camera. In this way, the deviation between the jig position and the reference position can be confirmed. When correcting in the XY direction, the jig position is used to find the XY position of the beam irradiation position. Therefore, it is necessary to understand the amount of deviation between the jig position and the reference position and create a correction formula based on that amount of deviation.

[0068] However, from the perspective of user operability and reproducibility of work, it is preferable to align the jig position with the reference position (reference position of the device). By adjusting the jig position at the time of factory shipment using this method that increases the reproducibility of installation, the user does not need to check or input the amount of misalignment of the jig installation position when making adjustments.

[0069] Regarding the amount of deviation, the center position of the powder sample in the center of the jig (second area) is determined by the procedure for checking the beam position in the X and Y directions. If there is a deviation between the center position of the powder sample and the beam reference position (the position where the laser is irradiated or the position observed by the camera), the amount of deviation must be added to the correction formula.

[0070] For example, the center position of the second region of the jig can be determined by X-rays. Meanwhile, the reference position on the X-ray diffraction device 200 is grasped by a camera or laser. For example, the amount of deviation can be confirmed on the XY stage using the camera of the X-ray diffraction device 200. When a laser is used, confirmation can also be made using a CCD camera from outside the X-ray diffraction device 200.

[0071] Next, the diffraction angle 2θ is measured at multiple χ values ​​on each diffraction plane and at the sample surface height Z (Step S2). When measuring Si powder with CuKα radiation, there are 11 diffraction angles in the range of 2θ = 28° to 140°. The 2θ angle is measured using the 2θ / θ relationship, and as the incident angle θ changes, the change in beam position, which also reflects the deflection of the mechanical axis, is measured.

[0072] When a powder sample is used as the standard sample, the diffracted beam is detected at the same diffraction angle 2θ even if χ changes. Furthermore, the diffracted beam is obtained at the same diffraction angle 2θ even if the beam irradiation position is shifted in the X and Y directions. This is because the powder sample is strain-free. When the sample rotation angle χ is changed on one diffraction plane, the diffraction angle 2θ changes depending on χ. This is because the sample surface height Z at which the beam is irradiated changes due to the deflection of the mechanical axis.

[0073] The beam irradiation position shifts from a specific XY position due to deflection of the mechanical axis and changes in the sample surface height Z. However, when using a powder sample, the diffraction angle 2θ does not change due to changes in the beam irradiation position in the XY directions caused by deviations in the XY irradiation position. The diffraction angle 2θ changes with changes in the Z direction. Therefore, the sample surface height Z at which the diffraction angle 2θ specific to the diffraction surface is measured is the sample surface height Z at which there is no deviation in the beam irradiation position due to deflection of the mechanical axis, etc.

[0074] Then, the relational expressions between 2θ and Z are summarized in relation to each χ, and these relations are also approximated using the most appropriate function (step S3). Note that the above relations are found for multiple diffraction planes, assuming that the amount of deviation between the rotation axis and the X-ray irradiation position changes as the diffraction angle 2θ changes. From the relations for all diffraction planes, the relationship between each coefficient of the relational expression between 2θ and Z and χ is found. Details will be described later.

[0075] From the obtained function (first correspondence relationship), arbitrary diffraction angles 2θ and χ are set, and the corrected sample surface height Z at those angles is calculated. For an arbitrary diffraction angle 2θ (incident angle θ) and an arbitrary χ, the sample surface height Z at which the same diffraction angle 2θ is obtained is obtained. The obtained sample surface height Z means that the height of the beam irradiation position is the same. The corrected sample surface height Z at an arbitrary χ at diffraction angles 2θ ranging from low to high angles is then calculated. Then, the sample surface height is moved to the calculated Z (step S4).

[0076] Next, the XY position is checked by changing χ for each 2θ / θ (step S5). The XY position can be checked using a jig based on the difference in intensity of the fluorescent X-rays of the SUS and Si powders. Since there is no need to check by diffraction angle, 2θ / θ can be checked at equal intervals from low to high angles. It is preferable to check at equal intervals in order to effectively approximate the relationship between 2θ / θ, χ, and XY position when correcting the beam irradiation position in the XY direction. Furthermore, the range of 2θ / θ from low to high angles can be the angle range actually used in the measurement.

[0077] The beam irradiation position in the X and Y directions is determined using the corrected sample surface height Z for each diffraction angle 2θ and each χ. At the Z-axis position determined from the sample rotation angle χ and the 2θ angle of the sample used in the measurement, the deviations of the X-ray irradiation position in the X and Y directions for multiple χ are confirmed and measured using fluorescent powder, photosensitive paper, or a jig that can identify the X-ray irradiation position. A function is fitted to the relationship between the deviations in the X and Y directions and χ to determine an approximate equation (second correspondence relationship) (step S6). This relationship is used to determine the deviations in the X and Y directions from an arbitrary diffraction angle 2θ and the χ used in the measurement.

[0078] If the deviation of the X-ray irradiation position changes with changes in the diffraction angle 2θ, check and measure the deviation of the X-ray irradiation position in the X-axis and Y-axis directions at multiple χ on multiple diffraction planes. From the equations for all diffraction planes, the relationship between χ and each coefficient in the equations relating 2θ to X and 2θ to Y is found. The coefficients in the equations relating 2θ to X and 2θ to Y are found from the χ used for measurement, and the deviation in the X-axis and Y-axis directions at each χ can be found from the 2θ angle of the object being measured.

[0079] Specifically, the XY stage's angle at each 2θ / θ and each χ Drive mechanism X- and Y-scans are performed using a fluorescein microscope (FGM) to measure the fluorescent X-ray intensity of the SUS and Si powder. For jig 400, scanning is performed in the order SUS, Si powder, and SUS, straddling the Si powder. Then, by finding the center of the low-intensity area, the center position in the XY directions of the jig can be determined. If the beam shifts, the coordinates of the XY center position of the standard sample will change. For jig 500, scanning is performed from the SUS to the Si powder to check the edge of the boundary. If the beam irradiation position shifts, the distance to the edge will change, so the current beam irradiation position can be determined.

[0080] Instead of the XY scan of X-ray intensity as described above, the X-ray irradiation position may be confirmed with a camera or the like using fluorescent powder or photosensitive paper, and the position may be digitized by image processing, etc. Alternatively, a laser or the like may be used, the optical path of the laser and the optical path of the X-ray may be aligned, the laser irradiation position may be confirmed with a camera, etc., and the position may be digitized by image processing, etc.

[0081] Then, the correction formula for the sample surface height Z and the correction formula for the XY position are stored as correction formulas specific to the device (step S7). This allows the XZ position to be corrected in accordance with changes in the incident angle θ, and also allows the deviation between the ω axis rotation axis and the beam irradiation position to be corrected. For example, by registering the correction formula in the software, the following can be done according to the incident angle θ and the sample rotation angle χ determined from the measurement conditions: obtained The beam or sample position can be corrected in the XYZ direction.

[0082] It is preferable that the manufacturer performs all steps before shipping, which eliminates the need for the user to determine the beam reference position or check the position of the jig and any deviations from the beam reference position when changing the measurement system.

[0083] (How to determine the correspondence in the Z direction) 12(a) is a flowchart showing a method for determining the correspondence relationship for obtaining the correction amount in the Z direction (corresponding to step S3 in FIG. 11). For each diffraction plane, a polynomial is fitted to the relationship between the diffraction angle 2θ at each χ and the sample surface height Z (step S31).

[0084] A function such as a linear function, quadratic function, or cubic function is selected depending on the distribution of the measured deviation. It is preferable that the function form be selected automatically, but it may also be user selectable. However, since the sample surface height Z is a linear change in one axis direction, it is believed that a linear or quadratic function can be sufficiently approximated. Since the relationship between the diffraction angle 2θ and the sample surface height Z is established for each sample rotation angle χ for each diffraction plane (hkl), the slope and intercept are coefficients for each diffraction plane and χ.

[0085]

number

[0086] A 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 polynomial of χ can be fitted to each of the slope Aχ and intercept Bχ.

[0087]

number

number

[0088] From these approximations, the intercept Bχ hklThe sample surface height Z at any χ at which the same diffraction angle 2θ is obtained can be determined.

[0089] Next, arbitrary diffraction angles 2θ and χ are set using the approximation formula for each diffraction surface, and the sample surface height Z at the arbitrary diffraction angle 2θ is determined (step S33). The following function can be determined from equations (1) to (3):

[0090]

number

[0091] The calculated Z changes as the diffraction angle 2θ changes. This is not due to the effect of the diffraction angle 2θ, but rather the effect of the X-ray incident angle θ. For convenience, it is expressed in 2θ, but strictly speaking it should be expressed in θ as follows:

[0092]

number

[0093] The sample surface height Z is calculated for each diffraction surface and plotted for each χ. Then, using the calculated sample surface height Z at any χ for each diffraction surface, a polynomial such as Equation (6) is fitted to the data relating to the diffraction angle 2θ of each diffraction surface and the sample surface height Z for each χ (step S34). A linear function, quadratic function, cubic function, or the like can be selected as the polynomial. Since the deviation involves both mechanical deflection on the χ axis and mechanical deflection on the 2θ / θ axis, it is not possible to uniformly determine the deviation. Therefore, it is preferable to select the most suitable function automatically or by the user.

[0094]

number

[0095] The relationship between the coefficients of the polynomial thus obtained and χ of The data is fitted with the following polynomial (step S35).

[0096]

number

number

number

[0097] The above equations (6), (7), and (8), From (9) Then, the sample surface height Z at which a certain diffraction angle 2θ is obtained for an arbitrary diffraction surface and an arbitrary χ is calculated as follows (step S36). At this time, once the diffraction angle 2θ is determined, the height of the beam irradiation position is determined.

[0098]

number

[0099] (How to determine the correspondence in the X and Y directions) 12(b) is a flowchart showing a method for determining the correspondence relationship of the correction amounts in the X and Y directions (corresponding to step S6 in FIG. 11). From the beam irradiation positions in the X and Y directions obtained by measurement, 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 polynomials (step S61).

[0100]

number

number

[0101] The data on the relationship between the coefficients of the polynomial obtained as an approximation and χ is fitted with the following polynomial (step S62).

[0102]

number

number

number

number

number

number

[0103] By setting arbitrary diffraction angles 2θ and χ using the obtained approximation formula, the X position and Y position at those angles can be obtained as follows. That is, formula (19) is obtained from formulas (11), (13) to (15). Furthermore, formula (20) is obtained from formulas (12), (16), (17), and (18).

[0104]

number

number

[0105] Then, the corrected X and Y positions are obtained by subtracting the deviation between the jig position and the reference position from the obtained X and Y positions. In other words, if the deviation between the jig position and the reference position is ΔX and ΔY, then equations (21) and (22) are obtained.

[0106]

number

number

[0107] (Measurement method) Using the correspondence relationship prepared or the correction amount calculated as described above, X-ray diffraction measurement can be performed while correcting and controlling the beam irradiation position. First, the user places the sample on the stage and inputs measurement conditions such as the diffraction angle and sample rotation angle. Then, the user commands the start of measurement.

[0108] The correction position in each of the X, Y, and Z directions is calculated from the diffraction angle 2θ and the sample rotation angles ω and χ set in the measurement conditions. In this case, a function or calculated correction amount is used as the correspondence relationship. Measurements are performed while moving the beam irradiation position to the correction position in each of the X, Y, and Z directions.

[0109] If the measurement is exposure and not scanning, it is sufficient to move to the corrected position before measurement. If the measurement is scanning, the XYZ position must be corrected in accordance with the movement of each sample rotation axis, so the XYZ position must be moved in accordance with the movement of each sample rotation axis. In this case, feedback control is preferable. Note that in the above example, correction is performed using multiple diffraction planes, but it is also possible to use only one diffraction plane. For example, such a method can be used in stress measurement.

[0110] [Example] (Verification of correction amount) An experiment was conducted on the above correction amount determination method. A well-used X-ray diffraction apparatus (Rigaku SmartLab) was operated at 9 kW, and a micro-optics unit was used as the incident optical system. CuKα X-rays with a beam diameter of approximately 0.5 mm were used.

[0111] To confirm the amount of deviation in the X-ray irradiation position in the X-axis and Y-axis directions, a jig was used in which Si powder and SUS were arranged in directions perpendicular to the X-axis and Y-axis directions. The scattered ray intensity was scanned along each of the X-axis and Y-axis, and the deviation in the X-ray irradiation position was confirmed from the difference in the fluorescent X-ray intensity between the Si powder and SUS.

[0112] The misalignment shown in the table below was confirmed for the micro optical system unit. This shows the difference between the center position when checking the amount of misalignment on the X and Y axes and the center position determined using the correction formula, i.e., the difference between the actual measured value and the value calculated using the correction formula. For a φ0.5mm beam, the misalignment in the X direction was less than ±0.05mm, so it was determined that the impact of this misalignment on measurement was small.

[0113] [Table 1]

[0114] Next, the beam irradiation position was aligned with the reference position, and the diffraction angle was measured for each diffraction plane by changing Z at each χ. The diffraction planes selected were (111), (220), (311), (400), (331), (422), (511), (440), (531), (620), and (533) (same below). The sample rotation angles χ were selected as 0°, 6°, 12°, 18°, 24°, 30°, 36°, 42°, 48°, 54°, and 60° (same below).

[0115] Figure 13 is a graph plotting 2θ measured for each χ and Z for the diffraction plane (111) of a Si powder sample. Such plots were made for each diffraction plane. Equation (1) was then fitted to each plot.

[0116] Using the approximate equations determined for each diffraction plane, the coefficients Aχ and Bχ were plotted by changing the sample rotation angle χ. Figures 14(a) and 14(b) are graphs plotting the coefficients Aχ and Bχ of the approximate equations against χ, respectively. Furthermore, equations (2) and (3) were fitted to the relationship between the coefficients Aχ and Bχ and χ.

[0117] Using the obtained approximation formula, Z was plotted for each χ and each θ, and equation (6) was fitted. Figure 15 is a graph plotting Z obtained using the approximation formula for each χ and each θ. Furthermore, the coefficients Dχ, Eχ, and Fχ of the obtained approximation formula were plotted for each χ. Figures 16(a) to 16(c) are graphs plotting the coefficients Dχ, Eχ, and Fχ of the approximation formula for each χ. Then, equations (7) to (9) were fitted to the relationship between the coefficients Dχ, Eχ, and Fχ and χ. In this way, an approximation formula for calculating Z for each θ and each χ was obtained.

[0118] Next, the surface height of the powder sample was adjusted to Z calculated for each θ and each χ, and the beam irradiation position in the X and Y directions was measured. X and Y were plotted for each χ and each θ, and equations (11) and (12) were fitted. Figures 17(a) and (b) are graphs plotting X obtained using the approximate equation for each θ at χ = ​​0° and 30°, respectively. Figures 18(a) and (b) are graphs plotting Y obtained using the approximate equation for each θ at χ = ​​0° and 30°, respectively.

[0119] Furthermore, the coefficients Hχ, Iχ, Jχ and Lχ, Mχ, Nχ of the obtained approximation formula were plotted for each χ. Figures 19(a) to 19(c) are graphs plotting the coefficients Hχ, Iχ, Jχ of the approximation formula for each χ. Figures 20(a) to 20(c) are graphs plotting the coefficients Lχ, Mχ, Nχ of the approximation formula for each χ. Through the above processing, the corrected positions of X, Y, and Z could be calculated using the approximation formula for each θ and each χ.

[0120] (Verification of measurements with or without correction) Using the above calculation results, X-ray diffraction measurements were performed on unstrained Si powder samples while varying χ to correct for the deviation. X-ray stress measurements were performed on the Si powder samples, and the change in the diffraction angle 2θ when χ was changed at each diffraction plane was evaluated.

[0121] In addition, X-ray stress measurement is sin 2X-ray stress measurements were performed using the ψ method (side tilt method). Figures 21 to 31 show the sin σ values ​​with and without correction for each diffraction plane of an unstrained Si powder sample. 2 This is a graph showing 2θ versus ψ. 2 In the ψ diagram, χ=ψ, and the horizontal axis of the graph coincides with χ in the case of the side tilt method.

[0122] 21 to 31, without correction, the diffraction angle 2θ changes significantly as χ increases. With correction, the change in the diffraction angle 2θ is smaller than without correction, and the value is almost constant. [Explanation of symbols]

[0123] 100 X-ray measurement system 200 X-ray Diffractometer 210 X-ray irradiation section 230 Sample stage 232 Cradle 235 Base 237 Head 238 Sample Plate 240 Goniometer 250 detectors 300 Computer (correction amount specifying device) 310 Diffraction data storage unit 320 Correspondence determination unit 330 Correction amount identification section 350 Reference position data storage unit 370 Correction amount storage unit 380 Sample position control unit 400, 500 jigs 410, 510 1st area 420, 520 2nd area R1 Incident X-ray R2 diffracted beam S0 sample

Claims

1. A correction amount specifying device that specifies a correction amount for a deviation of an X-ray irradiation position caused by a rotation of a sample relative to a measurement system, a diffraction data storage unit for storing diffraction data obtained by irradiating a standard sample, which is an assembly of isotropic and distortion-free crystal grains, with X-rays, the diffraction data being a combination of a sample rotation angle and a sample surface height with respect to the diffraction angle of the irradiated X-rays; a correspondence relationship determination unit that determines a first correspondence relationship based on the diffraction data; a correction amount specifying unit that specifies a correction amount of the sample surface height with respect to the desired sample rotation angle and the desired diffraction angle based on the first correspondence relationship.

2. 2. The correction amount specifying device according to claim 1, wherein the sample rotation angle is at least one of an angle χ around an axis perpendicular to a scattering vector and in a direction in which X-rays travel, and an angle ω around an axis perpendicular to an optical path plane.

3. 3. The correction amount specifying device according to claim 1, wherein the first correspondence relationship is a polynomial of the diffraction angle that has a polynomial of the sample rotation angle as a coefficient and represents a correction amount for the sample surface height.

4. 4. The correction amount specifying device according to claim 1, further comprising a sample position control unit that controls a relative position of the sample with respect to the desired sample rotation angle and diffraction angle using a correction amount for the sample surface height.

5. a reference position data storage unit that stores reference position data in a direction parallel to the sample surface measured using a jig that is controlled to correct a position in the height direction of the sample surface with respect to the desired sample rotation angle and the desired diffraction angle; 5. The correction amount specifying device according to claim 4, wherein the correction amount specifying section specifies the correction amount in a direction parallel to the sample surface based on the reference position data by using a second correspondence relationship.

6. 6. The correction amount specifying device according to claim 5, wherein the second correspondence relationship is a polynomial of the diffraction angle that has a polynomial of the sample rotation angle as a coefficient and represents a correction amount in a direction parallel to the sample surface.

7. A flat jig for correcting the deviation of the X-ray irradiation position caused by the rotation of the sample relative to the measurement system, a first region and a second region adjacent to each other and formed of materials having different intensities of scattered X-rays on a light receiving surface; A jig that is attached to an X-ray diffraction device so as to scan an irradiation position across the boundary between the first region and the second region and measure scattered X-ray intensity.

8. 8. The jig according to claim 7, wherein the boundary between the first region and the second region is a straight line that intersects at right angles.

9. 9. The jig according to claim 7, wherein the first region is made of stainless steel, and the second region is made of Si.

10. 10. The jig according to claim 7, wherein the second region is formed of an aggregate of crystal grains.

11. A correction amount specifying method for specifying a correction amount for a deviation of an X-ray irradiation position caused by a rotation of a sample with respect to a measurement system, comprising: A step of acquiring diffraction data obtained by irradiating a standard sample, which is an assembly of isotropic and distortion-free crystal grains, with X-rays, the diffraction data being a combination of the diffraction angle of the irradiated X-rays with respect to the sample rotation angle and the sample surface height; determining a first correspondence based on the diffraction data; and determining a correction amount for the sample surface height relative to the desired sample rotation angle and diffraction angle based on the first correspondence relationship.

12. A correction amount specification program for specifying a correction amount for a deviation of an X-ray irradiation position caused by a rotation of a sample with respect to a measurement system, A process of determining a first correspondence relationship based on diffraction data obtained by irradiating a standard sample, which is an assembly of isotropic and distortion-free crystal grains, with X-rays and which is a combination of a diffraction angle of the irradiated X-rays with respect to a sample rotation angle and a sample surface height; and specifying a correction amount for the sample surface height with respect to the desired sample rotation angle and diffraction angle based on the first correspondence relationship.

Images