An optical calibration measurement method for a hard x-ray band laboratory spectrometer

By employing an optical calibration measurement method for a laboratory spectrometer in the hard X-ray band, the problem of spectral accuracy caused by hardware processing and equipment assembly errors was solved, achieving error compensation and high-precision spectral acquisition.

CN117348055BActive Publication Date: 2026-06-05SHANGHAI INSTITUTE OF APPLIED PHYSICS CHINESE ACADEMY OF SCIENCES

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
SHANGHAI INSTITUTE OF APPLIED PHYSICS CHINESE ACADEMY OF SCIENCES
Filing Date
2023-09-18
Publication Date
2026-06-05

AI Technical Summary

Technical Problem

Existing hard X-ray band laboratory spectrometers have errors and uncertainties in hardware manufacturing and equipment assembly, which affect the accuracy of spectral acquisition.

Method used

The external structural features of key components such as the X-ray device, spherical curved crystal, and sample assembly are calibrated using optical calibration measurement methods to obtain their relative positional relationships, achieve error compensation, and ensure accurate movement of the X-ray source point, spherical curved crystal, and sample on the Rowland circle configuration.

Benefits of technology

It improves the spectral accuracy and data acquisition reliability of laboratory spectrometers, and reduces deformation or distortion problems caused by errors and uncertainties.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application provides an optical calibration measurement method for a hard X-ray band laboratory spectrometer, the laboratory spectrometer comprising an X-ray device, a detector, a first displacement table, a second displacement table, a spherical bending crystal, a sample assembly and a base, optical calibration is performed in the order of X-rays from the X-ray device, through the spherical bending crystal, to the detector, ensuring that the X-ray light source point, the spherical bending crystal and the sample always move according to a certain roll circle configuration when the laboratory spectrometer is operated, so that high-precision absorption spectrum acquisition of the sample is realized. According to the optical calibration measurement method for the hard X-ray band laboratory spectrometer provided by the application, the processing and installation errors of the laboratory spectrometer can be detected, detection means and data support are provided for subsequent compensation of the above errors, the roll circle configuration linkage accuracy is improved, the data acquisition reliability is improved, so that the requirements of the laboratory spectrometer on precision and reliability are met.
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Description

Technical Field

[0001] This invention relates to the field of X-ray absorption spectroscopy technology, and more specifically to an optical calibration measurement method for a laboratory spectrometer in the hard X-ray band. Background Technology

[0002] X-ray absorption spectroscopy is an experimental technique that has matured with the development of synchrotron radiation devices. It is one of the important methods for studying the structure of matter, and can study the local structure of atoms in the nearest neighbor under various conditions such as solid and liquid. It is widely used in many fields such as materials, biology, chemistry, environment and geology.

[0003] On December 30, 2022, the inventor's research group filed a Chinese patent application, application number ZL202211733446.6, which discloses a laboratory spectrometer that fixes an X-ray source on a base and moves a spherical curved crystal, a sample, and a detector through a motion component, so that the X-ray source, the spherical curved crystal, and the sample are always on the Rowland circle. Since the X-ray source does not need to move, the optical path is stable.

[0004] However, since measurement hardware inevitably produces certain errors and uncertainties during processing and equipment assembly, the Rowland circle configuration may also be deformed or twisted due to such errors, which will inevitably affect the spectral accuracy of the laboratory spectrometer to some extent. Summary of the Invention

[0005] The purpose of this invention is to provide an optical calibration measurement method for a laboratory spectrometer in the hard X-ray band, thereby solving the problem that the accuracy of spectral acquisition in the laboratory spectrometer is affected by errors and uncertainties in the processing and assembly of measurement hardware in the prior art.

[0006] To solve the above problems, the present invention adopts the following technical solution:

[0007] An optical calibration measurement method for a laboratory spectrometer in the hard X-ray band is provided. The laboratory spectrometer includes an X-ray device, a detector, a first displacement stage, a second displacement stage, a spherical curved crystal, a sample assembly, and a base. The optical calibration measurement method includes the following steps in sequence: S1, calibrating the position of the source point of the X-ray device; S2, calibrating the installation angle and orientation of the X-ray device; S3, calibrating the first included angle and the intersection position between the axes of the first and second displacement stages; S4, calibrating the geometric center of the spherical curved crystal; S5, calibrating the spherical curved crystal... The pitch position and the height reference position of the spherical curved crystal are calibrated; S6, the center height and position of the detector and sample assembly are calibrated; by calibrating the external structural features of the above key components or the relevant feature surfaces of their mounting structures, the position information of the key components is obtained indirectly and accurately through the conversion of relative positional relationships, thereby achieving the calibration of the key components; through the sequential completion of the above steps S1-S6, it is ensured that when the laboratory spectrometer is running, the X-ray source point, the spherical curved crystal, and the sample always move according to a certain Rowland circle configuration, thereby achieving high-precision absorption spectrum acquisition of the sample.

[0008] Step S1 includes: using an optical measuring arm to construct and fit a first plane on the side of the X-ray device, displacing it a certain distance inward along the first direction to reach the light source point, thus constructing a second plane; using the optical measuring arm to construct and fit a third plane on the back of the X-ray device, displacing it a certain distance inward along the second direction to reach the light source point, thus constructing a fourth plane; using the optical measuring arm to construct and fit a fifth plane on the top surface of the X-ray device, and a sixth plane on the bottom surface, displacing it a certain distance inward along the third direction to reach the light source point, thus constructing a seventh plane between the fifth and sixth planes; finally, intersecting the constructed second, fourth, and seventh planes at a point to obtain a first point, which is the X-ray light source point of the X-ray device.

[0009] Step S2 includes: using the back plate of the first displacement stage as the eighth plane, calibrating the angle between the third plane of the X-ray device and the eighth plane, which is equal to the angle between the X-ray emitted by the X-ray device and the first plane of the X-ray device, thereby calibrating the installation angle of the X-ray device; measuring the horizontal relationship between the fifth and sixth planes of the X-ray device and the ninth plane of the upper surface of the base, thereby ensuring that the X-ray device and the ninth plane of the base are in a parallel position, thereby calibrating the installation posture of the X-ray device.

[0010] Step S3 includes: continuously moving the first displacement stage along the guide rail direction, determining the fifth direction through fitting; then, taking the center plane of the tenth and eleventh planes along the fourth direction through the guide rails on both sides of the first displacement stage and the tenth and eleventh planes inside the guide rails as the twelfth plane, and defining the position of the twelfth plane in the fifth direction as the axis of the first displacement stage; continuously moving the second displacement stage along the guide rail direction, determining the sixth direction through fitting; then, taking the thirteenth and fourteenth planes along the sixth direction through the guide rails on both sides of the second displacement stage and the thirteenth and fourteenth planes inside the guide rails as the fifteenth plane, and defining the position of the fifteenth plane in the seventh direction as the axis of the second displacement stage; extending the axis of the first displacement stage and the axis of the second displacement stage to intersect at the second point, and obtaining the first included angle between the two axes to determine the installation angle and intersection point of the two axes.

[0011] Step S4 includes: taking multiple points along the cylindrical surface inside the crystal mounting base of the spherical curved crystal, fitting the first cylindrical surface inside the crystal mounting base, and fitting its central axis one based on the first cylindrical surface; the sixteenth plane of the front end face of the crystal mounting base is displaced a certain distance into the spherical curved crystal along the ninth direction, the distance value being related to the structure of the spherical curved crystal and the crystal mounting base, to obtain the seventeenth plane, the seventeenth plane intersecting the axis of the spherical curved crystal at the third point, which is the crystal geometric center of the spherical curved crystal.

[0012] Step S5 includes: calibrating the relative position of the ninth plane of the base and the sixteenth plane of the front end face of the crystal mounting base, gradually adjusting the pitch position of the spherical curved crystal so that the ninth plane and the sixteenth plane are perpendicular to each other, and recording the distance between the positive and negative limits of the motor controlling the pitch position of the spherical curved crystal and its direction of movement, and calibrating the pitch position and the height reference position of the spherical curved crystal.

[0013] Step S5 also includes: comparing whether the first point and the third point are at the same height in the third direction. If they are at the same height in the third direction, it means that the height of the geometric center of the spherical curved crystal is consistent with the height of the X-ray device light source point, and recording the readings of the relevant motors and their distances relative to the positive and negative limits in their respective directions of motion; when the motion axis is at the reference point position in its direction of motion, calibrating the Bragg angle position of the spherical curved crystal, calibrating the relative positions of the eighth plane and the sixteenth plane, and obtaining their deviation angle. This angle value is related to the overall physical design of the equipment and the reference position of the motion axis.

[0014] Step S6 includes: taking multiple points on the cylindrical surface of the detector front end, fitting a second cylindrical surface of the cylindrical surface of the detector front end, and fitting a second central axis based on the second cylindrical surface. The position of the second central axis in the third direction is the center height of the sample; taking multiple points on the rectangular front end surface of the detector, constructing an eighteenth plane, and displacing it a certain distance in the direction of the cylinder of the detector front end to obtain the nineteenth plane on the surface of the sample component. The nineteenth plane intersects the fitted axis at the fourth point, which is the center of the sample.

[0015] It should be understood that the specific value of the displacement distance mentioned in steps S1-S6 above depends on the physical structure of the laboratory spectrometer.

[0016] This invention improves the spectral acquisition accuracy of a laboratory spectrometer by performing optical calibration to achieve error compensation. The error compensation methods include: 1) adjusting the device position in real time through the above optical calibration to make it as close as possible to the theoretical design position; or 2) recording the calibrated deviation distance and angle, and then adding them to the calculation of the Rowland circle configuration linkage scanning relationship, and adding compensation values ​​based on the calibration values.

[0017] As mentioned in the background section of this invention, measurement hardware inevitably generates certain errors and uncertainties during processing and equipment assembly. The Rowland circle configuration, due to these errors, will also experience deformation or distortion, thus inevitably affecting the spectral accuracy of the laboratory spectrometer to some extent. However, since the X-ray source is located inside the radiation device, direct measurement is not possible, and the spherical curved crystal surface is not suitable for direct contact measurement. Similarly, the sample is fragile and cannot be directly calibrated.

[0018] Therefore, this invention calibrates the key components by indirectly and accurately obtaining their positional information through the conversion of relative positional relationships by calibrating the external structural features of the aforementioned key components or the relevant feature surfaces of their mounting structures. This invention is primarily used to detect and measure errors and uncertainties introduced during the hardware processing and equipment assembly of laboratory spectrometers. By employing the optical calibration measurement method used in this invention, the spectral acquisition accuracy of the laboratory spectrometer can be improved through error compensation or error reduction.

[0019] The key inventive point of this invention lies in reducing the processing and assembly errors of each structural component by calibrating the relative positions and orientations of key components (X-ray source point, geometric center of the spherical curved crystal, and sample center) along the propagation path of the X-rays in the laboratory spectrometer, based on the propagation path of the X-rays. This ensures the accuracy of the optical path propagation throughout the entire process, thereby improving the spectral acquisition accuracy. However, no prior art has ever disclosed such a calibration method for the entire energy scanning mechanism; therefore, this invention possesses outstanding substantive features and significant progress.

[0020] In summary, the optical calibration measurement method for a hard X-ray band laboratory spectrometer provided by the present invention can detect the processing and installation errors of the laboratory spectrometer, and provide detection means and data support for subsequent compensation of the above errors, improve the accuracy of the Rowland circle configuration linkage, enhance the reliability of data acquisition, and thus meet the accuracy and reliability requirements of the laboratory spectrometer. Attached Figure Description

[0021] Figure 1 A schematic diagram of the principle of a Rowland circle configuration for a laboratory spectrometer in the hard X-ray band;

[0022] Figure 2 This is a schematic diagram of the structure of an X-ray laboratory spectrometer calibrated using the method described in this invention;

[0023] Figure 3 This is a schematic diagram for calibrating the position of the X-ray source point of the X-ray device 100;

[0024] Figure 4 This is a schematic diagram for calibrating the installation angle and orientation of the X-ray device 100;

[0025] Figure 5 This is a schematic diagram for calibrating the included angle 1 between the axis 301 of the first displacement stage 300 and the axis 401 of the second displacement stage 400, as well as their intersection position.

[0026] Figure 6 This is a schematic diagram for calibrating the geometric center of a 500-degree spherical bent crystal.

[0027] Figure 7 This is a schematic diagram for calibrating the pitch position and height reference position of the spherical curved crystal 500.

[0028] Figure 8 This is a schematic diagram for calibrating the center height and position of the detector and sample assembly. Detailed Implementation

[0029] The present invention will be further described below with reference to specific embodiments. It should be understood that the following embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Unless otherwise specified, the techniques used in the embodiments are conventional practices in the art, or experimental methods recommended by the instrument manufacturer. Unless otherwise specified, the reagents and materials used in the embodiments are commercially available.

[0030] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," and "counterclockwise," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0031] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.

[0032] According to the present invention, an optical calibration measurement method for a laboratory spectrometer in the hard X-ray band is provided, wherein the calibration object is a laboratory spectrometer disclosed in patent ZL202211733446.6. It should be understood that the physical basis of this laboratory spectrometer is as follows: A spherical bent crystal with a radius of curvature of 500 mm (this radius of curvature is merely an example and not a limitation) is used as the analytical crystal; therefore, the corresponding Rowland circle diameter is 500 mm. The principle of this Rowland circle configuration is as follows... Figure 1 As shown, the incident beam emitted by the X-ray device is monochromated by a spherical curved crystal and transmitted onto the sample, where it is received by a subsequent detector. The angle between the incident beam and the normal to the crystal surface is the Bragg angle; changing this angle alters the energy used for scanning. Because the XRD-type X-ray device used in this invention is relatively heavy (approximately 55 kg), its position is fixed (i.e., the position of the light source point is fixed) to ensure good positional stability of the optical path during energy scanning.

[0033] like Figure 2As shown, the X-ray absorption spectrometer includes: an X-ray device 100, a detector 200, a electrically powered precision-assembled first displacement stage 300 and second displacement stage 400, a spherical curved crystal 500, a sample assembly 600, and a base 700. The X-ray device 100, the first displacement stage 300, and the second displacement stage 400 are all fixed to the base 700. The spherical curved crystal 500 is fixed to the first displacement stage 300. The first displacement stage 300 faces the light source of the X-ray source of the X-ray device 100, i.e., the first displacement stage 300 is along the direction of the incident beam. The second displacement stage 400 is set at an angle to the first displacement stage 300, the angle being 40° to 70°. The detector 200 and the sample assembly 600 are respectively fixed to the second displacement stage 400. The combination of the first displacement stage 300 and the second displacement stage 400 allows the spherical curved crystal 500, the sample assembly 600, and the detector 200 to move simultaneously, so that the X-ray source, the spherical curved crystal 500, and the sample are always located on the Rowland circle with a diameter equal to the radius of curvature of the spherical curved crystal. The incident beam emitted by the X-ray source is monochromated by the spherical curved crystal 500 and transmitted to the sample and received by the detector 200.

[0034] According to the optical calibration measurement method provided by this invention, the main calibration process involves precisely positioning and confirming the attitude of the three key components (X-ray device 100, detector 200, and spherical curved crystal 500) in the Rowland circle configuration linkage, thereby ensuring that the constructed dynamic Rowland circle will not deform or twist during the operation of the linkage scanning mechanism. The selection of the calibration sequence is based on the X-ray propagation path, performing optical calibration according to the order in which the X-rays travel from the X-ray device 100 through the spherical curved crystal 500 and then to the detector 200. This ensures the consistency and accuracy of the calibration results.

[0035] Step S1: As Figure 3As shown, the position of the X-ray source point of the X-ray device 100 is calibrated. First, using an optical measuring arm, multiple points are taken on one side of the X-ray device 100 to construct a fitted plane 1. Using the same method, plane 3 (located at the rear), plane 5 (located at the top), and plane 6 (located at the bottom) are constructed and fitted. Using plane 1 of the X-ray device 100, a certain distance is displaced along direction 1 into the interior of the X-ray device 100, and this plane is defined as plane 2. It should be understood that this distance value is related to the internal structure of the X-ray device, and the specific displacement amount depends on the distance between the outer surface and the source point in the drawings of the X-ray device provided by the X-ray device manufacturer. Next, using plane 3 of the X-ray device 100, a certain distance is displaced along direction 2 into the interior of the X-ray device 100, and this plane is defined as plane 4. Using planes 5 and 6 of the X-ray device 100, a plane is constructed by taking the center position of the two planes along direction 3 into the interior of the X-ray device 100, and this plane is defined as plane 7. Whether to construct a plane by taking the center position of the upper and lower planes of the X-ray device in direction 3 needs to be determined based on the internal structure of the X-ray device. Finally, the three constructed planes 2, 4 and 7 intersect at a point to obtain point 1, which is the light source point of the X-ray device 100.

[0036] Step S2: As Figure 4 As shown, the installation angle and orientation of the X-ray device 100 are calibrated. It should be understood that, considering the overall design of the equipment, in order to better focus X-rays onto the spherical curved crystal, and to make the installation structure of the absorption spectrometer more compact and save installation space, the X-ray device 100 usually needs to be deflected at a certain angle during installation. Therefore, the angle formed between the X-rays emitted by the X-ray device 100 and plane 3 of the X-ray device 100 is not a right angle, but may be other angle values. The specific deflection value is related to the internal structure of the X-ray device. Specifically, the calibration method uses the back plate 320 of the first displacement stage 300 as plane 8, calibrating whether the angle between plane 3 and plane 8 is equal to the angle between the X-rays emitted by the X-ray device 100 and plane 1 of the X-ray device 100. To ensure the rigor of the calibrated offset angle, it can be verified by whether the X-rays emitted by the X-ray device 100 are perpendicular to the back plate 320 of the first displacement stage 300. It should be understood that the backplate 320 is located behind the first displacement stage 300. During energy scanning, the crystal's geometric center moves in a direction perpendicular to the backplate 320; therefore, it is necessary to ensure that the center of the X-ray cone is parallel to this axis. Furthermore, the horizontal relationship between planes 5 and 6 of the X-ray device 100 and the upper surface of the base 700, i.e., plane 9, is measured to ensure that the X-ray device 100 and plane 9 of the base 700 are in a parallel position.

[0037] Step S3: As Figure 5 As shown (the X-ray device 100 is hidden in the figure for ease of observation), the angle 1 between the axis 301 of the first displacement stage 300 and the axis 401 of the second displacement stage 400, as well as their intersection position, are calibrated. First, by continuously moving the first displacement stage 300 along the guide rail direction, the positions of the two threaded holes 302 and 303 on the support block 310 are calibrated multiple times. Through fitting, the points taken multiple times on the threaded holes 302 and 303 are fitted into a straight line, which is defined as direction 5. Then, through the inner surfaces of the guide rails 321 and 322 on both sides of the first displacement stage 300, i.e., planes 10 and 11, the center plane of planes 10 and 11 is taken along direction 4 as plane 12. However, it should be understood that this method of taking the plane is related to the internal structure of the displacement stage. Not all displacement stages have their motion axes in the center position; there are cases where the displacement stages are off-axis. The central axis displacement stage used here takes the center position plane between planes 10 and 11 as plane 12. The position of plane 12 in direction 5 is defined as axis 301 of the first displacement stage 300. Through continuous movement of the second displacement stage 400 along the guide rail direction, the positions of the two threaded holes 402 and 403 on the support block 410 are repeatedly calibrated. A straight line is fitted to the points taken multiple times at threaded holes 402 and 403, and this straight line is defined as direction 7. Then, through the inner surfaces of the guide rails 421 and 422 on both sides of the second displacement stage 400, i.e., planes 13 and 14, the center plane of planes 13 and 14 is taken along direction 6 as plane 15. This plane selection method is related to the internal structure of the displacement stage. The position of plane 15 in direction 7 is defined as axis 401 of the second displacement stage 400. The straight line containing axis 301 and axis 401 is extended and intersects at a point. The included angle 1 between axis 301 and axis 401 is obtained to determine the installation angle of the two axes and the intersection point, point 2. The design value of this installation angle is related to the overall physical design of the equipment.

[0038] Step S4: As Figure 6As shown, the geometric center of the spherical bent crystal 500 is calibrated. Multiple points are taken along the cylindrical surface inside the crystal mount 510 of the spherical bent crystal 500 to fit the inner cylindrical surface 1 of the crystal mount 510. The central axis 1 of the cylindrical surface 1 is then fitted and identified as the axis 501 of the spherical bent crystal 500. The front end face plane 16 of the crystal mount 510 is displaced a certain distance inward along direction 9 into the spherical bent crystal 500; this plane is defined as plane 17. It should be understood that this distance is related to the structure of the spherical bent crystal and the crystal mount. The spherical bent crystal has a certain depth, and the front end face is a certain distance from the geometric center of the spherical bent crystal. This distance is determined by the processing of the spherical bent crystal. Simultaneously, the crystal mount also has a certain thickness, which is also determined by the processing conditions. Plane 17 intersects the axis 501 of the spherical bent crystal 500 at point 3, which is the geometric center of the spherical bent crystal 500.

[0039] Step S5: As Figure 7 As shown (the X-ray device 100 is hidden in the figure for ease of observation), the pitch position and height reference position of the spherical curved crystal 500 are calibrated. The relative positions of plane 9 and plane 16 are calibrated, and the pitch position of the spherical curved crystal 500 is gradually adjusted until plane 9 and plane 16 are perpendicular to each other. The distance between the motor 520 controlling the pitch position of the spherical curved crystal 500 and its positive and negative limits in the direction of movement is recorded.

[0040] Comparison point 1 ( Figure 3 (middle) and point 3 ( Figure 6 (middle) Whether they are at the same height position in direction 3. If they are at the same position in direction 3, it means that the height of the geometric center of the spherical curved crystal 500 is consistent with the height of the light source point of the X-ray device 100. Record the reading of the relevant motor and its distance relative to the positive and negative limits in their respective directions of motion.

[0041] When the motion axis 530 is at the reference point position in its motion direction, the Bragg angle position of the spherical bent crystal 500 is calibrated. The relative positions of plane 8 and plane 16 are calibrated to obtain their deviation angle. This angle value is related to the overall physical design of the equipment and the reference position of the motion axis 530.

[0042] Step S6: As Figure 8As shown, the center height and position of the detector and sample assembly are calibrated. Multiple points are taken on the cylindrical surface of the front end of detector 200 to fit the cylindrical surface 2 of detector 200. The central axis 2, i.e., axis 201, is then fitted using cylindrical surface 2. The position of axis 201 in direction 3 yields the center height of the sample. Multiple points are taken on the rectangular front end surface of detector 200 to construct plane 18. A certain distance is displaced towards the cylindrical front end of detector 200 to obtain plane 19 where the sample assembly 600 is located (this distance is related to the overall physical design of the device). Plane 19 intersects the fitted axis 201 at point 4, which is the sample center, and the coordinates of the sample center can be obtained. It should be understood that this translation distance depends on the actual physical structure of the device. The configuration of this device is designed to ensure that the sample center is on a Rowland circle, with the detector positioned behind the sample to receive X-rays. Therefore, there is a certain physical distance between plane 18 and the plane where the sample center is located. This physical distance is the offset distance described in the text.

[0043] The above describes a novel optical calibration method for a laboratory spectrometer in the hard X-ray band. This method aims to measure the errors and uncertainties generated during hardware processing and equipment assembly, providing detection methods and data support for addressing deformation or distortion of the Rowland circle configuration caused by such errors. The optical calibration technology employed in this invention can accurately assess the aforementioned errors and uncertainties, thereby achieving error compensation. Specifically, error compensation is achieved through: 1) real-time fine-tuning of the equipment position through calibration to bring it as close as possible to the theoretically designed position; 2) recording the calibrated deviation distance and angle, and then incorporating these values ​​into the calculation of the Rowland circle configuration's linkage scanning relationship. Using trigonometric functions and other methods, compensation values ​​(based on the calibration values) are added to improve the spectral accuracy of the laboratory spectrometer.

[0044] The above description is merely a preferred embodiment of the present invention and is not intended to limit the scope of the invention. Various variations can be made to the above embodiments of the present invention. That is, all simple and equivalent changes and modifications made based on the claims and description of this invention fall within the protection scope of the claims of this patent. All aspects not described in detail in this invention are conventional technical content.

Claims

1. An optical calibration measurement method for a laboratory spectrometer in the hard X-ray band, the laboratory spectrometer comprising: An X-ray apparatus (100), a detector (200), a first displacement stage (300), a second displacement stage (400), a spherical curved crystal (500), a sample assembly (600), and a base (700) are characterized in that the optical calibration measurement method sequentially includes the following steps: S1, calibrate the position of the light source point of the X-ray device (100); S2, calibrate the installation angle and orientation of the X-ray device (100); S3, calibrate the first included angle and the intersection position between the axis (301) of the first displacement stage (300) and the axis (401) of the second displacement stage (400); S4, calibrate the geometric center of the spherical curved crystal (500); S5, calibrate the pitch position of the spherical curved crystal (500) and the height reference position of the spherical curved crystal (500); S6, calibrate the center height and position of the detector (200) and sample assembly (600); By calibrating the external structural features of the aforementioned key components or the relevant feature surfaces of their mounting structures, and through the conversion of relative positional relationships, the positional information of the key components can be obtained indirectly and accurately, thereby achieving the calibration of the key components. By completing the above steps S1-S6 in sequence, it is ensured that the X-ray source point, the spherical curved crystal, and the sample always move according to a certain Rowland circle configuration when the laboratory spectrometer is running, thereby achieving high-precision absorption spectrum acquisition of the sample.

2. The optical calibration measurement method according to claim 1, characterized in that, Step S1 includes: using an optical measuring arm to construct and fit a first plane on the side of the X-ray device (100), displacing it a certain distance into the X-ray device (100) along the first direction to reach the light source point, and constructing a second plane; using an optical measuring arm to construct and fit a third plane on the back of the X-ray device (100), displacing it a certain distance into the X-ray device (100) along the second direction to reach the light source point, and constructing a fourth plane; using an optical measuring arm to construct and fit a fifth plane on the top surface of the X-ray device (100), construct and fit a sixth plane on the bottom surface, displacing it a certain distance into the X-ray device (100) along the third direction, and constructing a seventh plane between the fifth and sixth planes; finally, intersecting the constructed second, fourth, and seventh planes at a point to obtain a first point, which is the X-ray light source point of the X-ray device (100).

3. The optical calibration measurement method according to claim 2, characterized in that, Step S2 includes: taking the back plate (320) of the first displacement stage (300) as the eighth plane, calibrating the angle between the third plane of the X-ray device (100) and the eighth plane, which is equal to the angle between the X-ray emitted by the X-ray device (100) and the first plane of the X-ray device (100), thereby calibrating the installation angle of the X-ray device (100); The horizontal relationship between the fifth and sixth planes of the X-ray device (100) and the ninth plane of the upper surface of the base (700) is measured to ensure that the X-ray device (100) and the ninth plane of the base (700) are in a parallel position, thereby calibrating the installation posture of the X-ray device (100).

4. The optical calibration measurement method according to claim 3, characterized in that, Step S3 includes: by continuously moving the first displacement stage (300) along the guide rail direction, the fifth direction is determined by fitting; then, by taking the tenth plane and the eleventh plane on the inner side of the guide rails (321) and the guide rails (322) on both sides of the first displacement stage (300), the center plane of the tenth plane and the eleventh plane along the fourth direction is taken as the twelfth plane, and the position of the twelfth plane in the fifth direction is defined as the axis (301) where the first displacement stage (300) is located. By continuously moving the second displacement stage (400) along the guide rail direction, the sixth direction is determined by fitting. Then, by using the thirteenth and fourteenth planes inside the guide rails (421) and guide rails (422) on both sides of the second displacement stage (400), the fifteenth plane is determined between the thirteenth and fourteenth planes along the sixth direction. The position of the fifteenth plane in the seventh direction is defined as the axis (401) where the second displacement stage (400) is located. The axis (301) where the first displacement stage (300) is located and the axis (401) where the second displacement stage (400) is located are extended to intersect at the second point, and the first included angle between the two axes is obtained to determine the installation angle and intersection point of the two axes.

5. The optical calibration measurement method according to claim 4, characterized in that, Step S4 includes: taking multiple points along the inner cylindrical surface of the crystal mounting base (510) of the spherical curved crystal (500), fitting the first cylindrical surface along the inner edge of the crystal mounting base (510), and fitting its central axis (501) based on the first cylindrical surface; the sixteenth plane of the front end face of the crystal mounting base (510) is displaced a certain distance into the spherical curved crystal 500 along the ninth direction. This distance value is related to the structure of the spherical curved crystal and the crystal mounting base to obtain the seventeenth plane. The seventeenth plane intersects the central axis (501) of the spherical curved crystal (500) at the third point, which is the crystal geometric center of the spherical curved crystal (500).

6. The optical calibration measurement method according to claim 5, characterized in that, Step S5 includes: calibrating the relative position of the ninth plane of the base (700) and the sixteenth plane of the front end face of the crystal mounting base (510), gradually adjusting the pitch position of the spherical curved crystal (500) so that the ninth plane and the sixteenth plane are perpendicular to each other, and recording the distance between the positive and negative limits of the motor (520) controlling the pitch position of the spherical curved crystal (500) relative to its direction of movement, and calibrating the pitch position of the spherical curved crystal (500) and the height reference position of the spherical curved crystal (500).

7. The optical calibration measurement method according to claim 6, characterized in that, Step S5 also includes: comparing whether the first point and the third point are at the same height in the third direction. If they are at the same height in the third direction, it means that the height of the geometric center of the spherical curved crystal 500 is consistent with the height of the light source point of the X-ray device 100. Record the reading of the relevant motor and its distance relative to the positive and negative limits in their respective directions of motion. When the motion axis (530) is at the reference point position in its direction of motion, calibrate the Bragg angle position of the spherical curved crystal (500), calibrate the relative position of the eighth plane and the sixteenth plane, and obtain its deviation angle. This angle value is related to the overall physical design of the equipment and the reference position of the motion axis 530.

8. The optical calibration measurement method according to claim 7, characterized in that, Step S6 includes: taking multiple points on the cylindrical surface of the front end of the detector (200), fitting the second cylindrical surface of the cylindrical surface of the front end of the detector (200), and fitting its central axis II (201) based on the second cylindrical surface. The position of the central axis II (201) in the third direction is the center height of the sample; taking multiple points on the rectangular front end surface of the detector (200), constructing the eighteenth plane, and displacing it a certain distance in the direction of the cylinder of the front end of the detector (200) to obtain the nineteenth plane on the surface of the sample component (600). The nineteenth plane intersects the fitted central axis II (201) at the fourth point, which is the center of the sample.

9. The optical calibration measurement method according to claim 8, characterized in that, The specific value of the displacement distance depends on the physical structure of the laboratory spectrometer.

10. The optical calibration measurement method according to claim 9, characterized in that, By performing optical calibration on the laboratory spectrometer, error compensation can be achieved, thereby improving the spectral acquisition accuracy of the laboratory spectrometer. The error compensation methods include: 1) fine-tuning the position of the equipment in real time through the above optical calibration to make it as close as possible to the theoretical design position; or 2) recording the calibrated deviation distance and angle, and then adding them to the calculation of the Rowland circle configuration linkage scanning relationship, and adding compensation values ​​based on the calibration values.