Wavelength dispersive X-ray absorption spectrometer
By employing an eccentric layout and vacuum design in a wavelength dispersive X-ray absorption spectrometer, the problems of long acquisition time and low signal-to-noise ratio in existing technologies have been solved, achieving efficient low-energy spectrum acquisition and simplifying the system structure.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- GUOCHUANG SCIENCE INSTRUMENTS (SUZHOU) CO LTD
- Filing Date
- 2026-04-23
- Publication Date
- 2026-06-30
AI Technical Summary
Existing laboratory X-ray absorption spectrometers are inefficient in acquiring absorption spectra, have insufficient signal-to-noise ratios, and suffer from air scattering and absorption that affect spectral quality, especially in the low-energy band.
A wavelength dispersive X-ray absorption spectrometer is used. Through the design of an eccentrically arranged cylindrical bent crystal and a surface detector, combined with a vacuum environment, a complete spectrum can be obtained in a single acquisition, simplifying the system structure and eliminating the scattering and stray absorption of X-rays by air.
It greatly shortens the spectrum acquisition time, improves experimental efficiency, enhances the signal-to-noise ratio, and extends the working energy range of the spectrometer to the low-energy band.
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Figure CN122306849A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of laboratory spectrometer technology, and more particularly to a wavelength dispersive X-ray absorption spectrometer. Background Technology
[0002] X-ray absorption spectroscopy (XAFS) is a powerful analytical technique that can provide information on the nearest-neighbor local structure of specific elements in materials, such as the type, valence state, bond length, and coordination number of coordinating elements. Currently, most commercially available laboratory X-ray absorption spectrometers are based on the Rowland circle imaging principle. These spectrometers typically employ a point-by-point integration scanning mode when acquiring absorption spectra. Specifically, they need to scan point by point in different energy ranges of the target spectrum with different step sizes and acquisition times, ultimately stitching together a complete absorption spectrum.
[0003] However, this point-by-point scanning mode has inherent drawbacks. To obtain a spectrum with a good signal-to-noise ratio, it is usually necessary to perform signal integration for a long time at each energy point, resulting in a lengthy acquisition time for the entire spectrum and low experimental efficiency. In addition, the components in the air have a significant scattering and absorption effect on X-rays, especially in the low-energy band, which further degrades the signal-to-noise ratio of the spectrum and limits the lower limit of the energy that the spectrometer can measure. Summary of the Invention
[0004] The main objective of this invention is to provide a wavelength dispersive X-ray absorption spectrometer to reduce spectrum acquisition time and improve experimental efficiency, thereby overcoming the shortcomings of existing technologies.
[0005] To achieve the above-mentioned objectives, the present invention provides the following technical solution.
[0006] Some embodiments of the present invention provide a wavelength dispersive X-ray absorption spectrometer, including a light source unit, a vacuum acquisition unit, a surface detector water-cooling unit and a support structure, and further including a wavelength dispersive mechanism; The light source unit includes a jet pump, a three-axis manual displacement stage assembly disposed on one side of the jet pump, a support assembly disposed above the three-axis manual displacement stage assembly, a liquid target X-ray source disposed on top of the support assembly, and a sample chamber assembly disposed on one side of the liquid target X-ray source; the sample chamber assembly includes a shutter assembly, a beam-limiting aperture mounting plate, a sample chamber body, a sample slot, a bellows, and a clamp, the sample slot being used to hold a sample, and a sample chamber cover being disposed on top of the sample chamber body; The wavelength dispersion mechanism is set inside the vacuum cavity and includes a spliced base plate, a first linear module, a cylindrical bent crystal support adjustment assembly, a surface detector support adjustment assembly, and a second linear module. The vacuum acquisition unit is used to generate a vacuum environment within the vacuum chamber.
[0007] In one embodiment, the splicing base plate includes a second base plate, a first base plate disposed on one side of the second base plate, a third base plate disposed on the other side of the second base plate, and connecting plates disposed on both sides of the top of the second base plate; one side of each connecting plate contacts the top of the first base plate and the third base plate respectively; positioning pins are provided at the overlapping contact positions of the connecting plates and the first, second, and third base plates, and second screws are disposed in the positioning pins; first lifting rings are provided at the four corners of the top of the first, second, and third base plates; adjusting bolts are provided at both ends and both sides of the top of the first, second, and third base plates; the splicing base plate has two opposing sides, and the first linear module and the second linear module are respectively mounted on the two sides.
[0008] In one embodiment, the cylindrical bending crystal support adjustment assembly includes a micron head assembly mounting plate, micron head mounting blocks disposed on both sides of the top of the micron head assembly mounting plate, a micron head disposed on one side of the micron head mounting block, a turntable assembly fixing plate disposed on the top of the micron head assembly mounting plate, a first electric turntable disposed on the top of the turntable assembly fixing plate, and a crystal assembly turntable adapter disposed above the first electric turntable.
[0009] In one embodiment, the crystal assembly turntable adapter includes a mounting plate disposed on the top of the first electric turntable, a cylinder disposed on the top of the mounting plate, and a disk disposed on the top of the cylinder. The top of the disk is provided with a first electric arc swing stage, the first electric arc swing stage is provided with a magnetic seat mounting block, and a cylindrical bent crystal mounting assembly is provided above the magnetic seat mounting block.
[0010] In one embodiment, the cylindrical bent crystal mounting assembly includes an I-shaped bracket disposed above the magnetic base mounting block, a thin cylindrical bent crystal disposed on one side of the I-shaped bracket, a third screw disposed on the top of the I-shaped bracket, a mounting steel plate disposed on the bottom of the I-shaped bracket, a positioning round hole disposed on one end of the bottom side of the I-shaped bracket, a positioning waist hole disposed on the other end of the bottom side of the I-shaped bracket, and a knob-type magnetic suction seat disposed on the magnetic base mounting block; the first linear module includes a first motion platform, and the micro-head assembly mounting plate is disposed on the first motion platform; the top of the magnetic base mounting block is provided with a first positioning pin and a second positioning pin, which are adapted to the positioning round hole and the positioning waist hole; the first motion platform is provided with a third positioning pin and a fourth screw, which are used to position and install the cylindrical bent crystal support adjustment assembly on the first motion platform.
[0011] In one embodiment, the second linear module is provided with a second motion table, and a surface detector support and adjustment assembly is installed on the second motion table. The surface detector support and adjustment assembly includes an electric linear stage, and multiple sets of fifth screws are provided on the electric linear stage. The bottom ends of the fifth screws extend into the second motion table. A fourth base plate is provided above the electric linear stage, and a bracket is provided above the fourth base plate. The bracket includes a mounting base plate disposed on the top of the fourth base plate, side plates disposed on both sides of the top of the mounting base plate, a mounting top plate disposed on the top of the side plates, a second electric turntable disposed on the top of the mounting top plate, a middle plate disposed on the second electric turntable, a second electric arc swing table disposed on the top of the middle plate, a raised plate disposed on the top of the second electric arc swing table, and a surface detector disposed on the top of the raised plate.
[0012] In one embodiment, the support structure includes a first support component, a second support component, and a third support component; the bottoms of the first support component, the second support component, and the third support component are all composed of the same first aluminum profile frame structure; casters are provided at the bottom of the first aluminum profile frame structure, and a first aluminum plate is provided at the top of the first aluminum profile frame structure; a fourth support component is provided at one end of the first support component, and the fourth support component is composed of a second aluminum profile frame structure; a second welded sheet metal part is provided at the bottom of the surface of the second aluminum profile frame structure, and a second aluminum plate is provided at the top of the second aluminum profile frame structure; The first aluminum profile frame structure has a first end face sheet metal on both sides and a first side sheet metal on both ends. The second aluminum profile frame structure has a second end face sheet metal on both sides and a second side sheet metal on both ends.
[0013] In one embodiment, the sample chamber assembly is provided with a beryllium window welding flange.
[0014] In one embodiment, a first screw is provided on the sample slot for fixing the sample inside the sample slot.
[0015] In one embodiment, the sample chamber cover and the sample chamber body are magnetically fixed together.
[0016] In one embodiment, the vacuum cavity includes a first cylindrical cavity, a second cylindrical cavity, and a third cylindrical cavity; each of the first cylindrical cavity, the second cylindrical cavity, and the third cylindrical cavity is provided with a U-shaped support; a second lifting ring is installed on the top of each of the first cylindrical cavity, the second cylindrical cavity, and the third cylindrical cavity; circular side doors are installed on both sides of each of the first cylindrical cavity, the second cylindrical cavity, and the third cylindrical cavity, and an observation window is provided in the middle of each circular side door.
[0017] In one embodiment, a circular end door is installed at one end of the third cylindrical cavity, and a central observation window is provided at the middle position of the circular end door. A circular side plate is installed at one end of the first cylindrical cavity, and a functional feedthrough flange assembly is provided on the circular side plate. A first elongated mounting plate is installed on both sides inside the first cylindrical cavity. A second elongated mounting plate is installed on both sides inside the second cylindrical cavity. A third elongated mounting plate is installed on both sides inside the third cylindrical cavity. The wavelength dispersion mechanism is installed on the first elongated mounting plate, the second elongated mounting plate, and the third elongated mounting plate.
[0018] In one embodiment, the vacuum acquisition unit includes a multi-stage Roots pump assembly, the top of which is connected to a hydraulic bellows, and the hydraulic bellows is equipped with a manual angle valve, a venting valve, and a Pirani gauge.
[0019] In one embodiment, a cylindrical locating pin is mounted on the first elongated mounting plate, and rectangular blocks are mounted on the second and third elongated mounting plates, with set screws mounted on the rectangular blocks.
[0020] In one embodiment, a tricolor tower light is provided on the top of the first cylindrical cavity.
[0021] Compared with the prior art, the present invention has at least the following beneficial effects: (1) This invention abandons the existing point-by-point scanning mode and adopts the wavelength dispersion principle. Through a carefully designed eccentric layout, namely, the cylindrical curved crystal and the surface detector are both installed eccentrically and the surface detector always receives the emitted X-rays perpendicularly, the entire energy bandwidth corresponding to the near edge and the extended edge of the measured element is simultaneously presented on the surface detector. This process does not require changing the crystal or switching the optical path. A complete absorption spectrum can be obtained in one acquisition, which greatly shortens the spectrum acquisition time. Compared with the existing technology, the experimental efficiency is revolutionaryly improved.
[0022] (2) Since the present invention can cover the near edge and the extended edge with a single data acquisition, it does not require the use of complex dual crystals, dual detectors and high-precision electric displacement stages required for switching optical paths. Thus, while improving performance, the system structure is greatly simplified and the manufacturing cost of the instrument is effectively reduced.
[0023] (3) The present invention integrates the dispersive element and the detection element inside the vacuum cavity. The vacuum environment effectively eliminates the scattering and stray absorption of X-rays by air, significantly improving the signal-to-noise ratio of the spectrum acquisition. At the same time, the design also weakens the attenuation effect of air on low-energy X-rays, successfully extending the working energy range of the laboratory spectrometer to the low-energy band. Attached Figure Description
[0024] Figure 1This is a schematic diagram of the overall structure of a wavelength dispersive X-ray absorption spectrometer according to an embodiment of the present invention; Figure 2 This is a three-dimensional structural diagram of a light source unit according to an embodiment of the present invention; Figure 3 This is a top view of a light source unit according to an embodiment of the present invention; Figure 4 This is a schematic diagram of the structure of a sample chamber assembly according to an embodiment of the present invention; Figure 5 This is a three-dimensional structural diagram of a splicing base plate according to an embodiment of the present invention; Figure 6 This is a three-dimensional structural diagram of the first base plate, the second base plate, and the third base plate in one embodiment of the present invention; Figure 7 This is a schematic diagram of the second and third base plates in one embodiment of the present invention; Figure 8 This is a schematic diagram of the structure of two sides of a wavelength dispersive X-ray absorption spectrometer according to an embodiment of the present invention; Figure 9 This is a three-dimensional structural schematic diagram of a cylindrical bent crystal support adjustment component according to an embodiment of the present invention; Figure 10 This is a three-dimensional structural diagram of a crystal component turntable adapter according to an embodiment of the present invention; Figure 11 This is a schematic diagram of a three-dimensional structure of an I-shaped bracket according to an embodiment of the present invention; Figure 12 This is a schematic diagram of another perspective of the structure of an I-shaped bracket in one embodiment of the present invention; Figure 13 This is a three-dimensional structural diagram of a magnetic base mounting block according to an embodiment of the present invention; Figure 14 This is a schematic diagram of another perspective of the structure of a magnetic base mounting block in one embodiment of the present invention; Figure 15 This is a three-dimensional structural diagram of a first linear module according to an embodiment of the present invention; Figure 16 This is a three-dimensional structural diagram of a surface detector support adjustment assembly according to an embodiment of the present invention; Figure 17 This is a three-dimensional structural diagram of a bracket according to an embodiment of the present invention; Figure 18 This is a three-dimensional structural diagram of a second linear module according to an embodiment of the present invention; Figure 19 This is a three-dimensional structural diagram of a support structure according to an embodiment of the present invention; Figure 20This is a schematic diagram of another perspective of a support structure in one embodiment of the present invention; Figure 21 This is a three-dimensional structural diagram of a vacuum cavity according to an embodiment of the present invention; Figure 22 This is a side view of a vacuum cavity structure according to an embodiment of the present invention; Figure 23 This is a schematic diagram of the structure of a vacuum cavity from another perspective in one embodiment of the present invention; Figure 24 This is a cross-sectional view of a vacuum cavity according to an embodiment of the present invention; Figure 25 This is a three-dimensional structural diagram of a vacuum acquisition unit according to an embodiment of the present invention; Figure 26 This is a three-dimensional structural schematic diagram of a wavelength dispersion mechanism according to an embodiment of the present invention; Figure 27 This is a top-view optical path diagram of the working range of a wavelength dispersive X-ray absorption spectrometer according to an embodiment of the present invention.
[0025] Explanation of reference numerals in the attached figures: 1. Light source unit; 11. Liquid target X-ray source; 12. Jet pump; 13. Sample chamber assembly; 131. Shutter assembly; 132. Beam confinement aperture mounting plate; 133. Sample; 134. Sample chamber body; 135. Sample tank; 136. First screw; 137. Sample chamber cover; 138. Clamp; 139. Bellows; 14. Support assembly; 15. Three-axis manual displacement stage assembly; 16. Beryllium window welding flange; 17. Brinellation emission direction; 18. First coordinate axis; 19. Second coordinate axis; 2. Vacuum acquisition unit; 21. Multistage Roots pump set; 22. Hydraulic bellows; 23. Manual angle valve; 24. Air extraction / release valve; 25. Pirani gauge; 3. Water-cooled unit for surface detector; 4. Support structure; 41. First support component; 42. Second support component; 43. Third support component; 411. First aluminum profile frame structure; 412. First welded sheet metal part; 413. First aluminum plate; 414. Bottom sheet metal part; 415. Caster; 416. First end face sheet metal; 417. First side sheet metal; 44. Fourth support component; 441. Second aluminum profile frame structure; 442. Second welded sheet metal part; 443. Second aluminum plate; 444. Second end face sheet metal; 445. Second side sheet metal; 5. Vacuum chamber; 51. First cylindrical chamber; 52. Second cylindrical chamber; 53. Third cylindrical chamber; 511. Proximity switch; 512. Circular side plate; 513. Functional feedthrough flange assembly; 514. First long mounting plate; 515. Second long mounting plate; 516. Third long mounting plate; 517. Cylindrical locating pin; 518. Rectangular block; 519. Set screw; 54. U-shaped support; 55. Second lifting ring; 56. Tricolor tower light; 57. Circular side door; 58. Observation window; 59. Circular end side door; 510. Center-mounted observation window; 6. Interlocking base plate; 61. First base plate; 62. Second base plate; 63. Third base plate; 64. Connecting plate; 65. First lifting ring; 66. Adjusting bolt; 67. Second screw; 68. Locating pin; 69. Both sides; 7. First linear module; 71. First motion platform; 8. Cylindrical bent crystal support adjustment assembly; 81. Differential head assembly mounting plate; 82. Differential head mounting block; 83. Differential head; 84. Turntable assembly fixing plate; 85. First electric turntable; 86. Crystal assembly turntable adapter; 861. Disc; 862. Cylindrical; 863. Mounting plate; 87. First electric arc swing stage; 88. Magnetic seat mounting block; 89. Cylindrical bent crystal mounting assembly; 891. I-beam bracket; 892. Positioning round hole; 893. Positioning waist hole; 894. Thin cylindrical bent crystal; 895. Third screw; 896. Mounting steel plate; 810. First positioning pin; 811. Second positioning pin; 9. Surface detector support and adjustment assembly; 91. Electric linear stage; 92. Fourth base plate; 93. Bracket; 931. Mounting base plate; 932. Side plate; 933. Mounting top plate; 94. Second electric turntable; 95. Intermediate plate; 96. Second electric arc swing stage; 97. Elevation plate; 98. Surface detector; 10. Second linear module; 101. Second motion platform; 110. Third locating pin; 120. Fourth screw; 130. Fifth screw; 140. Wavelength dispersive mechanism. Detailed Implementation
[0026] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
[0027] An embodiment of the present invention provides a wavelength dispersive X-ray absorption spectrometer including a light source unit 1, a vacuum acquisition unit 2, a surface detector water-cooling unit 3, a support structure 4, a vacuum cavity 5, etc. Figure 1 As shown.
[0028] The light source unit 1 mainly consists of a liquid target X-ray source 11, a jet pump 12, a sample chamber assembly 13, a support assembly 14, a three-axis manual displacement stage assembly 15, and a beryllium window welding flange 16. Figure 2 As shown.
[0029] The bremsstrahlung emission direction of the liquid target X-ray source 11 is 17. The three-axis manual displacement stage assembly 15 can fine-tune the installation position of the liquid target X-ray source 11 in the first coordinate axis 18, the second coordinate axis 19 and the three directions of rotation around the axis in the spatial Cartesian coordinate system.
[0030] The sample chamber assembly 13 mainly consists of components such as the shutter assembly 131, the beam-limiting aperture mounting plate 132, the sample chamber body 134, the bellows 139, and the clamp 138. Figure 4 As shown. Sample 133 is inserted into sample slot 135 and fastened by first screw 136. Sample chamber cover 137 has a stepped structure and is magnetically fixed to sample chamber body 134.
[0031] It should be noted that this embodiment uses a liquid target X-ray source as the light source unit of the entire spectrometer. However, solid target X-ray sources and synchrotron radiation sources can also be used as the light source of this invention.
[0032] The wavelength dispersion mechanism 140 inside the entire spectrometer mainly consists of components such as a spliced base plate 6, a first linear module 7, a cylindrical bent crystal support and adjustment assembly 8, a surface detector support and adjustment assembly 9, and a second linear module 10. Figure 5 As shown. The modular base plate 6 consists of a first base plate 61, a second base plate 62, a third base plate 63, a connecting plate 64, a first lifting ring 65, and adjusting bolts 66, as follows. Figure 6 As shown.
[0033] After the second base plate 62 and the third base plate 63 overlap, the positioning pin 68 engages with the positioning hole on the connecting plate 64 to achieve positioning of the three components: the second base plate 62, the third base plate 63, and the connecting plate 64. The connection is then completed by the second screw 67. Figure 6 , Figure 7 As shown.
[0034] The positioning and installation of the first base plate 61, the second base plate 62, and the connecting plate 64 are also in the same manner. The two sides 69 of the spliced base plate 6 are the positioning and mounting surfaces for the first linear module 7 and the second linear module 10, as shown below. Figure 8 As shown.
[0035] The cylindrical bending crystal support adjustment assembly 8 mainly consists of components such as a micrometer head assembly mounting plate 81, a micrometer head mounting block 82, a micrometer head 83, a turntable assembly fixing plate 84, a first electric turntable 85, a crystal assembly turntable adapter 86, a first electric arc swing stage 87, a magnetic seat mounting block 88, and a cylindrical bending crystal mounting assembly 89. These components are stacked and connected by threads from bottom to top. Figure 9 As shown.
[0036] The crystal assembly turntable adapter 86 is mainly composed of a disk 861, a cylinder 862, and a mounting plate 863, which are connected and stacked from bottom to top by threaded connections, such as... Figure 10 As shown. The thin cylindrical bent crystal 894 is placed on the I-shaped bracket 891 in the cylindrical bent crystal mounting assembly 89, and can be tightened by two PPEK third screws 895. The bottom front end of the I-shaped bracket 891 has a positioning round hole 892 and a positioning waist hole 893. A steel plate 896 is installed at the bottom of the I-shaped bracket 891, as shown. Figure 11 , Figure 12 As shown.
[0037] The bottom front end of the I-shaped bracket 891 has a positioning round hole 892 and a positioning waist hole 893, which respectively cooperate with the first positioning pin 810 and the second positioning pin 811 to complete the positioning of the cylindrical bending crystal mounting assembly 89 on the cylindrical bending crystal support adjustment assembly 8, and achieve magnetic installation through the knob-type magnetic suction seat 812 installed in the magnetic seat mounting block 88, such as... Figure 13 , Figure 14 As shown. The cylindrical bent crystal support adjustment assembly 8 is positioned and installed on the first motion table 71 of the first linear module 7 by the third positioning pin 110 and the fourth screw 120, as follows. Figure 15 As shown.
[0038] The surface detector support and adjustment assembly 9 mainly consists of components such as an electric linear stage 91, a fourth base plate 92, a bracket 93, a second electric turntable 94, an intermediate plate 95, a second electric arc swing stage 96, a riser plate 97, and a surface detector 98. These components are stacked and connected by threads from bottom to top. Figure 16 As shown. The bracket 93 is constructed by stacking and threading the mounting base plate 931, side plate 932, and mounting top plate 933 from bottom to top, as shown. Figure 17 As shown.
[0039] The surface detector support adjustment assembly 9 is installed on the second motion platform 101 of the second linear module 10 by the fifth screw 130, as follows: Figure 18 As shown.
[0040] The support structure 4 is mainly composed of a first support component 41, a second support component 42, a third support component 43, and a fourth support component 44, all of which have the same structure. Figure 19As shown. The first support assembly 41, the second support assembly 42, and the third support assembly 43 are all bottom sheet metal parts 414 welded to the bottom of the first aluminum profile frame structure 411, and are fitted with casters 415. The top of the first aluminum profile frame structure 411 is fitted with a first aluminum plate 413. The fourth support assembly 44 is also a second welded sheet metal part 442 welded to the bottom of the second aluminum profile frame structure 441, and a second aluminum plate 443 is fitted to the top. The first support assembly 41, the second support assembly 42, and the third support assembly 43 are symmetrically fitted with first end face sheet metal 416 and first side face sheet metal 417 on each side of the first aluminum profile frame structure 411. The fourth support assembly 44 is fitted with second end face sheet metal 444 and second side face sheet metal 445 on each side of the second aluminum profile frame structure 441, as shown. Figure 19 , Figure 20 As shown.
[0041] The vacuum chamber 5 is mainly composed of a first cylindrical chamber 51, a second cylindrical chamber 52, and a third cylindrical chamber 53. Each chamber has a U-shaped support 54 welded to its bottom area, a lifting ring 55 installed on its top area, and circular side doors 57 and observation windows 58 installed on both sides. A circular end side door 59 is installed on the end face of the cylindrical chamber 53, and an observation window 510 is installed in the center. A circular side plate 512 is installed on the end face of the cylindrical chamber 53, on which a functional feedthrough flange assembly 513 is opened. Figure 21 , Figure 22 As shown.
[0042] A tri-color tower light 56 is installed on the top of the first cylindrical cavity 51, and proximity switches 511 are installed on both the circular side door 57 and the circular end side door 59. Figures 21-23 As shown. A first elongated mounting plate 514, a second elongated mounting plate 515, and a third elongated mounting plate 516 are welded to both sides of the interior of the vacuum chamber 5. Two cylindrical locating pins 517 are mounted on the first elongated mounting plate 514 on one side. Rectangular blocks 518 and set screws 519 are mounted on both the second elongated mounting plate 515 and the third elongated mounting plate 516. Figure 24 As shown.
[0043] Vacuum acquisition unit 2 consists of components such as a multi-stage Roots pump assembly 21, a hydraulic bellows 22, a manual angle valve 23, a venting valve 24, and a Pirani gauge 25. All components are mounted on the functional feedthrough flange assembly 513. Figure 25 As shown.
[0044] The entire wavelength dispersion mechanism 140 is mounted on the first elongated mounting plate 514, the second elongated mounting plate 515, and the third elongated mounting plate 516 on both sides inside the vacuum chamber 5, as follows: Figure 26 As shown.
[0045] Top-view optical path diagram of the entire spectrometer's working range as follows Figure 27As shown, the incident X-ray 160 emitted from the light source point 150 in the liquid target X-ray source 11 hits the receiving position 170 of the cylindrical curved crystal 894. At this time, the Bragg angle (the angle between the internal lattice plane of the crystal and the incident X-ray) is 180. The outgoing X-ray 190 dispersed by the cylindrical curved crystal 894 hits the receiving position 200 of the surface detector 98. The Bragg angle 180, the cylindrical curved crystal receiving position 170, and the surface detector receiving position 200 determine the lower limit of the operating range of the entire spectrometer.
[0046] When the incident X-ray 210 emitted from the light source point 150 in the liquid target X-ray source 11 hits the receiving position 220 of the cylindrical curved crystal 894, the Bragg angle of the crystal is 230°. The outgoing X-ray 240 dispersed by the cylindrical curved crystal 894 hits the receiving position 250 of the surface detector 98. The Bragg angle 230°, the receiving position 220 of the cylindrical curved crystal, and the receiving position 250 of the surface detector determine the upper limit of the working range of the entire spectrometer.
[0047] Throughout the entire operating range of the spectrometer, the linear travel of the cylindrical curved crystal 894 on the first linear module 7 is 260°, the linear travel of the surface detector 98 on the second linear module 10 and the motorized linear stage 91 are 270° and 280° respectively, and the angle travel of the surface detector 98 from the receiving position 200 to the receiving position 250 relative to the emitted X-rays dispersed by the cylindrical curved crystal 894 is 290°. Throughout the entire operating range, the internal sensor of the surface detector 98 always receives the emitted X-rays dispersed by the cylindrical curved crystal 894 perpendicularly.
[0048] It should be noted that in this embodiment, both the cylindrical curved crystal 894 and the surface detector 98 are eccentrically mounted to the first motorized turntable 85 and the second motorized turntable 94. That is, the geometric centers of the cylindrical curved crystal 894 and the surface detector 98 are not coaxial with the rotation axes of their respective motorized turntables 85 and 94. The principle behind this is that during the overall instrument design, parameters such as the X-ray source system's emission angle, the crystal's width along the incident light path, and the surface detector's width are rationally optimized based on the designed spectrometer's energy range, bandwidth, and energy resolution. By rationally eccentrically arranging the crystal and surface detector, and by using a receiving method where the surface detector is always perpendicular to the emitted X-rays (effectively reducing the width of the surface detector), the energy bandwidth corresponding to the near edge (XANES) and extended edge (EXAFS) of the analyte can be simultaneously presented on the surface detector during absorption spectrum acquisition. This allows for the simultaneous acquisition of a complete absorption spectrum without changing the crystal or switching the optical path. This greatly improves experimental efficiency and significantly reduces equipment costs (eliminating the need for dual crystals, dual detectors, and the associated electrically driven stages required for switching optical paths). Furthermore, by placing the crystal and surface detector within a vacuum chamber, this invention effectively eliminates stray absorption of X-rays by air scattering, further extending the spectrometer's energy range to lower energy bands.
[0049] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.
Claims
1. A wavelength dispersive X-ray absorption spectrometer, comprising a light source unit (1), a vacuum acquisition unit (2), a surface detector water-cooling unit (3), and a support structure (4), characterized in that, It also includes a wavelength dispersion mechanism (140); The light source unit (1) includes a jet pump (12), a three-axis manual displacement stage assembly (15) disposed on one side of the jet pump (12), a support assembly (14) disposed above the three-axis manual displacement stage assembly (15), a liquid target X-ray source (11) disposed on the top of the support assembly (14), and a sample chamber assembly (13) disposed on one side of the liquid target X-ray source (11); the sample chamber assembly (13) includes a shutter assembly (131), a beam-limiting aperture mounting plate (132), a sample chamber body (134), a sample slot (135), a bellows (139), and a clamp (138). The sample slot (135) is used to accommodate a sample (133), and a sample chamber cover (137) is disposed above the sample chamber body (134). The wavelength dispersion mechanism (140) is disposed in the vacuum cavity (5) and includes a spliced base plate (6), a first linear module (7), a cylindrical bent crystal support adjustment assembly (8), a surface detector support adjustment assembly (9), and a second linear module (10). The vacuum acquisition unit (2) is used to generate a vacuum environment in the vacuum cavity (5).
2. The wavelength dispersive X-ray absorption spectrometer according to claim 1, characterized in that: The spliced base plate (6) includes a second base plate (62), a first base plate (61) disposed on one side of the second base plate (62), a third base plate (63) disposed on the other side of the second base plate (62), and connecting plates (64) disposed on both sides of the top of the second base plate (62); and one side of the connecting plates (64) on both sides respectively contacts the top of the first base plate (61) and the third base plate (63), and the connecting plates (64) are provided at the overlapping contact positions of the first base plate (61), the second base plate (62), and the third base plate (63). There is a positioning pin (68), and a second screw (67) is provided inside the positioning pin (68). A first lifting ring (65) is provided at the four corners of the top of the first base plate (61), the second base plate (62) and the third base plate (63). Adjusting bolts (66) are provided at both ends and both sides of the top of the first base plate (61), the second base plate (62) and the third base plate (63). The spliced base plate (6) has two opposite sides (69). The first linear module (7) and the second linear module (10) are respectively installed on the two sides (69).
3. The wavelength dispersive X-ray absorption spectrometer according to claim 1, characterized in that: The cylindrical bending crystal support adjustment assembly (8) includes a microhead assembly mounting plate (81), microhead mounting blocks (82) disposed on both sides of the top of the microhead assembly mounting plate (81), a microhead (83) disposed on one side of the microhead mounting block (82), a turntable assembly fixing plate (84) disposed on the top of the microhead assembly mounting plate (81), a first electric turntable (85) disposed on the top of the turntable assembly fixing plate (84), and a crystal assembly turntable adapter (86) disposed above the first electric turntable (85).
4. The wavelength dispersive X-ray absorption spectrometer according to claim 3, characterized in that: The crystal assembly turntable adapter (86) includes a mounting plate (863) disposed on the top of the first electric turntable (85), a cylinder (862) disposed on the top of the mounting plate (863), and a disk (861) disposed on the top of the cylinder (862). The top of the disk (861) is provided with a first electric arc swing stage (87), a magnetic seat mounting block (88) is provided on the first electric arc swing stage (87), and a cylindrical curved crystal mounting assembly (89) is provided above the magnetic seat mounting block (88).
5. The wavelength dispersive X-ray absorption spectrometer according to claim 4, characterized in that: The cylindrical bent crystal mounting assembly (89) includes an I-shaped bracket (891) disposed above the magnetic base mounting block (88), a thin cylindrical bent crystal (894) disposed on one side of the I-shaped bracket (891), a third screw (895) disposed on the top of the I-shaped bracket (891), a mounting steel plate (896) disposed on the bottom of the I-shaped bracket (891), a positioning round hole (892) disposed on one end of the bottom side of the I-shaped bracket (891), a positioning waist hole (893) disposed on the other end of the bottom side of the I-shaped bracket (891), and a knob-type magnetic holder (812) disposed on the magnetic base mounting block (88); the magnetic The top of the sex seat mounting block (88) is provided with a first positioning pin (810) and a second positioning pin (811), the first positioning pin (810) and the second positioning pin (811) are adapted to the positioning round hole (892) and the positioning waist hole (893); the first linear module (7) includes a first motion table (71), the micro-head assembly mounting plate (81) is disposed on the first motion table (71), the first motion table (71) is provided with a third positioning pin (110) and a fourth screw (120), the third positioning pin (110) and the fourth screw (120) are used to position and install the cylindrical bending crystal support adjustment assembly (8) on the first motion table (71).
6. The wavelength dispersive X-ray absorption spectrometer according to claim 2, characterized in that: The second linear module (10) is provided with a second motion table (101), and a surface detector support adjustment assembly (9) is installed on the second motion table (101). The surface detector support adjustment assembly (9) includes an electric linear stage (91). The electric linear stage (91) is provided with multiple sets of fifth screws (130). The bottom end of the fifth screws (130) extends into the second motion table (101). A fourth base plate (92) is provided above the electric linear stage (91), and a bracket (93) is provided above the fourth base plate (92). The bracket (93) includes a mounting base plate (931) disposed on the top of the fourth base plate (92), side plates (932) are disposed on both sides of the top of the mounting base plate (931), a mounting top plate (933) is disposed on the top of the side plates (932), a second electric turntable (94) is disposed on the top of the mounting top plate (933), an intermediate plate (95) is disposed on the second electric turntable (94), a second electric arc swing table (96) is disposed on the top of the intermediate plate (95), a shim plate (97) is disposed on the top of the second electric arc swing table (96), and a surface detector (98) is disposed on the top of the shim plate (97).
7. The wavelength dispersive X-ray absorption spectrometer according to claim 1, characterized in that: The support structure (4) includes a first support component (41), a second support component (42), and a third support component (43); the bottoms of the first support component (41), the second support component (42), and the third support component (43) are all composed of the same first aluminum profile frame structure (411); casters (415) are provided at the bottom of the first aluminum profile frame structure (411); a first aluminum plate (413) is provided at the top of the first aluminum profile frame structure (411); a fourth support component (44) is provided at one end of the first support component (41); the fourth support component (44) is composed of a second aluminum profile frame structure (441); a second welded sheet metal part (442) is provided at the bottom of the surface of the second aluminum profile frame structure (441); a second aluminum plate (443) is provided at the top of the second aluminum profile frame structure (441). The first aluminum profile frame structure (411) has a first end face sheet metal (416) on both sides, a first side sheet metal (417) on both ends, a second end face sheet metal (444) on both sides, and a second side sheet metal (445) on both ends. And / or, the sample chamber assembly (13) is provided with a beryllium window welding flange (16); And / or, a first screw (136) is provided on the sample slot (135) for fixing the sample (133) in the sample slot (135); And / or, the sample chamber cover (137) and the sample chamber body (134) are magnetically fixed together.
8. The wavelength dispersive X-ray absorption spectrometer according to claim 1, characterized in that: The vacuum chamber (5) includes a first cylindrical chamber (51), a second cylindrical chamber (52), and a third cylindrical chamber (53); each of the first cylindrical chamber (51), the second cylindrical chamber (52), and the third cylindrical chamber (53) is provided with a U-shaped support (54); each of the first cylindrical chamber (51), the second cylindrical chamber (52), and the third cylindrical chamber (53) is provided with a second lifting ring (55); each of the first cylindrical chamber (51), the second cylindrical chamber (52), and the third cylindrical chamber (53) is provided with a circular side door (57) on both sides, and an observation window (58) is provided in the middle of the circular side door (57).
9. The wavelength dispersive X-ray absorption spectrometer according to claim 8, characterized in that: A circular end door (59) is installed at one end of the third cylindrical cavity (53), and a central observation window (510) is provided at the middle position of the circular end door (59). A circular side plate (512) is installed at one end of the first cylindrical cavity (51), and a functional feedthrough flange assembly (513) is provided on the circular side plate (512). A proximity switch (511) is installed on both the circular side door (57) and the circular end door (59). A first long strip mounting plate (514) is installed on both sides inside the first cylindrical cavity (51). A second long strip mounting plate (515) is installed on both sides inside the second cylindrical cavity (52). A third long strip mounting plate (516) is installed on both sides inside the third cylindrical cavity (53). The wavelength dispersion mechanism (140) is installed on the first long strip mounting plate (514), the second long strip mounting plate (515), and the third long strip mounting plate (516).
10. The wavelength dispersive X-ray absorption spectrometer according to claim 9, characterized in that: The vacuum acquisition unit (2) includes a multi-stage Roots pump group (21), and a hydraulic bellows (22) is connected to the top of the multi-stage Roots pump group (21). A manual angle valve (23), a venting valve (24), and a Pirani gauge (25) are provided on the hydraulic bellows (22). And / or, a cylindrical positioning pin (517) is installed on the first elongated mounting plate (514), and a rectangular block (518) is installed on the second elongated mounting plate (515) and the third elongated mounting plate (516), and a set screw (519) is installed on the rectangular block (518). And / or, a tricolor tower lamp (56) is provided on the top of the first cylindrical cavity (51).