Multifunctional laboratory spectrometer

By designing a multifunctional laboratory spectrometer and using the precisely linked Roland circular configuration, the problem of the inability to measure the bevel angle and curvature radius in the existing technology is solved, and the acquisition of a variety of X-ray spectrometers is realized, which improves the function and flexibility of the laboratory spectrometer.

CN119861095APending Publication Date: 2025-04-22SHANGHAI INSTITUTE OF APPLIED PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202311354502.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-10-19
Publication Date
2025-04-22

AI Technical Summary

Technical Problem

Existing laboratory spectrometers cannot realize the orientation and determination of spherical curved crystal tangent angles, as well as the determination of spherical curved crystal curvature radius, and cannot be used for the X-ray emission spectrum acquisition of samples.

Method used

A multifunctional laboratory spectrometer is designed, including a ray source assembly, a detection assembly and a crystal assembly. Through a precisely linked Roland circular configuration, the measurement of the bevel angle and curvature radius of spherical curved crystals is realized, and the acquisition of X-ray absorption spectrum and emission spectrum is supported.

Benefits of technology

The oblique tangent angle orientation and measurement of spherical curved crystals and the radius of curvature are realized, and the sample X-ray absorption spectrum and emission spectrum in the Bragg angle range can be collected, and it has multi-functional properties of one machine.

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Abstract

A radiation source assembly comprises an X-ray source and a first linear moving mechanism allowing the X-ray source to move, and a detection assembly comprises a first detector and a second linear moving mechanism allowing the first detector to linearly move. The crystal assembly comprises a spherical curved crystal and a motion table assembly allowing the spherical curved crystal to linearly move and rotate, the X-ray source, the spherical curved crystal and the first detector are precisely linked according to a Rowland circle configuration, first incident light emitted by the X-ray source is monochromatized by the spherical curved crystal, and then first focused reflected light is received by the first detector; therefore, the size and the direction of the chamfer angle of the spherical curved crystal can be measured. According to the multifunctional laboratory spectrometer provided by the invention, the transmission type X-ray source, the spherical curved crystal, the sample and the detector assembly are precisely linked according to a certain Rowland circle configuration, and the multifunctional laboratory spectrometer has multiple functions by changing the mounting positions of the X-ray source and the sample and matching different types of detectors.
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Description

Technical Field

[0001] The present invention relates to a laboratory spectrometer, and more particularly to a multifunctional laboratory spectrometer. Background Art

[0002] X-ray spectroscopy (including absorption and emission spectroscopy) is an experimental technique that has matured with the development of synchrotron radiation facilities. It is one of the important methods for studying the structure of matter. It can study the local structure of atomic neighbors under a variety of conditions such as solid and liquid states, and is widely used in many fields such as materials, biology, chemistry, environment, and geology.

[0003] The laboratory spectrometer is an analytical instrument based on the Rowland circle imaging principle and is composed of components such as an X-ray source, a spherical curved crystal, a detector, and a high-precision translation stage. It can measure the local structural information of different elements (such as the type, valence state, bond length, coordination number, etc. of the coordinated elements).

[0004] CN202211733446.6 discloses a laboratory spectrometer, the main disadvantages of which are: 1) it is impossible to achieve the orientation and measurement of the bevel angle of spherical curved crystals and the measurement of the curvature radius of spherical curved crystals; 2) it cannot be used for collecting X-ray emission spectra of samples. Summary of the invention

[0005] In order to solve the problem that the laboratory spectrometer in the prior art cannot realize the orientation and measurement of the bevel angle of spherical curved crystals, the present invention provides a multifunctional laboratory spectrometer.

[0006] According to the multifunctional laboratory spectrometer of the present invention, it includes a ray source assembly, a detection assembly and a crystal assembly. The ray source assembly includes an X-ray source and a first linear moving mechanism allowing the X-ray source to move. The detection assembly includes a first detector and a second linear moving mechanism allowing the first detector to move linearly. The crystal assembly includes a spherical curved crystal and a moving table assembly allowing the spherical curved crystal to move linearly and rotate. The X-ray source, the spherical curved crystal and the first detector are precisely linked according to a Rowland circle configuration. The first focused reflected light of the first incident light emitted by the X-ray source after being monochromatized by the spherical curved crystal is received by the first detector to measure the size and orientation of the bevel angle of the spherical curved crystal.

[0007] Preferably, the X-ray source is mounted on a first guide assembly, and the first guide assembly is mounted on a first bearing mounting seat via a first bearing.

[0008] Preferably, the first bearing is mounted in a circular groove of the first bearing mounting seat, the outer ring of the first bearing is fixedly connected to the first bearing mounting seat, and the inner ring of the first bearing is connected to the first guide assembly.

[0009] Preferably, the first detector is mounted on the second guide assembly, and the second guide assembly is mounted on the second bearing mounting seat via a second bearing.

[0010] Preferably, the second bearing is mounted in a circular groove of the second bearing mounting seat, the outer ring of the second bearing is fixedly connected to the second bearing mounting seat, and the inner ring of the second bearing is connected to the second guide assembly.

[0011] Preferably, the crystal assembly has a cylinder, and the first and second guide components respectively have a U-shaped long groove, and the two side surfaces of the U-shaped long groove form a small gap fit with the cylindrical surface of the cylinder.

[0012] Preferably, the first linear motion mechanism includes a first translation stage, the detection assembly also includes a second detector and a second translation stage, the second incident light emitted by the X-ray source and the second focused reflected light after being monochromatized by the spherical curved crystal are received by the second detector, and the curvature radius of the spherical curved crystal is measured by moving the first translation stage and the second translation stage in the same direction.

[0013] Preferably, the detection assembly includes a sample assembly, and the third incident light emitted by the X-ray source and the third focused reflected light after being monochromatized by the spherical curved crystal are transmitted through the sample assembly and received by the first detector, so as to realize the absorption spectrum collection of the sample within the energy range corresponding to the Bragg angle of 54.5° to 85.5°.

[0014] Preferably, the sample assembly is a standard sample mounting assembly or a prepared sample mounting assembly.

[0015] Preferably, the ray source assembly also includes a standard sample mounting assembly for mounting the sample to be measured. The fourth incident light emitted by the X-ray source hits the sample to be measured, and the fourth focused reflected light of the characteristic fluorescent X-ray excited by it is monochromatized by the spherical curved crystal and received by the first detector, so as to realize the emission spectrum collection of the sample within the energy range corresponding to the Bragg angle of 54.5° to 85.5°.

[0016] The multifunctional laboratory spectrometer according to the present invention precisely links the transmission X-ray source, spherical curved crystal, sample and detector assembly according to a certain Rowland circle configuration. By changing the installation positions of the X-ray source and the sample and matching different types of detectors, the X-ray absorption and emission spectrum collection of various conventional samples within the energy range corresponding to the Bragg angle of 54.5° to 83.5° can be realized. It can also be used for the orientation and measurement of the bevel angle of spherical curved crystals and the measurement of the curvature radius of spherical curved crystals, and has the multifunctional attribute of one machine with multiple uses. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 The X-ray absorption spectrum principle of the multifunctional laboratory spectrometer according to the present invention is shown.

[0018] Figure 2 Show Figure 1 The optical path for collecting the sample absorption spectrum corresponds to the Bragg angle range of the multifunctional laboratory spectrometer.

[0019] Figure 3 The X-ray emission spectrum principle of the multifunctional laboratory spectrometer according to the present invention is shown.

[0020] Figure 4 Show Figure 3 The optical path for collecting the sample emission spectrum corresponds to the Bragg angle range of the multifunctional laboratory spectrometer.

[0021] Figure 5 The angle between the normal vector of the geometric center of the substrate surface of the spherically bent crystal and the normal vector of the lattice plane in the coating is shown.

[0022] Figure 6 The deviation between the radius of curvature of the lattice plane in the spherical curved crystal coating and the radius of curvature of the substrate surface is shown.

[0023] Figure 7 It is a schematic diagram of the overall structure of the multifunctional laboratory spectrometer according to the present invention.

[0024] Figure 8 yes Figure 7 Schematic diagram of the structure of the radiation source assembly.

[0025] Fig. 9 yes Figure 8 Schematic diagram of the structure of the X-ray source related structure.

[0026] Fig.10 yes Fig. 9 Schematic diagram of the structure of the X-ray source assembly.

[0027] Fig.11 yes Fig.10 sectional view of .

[0028] Fig.12 yes Fig. 9 Schematic diagram of the structure of the standard installation component.

[0029] Fig.13 yes Fig.12 Schematic diagram of the structure of the mounting base.

[0030] Fig.14 yes Fig.12 Schematic diagram of the structure of the T-type limiter.

[0031] Fig.15 yes Fig.14 sectional view of .

[0032] Fig.16 yes Fig.12 Another perspective of the view.

[0033] Fig.17 yes Fig. 9 Another view of the standard mounting assembly and mount.

[0034] Fig.18 yes Figure 8 Schematic diagram of the assembly of the pad plate and translation stage.

[0035] Fig.19 yes Figure 8 Assembly diagram of the bearing mount, spacer plate and translation stage.

[0036] Fig. 20 yes Fig. 9 Schematic diagram of the structure of the guide component.

[0037] Fig.21 yes Fig. 20 Another perspective of the view.

[0038] Fig. 22 yes Figure 8 Assembly diagram of the guide assembly and bearing mount.

[0039] Fig.23 yes Fig. 9 Schematic diagram of the assembly of the translation stage and guide components.

[0040] Fig.24 yes Fig. 9 Schematic diagram of the assembly of the mounting plate and translation stage.

[0041] Fig.25 It is a schematic diagram of the structure of the detection assembly of 7.

[0042] Fig.26 yes Fig.25 Structural diagram of detector related structures.

[0043] Fig. 27 yes Fig.26 Schematic diagram of the structure of the silicon drift detector assembly.

[0044] Fig.28 yes Fig. 27 sectional view of .

[0045] Fig.29 yes Fig. 27 Another perspective of the view.

[0046] Fig.30 yes Fig.26 Schematic diagram of the structure of the surface detector assembly.

[0047] Fig.31 yes Fig.30 Assembly diagram of the base plate and support plate.

[0048] Fig.32 yes Fig.30 Another perspective of the view.

[0049] Fig.33 yes Fig.26 Schematic diagram of the structure of the sample component used as the standard installation component.

[0050] Fig.34 yes Fig.33 Another perspective of the view.

[0051] Fig.35 yes Fig.26 Schematic diagram of the structure of a sample assembly used to prepare a sample mounting assembly.

[0052] Fig.36 It is a schematic diagram of the assembly of the sample component and the magnetic plate.

[0053] Fig.37 yes Fig.26 Schematic diagram of the assembly of the mounting plate and translation stage.

[0054] Fig.38 yes Fig.25 Another perspective of the view.

[0055] Fig.39 It is a structural schematic diagram of the crystal assembly of 7.

[0056] Fig.40 yes Fig.39 Schematic diagram of the structure of the support component.

[0057] Fig.41 yes Fig.40 Another perspective of the view.

[0058] Fig.42 yes Fig.39 Assembly diagram of the support assembly and linear translation stage.

[0059] Fig.43 yes Fig.39 Assembly diagram of the turntable, support assembly and linear translation stage.

[0060] Fig.44 yes Fig.39 Assembly diagram of the vertical motion table, pitch motion table and turntable.

[0061] Fig.45 yes Fig.39 Schematic diagram of the structure of the crystal assembly.

[0062] Fig.46 yes Fig.45 Another perspective of the view.

[0063] Fig.47 yes Fig.45 Another perspective of the view.

[0064] Fig.48 yes Fig.45 Schematic diagram of the structure of the crystal positioning installation assembly.

[0065] Fig.49 yes Fig.48 sectional view of .

[0066] Fig.50 yes Fig.48 Another perspective of the view.

[0067] Fig.51 yes Fig.45 Schematic diagram of the turntable structure.

[0068] Fig.52 yes Fig.51 Another perspective of the view.

[0069] Fig.53 yes Fig.51 Another perspective of the view.

[0070] Fig.54 yes Fig.45 Schematic diagram of the assembly of the crystal positioning mounting assembly and the turntable.

[0071] Fig.55 yes Fig.39 Another perspective of the view.

[0072] Fig.56 yes Figure 7 Top view of the .

[0073] Fig.57 yes Figure 7 Another perspective of the view.

[0074] Fig.58 Show Figure 7 Spherical bend crystal bevel angle calibration mode for a versatile laboratory spectrometer.

[0075] Fig.59 Show Fig.58 of the light path.

[0076] Fig.60 Show Figure 7 The optical path of the spherical crystal curvature radius measurement mode of the multifunctional laboratory spectrometer.

[0077] Fig.61 Show Figure 7 Optical path of the multifunctional laboratory spectrometer in X-ray absorption spectrum acquisition mode.

[0078] Fig.62 Show Figure 7 Optical path of the multifunctional laboratory spectrometer in X-ray emission spectrum collection mode. DETAILED DESCRIPTION

[0079] In order to make the technical personnel in this field better understand the scheme of the present invention, the present invention is further described in detail below in conjunction with the drawings and specific embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention and are not used to limit the present invention.

[0080] In this article, X-ray absorption spectroscopy uses focused monochromatic X-rays to identify the elements contained in the sample being tested. The absorption lines have a specific relationship with atoms, so the chemical composition of the sample through which the X-rays pass can be distinguished.

[0081] In this article, X-ray emission spectroscopy is a technique for analyzing the properties of elements by detecting characteristic X-ray fluorescence, which can determine information such as the oxidation state, spin state, covalency, protonation state, and ligand environment of atoms.

[0082] In this article, spherical curved crystals are used to receive X-rays emitted by a radiation source, monochromatize them and focus them onto a sample. Usually, the surface of the glass substrate is spherical, and coatings of different materials and index surfaces are pasted or bonded on it to enable it to have focusing and splitting (monochromatization) capabilities.

[0083] The multifunctional laboratory spectrometer of the present invention uses a spherical curved crystal as the analysis crystal based on the Rowland circle imaging principle, and the corresponding Rowland circle diameter is the radius of the analysis crystal. The principle of the X-ray absorption spectrum of the Rowland circle configuration is as follows: Figure 1 As shown, from the perspective of the top view, the incident light 2 emitted by the X-ray source point 1 is monochromatized by the spherical curved crystal 3, and the focused reflected light 4 is transmitted through the sample 5 by the X-ray 6 and received by the silicon drift detector 7. The angle 10 between the incident light 2 at the spherical curved crystal 3 and the tangent 9 of the dynamic Rowland circle 8 (its position changes all the time during energy scanning, but the relative positions of the light source point 1, the spherical curved crystal 3 and the sample 5 must always be on the circle) is the Bragg angle. Changing the angle value and matching the spherical curved crystal 3 with different materials and index surfaces can change the energy used for scanning.

[0084] Since the transmission X-ray source used in the present invention has a small mass and no water cooling circuit, an electric high-precision translation stage (not shown here) is respectively configured for the ray source (i.e., the light source point 1), the spherical curved crystal 3, the sample 5 and the detector 7, and they are precisely linked according to the above-mentioned Rowland circle configuration to realize the absorption spectrum collection of different samples within the energy range corresponding to the Bragg angle of 54.5° to 83.5°.

[0085] The optical path for collecting the sample absorption spectrum corresponding to this Bragg angle range is as follows: Figure 2As shown, also from the perspective of the top view, the spherical curved crystal corresponding to the 54.5° Bragg angle 11 is located at position 12, and the incident light 14 emitted by the light source point at position 13 is monochromatized by the spherical curved crystal 12, and its focused reflected light 15 is transmitted through the sample at position 16 and is received by the detector at position 17. At this time, the center of the dynamic Rowland circle 18 is located at position 19. The spherical curved crystal corresponding to the 83.5° Bragg angle 20 is located at position 21, and the incident light 23 emitted by the light source point at position 22 is monochromatized by the spherical curved crystal 21, and its focused reflected light 24 is transmitted through the sample at position 25 and is received by the detector at position 26. At this time, the center of the dynamic Rowland circle 27 is located at position 28.

[0086] Similarly, the Rowland circle configuration X-ray emission spectrum principle based on the present invention is as follows Figure 3 As shown, from the perspective of the top view, the incident light 29 emitted by the X-ray source point 1 hits the sample 5 placed at a certain angle 30 with the incident light 29 (the angle 30 is 45°, which is most conducive to the excitation of the fluorescence signal), and the characteristic X-ray fluorescence 31 excited by it is monochromatized by the spherical curved crystal 3, and the focused reflected light 4 is received by the silicon drift detector 7. The angle 10 between the characteristic X-ray fluorescence 31 at the curved crystal 3 and the tangent 9 of the dynamic Rowland circle 8 (during energy scanning, its position changes all the time, but the relative positions of the sample 5, the spherical curved crystal 3 and the detector 7 must always be on the circle) is the Bragg angle. Changing the angle value and matching the spherical curved crystal 3 with different materials and index surfaces can change the energy used for scanning.

[0087] The optical path for collecting the sample emission spectrum corresponding to the Bragg angle range of 54.5° to 83.5° is as follows Figure 4 As shown, also from the perspective of the top view, it is Figure 2 The only difference is that at a Bragg angle of 54.5° 11, the incident light 32 is emitted from the light source at position 13 and hits the sample 33. The characteristic X-ray fluorescence 36 excited by it is monochromatized by the spherical curved crystal 12, and its focused reflected light 37 is received by the detector at position 17. At a Bragg angle of 83.5° 20, the incident light 34 is emitted from the light source at position 22 and hits the sample 35. The characteristic X-ray fluorescence 38 excited by it is monochromatized by the spherical curved crystal 21, and its focused reflected light 39 is received by the detector at position 26.

[0088] It should be noted that Figure 1 The absorption spectrum principle optical path diagram and Figure 3 In the optical path diagram of the emission spectrum principle shown in the figure, the length of the input and output arms symmetrical on the Rowland circle 8 ( Figure 1 The chord lengths of the incident light 2 and the focused reflected light 4 are, Figure 3 The chord lengths of the characteristic X-ray fluorescence 31 and the focused reflected light 4 are both Rc·Sinθ B, where Rc is the radius of curvature of the spherical curved crystal, θ B is the Bragg angle. That is, no matter when the absorption spectrum or emission spectrum energy scanning is linked, the relative position relationship of the key components (the light source point, the geometric center of the spherical curved crystal and the sample center when the absorption spectrum is collected; the sample center, the geometric center of the spherical curved crystal and the center of the detector receiving surface when the emission spectrum is collected) on the dynamic Rowland circle is only related to the radius of the spherical curved crystal and the size of the Bragg angle.

[0089] Generally, due to the processing error of the spherical curved crystal, there is a certain angle 44 between the normal vector 41 of the geometric center 40 of the glass substrate surface and the normal vector 43 of the lattice plane 42 in the coating. This angle is the bevel angle of the spherical curved crystal, such as Figure 5 shown.

[0090] In order to ensure that the light intensity signal received on the detector remains strong during the energy scanning process, the bevel angle of the spherical curved crystal must be corrected before the energy scanning, that is, the normal vector of the lattice plane in the coating is calibrated to the plane where the dynamic Rowland circle is located, and the lattice plane in the coating is tangent to the dynamic Rowland circle.

[0091] Similarly, due to the existence of processing errors and bevel angles, there is also a certain deviation between the curvature radius 46 of the lattice plane 42 in the spherical curved crystal coating and the curvature radius 45 of the substrate surface 40, such as Figure 6 shown.

[0092] Since the actual splitting surface is the lattice plane in the crystal coating, the curvature radius of the lattice plane must be accurately measured to ensure the relative position relationship of key components on the dynamic Rowland circle during energy scanning linkage.

[0093] In summary, according to the multifunctional laboratory spectrometer of the present invention, the bevel angle of the spherical curved crystal can be calibrated in advance, and the curvature radius of the lattice plane inside the coating can be measured to ensure the accuracy of the spectrum. Therefore, the multifunctional laboratory spectrometer provided by the present invention not only has the functions of X-ray absorption spectrum and emission spectrum acquisition, but also adds the functions of spherical curved crystal bevel angle orientation and measurement and spherical curved crystal curvature radius measurement, that is, it can not only be used for conventional laboratory X-ray energy spectrum acquisition, but also can be used as a calibration and measurement device for spherical curved crystals, which are key components in laboratory spectrometers, and has the multifunctional attribute of one machine for multiple uses.

[0094] The following first describes the structural composition of each part, and then reflects the changes in layout in combination with different usage modes and functions.

[0095] like Figure 7 As shown, the multifunctional laboratory spectrometer according to the present invention comprises a ray source assembly 100, a detection assembly 200 and a crystal assembly 300 mounted on a mounting base plate 47, see Figure 59-Figure 62The ray source assembly 100 includes an X-ray source 47 and a first linear moving mechanism that allows the X-ray source 47 to move linearly. The detection assembly 200 includes detectors 85, 109 and a second linear moving mechanism that allows the detectors 85, 109 to move linearly. The crystal assembly 300 includes a spherical curved crystal 128 and a moving table assembly that allows the spherical curved crystal 128 to move linearly and rotate.

[0096] like Figure 8 As shown, the ray source assembly 100 includes an X-ray source related structure 101, a bearing mounting seat 102, a padding plate 103 and a high-precision electric linear translation stage (hereinafter referred to as the translation stage) 104, wherein the X-ray source related structure 101 is rotatably mounted on the translation stage 104 through the bearing mounting seat 102 and the padding plate 103, and the translation stage 104 is mounted on the mounting base plate 47 (see Figure 7 )superior.

[0097] like Fig. 9 As shown, the X-ray source related structure 101 includes an X-ray source assembly 1011, a standard sample mounting assembly 1012, a mounting plate 1013, a translation stage 1014 and a guide assembly 1015, wherein the X-ray source assembly 1011 and the standard sample mounting assembly 1012 are fixedly mounted on the mounting plate 1013, the mounting plate 1013 is mounted on the translation stage 1014, the translation stage 1014 is mounted on the guide assembly 1015, and the guide assembly 1015 is mounted on the bearing mounting seat 102 (see Figure 8 )superior.

[0098] like Fig.10 As shown, the X-ray source assembly 1011 includes a commercial transmission X-ray source (hereinafter referred to as the ray source) 47, a small support plate 48, a small card plate 49, a large support plate 50, a large card plate 51, and a beam limiting cap 52. The opposite ends of the ray source 47 are respectively supported on the small support plate 48 and the large support plate 50. The small card plate 49 is connected to the small support plate 48 and the large card plate 51 is connected to the large support plate 50 to fix the ray source 47. The head area of ​​the ray source 47 extends into the beam limiting cap 52.

[0099] like Fig.11 As shown, the cylindrical surfaces 57 and 58 of the radiation source 47 are placed on the V-shaped surfaces 59 and 60 of the large support plate 50 and the small support plate 48, respectively, and the end surface 61 is against the back surface 62 of the small support plate 48 to complete the installation and positioning of the radiation source 47. The small clamping plate 49 and the large clamping plate 51 are clamped from the upper part of the radiation source 47, and are connected to the small support plate 48 and the large support plate 50 by screws 55 to complete the fixing of the radiation source 47, as shown in FIG. Fig.10 The positioning between the beam limiting cap 52 and the small support plate 48 is completed by the positioning pin 53, and is connected to the small support plate 48 by screws 54, as shown in FIG. Fig.10The beam limiting cap 52 has a circular small hole 63 on the front and a circular blind hole 64 on the back, so that the head region 65 of the radiation source 47 can extend into the blind hole 64. Fig.11 shown.

[0100] like Fig.12 As shown, the standard sample installation assembly 1012 includes a standard sample 66, a mounting seat 67, a base plate 68, a T-shaped limiting member 69 and a shielding plate 70, wherein the standard sample 66 and the T-shaped limiting member 69 are fixedly mounted on the mounting seat 67, the mounting seat 67 is fixedly mounted on the base plate 68, and the shielding plate 70 is fixedly mounted on the base plate 68.

[0101] like Fig.13 As shown, the mounting seat 67 is cylindrical, and a rectangular groove 74 of a certain depth is formed on its top surface 73, and flat surfaces 76 and 78 are formed on its cylindrical surface 75, and threaded holes 77 and 79 are formed respectively. Fig.12 The standard sample 66 is installed in the rectangular groove 74 and is passed through Fig.12 Screw 71 is inserted into Fig.13 The threaded holes 77, 79 in the bracket are used for fixing.

[0102] like Fig.14 and Fig.15 As shown, a tapered through hole 80 is opened in the middle of the T-shaped restraining member 69, and two circular through holes 81 are opened symmetrically at the bottom.

[0103] like Fig.16 As shown, the T-shaped limiter 69 is fixed to the mounting base 67 by a screw gasket assembly 82, the base plate 68 is connected to the mounting base 67 by screws 83, and the shielding plate 70 is fixed to the base plate 68 by a screw gasket assembly 84 to complete the assembly of the entire standard sample mounting assembly 1012.

[0104] The X-ray source assembly 1011 and the standard sample mounting assembly 1012 are positioned with the mounting plate 1013 by means of the positioning pins 1017, and are connected to the mounting plate 1013 by screws 56 and 72, respectively. Fig.17 As shown (it should be noted that in different modes of the present invention, the components installed on the mounting plate 1013 and their positions will be different).

[0105] like Fig.18 As shown, the elevation plate 103 is connected to the displacement platform 104 via screws 107 .

[0106] like Fig.19 As shown, the bearing mounting seat 102 is connected to the padding plate 103 by screws 105 , and the bearing 108 is installed in a circular groove 109 on the bearing mounting seat 102 and connected to the bearing mounting seat 102 by screws 110 .

[0107] like Fig. 20As shown, the guide assembly 1015 includes an adapter plate 10151, a guide plate 10152 and a connecting block 10153, wherein the adapter plate 10151 and the guide plate 10152 are connected by screws 10154.

[0108] like Fig.21 As shown, the connecting block 10153 is connected to the guide plate 10152 by screws 10157, and a U-shaped long groove 10155 is opened on the guide plate 10152.

[0109] like Fig. 22 As shown, the guide assembly 1015 is connected to the bearing 108 by a screw 111 .

[0110] like Fig.23 As shown, the positioning between the translation stage 1014 and the guide assembly 1015 is completed by the positioning pin 1016, and they are connected to each other by the screw 1018.

[0111] like Fig.24 As shown, the mounting plate 1013 is connected to the translation stage 1014 by screws 1019. Fig.17 The X-ray source assembly 1011 and the standard sample mounting assembly 1012 are positioned and mounted on the mounting plate 1013 to complete the overall assembly of the ray source assembly 100. Figure 8 shown.

[0112] like Fig.25 As shown, the detection assembly 200 includes a detector-related structure 201, a bearing mounting seat 202, a padding plate 203, a displacement platform 204 and a bearing 208, wherein the detector-related structure 201 is rotatably mounted on the displacement platform 204 through the bearing mounting seat 202 and the padding plate 203, and the displacement platform 204 is mounted on the mounting base 47 (see FIG. 4 ) through a screw washer assembly 206. Figure 7 )superior.

[0113] like Fig.26 As shown, the detector-related structure 201 includes a silicon drift detector assembly 2011, a surface detector assembly 2012, a mounting plate 2013, a translation stage 2014, a guide assembly 2015 and a sample assembly 2016, wherein the silicon drift detector assembly 2011, the surface detector assembly 2012 and the sample assembly 2016 are fixedly mounted on the mounting plate 2013, the mounting plate 2013 is mounted on the translation stage 2014, the translation stage 2014 is mounted on the guide assembly 2015, and the guide assembly 2015 is mounted on the bearing mounting seat 202 (see Fig.25 )superior.

[0114] like Fig. 27As shown, the silicon drift detector assembly 2011 includes a commercial silicon drift detector 85, a shielding cap 86, a connector 87, a base plate 88 and a support plate 89, wherein the shielding cap 86 is arranged in the head area of ​​the commercial silicon drift detector 85 and is fixedly mounted on the connector 87, the detector 85 and the connector 87 are connected to the base plate 88 by screws 90 and 91 respectively, and the base plate 88 and the two support plates 89 are connected by screws 92 on both sides.

[0115] like Figure 27-Figure 29 As shown in FIG. 1 , a rectangular through hole 95 is formed on the front side 94 of the shielding cap 86, and a circular blind hole 98 is formed on the back side 97 of the shielding cap. The shielding cap is mounted on the connecting member 87 by screws 99. After the shielding cap 86 is mounted, the head region 96 of the detector 85 can extend into the circular blind hole 98 on the back side 97 of the shielding cap 86, as shown in FIG. Fig.28 shown.

[0116] like Fig.30 As shown, the surface detector assembly 2012 includes a commercial surface detector 109, a base plate 110 and a support plate 111, wherein the surface detector 109 is mounted on the base plate 110 by screws 114, and the base plate 110 and the two support plates 111 are positioned by positioning pins 115 (see Fig.32 ) is completed and screwed by screw 113 (see Fig.31 )connect.

[0117] Sample components 2016 can be divided into the following types according to the types of samples being tested: Fig.33 The standard sample installation assembly 20161 shown and Fig.34 The prepared sample mounting assembly 20162 is shown.

[0118] like Fig.33 As shown, the standard sample installation assembly 20161 includes a standard sample 116, a mounting plate 117 and a clamping plate 118, wherein the clamping plate 118 is composed of a screw gasket assembly 122 (see Fig.34 ) is connected to the mounting plate 117, and the standard sample 116 is installed between the mounting plate 117 and the card plate 118.

[0119] like Fig.35 As shown, the sample preparation mounting assembly 20162 includes a magnetic sample holder assembly 119 and a mounting plate 120, wherein the magnetic sample holder assembly 119 is connected to the mounting plate 120 by screws 121. The structure of the magnetic sample holder assembly 119 can be referred to CN202310338245.4, which will not be repeated here.

[0120] like Fig.36As shown, the standard sample mounting assembly 20161 and the prepared sample mounting assembly 20162 are both connected to the commercial magnetic upper plate 124 by screws 123, and are connected to the commercial magnetic lower plate 125 by magnetic force, and are then connected to the mounting plate 2013 by screws 126.

[0121] like Fig.37 As shown, the mounting plate 2013 is connected to the translation stage 2014 by screws 2017 .

[0122] The structures, positioning and installation methods of the displacement platform 204, the raising plate 203, the bearing mounting seat 202, the bearing 208, the guide assembly 2015 and the displacement platform 2014 in the detection assembly 200 are the same as those of the corresponding components in the aforementioned radiation source assembly 100 and will not be repeated here.

[0123] like Fig.38 As shown, the positioning between the silicon drift detector assembly 2011, the surface detector assembly 2012 and the sample assembly 2016 and the mounting plate 2013 is completed by the positioning pin 2018, and the silicon drift detector assembly 2011 and the surface detector assembly 2012 can be combined with different usage modes and connected to the mounting plate 2013 by screw gasket assemblies 93, 112 to complete the overall assembly of the detection assembly 200, such as Fig.25 shown.

[0124] like Fig.39 As shown, the crystal assembly 300 includes a linear translation stage 301, a support assembly 302, a turntable 303, a vertical motion stage 304, a pitch motion stage 305, and a crystal assembly 306, wherein the crystal assembly 306 is rotatably mounted on the support assembly 302 through the turntable 303, the vertical motion stage 304, and the pitch motion stage 305, the support assembly 302 is mounted on the linear translation stage 301, and the linear translation stage 301 is mounted on the mounting base plate 47 (see Figure 7 )superior.

[0125] like Fig.40 As shown, the support assembly 302 includes a rectangular bottom plate 3021, a cylinder 3022, a disk 3023, and screws 3024 and 3025, wherein the rectangular bottom plate 3021 and the cylinder 3022 are connected by screws 3026 (see Fig.41 ), the disc 3023 and the cylinder 3022 are connected by screws 3024, and the rectangular bottom plate 3021 is installed on the linear translation stage 301 by screws 3025. Fig.42 shown.

[0126] like Fig.43 As shown, the positioning between the turntable 303 and the disk 3023 is completed by the positioning pin 307, and is installed on the disk 3023 by the screw 308.

[0127] like Fig.44 As shown, the vertical motion platform 304 is installed on the rotating platform 303 , and the pitch motion platform 305 is installed on the vertical motion platform 304 .

[0128] like Fig.45 As shown, the crystal assembly 306 includes a crystal positioning and mounting assembly 3061, a turntable 3062 and an L-shaped adapter plate 3063, wherein the positioning between the turntable 3062 and the L-shaped adapter plate 3063 is performed by a positioning pin 3064 (see Fig.46 ) and is completed by screw 3065 (see Fig.46 ) Install the turntable 3062 onto the L-shaped adapter plate 3063.

[0129] like Fig.47 As shown, a sheet metal part 3066 is installed on the side 127 of the L-shaped adapter plate 3063 and is fixed by a screw gasket combination 3067.

[0130] like Figure 48-Figure 50 As shown, the crystal positioning and mounting assembly 3061 includes a spherical curved crystal 128, a mounting plate 129 and an L-shaped clamp 131, wherein a circular through hole 134 is opened in the center of the mounting plate 129, the side surface 135 of the spherical curved crystal 128 is placed on the cylindrical surface 136 of the two shoulder screws 130, and the front edge 132 of the spherical curved crystal 128 is attached to the back surface 133 of the mounting plate 129 to complete the positioning of the spherical curved crystal 128 in the crystal assembly 306; four L-shaped clamps 131 are attached to the back surface 137 of the spherical curved crystal 128, and the crystal 128 is gently pressed by the screws 138 to complete its positioning and installation in the crystal assembly 306.

[0131] like Fig.51 As shown, a T-shaped adapter plate 3066 is installed on the surface 139 of the turntable 3062, and the positioning between the T-shaped adapter plate 3066 and the turntable 3062 is completed by the positioning pin 3067, and the T-shaped adapter plate 3066 is connected to the turntable 3062 by the screw 3068.

[0132] like Fig.52 and Fig.53 As shown, both side surfaces 140 of the T-shaped adapter plate 3066 are equipped with connection blocks 3069 , and the bottom is equipped with a connection plate 3070 , and all three are connected to the T-shaped adapter plate 3066 by screws 3071 .

[0133] like Fig.54 As shown, the crystal positioning and mounting assembly 3061 is connected to the connecting blocks 3069 on both sides by screws 3071 to complete the overall assembly of the crystal assembly 306.

[0134] like Fig.55As shown, a rectangular thin plate 309 is installed between the crystal assembly 306 and the pitch motion stage 305, and the crystal assembly 306 and the pitch motion stage 305 are connected by screws 310 to complete the overall assembly of the crystal assembly 300.

[0135] like Fig.56 As shown, the positioning between the radiation source assembly 100, the detection assembly 200, the crystal assembly 300 and the mounting base plate 47 is completed by the positioning pins 141, and they are all fixed to the mounting base plate 47 by the screw gasket combination 142 to complete the entire assembly.

[0136] like Fig.57 As shown, both side surfaces 10156 of the U-shaped groove 10155 of the two guide plates 10152 in the ray source assembly 100 and the detection assembly 200 form a H7 / h7 small clearance fit with the cylindrical surface 120 of the cylinder 3022 of the crystal assembly 300 .

[0137] The following will describe the corresponding optical path direction and component layout of the multifunctional laboratory spectrometer in different modes in combination with different usage modes (spherical curved crystal bevel angle calibration, spherical curved crystal curvature radius measurement, X-ray absorption spectrum acquisition, X-ray emission spectrum acquisition). It should be noted that the focus of the present invention is on structural description and protection, so the spherical curved crystal bevel angle calibration and the curvature radius measurement method will not be described in detail.

[0138] Spherical curved crystal bevel angle calibration mode: Fig.58 As shown, the turntable 303, the vertical motion stage 304, the pitch motion stage 305 and the turntable 3062 in the crystal assembly 300 can respectively enable the spherical curved crystal 128 to have a rotational freedom 148 around the coordinate axis 145, a linear motion freedom 149 along the coordinate axis 145, a rotational freedom 147 around the coordinate axis 144 and a rotational freedom 146 around the coordinate axis 143. The optical path in this mode is as follows Fig.59 As shown, from the perspective of the top view, at a certain Bragg angle 150 (the angle value is related to the material and index surface of the spherical curved crystal 128 used), the incident light 151 emitted by the X-ray source 47 is monochromatized by the spherical curved crystal 128, and its focused reflected light 152 enters the silicon drift detector 85. The size and orientation of the bevel angle of the spherical curved crystal 128 can be measured by combining the adjustment turntable 303, the pitch motion table 305 and the turntable 3062 to record the relevant information of the strongest point of the light intensity signal on the silicon drift detector 85.

[0139] Spherical curved crystal curvature radius measurement mode: In this mode, the optical path is as follows: Fig.60As shown in the top view, at a certain Bragg angle 153 (the angle value is related to the material and index surface of the spherical curved crystal 128 used), the incident light 154 emitted by the X-ray source 47 is monochromatized by the spherical curved crystal 128, and its focused reflected light 155 hits the surface detector 109. Fig. 9 The translation stage 1014 and Fig.26 The displacement stage 2014 is used to find the position on the surface detector 109 where the light spot is the smallest in the plane where the Rowland circle 156 is located, and the curvature radius of the spherical curved crystal 128 can be inferred from the position.

[0140] X-ray absorption spectrum acquisition mode: The optical path in this mode is as follows Fig.61 As shown, from the perspective of the top view, at a certain Bragg angle 157 (the angle value is related to the sample being measured and its specific absorption edge), the incident light 158 ​​emitted by the X-ray source 47 is monochromatized by the spherical curved crystal 128, and its focused reflected light 159 is transmitted through the standard sample mounting assembly 20161 or the prepared sample mounting assembly 20162 and then enters the silicon drift detector 85.

[0141] X-ray emission spectrum acquisition mode: The optical path in this mode is as follows: Fig.62 As shown, from the perspective of the top view, at a certain Bragg angle 160 (the angle value is related to the sample to be tested and its characteristic fluorescence peak), the incident light 161 emitted by the X-ray source 47 hits the sample to be tested 162, and the characteristic fluorescence X-ray 163 excited by it is monochromatized by the spherical curved crystal 128, and its focused reflected light 164 enters the silicon drift detector 85.

[0142] Therefore, the multifunctional laboratory spectrometer according to the present invention can be used for the orientation and measurement of the bevel angle of spherical curved crystals, the measurement of the radius of curvature of spherical curved crystals, and can be used as a collection device for X-ray absorption spectra and emission spectra of different samples under test.

[0143] The above is a detailed introduction to the multifunctional laboratory spectrometer provided by the present invention. The principle, components and different usage modes of the multifunctional laboratory spectrometer are described herein, and the above description is only used to help understand the method and core idea of ​​the present invention. It should be pointed out that for ordinary technicians in this technical field, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention.

Claims

1. A multifunctional laboratory spectrometer, characterized in that: The multifunctional laboratory spectrometer comprises a ray source assembly (100), a detection assembly (200) and a crystal assembly (300). The ray source assembly (100) comprises an X-ray source (47) and a first linear motion mechanism allowing the X-ray source (47) to move. The detection assembly (200) comprises a first detector (85) and a second linear motion mechanism allowing the first detector (85) to move linearly. The crystal assembly (300) comprises a spherical curved crystal (128) and a motion table assembly allowing the spherical curved crystal (128) to move linearly and rotate. The X-ray source (47), the spherical curved crystal (128) and the first detector (85) are precisely linked in a Rowland circle configuration. The first incident light (151) emitted by the X-ray source (47) is monochromatized by the spherical curved crystal (128) and the first focused reflected light (152) is received by the first detector (85) to measure the size and orientation of the bevel angle of the spherical curved crystal (128).

2. The multifunctional laboratory spectrometer according to claim 1, characterized in that: The X-ray source (47) is mounted on a first guide assembly (1015), and the first guide assembly (1015) is mounted on a first bearing mounting seat (102) via a first bearing (108).

3. The multifunctional laboratory spectrometer according to claim 2, characterized in that: The first bearing (108) is installed in the circular groove of the first bearing mounting seat (102), the outer ring of the first bearing (108) is fixedly connected to the first bearing mounting seat (102), and the inner ring of the first bearing (108) is connected to the first guide assembly (1015).

4. The multifunctional laboratory spectrometer according to claim 2, characterized in that: The first detector (85) is mounted on the second guide assembly (2015), and the second guide assembly (2015) is mounted on the second bearing mounting seat (202) via a second bearing (208).

5. The multifunctional laboratory spectrometer according to claim 4, characterized in that: The second bearing (208) is installed in the circular groove of the second bearing mounting seat (202), the outer ring of the second bearing (208) is fixedly connected to the second bearing mounting seat (202), and the inner ring of the second bearing (208) is connected to the second guide assembly (2015).

6. The multifunctional laboratory spectrometer according to claim 4, characterized in that: The crystal assembly (300) has a cylinder (3022), and the first and second guide components (1015, 2015) respectively have a U-shaped long groove (10155), and the two side surfaces of the U-shaped long groove (10155) form a small gap fit with the cylindrical surface of the cylinder (3022).

7. The multifunctional laboratory spectrometer according to claim 1, characterized in that: The first linear motion mechanism comprises a first displacement stage (1014), and the detection assembly (200) further comprises a second detector (109) and a second displacement stage (2014). The second incident light (154) emitted by the X-ray source (47) is monochromatized by the spherical curved crystal (128), and the second focused reflected light (155) is received by the second detector (109). The first displacement stage (1014) and the second displacement stage (2014) are moved in the same direction to measure the radius of curvature of the spherical curved crystal (128).

8. The multifunctional laboratory spectrometer according to claim 1, characterized in that: The detection assembly (200) includes a sample assembly (2016). A third incident light (158) emitted by an X-ray source (47) is monochromatized by a spherical curved crystal (128), and then a third focused reflected light (159) is transmitted through the sample assembly (2016) and received by a first detector (85), so as to collect an absorption spectrum of the sample within an energy range corresponding to a Bragg angle of 54.5° to 85.5°.

9. The multifunctional laboratory spectrometer according to claim 8, characterized in that: The sample assembly (2016) is a standard sample mounting assembly (20161) or a prepared sample mounting assembly (20162).

10. The multifunctional laboratory spectrometer according to claim 1, characterized in that: The ray source assembly (100) also includes a standard sample mounting assembly (1012) for mounting the sample (162) to be tested. The fourth incident light (161) emitted by the X-ray source (47) hits the sample (162) to be tested, and the characteristic fluorescent X-ray (163) excited by the fourth incident light (161) is monochromatized by the spherical curved crystal (128) and then received by the first detector (85). This enables the emission spectrum of the sample to be collected within the energy range corresponding to the Bragg angle of 54.5° to 85.5°.

Citation Information

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