Laboratory spectrometer

Abstract

This invention relates to a laboratory spectrometer, comprising: a base; a motion assembly disposed on the base; a radiation source assembly including an X-ray source and a mounting frame, the mounting frame being fixed to the base and the X-ray source being fixed to the mounting frame; a curved crystal assembly including a spherical curved crystal and a positioning frame, the spherical curved crystal being fixed to the positioning frame and the positioning frame being fixed to the motion assembly; and a detection assembly including a detector and a support frame, the detector being fixed to the support frame and the support frame being fixed to the motion assembly, the support frame also being used to fix a sample; the motion assembly is configured to move the spherical curved crystal, the sample, and the detector so that the X-ray source, the spherical curved crystal, and the sample are always aligned on a Rowland circle. In this laboratory spectrometer, the X-ray source is fixed, and only the spherical curved crystal, the sample, and the detector need to be moved during energy scanning, resulting in a stable optical path.

Description

Technical Field

[0001] This invention relates to the field of X-ray absorption spectroscopy, and more specifically to a laboratory spectrometer. Background Technology

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

[0003] Laboratory spectrometers are analytical instruments based on the Loland circle imaging principle, consisting of components such as an X-ray source, a spherical curved crystal, a detector, and a displacement stage. The displacement stage moves the X-ray source, the spherical curved crystal, the sample, and the detector on the Loland circle to acquire the absorption spectra of different samples within the energy range corresponding to different Bragg angles. This allows for the measurement of the local structural information of the nearest neighbor of different elements (such as the type of coordinating element, valence state, bond length, coordination number, etc.).

[0004] However, existing laboratory spectrometers involve simultaneous movement of the X-ray source, spherical curved crystal, sample, and detector. Due to the large mass of the X-ray source, movement is difficult, and the optical path is unstable. Summary of the Invention

[0005] The purpose of this invention is to provide a laboratory spectrometer in which the X-ray source is fixed, and only the spherical curved crystal, sample and detector need to be moved during energy scanning, thus ensuring a stable optical path.

[0006] To achieve the above objectives, the present invention provides a laboratory spectrometer, comprising:

[0007] Base;

[0008] A motion component is disposed on the base;

[0009] An X-ray source assembly includes an X-ray source and a mounting bracket, wherein the mounting bracket is fixed on the base and the X-ray source is fixed on the mounting bracket;

[0010] A bent crystal assembly includes a spherical bent crystal and a positioning frame, wherein the spherical bent crystal is fixed on the positioning frame, and the positioning frame is fixed on a motion assembly;

[0011] The detection assembly includes a detector and a support frame, wherein the detector is fixed on the support frame, the support frame is fixed on the motion assembly, and the support frame is also used to fix the sample;

[0012] The motion assembly is configured to move the spherical curved crystal, the sample, and the detector so that the X-ray source, the spherical curved crystal, and the sample are always on the Rowland circle.

[0013] Furthermore, the mounting frame includes an L-shaped plate and a base plate. A reinforcing plate is provided on the L-shaped plate. The L-shaped plate includes a horizontal plate and a vertical plate. The vertical plate is fixed on the horizontal plate, the horizontal plate is fixed on the base plate, the base plate is fixed on the base, and the X-ray source is fixed on the vertical plate.

[0014] Furthermore, the bottom of the X-ray source is supported by a support plate, which is fixed to the vertical plate.

[0015] Furthermore, a light-blocking device and a light-absorbing device are sequentially provided at the exit of the X-ray source. The light-blocking device is configured to block the exit of the X-ray source, and the light-absorbing device is configured to absorb the fluorescence and scattering of X-rays near the exit of the X-ray source.

[0016] Furthermore, the motion assembly includes a first linear displacement stage, a second linear displacement stage, a third linear displacement stage, a linkage mechanism, a first rotary displacement stage, and an attitude adjustment displacement stage. The first and second linear displacement stages are both fixed to the base. The first linear displacement stage faces the X-ray source, and the second linear displacement stage forms an angle with the first linear displacement stage. The two ends of the linkage mechanism are respectively located on the first and second linear displacement stages. The linkage mechanism can slide and rotate relative to the first linear displacement stage, and it can also rotate relative to the second linear displacement stage. The first rotary displacement stage is fixed to one end of the linkage mechanism, and the third linear displacement stage is fixed to the other end of the linkage mechanism. The attitude adjustment displacement stage is disposed on the first rotary displacement stage, the bending crystal assembly is fixed on the attitude adjustment displacement stage, and the detection assembly is fixed on the third linear displacement stage.

[0017] Furthermore, the linkage mechanism includes a first connecting plate and a second connecting plate connected to each other. A rotating bracket is fixed on the first linear displacement stage, and a first driven turntable is fixed on the rotating bracket. A slider bracket is provided on the first driven turntable, and the slider bracket is slidably connected to the first connecting plate. The first rotary displacement stage is fixed on the rotating bracket. A shim is provided on the second linear displacement stage, and a second driven turntable is provided on the shim. The second connecting plate is located on the second driven turntable, and the third linear displacement stage is located on the second connecting plate.

[0018] Furthermore, the rotating bracket includes a rotating base, a rotating shaft, and a mounting base. The two ends of the rotating shaft are connected to the rotating base and the mounting base, respectively. The first driven turntable is fixed on the rotating base, the rotating base is fixed on the first linear displacement platform, and the first rotary displacement platform is fixed on the mounting base. The first connecting plate is provided with a sliding groove, the rotating shaft passes through the sliding groove and the first driven turntable, and the rotating base and the mounting base are located above and below the first connecting plate, respectively.

[0019] Furthermore, the attitude adjustment displacement stage includes a fourth linear displacement stage and a second rotary displacement stage, the second rotary displacement stage is disposed on the fourth linear displacement stage, the fourth linear displacement stage is disposed on the first rotary displacement stage, and the bent crystal assembly is disposed on the second rotary displacement stage.

[0020] Furthermore, the positioning frame includes a positioning base and a positioning ring. The positioning base is fixed on the motion component, the positioning ring is fixed on the positioning base, the spherical curved crystal is inserted into the positioning ring, and the positioning ring is provided with a screw cap.

[0021] Furthermore, the support frame includes a support base, a sample holder, and a detector support mechanism. The sample holder and the detector support mechanism are fixed on the support base, the support base is fixed on the motion component, the sample is fixed on the sample holder, and the detector is fixed on the detector support mechanism.

[0022] Furthermore, the sample holder includes an adapter plate, a fixing plate is fixed on the adapter plate, a cover plate and a magnetic component are provided on the fixing plate, the magnetic component attracts the cover plate to the fixing plate, and the sample is clamped between the magnetic component and the cover plate; the magnetic component, the cover plate, the fixing plate and the adapter plate are all provided with through holes.

[0023] Furthermore, the magnetic component has a protrusion on the side near the cover plate, and the protrusion has a receiving groove to accommodate the sample; both the cover plate and the fixing plate have grooves, the groove of the fixing plate is used to accommodate the cover plate, and the groove of the cover plate is used to accommodate the protrusion.

[0024] Furthermore, the detector support mechanism includes two opposing support members, on which an insulating base plate is provided. The insulating base plate is fixed on the two support members, and the detector is fixed on the insulating base plate and located behind the sample.

[0025] Furthermore, a protective cover is provided at the end of the detector, the protective cover has holes, and the protective cover is fixed to the insulating base.

[0026] Furthermore, the base is provided with multiple lifting rings and multiple fasteners.

[0027] Furthermore, it also includes a helium storage device fixed on the base, the helium storage device storing helium.

[0028] Furthermore, the helium storage device includes a box body, which includes an upper cover plate, a lower cover plate, and a first side plate, a second side plate, a third side plate, a fourth side plate, and a fifth side plate connected end to end in sequence. The upper cover plate is connected to the upper end of each side plate, and the lower cover plate is connected to the lower end of each side plate. The box body stores helium gas. The first side plate has a first opening, the third side plate has a second opening, and the fourth side plate has a third opening. The first opening, the second opening, and the third opening are all sealed with tape to create a sealed environment inside the box body.

[0029] Furthermore, it also includes an air inlet pipe and an air outlet pipe, both of which are connected to the interior of the housing.

[0030] Furthermore, the helium storage device also includes a support mechanism, the housing is fixed on the support mechanism, and the support mechanism is fixed on the base.

[0031] The laboratory spectrometer of this invention fixes the X-ray source on a base and moves the spherical curved crystal, sample and detector through a motion component, so that the X-ray source, spherical curved crystal and sample are always on the Rowland circle. Since the X-ray source does not need to move, the optical path is stable. Attached Figure Description

[0032] Figure 1 A schematic diagram of the Rowland circle of a laboratory spectrometer according to an embodiment of the present invention;

[0033] Figure 2 This is a schematic diagram of the structure of a laboratory spectrometer according to an embodiment of the present invention;

[0034] Figure 3A This is a schematic diagram of the structure of the X-ray source assembly of a laboratory spectrometer according to an embodiment of the present invention;

[0035] Figure 3B This is a schematic diagram of the mounting bracket for the X-ray source assembly according to an embodiment of the present invention;

[0036] Figure 3C This is a schematic diagram of the L-shaped frame of the X-ray source assembly according to an embodiment of the present invention;

[0037] Figure 3D This is a schematic diagram from another perspective of the mounting bracket for the X-ray source assembly according to an embodiment of the present invention;

[0038] Figure 3E This is a cross-sectional view of the X-ray source, light-blocking device, and light-absorbing device according to an embodiment of the present invention;

[0039] Figure 3F This is a schematic diagram of the structure of a light-absorbing device according to an embodiment of the present invention;

[0040] Figure 3G This is a schematic diagram of the structure of the X-ray source, light-blocking device, and light-absorbing device according to an embodiment of the present invention;

[0041] Figure 3H This is a cross-sectional view of the aperture of the light-absorbing device according to an embodiment of the present invention;

[0042] Figure 4A This is a schematic diagram of the structure of a motion component according to an embodiment of the present invention;

[0043] Figure 4B This is a schematic diagram of the linkage mechanism of the motion component according to an embodiment of the present invention;

[0044] Figure 4C This is a schematic diagram of the structure of the rotating support of the linkage mechanism according to an embodiment of the present invention;

[0045] Figure 4D This is a schematic diagram of the structure of the first driven turntable of the linkage mechanism according to an embodiment of the present invention;

[0046] Figure 4E This is a schematic diagram of the posture adjustment displacement stage of the motion component according to an embodiment of the present invention;

[0047] Figure 5 This is a schematic diagram of the structure of a bent crystal assembly according to an embodiment of the present invention;

[0048] Figure 6A This is a schematic diagram of the structure of the detection component according to an embodiment of the present invention;

[0049] Figure 6B A cross-sectional view of a sample holder according to an embodiment of the present invention;

[0050] Figure 6C This is a schematic diagram of the detection component according to an embodiment of the present invention from another perspective;

[0051] Figure 6D This is a top view of the detection component according to an embodiment of the present invention;

[0052] Figure 7 This is a schematic diagram of the structure of the base according to an embodiment of the present invention;

[0053] Figure 8A This is a schematic diagram of a helium storage device according to an embodiment of the present invention;

[0054] Figure 8B This is a side view of the housing of a helium storage device according to an embodiment of the present invention;

[0055] Figure 8C This is a structural schematic diagram of the box body from another perspective according to an embodiment of the present invention;

[0056] Figure 8D This is a schematic diagram of the structure of the box body and support mechanism according to an embodiment of the present invention;

[0057] Figure 8E This is a schematic diagram of the optical path of a helium storage device according to an embodiment of the present invention during use. Detailed Implementation

[0058] The preferred embodiments of the present invention are given below with reference to the accompanying drawings and described in detail.

[0059] This invention provides a laboratory spectrometer comprising an X-ray source, a spherical curved crystal, and a detector. The X-ray source is fixed, while the spherical curved crystal, the sample, and the detector are moved to ensure that the X-ray source, the spherical curved crystal, and the sample remain on a Rowland circle. Figure 1 As shown, the X-ray source point P1, the geometric center P2 of the spherical curved crystal, and the geometric center P3 of the sample surface are always on a Rowland circle with a diameter of Rc, where Rc is the radius of curvature of the spherical curved crystal. Thus, the incident X-ray beam, after being monochromated by the spherical curved crystal, is transmitted to the sample and received by the subsequent detector. The angle between the incident beam and the normal to the spherical curved crystal is the Bragg angle θ; changing this angle changes the energy used for scanning. The distance between the source point P1 and the geometric center P2 of the spherical curved crystal is P1P2 = Rc·sinθ, and the distance between the source point P1 and the geometric center P3 of the sample surface is P1P3 = Rc·sinθcosθ. Since Rc is the radius of curvature of the spherical curved crystal, its size is fixed once the spherical curved crystal is determined. Therefore, the values ​​of P1P2 and P1P3 are related to θ; when θ changes, the values ​​of P1P2 and P1P3 also need to change accordingly. In this invention, θ = 55°-82°, and the spherical curved crystal, sample and detector can move simultaneously to satisfy the above distance relationship at different θ values.

[0060] like Figure 2As shown, the laboratory spectrometer includes a radiation source assembly 100, a curved crystal assembly 200, a detector assembly 300, a motion assembly 400, and a base 500. The radiation source assembly 100 includes an X-ray source 101 and a mounting frame 102, with the mounting frame 102 fixed to the base 500 and the X-ray source 101 fixed to the mounting frame 102. The curved crystal assembly 200 includes a spherical curved crystal 201 and a positioning frame 202, with the positioning frame 102 fixed to the motion assembly 400 and the spherical curved crystal 201 fixed to the positioning frame 202. The detector assembly 300 includes a detector 301. The support frame 302 is fixed on the motion component 400, and the sample and detector 301 are fixed on the support frame 302. The motion component 400 is mounted on the base 500. The motion component 400 can make the spherical curved crystal 201, the sample and the detector 301 move simultaneously, so that the X-ray source 101, the spherical curved crystal 201 and the sample are always located on the Rowland circle with a diameter equal to the radius of curvature of the spherical curved crystal 201. The incident beam emitted by the X-ray source 101 is monochromated by the spherical curved crystal 201 and transmitted to the sample and received by the detector 301.

[0061] like Figure 3A and Figure 3B As shown, the mounting bracket 102 includes an L-shaped plate 103 and a base plate 104, as... Figure 3C As shown, the L-shaped plate 103 includes a horizontal plate 105 and a vertical plate 106 welded together. A reinforcing plate 107 is also welded to the L-shaped plate 103. The bottom surface of the reinforcing plate 107 is welded to the horizontal plate 105, and the side surface of the reinforcing plate 107 is welded to the vertical plate 106, thereby increasing the stability of the L-shaped plate 103. The horizontal plate 105 can be detachably connected to the base plate 104 by multiple M8x25 socket head cap screws 108. The base plate 104 can be detachably connected to the base 500 by multiple M6x16 socket head cap screws 109. The X-ray source 101 can be an existing X-ray source device, such as the standard XRD type X-ray source model 3003 from XRD Eigenmann GmbH, the specific structure and principle of which will not be described here. The X-ray source 101 can be fixed to the vertical plate 106 by multiple M6x25 socket head cap screws 110. A support plate 111 may also be provided at the bottom of the X-ray source 101 to provide auxiliary support for the X-ray source 101. The end of the support plate 111 is fixed to the vertical plate 106 by screws.

[0062] Since the mounting positions of the X-ray source 101 on the vertical plate 106 and the horizontal plate 105 on the base plate 104 determine the final position of the X-ray source 101 on the base 500, multiple positioning pins 112 can be provided on the vertical plate 106 to position the X-ray source 101 on the vertical plate 106, and multiple positioning pins 113 can be provided on the base plate 104 to position the horizontal plate 105. The installation of the X-ray source assembly 100 can be completed quickly using the positioning pins 112 and 113.

[0063] The installation process of the X-ray source assembly 100 is as follows:

[0064] First, fix the base plate 104 to the base 500 using screws 109. Then, place the horizontal plate 105 of the L-shaped frame 103 on the base plate 104, ensuring that one side of the horizontal plate 105 contacts the two rightmost locating pins 113 of the base plate 104. Figure 3D As shown; then, the horizontal plate 105 and the base plate 104 are fixed with screws 108; then, the X-ray source 101 is moved to the position defined by the positioning pins 112 of the vertical plate 106, so that the bottom surface of the X-ray source 101 contacts the two positioning pins 112 on the lower side, and the side of the X-ray source 101 contacts the positioning pin 112 on the right side. Then, the X-ray source 101 is fixed to the vertical plate 106 with screws 110; then, the support plate 111 is placed at the bottom of the X-ray source 101 and attached to it, and the support plate 111 is fixed to the vertical plate 106 with screws, thereby providing auxiliary support for the X-ray source 101. If optical aberrations are found to cause spectral energy broadening during absorption spectrum acquisition, the X-ray source 101 can be switched to a position closer to the inside of the Rowland circle (generally a few millimeters away from the circumference of the Rowland circle). Specifically, screw 108 can be loosened, and then the horizontal plate 105 can be moved to contact the two rightmost locating pins 113 on the base plate 104. Then, screw 108 can be tightened (solid grease can be applied to the bottom surface of the horizontal plate 105 to facilitate movement). The X-ray source 101 is located inside the Rowland circle, which can reduce the size of the virtual light source on the Rowland circle, thereby reducing spectral energy broadening and improving the energy resolution of the entire scanning mechanism.

[0065] Continue to refer to Figure 3A In some embodiments, a light-blocking device 114 and a light-absorbing device 115 are sequentially provided at the exit of the X-ray source 101. The light-blocking device 114 is used to block the exit of the X-ray source 101 as needed during the measurement process to prevent X-rays from irradiating the experimental personnel. The light-absorbing device 115 is used to absorb fluorescence and scattering near the exit of the X-ray source 101 to avoid affecting the detector of the laboratory spectrometer.

[0066] The light-blocking device 114 includes a shielding block 116 and a shutter 117, such as Figure 3EAs shown, the shielding block 116 has a protrusion 118 with a through hole 119. The shielding block 116 is fixed to the X-ray source 101, and one end of the protrusion 118 extends into the oblong hole on the turntable 120 at the exit of the X-ray source 101, while the other end extends into the light-transmitting hole 121 of the shutter 117. The shutter 117 can be a standard optical shutter of the existing model FS25, the structure and principle of which will not be described here.

[0067] The shielding block 116 and the shutter 117's outer shell and baffle are both made of copper with a thickness of not less than 3 mm, so that when the shutter is closed, the leakage rate of X-rays emitted by the X-ray source 101 under the highest voltage of 45 kV can be controlled within the range of <1 μSv / h, so as to ensure that the experimental personnel are protected from radiation damage.

[0068] The shutter 117 can be mounted on the X-ray source 101 via the L-shaped connecting plate 122. Specifically, the vertical plate of the L-shaped connecting plate 122 is fixedly connected to the X-ray source 101, and the horizontal plate of the L-shaped connecting plate 122 is fixedly connected to the housing of the shutter 117, thereby fixing the shutter 117 on the X-ray source 101.

[0069] like Figure 3F As shown, the light-absorbing device 115 includes an aperture 123, a first clamping block 124, and a second clamping block 125. The aperture 123 is clamped between the first clamping block 124 and the second clamping block 125, and the first clamping block 124 and the second clamping block 125 are fixedly connected by screws. The bottom of the second clamping block 125 is connected to the fixing plate 126, as shown. Figure 3G As shown, the fixing plate 126 is fixed to the shielding block 116, so that the aperture 123 is located at the light-transmitting hole 121 of the shutter 117. Multiple positioning pins 127 can be provided on the shielding block 116 for positioning the fixing plate 126, so that when the fixing plate 126 is fixed to the shielding block 116, the aperture 123 is exactly located at the light-transmitting hole 121 of the shutter 117.

[0070] like Figure 3H As shown, the aperture 123 consists of an inner ring 128 and an outer ring 129. The inner ring 128 is made of pure aluminum (1060) and is responsible for absorbing the fluorescence generated when X-rays pass through the region. The outer ring 129 is made of copper and is used to absorb the scattered light generated when X-rays pass through the region. The inner diameters of the inner ring 128 and the outer ring 129 are matched and assembled with a small gap of H8 / h7.

[0071] To prevent X-ray leakage, such as Figure 3E As shown, part of the aperture 123 needs to extend into the light-transmitting hole 121 of the shutter 117.

[0072] X-ray source 101 can be an XRD source of model 3003 from XRD Eigenmann GmbH, which emits X-rays such as Figure 3E As shown, P1 is the light source point, L is the beam center, and the focal spot size at the light source point P1 is 0.8 mm. 2 The beam center L makes an angle of α = 6° with the Y-axis in the clockwise direction in the horizontal plane. The spatial divergence angle of the X-ray beam symmetrical about the beam center L is c = 5.9°, and the angle between the beam center L and the beam edge is b = 2.95°. When the shutter 117 is open, X-rays can be emitted from the aperture 123 without being blocked by the light-blocking device 114 or the light-absorbing device 115, thus not affecting the normal use of the X-ray source 101. When the shutter 117 is closed, the X-rays will be blocked and cannot be emitted, thereby preventing the experimenters from being exposed to radiation.

[0073] like Figure 4A As shown, the motion assembly 400 includes a first linear displacement stage 401, a second linear displacement stage 402, a third linear displacement stage 403, a linkage mechanism 404, a first rotary displacement stage 405, and an attitude adjustment displacement stage 406. The first linear displacement stage 401 and the second linear displacement stage 402 are both fixed to the base 500. The first linear displacement stage 401 faces the light source point of the X-ray source 101, i.e., the first linear displacement stage 401 is along the direction of the incident beam. The second linear displacement stage 402 is set at an angle to the first linear displacement stage 401, which can be 40°-70°. The two ends of the linkage mechanism 404 are respectively located on the first linear displacement stage 401 and the second linear displacement stage 402, and can rotate relative to the first linear displacement stage 401 and the second linear displacement stage 402. Thus, the two ends of the linkage mechanism 404 can move along the first linear displacement stage 401 and the second linear displacement stage 402, respectively. And there will be no interference; the first rotary displacement stage 405 is fixed at one end of the linkage mechanism 404, the third linear displacement stage 403 is fixed at the other end of the linkage mechanism 404, the attitude adjustment displacement stage 406 is set on the first rotary displacement stage 405, and the bent crystal assembly 200 is fixed on the attitude adjustment displacement stage 406. The first rotary displacement stage 405 can make the attitude adjustment displacement stage 406 and the bent crystal assembly 200 rotate, thereby changing the size of the Bragg angle. The attitude adjustment displacement stage 406 is used to adjust the geometric center height and the lattice plane oblique angle normal vector of the spherical bent crystal 201, so that the geometric center height and the lattice plane oblique angle normal vector of the spherical bent crystal 201 are both located in the plane of the Rowland circle, so as to obtain better diffraction efficiency; the detector assembly 300 is fixed on the third linear displacement stage 403, and the distance between the sample and the detector 301 and the spherical bent crystal 201 can be moved through the third linear displacement stage 403.

[0074] like Figure 4BAs shown, the linkage mechanism 404 includes a first connecting plate 407 and a second connecting plate 408 that are connected to each other. A slide rail 421 is provided on the first connecting plate 407. The slide rail 421 is slidably engaged with the slider 409. The slider 409 is mounted on the slider bracket 410. The slider bracket 410 is fixed on the first driven turntable 412. The first driven turntable 412 is fixed on the rotating bracket 411. The rotating bracket 411 is fixed on the first linear displacement stage 401.

[0075] like Figure 4C As shown, the rotating bracket 411 includes a rotating base 413, a rotating shaft 414, and a mounting base 415. The two ends of the rotating shaft 414 are connected to the rotating base 413 and the mounting base 415, respectively. The first rotating displacement stage 405 is fixed to the mounting base 415. A sliding groove 416 is provided on the first connecting plate 407, through which the rotating shaft 414 passes. The rotating base 413 and the mounting base 415 are located above and below the first connecting plate 407, respectively. Thus, the rotating bracket 411 can slide relative to the first connecting plate 407 along the direction of the sliding groove 416.

[0076] like Figure 4D As shown, the first driven turntable 412 includes a turntable base 417 and a rotary table 418 mounted on the turntable base 417. The rotary table 418 can rotate 360° on the turntable base 417. During installation, the pivot 414 of the rotating bracket 411 passes through the first driven turntable 412, and the turntable base 417 is fixed to the rotating base 413 of the rotating bracket 411. The slider bracket 410 is fixed to the turntable 418. In this way, the slider bracket 410 can follow the turntable 418 and rotate around the pivot 414 on the turntable base 417. The first driven turntable 412 can be a rotary platform of model RM16A-C1 from KOHZU Corporation, the structure and principle of which will not be described in detail here.

[0077] The second connecting plate 408 is mounted on the second driven turntable 419, which is fixed to the shim block 420, which is fixed to the second linear displacement stage 402. The structure of the second driven turntable 419 is the same as that of the first driven turntable 412. The second connecting plate 408 can be fixed to the rotating platform of the second driven turntable 419, and the base of the turntable 419 is fixed to the shim block 420, thereby allowing the second connecting plate 408 to rotate relative to the second linear displacement stage 402. By setting the rotating bracket 411 and the shim block 420, the spherical curved crystal 201 and the sample and detector 301 can be at the same height. When the first linear displacement stage 401 and the second linear displacement stage 402 are working, the first driven turntable 412 and the rotating bracket 411 will move along the first linear displacement stage 401, and the shim block 420, the second driven turntable 419 and the second connecting plate 408 will move along the second linear displacement stage 402. Since the first connecting plate 407 and the second connecting plate 408 are connected, the first connecting plate 407 and the slider bracket 410 will rotate relative to the first linear displacement stage 401, and the second connecting plate 408 will rotate relative to the second linear displacement stage 402 to avoid motion interference.

[0078] like Figure 4E As shown, the attitude adjustment stage 406 includes a fourth linear stage 422 and a second rotary stage 423. The second rotary stage 423 is fixed on the fourth linear stage 422, and the fourth linear stage 422 is fixed on the first rotary stage 405. The bent crystal assembly 200 is fixed on the second rotary stage 423. The fourth linear stage 422 is used to adjust the geometric center height of the spherical bent crystal 201, and the second rotary stage 423 is used to adjust the lattice bevel angle normal vector.

[0079] In an exemplary embodiment, the first linear displacement stage 401 can be a "XA16F-L2201-modified" linear displacement stage with a stroke of 200 mm and a full step resolution of 10 μm, used for the linear movement of the spherical bent crystal along the X-ray incident light direction during energy scanning. The second linear displacement stage 402 can be a "XA16F-L2301-modified" linear displacement stage with a stroke of 330 mm and a full step resolution of 4 μm. The third linear displacement stage 403 is of the same model as the first linear displacement stage 401. The first rotary stage 405 can be a model "RA07A-W02-modified" rotary stage with a travel distance of 270° and a full step resolution of 14.4″, used for adjusting the Bragg angle of the spherical bent crystal during energy scanning. To ensure motion repeatability during energy scanning, the first linear stage 401, the second linear stage 402, the third linear stage 403, and the first rotary stage 405 are all equipped with a TONIC series incremental encoder system from Renishaw, UK. The encoder resolutions of the first linear stage 401, the second linear stage 402, and the third linear stage 403 are all 0.1μm, while the encoder resolution of the first rotary stage 405 is 0.6″. The fourth linear stage 422 can be a model "ZA05A-W2C01" linear stage with a travel distance of 3mm and a full step resolution of 0.5μm. The second rotary stage 423 can be a rotary stage of model "SA05A-R2M01", with a stroke of 9° and a full step resolution of 5.76″.

[0080] During energy scanning, the Bragg angle can be changed via the first rotary displacement stage 405, and then adjusted through the coordination of the first linear displacement stage 401, the second linear displacement stage 402, and the third linear displacement stage 403. Figure 1 The distances between P1P2 and P1P3 shown are such that P1P2 = Rc·sinθ and P1P3 = Rc·sinθcosθ, thus ensuring that the X-ray source 101, the spherical curved crystal 201, and the sample are always on the Rowland circle. The specific adjustment process can be implemented through programming, i.e., by inputting the pre-written program into the control system of each displacement stage, and then achieving automatic control.

[0081] like Figure 5As shown, the bending crystal assembly 200 includes a spherical bending crystal 201 and a positioning frame 202. The positioning frame 202 includes a positioning base 203 and a positioning ring 204 fixed to the positioning base 203. The positioning base 203 is fixed to the attitude adjustment displacement stage 406 of the motion assembly 400 by multiple M3x10 socket head cap screws 205. The positioning ring 204 is used to accommodate the spherical bending crystal 201. After the spherical bending crystal 201 is engaged with the positioning ring 204, the edge of the front side (i.e., the working surface) of the spherical bending crystal 201 is in contact with the inner surface of the positioning ring 204. A cap 206 is provided on the side of the positioning ring 204 near the back side of the spherical bending crystal 201 to prevent the spherical bending crystal 201 from coming out from that side. The cap 206 can be threadedly connected to the positioning ring 204 so that it can be tightened or loosened by rotation. An M6x13 socket head cap screw 207 can be installed on the top of the positioning ring 204. After the spherical bent crystal 201 is installed into the positioning ring 204, the screw 207 is rotated to make it press against the side (i.e., the circumferential surface) of the spherical bent crystal 201, thereby positioning it.

[0082] A boss may be formed on the positioning base 203, and the front side of the positioning ring 204 (the side closest to the front of the spherical bent crystal 201) is in close contact with the boss. A stop 208 may also be provided on the positioning base 203, which is in close contact with the rear side of the positioning ring (i.e., the side opposite to the front side or the side closest to the back of the spherical bent crystal 201). The stop 208 is fixed to the positioning base 203 by two M3x8 beveled hex socket head cap screws 209, thus confining the positioning ring 204 between the boss and the stop 208. The positioning ring 204 can be fixedly connected to the positioning base 203 by M5x10 hex socket head cap screws 210.

[0083] like Figure 6A As shown, the support frame 302 includes a support base 303, a sample holder 304, and a detector support mechanism 305. The sample holder 304 includes an adapter plate 306, which is fixed to the support base 303. A fixing plate 307 is provided on the adapter plate 306, which is fixed to the adapter plate 306 by multiple M2.5x8 stainless steel hexagon socket head cap screws 308. A cover plate 309 and a magnetic component 310 are provided on the fixing plate 307. The magnetic component 310 attracts the cover plate 309 to the fixing plate 307, and the sample 311 is sandwiched between the magnetic component 310 and the cover plate 309 and fixed by the attraction force of the magnetic component 310.

[0084] like Figure 6BAs shown, a groove may be provided on the fixing plate 307, and the cover plate 309 is installed in the groove to position the cover plate 309. A groove may also be provided on the cover plate 309, and a protrusion may be provided on the magnetic component 310. The protrusion of the magnetic component 310 can be inserted into the groove of the cover plate 309 to achieve positioning of the two. A receiving groove may be provided on the protrusion of the magnetic component 310 to accommodate the sample 311. After the sample 311 is placed in the receiving groove, the protrusion of the magnetic component 310 is inserted into the groove of the cover plate 309, and then the cover plate 309 is placed into the groove of the fixing plate 307 as a whole. Under the adsorption force of the magnetic component 310, the magnetic component 310, the sample 311, and the cover plate 309 will be fixed on the fixing plate 307, thereby completing the installation of the sample 311. When sample 311 needs to be replaced, simply remove the magnetic component 310, sample 311, and cover plate 309 from the fixing plate 307, then replace sample 311. After replacement, reinstall them on the fixing plate 307. The adapter plate 306, fixing plate 307, cover plate 309, and magnetic component 310 are all provided with through holes for X-rays to pass through. This allows X-rays to smoothly reach detector 301 after passing through sample 311.

[0085] Continue to refer to Figure 6A The detector support mechanism 305 includes two opposing support members 312, on which an insulating base plate 313 is mounted. The base plate 313 is fixed to the support members 312 by multiple M4x12 hexagon socket head cap screws 314. The detector 301 is fixed to the insulating base plate 313 by multiple M3x12 hexagon socket head cap screws 315. The detector 301 can be an AXAS-M H150 silicon drift detector from KETEK GmbH, Germany, with an energy resolution better than 136 eV. A protective cover 316 is provided at the end of the detector 301, with a 5mm × 12mm rectangular hole. All surfaces of the rectangular hole must be polished to a surface roughness of 0.8 Ra. The protective cover 316 is made of tungsten and its function is to absorb stray light in front of the detector 301 and shape the monochromatic light entering the detector 301, thereby improving the data acquisition quality of the detector 301. Figure 6C and Figure 6D As shown, the protective cover 316 is fixedly connected to the connecting plate 318 by multiple M2.5x10 socket head cap screws 317, and the connecting plate 318 is fixed to the insulating base plate 313 by multiple M3x10 socket head cap screws 319. Both the connecting plate 318 and the insulating base plate 313 are made of polyetheretherketone (PEEK) material to achieve electrical insulation of the detector 301, thereby improving the signal-to-noise ratio during data acquisition. Both support members 312 can be fixed to the support base 303 by multiple M4x16 socket head cap screws 320.

[0086] Since the detector 301 needs to be positioned directly behind the sample 311 after installation to receive X-rays transmitted through the sample, the installation positions of the adapter plate 306 and the detector support mechanism 305 can be pre-positioned on the support base 303. Specifically, the adapter plate 306 can be fixed to the first magnetic base 322 by multiple M6x16 socket head cap screws 321. The first magnetic base 322 is attached to the second magnetic base 323, which in turn is attached to the support base 303. The first magnetic base 322 and the second magnetic base 323 can be magnetic bases of model KBT50M and KBB50M from THORLABS, USA, respectively. The position of the second magnetic base 320 on the support base 303 can be positioned by three positioning pins 324 of model MSVC5-25. In this way, after installation, the detector 301 can be positioned directly behind the sample 311.

[0087] The support base plate 303 is fixed to the third linear displacement stage 403 of the motion assembly 400 by multiple M5x16 socket head cap screws 325, thereby adjusting the position of the sample and detector 301 through the motion assembly 400.

[0088] like Figure 7 As shown, the base 500 is provided with multiple lifting rings 501 and multiple fasteners 502. The lifting rings 501 facilitate the hoisting operation of the base 500 and its components. One end of the fastener 502 is fixed to the base 500 by an M6x10 socket head cap screw 503, and the other end is fixedly connected to the aluminum profile frame of the laboratory (not shown in the figure) by an M6x12 socket head cap screw 504 to complete the installation of the base 500 in the laboratory.

[0089] The fastener 502 can be a Z-shaped structure made of three plates welded together in sequence, and its material is 6061 aluminum alloy.

[0090] The base 500 may be equipped with positioning pins for precise positioning of the X-ray source assembly 100 and the motion assembly 400 to ensure installation accuracy.

[0091] Continue to refer to Figure 2 The base 500 is also equipped with a helium storage device 600, which is located in the X-ray propagation path. The helium storage device 600 stores helium, which has a small mass number and absorbs X-rays much less than air. Therefore, setting the helium storage device 600 in the X-ray propagation path can reduce the scattering and absorption of X-rays by air, thereby improving the received light intensity of the detector 301.

[0092] like Figure 8AAs shown, the helium storage device 600 includes a housing 601, an inlet pipe 602, and an outlet pipe 603. Both the inlet pipe 602 and the outlet pipe 603 are connected to the interior of the housing 601, thereby allowing helium to enter or exit.

[0093] The intake pipe 602 includes an integral needle valve with a φ6mm diameter cap 604, a φ6mm diameter compression fitting right-angle connector 605, a φ6mm diameter compression fitting tee connector 606, and a φ6mm diameter compression fitting low-pressure unloading valve 607. The inlet of the needle valve 604 is connected to a helium source (not shown in the figure), and the outlet is connected to the first port of the tee connector 606 via a connecting pipe. The second port of the tee connector 606 is connected to the unloading valve 607 via a copper pipe, and the third port of the tee connector 606 is connected to the first port of the right-angle connector 605 via a copper pipe. The second port of the right-angle connector 605 is connected to the interior of the housing 601 to introduce helium into the housing 601. The unloading valve 607 is manufactured with the working pressure of the internal spring set to 1.5 bar. This ensures that if the helium pressure inside the housing 601 exceeds 1.5 bar, the unloading valve 607 will automatically open to release gas, preventing excessive pressure inside the housing 601.

[0094] The exhaust pipe 603 includes an integral valve cap needle valve 608 with a diameter of φ6mm and a compression right-angle connector 609 with a diameter of φ6mm. The inlet of the needle valve 608 is connected to the first interface of the right-angle connector 609 through a copper pipe. The second interface of the right-angle connector 609 is connected to the inside of the housing 601. The outlet of the needle valve 608 is connected to the outside, thereby exhausting the helium gas inside the housing 601 through the exhaust pipe 603.

[0095] like Figure 8B and 8C As shown, the box body 601 includes a first side plate 610, a second side plate 611, a third side plate 612, a fourth side plate 613, and a fifth side plate 614 connected end to end. The box body 601 also includes an upper cover plate 615 and a lower cover plate 616, which are respectively connected to the upper and lower ends of each side plate, thus forming a box structure. The first side plate 610 has a first opening 617, the third side plate 612 has a second opening 618, and the fourth side plate 613 has a third opening 619. The first opening 617 is connected by 0.01mm thick polyimide tape 620 (see...). Figure 8AThe second opening 618 and the third opening 619 can also be sealed with 0.01mm thick polyimide tape. This ensures a sealed environment inside the box 601 while allowing X-rays to pass through the tape and through the box 601. Both the second side plate 611 and the top cover 615 are equipped with connectors 621. The connector 621 on the second side plate 611 connects to the second interface of the right-angle connector 609 of the exhaust pipe 603, and the connector 621 on the top cover 615 connects to the second interface of the right-angle connector 605 of the intake pipe 602. This allows air to enter through the top cover 615 and exit through the second side plate 611.

[0096] To mount the helium storage device 600 onto the base 500 without interfering with other components, the housing 601 needs to be mounted onto the base 500 via a support mechanism 622. Figure 8D As shown, the helium storage device 600 also includes a support mechanism 622. The housing 601 is fixed to the support mechanism 622, which in turn is fixed to the base 500. The support mechanism 622 includes four support rods 623 and a support plate 624. The support plate 624 is fixed to the support rods 623, and the housing 601 is fixed to the support plate 624. Each support rod 623 can be distributed at one of the four corners of the support plate 624 and fixed to the support plate 624 by M8x20 socket head cap screws 625. The bottom of the support rod 623 can be threaded, thereby fixing it to the base 500 by threaded connection.

[0097] like Figure 8EAs shown, during use, the fourth side plate 613 of the helium storage device 600 faces the X-ray source 101, the first side plate 610 faces the spherical curved crystal 201, and the third side plate 612 faces the sample and detector. Thus, when the Bragg angle is 55°, the incident beam L1 passes through the tape at the third opening 619 on the fourth side plate 613 of the helium storage device 600 and enters the housing 601. It then passes through the tape at the first opening 617 on the first side plate 610 and exits the housing 601, reaching the spherical curved crystal 201. After reflection by the spherical curved crystal 201, it forms the outgoing beam L2. The outgoing beam L2 passes through the tape at the first opening 617 on the first side plate 610 and enters the housing 601. It then passes through the tape at the second opening 618 on the third side plate 612 and exits the housing 601, reaching the sample and detector. When the Bragg angle is 82°, the incident beam L1 passes through... After passing through the tape at the third opening 619 on the fourth side plate 613 of the helium storage device 600, the beam enters the interior of the box 601. Then, it passes through the tape at the first opening 617 on the first side plate 610 and exits the interior of the box 601, reaching the spherical curved crystal 201. After being reflected by the spherical curved crystal 201, it forms an outgoing beam L3. The outgoing beam L3 passes through the tape at the first opening 617 on the first side plate 610 and enters the interior of the box 601. Then, it passes through the tape at the second opening 618 on the third side plate 612 and exits the interior of the box 601, reaching the sample and detector. When the Bragg angle is between 55° and 82°, the outgoing beam will be between L2 and L3. Both can pass through the tape at the first opening 617 on the first side plate 610 and enter the interior of the box 601. Then, they pass through the tape at the second opening 618 on the third side plate 612 and exit the interior of the box 601, reaching the sample and detector. By passing X-rays through the helium storage device 600, the scattering and absorption of X-rays by the air can be reduced, thereby increasing the received light intensity of the detector.

[0098] In the laboratory spectrometer of this invention, the X-ray source 101 is fixed on the base, and the spherical curved crystal 201, the sample and the detector 301 are moved by the motion component 400, so that the X-ray source 101, the spherical curved crystal 201 and the sample are always on the Rowland circle. Since the X-ray source 101 does not need to move, the optical path is stable.

[0099] The above description is merely a preferred embodiment of the present invention and is not intended to limit the scope of the invention. Various variations can be made to the above embodiments of the present invention. That is, all simple and equivalent changes and modifications made based on the claims and description of this invention fall within the protection scope of the claims of this patent. All aspects not described in detail in this invention are conventional technical content.

Claims

1. A laboratory spectrometer characterized by, The application relates to a kind of X-ray diffraction equipment, including: Base; Motion component, set on the base; Radiation source component, including X-ray source and mounting frame, the mounting frame is fixed on the base, the X-ray source is fixed on the mounting frame; Bent crystal component, including spherical bent crystal and positioning frame, the spherical bent crystal is fixed on the positioning frame, the positioning frame is fixed on the motion component; Detection component, including detector and support frame, the detector is fixed on the support frame, the support frame is fixed on the motion component, and the support frame is also used to fix sample; The motion component is set to move the spherical bent crystal, sample and detector, so that the X-ray source, the spherical bent crystal and the sample are always on the roll circle; The motion component includes first linear displacement table, second linear displacement table, third linear displacement table, linkage mechanism, first rotary displacement table and attitude adjustment displacement table, the first linear displacement table and the second linear displacement table are both fixed on the base, the first linear displacement table is towards the X-ray source, the second linear displacement table is at an angle with the first linear displacement table, two ends of the linkage mechanism are located on the first linear displacement table and the second linear displacement table respectively, the linkage mechanism can slide and rotate relative to the first linear displacement table, and the linkage mechanism can rotate relative to the second linear displacement table; The first rotary displacement table is fixed on one end of the linkage mechanism, and the third linear displacement table is fixed on the other end of the linkage mechanism; The attitude adjustment displacement table is arranged on the first rotary displacement table, the bent crystal component is fixed on the attitude adjustment displacement table, and the detection component is fixed on the third linear displacement table; The linkage mechanism includes first connecting plate and second connecting plate connected with each other, the first linear displacement table is fixed with rotary support, the rotary support is fixed with first driven turntable, the first driven turntable is provided with slide block support, the slide block support is slidably connected with the first connecting plate, and the first rotary displacement table is fixed on the rotary support; The second linear displacement table is provided with pad block, the pad block is provided with second driven turntable, the second connecting plate is arranged on the second driven turntable, and the third linear displacement table is arranged on the second connecting plate; The rotary support includes rotary base, shaft and mounting seat, two ends of the shaft are connected with the rotary base and the mounting seat respectively, the first driven turntable is fixed on the rotary base, the rotary base is fixed on the first linear displacement table, and the first rotary displacement table is fixed on the mounting seat; The first connecting plate is provided with sliding groove, the shaft passes through the sliding groove and the first driven turntable, and the rotary base and the mounting seat are located above and below the first connecting plate respectively; The attitude adjustment displacement table includes fourth linear displacement table and second rotary displacement table, the second rotary displacement table is arranged on the fourth linear displacement table, the fourth linear displacement table is arranged on the first rotary displacement table, and the bent crystal component is arranged on the second rotary displacement table.

2. The laboratory spectrometer of claim 1, wherein, The mounting frame comprises an L-shaped plate and a bottom plate, the L-shaped plate is provided with a reinforcing plate, the L-shaped plate comprises a horizontal plate and a vertical plate, the vertical plate is fixed on the horizontal plate, the horizontal plate is fixed on the bottom plate, the bottom plate is fixed on the base, and the X-ray source is fixed on the vertical plate.

3. The laboratory spectrometer of claim 2, wherein, The bottom of the X-ray source is supported by a support plate, and the support plate is fixed on the vertical plate.

4. The laboratory spectrometer of claim 1, wherein, A light blocking device and a light absorbing device are sequentially arranged at the outlet of the X-ray source, the light blocking device is arranged to block the outlet of the X-ray source, and the light absorbing device is arranged to absorb the fluorescence and scattering of X-rays near the outlet of the X-ray source.

5. The laboratory spectrometer of claim 1, wherein, The positioning frame comprises a positioning base and a positioning ring, the positioning base is fixed on the motion assembly, the positioning ring is fixed on the positioning base, the spherical curved crystal is clamped in the positioning ring, and a rotating cover is arranged on the positioning ring.

6. The laboratory spectrometer of claim 1, wherein, The support frame comprises a support base, a sample holder and a detector support mechanism, the sample holder and the detector support mechanism are fixed on the support base, the support base is fixed on the motion assembly, the sample is fixed on the sample holder, and the detector is fixed on the detector support mechanism.

7. The laboratory spectrometer of claim 6, wherein, The sample holder comprises an adapter plate, a fixed plate is fixed on the adapter plate, a cover plate and a magnetic member are arranged on the fixed plate, the magnetic member adsorbs the cover plate on the fixed plate, and the sample is clamped between the magnetic member and the cover plate; through holes are arranged on the magnetic member, the cover plate, the fixed plate and the adapter plate.

8. The laboratory spectrometer of claim 7, wherein, A protrusion is arranged on one side of the magnetic member close to the cover plate, a containing groove is formed in the protrusion to contain the sample; grooves are arranged on the cover plate and the fixed plate, the fixed plate groove is used for containing the cover plate, and the cover plate groove is used for containing the protrusion.

9. The laboratory spectrometer of claim 6, wherein, The detector support mechanism comprises two oppositely arranged support members, insulating bottom plates are arranged on the two support members, the insulating bottom plates are fixed on the two support members, and the detector is fixed on the insulating bottom plates and located behind the sample.

10. The laboratory spectrometer of claim 9, wherein, End portions of the detector are provided with protective covers, holes are formed in the protective covers, and the protective covers are fixed on the insulating bottom plates.

11. The laboratory spectrometer of claim 1, wherein, A plurality of lifting rings and a plurality of fixing members are arranged on the base.

12. The laboratory spectrometer of claim 1, wherein, A helium storage device is further arranged on the base, and the helium storage device stores helium.

13. The laboratory spectrometer of claim 12, wherein, The helium storage device comprises a box body, the box body comprises an upper cover plate, a lower cover plate, and first, second, third, fourth and fifth side plates which are sequentially connected in a head-to-tail manner, the upper cover plate is connected with upper ends of the side plates, the lower cover plate is connected with lower ends of the side plates, and the box body stores helium; the first side plate has a first opening, the third side plate has a second opening, and the fourth side plate has a third opening; the first, second and third openings are sealed by adhesive tapes to form a sealed environment in the box body.

14. The laboratory spectrometer of claim 13, wherein, An air inlet pipeline and an air outlet pipeline are further arranged, and the air inlet pipeline and the air outlet pipeline are in communication with the inside of the box body.

15. The laboratory spectrometer of claim 13, wherein, The helium storage device further comprises a supporting mechanism, the box body is fixed on the supporting mechanism, and the supporting mechanism is fixed on the base.

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