CN115963126A - laboratory spectrometer - Google Patents

Abstract

The invention relates to a laboratory spectrometer comprising: a base; the moving assembly is arranged on the base; the X-ray source assembly comprises an X-ray source and a mounting rack, the mounting rack is fixed on the base, and the X-ray source is fixed on the mounting rack; the crystal bending assembly comprises a spherical crystal bending part and a positioning frame, the spherical crystal bending part is fixed on the positioning frame, and the positioning frame is fixed on the moving assembly; the detection assembly comprises a detector and a support frame, the detector is fixed on the support frame, the support frame is fixed on the movement assembly, and the support frame is also used for fixing a sample; the motion assembly is configured to move the spherical curved crystal, the sample and the detector such that the X-ray source, the spherical curved crystal and the sample are always on a rowland circle. The X-ray source of the laboratory spectrometer is fixed, the spherical curved crystal, the sample and the detector only need to be moved during energy scanning, and the light path is stable.

Description

laboratory spectrometer

technical field

The invention relates to the technical field of X-ray absorption spectroscopy, and more specifically relates to a laboratory spectrometer.

Background technique

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. It can study the local structure of atoms in solid state and liquid state, and is widely used. In many fields such as materials, biology, chemistry, environment and geology.

The laboratory spectrometer is an analytical instrument based on the principle of Rowland circle imaging, using X-ray sources, spherical curved crystals, detectors and displacement stages. Through the displacement stage, the X-ray source, spherical curved crystals, samples and detectors Upward movement to realize the absorption spectrum collection of different samples in the energy range corresponding to different Bragg angles, so that the local structure information of different elements can be measured (such as the type of coordination element, valence state, bond length, coordination number, etc.).

However, the existing laboratory spectrometer will move the X-ray source, spherical curved crystal, sample and detector at the same time. Due to the large mass of the X-ray source, it is difficult to move and the optical path is unstable.

Contents of the invention

The object of the present invention is to provide a 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, and the optical path is stable.

Based on the above object, the invention provides a kind of laboratory spectrometer, comprising:

base;

a motion component arranged on the base;

A ray source assembly, including an X-ray source and a mounting frame, the mounting frame is fixed on the base, and the X-ray source is fixed on the mounting frame;

The crystal bending assembly includes a spherical bending crystal and a positioning frame, the spherical bending crystal is fixed on the positioning frame, and the positioning frame is fixed on the moving assembly;

The detection assembly includes a detector and a support frame, the detector is fixed on the support frame, the support frame is fixed on the movement assembly, and the support frame is also used to fix the sample;

The moving component 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.

Further, the installation frame includes an L-shaped plate and a bottom plate, the L-shaped plate is provided with a reinforcing plate, the L-shaped plate includes a horizontal plate and a vertical plate, and 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.

Further, the bottom of the X-ray source is supported by a support plate, and the support plate is fixed on the vertical plate.

Further, a light blocking device and a light absorbing device are sequentially arranged at the exit of the X-ray source, the light blocking device is set to block the exit of the X-ray source, and the light absorbing device is set to absorb the light of the X-ray source Fluorescence and scattering of X-rays near the exit.

Further, the motion assembly includes a first linear displacement platform, a second linear displacement platform, a third linear displacement platform, a linkage mechanism, a first rotary displacement platform and an attitude adjustment displacement platform, and the first linear displacement platform and the The second linear displacement stage is fixed on the base, the first linear displacement stage faces the X-ray source, and the second linear displacement stage forms an included angle with the first linear displacement stage , the two ends of the linkage mechanism are respectively located on the first linear displacement stage and the second linear displacement stage, the linkage mechanism can slide and rotate relative to the first linear displacement stage, the linkage The mechanism can rotate relative to the second linear displacement stage; the first rotary displacement stage is fixed at one end of the linkage mechanism, and the third linear displacement stage is fixed at the other end of the linkage mechanism; the attitude adjustment The translation platform is arranged on the first rotary translation platform, the crystal bending assembly is fixed on the attitude adjustment translation platform, and the detection assembly is fixed on the third linear translation platform.

Further, 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, a first driven turntable is fixed on the rotating bracket, and the A slider bracket is arranged on the first driven turntable, and the slider bracket is slidably connected with the first connecting plate, and the first rotary displacement platform is fixed on the rotation bracket; on the second linear displacement platform A riser block is provided, and a second driven turntable is arranged on the riser block, the second connecting plate is arranged on the second driven turntable, and the third linear displacement stage is arranged on the second driven turntable. connection board.

Further, the rotating bracket includes a rotating base, a rotating shaft and a mounting seat, the two ends of the rotating shaft are respectively connected to the rotating base and the mounting seat, the first driven turntable is fixed on the rotating base, The rotating base is fixed on the first linear displacement stage, and the first rotating displacement stage is fixed on the mounting seat; a chute is provided on the first connecting plate, and the rotating shaft passes through the The chute and the first driven turntable, and the rotating base and the mounting seat are respectively located above and below the first connecting plate.

Further, the posture adjustment translation platform includes a fourth linear translation platform and a second rotation translation platform, the second rotation translation platform is arranged on the fourth linear translation platform, and the fourth linear translation platform is arranged on the on the first rotary translation platform, and the crystal bending assembly is arranged on the second rotary translation platform.

Further, the positioning frame includes a positioning base and a positioning ring, the positioning base is fixed on the moving assembly, the positioning ring is fixed on the positioning base, and the spherical curved crystal is snapped into the positioning ring , the positioning ring is provided with a screw cap.

Further, 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, and the support base is fixed on the moving assembly, The sample is fixed on the sample holder, and the detector is fixed on the detector supporting mechanism.

Further, the sample holder includes an adapter plate, a fixing plate is fixed on the adapter plate, a cover plate and a magnetic part are arranged on the fixing plate, and the magnetic part adsorbs the cover plate on the fixed plate. On the plate, the sample is clamped between the magnetic piece and the cover plate; the magnetic piece, the cover plate, the fixing plate and the adapter plate are all provided with through holes.

Further, a protrusion is provided on the side of the magnetic member close to the cover plate, and a receiving groove is opened on the protrusion to accommodate the sample; both the cover plate and the fixing plate are provided with A groove, 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.

Further, the detector support mechanism includes two oppositely arranged supports, the two supports are provided with an insulating base plate, the insulating base plate is fixed on the two supports, the detector is fixed on the insulating base plate, and located behind the sample.

Further, a protective cover is provided at the end of the detector, holes are opened in the protective cover, and the protective cover is fixed on the insulating base.

Further, the base is provided with a plurality of suspension rings and a plurality of fixing pieces.

Further, a helium gas storage device fixed on the base is also included, and helium gas is stored in the helium gas storage device.

Further, the helium gas storage device includes a box body, and the box body 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 The fifth side plate, the upper cover plate is connected to the upper end of each side plate, the lower cover plate is connected to the lower end of each side plate, and helium gas is stored inside the box body; the first side plate has a first opening, the third side plate has a second opening, the fourth side plate has a third opening, the first opening, the second opening and the third opening are all sealed by adhesive tape, so that the The inside of the box body is formed as a sealed environment.

Further, it also includes an air intake pipeline and an air outlet pipeline, both of which communicate with the inside of the box body.

Further, the helium gas storage device further includes a supporting mechanism, the box body is fixed on the supporting mechanism, and the supporting mechanism is fixed on the base.

In the laboratory spectrometer of the embodiment of the present invention, the X-ray source is fixed on the base, and the spherical curved crystal, the sample and the detector are moved through the moving components, so that the X-ray source, the spherical curved crystal and the sample are always on the Rowland circle , since the X-ray source does not need to move, the optical path is stable.

Description of drawings

1 is a schematic diagram of a Rowland circle of a laboratory spectrometer according to an embodiment of the present invention;

Fig. 2 is a schematic structural diagram of a laboratory spectrometer according to an embodiment of the present invention;

3A is a schematic structural diagram of a radiation source assembly of a laboratory spectrometer according to an embodiment of the present invention;

Fig. 3B is a schematic structural diagram of a mounting bracket of a radiation source assembly according to an embodiment of the present invention;

3C is a schematic structural diagram of an L-shaped frame of a radiation source assembly according to an embodiment of the present invention;

Fig. 3D is a schematic diagram of another viewing angle of the mounting frame of the radiation source assembly according to the embodiment of the present invention;

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

3F is a schematic structural diagram of a light absorbing device according to an embodiment of the present invention;

3G is a schematic structural diagram of an X-ray source, a light blocking device and a light absorbing device according to an embodiment of the present invention;

3H is a cross-sectional view of a diaphragm of a light absorbing device according to an embodiment of the present invention;

FIG. 4A is a schematic structural diagram of a motion assembly according to an embodiment of the present invention;

4B is a schematic structural diagram of a linkage mechanism of a motion assembly according to an embodiment of the present invention;

4C is a schematic structural diagram of a rotating bracket of a linkage mechanism according to an embodiment of the present invention;

FIG. 4D is a schematic structural diagram of a first driven turntable of a linkage mechanism according to an embodiment of the present invention;

Fig. 4E is a schematic structural diagram of the attitude adjustment translation platform of the motion assembly according to the embodiment of the present invention;

5 is a schematic structural diagram of a bent crystal assembly according to an embodiment of the present invention;

FIG. 6A is a schematic structural diagram of a detection assembly according to an embodiment of the present invention;

6B is a cross-sectional view of a sample holder according to an embodiment of the present invention;

FIG. 6C is a schematic diagram of another viewing angle of a detection component according to an embodiment of the present invention;

6D is a top view of a detection assembly according to an embodiment of the present invention;

7 is a schematic structural diagram of a base according to an embodiment of the present invention;

8A is a schematic structural diagram of a helium storage device according to an embodiment of the present invention;

8B is a side view of a box of a helium storage device according to an embodiment of the present invention;

Fig. 8C is a structural schematic diagram of another viewing angle of the box body according to the embodiment of the present invention;

Fig. 8D is a schematic structural diagram of a box body and a supporting mechanism according to an embodiment of the present invention;

Fig. 8E is a schematic diagram of the optical path of the helium gas storage device in use according to an embodiment of the present invention.

Detailed ways

Below in conjunction with the drawings, preferred embodiments of the present invention are given and described in detail.

An embodiment of the present invention provides a laboratory spectrometer, which includes an X-ray source, a spherical curved crystal, and a detector. The X-ray source is fixed, and the spherical curved crystal, the sample, and the detector are moved, so that the X-ray source, the spherical surface Bent crystals and samples are always on the Rowland circle. As shown in Figure 1, the source point P ₁ of the X-ray source, the geometric center P ₂ of the spherical curved crystal, and the geometric center P ₃ of the sample surface are always on the Rowland circle with a diameter of Rc, where Rc is the curvature of the spherical curved crystal radius. In this way, the incident beam emitted by the X-ray will be transmitted on the sample after being monochromatized by the spherical curved crystal and received by the subsequent detector. The angle between the incident beam and the normal of the spherical curved crystal is the Bragg angle θ, and changing the value of this angle can change the energy used for scanning. The distance between the light source point P ₁ and the geometric center P ₂ of the spherical curved crystal is P ₁ P ₂ =Rc·sinθ, and the distance between the light source point P ₁ and the geometric center P ₃ of the sample surface is P ₁ P ₃ =Rc · sin θ cos θ. Since Rc is the radius of curvature of the spherically curved crystal, when the spherically curved crystal is determined, its size is also determined. Therefore, the values of P ₁ P ₂ and P ₁ P ₃ are related to θ. When θ changes, P ₁ P ₂ and The values of P _{1 and} P ₃ also need to be changed accordingly. In the present invention, θ=55°-82°, the spherical curved crystal, the sample and the detector can move at the same time, so as to satisfy the above-mentioned distance relationship at different θ values.

As shown in Figure 2, the laboratory spectrometer includes a radiation source assembly 100, a bent crystal assembly 200, a detection assembly 300, a motion assembly 400 and a base 500, and the radiation source assembly 100 includes an X-ray source 101 and a mounting frame 102, and the mounting frame 102 Fixed on the base 500, the X-ray source 101 is fixed on the mounting frame 102, the bending crystal assembly 200 includes a spherical bending crystal 201 and a positioning frame 202, the positioning frame 102 is fixed on the moving assembly 400, and the spherical bending crystal 201 is fixed on the positioning frame 202, the detection assembly 300 includes a detector 301 and a support frame 302, the support frame 302 is fixed on the motion assembly 400, the sample and the detector 301 are fixed on the support frame 302, the motion assembly 400 is installed on the base 500, and the motion assembly 400 The spherical curved crystal 201, the sample and the detector 301 can be moved simultaneously so that the X-ray source 101, the spherical curved crystal 201 and the sample are always located on the Rowland circle whose diameter is the radius of curvature of the spherical curved crystal 201, and the X-ray source 101 emits The incident light beam is monochromatized by the spherical curved crystal 201 , then transmitted on the sample and received by the detector 301 .

As shown in Figures 3A and 3B, the mounting frame 102 includes an L-shaped plate 103 and a base plate 104, and as shown in Figure 3C, the L-shaped plate 103 includes a horizontal plate 105 and a vertical plate 106 welded to each other, and the L-shaped plate 103 also includes A reinforcing plate 107 is welded, the bottom surface of the reinforcing plate 107 is welded with the horizontal plate 105, and the side of the reinforcing plate 107 is welded with the vertical plate 106, thereby increasing the stability of the L-shaped plate 103. The horizontal plate 105 can be detachably connected to the bottom plate 104 through a plurality of M8x25 hex socket head cap screws 108 . The bottom plate 104 can be detachably connected to the base 500 through a plurality of M6x16 hex socket head cap screws 109 . The X-ray source 101 can be an existing X-ray source device, such as a standard XRD-type X-ray source of model 3003 manufactured by XRD Eigenmann GmbH, and its specific structure and principle will not be repeated here. The X-ray source 101 can be fixed on the vertical plate 106 by a plurality of M6x25 socket cap screws 110 . The bottom of the X-ray source 101 can also be provided with a support plate 111 for auxiliary support of the X-ray source 101 , and the end of the support plate 111 is fixed on the vertical plate 106 by screws.

Since the installation position of the X-ray source 101 on the vertical plate 106 and the installation position of the horizontal plate 105 on the base plate 104 will determine the final position of the X-ray source 101 on the base 500, therefore, it can be arranged on the vertical plate 106 Multiple positioning pins 112 position the X-ray source 101 on the vertical plate 106 , and multiple positioning pins 113 may be provided on the bottom plate 104 to position the horizontal plate 105 . Through the positioning pins 112 and 113, the installation of the radiation source assembly 100 can be completed quickly.

The installation process of the radiation source assembly 100 is as follows:

First base plate 104 is fixed on the base 500 by screws 109, then the horizontal plate 105 of the L-shaped frame 103 is placed on the base plate 104, and one side of the horizontal plate 105 is connected to the two positioning pins 113 on the right side of the base plate 104. contact, as shown in Figure 3D; then the horizontal plate 105 and the bottom plate 104 are fixed by screws 108; then the X-ray source 101 is moved to the position defined by the positioning pin 112 of the vertical plate 106, so that the bottom surface of the X-ray source 101 is in line with the bottom The two positioning pins 112 on the side are in contact, and the side of the X-ray source 101 is in contact with the positioning pin 112 on the right side, and then the X-ray source 101 is fixed on the vertical plate 106 by screws 110; then the supporting plate 111 is placed on the X-ray The bottom of the source 101, and after being attached to it, the support plate 111 is fixed on the vertical plate 106 by screws, so as to provide auxiliary support for the X-ray source 101. If it is found that optical aberrations cause spectral energy broadening during absorption spectrum collection, the X-ray source 101 can be switched to a position close to a point inside the Rowland circle (generally a few millimeters away from the Rowland circle circumference). Specifically, the screw 108 can be loosened, then the horizontal plate 105 can be moved to make it contact with the two rightmost positioning pins 113 on the bottom plate 104, and then the screw 108 can be tightened (solid lubricant can be applied to the bottom surface of the horizontal plate 105 grease to facilitate movement). The location of the X-ray source 101 inside the Rowland circle 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.

Continuing to refer to FIG. 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, and the light blocking device 114 is used to block the exit of the X-ray source 101 as required during the measurement process, To prevent X-rays from causing radiation to experimenters; the light absorbing device 115 is used to absorb fluorescence and scattering near the exit of the X-ray source 101, so as to avoid affecting the detector of the laboratory spectrometer.

The light blocking device 114 includes a shielding block 116 and a shutter 117, as shown in FIG. One end of the protruding portion 118 extends into the waist-shaped hole on the turntable 120 at the exit of the X-ray source 101 , and the other end of the protruding portion 118 protrudes into the light-through hole 121 of the shutter 117 . The shutter 117 can adopt an existing standard optical shutter model FS25, and its structure and principle will not be repeated here.

The shielding block 116 and the shutter 117 are made of copper with a thickness of not less than 3mm, so that when the shutter is closed, the leakage rate of the X-rays emitted by the X-ray source 101 at a high voltage of up to 45kV can be controlled to <1μSv/ h to ensure that experimenters are protected from radiation damage.

The shutter 117 can be installed on the X-ray source 101 through an 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 , so that the shutter 117 is fixed on the X-ray source 101 .

As shown in Figure 3F, 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 in FIG. 3G , the fixing plate 126 is fixed on the shielding block 116 , so that the aperture 123 is located at the light hole 121 of the shutter 117 . A plurality of 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 on the shielding block 116 , the aperture 123 is just positioned at the light hole 121 of the shutter 117 .

As shown in FIG. 3H , the aperture 123 is composed of an inner ring 128 and an outer ring 129. The material of the inner ring 128 is pure aluminum (1060), which is responsible for absorbing the fluorescence generated when X-rays pass through this area. The material of the outer ring 129 is Copper is used to absorb the scattered light generated when X-rays pass through this area. The inner diameters of the inner ring 128 and the outer ring 129 are matched, and the H8/h7 small gap fit is used for assembly.

In order to prevent leakage of X-rays, as shown in FIG. 3E , part of the diaphragm 123 needs to extend into the aperture 121 of the shutter 117 .

X-ray source 101 can adopt XRD Eigenmann GmbH company's model to be the XRD ray source of 3003, and the X-ray that it sends is as shown in Figure 3E, wherein P ₁ is the light source point, L is the beam center, the focal point at the light source point P ₁ place The spot size is 0.8mm ² , the angle between the center L of the beam and the Y axis along the clockwise direction in the horizontal plane is a=6°, the spatial divergence angle of the X-ray beam symmetrical to the center L of the beam is c=5.9°, the center L of the beam and the Y axis are The included angle b=2.95° at the edge of the beam. When the shutter 117 is opened, X-rays can be emitted from the diaphragm 123, and neither the light blocking device 114 nor the light absorbing device 115 will block it, so the normal use of the X-ray source 101 will not be affected; and when the shutter 117 is closed, X-rays would be blocked so they could not be emitted, thus protecting experimenters from radiation.

As shown in FIG. 4A, the motion assembly 400 includes a first linear translation stage 401, a second linear translation stage 402, a third linear translation stage 403, a linkage mechanism 404, a first rotary translation stage 405, and an attitude adjustment translation stage 406. Both a linear displacement stage 401 and a second linear displacement stage 402 are fixed on the base 500, and the first linear displacement stage 401 faces the light source point of the X-ray source 101, that is, the first linear displacement stage 401 is positioned along the direction of the incident light beam. direction, the second linear translation stage 402 and the first linear translation stage 401 are set at an included angle, and the included angle can be 40°-70°; the two ends of the linkage mechanism 404 are respectively located on the first linear translation stage 401 and the second On the linear displacement stage 402, and can rotate relative to the first linear displacement stage 401 and the second linear displacement stage 402, like this, the two ends of the linkage mechanism 404 can respectively move along the first linear displacement stage 401 and the second linear displacement stage 402 moves without interference; the first rotary translation platform 405 is fixed at one end of the linkage mechanism 404, the third linear translation platform 403 is fixed at the other end of the linkage mechanism 404, and the attitude adjustment translation platform 406 is set on the first rotation translation platform 405, the crystal bending assembly 200 is fixed on the attitude adjustment translation stage 406, the first rotating translation stage 405 can make the attitude adjustment translation stage 406 and the crystal bending assembly 200 rotate, thereby changing the size of the Bragg angle, and the attitude adjustment translation stage 406 is used Adjust the geometric center height of the spherical curved crystal 201 and the normal vector of the bevel angle of the lattice plane so that the geometric center height of the spherical curved crystal 201 and the normal vector of the bevel angle of the lattice plane are all located in the plane where the Rowland circle is located to obtain better Diffraction efficiency; the detection assembly 300 is fixed on the third linear displacement stage 403, and the distance between the sample and the detector 301 relative to the spherical curved crystal 201 can be moved by the third linear displacement stage 403.

As shown in Figure 4B, the linkage mechanism 404 includes a first connecting plate 407 and a second connecting plate 408 connected to each other, the first connecting plate 407 is provided with a slide rail 421, the slide rail 421 is slidably matched with the slide block 409, and the slide block 409 Then it is installed 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 rotation bracket 411, and the rotation bracket 411 is fixed on the first linear displacement stage 401 .

As shown in Figure 4C, 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 respectively connected with the rotating base 413 and the mounting base 415, and the first rotating displacement stage 405 is fixed on the mounting base 415 . The first connecting plate 407 is provided with a chute 416, the rotating shaft 414 passes through the chute 416, and the rotating base 413 and the mounting seat 415 are respectively located above and below the first connecting plate 407, so that the rotating bracket 411 can be positioned relative to the first connecting plate 407. A connecting plate 407 slides along the sliding slot 416 .

As shown in Figure 4D, the first driven turntable 412 includes a turntable base 417 and a turntable 418 arranged on the turntable base 417, the turntable 418 can rotate 360° on the turntable base 417, and when installed, the rotating shaft of the rotating bracket 411 414 passes through the first driven turntable 412, and the turntable base 417 is fixed on the rotating base 413 of the rotating bracket 411, and the slider bracket 410 is fixed on the rotating platform 418, so that the slider bracket 410 can follow the rotating platform 418 on the turning platform The base 417 rotates around the rotating shaft 414 . The first driven turntable 412 can be a rotary platform of the model RM16A-C1 of KOHZU Company, and its structure and principle will not be repeated here.

The second connecting plate 408 is arranged on the second driven turntable 419 , and the second driven turntable 419 is fixed on the raising block 420 , and the raising block 420 is fixed on the second linear translation 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 on the turntable of the second driven turntable 419, and the turntable base of the second driven turntable 419 is then fixed on On the block 420 , the second connecting plate 408 can rotate relative to the second linear displacement stage 402 . By setting the rotating bracket 411 and the stand-up block 420, the spherical curved crystal 201, the sample and the detector 301 can be at the same height. When the first linear translation stage 401 and the second linear translation stage 402 are working, the first driven turntable 412 and the rotating bracket 411 will move along the first linear translation stage 401, and the raising block 420 and the second driven turntable 419 and the second connecting plate 408 will move along the second linear translation stage 402, because the first connecting plate 407 and the second connecting plate 408 are connected, so the first connecting plate 407 and the slider bracket 410 will move relative to the first linear translation stage 401 rotates, the second connecting plate 408 will rotate relative to the second linear translation stage 402 to avoid motion interference.

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

In an exemplary embodiment, the first linear translation stage 401 can adopt the model "XA16F-L2201-modified" linear translation stage, its motion range is 200mm, and the full step resolution is 10μm, which is used for spherical surface during energy scanning. The curved crystal moves in a straight line along the direction of the X-ray incident light. The second linear translation stage 402 can adopt the model "XA16F-L2301-Changed" linear translation stage, its motion stroke is 330 mm, and the full step resolution is 4 μm. The model of the third linear displacement stage 403 is the same as that of the first linear displacement stage 401 . The first rotary translation stage 405 can adopt the model "RA07A-W02-Change" rotary translation platform, its motion range is 270°, and the full step resolution is 14.4", which is used for adjusting the Bragg angle of spherical curved crystals during energy scanning. To ensure the motion repeatability during energy scanning, the first linear translation stage 401, the second linear translation stage 402, the third linear translation stage 403 and the first rotary translation stage 405 are all equipped with TONIC series incremental codes from the British Renishaw company The encoder system, wherein the encoder resolutions of the first linear translation stage 401, the second linear translation stage 402 and the third linear translation stage 403 are all 0.1 μm, and the encoder resolution of the first rotary translation stage 405 is 0.6″. The fourth linear displacement stage 422 can adopt the model "ZA05A-W2C01" linear displacement stage, its motion stroke is 3 mm, and the full step resolution is 0.5 μm. The second rotary translation stage 423 can adopt the model "SA05A-R2M01" rotary translation platform, its motion stroke is 9°, and the full step resolution is 5.76".

During energy scanning, the Bragg angle can be changed through the first rotary stage 405, and then adjusted through the cooperation between the first linear stage 401, the second linear stage 402 and the third linear stage 403 The distance between P ₁ P ₂ and P ₁ P ₃ shown in Figure 1 makes P ₁ P ₂ =Rc·sinθ, P ₁ P ₃ =Rc·sinθcosθ, so that X-ray source 101, spherical curved crystal 201 and sample Always on the Rowland circle. The specific adjustment process can be realized by programming, that is, input the written program in the control system of each displacement platform, and then realize automatic control.

As shown in FIG. 5 , the crystal bending 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 on the positioning base 203 , and the positioning base 203 is fixed on the attitude adjustment translation platform 406 of the motion assembly 400 through a plurality of M3x10 hex socket head cap screws 205 . The positioning ring 204 is used to accommodate the spherical curved crystal 201 . After the spherical curved crystal 201 is snapped into the positioning ring 204 , the edge of the front side (ie, the working surface) of the spherical curved crystal 201 is attached to the inner surface of the positioning ring 204 . The side of the positioning ring 204 close to the back of the spherical curved crystal 201 is provided with a screw cap 206 for preventing the spherical curved crystal 201 from coming out from this side. The screw cap 206 can be threadedly connected with the positioning ring 204 so as to realize tightness and looseness through rotation. An M6x13 hexagon socket set screw 207 can be provided on the top of the positioning ring 204. After the spherical curved crystal 201 is loaded into the positioning ring 204, the screw 207 is rotated to make it withstand the side (i.e. the circumferential surface) of the spherical curved crystal 201, thereby It is positioned.

A boss can be formed on the positioning base 203 , and the front side of the positioning ring 204 (the side close to the front side of the spherical curved crystal 201 ) is in close contact with the boss. The positioning base 203 can also be provided with a stopper 208, which is close to the rear side of the positioning ring (that is, the side opposite to the front side or the side near the back of the spherical curved crystal 201), and the stopper 208 passes through two M3x8 The hex socket head cap screws 209 with oblique flat heads and chamfered edges are fixed to the positioning base 203 , so that the positioning ring 204 will be limited between the boss and the stopper 208 . The positioning ring 204 can be fixedly connected to the positioning base 203 through the M5x10 hexagon socket head cap screw 210 .

As shown in FIG. 6A , 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 on the support base 303, and the adapter plate 306 is provided with a fixed plate 307, which is fixed on the adapter plate 306 by a plurality of M2.5x8 stainless steel hex socket head cap screws 308, The fixed plate 307 is provided with a cover plate 309 and a magnetic piece 310, the magnetic piece 310 adsorbs the cover plate 309 on the fixed plate 307, and the sample 311 is sandwiched between the magnetic piece 310 and the cover plate 309, through the adsorption of the magnetic piece 310 force fixed.

As shown in FIG. 6B , 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 can also be provided on the cover plate 309 , and a protrusion can be provided on the magnetic member 310 , and the protrusion of the magnetic member 310 can be inserted into the groove of the cover plate 309 to realize the positioning of the two. The protrusion of the magnetic part 310 can be provided with a receiving groove for accommodating the sample 311. After the sample 311 is placed in the receiving groove, insert the protrusion of the magnetic part 310 into the groove of the cover plate 309, and then put the cover plate 309 together Put it into the groove of the fixing plate 307, under the action of the adsorption force of the magnetic piece 310, the magnetic piece 310, the sample 311 and the cover plate 309 will be fixed on the fixing plate 307, thus completing the installation of the sample 311. When the sample 311 needs to be replaced, only the magnetic part 310, the sample 311 and the cover plate 309 are removed from the fixing plate 307, and then the sample 311 is replaced, and then installed on the fixing plate 307 after replacement. The adapter plate 306 , the fixing plate 307 , the cover plate 309 and the magnetic piece 310 are all provided with through holes for X-rays to pass through. In this way, when the X-rays pass through the sample 311 , they can reach the detector 301 smoothly.

Continuing to refer to FIG. 6A , the detector support mechanism 305 includes two oppositely arranged supports 312, and an insulating base plate 313 is arranged on the two supports 312, which are fixed to the two supports 312 by a plurality of M4x12 socket head cap screws 314, and the detector 301 is fixed on the insulating base plate 313 by a plurality of M3x12 hexagon socket head cap screws 315 . The detector 301 can be AXAS-M H150 silicon drift detector from KETEK Company of Germany, whose energy resolution can be better than 136eV. The end of the detector 301 is provided with a protective cover 316, on which a rectangular hole of 5mm×12mm is opened, and each surface of the rectangular hole needs to be polished to a surface roughness of 0.8Ra. 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 to improve the data collection quality of the detector 301 . As shown in Figure 6C and Figure 6D, the protective cover 316 is fixedly connected to the connecting plate 318 through a plurality of M2. superior. Both the connection plate 318 and the insulating base plate 313 are made of polyetheretherketone (PEEK) material to realize the electrical insulation installation of the detector 301, thereby improving the signal-to-noise ratio during data collection. The two support members 312 can be fixed on the support base 303 by a plurality of M4x16 socket head cap screws 320 .

After installation, the detector 301 needs to be located just behind the sample 311 to receive the X-rays passing through the sample, so the installation positions of the adapter plate 306 and the detector support mechanism 305 can be positioned on the support base 303 first. Specifically, the adapter plate 306 can be fixed on the first magnetic base 322 by a plurality of M6x16 hexagon socket head cap screws 321, the first magnetic base 322 is adsorbed on the second magnetic base 323, and the second magnetic base 323 is adsorbed on the support on the base 303. The first magnetic base 322 and the second magnetic base 323 can respectively adopt the magnetic bases modeled as KBT50M and KBB50M of THORLABS Company of the United States. The position of the second magnetic base 320 on the support base 303 can be positioned by three positioning pins 324 whose model is MSVC5-25, so that after installation, the detector 301 can be located just behind the sample 311.

The support base plate 303 is fixed on the third linear translation stage 403 of the motion assembly 400 through a plurality of M5x16 socket head cap screws 325 , so that the position of the sample and the detector 301 can be adjusted through the motion assembly 400 .

As shown in Figure 7, the base 500 is provided with a plurality of lifting rings 501 and a plurality of fixing parts 502, the lifting rings 501 can facilitate the hoisting operation of the base 500 and the components on it, and one end of the fixing parts 502 is passed through M6x10 hexagon socket head cap screws 503 It is fixed on the base 500, and the other end can be fixedly connected with the aluminum profile frame (not shown in the figure) of the laboratory through the M6x12 hex socket head cap screw 504, so as to complete the installation of the base 500 in the laboratory.

The fixing part 502 can be a Z-shaped structure welded by three plates in sequence, and its material is 6061 aluminum alloy.

Positioning pins may be provided on the base 500 for precise positioning of the X-ray source assembly 100 and the moving assembly 400 to ensure installation accuracy.

Continuing to refer to FIG. 2, a helium gas storage device 600 is also provided on the base 500, which is located on the propagation path of X-rays. Helium gas is stored in the helium gas storage device 600, and its mass number is relatively small compared to air The absorption of X-rays is much smaller, so setting the helium gas storage device 600 on the propagation path of X-rays can reduce the scattering and absorption of X-rays by air, thereby increasing the received light intensity of the detector 301 .

As shown in FIG. 8A, the helium gas storage device 600 includes a box body 601, an air inlet pipeline 602 and an air outlet pipeline 603. Both the air inlet pipeline 602 and the gas outlet pipeline 603 communicate with the inside of the box body 601, so that helium can be introduced or exhausted. gas.

The intake pipeline 602 includes an integral bonnet needle valve 604 with a pipe diameter of φ6mm, a ferrule right-angle joint 605 with a diameter of 6mm, a three-way joint 606 with a ferrule with a diameter of 6mm, a low-pressure unloading valve 607 for a ferrule joint with a diameter of 6mm, and a needle valve The inlet of 604 communicates with the helium source (not shown in the figure), the outlet communicates with the first interface of the three-way joint 606 through the through pipe, and the second interface of the three-way joint 606 communicates with the unloading valve 607 through the copper pipe, The third interface of the three-way joint 606 communicates with the first interface of the right-angle joint 605 through a copper tube, and the second interface of the right-angle joint 605 communicates with the inside of the box body 601 to pass helium gas into the box body 601 . When the unloading valve 607 leaves the factory, the working pressure of the spring in the valve needs to be set to 1.5 bar. In this way, if the helium pressure inside the box body 601 exceeds 1.5 bar, the unloading valve 607 will automatically open to exhaust, so as to prevent the box The internal pressure of body 601 is too high.

The air outlet pipeline 603 includes a needle valve 608 with integral bonnet with a pipe diameter of φ6mm and a ferrule right-angle joint 609 with a pipe diameter of 6mm. It communicates with the inside of the box body 601 , and the outlet of the needle valve 608 communicates with the outside, so that the helium inside the box body 601 is discharged through the gas outlet pipeline 603 .

As shown in Figures 8B and 8C, the box body 601 includes a first side panel 610, a second side panel 611, a third side panel 612, a fourth side panel 613 and a fifth side panel 614 connected end to end in sequence, and the box body 601 also It includes an upper cover plate 615 and a lower cover plate 616, which are respectively connected with the upper end and the lower end of each side plate, thereby jointly 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, and the first opening 617 is passed through a 0.01 mm thick polyimide adhesive tape 620 (see Fig. 8A) Sealing, the second opening 618 and the third opening 619 can also be sealed by a 0.01mm thick polyimide tape, so that the inside of the box body 601 can be a sealed environment, and the X-ray can pass through the tape and pass through the box body 601. Both the second side plate 611 and the upper cover plate 615 are provided with joints 621, the joints 621 on the second side plate 611 communicate with the second interface of the right angle joint 609 of the air outlet pipeline 603, the joints 621 on the upper cover plate 615 are connected with The second port of the right-angle joint 605 of the air intake pipeline 602 is communicated, so that the air enters through the upper cover plate 615 and the air exits through the second side plate 611 .

In order to install the helium gas storage device 600 on the base 500 without interfering with other components, the box body 601 needs to be installed on the base 500 through the supporting mechanism 622 . As shown in FIG. 8D , the helium gas storage device 600 further includes a supporting mechanism 622 , the box body 601 is fixed on the supporting mechanism 622 , and the supporting mechanism 622 is fixed on the base 500 . The support mechanism 622 includes four support rods 623 and a support plate 624 , the support plate 624 is fixed on the support rods 623 , and the box body 601 is fixed on the support plate 624 . Each support rod 623 can be respectively distributed on the four corners of the support plate 624 , and fixed to the support plate 624 by M8x20 hex socket head cap screws 625 . The bottom of the support rod 623 may be provided with threads, so as to be fixed on the base 500 through threaded connection.

As shown in Figure 8E, when in use, the fourth side plate 613 of the helium gas 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 the detector , In this way, when the Bragg angle is 55°, the incident light beam L ₁ passes through the adhesive tape at the third opening 619 on the fourth side plate 613 of the helium gas storage device 600 and then enters the inside of the box body 601, and then passes through The adhesive tape at the first opening 617 on the first side plate 610 leaves the inside of the box body 601 and reaches the spherical curved crystal 201. After being reflected by the spherical curved crystal 201, the outgoing beam L ₂ is formed, and the outgoing beam L ₂ passes through the first side plate. The adhesive tape at the first opening 617 on the 610 enters the inside of the box body 601, then passes through the adhesive tape at the second opening 618 on the third side plate 612 and leaves the inside of the box body 601, and reaches the sample and the detector; When the Bragg angle is 82°, the incident light beam _L1 enters the inside of the box body 601 after passing through the adhesive tape at the third opening 619 on the fourth side plate 613 of the helium gas storage device 600, and then passes through the first side plate The adhesive tape at the first opening 617 on 610 leaves the inside of the box body 601 and reaches the spherical curved crystal 201. After being reflected by the spherical curved crystal 201, the outgoing beam L ₃ is formed, and the outgoing beam L ₃ passes through the first side plate 610. The adhesive tape at the first opening 617 enters the inside of the box body 601, then passes through the adhesive tape at the second opening 618 on the third side plate 612 and leaves the inside of the box body 601, and reaches the sample and the detector; when the Bragg angle is at 55 When between °-82°, the outgoing light beam will be between _L2 and _L3 , both of which can pass through the adhesive tape at the first opening 617 on the first side plate 610 and then enter the inside of the box body 601, and then pass through the second The adhesive tape at the second opening 618 on the three side plates 612 then leaves the inside of the box body 601 and reaches the sample and the detector. By passing the X-rays through the helium gas storage device 600, the scattering and absorption of the X-rays by the air can be reduced, thereby increasing the received light intensity of the detector.

In the laboratory spectrometer of the embodiment of the present 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 moving assembly 400, so that the X-ray source 101, the spherical curved crystal 201 and the The sample is always on the Rowland circle, and since the X-ray source 101 does not need to move, the optical path is stable.

What is described above is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Various changes can also be made to the above embodiments of the present invention. That is to say, all simple and equivalent changes and modifications made according to the claims and description of the application for the present invention fall within the protection scope of the claims of the patent of the present invention. What is not described in detail in the present invention is conventional technical content.

Claims (19)

1. A laboratory spectrometer, characterized in that, comprising: base; a motion component arranged on the base; A ray source assembly, including an X-ray source and a mounting frame, the mounting frame is fixed on the base, and the X-ray source is fixed on the mounting frame; The crystal bending assembly includes a spherical bending crystal and a positioning frame, the spherical bending crystal is fixed on the positioning frame, and the positioning frame is fixed on the moving assembly; The detection assembly includes a detector and a support frame, the detector is fixed on the support frame, the support frame is fixed on the movement assembly, and the support frame is also used to fix the sample; The moving component 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. 2. The laboratory spectrometer according to claim 1, wherein the mounting bracket comprises an L-shaped plate and a base plate, the L-shaped plate is provided with a reinforcing plate, and the L-shaped plate comprises a horizontal plate and a vertical plate. straight 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 superior. 3. The laboratory spectrometer according to 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. laboratory spectrometer according to claim 1, is characterized in that, the outlet of described X-ray source is provided with light-shielding device and light-absorbing device successively, and described light-shielding device is set to block the X-ray source The light-absorbing device is arranged to absorb fluorescence and scattering of X-rays near the outlet of the X-ray source. 5. The laboratory spectrometer according to claim 1, wherein the motion assembly comprises a first linear displacement stage, a second linear displacement stage, a third linear displacement stage, a linkage mechanism, and a first rotary displacement stage and an attitude adjustment translation platform, the first linear translation platform and the second linear translation platform are fixed on the base, the first linear translation platform faces the X-ray source, and the second linear translation platform The linear displacement platform forms an included angle with the first linear displacement platform, and the two ends of the linkage mechanism are respectively located on the first linear displacement platform and the second linear displacement platform, and the linkage mechanism can be relatively The first linear displacement stage slides and rotates, and the linkage mechanism can rotate relative to the second linear displacement stage; the first rotary displacement stage is fixed at one end of the linkage mechanism, and the third linear displacement stage The platform is fixed on the other end of the linkage mechanism; the attitude adjustment translation platform is set on the first rotary translation platform, the crystal bending assembly is fixed on the attitude adjustment translation platform, and the detection assembly is fixed on the on the third linear translation stage. 6. The laboratory spectrometer according to claim 5, wherein the linkage mechanism comprises a first connecting plate and a second connecting plate connected to each other, and a rotating bracket is fixed on the first linear displacement stage, A first driven turntable is fixed on the rotating support, and a slider bracket is arranged on the first driven turntable, and the slider bracket is slidably connected with the first connecting plate, and the first rotating displacement table is fixed On the rotating bracket; the second linear displacement platform is provided with a riser block, the riser block is provided with a second driven turntable, and the second connecting plate is arranged on the second driven turntable above, the third linear displacement stage is arranged on the second connecting plate. 7. The laboratory spectrometer according to claim 6, wherein the rotating bracket comprises a rotating base, a rotating shaft and a mounting base, and the two ends of the rotating shaft are respectively connected to the rotating base and the mounting base, The first driven turntable is fixed on the rotating base, the rotating base is fixed on the first linear displacement platform, and the first rotating displacement platform is fixed on the mounting seat; the first A chute is provided on the connecting plate, the rotating shaft passes through the chute and the first driven turntable, and the rotating base and the mounting seat are respectively located above and below the first connecting plate. 8. The laboratory spectrometer according to claim 5, wherein the attitude adjustment translation platform comprises a fourth linear translation platform and a second rotation translation platform, and the second rotation translation platform is arranged on the fourth On the linear translation platform, the fourth linear translation platform is arranged on the first rotary translation platform, and the crystal bending assembly is arranged on the second rotary translation platform. 9. The laboratory spectrometer according to claim 1, wherein the positioning frame comprises a positioning base and a positioning ring, the positioning base is fixed on the moving assembly, and the positioning ring is fixed on the positioning On the base, the curved spherical crystal is snapped into the positioning ring, and the positioning ring is provided with a screw cap. 10. The laboratory spectrometer according to claim 1, wherein the support frame comprises a support base, a sample holder and a detector support mechanism, and the sample holder and the detector support mechanism are fixed on the support On the base, the support base is fixed on the moving assembly, the sample is fixed on the sample holder, and the detector is fixed on the detector supporting mechanism. 11. The laboratory spectrometer according to claim 10, wherein the sample holder comprises an adapter plate, a fixed plate is fixed on the adapter plate, and a cover plate and a magnetic piece are arranged on the fixed plate , the magnetic piece adsorbs the cover plate on the fixed plate, and the sample is clamped between the magnetic piece and the cover plate; the magnetic piece, the cover plate, the fixed plate and The adapter plates are all provided with through holes. 12. The laboratory spectrometer according to claim 11, wherein a protrusion is provided on the side of the magnetic member close to the cover plate, and a receiving groove is opened on the protrusion to accommodate the Sample; the cover plate and the fixed plate are provided with grooves, the fixed plate groove is used to accommodate the cover plate, and the groove of the cover plate is used to accommodate the protrusion. 13. The laboratory spectrometer according to claim 10, wherein the detector supporting mechanism comprises two oppositely arranged supports, and the two supports are provided with insulating base plates, and the insulating base plates are fixed on the two supports , the detector is fixed on the insulating base plate and located behind the sample. 14. The laboratory spectrometer according to claim 13, wherein the end of the detector is provided with a protective cover, the protective cover is provided with holes, and the protective cover is fixed on the insulating base . 15. The laboratory spectrometer according to claim 1, wherein a plurality of lifting rings and a plurality of fixing pieces are arranged on the base. 16. The laboratory spectrometer according to claim 1, further comprising a helium storage device fixed on the base, and helium is stored in the helium storage device. 17. The laboratory spectrometer according to claim 16, wherein the helium storage device comprises a box body, and the box body comprises an upper cover plate, a lower cover plate, and a first side plate connected end to end in sequence, The second side plate, the third side plate, the fourth side plate and the fifth side plate, the upper cover plate is connected with the upper end of each side plate, the lower cover plate is connected with the lower end of each side plate, and the box body Helium is stored inside; the first side plate has a first opening, the third side plate has a second opening, the fourth side plate has a third opening, the first opening, the second opening and the third opening are sealed by adhesive tape, so that the inside of the box body is formed into a sealed environment. 18. The laboratory spectrometer according to claim 17, further comprising an air inlet pipeline and an air outlet pipeline, both of which communicate with the inside of the box body. 19. The laboratory spectrometer according to claim 17, wherein the helium storage device further comprises a support mechanism, the box body is fixed on the support mechanism, and the support mechanism is fixed on the base seat.

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