Synchrotron radiation scanning imaging system

Abstract

The invention provides a synchrotron radiation scanning imaging system which comprises a first support, a second support and a third support, a through hole is formed in the first support so that X-rays input from the outside can penetrate through the through hole, and the first support is provided with a diffraction assembly, a first lens and a second lens, the diffraction assembly is installed on the first support and used for diffracting the X-rays and focusing the X-rays to obtain X-ray focusing light spots; the sample assembly is used for bearing samples; the laser interference assembly is used for emitting emission laser and receiving reflection laser, calculating an optical path difference generated by vibration between the emission laser and the reflection laser, and converting the optical path difference into a first electric signal; the controller is connected with the laser interference assembly and the sample assembly, and the controller is used for controlling the sample assembly to move based on the first electric signal, so that the X-ray focusing light spot is aligned with the sample for radiation, and an X-ray radiation signal is obtained; and the detection assembly is used for performing laminated coherent diffraction imaging or scanning transmission X-ray microscopic imaging on the sample through the X-ray radiation signal.

Description

Technical Field

[0001] The present disclosure relates to the technical fields of nuclear science and technology, synchrotron radiation experimental technology, precision translation stage system, and laser interferometer application, and more specifically, to a synchrotron radiation scanning imaging system. Background Art

[0002] Synchrotron radiation spectroscopy imaging is an important means to study and solve the problem of non-uniform distribution in materials. Many studies in the fields of energy catalysis, lightweight materials, life and health, geological environment, quantum materials, etc. face the problem of non-uniform systems, such as: research on high-performance batteries, lightweight composite materials on aircraft, research on cell diseases, formation and prevention of heavy metal pollution, components, valence states, electron cloud (bond) orientations, spin orientations in complex quantum materials, etc. These all require the use of spectroscopy microscopy imaging technology with excellent spatial resolution, chemical resolution, and orientation resolution capabilities.

[0003] Synchrotron radiation scanning transmission x-ray microscopy (STXM) is one of the most common spectral imaging techniques. The hardware device of this technology includes three parts: spot focusing system, sample scanning system, and detection system. The spatial resolution of this technology is determined by the size of the focused spot. In the soft X-ray band, the main focusing optical element currently used is the Fresnel zone plate, and its spatial resolution is determined by the width of the outermost ring of the Fresnel zone plate, which is usually around 25nm.

[0004] On the other hand, the development of the fourth-generation synchrotron radiation technology has brought new breakthroughs to STXM technology, such as the stacked coherent diffraction imaging technology Ptychography. Ptychography is a combination of STXM and coherent diffraction imaging technology (CDI). The highly coherent incident X-rays of the fourth-generation synchrotron radiation source have brought STXM technology the opportunity to achieve coherent diffraction imaging, which may achieve ultra-high resolution imaging of 1nm~3nm. However, this places high demands on the position stability of the system and also places unprecedented strict requirements on the mechanical design and selection of the entire set of equipment. Summary of the invention

[0005] In order to solve at least one of the technical problems in the prior art, an embodiment of the present disclosure provides a synchrotron radiation scanning imaging system that can ensure the dynamic stability of the relative position between the diffraction component and the sample component.

[0006] The embodiment of the present disclosure provides a synchrotron radiation scanning imaging system, comprising: a first bracket, a through hole is provided on the first bracket to allow X-rays input from the outside to pass through, and the first bracket carries: a diffraction component, which is installed on the first bracket, and the diffraction component is used to diffract the X-rays and focus them to obtain an X-ray focused spot; a sample component, which is used to carry a sample; a laser interference component, which is used to emit a transmitting laser and receive a reflected laser, and calculate the optical path difference between the transmitting laser and the reflected laser due to vibration, and convert the optical path difference into a first electrical signal, and the reflected laser represents the reflected laser that is sent to the sample component and then returns to the laser interference component; a controller, which is connected to the laser interference component and the sample component, and the controller is used to control the movement of the sample component based on the first electrical signal, so that the X-ray focused spot is aimed at the sample to radiate, and obtain an X-ray radiation signal; a detection component, which is used to perform stacked coherent diffraction imaging on the sample or scanning transmission X-ray microscopy imaging on the sample through the X-ray radiation signal.

[0007] According to some embodiments of the present disclosure, the laser interference assembly includes: a laser transceiver unit, which is arranged on the first bracket, and the laser transceiver unit is used to emit the emission laser and receive the reflected laser; a reflector, which is arranged on the sample assembly, and the reflector is used to receive the emission laser and reflect it back to the laser transceiver unit; a detection unit, which is connected to the laser transceiver unit, and the detection unit is used to collect the optical path difference between the emission laser and the reflected laser, and convert the optical path difference into the first electrical signal.

[0008] According to some embodiments of the present disclosure, there are two laser transceiver units, there are two reflectors, the two emitted lasers are emitted along a first direction and a second direction respectively, and are incident on the two reflectors along a direction perpendicular to the planes where the two reflectors are located, and the first direction is perpendicular to the second direction.

[0009] According to some embodiments of the present disclosure, the diffraction component includes: a wave zone plate, mounted on the first bracket, the wave zone plate is used to receive the X-rays and focus the X-rays to obtain the X-ray focused spot; a level selection hole, mounted on the first bracket, the geometric center of the level selection hole is aligned with the geometric center of the wave zone plate in a third direction, the level selection hole is used to select the diffraction order of the X-ray focused spot, wherein the third direction is perpendicular to the first direction, and the third direction is perpendicular to the second direction.

[0010] According to some embodiments of the present disclosure, the above-mentioned selection hole is provided with: a fluorescence detector for collecting X-ray fluorescence formed when the above-mentioned sample absorbs the above-mentioned X-rays due to the release of energy due to electron transition.

[0011] According to some embodiments of the present disclosure, a first three-dimensional displacement platform is arranged below the above-mentioned first bracket and the above-mentioned detection component, and each of the above-mentioned first three-dimensional displacement platforms includes: a first slide rail, configured to drive the above-mentioned first bracket or the above-mentioned detection component to move in the above-mentioned first direction; a lifting platform, arranged on the above-mentioned first slide rail, and the above-mentioned lifting platform is configured to drive the above-mentioned first bracket or the above-mentioned detection component to move in the above-mentioned second direction; a second slide rail, arranged on the above-mentioned lifting platform, and the above-mentioned second slide rail is configured to drive the above-mentioned first bracket or the above-mentioned detection component to move in the above-mentioned third direction.

[0012] According to some embodiments of the present disclosure, the detection assembly includes: a two-dimensional detector, which is arranged on the second slide rail, and the two-dimensional detector is configured to perform stacked coherent diffraction imaging of the sample through the X-ray radiation signal; a point detector, which is arranged on the second slide rail and is arranged parallel to the two-dimensional detector in the first direction, and the point detector is configured to convert the X-ray radiation signal into a second electrical signal and amplify the second electrical signal to perform scanning transmission X-ray microscopy imaging of the sample; a photoelectron detector, which is arranged above the point detector, and the photoelectron detector is configured to obtain the partial electron yield information of the sample through the X-ray radiation signal.

[0013] According to some embodiments of the present disclosure, the sample assembly includes: a first two-dimensional translation stage, configured to drive the sample assembly to move in the first direction and the second direction; a second two-dimensional translation stage, disposed on the first two-dimensional translation stage, wherein the second two-dimensional translation stage is configured to control the movement of the second two-dimensional translation stage in the first direction and the second direction via the controller upon receiving the first electrical signal, so that the X-ray focusing spot is aligned with the sample for radiating.

[0014] According to some embodiments of the present disclosure, when performing two-dimensional imaging on the above-mentioned sample, the above-mentioned sample assembly includes: a two-dimensional sample holder, mounted on the above-mentioned second two-dimensional translation stage, and the above-mentioned two-dimensional sample holder is provided with a plurality of spaced holes, each of the above-mentioned holes is used to carry the above-mentioned sample.

[0015] According to some embodiments of the present disclosure, when performing three-dimensional imaging on the above-mentioned sample, the above-mentioned sample assembly includes: a second three-dimensional translation stage, which is arranged on the above-mentioned second two-dimensional translation stage; a three-dimensional sample holder, which is installed on the above-mentioned second three-dimensional translation stage, and the above-mentioned three-dimensional sample holder is used to carry the above-mentioned sample; wherein the above-mentioned second three-dimensional translation stage is configured to drive the above-mentioned three-dimensional sample holder to move in the above-mentioned first direction and the above-mentioned third direction, and to rotate around the axis where the above-mentioned second direction is located.

[0016] According to a synchrotron radiation scanning imaging system of an embodiment of the present disclosure, a through hole is provided on the first bracket to allow X-rays input from the outside to pass through, the first bracket carries a diffraction component, the diffraction component is installed on the first bracket, the diffraction component is used to diffract and focus the X-rays to obtain an X-ray focused spot, the sample component is used to carry the sample, the laser interference component is used to emit a transmitting laser and receive a reflected laser, and calculate the optical path difference between the transmitting laser and the reflected laser due to vibration, and convert the optical path difference into a first electrical signal, the reflected laser represents the reflected laser that returns to the laser interference component after the transmitting laser is sent to the sample component, the controller is connected to the laser interference component and the sample component, the controller is used to control the movement of the sample component in real time based on the first electrical signal to compensate for the position deviation, thereby realizing active vibration reduction, and can ensure the dynamic stability of the relative position between the diffraction component and the sample component, so that the X-ray focused spot is aligned with the sample to radiate, and an X-ray radiation signal is obtained, and the detection component is used to perform stacked coherent diffraction imaging of the sample or scanning transmission X-ray microscopy imaging of the sample through the X-ray radiation signal. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 is a stereoscopic diagram of a synchrotron radiation scanning imaging system according to an exemplary embodiment of the present disclosure;

[0018] Figure 2 is a perspective view of a first bracket according to an exemplary embodiment of the present disclosure;

[0019] Figure 3 is a partial enlarged view of part A of a synchrotron radiation scanning imaging system according to an exemplary embodiment of the present disclosure;

[0020] Figure 4 is a stereogram of a diffraction assembly and a first three-dimensional translation stage according to an exemplary embodiment of the present disclosure;

[0021] Figure 5 is a stereoscopic diagram of a detection assembly and a first three-dimensional translation stage according to an illustrative embodiment of the present disclosure;

[0022] Figure 6 is a perspective view of a sample assembly according to an illustrative embodiment of the present disclosure;

[0023] Figure 7 is a stereoscopic view of a second bracket and a two-dimensional sample holder according to an exemplary embodiment of the present disclosure;

[0024] Figure 8 is a stereoscopic diagram of a second three-dimensional translation stage and a three-dimensional sample holder according to an exemplary embodiment of the present disclosure;

[0025] Fig. 9 is a YX axis open-loop and closed-loop displacement-time diagram in a vacuum environment according to an illustrative embodiment of the present disclosure;

[0026] Fig.10 It is a YX-axis closed-loop 5nm step diagram in a vacuum environment according to an illustrative embodiment of the present disclosure.

[0027] In the drawings, the meanings of the reference numerals are as follows:

[0028] 1. The first bracket;

[0029] 100, through hole;

[0030] 2. Zone plate;

[0031] 3. Level selection hole;

[0032] 4. Laser transceiver unit;

[0033] 5. Optical adjustment frame;

[0034] 6. First slide rail;

[0035] 7. Lifting platform;

[0036] 8. Second slide rail;

[0037] 9. Substrate;

[0038] 10. Second bracket;

[0039] 11. Two-dimensional sample holder;

[0040] 110, hole position;

[0041] 12. Three-dimensional sample holder;

[0042] 13. Second three-dimensional translation stage X;

[0043] 14. Second three-dimensional translation stage Z;

[0044] 15. Second three-dimensional translation stage θ;

[0045] 16. Adapter plate;

[0046] 17. Spring steel sheet;

[0047] 18. Reflector;

[0048] 19. Second two-dimensional translation stage;

[0049] 20. The first two-dimensional translation stage X;

[0050] 21. The first two-dimensional translation stage Y;

[0051] 22. Two-dimensional detector;

[0052] 23. Point detector;

[0053] 24. Photoelectron detector;

[0054] 25. Support plate;

[0055] 26. The third three-dimensional translation stage;

[0056] 27. Invar steel plate. DETAILED DESCRIPTION

[0057] Hereinafter, embodiments of the present disclosure will be described with reference to the accompanying drawings. However, it should be understood that these descriptions are exemplary only and are not intended to limit the scope of the present disclosure. In the following detailed description, for ease of explanation, many specific details are set forth to provide a comprehensive understanding of the embodiments of the present disclosure. However, it is apparent that one or more embodiments may also be implemented without these specific details. In addition, in the following description, descriptions of known structures and technologies are omitted to avoid unnecessary confusion of the concepts of the present disclosure.

[0058] The terms used herein are only for describing specific embodiments and are not intended to limit the present disclosure. The terms "comprise", "include", etc. used herein indicate the existence of the features, steps, operations and / or components, but do not exclude the existence or addition of one or more other features, steps, operations or components.

[0059] All terms (including technical and scientific terms) used herein have the meanings commonly understood by those skilled in the art unless otherwise defined. It should be noted that the terms used herein should be interpreted as having a meaning consistent with the context of this specification and should not be interpreted in an idealized or overly rigid manner.

[0060] In the case of using expressions such as "at least one of A, B, and C, etc.", it should generally be interpreted in accordance with the meaning of the expression generally understood by those skilled in the art (for example, "a system having at least one of A, B, and C" should include but is not limited to a system having A alone, B alone, C alone, A and B, A and C, B and C, and / or A, B, C, etc.). In the case of using expressions such as "at least one of A, B, or C, etc.", it should generally be interpreted in accordance with the meaning of the expression generally understood by those skilled in the art (for example, "a system having at least one of A, B, or C" should include but is not limited to a system having A alone, B alone, C alone, A and B, A and C, B and C, and / or A, B, C, etc.).

[0061] Synchrotron radiation scanning transmission x-ray microscopy (STXM) is one of the most common spectral imaging techniques. The hardware device of this technology includes three parts: spot focusing system, sample scanning system, and detection system. The X-ray focusing element focuses the incident X-ray into a nano-spot (probe). Then, through the relative movement of the sample, the probe spot is used to scan and measure the sample. The signal generated by the sample is collected by various detectors placed at different positions, thereby achieving the purpose of scanning microscopic analysis, such as XAS / XRF / XEOL and even XRD in the soft X-ray band.

[0062] On the other hand, the development of the fourth generation of synchrotron radiation technology has brought new breakthroughs to STXM technology, such as the stacked coherent diffraction imaging technology Ptychography. Ptychography is a combination of STXM and coherent diffraction imaging technology (CDI). This technology uses a coherent light spot focused by a zone plate to scan the sample, and collects diffraction signals through a two-dimensional detector. These diffraction patterns contain the relative position information between different scattering points in the object, which is the Fourier transform of the sample's electron density. The sample scanning points are partially overlapped in space to obtain correlation information, and finally the electron density distribution information of the sample in real space is inverted from these diffraction patterns through an iterative algorithm. Coherent diffraction imaging technology is essentially a computational imaging technology. Its spatial resolution is no longer limited by optical focusing elements and can be below 10 nanometers, even close to the wavelength limit of 1nm. The main factors that determine the resolution of coherent diffraction imaging are the coherent photon flux and the position stability of the system.

[0063] In order to solve the problem of position stability, according to the inventive concept of one aspect of the present disclosure, a through hole is opened on the first bracket to allow X-rays input from the outside to pass through, the first bracket carries a diffraction component, the diffraction component is installed on the first bracket, the diffraction component is used to diffract and focus the X-rays to obtain an X-ray focused spot, the sample component is used to carry the sample, the laser interference component is used to emit a transmitting laser and receive a reflected laser, and calculate the optical path difference between the transmitting laser and the reflected laser due to vibration, and convert the optical path difference into a first electrical signal, the reflected laser represents the reflected laser that returns to the laser interference component after the transmitting laser is sent to the sample component, the controller is connected to the laser interference component and the sample component, the controller is used to control the movement of the sample component in real time based on the first electrical signal to compensate for the position deviation, thereby realizing active vibration reduction, and can ensure the dynamic stability of the relative position between the diffraction component and the sample component, so that the X-ray focused spot is aligned with the sample for radiating to obtain an X-ray radiation signal, and the detection component is used to perform stacked coherent diffraction imaging of the sample or scanning transmission X-ray microscopy imaging of the sample through the X-ray radiation signal.

[0064] Figure 1 is a stereoscopic diagram of a synchrotron radiation scanning imaging system according to an illustrative embodiment of the present disclosure.

[0065] According to an embodiment of the present disclosure, a synchrotron radiation scanning imaging system is provided, such as Figure 1 As shown, it includes a first bracket 1, a sample assembly, a laser interference assembly, a controller and a detection assembly. A through hole 100 is provided on the first bracket 1 to allow X-rays input from the outside to pass through. The first bracket 1 carries a diffraction assembly, which is installed on the first bracket 1. The diffraction assembly is used to diffract and focus X-rays to obtain an X-ray focused spot. The sample assembly is used to carry the sample. The laser interference assembly is used to emit a transmitting laser and receive a reflected laser, and calculate the optical path difference between the transmitting laser and the reflected laser due to vibration, and convert the optical path difference into a first electrical signal. The reflected laser represents the reflected laser that is sent to the sample assembly and then returned to the laser interference assembly. The controller is connected to the laser interference assembly and the sample assembly. The controller is used to control the movement of the sample assembly based on the first electrical signal so that the X-ray focused spot is aligned with the sample for radiation to obtain an X-ray radiation signal. The detection assembly is used to perform stacked coherent diffraction imaging of the sample or scanning transmission X-ray microscopy imaging of the sample through the X-ray radiation signal.

[0066] According to an embodiment of the present disclosure, the vibration is caused during the sample replacement process or by the external environment. The vibration of the external environment is, for example, the sound of a chassis fan rotating, the flow of air, and the like.

[0067] According to the embodiment of the present disclosure, the diffraction assembly and the sample assembly share a substrate 9, and the substrate 9 is arranged below the first three-dimensional displacement stage and the first two-dimensional displacement stage under the first bracket 1. A plurality of threaded holes are arranged on the substrate 9, so that the first three-dimensional displacement stage and the first two-dimensional displacement stage have a certain relative adjustment range thereon. The multi-hole design can also speed up the air flow speed on the surface of the substrate when evacuating the vacuum, so that the vacuum degree on the surface of the substrate 9 is more uniform. In the experiment, these threaded holes can also increase the heat dissipation area, providing a better heat dissipation effect for the first three-dimensional displacement stage and the first two-dimensional displacement stage. In order to reduce the relative vibration between the zone plate 2 and the sample, the two share a substrate 9 connected to a low thermal expansion Invar steel plate 27. The detector assembly is supported by another support plate 25. This design can prevent the vibration and heat of the detector assembly from being transferred to the precision piezoelectric displacement stage system.

[0068] Figure 2 is a stereoscopic view of a first bracket according to an exemplary embodiment of the present disclosure.

[0069] According to the embodiments of the present disclosure, Figure 2 As shown, the first bracket 1 adopts a special-shaped integrated structure, made of lightweight and high-strength seventh-series aluminum alloy material, and weighs only 354.17g. The load-bearing capacity of the first three-dimensional displacement platform set below the first bracket 1 is relatively limited. Therefore, a triangular hollow design is adopted on the side of the first bracket 1 to reduce the weight of the first bracket 1 while also trying to make the center of gravity located at the center of the first three-dimensional displacement platform. After the load calculation of the first three-dimensional displacement platform, the load margin is 142.7g, and the design meets the load requirements.

[0070] According to an embodiment of the present disclosure, the sample may be a nanosheet or a nanoparticle.

[0071] According to an embodiment of the present disclosure, a through hole 100 is provided on the first bracket 1 to allow X-rays input from the outside to pass through. The first bracket 1 carries a diffraction component, which is installed on the first bracket 1. The diffraction component is used to diffract and focus the X-rays to obtain an X-ray focused spot. The sample component is used to carry the sample. The laser interference component is used to emit a transmitting laser and receive a reflected laser, and calculate the optical path difference between the transmitting laser and the reflected laser due to vibration, and convert the optical path difference into a first electrical signal. The reflected laser represents the reflected laser that returns to the laser interference component after the transmitting laser is sent to the sample component. The controller is connected to the laser interference component and the sample component. The controller is used to control the movement of the sample component in real time based on the first electrical signal to compensate for the position deviation, thereby realizing active vibration reduction, and can ensure the dynamic stability of the relative position between the diffraction component and the sample component, so that the X-ray focused spot is aligned with the sample for radiating to obtain an X-ray radiation signal. The detection component is used to perform stacked coherent diffraction imaging of the sample or scanning transmission X-ray microscopy imaging of the sample through the X-ray radiation signal.

[0072] Figure 3 It is a partial enlarged view of part A of a synchrotron radiation scanning imaging system according to an illustrative embodiment of the present disclosure.

[0073] According to the embodiments of the present disclosure, Figure 3 As shown, the laser interference assembly includes a laser transceiver unit 4, a reflector 18 and a detection unit. The laser transceiver unit is arranged on the first bracket 1, and the laser transceiver unit 4 is used to emit a transmission laser and receive a reflected laser. The reflector 18 is arranged on the sample assembly, and the reflector 18 is used to receive the transmission laser and reflect it back to the laser transceiver unit 4. The detection unit is connected to the laser transceiver unit 4, and the detection unit is used to collect the optical path difference between the transmission laser and the reflected laser, and convert the optical path difference into a first electrical signal.

[0074] According to the embodiments of the present disclosure, the operating wavelength of the laser transceiver unit 4 needs to deviate from the soft X-ray band to avoid generating noise signals. The hollow design of the first bracket 1 can ensure that the installation of the laser transceiver unit 4 remains stable, providing a guarantee for the smooth progress of the experiment. The optical adjustment frame 5 is mounted on the first bracket 1, and the laser transceiver unit 4 is mounted on the optical adjustment frame 5. The optical adjustment frame 5 can be a precision optical adjustment frame, and the optical adjustment frame 5 uses a three-point adjustment method to change the pitch angle of the laser transceiver unit 4.

[0075] According to an embodiment of the present disclosure, a spring steel sheet 17 is installed on the sample assembly, and the reflector 18 is fixed on the spring steel sheet 17 by bonding. For example, AB glue can be used to stick the reflector 18 on the spring steel sheet 17. The spring steel sheet 17 is installed on the sample assembly in a three-point fixing manner, two of which adopt a "screw-spring" structure, and the other point adopts a threaded connection, thereby achieving the angle adjustment of the reflector 18. The thickness of the spring steel sheet 17 will affect its elastic deformation ability, and thus affect the adjustment ability of the reflector 18. After testing with spring steel sheets 17 with thicknesses of 5 mm, 8 mm and 12 mm respectively, the spring steel sheet 17 with a thickness of 8 mm is preferably installed.

[0076] According to an embodiment of the present disclosure, a reflector 18 arranged on the sample assembly receives a transmission laser emitted by a laser transceiver unit 4 arranged on the first bracket 1 and reflects the transmission laser back to the laser transceiver unit 4. The detection unit collects the optical path difference between the transmission laser and the reflected laser, and converts the optical path difference into a first electrical signal, so as to obtain the relative displacement between the diffraction assembly and the sample assembly due to the vibration of the external environment.

[0077] According to the embodiments of the present disclosure, Figure 3 As shown, there are two laser transceiver units 4 and two reflectors 18. The two transmitted lasers are emitted in a first direction and a second direction respectively, and are incident on the two reflectors 18 in a direction perpendicular to the planes where the two reflectors 18 are located respectively. The first direction and the second direction are perpendicular to each other.

[0078] According to an embodiment of the present disclosure, there are two laser transceiver units 4, two reflectors 18, and the two lasers are emitted in a first direction and a second direction respectively. The first direction is as follows: Figure 3 The X direction in the second direction is Figure 3 In the Y direction, the two emitted lasers are incident on the two reflecting mirrors 18 along directions perpendicular to the planes where the two reflecting mirrors 18 are located.

[0079] According to the embodiment of the present disclosure, the laser optical path monitors the relative displacement between the diffraction assembly and the sample assembly from the X direction and the Y direction respectively. The focal length range of the zone plate 2 in the diffraction assembly varies between 4.2 mm and 27.2 mm. In order to ensure that the emitted laser can always irradiate the reflector 18 when the zone plate 2 is moved, the reflector 18 must have a sufficient length. During two-dimensional imaging at room temperature, the maximum distance of the six samples carried on the sample assembly in the X direction is 12.5 mm, and the maximum distance in the Y direction is 7.5 mm. When the zone plate 2 moves, it is necessary to ensure that all samples can be aligned. Therefore, the reflector 18 that receives the emitted laser incident along the Y direction has a size of 40 mm × 30 mm, and the reflector 18 that receives the emitted laser incident along the X direction has a size of 40 mm × 17.5 mm, which can meet the large travel range of the zone plate 2.

[0080] Figure 4 is a stereoscopic diagram of a diffraction assembly and a first three-dimensional translation stage according to an illustrative embodiment of the present disclosure.

[0081] According to the embodiments of the present disclosure, Figure 4 As shown, the diffraction assembly includes a zone plate 2 and a level selection hole 3. The zone plate 2 is mounted on the first bracket 1, and the zone plate 2 is used to receive and focus the X-rays to obtain an X-ray focused spot. The level selection hole 3 is mounted on the first bracket 1, and the geometric center of the level selection hole 3 is aligned with the geometric center of the zone plate 2 in a third direction, and the level selection hole 3 is used to select the diffraction order of the X-ray focused spot. The third direction is perpendicular to the first direction, and the third direction is perpendicular to the second direction.

[0082] According to an embodiment of the present disclosure, the third direction is as follows Figure 4 The Z direction in .

[0083] According to the embodiment of the present disclosure, the zone plate 2 is integrated on the Si3N4 substrate. The zone plate 2 itself is very fragile and easily damaged, which makes its installation, replacement and maintenance difficult. First, the Si3N4 substrate is bonded to a cylindrical bracket. The bracket can be made of copper, which is convenient for replacement and can also enhance its stability. Then, the bracket is installed on the first bracket 1. The zone plate bracket and the first bracket 1 are designed to be hollow in the third direction (the direction of the optical path of the X-ray) to ensure that the X-ray can pass unimpeded. The Si3N4 substrate has a high degree of integration and can carry multiple zone plates 2 at the same time, so that the zone plates 2 can be flexibly switched as needed during the experiment, which greatly improves the convenience and efficiency of the experiment.

[0084] According to the embodiment of the present disclosure, after the soft X-ray is diffracted by the wave zone plate 2, different orders of X-ray focused spots will be diffracted along the optical axis direction, so it is necessary to install an OSA 3, which is combined with the center of the wave zone plate 2. The OSA 3 is used to select the diffraction order of the X-ray focused spot. When the energy of the X-ray changes, the distance between the OSA 3 and the wave zone plate 2 is adjusted so that the geometric center of the OSA 3 is aligned with the geometric center of the wave zone plate 2 in the third direction, that is, the central axis of the OSA 3 is consistent with that of the wave zone plate 2. The OSA 3 is additionally installed with an independent third three-dimensional displacement stage 26, which is configured to drive the OSA 3 to move in the first direction, the second direction and the third direction.

[0085] According to an embodiment of the present disclosure, a fluorescence detector is provided on the grade selection hole 3. The fluorescence detector is used to collect X-ray fluorescence formed by releasing energy due to electron transition after the sample absorbs X-rays.

[0086] Figure 5 is a stereoscopic diagram of a detection assembly and a first three-dimensional translation stage according to an illustrative embodiment of the present disclosure.

[0087] According to the embodiments of the present disclosure, Figure 1 , Figure 4 and Figure 5 As shown, a first three-dimensional displacement platform is provided below the first bracket 1 and the detection assembly, and each first three-dimensional displacement platform includes a first slide rail 6, a lifting platform 7, and a second slide rail 8. The first slide rail 6 is configured to drive the first bracket 1 or the detection assembly to move in the first direction. The lifting platform 7 is arranged on the first slide rail 6, and the lifting platform 7 is configured to drive the first bracket 1 or the detection assembly to move in the second direction. The second slide rail 8 is arranged on the lifting platform 7, and the second slide rail 8 is configured to drive the first bracket 1 or the detection assembly to move in the third direction.

[0088] According to an embodiment of the present disclosure, in the room temperature two-dimensional imaging experimental mode, the zone plate 2 must be able to be independently adjusted to perform optical path alignment, and the relative position of the zone plate 2 and the sample must also be adjusted, so the zone plate 2 is installed together with the first bracket 1 on the first three-dimensional translation stage.

[0089] According to the embodiment of the present disclosure, the first three-dimensional displacement stage is arranged below the first bracket 1. The first three-dimensional displacement stage can be a high-precision friction piezoelectric displacement stage, which has the advantages of fast heat dissipation and small vibration. The lifting platform 7 is arranged on the first slide rail 6, and the second slide rail 8 is arranged on the lifting platform 7, which can avoid the collision between the diffraction component and the sample component. Since the space between the diffraction component and the sample component is narrow, and the sample is close to the precision optical components such as the wave zone plate 2 and the level selection hole 3, when changing the sample, the components such as the wave zone plate 2 and the level selection hole 3 are first moved out as a whole through the second slide rail 8 to ensure sufficient space for sample change. After changing the sample, the wave zone plate 2 and the level selection hole 3 are moved to the working position.

[0090] According to an embodiment of the present disclosure, the first three-dimensional translation stage arranged under the detection assembly adopts a vacuum stepper motor translation stage. The vacuum stepper motor translation stage has the advantages of strong load-bearing capacity and wide travel range, so as to obtain the most accurate sample structure information, and also greatly facilitates the rapid switching between different detectors in the detector assembly.

[0091] According to the embodiments of the present disclosure, Figure 5 As shown, the detection assembly includes a two-dimensional detector 22, a point detector 23 and a photoelectron detector 24. The two-dimensional detector 22 is arranged on the second slide rail 8, and the two-dimensional detector 22 is configured to perform stacked coherent diffraction imaging of the sample through X-ray radiation signals. The point detector 23 is arranged on the second slide rail 8 and is arranged parallel to the two-dimensional detector 22 in the first direction. The point detector 23 is configured to convert the X-ray radiation signal into a second electrical signal and amplify the second electrical signal to perform scanning transmission X-ray microscopic imaging of the sample. The photoelectron detector 24 is arranged above the point detector 23, and the photoelectron detector 24 is configured to obtain partial electron yield information of the sample through the X-ray radiation signal.

[0092] According to an embodiment of the present disclosure, the two-dimensional detector 22 may be a sCMOS detector, which has the advantages of high sensitivity, wide dynamic range, low noise, and excellent performance, and can meet the needs of soft X-ray coherent diffraction imaging experiments.

[0093] According to the embodiment of the present disclosure, the point detector 23 can achieve rapid response and accurate counting of single photons. The point detector 23 performs scanning transmission X-ray microscopy imaging on the sample. The point detector 23 can be an avalanche photodiode (APD). Due to the limitation of the layout space, the point detector 23 and the two-dimensional detector 22 are both integrated on the second slide rail 8 of the first three-dimensional displacement stage, and the point detector 23 and the two-dimensional detector 22 are arranged in parallel in the first direction. In order to further meet the needs of the soft X-ray coherent diffraction imaging experiment, the positions of the point detector 23 and the two-dimensional detector 22 can be switched and adjusted at any time to improve the flexibility and efficiency of the experiment.

[0094] According to an embodiment of the present disclosure, the photoelectron detector 24 (Channel Electron Multipliers, CEM) uses the ionization effect of ionizing radiation to measure the radiation intensity, and the photoelectron detector 24 is integrated above the point detector 23, so that while obtaining partial electron yield information (PEY detection) of the sample, the photoelectron detector 24 is used to obtain the light intensity of the direct transmission signal. This configuration can compare the PEY signal and the X-ray absorption spectrum (XAS) signal to gain a deeper understanding of the properties of the sample. The photoelectron detector 24 can also obtain partial electron yield information of the sample through the X-ray radiation signal. In this configuration, the sample detection surfaces of the two-dimensional detector 22, the point detector 23, and the photoelectron detector 24 should face one side of the sample to ensure the effective collection of the X-ray radiation signal.

[0095] Figure 6 is a perspective view of a sample assembly according to an illustrative embodiment of the present disclosure, Figure 7 is a stereoscopic view of a second bracket and a two-dimensional sample holder according to an exemplary embodiment of the present disclosure.

[0096] According to the embodiments of the present disclosure, Figure 6 As shown, the sample assembly includes a first two-dimensional translation stage and a second two-dimensional translation stage 19. The first two-dimensional translation stage is configured to drive the sample assembly to move in a first direction and a second direction. The second two-dimensional translation stage 19 is disposed on the first two-dimensional translation stage, and the second two-dimensional translation stage 19 is configured to control the second two-dimensional translation stage 19 to move in the first direction and the second direction via a controller when receiving a first electrical signal, so that the X-ray focus spot is aligned with the sample for irradiation.

[0097] According to the embodiment of the present disclosure, in the room temperature two-dimensional imaging experiment, the sample assembly carries multiple samples (more than 6) at a time, so the first two-dimensional displacement stage and the second two-dimensional displacement stage 19 must have a sufficiently large stroke. Therefore, a combination of a coarse adjustment stage and a fine adjustment stage is adopted, that is, the first two-dimensional displacement stage is a coarse adjustment stage for a wide range of position adjustment, and the second two-dimensional displacement stage 19 is a fine adjustment stage to achieve high-precision scanning positioning, which can achieve a large adjustment range and a movement accuracy of approximately 1nm. The first two-dimensional displacement stage is adjusted in the X direction (the first two-dimensional displacement stage X 20) and the Y direction (the first two-dimensional displacement stage Y 21), and the movement accuracy of the first two-dimensional displacement stage X 20 and the first two-dimensional displacement stage Y 21 is 0.04μm, and the movement range is 63mm and 20mm respectively. The second two-dimensional displacement stage 19 thereon has X-direction and Y-direction adjustment, with a movement accuracy of 1μm and a movement range of 100μm.

[0098] According to the embodiment of the present disclosure, the parameters of the translation stage are shown in Table 1.

[0099] Table 1 Selection parameters of the translation stage

[0100]

[0101] According to the embodiments of the present disclosure, through the combination of macro and micro, the first three-dimensional translation stage (friction piezoelectric translation stage) and the second two-dimensional translation stage 19 (piezoelectric direct-drive translation stage) are used to control the relative movement between the wave zone plate 2 and the sample, and the first electrical signal of the laser interference component is used to drive the second two-dimensional translation stage 19 in real time to compensate for the position deviation, thereby realizing closed-loop active vibration reduction, and being able to achieve an accurate displacement dynamic range of approximately 8 orders of magnitude (63mm stroke, 1nm accuracy), laying the foundation for high-resolution imaging of a few nanometers at the fourth-generation synchrotron radiation source.

[0102] According to an embodiment of the present disclosure, when a sample is subjected to two-dimensional imaging, Figure 7 As shown, the sample assembly includes a two-dimensional sample holder 11, which is mounted on a second two-dimensional displacement stage 19. The two-dimensional sample holder 11 is provided with a plurality of holes 110 arranged at intervals, and each hole 110 is used to carry a sample.

[0103] According to an embodiment of the present disclosure, the sample assembly also includes a second bracket 10. In the case of two-dimensional imaging of the sample, the second bracket 10 and the two-dimensional sample holder 11 form a two-dimensional sample stage. The second bracket 10 is mounted on the second two-dimensional displacement stage 19 through the adapter plate 16, and the two-dimensional sample holder 11 is mounted on the second bracket 10. Since the experiment is in a vacuum environment, it is difficult to replace the sample. In order to improve the experimental efficiency, the placement and removal of the two-dimensional sample holder 11 need to be accurate and convenient, and have the advantages of high positioning accuracy and easy fixation. The two-dimensional sample holder 11 adopts an inverted trapezoidal sample holder design, and is provided with 6 holes 110 for placing samples. It can place multiple samples at a time to improve the experimental efficiency, and can also avoid large-scale movement when changing samples, which is conducive to stable operation. The diameter of the hole 110 is 3mm. In the experiment, the copper mesh sample can be fixed in the hole 110, or the Si3N4 window can be used to support the sample. The fastening screw on the second bracket 10 has a positioning slot, which can quickly install and remove the inverted trapezoidal sample holder with accurate positioning. In addition, this structure is also convenient for the design and installation of the in-situ sample pool.

[0104] Figure 8 is a stereoscopic diagram of a second three-dimensional translation stage and a three-dimensional sample holder according to an illustrative embodiment of the present disclosure.

[0105] According to an embodiment of the present disclosure, when a sample is subjected to three-dimensional imaging, Figure 8 As shown, the sample assembly includes a second three-dimensional translation stage and a three-dimensional sample holder 12. The second three-dimensional translation stage is arranged on a second two-dimensional translation stage 19. The three-dimensional sample holder 12 is mounted on the second three-dimensional translation stage, and the three-dimensional sample holder 12 is used to carry the sample. The second three-dimensional translation stage is configured to drive the three-dimensional sample holder 12 to move in the first direction and the third direction, and to rotate around the axis where the second direction is located.

[0106] According to the embodiment of the present disclosure, when performing room temperature three-dimensional imaging of a sample, it is necessary to Figure 6 The second bracket 10 and the two-dimensional sample holder 11 are replaced with a second three-dimensional displacement stage and a three-dimensional sample holder 12, and the second three-dimensional displacement stage and the three-dimensional sample holder 12 form a three-dimensional sample stage, and the second three-dimensional displacement stage is installed on the second two-dimensional displacement stage 19 through the adapter plate 16. The second three-dimensional displacement stage includes a second three-dimensional displacement stage X 13, a second three-dimensional displacement stage Z 14 and a second three-dimensional displacement stage 15, the second three-dimensional translation stage X 13 and the second three-dimensional translation stage Z 14 can realize two-dimensional translation. 15 can realize θ rotation, with a rotation range of 0~360° and a repeatability of 25μ°. During the experiment, it is necessary to realize two-dimensional scanning imaging at different angles and finally perform three-dimensional reconstruction. The three-dimensional sample holder 12 can use various types of OMNY sample holders, which can meet the testing needs of various samples such as particles, copper mesh loads, Si3N4 window loads, etc.

[0107] According to the embodiments of the present disclosure, the interchange between room temperature two-dimensional imaging and high-resolution three-dimensional imaging is achieved by replacing the sample stage. The X-ray focused spot (nano X-ray spot) is irradiated onto the sample, and STXM two-dimensional point scanning imaging and Ptychography coherent imaging can be performed respectively. For STXM, the designed X-ray focused spot has a spot size of no more than 30nm at the focal point. To achieve high spatial resolution imaging below 7nm, ptychography technology is required, so high requirements are placed on the movement accuracy and stability of the sample stage.

[0108] According to an embodiment of the present disclosure, in order to isolate the transmission of vibration, a marble material with good vibration absorption performance is used as the overall supporting structure under the overall device of the synchrotron radiation scanning imaging system.

[0109] Example

[0110] According to the implementation scheme proposed in this case, a set of model samples was built. In this embodiment, all components except the translation stage are precision machined at a 1:1 ratio, and the translation stage is replaced by an aluminum block of the same size and material to ensure the reliability of the test results. The piezoelectric scanning stage has a stroke of 100 microns and a resonant frequency of 80Hz@200g load. The repeatability of the laser interferometer component is no more than 1nm, and the maximum bandwidth is 2.9 MHz.

[0111] In order to simulate the actual operating environment of the STXM system, the device was assembled and placed in a vacuum chamber for testing. The chamber was placed on a vibration-isolating optical platform with a vacuum degree of 200 Pa. Two lasers were used to test the relative vibration of the diffraction component and the sample component in the Y and X directions respectively.

[0112] Fig. 9 1 is a YX axis open-loop and closed-loop displacement-time diagram in a vacuum environment according to an illustrative embodiment of the present disclosure.

[0113] When the stage is stationary, data is collected for 30 seconds in the "open loop" and "closed loop" states of the nanoscanner, and the time domain vibration spectrum is plotted. Fig. 9As shown in the data, in the open-loop state, that is, when only vibration is monitored without active vibration reduction, there is obvious position drift between the diffraction component and the sample component, and the position changes are irregular and messy. In the closed-loop control state, the position drift phenomenon over a long period of time is significantly suppressed, and the irregular jitter is relatively reduced.

[0114] Fig.10 It is a YX-axis closed-loop 5nm step diagram in a vacuum environment according to an illustrative embodiment of the present disclosure.

[0115] In addition to the static state, the position stability of the translation stage in motion is also very important. Therefore, under closed-loop control, the second two-dimensional translation stage performs a step-type motion of 5 nm in the X and Y directions respectively. The position test results are as follows: Fig.10 The results show that the 5nm step in the X and Y directions can be clearly displayed and completely separated, which means that the amplitude PV value of the relative vibration of the diffraction component and the sample component is less than 5nm (PV, Peak to Valley), that is, the change from the peak to the trough is less than 5nm.

[0116] The root mean square (RMS) value of the data is calculated according to the following formula (1):

[0117] RMS= (1);

[0118] Where N is the total number of data points in the vibration data set, X i Represented as each data point in the data set, that is, the specific value of the vibration data, i=0, 1, 2…

[0119] From formula (1), we can get the position standard deviation in the X direction to be 0.622nm, and the position standard deviation in the Y direction to be 0.690nm, which shows that the closed-loop feedback between the laser interferometer component and the nanopiezoelectric stage can effectively suppress such vibrations. Such a low vibration level can ensure that the 2nm spatial resolution imaging will not be blurred due to the relative jitter of the diffraction component and the sample component.

[0120] Based on the core idea of ​​active vibration reduction, the present invention combines laser interferometer component sensing, a large-range high-precision nano-combined displacement stage system and a control system to ensure the dynamic stability of the relative position between the zone plate and the sample, laying the foundation for realizing synchrotron radiation scanning transmission X-ray microscopy with a resolution of a few nanometers.

[0121] It will be appreciated by those skilled in the art that the features described in the various embodiments and / or claims of the present disclosure may be combined or coupled in a variety of ways, even if such combinations or couplings are not explicitly described in the present disclosure. In particular, the features described in the various embodiments and / or claims of the present disclosure may be combined or coupled in a variety of ways without departing from the spirit and teachings of the present disclosure. All of these combinations and / or couplings fall within the scope of the present disclosure.

[0122] It should also be noted that the directional terms mentioned in the embodiments, such as "upper", "lower", "front", "back", "left", "right", etc., are only reference directions of the drawings and are not intended to limit the scope of protection of the present disclosure. Throughout the drawings, the same elements are represented by the same or similar reference numerals. Conventional structures or configurations will be omitted when they may cause confusion in the understanding of the present disclosure, and the shapes and sizes of the components in the drawings do not reflect the actual size and proportion, but only illustrate the contents of the embodiments of the present disclosure.

[0123] Unless otherwise indicated, the numerical parameters in this specification and the appended claims are approximate values ​​and can be changed according to the desired properties obtained by the content of the present disclosure. Specifically, all numbers used in the specification and claims to express the content of the composition, reaction conditions, etc., should be understood to be modified by the term "about" in all cases. In general, the meaning of the expression is to include changes in some embodiments of ±10%, in some embodiments of ±5%, in some embodiments of ±1%, and in some embodiments of ±0.5% by a specific number.

[0124] The ordinal numbers used in the specification and claims, such as "first", "second", "third", etc., to modify the corresponding elements, do not themselves mean that the elements have any ordinal numbers, nor do they represent the order of one element and another element, or the order in the manufacturing method. The use of these ordinal numbers is only used to clearly distinguish a component with a certain name from another component with the same name.

[0125] In addition, unless the steps are specifically described or must occur in sequence, the order of the above steps is not limited to the above list, and can be changed or rearranged according to the required design. And the above embodiments can be mixed and matched with each other or with other embodiments based on design and reliability considerations, that is, the technical features in different embodiments can be freely combined to form more embodiments.

[0126] The embodiments of the present disclosure are described above. However, these embodiments are only for illustrative purposes and are not intended to limit the scope of the present disclosure. Although the embodiments are described above separately, this does not mean that the measures in the various embodiments cannot be used in combination to advantage. The scope of the present disclosure is defined by the attached claims and their equivalents. Without departing from the scope of the present disclosure, those skilled in the art may make a variety of substitutions and modifications, which should all fall within the scope of the present disclosure.

Claims

1. A synchrotron radiation scanning imaging system, wherein: include: A first bracket, wherein a through hole is provided on the first bracket to allow X-rays input from the outside to pass through, and the first bracket carries: a diffraction component mounted on the first bracket, wherein the diffraction component is used to diffract and focus the X-rays to obtain a focused X-ray spot; A sample assembly, used for carrying a sample; A laser interference assembly, configured to emit a transmitted laser and receive a reflected laser, calculate an optical path difference between the transmitted laser and the reflected laser due to vibration, and convert the optical path difference into a first electrical signal, wherein the reflected laser represents the reflected laser that is returned to the laser interference assembly after the transmitted laser is sent to the sample assembly; a controller connected to the laser interference assembly and the sample assembly, the controller being used to control the movement of the sample assembly based on the first electrical signal so that the X-ray focused spot is aligned with the sample to radiate and obtain an X-ray radiation signal; The detection component is used to perform stacked coherent diffraction imaging of the sample or scanning transmission X-ray microscopy imaging of the sample through the X-ray radiation signal.

2. The synchrotron radiation scanning imaging system according to claim 1, wherein: The laser interference assembly comprises: A laser transceiver unit, disposed on the first bracket, and configured to emit the transmitted laser and receive the reflected laser; A reflector, disposed on the sample assembly, for receiving the emitted laser and reflecting it back to the laser transceiver unit; A detection unit is connected to the laser transceiver unit, and is used to collect the optical path difference between the emitted laser and the reflected laser, and convert the optical path difference into the first electrical signal.

3. The synchrotron radiation scanning imaging system according to claim 2, wherein: There are two laser transceiver units and two reflectors. The two emitted lasers are emitted in a first direction and a second direction respectively, and are incident on the two reflectors in directions perpendicular to the planes where the two reflectors are located respectively. The first direction and the second direction are perpendicular to each other.

4. The synchrotron radiation scanning imaging system according to claim 3, wherein: The diffraction component comprises: a zone plate, mounted on the first bracket, the zone plate being used to receive the X-ray and focus the X-ray to obtain the X-ray focused spot; A level selection hole is mounted on the first bracket, the geometric center of the level selection hole is aligned with the geometric center of the wave zone plate in a third direction, and the level selection hole is used to select the diffraction order of the X-ray focused spot, wherein the third direction is perpendicular to the first direction, and the third direction is perpendicular to the second direction.

5. The synchrotron radiation scanning imaging system according to claim 4, wherein: The level selection hole is provided with: The fluorescence detector is used to collect X-ray fluorescence generated by the energy released by electron transition after the sample absorbs the X-ray.

6. The synchrotron radiation scanning imaging system according to claim 4, wherein: A first three-dimensional displacement platform is disposed below the first bracket and the detection assembly, and each of the first three-dimensional displacement platforms includes: A first slide rail is configured to drive the first bracket or the detection assembly to move in the first direction; a lifting platform, disposed on the first slide rail, and configured to drive the first bracket or the detection assembly to move in the second direction; A second slide rail is disposed on the lifting platform, and the second slide rail is configured to drive the first bracket or the detection component to move in the third direction.

7. The synchrotron radiation scanning imaging system according to claim 6, wherein: The detection component comprises: a two-dimensional detector, disposed on the second slide rail, and configured to perform stacked coherent diffraction imaging of the sample through the X-ray radiation signal; a point detector, disposed on the second slide rail and arranged in parallel with the two-dimensional detector in the first direction, the point detector being configured to convert the X-ray radiation signal into a second electrical signal and amplify the second electrical signal to perform scanning transmission X-ray microscopic imaging of the sample; A photoelectron detector is arranged above the point detector, and the photoelectron detector is configured to obtain the partial electron yield information of the sample through the X-ray radiation signal.

8. The synchrotron radiation scanning imaging system according to claim 6, wherein: The sample assembly includes: A first two-dimensional translation stage, configured to drive the sample assembly to move in the first direction and the second direction; The second two-dimensional translation stage is arranged on the first two-dimensional translation stage, and the second two-dimensional translation stage is configured to control the second two-dimensional translation stage to move in the first direction and the second direction via the controller when receiving the first electrical signal, so that the X-ray focusing spot is aimed at the sample for irradiation.

9. The synchrotron radiation scanning imaging system according to claim 8, wherein: In the case of performing two-dimensional imaging on the sample, the sample assembly comprises: The two-dimensional sample holder is mounted on the second two-dimensional displacement stage. The two-dimensional sample holder is provided with a plurality of holes arranged at intervals, and each of the holes is used to carry the sample.

10. The synchrotron radiation scanning imaging system according to claim 8, wherein: In the case of performing three-dimensional imaging on the sample, the sample assembly comprises: A second three-dimensional translation stage, arranged on the second two-dimensional translation stage; A three-dimensional sample holder, mounted on the second three-dimensional displacement stage, and the three-dimensional sample holder is used to carry the sample; The second three-dimensional translation stage is configured to drive the three-dimensional sample holder to move in the first direction and the third direction, and to rotate around an axis where the second direction is located.

Images