Synchronous radiation scanning imaging system

Abstract

The present disclosure provides a kind of synchrotron scanning imaging system, comprising: first support, first support is opened with through hole, to allow by the X-ray of external input to pass through, first support is carried with: diffraction component is installed on first support, diffraction component is used to diffract X-ray and focus, obtains X-ray focused spot;Sample component is used to carry sample;Laser interference component is used to emit emission laser and receive reflected laser, and the optical path difference between emission laser and reflected laser due to vibration is calculated, and the optical path difference is converted into first electric signal;Controller is connected with laser interference component and sample component, controller is used to control sample component to move based on first electric signal, so that X-ray focused spot is aligned sample and is radiated, obtains X-ray radiation signal;Detection component is used to carry out laminar coherent diffraction imaging or scanning transmission X-ray microscopic imaging to sample by X-ray radiation signal.

Description

Technical Field

[0001] This disclosure relates to the technical fields of nuclear science and technology, synchrotron radiation experimental technology, precision displacement stage systems, and laser interferometer applications, and more specifically, to a synchrotron radiation scanning imaging system. Background Technology

[0002] Synchrotron radiation spectroscopic imaging is an important tool for studying and solving problems related to non-uniform distribution in materials. Many research fields, including energy catalysis, lightweight materials, life sciences, geology and environment, and quantum materials, face the challenge of non-uniform systems. Examples include research on high-performance batteries, lightweight composite materials for aircraft, cell-related diseases, the formation and prevention of heavy metal pollution, and the inhomogeneity of components, valence states, electron cloud (bond) orientation, and spin orientation in complex quantum materials. These all require the use of spectroscopic microscopy imaging techniques that simultaneously possess excellent spatial resolution, chemical resolution, and orientation resolution capabilities.

[0003] Synchrotron radiation scanning transmission X-ray microscopy (STXM) is one of the most common spectroscopic imaging techniques. The hardware of this technique consists of three parts: a beam focusing system, a sample scanning system, and a detection system. The spatial resolution of this technique is determined by the size of the focused beam. In the soft X-ray band, the main focusing optics currently used are Fresnel zone plates, whose spatial resolution is determined by the width of the outermost ring of the Fresnel zone plate, typically around 25 nm.

[0004] On the other hand, the development of fourth-generation synchrotron radiation technology has brought new breakthroughs to STXM technology, such as ptychography, a technique combining STXM with coherent diffraction imaging (CDI). The highly coherent incident X-rays from fourth-generation synchrotron radiation sources provide STXM with the opportunity to achieve coherent diffraction imaging, potentially enabling ultra-high resolution imaging at 1nm to 3nm. However, this places high demands on system positional stability and imposes unprecedentedly stringent requirements on the mechanical design and selection of the entire system. Summary of the Invention

[0005] To address at least one of the technical problems in the prior art, embodiments of this disclosure provide a synchrotron radiation scanning imaging system capable of ensuring dynamic stability of the relative positions between the diffraction components and the sample components.

[0006] This disclosure provides a synchrotron radiation scanning imaging system, comprising: a first support with a through-hole to allow externally input X-rays to pass through; a diffraction assembly mounted on the first support for diffracting and focusing the X-rays to obtain a focused X-ray spot; a sample assembly for carrying a sample; a laser interferometer for emitting and receiving reflected laser light, calculating the optical path difference between the emitted and reflected laser light due to vibration, and converting the optical path difference into a first electrical signal; the reflected laser light representing the reflected laser light that returns to the laser interferometer after being sent to the sample assembly; a controller connected to the laser interferometer and the sample assembly for controlling the movement of the sample assembly based on the first electrical signal, so that the focused X-ray spot is aligned with the sample for radiation to obtain an X-ray radiation signal; and a detection assembly for performing stacked coherent diffraction imaging or scanning transmission X-ray microscopy imaging on the sample using the X-ray radiation signal.

[0007] According to some embodiments of this disclosure, the laser interference assembly includes: a laser transceiver unit disposed on the first support, the laser transceiver unit being used to emit the emitted laser and receive the reflected laser; a reflector disposed on the sample assembly, the reflector being used to receive the emitted laser and reflect it back to the laser transceiver unit; and a detection unit connected to the laser transceiver unit, the detection unit being 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.

[0008] According to some embodiments of this disclosure, the laser transceiver unit has two components, and the reflector has two components. The two 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 plane where the two reflectors are located. The first direction and the second direction are perpendicular to each other.

[0009] According to some embodiments of this disclosure, the diffraction assembly includes: a zone plate mounted on the first support, the zone plate being used to receive and focus the X-rays to obtain the focused X-ray spot; and a diffraction order aperture mounted on the first support, the geometric center of the diffraction order aperture being aligned with the geometric center of the zone plate in a third direction, the diffraction order aperture being used to select the diffraction order of the focused X-ray spot, wherein the third direction is perpendicular to the first direction and perpendicular to the second direction.

[0010] According to some embodiments of this disclosure, the above-mentioned graded selection aperture is provided with a fluorescence detector for collecting X-ray fluorescence formed by the release of energy due to electron transition after the sample absorbs the above-mentioned X-rays.

[0011] According to some embodiments of this disclosure, a first three-dimensional displacement stage is provided below both the first support and the detection component. Each of the first three-dimensional displacement stages includes: a first slide rail configured to drive the first support or the detection component to move in the first direction; a lifting platform disposed on the first slide rail, configured to drive the first support or the detection component to move in the second direction; and a second slide rail disposed on the lifting platform, configured to drive the first support or the detection component to move in the third direction.

[0012] According to some embodiments of this disclosure, the detection assembly includes: a two-dimensional detector disposed on the second slide rail, the two-dimensional detector being configured to perform stacked coherent diffraction imaging of the sample using the X-ray radiation signal; a point detector disposed on the second slide rail and arranged parallel to 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 microscopy imaging of the sample; and a photoelectron detector disposed above the point detector, the photoelectron detector being configured to obtain the partial electron yield information of the sample using the X-ray radiation signal.

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

[0014] According to some embodiments of this disclosure, when performing two-dimensional imaging on the above-mentioned sample, the sample assembly includes: a two-dimensional sample holder, which is mounted on the second two-dimensional displacement stage, and the two-dimensional sample holder has a plurality of spaced holes, each of which is used to hold the sample.

[0015] According to some embodiments of this disclosure, when performing three-dimensional imaging on the above-mentioned sample, the sample assembly includes: a second three-dimensional displacement stage disposed on the second two-dimensional displacement stage; and a three-dimensional sample holder mounted on the second three-dimensional displacement stage, wherein the three-dimensional sample holder is used to support the above-mentioned sample; wherein the second three-dimensional displacement stage is configured to drive the three-dimensional sample holder to move upward in the first direction and the third direction, and to rotate about the axis containing the second direction.

[0016] According to an embodiment of the present disclosure, a synchrotron radiation scanning imaging system includes a first support with a through hole to allow externally input X-rays to pass through. A diffraction component is mounted on the first support and is used to diffract and focus X-rays to obtain a focused X-ray spot. A sample component is used to carry a sample. A laser interferometer is used to emit and receive reflected lasers, calculate the optical path difference between the emitted and reflected lasers 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 interferometer after being sent to the sample component. A controller is connected to the laser interferometer 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 positional deviations, thereby achieving active vibration reduction. This ensures the dynamic stability of the relative position between the diffraction component and the sample component, allowing the focused X-ray spot to radiate onto the sample and obtain an X-ray radiation signal. A detection component is used to perform stacked coherent diffraction imaging or scanning transmission X-ray microscopy imaging of the sample using the X-ray radiation signal. Attached Figure Description

[0017] Figure 1 This is a perspective view of a synchrotron radiation scanning imaging system according to an illustrative embodiment of the present disclosure;

[0018] Figure 2 This is a perspective view of a first support according to an illustrative embodiment of the present disclosure;

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

[0020] Figure 4 This is a perspective view of a diffraction assembly and a first three-dimensional displacement stage according to an illustrative embodiment of the present disclosure;

[0021] Figure 5 This is a perspective view of a detection component and a first three-dimensional displacement stage according to an illustrative embodiment of the present disclosure;

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

[0023] Figure 7 This is a perspective view of a second support and a two-dimensional sample holder according to an illustrative embodiment of the present disclosure;

[0024] Figure 8 This is a perspective view of a second three-dimensional displacement stage and a three-dimensional sample holder according to an illustrative embodiment of the present disclosure;

[0025] Figure 9 This is an example of an embodiment of the present disclosure showing open-loop and closed-loop displacement-time diagrams of the YX axis in a vacuum environment.

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

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

[0028] 1. First support;

[0029] 100. Through hole;

[0030] 2. Zone plates;

[0031] 3. Stage 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 support;

[0039] 11. Two-dimensional sample holder;

[0040] 110. Hole position;

[0041] 12. Three-dimensional sample holder;

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

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

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

[0045] 16. Adapter board;

[0046] 17. Spring steel sheet;

[0047] 18. Reflector;

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

[0049] 20. First two-dimensional displacement stage X;

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

[0056] 27. Invar steel plate. Detailed Implementation

[0057] The embodiments of the present disclosure will now 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 disclosure. In the following detailed description, numerous specific details are set forth to provide a thorough understanding of the embodiments of the present disclosure for ease of explanation. However, it will be apparent that one or more embodiments may be practiced without these specific details. Furthermore, descriptions of well-known structures and techniques are omitted in the following description to avoid unnecessarily obscuring the concepts of the present disclosure.

[0058] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit this disclosure. The terms “comprising,” “including,” etc., as used herein indicate the presence of the stated features, steps, operations, and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, or components.

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

[0060] When using expressions such as "at least one of A, B, and C," the expression should generally be interpreted in accordance with the meaning commonly understood by a person skilled in the art (e.g., "a system having at least one of A, B, and C" should include, but is not limited to, systems having A alone, having B alone, having C alone, having A and B, having A and C, having B and C, and / or having A, B, and C, etc.). When using expressions such as "at least one of A, B, or C," the expression should generally be interpreted in accordance with the meaning commonly understood by a person skilled in the art (e.g., "a system having at least one of A, B, or C" should include, but is not limited to, systems having A alone, having B alone, having C alone, having A and B, having A and C, having B and C, and / or having A, B, and C, etc.).

[0061] Synchrotron radiation scanning transmission X-ray microscopy (STXM) is one of the most common spectroscopic imaging techniques. The hardware of this technique consists of three parts: a beam focusing system, a sample scanning system, and a detection system. The X-ray focusing element focuses the incident X-rays into a nano-spot (probe). Then, through the relative motion of the sample, the probe spot scans and measures the sample. The signals generated by the sample are collected by various detectors placed at different positions, thereby achieving the purpose of scanning microscopy analysis, such as XAS / XRF / XEOL and even XRD in the soft X-ray band.

[0062] On the other hand, the development of fourth-generation synchrotron radiation technology has brought new breakthroughs to STXM technology, such as Ptychography, a stacked coherent diffraction imaging technique. Ptychography is a combination of STXM and coherent diffraction imaging (CDI). This technique uses a coherent 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, representing the Fourier transform of the sample's electron density. The spatial overlap between sample scanning points provides correlation information, and finally, an iterative algorithm is used to inversely solve for the sample's real-space electron density distribution from these diffraction patterns. Coherent diffraction imaging is essentially a computational imaging technique, and its spatial resolution is no longer limited by optical focusing elements, reaching below 10 nanometers, and even approaching the wavelength limit of 1 nm. The main factors determining the resolution of coherent diffraction imaging are the coherent photon flux and the system's positional stability.

[0063] To address the issue of positional stability, according to one aspect of the present disclosure, a first support has a through hole to allow externally input X-rays to pass through. A diffraction component is mounted on the first support and is used to diffract and focus X-rays to obtain a focused X-ray spot. A sample assembly is used to hold the sample. A laser interferometer is used to emit and receive reflected laser light, calculate the optical path difference between the emitted and reflected laser light due to vibration, and convert the optical path difference into a first electrical signal. The reflected laser light represents the reflected laser light that returns to the laser interferometer after being sent to the sample assembly. A controller is connected to the laser interferometer and the sample assembly and is used to control the movement of the sample assembly in real time based on the first electrical signal to compensate for positional deviations, thereby achieving active vibration reduction. This ensures the dynamic stability of the relative position between the diffraction component and the sample assembly, allowing the focused X-ray spot to radiate onto the sample and obtain an X-ray radiation signal. A detection component is used to perform stacked coherent diffraction imaging or scanning transmission X-ray microscopy imaging of the sample using the X-ray radiation signal.

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

[0065] A synchrotron radiation scanning imaging system is provided according to embodiments of this disclosure, such as... Figure 1 As shown, the system includes a first support 1, a sample assembly, a laser interferometer assembly, a controller, and a detector assembly. The first support 1 has a through-hole 100 to allow externally input X-rays to pass through. A diffraction assembly is mounted on the first support 1 and is used to diffract and focus X-rays to obtain a focused X-ray spot. The sample assembly carries the sample. The laser interferometer assembly emits and receives reflected laser light, calculates the optical path difference between the emitted and reflected lasers due to vibration, and converts this optical path difference into a first electrical signal. The reflected laser light characterizes the reflected laser light that returns to the laser interferometer assembly after being sent to the sample assembly. The controller is connected to the laser interferometer assembly and the sample assembly. Based on the first electrical signal, the controller controls the movement of the sample assembly so that the focused X-ray spot is aligned with the sample for radiation, obtaining an X-ray radiation signal. The detector assembly is used to perform stacked coherent diffraction imaging or scanning transmission X-ray microscopy imaging of the sample using the X-ray radiation signal.

[0066] According to embodiments of this disclosure, the vibration is caused by the sample changing process or by the external environment, such as the sound of the chassis fan rotating or the flow of air.

[0067] According to embodiments of this disclosure, the diffraction assembly and the sample assembly share a single substrate 9, which is positioned below the first three-dimensional displacement stage and the first two-dimensional displacement stage, located below the first support 1. The substrate 9 has multiple threaded holes, allowing the first three-dimensional and first two-dimensional displacement stages a certain relative adjustment range. The porous design also accelerates the airflow velocity on the substrate surface during vacuuming, resulting in a more uniform vacuum level on the substrate 9 surface. In experiments, these threaded holes also increase the heat dissipation area, providing better heat dissipation for the first three-dimensional and first two-dimensional displacement stages. To reduce the relative vibration between the zone plate 2 and the sample, both are connected to a low-thermal-expansion Invar steel plate 27 via a single substrate 9. The detector assembly is supported by a separate support plate 25. This design prevents vibration and heat transfer from the detector assembly to the precision piezoelectric displacement stage system.

[0068] Figure 2 This is a perspective view of a first support according to an illustrative embodiment of the present disclosure.

[0069] According to embodiments of this disclosure, such as Figure 2 As shown, the first support 1 adopts an integrated, irregularly shaped structure, made of lightweight, high-strength 7-series aluminum alloy, weighing only 354.17g. The load-bearing capacity of the first three-dimensional displacement stage located beneath the first support 1 is relatively limited. Therefore, a triangular hollow design is used on the side of the first support 1 to reduce its weight while also ensuring the center of gravity is positioned as close as possible to the center of the first three-dimensional displacement stage. Load calculations for the first three-dimensional displacement stage show a load margin of 142.7g, which meets the load requirements.

[0070] According to embodiments of this disclosure, the sample may be a nanosheet or nanoparticle.

[0071] According to an embodiment of this disclosure, a through hole 100 is provided on the first support 1 to allow externally input X-rays to pass through. A diffraction component is supported on the first support 1 and is used to diffract and focus X-rays to obtain a focused X-ray spot. A sample component is used to support the sample. A laser interferometer is used to emit emitted laser and receive reflected laser, and calculate the optical path difference between the emitted and reflected lasers 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 interferometer after being sent to the sample component. A controller is connected to the laser interferometer 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 positional deviations, thereby achieving active vibration reduction. This ensures the dynamic stability of the relative position between the diffraction component and the sample component, so that the focused X-ray spot is aligned with the sample for radiation, and an X-ray radiation signal is obtained. A detection component is used to perform stacked coherent diffraction imaging or scanning transmission X-ray microscopy imaging of the sample using the X-ray radiation signal.

[0072] Figure 3 This 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 embodiments of this disclosure, such as Figure 3 As shown, the laser interferometer assembly includes a laser transceiver unit 4, a reflector 18, and a detection unit. The laser transceiver unit 4 is mounted on the first support 1 and is used to emit emitted laser light and receive reflected laser light. The reflector 18 is mounted on the sample assembly and is used to receive emitted laser light and reflect it back to the laser transceiver unit 4. The detection unit is connected to the laser transceiver unit 4 and is used to acquire the optical path difference between the emitted and reflected laser light and convert the optical path difference into a first electrical signal.

[0074] According to embodiments of this 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 ensures the stable installation of the laser transceiver unit 4, providing a guarantee for the smooth conduct 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 embodiments of this disclosure, a spring steel sheet 17 is mounted on the sample assembly, and a reflector 18 is fixed to the spring steel sheet 17 by adhesive bonding. For example, AB glue can be used to attach the reflector 18 to the spring steel sheet 17. The spring steel sheet 17 is mounted on the sample assembly using a three-point fixing method, where two points use a "screw-spring" structure and the third point uses a threaded connection, thereby enabling the angle adjustment of the reflector 18. The thickness of the spring steel sheet 17 affects its elastic deformation capability, and thus affects the adjustment capability of the reflector 18. After testing with spring steel sheets 17 of thicknesses of 5mm, 8mm, and 12mm respectively, a spring steel sheet 17 with a thickness of 8mm is preferred for installation.

[0076] According to an embodiment of this disclosure, a reflector 18 disposed on the sample assembly receives the emitted laser emitted by the laser transceiver unit 4 disposed on the first support 1 and reflects the emitted laser back to the laser transceiver unit 4. The detection unit collects the optical path difference between the emitted laser and the reflected laser and converts the optical path difference into a first electrical signal, thereby obtaining the relative displacement between the diffraction assembly and the sample assembly caused by the vibration of the external environment.

[0077] According to embodiments of this disclosure, such as Figure 3 As shown, there are two laser transceiver units 4 and two reflectors 18. The two lasers are emitted along the first direction and the second direction, respectively, and are incident on the two reflectors 18 along the direction perpendicular to the plane where the two reflectors 18 are located. The first direction and the second direction are perpendicular to each other.

[0078] According to embodiments of this disclosure, the laser transceiver unit 4 has two components, and the reflector 18 has two components. The two emitting lasers are emitted along a first direction and a second direction, respectively. The first direction is as follows: Figure 3 The X direction in the middle, the second direction as... Figure 3 In the Y direction, the two emitted lasers are incident on the two reflectors 18 in a direction perpendicular to the plane where the two reflectors 18 are located.

[0079] According to embodiments of this disclosure, the laser path monitors the relative displacement between the diffraction component and the sample component from the X and Y directions, respectively. The focal length of the zone plate 2 in the diffraction component varies between 4.2 mm and 27.2 mm. To ensure that the emitted laser always illuminates the reflector 18 when the zone plate 2 is moved, the reflector 18 must have sufficient length. During room temperature two-dimensional imaging, the maximum distance between the six samples carried on the sample component 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 needs to be able to align with all samples. 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 range of movement of the zone plate 2.

[0080] Figure 4 This is a perspective view of a diffraction assembly and a first three-dimensional displacement stage according to an illustrative embodiment of the present disclosure.

[0081] According to embodiments of this disclosure, such as Figure 4 As shown, the diffraction assembly includes a zone plate 2 and a diffraction aperture 3. The zone plate 2 is mounted on the first support 1 and is used to receive and focus X-rays to obtain a focused X-ray spot. The diffraction aperture 3 is mounted on the first support 1, and its geometric center is aligned with the geometric center of the zone plate 2 in a third direction. The diffraction aperture 3 is used to select the diffraction order of the focused X-ray spot. The third direction is perpendicular to the first direction and also perpendicular to the second direction.

[0082] According to embodiments of this disclosure, a third party provides such Figure 4 The Z direction in the equation.

[0083] According to embodiments of this disclosure, the zone plate 2 is integrated onto a Si3N4 substrate. The zone plate 2 itself is very fragile and easily damaged, making its installation, replacement, and maintenance difficult. First, the Si3N4 substrate is bonded to a cylindrical bracket, which can be made of copper, facilitating replacement and enhancing stability. Then, this bracket is mounted on a first support 1. Both the zone plate bracket and the first support 1 are designed to be hollow in the third direction (the X-ray path direction) to ensure unobstructed X-ray passage. The Si3N4 substrate has high integration, capable of simultaneously supporting multiple zone plates 2, allowing for flexible switching of the zone plates 2 as needed during experiments, significantly improving the convenience and efficiency of the experiment.

[0084] According to embodiments of this disclosure, after soft X-rays are diffracted by the zone plate 2, they will diffract into X-ray focused spots of different orders along the optical axis. Therefore, an order selection aperture 3 (OSA) is required, which is coupled to the center of the zone plate 2. The OSA 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 and the zone plate 2 is adjusted so that the geometric center of the OSA 3 is aligned with the geometric center of the zone plate 2 in a third direction, that is, the central axis of the OSA 3 is consistent with that of the zone plate 2. The OSA 3 is also equipped 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 this disclosure, a fluorescence detector is provided on the selection aperture 3. The fluorescence detector is used to collect X-ray fluorescence formed by the release of energy due to electron transitions after the sample absorbs X-rays.

[0086] Figure 5 This is a perspective view of a detection component and a first three-dimensional displacement stage according to an illustrative embodiment of the present disclosure.

[0087] According to embodiments of this disclosure, such as Figure 1 , Figure 4 and Figure 5 As shown, a first three-dimensional displacement stage is provided below both the first support 1 and the detection component. Each first three-dimensional displacement stage 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 support 1 or the detection component to move in a first direction. The lifting platform 7 is disposed on the first slide rail 6 and is configured to drive the first support 1 or the detection component to move in a second direction. The second slide rail 8 is disposed on the lifting platform 7 and is configured to drive the first support 1 or the detection component to move in a third direction.

[0088] According to the embodiments of this disclosure, in the room temperature two-dimensional imaging experimental mode, the zone plate 2 needs to be able to be independently adjusted for optical path collimation, and the relative position of the zone plate 2 and the sample also needs to be adjusted. Therefore, the zone plate 2, together with the first support 1, is installed on the first three-dimensional displacement stage.

[0089] According to embodiments of this disclosure, a first three-dimensional displacement stage is disposed below the first support 1. This first three-dimensional displacement stage can be a high-precision triboelectric displacement stage, which has the advantages of rapid heat dissipation and low vibration. A lifting platform 7 is disposed on the first slide rail 6, and a second slide rail 8 is disposed on the lifting platform 7, which can prevent collisions between the diffraction component and the sample component. Because the space between the diffraction component and the sample component is small, and the sample is adjacent to precision optical elements such as the zone plate 2 and the stage selection aperture 3, during sample change, the zone plate 2 and the stage selection aperture 3 are first moved out as a whole via the second slide rail 8 to ensure sufficient space for sample change. After changing the sample, the zone plate 2 and the stage selection aperture 3 are then moved to the working position.

[0090] According to the embodiments of this disclosure, the first three-dimensional displacement stage disposed below the detection assembly is a vacuum stepper motor displacement stage. The vacuum stepper motor displacement stage has the advantages of strong load-bearing capacity and wide stroke range, thereby obtaining the most accurate sample structure information, and also greatly facilitating the rapid switching between different detectors in the detector assembly.

[0091] According to embodiments of this disclosure, such as 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 mounted on the second slide rail 8 and is configured to perform stacked coherent diffraction imaging of the sample using X-ray radiation signals. The point detector 23 is mounted on the second slide rail 8 and arranged parallel to the two-dimensional detector 22 in a 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 microscopy imaging of the sample. The photoelectron detector 24 is positioned above the point detector 23 and is configured to obtain partial electron yield information of the sample using X-ray radiation signals.

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

[0093] According to embodiments of this 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 of the sample. The point detector 23 can be an avalanche photodiode (APD). Due to space constraints, both the point detector 23 and the two-dimensional detector 22 are 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 parallel to each other in the first direction. To further meet the needs of soft X-ray coherent diffraction imaging experiments, the positions of the point detector 23 and the two-dimensional detector 22 can be switched and adjusted at any time, improving the flexibility and efficiency of the experiment.

[0094] According to embodiments of this disclosure, the photoelectron detector 24 (Channel Electron Multipliers, CEM) measures radiation intensity using the ionization effect of ionizing radiation. The photoelectron detector 24 is integrated above the point detector 23 to acquire partial electron yield information (PEY detection) of the sample while simultaneously acquiring the intensity of the direct transmission signal. This configuration allows for comparative analysis of the PEY signal and the X-ray absorption spectrum (XAS) signal, leading to a deeper understanding of the sample's properties. The photoelectron detector 24 can also acquire partial electron yield information of the sample via X-ray radiation signals. In this configuration, the sample detection surfaces of the two-dimensional detector 22, the point detector 23, and the photoelectron detector 24 should face the sample side to ensure effective acquisition of the X-ray radiation signal.

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

[0096] According to embodiments of this disclosure, such as Figure 6 As shown, the sample assembly includes a first two-dimensional displacement stage and a second two-dimensional displacement stage 19. The first two-dimensional displacement stage is configured to drive the sample assembly to move in a first direction and a second direction. The second two-dimensional displacement stage 19 is disposed on the first two-dimensional displacement stage, and the second two-dimensional displacement stage 19 is configured to be controlled by a controller to move in the first direction and the second direction upon receiving a first electrical signal, so that the X-ray focused spot is aligned with the sample for radiation.

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

[0098] According to embodiments of this disclosure, the parameters of the displacement stage are shown in Table 1.

[0099] Table 1 Selection parameters of the displacement stage

[0100]

[0101] According to embodiments of this disclosure, by combining macro and micro methods, a first three-dimensional displacement stage (triboelectric displacement stage) and a second two-dimensional displacement stage 19 (piezoelectric direct-drive displacement stage) are used to control the relative motion between the zone plate 2 and the sample. At the same time, the first electrical signal of the laser interference component is used to drive the second two-dimensional displacement stage 19 in real time to compensate for positional deviations, thereby achieving closed-loop active vibration reduction. This can achieve a precise dynamic range of displacement of approximately eight orders of magnitude (63 mm stroke, 1 nm accuracy), laying the foundation for nanometer-level high-resolution imaging of fourth-generation synchrotron radiation sources.

[0102] According to embodiments of this disclosure, in the case of two-dimensional imaging of a sample, such as 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 has a plurality of spaced holes 110, each hole 110 being used to hold a sample.

[0103] According to embodiments of this disclosure, the sample assembly further includes a second support 10. When performing two-dimensional imaging of the sample, the second support 10 and the two-dimensional sample holder 11 form a two-dimensional sample stage. The second support 10 is mounted on a second two-dimensional displacement stage 19 via an adapter plate 16, and the two-dimensional sample holder 11 is mounted on the second support 10. Since the experiment is conducted in a vacuum environment, sample replacement is difficult. To improve experimental efficiency, the placement and removal of the two-dimensional sample holder 11 needs to be accurate and convenient, possessing high positioning accuracy and easy fixation. The two-dimensional sample holder 11 adopts an inverted trapezoidal sample holder design with six sample placement holes 110. This allows for the placement of multiple samples at once, improving experimental efficiency, and avoids large-scale movement during sample replacement, facilitating stable operation. The diameter of the hole 110 is 3mm. During the experiment, the copper mesh sample can be fixed within the hole 110, or a Si3N4 window can be used to support the sample. The fastening screw on the second support 10 has a positioning slot, allowing for quick installation and removal of the inverted trapezoidal sample holder with precise positioning. Furthermore, this structure also facilitates the design and installation of in-situ sample cells.

[0104] Figure 8 This is a perspective view of a second three-dimensional displacement stage and a three-dimensional sample holder according to an illustrative embodiment of the present disclosure.

[0105] According to embodiments of this disclosure, in the case of performing three-dimensional imaging of a sample, such as Figure 8 As shown, the sample assembly includes a second three-dimensional displacement stage and a three-dimensional sample holder 12. The second three-dimensional displacement stage is disposed on a second two-dimensional displacement stage 19. The three-dimensional sample holder 12 is mounted on the second three-dimensional displacement stage and is used to hold the sample. The second three-dimensional displacement stage is configured to drive the three-dimensional sample holder 12 to move upwards in a first direction and a third direction, and to rotate about the axis containing the second direction.

[0106] According to embodiments of this disclosure, in the case of performing room temperature three-dimensional imaging of a sample, it is necessary to... Figure 6 The second support 10 and the two-dimensional sample holder 11 are replaced with a second three-dimensional displacement stage and a three-dimensional sample holder 12. The second three-dimensional displacement stage and the three-dimensional sample holder 12 form a three-dimensional sample stage. The second three-dimensional displacement stage is mounted on the second two-dimensional displacement stage 19 via an 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 Z 15. 15. The second three-dimensional translation stage X 13 and the second three-dimensional translation stage Z 14 can realize two-dimensional translation. The 15-inch sample holder can achieve theta rotation, with a rotation range of 0~360° and a repeatability of 25μ°. During the experiment, two-dimensional scanning imaging is required at different angles, followed by three-dimensional reconstruction. The three-dimensional sample holder 12 can use various models of OMNY sample holders to meet the testing needs of various samples, including particles, copper mesh loads, and Si3N4 window loads.

[0107] According to embodiments of this disclosure, room-temperature two-dimensional imaging and high-resolution three-dimensional imaging are interchangeable by changing the sample stage. An X-ray focused spot (nano-X-ray spot) irradiates the sample, enabling both STXM two-dimensional point scanning imaging and Ptychography coherent imaging. For STXM, the designed X-ray focused spot size at the focal point is no greater than 30 nm. To achieve high spatial resolution imaging below 7 nm, ptychography is required, thus placing high demands on the accuracy and stability of the sample stage movement.

[0108] According to embodiments of this disclosure, in order to isolate the transmission of vibration, marble with good vibration absorption properties is used as the overall support structure below the synchrotron radiation scanning imaging system.

[0109] Example

[0110] According to the implementation plan proposed in this case, a model sample was constructed. In this embodiment, all components except the displacement stage were precision machined to a 1:1 scale. The displacement stage was replaced with an aluminum block of the same size and material to ensure the reliability of the test results. The piezoelectric scanning stage had a stroke of 100 micrometers and a resonant frequency of 80Hz at a 200g load. The repeatability of the laser interference component was no greater than 1nm, and the maximum bandwidth was 2.9 MHz.

[0111] To simulate the real operating environment of the STXM system, the assembled device was placed inside a vacuum chamber for testing. The chamber was positioned on a vibration-isolation optical platform with a vacuum level of 200 Pa. Two laser beams were used to test the relative vibrations of the diffraction component and the sample component in the Y and X directions, respectively.

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

[0113] With the displacement stage stationary, data were collected for 30 seconds in both the "open loop" and "closed loop" states of the nano-scanning stage, and the time-domain vibration spectrum was plotted as follows. Figure 9As shown in the data, in the open-loop state, i.e., when only vibration is monitored without active vibration damping, there is significant positional drift between the diffraction component and the sample component, and the positional changes are irregular and chaotic. However, in the closed-loop control state, the positional drift over a long time period is significantly suppressed, and the irregular jitter is relatively reduced.

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

[0115] Besides the static state, the positional stability of the displacement stage during motion is also crucial. Therefore, under closed-loop control, the second two-dimensional displacement stage undergoes step-like motions of 5 nm along both the X and Y directions. The position test results are as follows: Figure 10 As shown in the figure. The results show that the 5nm step in both the X and Y directions can be clearly displayed and completely separated, which indicates that the amplitude PV of the relative vibration of the diffraction component and the sample component is less than 5nm (PV, Peak to Valley), that is, the change in amplitude from peak to valley is less than 5nm.

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

[0117] RMS= (1);

[0118] Where N represents the total number of data points in the vibration dataset, X i This is represented by each data point in the dataset, i.e., the specific value of the vibration data, i=0, 1, 2...

[0119] From formula (1), the standard deviation of the position in the X direction is 0.622 nm and the standard deviation of the position in the Y direction is 0.690 nm. This indicates that the closed-loop feedback between the laser interference component and the nano-voltage radio can effectively suppress this type of vibration. Such a low vibration level can ensure that the 2 nm spatial resolution imaging will not become blurred due to the relative jitter of the diffraction component and the sample component.

[0120] Based on the core concept of active vibration reduction, this disclosure combines laser interferometric component sensing, a large-scale 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 resolution of several nanometers.

[0121] Those skilled in the art will understand that the features described in the various embodiments and / or claims of this disclosure can be combined or combined in various ways, even if such combinations or combinations are not explicitly described in this disclosure. In particular, the features described in the various embodiments and / or claims of this disclosure can be combined and / or combined in various ways without departing from the spirit and teachings of this disclosure. All such combinations and / or combinations fall within the scope of this disclosure.

[0122] It should also be noted that the directional terms mentioned in the embodiments, such as "up," "down," "front," "back," "left," and "right," are only for reference to the directions in the accompanying drawings and are not intended to limit the scope of protection of this disclosure. Throughout the drawings, the same elements are represented by the same or similar reference numerals. Conventional structures or constructions will be omitted where they may cause confusion in understanding this disclosure, and the shapes and dimensions of the components in the drawings do not reflect actual size and proportion, but are only schematic representations of the embodiments of this disclosure.

[0123] Unless otherwise stated, the numerical parameters in this specification and the appended claims are approximate values ​​and can be varied according to desired characteristics derived from the content of this disclosure. Specifically, all figures used in the specification and claims to indicate composition, reaction conditions, etc., should be understood to be modified by the term "about" in all cases. Generally, this means that a specific amount may vary by ±10% in some embodiments, ±5% in some embodiments, ±1% in some embodiments, and ±0.5% in some embodiments.

[0124] The use of ordinal numbers such as "first," "second," "third," etc., in the specification and claims to modify the corresponding elements does not imply that the element has any ordinal number, nor does it represent the order of one element with another element, or the order of manufacturing methods. The use of these ordinal numbers is only to enable a named element to be clearly distinguished from another element with the same name.

[0125] Furthermore, unless specifically described or required to occur in a specific order, the order of the above steps is not limited to those listed above and can be varied or rearranged according to the desired design. Moreover, the above embodiments can be used in combination with each other or with other embodiments based on design and reliability considerations; that is, technical features from different embodiments can be freely combined to form more embodiments.

[0126] The embodiments of this disclosure have been described above. However, these embodiments are for illustrative purposes only and are not intended to limit the scope of this disclosure. Although various embodiments have been described above, this does not mean that the measures in the various embodiments cannot be used advantageously in combination. The scope of this disclosure is defined by the appended claims and their equivalents. Various substitutions and modifications can be made by those skilled in the art without departing from the scope of this disclosure, and all such substitutions and modifications should fall within the scope of this disclosure.

Claims

1. A synchrotron radiation scanning imaging system, wherein, include: A first support has a through hole to allow externally input X-rays to pass through. The first support carries a diffraction assembly mounted on the first support. The diffraction assembly is used to diffract and focus the X-rays to obtain a focused X-ray spot. Sample assembly, used to hold the sample; A laser interferometer is used to emit emitted laser light and receive reflected laser light, calculate the optical path difference between the emitted laser light and the reflected laser light due to vibration, and convert the optical path difference into a first electrical signal. The reflected laser light represents the reflected laser light that returns to the laser interferometer after the emitted laser light is sent to the sample assembly. A controller, connected to the laser interference assembly and the sample assembly, 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, thereby obtaining an X-ray radiation signal; The detection component is used to perform stacked coherent diffraction imaging or scanning transmission X-ray microscopy imaging of the sample using the X-ray radiation signal. The laser interference component includes: A laser transceiver unit is mounted on the first bracket, and the laser transceiver unit is used to emit the emitted laser and receive the reflected laser. A reflector is disposed on the sample assembly, the reflector being used to receive the emitted laser and reflect it back to the laser transceiver unit; A detection unit is connected to the laser transceiver unit. The detection unit 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. The laser transceiver unit has two components, and the reflector has two components. The two 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 plane where the two reflectors are located. The first direction and the second direction are perpendicular to each other. The diffraction component includes: A zone plate is mounted on the first support. The zone plate is used to receive the X-rays and focus the X-rays to obtain the focused X-ray spot. A diffraction order selection aperture is mounted on the first support. The geometric center of the diffraction order selection aperture is aligned with the geometric center of the zone plate in a third direction. The diffraction order selection aperture is used to select the diffraction order of the X-ray focused spot. The third direction is perpendicular to the first direction and perpendicular to the second direction. The graded selection hole is provided with: A fluorescence detector is used to collect X-ray fluorescence formed by the release of energy due to electron transitions after the sample absorbs the X-rays. A first three-dimensional displacement stage is provided below both the first support and the detection component, and each first three-dimensional displacement stage includes: The first slide rail is configured to drive the first bracket or the detection component to move in the first direction; A lifting platform is mounted on the first slide rail, and the lifting platform is configured to drive the first bracket or the detection component 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 upward on the third party; The detection component includes: A two-dimensional detector is disposed on the second slide rail, and the two-dimensional detector is configured to perform stacked coherent diffraction imaging of the sample by means of the X-ray radiation signal; A point detector is disposed on the second slide rail and arranged parallel to the two-dimensional detector in the first direction. 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 on the sample. A photoelectron detector is disposed above the point detector and is configured to obtain partial electron yield information of the sample by passing the X-ray radiation signal. The sample assembly includes: A first two-dimensional displacement stage is configured to drive the sample assembly to move in the first direction and the second direction; A second two-dimensional displacement stage is disposed on the first two-dimensional displacement stage. The second two-dimensional displacement stage is configured to move in the first direction and the second direction via the controller when the first electrical signal is received, so that the X-ray focused spot is aligned with the sample for irradiation. The diffraction component and the sample component share a single substrate, and the detection component is supported by a support plate.

2. The synchrotron radiation scanning imaging system according to claim 1, wherein, In the case of performing two-dimensional imaging on the sample, the sample assembly includes: A two-dimensional sample holder is installed on the second two-dimensional displacement stage. The two-dimensional sample holder has a plurality of spaced holes, each of which is used to hold the sample.

3. The synchrotron radiation scanning imaging system according to claim 1, wherein, In the case of performing three-dimensional imaging on the sample, the sample components include: The second three-dimensional displacement stage is set on the second two-dimensional displacement stage; A three-dimensional sample holder is mounted on the second three-dimensional displacement stage, and the three-dimensional sample holder is used to support the sample. The second three-dimensional displacement stage is configured to drive the three-dimensional sample holder to move upward in the first direction and the third direction, and to rotate about the axis containing the second direction.

Images