Integrated Data Collaborative Acquisition Method, Device and Readable Storage Medium for Small-Angle Scattering and Wide-Angle Scattering Based on a Single Crystal Diffractometer

Abstract

The present invention relates to an integrated data collaborative acquisition method, device and readable storage medium for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer. The method realizes vertical fixation of the sample and high-precision control of the incident angle by designing two improved sample holders (the first sample holder is for the grazing incidence mode, and the second sample holder is for the transmission mode) to replace the magnetic head structure of the original single-crystal diffractometer. The first sample holder adopts a structure of "fixed plate + vertical backrest + groove" to fix the sample through a rigid connecting piece; the second sample holder adopts a back plate with a detection hole to support the fixation of the substrate-free film. The present invention breaks through the limitation of the traditional test range, eliminates the signal splicing error, realizes the full-dimensional characterization of the material structure, and is applicable to the depth gradient analysis of thin films, free films and bulk samples.

Description

Technical Field

[0001] The present invention relates to a method, apparatus and readable storage medium for integrated data collaborative acquisition of small-angle scattering and wide-angle scattering based on a single-crystal diffractometer. Background Art

[0002] The existing wide-angle scattering test method based on a single-crystal diffractometer (such as CN113049617B) has the following limitations:

[0003] 1. Inaccurate control of the incident angle: It is difficult to vertically fix a flaky sample by the traditional fixed method of the magnetic head (or crystal ring), and relying on flexible plasticine for fixation leads to angular deviation and sample collapse.

[0004] 2. Limited test range: The starting angle of 2θ in the grazing incidence mode is limited to 3°, and the scattering signals in the small-angle region of 0 - 3° cannot be detected.

[0005] 3. Incomplete signal acquisition: The support rod of the beamstop blocks the scattering signals in the qz direction (perpendicular to the sample surface), and only the information in the qx direction (horizontal direction) can be obtained.

[0006] 4. Signal stitching error: Traditional small-angle and wide-angle scattering need to be collected by separate devices, and the intensity difference leads to manual adjustment during stitching, affecting the objectivity of the data.

[0007] Therefore, there is an urgent need for an integrated data collaborative acquisition method of small-angle scattering and wide-angle scattering based on a single-crystal diffractometer to solve the problems that the existing technology cannot synchronously achieve accurate acquisition of small-angle and wide-angle scattering signals on a single-crystal diffractometer, and there are problems such as low accuracy of incident angle control, signal occlusion in the qz direction, limited test range, and signal stitching error. Summary of the Invention

[0008] The object of the present invention is to provide a method, apparatus and readable storage medium for integrated data collaborative acquisition of small-angle scattering and wide-angle scattering based on a single-crystal diffractometer for the above problems existing in the prior art.

[0009] The core technology of the present invention is mainly to design a rigid sample holder to achieve vertical sample fixation and high-precision incident angle control, combined with specific parameter settings and four-circle diffractometer degree-of-freedom regulation, to break through the occlusion limitation of the beamstop (mainly its two brackets, the first beamstop bracket and the second beamstop bracket), synchronously collect small-angle and wide-angle scattering signals starting from 0.5°, and achieve full-dimensional characterization of the material structure.

[0010] To achieve the above application object, in the first aspect, the present invention adopts the following technical solutions:

[0011] The integrated data collaborative acquisition method for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer includes the following steps:

[0012] S00. Select an improved sample holder according to the requirements of the grazing incidence mode and the transmission mode;

[0013] Among them, the improved sample holder is used to replace the magnetic head on the original sample stage of the single-crystal diffractometer, and the improved sample holder includes a first sample holder for the grazing incidence mode and a second sample holder for the transmission mode;

[0014] The first sample holder includes a fixing plate provided with fixing holes and a vertical backrest higher than the fixing plate. A connecting piece for fixing the sample is provided on the fixing holes. A groove for placing the sample is formed between the vertical backrest and the fixing plate, and a stud for installing on the original sample stage of the single-crystal diffractometer is provided at the bottom of the groove;

[0015] The second sample holder includes a back plate provided with detection holes, and studs for installing on the original sample stage of the single-crystal diffractometer are also provided at the bottom of the back plate;

[0016] S10. Prepare the sample and place it on the improved sample holder, and place it along the direction of the X-ray advancement;

[0017] S20. Select an X-ray light source so that the X-ray light source is aligned with the sample, where the X-ray light source is a gallium target;

[0018] S30. Set the sample rotation angle of the original sample stage of the single-crystal diffractometer, and move the sample back and forth in the y direction until the sample cuts half of the light blocker to find the zero position of the sample;

[0019] S40. Rotate the sample along the incident angle direction on the improved sample holder for scanning, and start the test;

[0020] S50. Set the distance between the sample and the area detector of the single-crystal diffractometer, set the incident angle by setting the sample rotation angle of the original sample stage of the single-crystal diffractometer, and set the exposure time to collect the scattering signal;

[0021] S60. Collect the scattered X-ray signal through a two-dimensional area detector and perform integration through software to obtain the one-dimensional diffraction angle 2theta diagram or one-dimensional scattering diagram of the X-ray.

[0022] Further, in step S30, if the sample is inclined in the vertical direction, change the vertical tilting angle of the original sample stage of the single-crystal diffractometer to adjust the collimation of the sample in the vertical direction.

[0023] Further, in step S50, set the distance between the sample and the detection surface of the single-crystal diffractometer to be 100-240 mm, set the incident angle to be 0.1-1°, and set the exposure time to be 1-60 s.

[0024] Furthermore, in step S00, the depth of the groove is 2 mm.

[0025] Furthermore, in step S00, the diameter of the detection hole is 5 - 8 mm.

[0026] Furthermore, in step S30, the sample rotation angle of the original sample stage of the single crystal diffractometer is set to a value between 85° and 95°.

[0027] Furthermore, in step S00, the sample is fixed to the backing plate by double - sided tape or glue.

[0028] In a second aspect, the present invention provides an electronic device, including a memory and a processor. A computer program is stored in the memory, and the processor is configured to run the computer program to execute the above - mentioned integrated data collaborative acquisition method of small - angle scattering and wide - angle scattering based on a single crystal diffractometer.

[0029] In a third aspect, the present invention provides a readable storage medium, in which a computer program is stored. The computer program includes program codes for controlling a process to execute the process, and the process includes the integrated data collaborative acquisition method of small - angle scattering and wide - angle scattering based on the single crystal diffractometer as described above.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0031] 1. Full - angle coverage and low - angle breakthrough: By optimizing the sample holder design and detector distance (≥200 mm), the starting test angle is extended from 3° (Cu target) in the traditional technology to 0.5°, realizing the integrated acquisition of small - angle scattering (SAXS) and wide - angle scattering (WAXS) signals and covering the full - angle range starting from 0.5°.

[0032] 2. Signal integrity improvement: The sample is vertically fixed and the incident angle is adjusted (0.1 - 1°) to avoid the occlusion of the beamstop, completely capturing the scattering signals in the qz direction (perpendicular to the sample surface), solving the problem of signal loss in the traditional technology and supporting the in - depth analysis of the ordered stacking structure of materials.

[0033] 3. Data objectivity and accuracy: Synchronously acquire small - angle and wide - angle signals, eliminate the subjective error introduced by the intensity difference in manual splicing, and ensure the incident angle accuracy (±0.01°) and data reproducibility through a rigid sample stage and the control of the degrees of freedom of the four - circle diffractometer (Chi, Phi, 2Theta, Omega).

[0034] 4. Application Expansion and Operational Flexibility: It supports the switching between grazing incidence and transmission modes, is applicable to the gradient analysis of the superficial to bulk structure of thin film materials (such as organic photovoltaics and data storage chips), and the improved sample stage is compatible with the original diffractometer base, featuring convenient operation and high safety. Description of the Drawings

[0035] Figure 1 is the flowchart of the method according to an embodiment of the present invention;

[0036] Figure 2 is the schematic structural diagram of the first sample holder according to an embodiment of the present invention;

[0037] Figure 3 is the schematic structural diagram of the second sample holder according to an embodiment of the present invention;

[0038] Figure 4 is the schematic structural diagram of the prior art;

[0039] Figure 5 is the scattering pattern detectable by the prior art;

[0040] Figure 6 is the schematic during the method debugging process according to an embodiment of the present invention Figure 1 ;

[0041] Figure 7 is the schematic during the method debugging process according to an embodiment of the present invention Figure 2 ;

[0042] Figure 8 is the schematic during the method debugging process according to an embodiment of the present invention Figure 3 ;

[0043] Figure 9 is the scattering pattern of the organic small molecule thin film deposited on a silicon substrate according to an embodiment of the present invention;

[0044] Figure 10 is the diffraction angle 2theta pattern of the organic small molecule thin film deposited on a silicon substrate according to an embodiment of the present invention.

[0045] In the figures, 1 is the first sample holder; 2 is the second sample holder; 3 is the magnetic head; 4 is the first beam blocker bracket; 5 is the second beam blocker bracket; 6 is the sample stage; 11 is the fixing plate; 12 is the vertical backrest; 13 is the fixing hole; 14 is the connecting member; 15 is the groove; 21 is the back plate; 22 is the detection hole. Detailed Embodiments

[0046] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention are within the scope of protection of the present invention.

[0047] Those skilled in the art should understand that, in the disclosure of the present invention, the terms "longitudinal", "transverse", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", etc., indicating the orientation or position relationship, are based on the orientation or position relationship shown in the accompanying drawings, which are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, the above terms cannot be understood as limiting the present invention.

[0048] Currently available technologies such as Figure 4 As shown, since the original magnetic head 3 cannot support the sheet sample standing upright on the magnetic head 3, if the vertical sample is fixed on the magnetic head 3 with plasticine, the incident angle cannot be accurately controlled due to the flexibility of the plasticine, and the upright sample will collapse to one side over time. Therefore, the final scattering diagram is as follows Figure 5 As shown, the qz direction (perpendicular to the sample surface) is blocked by the fixed rods of the beamstop (primarily consisting of two brackets: the first beamstop bracket 4 and the second beamstop bracket 5), limiting extraction to the qx direction (horizontal to the sample surface). The single crystal diffractometer, consistent with that disclosed in CN113049617B, features four rotational degrees of freedom: Chi (vertical tilt), Phi (horizontal rotation), 2Theta (detector rotation), and Omega (sample rotation). Furthermore, height adjustment, left-right, and front-back position adjustment on the goniometer head allow for precise sample centering, greater operational controllability, and improved collection of scattered signals. The goniometer head is part of the goniometer. The single crystal diffractometer also features a temperature control system and an imaging system.

[0049] In order to solve the problems existing in the prior art, the present invention proposes the following technical solutions to solve the problems existing in the prior art:

[0050] like Figure 1 As shown, the integrated small-angle scattering and wide-angle scattering data collaborative acquisition method based on a single crystal diffractometer includes the following steps:

[0051] S00, select and improve the sample holder according to the requirements of grazing incidence mode and transmission mode;

[0052] The improved sample holder is used to replace the magnetic head 3 on the original sample stage 6 of the single crystal diffractometer (the magnetic head 3 is directly mounted on the mounting hole of the sample stage 6 via a stud and then fixed with a screw), and the improved sample holder includes a first sample holder 1 for grazing incidence mode and a second sample holder 2 for transmission mode;

[0053] like Figure 2 As shown, the first sample holder 1 includes a fixing plate 11 with a fixing hole 13 and a vertical backrest 12 that is higher than the fixing plate 11. The fixing hole 13 is provided with a connector 14 for fixing the sample. A groove 15 for placing the sample is formed between the vertical backrest 12 and the fixing plate 11. The bottom of the groove 15 is provided with a stud for mounting on the original sample stage 6 of the single crystal diffractometer. The installation method of this stud is the same as that of the original magnetic head 3. During installation, the magnetic head 3 can be removed and replaced with the first sample holder 1.

[0054] The rigidity of the fixture (first sample holder 1) ensures high precision and reproducibility of the incident angle. The upright backrest (high flat plate) aligns the sample vertically, allowing it to stand upright. Horizontally, the sample is secured using screws (connector 14) included with the first sample holder 1. The recess 15 is 2 mm deep and can accommodate nearly any bulk or thin film sample.

[0055] like Figure 3 As shown, the second sample holder 2 includes a support plate 21 with a 5-8 mm detection hole 22. The bottom of the support plate 21 is also provided with a stud for mounting on the original sample stage 6 of the single crystal diffractometer. The installation method of this stud is consistent with the original magnetic head 3. During installation, the magnetic head 3 can be removed and replaced with the second sample holder 2; wherein, the sample is fixed to the support plate 21 by double-sided tape or glue.

[0056] The rigid mold (second sample holder 2) ensures high precision and reproducibility of the incident angle. Double-sided tape is used to vertically support the sample mounted on this mold and allows it to be adjusted to the center of the goniometer, the area irradiated by the X-rays. The detection aperture 22 has a diameter of 5-8 mm and can accommodate all (substrate-free) sheet-like thin film samples.

[0057] S10, preparing the sample and placing it on the improved sample holder, along the direction of X-ray travel;

[0058] S20, selecting an X-ray light source so that the X-ray light source is aimed at the sample, wherein the X-ray light source is a gallium target;

[0059] S30, setting the sample rotation angle of the original sample stage 6 of the single crystal diffractometer to a value between 85 and 95 degrees, and moving the sample back and forth in the y direction until the sample cuts half of the beam stop (beam blocker) to find the zero point position of the sample; Figure 6This is the zero point position when the sample stage 6 moves back and forth, that is, the substrate needs to cut half of the beamstop in the vertical direction. At this time, the substrate is tilted in the vertical direction. Here, chi needs to be adjusted so that the sample is also a straight line in the vertical direction instead of a slant line, and cuts half of the beamstop.

[0060] Among them, Figure 7 As shown, if the sample is tilted in the vertical direction, the vertical tilt angle of the original sample stage 6 of the single crystal diffractometer is changed to adjust the collimation of the sample in the vertical direction.

[0061] like Figure 8 It is the zero point position when the sample stage 6 moves back and forth, that is, the substrate needs to cut the beamstop in half in the vertical direction. At this time, the substrate not only cuts the beamstop in half, but also is perpendicular to the horizontal frame in the vertical direction.

[0062] S40, rotating the sample along the incident angle direction on the improved sample holder for scanning (i.e., changing the omega angle (incident angle)), and starting the test;

[0063] S50, setting the distance between the sample and the surface detector of the single crystal diffractometer to 100-240 mm, setting the incident angle to 0.1-1° (omega angle value) by adjusting the sample rotation angle of the original sample stage 6 of the single crystal diffractometer, and setting the exposure time to 1-60 s to collect the scattered signal;

[0064] like Figure 9 For organic small molecule films deposited on silicon substrates, the distance from the detector to the sample is 100-240 mm, the incident angle is 0.1-1°, and the exposure time is 30-60 seconds.

[0065] S60 , collecting scattered X-ray signals through a two-dimensional surface detector and integrating them through software to obtain a one-dimensional diffraction angle 2theta diagram or a one-dimensional scattering diagram of the X-rays.

[0066] In this step, the software that comes with the device is used to integrate the X-ray one-dimensional diffraction angle 2theta diagram or phase angle gamma diagram, such as Figure 10 The 2theta diffraction angle diagram is a graph in which the ordinate represents signal intensity counts and the abscissa represents the 2theta diffraction angle. The specific method of obtaining a one-dimensional 2theta diffraction angle diagram or a one-dimensional scattering diagram of X-rays is consistent with the prior art and will not be repeated here.

[0067] Example 2

[0068] An electronic device includes a memory and a processor. A computer program is stored in the memory, and the processor is configured to run the computer program to execute the integrated data collaborative acquisition method of small-angle scattering and wide-angle scattering based on a single-crystal diffractometer in Embodiment 1.

[0069] Embodiment 3

[0070] This embodiment also provides a readable storage medium. A computer program is stored in the readable storage medium. The computer program includes program codes for controlling a process to execute the process, and the process includes the integrated data collaborative acquisition method of small-angle scattering and wide-angle scattering based on a single-crystal diffractometer in Embodiment 1.

[0071] It should be noted that the specific examples in this embodiment can refer to the examples described in the above embodiments and alternative embodiments, and will not be elaborated here.

[0072] Generally, various embodiments can be implemented in hardware or special circuits, software, logic, or any combination thereof. Some aspects of the present invention can be implemented in hardware, while other aspects can be implemented by firmware or software executed by a controller, microprocessor, or other computing device. However, the present invention is not limited thereto. Although various aspects of the present invention can be shown and described as block diagrams, flowcharts, or using some other graphical representation, it should be understood that, as a non-limiting example, the blocks, devices, systems, technologies, or methods described herein can be implemented in hardware, software, firmware, special circuits or logic, general hardware or a controller, or other computing devices, or some combination thereof.

[0073] Embodiments of the present invention can be implemented by computer software, which can be executed by a data processor of a mobile device, such as in a processor entity, or implemented by hardware, or implemented by a combination of software and hardware. A computer software or program (also referred to as a program product), including software routines, applets, and / or macros, can be stored in any device-readable data storage medium, and they include program instructions for performing specific tasks. The computer program product can include one or more computer-executable components configured to execute the embodiments when the program runs. One or more computer-executable components can be at least one software code or a part thereof. Additionally, at this point, it should be noted that, as Figure 1 any box in the logical flow in can represent a program step, or an interconnected logical circuit, box, and function, or a combination of a program step and a logical circuit, box, and function. The software can be stored on physical media such as memory chips or storage blocks implemented within a processor, magnetic media such as hard disks or floppy disks, and optical media such as, for example, DVDs and their data variants, CDs. The physical media is a non-transitory medium.

[0074] The parts not detailed in the present invention are the prior art, so the present invention does not elaborate on them.

[0075] It can be understood that the term "a" should be construed as "at least one" or "one or more". That is, in one embodiment, the number of an element can be one, while in other embodiments, the number of the element can be multiple. The term "a" should not be construed as a limitation on the number.

[0076] Although terms such as the first sample holder 1, the second sample holder 2, the magnetic head 3, the first beam blocker bracket 4, the second beam blocker bracket 5, the sample stage 6, the fixing plate 11, the vertical backrest 12, the fixing hole 13, the connecting member 14, the groove 15, the backing plate 21, the detection hole 22, etc. are used more frequently herein, the possibility of using other terms is not excluded. The use of these terms is only for more conveniently describing and explaining the essence of the present invention; construing them as any additional limitation is contrary to the spirit of the present invention.

[0077] The present invention is not limited to the above best embodiment, and anyone can obtain other various forms of products under the inspiration of the present invention. However, no matter what changes are made in its shape or structure, as long as it has a technical solution identical or similar to that of the present invention, it falls within the protection scope of the present invention.

Claims

1. An integrated data collaborative acquisition method for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer, characterized in that, It includes the following steps: S00. Select an improved sample holder according to the requirements of the grazing incidence mode and the transmission mode; Wherein, the improved sample holder is used to replace the magnetic head on the original sample stage of the single crystal diffractometer, and the improved sample holder includes a first sample holder for the grazing incidence mode and a second sample holder for the transmission mode; The first sample holder includes a fixing plate provided with fixing holes and a vertical backrest higher than the fixing plate, and the first sample holder is rigid so that the vertical backrest can align the sample in the vertical direction and make the sample stand upright in the vertical direction. A connecting piece for fixing the sample in the horizontal direction is provided on the fixing hole. A 2-mm deep groove for placing the sample is formed between the vertical backrest and the fixing plate, and a stud for installing on the original sample stage of the single crystal diffractometer is provided at the bottom of the groove; The second sample holder includes a back plate provided with a detection hole, and studs for installing on the original sample stage of the single crystal diffractometer are also provided at the bottom of the back plate; S10. Prepare the sample and place it on the improved sample holder, and place it along the advancing direction of the X-ray; S20. Select an X-ray light source so that the X-ray light source is aligned with the sample, wherein the X-ray light source is a gallium target; S30. Set the sample rotation angle of the original sample stage of the single crystal diffractometer to a value between 85° and 95°, and move the sample back and forth in the y direction until the sample cuts half of the light blocker to find the zero position of the sample; S40. Rotate the sample along the incident angle direction on the improved sample holder for scanning, and start the test; S50. Set the distance between the sample and the area detector of the single crystal diffractometer, set the incident angle by setting the sample rotation angle of the original sample stage of the single crystal diffractometer, and set the exposure time to collect the scattering signal; S60. Collect the scattered X-ray signal through a two-dimensional area detector and perform integration through software to obtain the one-dimensional diffraction angle 2theta diagram or one-dimensional scattering diagram of the X-ray.

2. The integrated data collaborative acquisition method for small-angle scattering and wide-angle scattering based on a single crystal diffractometer according to claim 1, wherein In step S30, if the sample is tilted in the vertical direction, change the vertical tilt angle of the original sample stage of the single crystal diffractometer to adjust the collimation of the sample in the vertical direction.

3. The integrated data collaborative acquisition method for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer according to claim 1, wherein In step S50, set the distance between the sample and the detection surface of the single crystal diffractometer to be 100 - 240 mm, set the incident angle to be 0.1 - 1°, and set the exposure time to be 1 - 60 s.

4. The integrated data collaborative acquisition method for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer according to claim 1, wherein, In step S00, the diameter of the detection hole is 5 - 8 mm.

5. The integrated data collaborative acquisition method for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer according to claim 1, wherein In step S00, the sample is fixed to the back plate with double-sided tape or glue.

6. An electronic device, comprising a memory and a processor, characterized in that, A computer program is stored in the memory, and the processor is set to run the computer program to execute the small-angle scattering and wide-angle scattering integrated data collaborative acquisition method based on a single crystal diffractometer according to any one of claims 1 to 5.

7. A readable storage medium, characterized in that, A computer program is stored in the readable storage medium, and the computer program includes program codes for controlling a process to execute the process, and the process includes the small-angle scattering and wide-angle scattering integrated data collaborative acquisition method based on a single crystal diffractometer according to any one of claims 1 to 5.

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