Sample holder for micro-area variable-angle grazing incidence wide-angle scattering test

Abstract

The utility model relates to a sample holder for a micro-area variable-angle grazing incidence wide-angle scattering test. According to the scheme, a table top used for placing a test material, a Z-axis height reference position and a height adjusting driver used for driving the sample frame to move back and forth along a Z axis are arranged on the sample frame; the radian adjusting driver is used for driving the sample holder to do curve swinging motion along the light path direction and in the direction perpendicular to the light path; the connecting part is matched with a sample table of the single crystal diffractometer; wherein the radian adjusting driver is used for driving the table board to swing, so that the incident angle is controlled. The defects of an existing wide-angle scattering test technology based on single crystal XRD in the aspect of incident angle and height control can be overcome.

Description

Technical Field

[0001] This utility model relates to a support, specifically a sample holder for micro-area variable angle grazing incidence wide-angle scattering testing. Background Technology

[0002] Currently, wide-angle scattering testing methods and devices based on X-ray small-angle scattering (XARS) instruments are commonly used materials analysis tools, and wide-angle scattering testing methods based on single-crystal XRD (single-crystal diffractometer) are also being gradually developed and promoted. However, current technologies have problems such as inaccurate control of the incident angle and height in grazing-incidence wide-angle scattering, which affects the scattering intensity and causes diffraction peak position drift, as well as insufficient sample surface flatness.

[0003] Therefore, there is an urgent need for a new technical solution to address these issues, improve the accuracy, reproducibility, and reliability of testing, and expand its application scope in the field of materials analysis. Utility Model Content

[0004] The purpose of this invention is to address the aforementioned problems in the prior art by providing a sample holder for micro-area variable-angle grazing incidence wide-angle scattering testing.

[0005] To achieve the above-mentioned application objectives, the present invention adopts the following technical solution: a sample holder for micro-area variable angle grazing incidence wide-angle scattering test, the sample holder is provided with a platform for placing test materials, a Z-axis height reference position, a height adjustment driver for driving the sample holder to move back and forth along the Z-axis, an arc adjustment driver for driving the sample holder to make curved swing motion along the optical path direction, and a connection part that cooperates with the sample stage of a single crystal diffractometer.

[0006] The tabletop is oscillating via an arc adjustment driver to control the angle of incidence.

[0007] Furthermore, the sample holder is also equipped with an arc adjustment screw for the oscillation arc of the platform. This arc adjustment screw is set perpendicular to the output shaft of the arc adjustment driver, which can adjust the substrate to a flat horizontal line to optimize the scattering intensity.

[0008] Furthermore, an arc adjustment drive is also connected to the arc adjustment screw.

[0009] Furthermore, the improved sample holder is also equipped with an adjustment structure for adjusting the horizontal position of the platform.

[0010] Furthermore, the adjustment structure includes an X-axis adjusting screw for adjusting the X-axis position of the platform and a Y-axis adjusting screw for adjusting the Y-axis position of the platform.

[0011] Furthermore, the sample holder is equipped with two layers of arc-shaped tracks that are perpendicular to each other. The platform is mounted on the upper arc-shaped track via a transfer bracket and can be moved on the arc-shaped track by the transfer bracket under the drive of the arc adjustment driver. The upper arc-shaped track is also mounted on the lower arc-shaped track via a transfer bracket and can slide on the arc-shaped track by the transfer bracket under the drive of the arc adjustment screw.

[0012] Furthermore, the improved sample holder is mounted on the sample stage base of the single crystal diffractometer by means of screw connection.

[0013] Compared with the prior art, the present invention has the following beneficial effects:

[0014] 1. Precise control of incident angle: By improving the sample holder design, an arc adjustment actuator is provided to drive the sample stage to make curved swinging motion along the optical path direction. This enables precise control of the incident angle of variable angle grazing scattering, avoiding the problem of inaccurate incident angle caused by relying solely on experience and feel to place samples in the existing technology. This improves the parallelism and reproducibility of the test, thereby enabling more accurate acquisition of the scattering information of the material.

[0015] 2. High-precision height control: The improved sample holder has a Z-axis height reference position, and digital high-precision height control is achieved through related components. This ensures that the scattering spectrum of all samples does not drift, guarantees the standardization and reproducibility of the test peak positions, improves data quality, and overcomes the problems of scattering intensity being affected and diffraction peak position drift caused by inaccurate height control in the existing technology.

[0016] 3. Depth gradient profiling: Precisely controlled incident angles can extend the depth gradient profiling of thin film materials deposited on substrates, realizing structural gradient changes from the surface to the bulk of the material. This can be applied to the analysis of various materials such as solar cell materials, solid fuel cells, green energy catalysts, organic photovoltaics, and chips for data storage and transmission, where existing technologies have limitations.

[0017] 4. Micro-area analysis capability: The improved sample holder can achieve high-precision micro-area analysis through relevant settings. By fine-tuning X and Y, it can achieve micro-area variable angle grazing incidence wide-angle scattering characterization of different regions. Existing technologies cannot meet the needs of this micro-area analysis.

[0018] 5. Protecting component safety: The improved sample holder is flexible and compact, overcoming the limitations of the narrow space between the collimator and the light blocker. It can not only meet all the testing requirements of micro-area variable angle grazing incidence scattering, but also maximize the protection of the safety of components such as detectors. Existing technologies are insufficient in this regard.

[0019] 6. Low modification cost: The sample holder can be directly modified and replaced on an existing quaternary single crystal diffractometer without complex structural modifications, resulting in low modification cost. Attached Figure Description

[0020] Figure 1 This is a schematic diagram of an improved sample holder structure for a micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention.

[0021] Figure 2 This is a schematic diagram of the basic structure of a single-crystal diffractometer according to an embodiment of the present invention;

[0022] Figure 3 This is a scattering map obtained by a two-dimensional surface detector during the scanning process of the micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of this utility model;

[0023] Figure 4 The image is a two-dimensional scattering pattern obtained by adjusting the parameters (using arc adjustment along the optical path direction) of a two-dimensional surface detector during the scanning process of the micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of this utility model.

[0024] Figure 5 The image is a two-dimensional scattering pattern obtained by a two-dimensional surface detector after the second parameter adjustment (using another radian adjustment) during the scanning process of the micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of this utility model.

[0025] Figure 6 This is a two-dimensional scattering image obtained from a two-dimensional surface detector after adjustment during the scanning process according to the micro-area variable angle grazing incidence wide-angle scattering test method of this utility model embodiment;

[0026] Figure 7 The diffraction angle 2Theta diagram (one-dimensional X-ray scattering diagram) is obtained by scanning according to the micro-area variable angle grazing incidence wide-angle scattering test method of this utility model embodiment.

[0027] In the diagram, 1. Two-dimensional surface detector; 2. Horizontal guide rail; 3. Sample stage; 4. Focusing lens; 5. X-ray source; 6. Temperature control system; 7. Imaging system; 8. Collimator; 9. Direct light blocker; 10. Improved sample holder; 11. Stage; 12. Height adjustment driver; 13. Curvature adjustment driver; 14. Connection part; 15. X-axis adjustment screw; 16. Y-axis adjustment screw; 17. Curvature adjustment screw; 18. Z-axis height reference position; 19. Curved track. Detailed Implementation

[0028] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present utility model are within the protection scope of the present utility model.

[0029] Those skilled in the art should understand that in the disclosure of this utility model, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, the above terms should not be construed as limitations on this utility model.

[0030] This invention aims to provide a sample holder for micro-area variable-angle grazing incidence wide-angle scattering testing. Specifically, taking a PTO (PtTiO3) thin film material deposited on an STO (SrTiO3, strontium titanate) substrate as an example, the testing method includes the following steps:

[0031] S00: Prepare a sample of PTO thin film material deposited on an STO substrate and place it on the improved sample holder 10.

[0032] The single-crystal diffractometer is an existing quaternary diffractometer, which has four rotational degrees of freedom: vertical tilt, horizontal rotation, detector rotation, and sample rotation. However, based on this, this invention designs digitally controlled tilt along the optical path, digital z-height precision control and feedback, and horizontal XY-direction adjustment, i.e., an improved sample holder 10. The improved sample holder 10 directly replaces the original sample holder of the single-crystal diffractometer and is installed on the sample stage 3 of the single-crystal diffractometer using the same installation method as the original sample holder (since the structure of connecting the sample stage 3 is different for different single-crystal diffractometers, the connection method is different. Taking the common structure as an example, a threaded connection structure is used).

[0033] Among them, single-crystal diffractometers mainly include, for example, Figure 2The two-dimensional surface detector 1, horizontal guide rail 2, improved sample holder 10, focusing lens 4, X-ray source 5 (equipped with copper target or molybdenum target), temperature control system 6, imaging system 7, collimator 8, and direct light blocker 9 are shown. A two-dimensional surface detector 1 is slidably mounted on a horizontal guide rail 2, and can move away from or towards the sample stage 3 along the horizontal guide rail 2 or rotate horizontally. The horizontal guide rail 2 is located at the end of the sample stage 3 away from the focusing lens 4. An improved sample holder 10 is provided on the sample stage 3. The focusing lens 4 is connected to the X-ray source 5 and is located at the end of the sample stage 3 away from the horizontal guide rail 2, and the focusing lens 4 is provided with a collimating tube 8 facing the sample stage 3. The temperature control system 6 is located directly above the sample stage 3 and can move up and down to adjust its height, tilt angle along the optical path, tilt angle perpendicular to the optical path, and horizontal xy movement. The temperature control system 6 is provided with a direct light blocker 9. The imaging system 7 is positioned facing the improved sample holder 10. The specific single-crystal XRD structure is consistent with the authorized patent CN118243709B, the only difference being the sample holder, and it does not have the external light source of the patent. Of course, it can also be combined with the external light source of the patent to further expand and realize the single-crystal-single-crystal in-situ phase transition atomic-level structure monitoring method.

[0034] Among them, the authorized patent CN118243709B cannot achieve variable-angle grazing incidence wide-angle scattering. However, the introduction of this improved sample holder 10 solves the technical bottleneck of in-depth analysis of the atomic-level structure of functional materials. It not only saves the purchase cost of another X-ray wide-angle scattering instrument, but also saves the cost of purchasing an in-situ cavity. Most importantly, it expands the function of two-dimensional in-depth structural analysis driven by atmosphere and thermal energy in multiple fields, successfully capturing the growth, aging, or stability processes and mechanisms of two-dimensional photovoltaic materials and semiconductor materials. It has extraordinary scientific research significance and broadens the scope of characterization technology.

[0035] S10: Select X-ray source 5 and align it with the sample. X-ray source 5 is a combination of copper target and molybdenum target.

[0036] S20: In the Z-scan scanning mode of the diffractometer, X-ray light intensity is scanned in the vertical direction. The thin film material with substrate is adjusted to the test height by the lifting drive component; that is, the Z coordinate is scanned from the lowest to the highest, and the light intensity is scanned from the highest intensity to the lowest intensity. Then, the Z height is taken when the substrate material just blocks half of the beamstop (direct light blocker 9), at which point the light intensity is about half of the direct light. The Z-scan range is 0-20mm, the step size is 0.1mm / step, and the scan speed is 0.1s / step.

[0037] The lifting drive component is an additional structure added to the single-crystal diffractometer, used to drive the lifting of the sample stage 3.

[0038] like Figure 3As shown, in Z-scan scanning mode, the scattering pattern obtained on the detector shows that the sample reaches the center position of the photoblock as the Z-axis changes, which is the appropriate Z-coordinate height. Furthermore... Figure 3 The alternation of light and dark areas is due to the substrate gradually blocking direct light, leaving dark shadows.

[0039] S30: Rocking is performed along the optical path under the improved sample stage 3, scanning from the minimum luminous flux to the maximum light intensity and then back to the minimum light intensity. The Theta angle at the point of maximum light intensity is taken as the zero point of the optical path direction. The axis of rocking rotation is omega, and the direction is the horizontal plane of light propagation. The rocking scan range is -5 to 5°, the step size is 0.01° / step, and the scan speed is 0.1s / step.

[0040] like Figure 4 As shown, this is a two-dimensional scattering pattern after the detector detects the signal.

[0041] S40: Set the distance between the sample and the detector surface of the single crystal diffractometer to 40-120mm, set the exposure time to 1-300s to collect the scattered signal, and set the incident angle to 0.1-10°.

[0042] like Figure 5 As shown, this is a two-dimensional scattering pattern of the detector after receiving the signal following parameter settings.

[0043] S50: The scattered X-rays are acquired using the two-dimensional surface detector 1. If the substrate is tilted in the collected two-dimensional scattering pattern, another curvature adjuster perpendicular to the optical path can be manually adjusted to place the substrate on a flat horizontal line to optimize the scattering intensity. Figure 5 and Figure 6 As shown.

[0044] S60: The diffraction angle 2θ pattern (one-dimensional X-ray scattering pattern) obtained by integration using software (the software package included with the single-crystal diffractometer); by continuously changing the incident angle and continuously collecting scattered X-rays through a two-dimensional surface detector, and integrating them using software, a series of one-dimensional X-ray scattering patterns are obtained, such as... Figure 7 As shown (x-axis: 2θ, y-axis: intensity), as the depth changes, X-rays penetrate deeper from the shallow surface of the sample towards the bulk, carrying structural information at different depths. This manifests as the appearance of new peaks, the disappearance of existing peaks, changes in peak intensity, and peak position shifts.

[0045] In this embodiment, the improved sample holder 10 is as follows: Figure 1As shown, the improved sample holder 10 is equipped with a platform 11 for placing test materials, a Z-axis height reference position 18, a height adjustment driver 12 (Z-axis height lifting motor) for driving the improved sample holder 10 to move back and forth along the Z-axis, an arc adjustment driver 13 (arc adjustment drive motor) for driving the improved sample holder 10 to make curved swinging motion along the optical path direction, and a connection part 14 that cooperates with the sample stage 3 of the single crystal diffractometer. The incident angle is controlled by the arc adjustment driver 13. Specifically, the arc adjustment driver 13 drives the platform 11 to slide back and forth on the arc track of the improved sample holder 10 through a lead screw drive to adjust the swing angle. The swing angle is -15 to 15°. The platform 11 and the arc adjustment driver 13 are connected by a transition bracket. That is, the arc adjustment driver 13 drives the transition bracket to move horizontally. Then, the platform 11 and the transition bracket are movably connected (such as hinged). Therefore, the bottom of the platform 11 can slide back and forth on the arc track 19 of the improved sample holder 10 to adjust the swing angle. Preferably, an additional arc adjustment screw 17 and arc track 19 in another direction can be added to achieve the same operation. The two directions are perpendicular to each other. The arc adjustment screw 17 can also be adjusted by sliding back and forth on another arc track 19 of the improved sample holder 10 through the installation of an arc adjustment driver 13, thereby achieving the flatness of the sample in the horizontal plane perpendicular to the light path direction, thus enabling the sample to obtain a higher scattering intensity. Note: The two arc tracks 19 have the same function, only different in direction, therefore the same reference numerals are used.

[0046] The improved sample holder 10 is also equipped with an XY-axis adjustment structure – two adjustment screws (X-axis adjustment screw 15 and Y-axis adjustment screw 16), which also utilize the lead screw transmission principle to achieve horizontal adjustment of the improved sample holder 10. The height adjustment driver 12 converts rotary motion into linear motion through a worm gear transmission combined with lead screw transmission or other transmission methods, thereby achieving height adjustment of the table 11.

[0047] The preferred driving method for the motor here is a worm gear and screw drive (i.e., the principle of existing worm screw jacks; all transmission methods in this solution are common in the mechanical field, and their advantage lies in integrating them onto a single sample holder to achieve multi-degree-of-freedom adjustment, thereby expanding the testing methods of existing XRD equipment). This sample holder has the following advantages:

[0048] 1. The improved sample holder 10 is flexible and compact, breaking through the limitations of the narrow space between the collimator and the light blocker. It can not only meet all the testing requirements of variable angle grazing incidence scattering, but also maximize the protection of the safety of the detector and other components.

[0049] The space between the collimator and the light blocker is very limited, only enough to accommodate a 1cm x 1cm sample. Therefore, a small plate needs to be supported on the sample holder using a thin rod to support the 1cm x 1cm sample. In this way, the sample will not touch any part of the original diffractometer.

[0050] 2. An incident angle that can precisely control variable angle grazing incident scattering was designed, which expanded the depth gradient analysis of thin film materials deposited on substrate materials based on the original technology, realizing the structural gradient change from the shallow surface to the bulk of the material, such as solar cell materials, organic photovoltaics, perovskite thin film samples, data storage and transmission chips, etc.

[0051] Due to the precise control of the motor along the optical path, the improved sample holder 10 can perform a high-precision curved swaying motion in the optical path direction, thus enabling precise control of the incident angle.

[0052] Digital high-precision height control, with a reference position as a standard reference point, ensures that the scattering spectrum of all samples does not drift, that is, the standardization and reproducibility of the test peak position are ensured, and the data quality is improved (the height reference position is determined by determining that the sample stage 3 is at its lowest position, then the reference position value of the lowest position is 0 mm; then the height based on this is accurate and has high reproducibility).

[0053] The Z-axis height is controlled by a lifting motor, enabling high-precision digital control. Furthermore, the newly designed sample stage 3 has a reference point, providing a standard reference point as the zero point for the Z-axis height, improving repeatability and ensuring high precision.

[0054] 4. Enables high-precision micro-area analysis: By fine-tuning X and Y, grazing incidence scattering characterization of different regions can be achieved. Figure 1 Adjust the front and rear positions of sample stage 3 using the screws in the middle.

[0055] 5. All motors in this utility model can be digitized and controlled by specialized external software.

[0056] Those skilled in the art should understand that the technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments have been described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0057] The above embodiments only illustrate several implementation methods of this utility model, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of this utility model. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this utility model, and these all fall within the protection scope of this utility model. Therefore, the protection scope of this utility model should be determined by the appended claims.

[0058] The parts of this utility model not described in detail are existing technologies, therefore, this utility model does not describe them in detail.

[0059] It is understood that the term "a" should be understood as "at least one" or "one or more", that is, in one embodiment, the number of an element can be one, while in another embodiment, the number of the element can be multiple, and the term "a" should not be understood as a limitation on the number.

[0060] Although this document uses a considerable amount of technical terminology, the possibility of using other terms is not excluded. These terms are used merely for the convenience of describing and explaining the essence of this utility model; interpreting them as any additional limitation would contradict the spirit of this utility model.

[0061] This utility model is not limited to the above-described preferred embodiment. Anyone can derive other forms of products under the guidance of this utility model. However, regardless of any changes made to their shape or structure, any technical solution that is the same as or similar to this utility model falls within the protection scope of this utility model.

Claims

1. A sample holder for micro-area variable-angle grazing incidence wide-angle scattering testing, characterized in that, The sample holder is provided with a platform for placing test materials, a Z-axis height reference position, a height adjustment driver for driving the sample holder to move back and forth along the Z-axis, an arc adjustment driver for driving the sample holder to make curved swinging motion along the optical path direction, and a connection part that cooperates with the sample stage of the single crystal diffractometer. The tabletop is oscillating via an arc adjustment driver to control the angle of incidence.

2. The sample holder for micro-area variable-angle grazing incidence wide-angle scattering testing according to claim 1, characterized in that, The sample holder is also equipped with an arc adjustment screw for the swing radius of the platform. The arc adjustment screw is set perpendicular to the output shaft of the arc adjustment driver, which can adjust the substrate to a flat horizontal line to optimize the scattering intensity.

3. The sample holder for micro-area variable angle grazing incidence wide-angle scattering testing according to claim 2, characterized in that, An arc adjustment drive is also connected to the arc adjustment screw.

4. The sample holder for micro-area variable angle grazing incidence wide-angle scattering testing according to claim 1, characterized in that, The sample holder is also equipped with an adjustment structure for adjusting the horizontal position of the platform.

5. The sample holder for micro-area variable angle grazing incidence wide-angle scattering testing according to claim 4, characterized in that, The adjustment structure includes an X-axis adjusting screw for adjusting the X-axis position of the platform and a Y-axis adjusting screw for adjusting the Y-axis position of the platform.

6. The sample holder for micro-area variable angle grazing incidence wide-angle scattering testing according to claim 2, characterized in that, The sample holder is also provided with two layers of arc-shaped tracks that are perpendicular to each other. The platform is mounted on the upper arc-shaped track through a transfer bracket. Under the drive of the arc adjustment driver, it can be moved on the arc-shaped track by the transfer bracket. The upper arc-shaped track is also mounted on the lower arc-shaped track through the transfer bracket and slides on the arc-shaped track. Under the drive of the arc adjustment screw, it can be moved on the arc-shaped track by the transfer bracket.

7. The sample holder for micro-area variable-angle grazing incidence wide-angle scattering testing according to any one of claims 1-6, characterized in that, The connection part uses screws to mount the sample holder onto the sample stage base of the single crystal diffractometer.

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