Portable multifunctional GIWAXS remote testing device

Abstract

The invention provides a portable and multifunctional GIWAXS remote testing device and a testing method of the portable and multifunctional GIWAXS remote testing device. The device comprises a support and motion control system, a sample multi-environment variable system and a signal receiving system, the support and motion control system has a multi-direction moving function, so that a sample can be accurately placed between an X-ray path and a detector in an experiment; the sample multi-environment variable system is accurately set according to user requirements, and various parameters including temperature, spin-coating speed, atmosphere environment and humidity are included; the signal receiving system receives the X-rays penetrating through the sample and converts received X-ray signals into electric signals. According to the portable multifunctional GIWAXS remote testing device provided by the invention, personnel in different fields can operate conveniently and quickly during GIWAXS experiment testing, and meanwhile, efficient work is realized.

Description

Technical Field

[0001] The invention belongs to the technical field of in-situ detection, and in particular, relates to a portable multifunctional GIWAXS remote testing device. Background Art

[0002] The crystal structure of material surfaces (such as thin films) has always been a difficult point in research, so how to achieve accurate crystal structure detection of these samples has always attracted much attention. We need to perform accurate crystal structure analysis of the samples to be tested at a microscopic scale and in multiple dimensions, which is an important focus of current research.

[0003] Grazing-incidence wide-angle X-ray scattering (GIWAXS) technology came into being. Through this technology, we can penetrate thin films and material surfaces at different depths and deeply study the changes in the crystal structure of the material. The data provided by GIWAXS is a two-dimensional diffraction pattern with different crystal planes. It has many advantages, including high signal-to-noise ratio, high structural resolution, non-contact detection, non-destructive detection, rich structural information, depth resolution, and in-situ observation. Therefore, GIWAXS technology is very popular in the field of material surface research (such as thin films). It can be used to reveal the preferred orientation of crystals from multiple angles and to describe in detail the changes in the microstructure reconstruction process.

[0004] In-situ measurements are very attractive for studying the surface of thin film materials. They provide us with a way to quickly track changes in the microstructure of materials, including processes such as crystallization and aging, which is crucial for revealing the dynamics of materials. The formation process of the crystal structure on the surface of thin film materials is still not fully understood. The film formation process involves the gelation stage and the crystallization stage of the liquid film. In-situ GIWAXS technology provides us with important information about the evolution of the composition during the spin coating process. This technology plays an indispensable role in studying thin films and surface materials.

[0005] From 2015 to 2023, several research teams have used synchrotron radiation sources such as the Spring-8 light source in Japan, the Cornell High Energy Synchrotron Source, the Advanced Photon Source at Argonne National Laboratory in the United States, and the Advanced Light Source at Lawrence Berkeley National Laboratory to in-situ characterize the crystallization process of thin film materials, and explored the influence of additive types on the crystal structure and orientation of thin film materials based on GIWAXS technology. This shows that in this field, it is of great significance to build a GIWAXS test device based on a synchrotron radiation light source line station.

[0006] However, it is worth noting that the existing related devices usually have problems such as low working efficiency, complex operation and limited functions. Therefore, how to solve these problems has become one of the important challenges that technicians in this field need to solve. Our invention aims to solve these problems and provide an efficient, reliable and convenient tool for the study of the crystal structure of thin films and material surfaces. Summary of the invention

[0007] The purpose of the present invention is to provide a portable and multifunctional GIWAXS remote testing device, so that personnel in different fields can operate conveniently and quickly when conducting GIWAXS experimental tests, and at the same time can conduct experiments in a variety of environments such as different systems (such as liquids, solids) and different atmospheres (such as nitrogen, oxygen), thereby achieving efficient work.

[0008] To achieve the above-mentioned object, in a first aspect, the present invention provides a portable multifunctional GIWAXS remote testing device, the device comprising: a support and motion control system, a sample multi-environmental variable system and a signal receiving system;

[0009] The support and motion control system has multi-directional movement capabilities so that the sample can be accurately placed between the X-ray path and the detector during the experiment;

[0010] The sample multi-environment variable system can be precisely set according to user needs, including temperature, spin coating speed, atmosphere environment, humidity and other parameters;

[0011] The signal receiving system receives the X-rays after passing through the sample and converts the received X-ray signals into electrical signals.

[0012] In some embodiments, the support and motion control system includes: a counterweight chassis, a linear motor, a control chassis, a support frame, a support platform, a level, and an inclinometer Roll and Pitch axes.

[0013] In some embodiments, the level of the workbench is adjusted by adjusting the Roll axis and the Pitch axis of the inclinometer.

[0014] In some embodiments, whether the workbench is level is determined by a level.

[0015] In some embodiments, the linear motor is adjusted to adjust the Z-axis direction so that the sample is parallel to the X-ray and a portion of the sample just blocks the light beam, ensuring that the X-ray can hit the sample.

[0016] In some embodiments, the sample multi-environmental variable system includes: a pipette, an air tube, a bracket, a manual two-axis stage, a spin coating protective cover, a sample stage, a heated spin coater, a heated spin coater controller, a cold head, and an atmosphere cover connected to the detector.

[0017] In some embodiments, the sample needs to be placed in the pipette in advance, and then the Y-axis direction is adjusted by a manual two-axis stage so that the pipette is on top of the middle position of the sample stage.

[0018] In some embodiments, the air pump injects air into the air tube, and then the button on the top of the pipette is hit to inject the liquid into the middle of the sample stage.

[0019] In some embodiments, the signal receiving system includes: a photodiode proximal to the detector, a photodiode support rod, and a picoammeter.

[0020] In a second aspect, the present invention further provides a remote control system, the system comprising:

[0021] A portable and multifunctional GIWAXS remote testing device as described above; and

[0022] The server corresponds to a software operation interface, which can remotely control the portable multifunctional GIWAXS remote testing device as described above.

[0023] The system provided by the embodiment of the present invention realizes GIWAXS testing of various types of test samples through the coordination between the support and motion control system, the sample multi-environment variable system and the signal receiving system. It is easy to operate and has strong usability, and realizes convenient and fast operation, helping testers to work efficiently. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 A schematic diagram of three-dimensional coordinates provided by an embodiment of the present invention;

[0025] Figure 2 A structural diagram of a support and motion control system provided by an embodiment of the present invention;

[0026] Figure 3 A structural diagram of a sample multi-environment variable system provided by an embodiment of the present invention;

[0027] Figure 4 A structural diagram of a signal receiving system provided by an embodiment of the present invention;

[0028] Figure 5 A schematic diagram of a software operation interface provided by an embodiment of the present invention.

[0029] Description of reference numerals:

[0030] Chassis 1, linear motor 2, control chassis 3, 4, support frame 5, support platform 6, level 7, inclinometer 8, pipette 9, air pipe 10, bracket 11, manual two-axis stage 12, spin coating protective cover 13, sample stage 14, heated spin coater 15, heated spin coater controller 16, cold head 17, detector 18, atmosphere cover 19, photodiode 20, photodiode support rod 21, picoammeter 22, software operation interface 23. DETAILED DESCRIPTION

[0031] In the detailed description below, many specific details of the present invention are set forth by way of example in order to provide a thorough understanding of the relevant disclosure. However, it will be apparent to one of ordinary skill in the art that the present invention can be implemented without these details. It should be understood that the use of the terms "system," "device," "unit," and / or "module" in the present invention is a method for distinguishing different parts, elements, parts, or assemblies at different levels in a sequential arrangement. However, these terms may be replaced by other expressions if other expressions can achieve the same purpose.

[0032] It should be understood that when a device, unit or module is referred to as being "on," "connected to," or "coupled to" another device, unit or module, it may be directly on, connected to, coupled to, or communicating with other devices, units or modules, or there may be intermediate devices, units or modules, unless the context clearly indicates an exception. For example, the term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0033] The terms used in the present invention are only for describing specific embodiments and are not intended to limit the scope of the present invention. As shown in the specification and claims of the present invention, unless the context clearly indicates an exception, the words "a", "an", "a kind" and / or "the" are not specifically singular and may also include the plural. Generally speaking, the terms "include" and "comprise" only indicate the inclusion of clearly identified features, wholes, steps, operations, elements and / or components, and such specifications do not constitute an exclusive list, and other features, wholes, steps, operations, elements and / or components may also be included.

[0034] These and other features and characteristics of the present invention, methods of operation, functions of related elements of structure, combinations of parts and economies of manufacture may be better understood with reference to the following description and accompanying drawings, which form a part of the specification. However, it is to be clearly understood that the drawings are for illustration and description purposes only and are not intended to limit the scope of protection of the present invention. It is to be understood that the drawings are not drawn to scale.

[0035] The present invention uses a variety of structural diagrams to illustrate various variations of the embodiments of the present invention. It should be understood that the above or below structures are not intended to limit the present invention. The scope of protection of the present invention shall be subject to the claims.

[0036] The present invention aims to achieve in-situ characterization of the lattice information of thin films and material surfaces, and to make full use of high-intensity synchrotron radiation sources and high-performance surface detectors. Our goal is to develop a portable multifunctional GIWAXS test device to achieve efficient, in-situ, and rapid testing of structural changes in liquid solutions, thin films, and various material surfaces, while also having the ability to detect the effects of the environment such as temperature and atmosphere on the sample. In addition, we also focus on introducing a remote control system so that users can conveniently remotely operate and manage the test system to meet diverse experimental needs.

[0037] In order to achieve in-situ characterization of the crystal phase structure of thin films, solid material surfaces and solution samples during the crystallization process, we have successfully established a portable multifunctional GIWAXS test device and remote control system based on the crystallography line station at the synchrotron radiation light source. The whole is mainly composed of three parts, including the support and motion control system, the sample multi-environmental variable system and the signal receiving system. The support and motion control system has a multi-directional movement function so that the device can be accurately placed between the X-ray path and the detector 18 in the experiment. The linear motor 2 equipped on the support system is responsible for moving the sample on the Z axis on the support table 6 to ensure that the X-rays are accurately irradiated on the sample, and the X-rays are monitored by the readings of the photodiode 20 and the picoammeter 22 in the signal receiving system. In addition, we can also adjust the tilt angle of the electric turntable by the motion control system to accurately control the incident angle and penetration depth of the X-rays to meet the requirements of different samples. This system allows us to flexibly adapt to different experimental needs to achieve a detailed study of the crystallization behavior of the sample. The multi-environmental variable system of the sample can be accurately set according to user needs, including but not limited to temperature, spin coating speed, atmosphere environment, humidity and other parameters. The flexibility and adjustability of this system allow researchers to fully control and adjust for different experimental purposes and material properties to ensure the best match of experimental conditions and obtain accurate and reliable experimental results. Finally, a user-friendly interface23 is designed so that users can easily set experimental parameters and monitor experimental progress. The remote control system should have the ability of remote control to facilitate remote experimental operation and data acquisition.

[0038] The present invention designs a portable multifunctional instrument testing device and a remote control system, which enables personnel in different fields to operate conveniently and quickly when conducting GIWAXS experimental tests. At the same time, experiments can be performed in a variety of environments such as different systems (such as liquids, solids) and different atmospheres (such as nitrogen, oxygen), thereby achieving efficient work.

[0039] In order to achieve the above-mentioned objectives, the present invention provides a portable multifunctional GIWAXS remote testing device, which builds a testing platform based on a line station. The device includes: a chassis 1, a heating spin coater 15, a liquid spin coating protective cover 13, an atmosphere cover 19, a photodiode 20, a cooling device, a picoammeter 22 and a control system.

[0040] The system controller and the linear motor 2 are stored inside the chassis 1 , and a support frame 5 is arranged on the top of the chassis 1 .

[0041] The support platform 6, the level 7, the manual two-axis platform 12 and the pipette fixing frame are placed on the frame rod.

[0042] The support platform 6 is provided with a heating spin coater 15, wherein heating and spin coating can be performed simultaneously or separately, the solution sample is spin coated evenly, and drying is accelerated by heating to form a film, and conformational changes with temperature are observed in situ.

[0043] The level 7 needs to maintain the balance of the supporting platform 6 and can also facilitate the adjustment of the angle change of the sample.

[0044] The manual two-axis platform 12 is equipped with a controller and can move in front and back, left and right axes.

[0045] The pipette fixing frame fixes the pipette 9 containing the sample.

[0046] The liquid discharge mode of the liquid transfer gun 9 is controlled by an air pump.

[0047] The top of the heating spin coater 15 is provided with a liquid spin coating protective cover 13 and an atmosphere cover 19 ; the material of the protective cover 13 is a polyimide film, and light path holes are opened at both ends of the light path of the atmosphere cover 19 .

[0048] The spin coating protective cover 13 can prevent the sample from splashing during the spin coating process.

[0049] The atmosphere cover 19 fills the sample and the distance from the sample to the detector 18 with a specific atmosphere.

[0050] The liquid protection cover 13 and the atmosphere cover 19 are selected to use a polyimide film in the light path, which does not diffract X-rays and will not affect the sample signal.

[0051] After the X-ray light passes through the sample, a photodiode 20 is required to receive a signal, and a picoammeter 22 is used to display corresponding current signal information.

[0052] The photodiode 20 is placed at the front end of the detector 18 to facilitate receiving signals.

[0053] The cooling device includes a cold head 17 located at the front end of the sample stage and filled with liquid nitrogen. The function of the cold head 17 is to quickly lower the temperature of the sample stage by blowing out low-temperature nitrogen after the sample stage is heated, thereby reducing the waiting time of the user.

[0054] like Figures 1 to 5 As shown, the present invention relates to a support and motion control system, a sample multi-environment variable system and a signal receiving system.

[0055] As an example, the support and motion control system includes a counterweight chassis 1, a linear motor (Z axis) 2, a control chassis 3, 4, a support frame 5, a support platform 6, a level 7 and an inclinometer 8 Roll and Pitch axes; the sample multi-environmental variable system includes a pipette 9, an air tube 10, a bracket 11, a manual two-axis table 12, a spin coating protective cover 13, a sample table 14, a heated spin coater 15, a heated spin coater controller 16, a cold head 17 and an atmosphere cover 19 connected to a detector 18; the signal receiving system includes a photodiode 20 connected to the detector 18, a photodiode support rod 21 and a picoammeter 22, and finally a software operation interface 23 corresponding to a server that can remotely control the entire device.

[0056] The specific steps are as follows:

[0057] First, you need to find the position of the X-ray, and adjust the Z-axis direction by adjusting the linear motor 2 so that the sample is parallel to the X-ray and just partially blocks the light path, thereby ensuring that the light beam is irradiated on the sample surface in the form of grazing incidence during the test. The way to determine whether the sample blocks the light beam is to read the information on the picoammeter 22 based on the current signal received by the photodiode 20. Compared with the full passage of the light beam, the blocked current reading can be about half of the full passage. Then adjust the level of the workbench 6 by adjusting the Roll axis and Pitch axis of the inclinometer 8. The level meter 7 can be used to determine whether the level judgment standard is the maximum value of the current signal on the picoammeter 22 that can be reached after blocking part of the light beam.

[0058] Secondly, the incident angle is controlled by adjusting the inclinometer 8 by adjusting the pitch axis to control the tilted sample stage, so that the X-ray passes through the sample. The penetrating ability of X-rays is closely related to the energy and incident angle selected in the experiment. It can be arbitrarily selected within the energy range of 5 to 20 KeV according to user needs and sample characteristics.

[0059] If it is a solution sample, the sample needs to be placed in the pipette 9 in advance, and then the Y-axis direction is adjusted through the manual two-axis stage 12 so that the pipette 9 is on top of the middle position of the sample stage 14, and then click on the glue gun injection on the software operation interface 23, and the air pump injects air through the air tube 10 in a short time, and then hit the button on the top of the pipette 9 to quickly inject the liquid into the middle of the sample stage 14.

[0060] After the liquid is added, click to start spin coating. Before spin coating, the spin coating protective cover 13 should be placed to avoid liquid splashing, click the switch of the heated spin coater 15, and adjust the spin coating speed and time through the heated spin coater controller 16.

[0061] If the sample needs to be heated, the heating speed and time need to be adjusted through the heating spin coater controller 16; after the heating is completed, the sample stage is cooled by adjusting the position of the cold head 17 to improve the test efficiency.

[0062] If the sample needs to be exposed to atmosphere, the atmosphere cover 19 needs to be placed on the sample stage 14, with the other end close to the detector 18, and the X-ray passage direction needs to be sealed with a polyimide film.

[0063] After passing through the optical path, the X-ray hits the photodiode 20, and the optical signal is transmitted to the picoammeter 22. The change in the current value of the picoammeter 22 is used to determine whether the X-ray hits the sample.

[0064] All adjustment steps of the experiment can be operated on the software operation interface 23 through the remote control system.

[0065] The technical effects of the present invention not only have advanced experimental performance and reliability, but also have broad application potential, and are expected to promote the development of scientific research and engineering applications, providing a powerful tool for researchers in materials science and related fields. Specifically,

[0066] 1. Simple and easy to operate: The design of this device platform focuses on user-friendliness, making the testing of thin films, solid material surfaces and solution samples extremely simple and easy to operate. Its intuitive user interface and automated control system simplify the preparation and conduct of experiments, thereby lowering the technical threshold and enabling more researchers to easily carry out experimental work.

[0067] 2. In-situ testing for multiple conditions: The device is not only capable of in-situ testing, but also can work under multiple environmental conditions as needed, such as different temperatures, humidity and atmospheres. The flexibility of this multi-environmental variable system enables researchers to simulate and explore the behavior of samples under various complex conditions, thereby gaining a deeper understanding of their properties and behaviors.

[0068] 3. Improved reliability: By relying on synchrotron radiation X-ray sources, the device platform of the present invention ensures high reliability of the film preparation process and atmosphere. This means that the experimental results are more accurate and repeatable, which helps researchers obtain stable and consistent data in material characterization and research.

[0069] 4. Improve work efficiency: The efficiency and versatility of this device greatly improve work efficiency. It allows multiple experiments on atmosphere, temperature, and sample status to be conducted simultaneously, reducing the waiting time for experiments, so that experimental results can be obtained faster. This is very beneficial for high-throughput sample testing and material research.

[0070] Those skilled in the art can clearly understand that, for the convenience and brevity of description, the specific working processes of the above-described devices and modules can refer to the corresponding descriptions in the aforementioned device embodiments and will not be repeated here.

[0071] It should be understood that the above specific embodiments of the present invention are only used to illustrate or explain the principles of the present invention, and do not constitute a limitation of the present invention. Therefore, any modifications, equivalent substitutions, improvements, etc. made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. In addition, the appended claims of the present invention are intended to cover all changes and modifications that fall within the scope and boundaries of the appended claims, or the equivalent forms of such scope and boundaries.

Claims

1. A portable and multifunctional GIWAXS remote testing device, include: Support and motion control system, sample multi-environment variable system and signal receiving system; The support and motion control system has multi-directional movement capabilities so that the sample can be accurately placed between the X-ray path and the detector during the experiment; The sample multi-environment variable system can be precisely set according to user needs, including temperature, spin coating speed, atmosphere environment, humidity and other parameters; The signal receiving system receives the X-rays after passing through the sample and converts the received X-ray signals into electrical signals.

2. The device according to claim 1, It is characterized in that The support and motion control system includes: counterweight chassis, linear motor, control chassis, support frame, support platform, level, and inclinometer Roll and Pitch axes.

3. The device according to claim 2, It is characterized in that Adjust the level of the workbench by adjusting the Roll and Pitch axes of the inclinometer.

4. The device according to claim 3, It is characterized in that Whether the workbench is level is determined by a level.

5. The device according to claim 2, It is characterized in that By adjusting the linear motor and the Z-axis direction, the sample is made parallel to the X-rays and part of the sample just blocks the light to ensure that the X-rays can hit the sample.

6. The device according to claim 1, It is characterized in that The sample multi-environment variable system comprises: a pipette gun, an air pipe, a bracket, a manual two-axis stage, a spin coating protective cover, a sample stage, a heated spin coater, a heated spin coater controller, a cold head and an atmosphere cover connected to a detector.

7. The device according to claim 6, It is characterized in that The sample needs to be placed in the pipette in advance, and then the Y-axis direction is adjusted through the manual two-axis stage so that the pipette is at the top of the middle position of the sample stage.

8. The device according to claim 6, It is characterized in that The air pump injects air into the air tube, and then hits the button on the top of the pipette to inject the liquid into the middle of the sample stage.

9. The device according to claim 1, It is characterized in that The signal receiving system comprises: a photodiode close to the detector, a photodiode supporting rod and a picoammeter.

10. A remote control system, It is characterized in that include: A portable multifunctional GIWAXS remote testing device according to any one of claims 1 to 9; as well as The software operation interface corresponding to the server can remotely control the portable multifunctional GIWAXS remote testing device according to any one of claims 1 to 9.

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