Portable multifunctional GIWAXS remote testing device

Abstract

The application provides a portable 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-directional movement function so as to accurately place the sample in the position between the X-ray path and the detector in the experiment; the sample multi-environment variable system accurately sets various parameters according to the user's demand, including temperature, spin coating speed, atmosphere environment and humidity; and the signal receiving system receives the X-ray after passing through the sample and converts the received X-ray signal into an electric signal.The portable multifunctional GIWAXS remote testing device provided by the application can be conveniently and quickly operated by personnel in different fields when they perform GIWAXS experiment testing, and high-efficiency work is realized.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of in-situ detection, and particularly relates to a portable multifunctional GIWAXS remote testing device. BACKGROUND

[0002] The crystal structure of material surfaces (such as thin films) has always been a difficulty in research, and therefore how to accurately detect the crystal structure of these samples has always been a focus of attention. We need to accurately analyze the crystal structure of the sample under test on a microscopic scale and in multiple dimensions, which is an important focus of current research.

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

[0004] In-situ measurement is of great interest for the study of thin film material surfaces, as it provides us with a method for quickly tracking the changes in the microstructure of materials, including crystallization and aging processes, which are crucial for revealing the dynamics of the material. The formation process of the crystal structure of the thin film material surface is not yet fully understood, and the film formation process involves a liquid film gelation stage and a crystallization stage. In-situ GIWAXS technology provides us with important information about the composition evolution during the spin coating process, and this technology plays an indispensable role in the study of thin films and surface materials.

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

[0006] However, it is worth noting that the current existing related devices generally have low work efficiency, complex operation and limited functions. Therefore, how to solve these problems has become one of the important challenges for the technical personnel in the field 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

[0007] The purpose of the present application is to provide a portable multifunctional GIWAXS remote testing device, which enables personnel from different fields to operate conveniently and quickly during GIWAXS experimental testing, and at the same time can perform experiments in different systems (such as liquid, solid) and different atmospheres (such as nitrogen, oxygen) and other diverse environments, achieving efficient work.

[0008] To achieve the above-mentioned purpose, in a first aspect, the present application provides a portable multifunctional GIWAXS remote testing device, which comprises a support and motion control system, a sample multi-environment variable system and a signal receiving system.

[0009] The support and motion control system has a multi-directional movement function, so as to accurately place the sample between the X-ray path and the detector during the experiment;

[0010] The sample multi-environment variable system is accurately set according to user requirements, including multiple parameters such as temperature, spin coating speed, atmosphere environment and humidity;

[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 comprises a counterweight machine box, a linear motor, a control machine box, a support frame, a support platform, a level and an inclination instrument Roll and Pitch axis.

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

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

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

[0016] In some embodiments, the sample multi-environment variable system comprises a pipette, an air pipe, a support, a manual two-axis table, a spin coating protective cover, a sample table, a heating spin coater, a heating spin coater controller, a cold head and an atmosphere cover connected with the detector.

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

[0018] In some embodiments, the air pump injects air into the air pipe, and then hits the top button of the pipette to inject liquid into the middle of the sample table.

[0019] In some embodiments, the signal receiving system comprises a photodiode near the detector, a photodiode support rod, and a picoammeter.

[0020] In a second aspect, the application further provides a remote control system, which comprises:

[0021] According to the portable multifunctional GIWAXS remote testing device described above; and

[0022] A software operation interface corresponding to the server, which can remotely control the portable multifunctional GIWAXS remote testing device described above.

[0023] The system provided by the embodiments of the application realizes GIWAXS testing of various different types of test samples through cooperation between the support and motion control system, the sample multi-environment variable system, and the signal receiving system, and is easy to operate and has strong usability, realizes convenient and rapid operation, and helps test personnel to realize efficient work. BRIEF DESCRIPTION OF DRAWINGS

[0024] Figure 1 A three-dimensional coordinate diagram is provided for the embodiments of the application;

[0025] Figure 2 A structural diagram of the support and motion control system is provided for the embodiments of the application;

[0026] Figure 3 A structural diagram of the sample multi-environment variable system is provided for the embodiments of the application;

[0027] Figure 4 A structural diagram of the signal receiving system is provided for the embodiments of the application;

[0028] Figure 5 A schematic diagram of the software operation interface is provided for the embodiments of the application.

[0029] EXPLANATION OF REFERENCE NUMBERS:

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

[0031] In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the application. However, it will be apparent to one skilled in the art that the application can be practiced without these specific details. In other instances, well-known methods have not been described in detail in order to avoid unnecessarily obscuring the present application. It will be understood that the terms "system," "device," "unit," and / or "module" as used herein are used in their broadest context to mean different components, elements, parts, or assemblies at different levels in a sequential arrangement. However, these terms can be replaced by other expressions if the same purpose can be achieved.

[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 can be directly on, connected, or coupled to the other device, unit, or module, or intervening devices, units, or modules can be present, unless the context clearly dictates otherwise. For example, as used herein, the term "and / or" includes any and all combinations of one or more of the associated listed items.

[0033] The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used herein, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and / or "comprising," when used in this specification, specify the presence of stated features, integers, steps, operations, elements, and / or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and / or groups thereof.

[0034] These and other features and characteristics of the present application, as well as the methods of operation and functions of the related elements of the structure and the combination of parts and economies of manufacture, will become more apparent upon consideration of the following description and the appended claims with reference to the accompanying drawings, all of which form a part of this specification. It is to be expressly understood, however, that the drawings are for the purpose of illustration and description only and are not intended as a definition of the limits of the application. It should be understood that the drawings are not drawn to scale.

[0035] Various structural diagrams are used in the present application to illustrate various modifications of embodiments according to the present application. It should be understood that the foregoing or the following structures are not intended to limit the present application. The scope of protection of the present application is subject to the claims.

[0036] The present application aims to realize in-situ characterization of thin film and material surface lattice information, and make full use of high-intensity synchrotron radiation source and high-performance area detector. Our goal is to develop a portable multifunctional GIWAXS testing device to realize efficient, in-situ, rapid testing of structural changes of liquid solution, thin film and various material surfaces, while also having the ability to detect the influence of temperature and atmosphere and other environments on the sample. In addition, we also focus on introducing a remote control system, so that users can conveniently remotely operate and manage the testing system to meet diverse experimental needs.

[0037] In order to realize in-situ characterization of the crystal phase structure of thin films, solid material surfaces and solution samples during crystallization, we have successfully established a portable multifunctional GIWAXS testing device and remote control system based on crystallography line station at the synchrotron radiation source. The whole is mainly composed of three parts, including support and motion control system, sample multi-environment variable system and signal receiving system. The support and motion control system has multi-directional movement function, so as to accurately place the device in the position 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 of the support table 6, ensuring that the X-ray is accurately irradiated on the sample, and monitoring the X-ray through the readings of the photodiode 20 and the picoammeter 22 in the signal receiving system. In addition, we can also adjust the inclination angle of the motorized turntable through the motion control system to accurately control the incident angle and penetration depth of the X-ray, meeting the requirements of different samples. This system allows us to flexibly adapt to different experimental needs to realize detailed study of the crystallization behavior of the sample. The multi-environment 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 enable researchers to comprehensively control and adjust for different experimental purposes and material characteristics, to ensure the best match of experimental conditions, so as to obtain accurate and reliable experimental results. Finally, a user-friendly interface 23 is designed to allow users to 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 application is designed to develop a portable multifunctional instrument testing device and remote control system, so that personnel in different fields can conveniently and quickly operate during GIWAXS experimental testing, while being able to conduct experiments in different systems (such as liquid, solid) and different atmospheres (such as nitrogen, oxygen) and other diverse environments, to realize efficient work.

[0039] In order to achieve the above-mentioned purpose, the application provides a portable multifunctional GIWAXS remote testing device, which is based on a line station to build a testing platform, and comprises a case 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 case 1 internally stores a system controller and a linear motor 2, and a support frame 5 is arranged on the top of the case 1.

[0041] The frame rod is provided with a support platform 6, a level 7, a manual two-axis table 12 and a pipette fixing frame.

[0042] The heating spin coater 15 is arranged on the support platform 6, wherein the heating and the spin coating can be simultaneously performed or separately operated, the solution sample is uniformly spin coated, and the film is formed by accelerating drying through heating, and the conformation change with temperature change is observed in situ.

[0043] The level 7 needs to keep the balance of the support platform 6, and can also conveniently adjust the angle change of the sample.

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

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

[0046] The liquid outlet mode of the pipette 9 adopts a gas pump control liquid outlet mode.

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

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

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

[0050] The polyimide film is adopted on the light path of the liquid protective cover 13 and the atmosphere cover 19, which does not diffract X-rays and does not affect the sample signal.

[0051] The X-ray light needs to be received by the photodiode 20 after passing through the sample, and the corresponding current signal information is displayed through the picoammeter 22.

[0052] The photodiode 20 is arranged at the front end of the detector 18, and is convenient for receiving signals.

[0053] The cooling device includes a cold head 17 at the front end of the sample stage, which is connected to liquid nitrogen. The cold head 17 can quickly reduce the temperature of the sample stage by blowing low-temperature nitrogen gas after the sample stage is heated, thereby reducing the waiting time of the user.

[0054] As shown in Figures 1 to 5 The present application 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 box 1, a linear motor (Z-axis) 2, control boxes 3, 4, a support frame 5, a support platform 6, a level 7, and a tilt angle instrument 8 Roll and Pitch axes; the sample multi-environment variable system includes a pipette 9, an air pipe 10, a support 11, a manual two-axis stage 12, a spin coating protective cover 13, a sample stage 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 operation steps are as follows:

[0057] First, the position of the X-ray is found by adjusting the linear motor 2 to adjust the Z-axis direction so that the sample is parallel to the X-ray and just partially blocks the light path, thereby ensuring that the light beam is incident on the sample surface in the form of a grazing incidence. The way to determine whether the sample blocks the light beam is to read the current signal received by the photodiode 20 on the picoammeter 22. Compared with the full passage, the current reading when blocked is about half of the full passage. Then, by adjusting the tilt angle instrument 8 Roll and Pitch axes, the level of the workbench 6 is adjusted, and the level is determined by the level 7. The horizontal determination standard is whether the maximum current signal on the picoammeter 22 can be reached after partially blocking the light beam.

[0058] Second, the incident angle is controlled by adjusting the pitch axis of the tilt angle instrument 8 to control the inclined sample stage, so that the X-ray passes through the sample. The penetration ability of the X-ray is closely related to the selected energy and the incident angle of the experiment. According to the user's needs and the characteristics of the sample, the energy can be selected within the range of 5-20 KeV.

[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 by the manual two-axis stage 12 so that the pipette 9 is on top of the middle position of the sample stage 14. Then click the glue gun injection on the software operation interface 23, and the air pump injects air through the air pipe 10 in a short time, and then press the top button of the pipette 9 to quickly inject the liquid into the middle of the sample stage 14.

[0060] After the liquid sample is added, click to start the spin coating. Before spin coating, place the spin coating shield 13 to prevent liquid splashing, and click the heating spin coater 15 switch to adjust the spin coating speed and time through the heating 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, improving the test efficiency.

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

[0063] After the X-ray passes through the light path, it hits the photodiode 20, and the optical signal is transmitted to the picoammeter 22, which judges whether the X-ray hits the sample by the current value change.

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

[0065] The technical effect of the present application not only has advanced experimental performance and reliability, but also has wide application potential, and is expected to promote the development of scientific research and engineering application, and provides a powerful tool for researchers in the field of materials science and related fields. The specific performance is:

[0066] 1. Simple and easy to operate: The design of the device platform focuses on user friendliness, making the testing of thin films, solid material surfaces and solution samples extremely simple and easy to operate. The intuitive user interface and automatic control system simplify the preparation and operation process of the experiment, thereby reducing the technical threshold, so that more researchers can easily carry out experimental work.

[0067] 2. In-situ testing under multiple conditions: The device not only can perform in-situ testing, but also can work under various environmental conditions such as different temperatures, humidities and atmospheres as needed. The flexibility of this multi-environmental variable system allows 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 a synchrotron X-ray source, the device platform of the present application ensures the high reliability of thin film preparation process and atmosphere. This means that the experimental results are more accurate and repeatable, which helps researchers to obtain stable and consistent data in material characterization and research.

[0069] 4. Improve work efficiency: The high efficiency and multi-functionality of the device greatly improve the work efficiency. It allows atmosphere, temperature, sample state to carry out multiple experiments at the same time, reduces the waiting time of the experiment, so as to obtain the experimental results faster. This is very advantageous 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 process of the above-described devices and modules can refer to the corresponding description in the foregoing device embodiments, and will not be described here.

[0071] It should be understood that the above specific embodiments of the present application are only used for illustrative or explanatory purposes of the principles of the present application, and do not constitute a limitation on the present application. Therefore, any modification, equivalent replacement, improvement, etc. made without departing from the spirit and scope of the present application shall be included in the protection scope of the present application. In addition, the appended claims of the present application are intended to cover all variations and modifications falling within the scope and boundary of the appended claims, or the equivalent forms of such scope and boundary.

Claims

1. A portable multifunctional GIWAXS remote testing device, comprising: Support and motion control system, sample multi-environment variable system and signal receiving system; The support and motion control system has a multi-directional movement function, so as to accurately place the sample in the position between the X-ray path and the detector in the experiment; The sample multi-environment variable system accurately sets various parameters according to user requirements, including temperature, spin coating speed, atmosphere environment, humidity, etc., and comprises a pipette, an air pipe, a support, a manual two-axis table, a spin coating protective cover, a sample table, a heating spin coater, a heating spin coater controller, a cold head, and an atmosphere cover connected with the detector; The liquid outlet mode of the pipette adopts an air pump control liquid outlet mode, the air pump injects air into the air pipe, and then strikes the top button of the pipette to inject liquid into the middle of the sample table; The heating spin coater is provided with a liquid spin coating protective cover and an atmosphere cover at the top end, the spin coating protective cover can avoid sample splashing during spin coating, and the atmosphere cover fills the distance between the sample and the detector with a specific atmosphere environment; The signal receiving system comprises a photodiode connected with the detector, a photodiode support rod, and a picoammeter, X-rays hit the photodiode after passing through the light path, the optical signal is transmitted to the picoammeter, and whether the X-rays hit the sample is judged by the current value change of the picoammeter.

2. The apparatus of claim 1, wherein, The support and motion control system comprises a counterweight machine box, a linear motor, a control machine box, a support frame, a support platform, a level, and a tilt angle instrument Roll and Pitch shaft.

3. The apparatus of claim 2, wherein, The level of the workbench is adjusted by adjusting the tilt angle instrument Roll and Pitch shaft.

4. The apparatus of claim 3, wherein, Whether the workbench is level is judged by the level.

5. The apparatus of claim 2, wherein, The Z-axis direction is adjusted by adjusting the linear motor, so that the sample is parallel to the X-ray, and part of the sample just blocks the light, so that the X-ray can hit the sample.

6. The apparatus of claim 1, wherein, The sample needs to be placed in the pipette in advance, and then the Y-axis direction is adjusted by the manual two-axis table, so that the pipette is on the top of the middle position of the sample table.

7. A remote control system characterized by comprising: It comprises: The portable multifunctional GIWAXS remote testing device according to any one of claims 1 to 6; And The software operation interface corresponding to the server, the software operation interface can remotely control the portable multifunctional GIWAXS remote testing device according to any one of claims 1 to 6.

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