Photothermoelectric multi-physical field in-situ X-ray diffraction testing device

Abstract

The invention discloses a photo-thermoelectric multi-physical field in-situ X-ray diffraction testing device, which comprises a device main body structure and a device upper cover, and is characterized in that the device main body structure is connected with the device upper cover to form a closed cavity; a light source is arranged at the top of the device upper cover and used for providing excitation irradiation for a to-be-detected sample; a butt joint support is arranged on the outer side of the device body structure and used for being in butt joint with an X-ray diffractometer, and in-situ XRD testing of a to-be-tested sample is achieved. An ITO heating glass sample table, an ITO glass heating probe, a spectrograph and an electrical logging probe are arranged in the device main body structure, the ITO heating glass sample table is used for placing a sample to be tested, and the ITO glass heating probe is in contact with the ITO heating glass sample table and is used for performing heating temperature control on the sample to be tested; the spectrograph is arranged below the ITO heating glass sample table and is used for testing the fluorescence emission spectrum of the sample to be tested; the electric testing probe is in direct contact with the to-be-tested sample and is used for testing an electric signal of the to-be-tested sample and / or providing electric excitation for the to-be-tested sample.

Description

Technical Field

[0001] This invention relates to the field of in-situ characterization and structural analysis of materials using multiphysics, specifically to an in-situ X-ray diffraction testing device using photothermal and electrophysical multiphysics. Background Technology

[0002] In-situ X-ray diffraction (XRD) is an important technique for studying the evolution of material structures, and it is widely used in research fields such as thermal stability, phase transition behavior, and stress evolution of battery materials, optoelectronic materials, catalysts, and other functional materials. Especially in the development of new energy materials and devices, in-situ XRD can provide real-time, non-destructive crystal structure information, making it a key tool for analyzing structure-property relationships.

[0003] In practical applications, many advanced materials (such as perovskite solar cells, polymer electrode materials, and low-dimensional nanomaterials) are highly sensitive to operating conditions such as light, temperature, and electric fields. Their crystal structure, electronic structure, and device performance may undergo complex evolution with changes in the external environment. Studying the influence of these physical fields on material performance has significant scientific and engineering value. Among these, the effect of light: Light is a direct operating condition for optoelectronic functional materials, directly affecting processes such as light absorption, carrier generation and transport, and photoinduced defect formation. In perovskite solar cells or light-emitting devices, light not only drives charge separation and photoelectric conversion but may also induce photoinduced ion migration or photoinduced degradation. Therefore, studying the structural evolution and performance changes under light is crucial for understanding material stability and improving device efficiency. The effect of temperature: Temperature changes can cause phenomena such as lattice expansion, phase transitions, stress-strain evolution, and interface mismatch, thereby affecting the structural stability and electrical performance of materials. In the actual operation of optoelectronic devices, temperature fluctuations are unavoidable. Therefore, studying the in-situ structural evolution of materials under different temperature conditions helps to reveal thermal failure mechanisms, optimize material heat resistance, and improve the long-term stability of devices. The effect of electric fields: Electric fields are a critical condition for the normal operation of optoelectronic devices and an important stimulus for electrochemical or electronic device research. An applied electric field can not only drive carrier migration but also potentially lead to ion migration, interfacial reactions, or field-induced phase transitions. In the study of optoelectronic materials and devices, applying an electric field and simultaneously monitoring structural and performance changes helps to understand carrier dynamics, electrode interface effects, and electrodegradation mechanisms, thus providing a basis for device design and reliability assessment.

[0004] Currently, existing testing devices still have limitations in terms of multiphysics coupling capabilities, mainly including: 1) The Challenge of Multi-Physics Coupling: Existing technologies typically only consider single or dual physical fields in their structural design, lacking a holistic solution for the synchronous coupling of multiple fields such as light, heat, and electricity. The incident and diffracted X-ray light, the fluorescence excitation source and spectrometer, the electrical probe, and the temperature control device need to work simultaneously and coordinately within a limited space. Furthermore, interference may exist between modules, leading to complex device structures and significant engineering challenges in implementing in-situ multi-field testing. For example, existing technologies propose temperature-controlled in-situ optical observation cavities capable of optical testing under high-temperature conditions, but their structures are not adapted to X-ray diffractometers and do not consider electrical testing modules. Existing technologies also disclose an X-ray diffraction and X-ray fluorescence analysis instrument capable of rapid sample analysis without sample preparation, but its design does not consider temperature control or electrical stimulation, nor does it take into account illumination conditions, making it impossible to conduct in-situ multi-physics coupling studies.

[0005] 2) The importance of multi-field coupling has not been fully considered: Most existing devices only focus on a single physical field (such as temperature control or optics), and the combined effects of multiple physical fields such as light, heat, and electricity have not been studied. However, these coupling effects have a critical impact on the structural stability and performance evolution of optoelectronic materials and devices under actual operating conditions. Therefore, the lack of multi-field coupling testing capabilities limits our understanding of the behavior of materials under real operating conditions.

[0006] 3) Limitations on simultaneous in-situ measurement and data acquisition: Existing technologies typically cannot simultaneously acquire XRD structural information, optical signals, and electrical responses under multi-physics conditions, making it impossible to analyze the structure-property relationship of materials under actual working conditions in real time. Furthermore, some devices are large in size, and their cavities are incompatible with XRD optical paths or electrical interfaces, making long-term stable testing or portable operation difficult, thus limiting comprehensive research on the evolution of material properties.

[0007] Therefore, current technologies do not yet provide a testing device that can simultaneously support the coupling effects of multiple physical fields such as light, temperature, and electric fields, and has in-situ XRD measurement capabilities. Thus, developing a compact testing device that can realize multi-physical field coupling (photothermal and electrical), simultaneously support in-situ XRD measurements, and has the ability to apply an electric field to the sample and acquire electrical signals is of significant engineering value and application potential for revealing the structural evolution and performance correlation of optoelectronic functional materials under actual working conditions, and for promoting material reliability evaluation and device optimization. Summary of the Invention

[0008] The present invention aims to at least solve one of the technical problems existing in the prior art. Therefore, in response to the above-mentioned problems, the object of the present invention is to provide a photothermal-electric multi-physics field in-situ X-ray diffraction testing device, capable of simultaneously performing in-situ XRD testing, optical measurement, and electrical signal acquisition under the influence of multiple physical fields such as illumination, temperature, and electric field.

[0009] To achieve the above-mentioned objectives, the technical solution adopted by this invention is as follows: The present invention provides an in-situ X-ray diffraction testing device for photothermal and electro-optical multiphysics fields, comprising a main device structure and a device cover, wherein the main device structure is connected to the device cover to form a sealed cavity; The device is equipped with a light source on the top of its cover, which is used to provide excitation irradiation for the sample to be tested; The main structure of the device is provided with a docking bracket on the outside for docking with an X-ray diffractometer to realize in-situ XRD testing of the sample to be tested. The main structure of the device includes an ITO heated glass sample stage, an ITO heated glass probe, a spectrometer, and an electrical probe, wherein: The ITO heated glass sample stage is used to place the sample to be tested, and the ITO glass heating probe is in contact with the ITO heated glass sample stage to heat and control the sample to be tested. The spectrometer is positioned below the ITO heated glass sample stage and is used to test the fluorescence emission spectrum of the sample to be tested. The electrical probe directly contacts the sample under test and is used to test the electrical signal of the sample under test and / or provide electrical excitation to the sample under test.

[0010] In some possible implementations, the main structure of the device is further provided with a light source shielding ring, a light source focusing ring, and a light transmission window, wherein the light emitted by the light source passes through the light source shielding ring, the light source focusing ring, and the light transmission window in sequence to illuminate the sample to be tested, thereby providing optical excitation to the sample to be tested.

[0011] In some possible implementations, the main structure of the device is further provided with a light source heat sink and a light source cooling fan. The light source is an LED lamp bead, which is mounted on the light source heat sink. The light source cooling fan is also mounted on the side of the light source heat sink to dissipate heat for the LED lamp bead.

[0012] In some possible implementations, the main structure of the device is further provided with a sample stage holder and a holder mounting column. The ITO heated glass sample stage is mounted on the sample stage holder, and the ITO glass heating probe is also mounted on the sample stage holder. The holder mounting column is used to fix the sample stage holder to the main structure of the device, keeping the position of the sample stage holder and the ITO heated glass sample stage fixed.

[0013] In some possible implementations, the electrical probe is fixed to the sample stage holder by an electrical probe fixing stud and is connected to the electrical testing and power supply penetrator by a connecting wire. The electrical testing and power supply penetrator is connected to external testing equipment through a DB9 connector.

[0014] In some possible implementations, a temperature detector is also provided inside the main structure of the device, and a thermocouple connector is provided at the bottom of the main structure of the device, wherein the temperature detector is connected to the thermocouple connector for testing the temperature of the surface of the sample to be tested.

[0015] In some possible implementations, a ball valve is also provided on the side of the main body of the device for injecting the required gas into the main body of the device.

[0016] In some possible implementations, a clamping screw is also provided, which is used to press the device cover onto the main structure of the device to achieve a seal for the entire device.

[0017] In some possible implementations, the side of the device cover is provided with a transmission window for observing the state of the sample to be tested inside the main structure of the device.

[0018] In some possible implementations, the X-ray diffractometer is provided with a slot, through which the X-ray diffractometer is docked with the main structure of the device via the docking bracket.

[0019] Because the present invention adopts the above technical solution, it has the following characteristics: 1. The optical path and the XRD optical path do not interfere with each other, achieving efficient optical measurement: This invention employs an optical path design that irradiates the excitation light from above the device. The spectrometer is positioned below a transparent sample stage. The excitation light irradiates the sample stage from above, and the spectrometer receives the emitted light signal from below the sample stage. Simultaneously, it does not affect the transmission of the X-ray incident and diffraction optical paths. The optical measurement path is spatially isolated from the XRD incident and diffraction optical paths, avoiding mutual interference. This improves the accuracy and repeatability of multi-physics in-situ measurements, ensures high-sensitivity acquisition of optical signals under heating or electrical excitation conditions, and enables in-situ analysis with optical-thermal-electric coupling.

[0020] 2. Transparent, heatable ITO glass sample stage, enabling both sample temperature control and optical observation: This invention employs a transparent, heatable ITO glass sample stage, which not only enables precise temperature control of the sample but also ensures that the spectrometer below can directly receive the emitted light signal. This design combines optical observation and thermal control functions, while supporting sample heating and electrical testing. It enables high-sensitivity optical signal acquisition even when the sample is heated, providing reliable technical support for the simultaneous study of the structural and performance evolution of materials under temperature control conditions. It effectively integrates the functions of optical observation, thermal control, and electrical application, improving the multifunctionality and repeatability of the experiment.

[0021] 3. Simultaneously considering both electrical excitation and electrical signal measurement, enabling multi-physics coupled analysis: This invention introduces an electrical probe that can apply an external electric field to the sample and simultaneously acquire electrical signals. Compared with existing technologies, this invention can simultaneously monitor the structural, optical, and electrical changes of materials under the coupling of multiple physical fields (optical, thermal, and electrical), significantly improving the ability to analyze the behavior of optoelectronic functional materials under actual working conditions.

[0022] 4. The ingenious structure and non-interfering coupling enhance experimental accuracy and data reliability: This invention achieves coordination between the X-ray incident and diffraction optical paths, optical excitation source and spectrometer, electrical probe and temperature control device through overall cavity design and module layout optimization. It solves the problem of possible mutual interference between functional modules during the synchronous application of multiple physical fields. It can simultaneously carry out in-situ XRD measurement, optical measurement and electrical signal acquisition under the action of multiple physical fields such as light, temperature and electric field, realize efficient synergy of XRD, optical and electrical measurements, significantly improve the accuracy and data reliability of in-situ multi-physics field experiments, and provide a reliable technical means for revealing the evolution mechanism of material properties.

[0023] 5. Electrical excitation and electrical signal acquisition functions: This invention is equipped with an electrical interface that can apply an external electric field to the sample while simultaneously acquiring electrical signals in real time. It can be performed synchronously with optical and XRD measurements, and can fully reflect the behavior of materials under the action of multiple physical fields of light, heat and electricity. This enhances the scientific value of studying the structural and performance evolution of optoelectronic functional materials under actual working conditions.

[0024] 6. Multiphysics Co-loading and Environmental Stability Design: This invention achieves stable application and mutual isolation of various physical fields through overall cavity and module layout optimization; ensures continuous monitoring of the structure and performance of samples under controlled environment in long-term multi-field coupling experiments; improves experimental accuracy and data reliability, and provides a solid technical foundation for material performance optimization.

[0025] In summary, this invention achieves in-situ XRD testing capabilities with simultaneous coupling of photothermal and electrical multi-physics fields through optical path optimization, a transparent and heatable sample stage, and electrical measurement design. This is significantly superior to existing technologies and has important scientific research value and engineering application prospects. It can be applied to light, heat, and electricity-sensitive material systems such as perovskite solar cells, flexible electronic devices, energy storage electrode materials, and MOFs. It can also be extended to the research of other functional materials that require in-situ analysis with multi-physics field coupling, demonstrating high versatility and engineering adaptability. Attached Figure Description

[0026] Various other advantages and benefits will become apparent to those skilled in the art upon reading the following detailed description of preferred embodiments. The accompanying drawings are for illustrative purposes only and are not intended to limit the invention. Throughout the drawings, the same reference numerals denote the same parts. In the drawings: Figure 1 This is a cross-sectional view of the device structure according to an embodiment of the present invention; Figure 2 The diagram shows the structure of the device when it is open and closed according to an embodiment of the present invention, wherein (a) is the open state and (b) is the closed state; Figure 3 This is a schematic diagram of the photoluminescence spectra of the sample in state a and state b before and after heating in an embodiment of the present invention; Figure 4 This is a schematic diagram of the XRD patterns of the a-state and b-state before and after heating in an embodiment of the present invention. Detailed Implementation

[0027] It should be understood that the terminology used herein is for the purpose of describing particular exemplary embodiments only and is not intended to be limiting. Unless the context clearly indicates otherwise, the singular forms “a,” “an,” and “described” as used herein may also include the plural forms. The terms “comprising,” “including,” “containing,” and “having” are inclusive and therefore indicate the presence of the stated features, steps, operations, elements, and / or components, but do not exclude the presence or addition of one or more other features, steps, operations, elements, components, and / or combinations thereof. The method steps, processes, and operations described herein are not construed as requiring them to be performed in a particular order described or illustrated unless the order of performance is explicitly indicated. It should also be understood that additional or alternative steps may be used.

[0028] Although terms such as first, second, third, etc., may be used in this document to describe multiple elements, components, regions, layers, and / or segments, these elements, components, regions, layers, and / or segments should not be limited by these terms. These terms may be used only to distinguish one element, component, region, layer, or segment from another. Unless the context clearly indicates otherwise, terms such as "first," "second," and other numerical terms used herein do not imply order or sequence. Therefore, the first element, component, region, layer, or segment discussed below may be referred to as the second element, component, region, layer, or segment without departing from the teachings of the exemplary embodiments.

[0029] For ease of description, spatial relative terms may be used in the text to describe the relationship of one element or feature relative to another element or feature as shown in the figure. These relative terms include, for example, "inside," "outside," "middle," "outer," "below," "above," etc. Such spatial relative terms are intended to include different orientations of the device in use or operation, other than those depicted in the figure.

[0030] To address the technical challenges of existing in-situ XRD testing devices, such as difficulty in achieving simultaneous optical, thermal, and electrical effects under multi-physics coupling conditions, ensuring that XRD structural measurements and electrical signal acquisition do not interfere with each other, maintaining the stability of the testing environment, and the complexity of the device structure. This invention provides an in-situ X-ray diffraction testing device using photothermoelectric multiphysics fields, comprising a main structure and a top cover. The main structure and the top cover form a sealed cavity. A light source is located on the top of the top cover to provide excitation irradiation for the sample under test. A docking bracket is located on the outside of the main structure for docking with an X-ray diffractometer to achieve in-situ XRD testing of the sample. The main structure contains an ITO heated glass sample stage, an ITO heated glass probe, a spectrometer, and an electrical probe. The ITO heated glass sample stage is used to place the sample under test. The ITO heated glass probe contacts the ITO heated glass sample stage for heating and temperature control of the sample. The spectrometer is located below the ITO heated glass sample stage for testing the fluorescence emission spectrum of the sample. The electrical probe directly contacts the sample to test the electrical signal and / or provide electrical excitation to the sample. Therefore, this invention enables simultaneous in-situ testing of samples under controlled illumination, temperature, and electric fields, allowing for the correlation analysis of the crystal structure, optical and electrical properties of materials under real working conditions. It can not only apply an external electric field or current to the sample but also achieve in-situ acquisition of electrical signals, thereby constructing a multi-field coupling environment together with illumination and temperature control. This invention is suitable for in-situ research on optoelectronic materials, energy conversion and storage devices (such as perovskite solar cells, photodetectors and light-emitting devices), and can be used to reveal the mechanism of material structure evolution and performance change under the synergistic effect of multiple physical fields.

[0031] Exemplary embodiments of the invention will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the invention and to fully convey the scope of the invention to those skilled in the art.

[0032] like Figure 1 , Figure 2As shown, the photothermal-electric multiphysics field in-situ X-ray diffraction testing device provided in this embodiment includes a main device structure 1 and a device cover 2.

[0033] The main structure 1 of the device is connected to the device cover 2 via a rotating shaft 3. A light source 4 is installed on the top of the device cover 2 to provide excitation irradiation for the sample to be tested.

[0034] The main structure 1 of the device is equipped with an ITO heated glass sample stage 5 and an ITO glass heated probe 6. The ITO heated glass sample stage 5 is used to place the test sample, and the ITO glass heated probe 6 is in contact with the ITO heated glass sample stage 5 to heat and control the temperature of the test sample on the ITO heated glass sample stage 5. The main structure 1 of the device also includes a spectrometer 7, which is located below the ITO heated glass sample stage 5 and is used to detect the fluorescence emission spectrum of the sample to be tested.

[0035] The main structure 1 of the device is also equipped with an electrical probe 8. The tip of the electrical probe 8 directly contacts the sample to be tested and is used to test the electrical signal of the sample to be tested and / or to provide electrical excitation to the sample to be tested. The main structure 1 of the device is provided with a docking bracket 9 on the outside, which is used to dock with the X-ray diffractometer to realize in-situ XRD testing of the sample to be tested.

[0036] In a preferred embodiment of the present invention, the light source 1 is disposed at the top of the device cover 2 via the light source limiting flange 10, and is used to provide excitation irradiation for the sample to be tested.

[0037] Furthermore, the light source 1 can be configured as a replaceable structure, and can be replaced with a light source of selected wavelength or color temperature as needed. For example, the spectrum that the light source 1 can use is not limited to monochromatic light, white light, etc. in the range of 300-1400nm.

[0038] Furthermore, the light source 1 can be an LED lamp bead. The light emitted by the LED lamp bead is projected onto the light transmission window 13 through the light source shielding ring 11 and the light source focusing lens 12, and then shines on the sample to be tested through the light transmission window 13, providing optical excitation for the sample to be tested.

[0039] Furthermore, the LED beads are fixed on the heat sink 14, and the heat sink 14 has a heat sink fan 15 on its side to dissipate heat for the LED beads.

[0040] In a preferred embodiment of the present invention, the ITO heated glass sample stage 5 is disposed on the sample stage holder 16, and the sample stage holder 16 is provided with an ITO glass heating probe 6. The ITO glass heating probe 6 contacts the ITO heated glass sample stage 5 and is used to heat and control the sample on the ITO heated glass sample stage 5.

[0041] Furthermore, the temperature control range of the ITO heated glass sample stage 5 is from room temperature to 220 °C.

[0042] Furthermore, a mounting bracket 17 is provided to fix the sample stage mounting bracket 16 to the main structure of the device, keeping the sample stage mounting bracket 16 and the ITO heated glass sample stage 5 in a fixed position.

[0043] In a preferred embodiment of the present invention, the electrical probe 8 is fixed to the sample stage holder 16 by the electrical probe fixing stud 18, and is connected to the internal circuit connector 20 of the electrical measurement and power supply penetrating element 19 by a connecting wire. The penetrating element circuit board 21 is then connected to an external testing device through a DB9 connector 22. The external testing device can test the optical, electrical, and other information of the sample inside the device by connecting to this connector. In use, the tip of the electrical probe 8 directly contacts the sample to be tested. This circuit is used for the electrical signals (resistance, voltage, current, etc.) of the sample to be tested, and also for providing electrical excitation to the sample to be tested (such as applying a constant voltage, current, etc.). Combined with the light source 4 and the ITO heated glass sample stage 5, it realizes the control and testing of three physical fields: electricity, light, and temperature. For example, it can be used to control and test the electricity, light, and temperature of samples such as PVDF thin films and photochromic thin films.

[0044] Furthermore, a thermocouple connector 23 is provided at the bottom of the main body structure 1 of the device, and a temperature detector is also provided inside the main body structure 1 of the device. The temperature information of the surface of the sample to be tested is tested by connecting an independent temperature detector to the thermocouple connector 23.

[0045] In a preferred embodiment of the present invention, the spectrometer 7 is located below the ITO heated glass sample stage 5. Since the ITO heated glass sample stage 5 is made of transparent glass, the spectrometer 7 located below the ITO heated glass sample stage 5 can test the fluorescence emission spectrum of the sample to be tested.

[0046] Furthermore, the spectral detection range of spectrometer 7 is 400-1050 nm.

[0047] In a preferred embodiment of the present invention, the docking bracket 9 is used to dock with an X-ray diffractometer. In use, each X-ray diffractometer is provided with a slot, and docking is achieved by connecting with the docking bracket 9 through the slot to complete the in-situ XRD test of the sample to be tested.

[0048] In a preferred embodiment of the present invention, a ball valve 24 is provided on the left side of the main body structure 1 of the device for injecting a special gas, such as nitrogen, into the main body structure 1 of the device.

[0049] In a preferred embodiment of the present invention, a clamping screw 25 is also provided to clamp the device cover 2 onto the main structure 1 of the device, thereby achieving a seal for the entire device.

[0050] In a preferred embodiment of the present invention, the side of the device cover 2 has a transmission window 26 for observing the sample state inside the main structure 1 of the device.

[0051] The performance of the photothermal-electric multiphysics in-situ X-ray diffraction testing device of the present invention will be described in detail below through specific embodiments.

[0052] Example 1: In-situ XRD testing of thermochromic phase change materials based on the photothermoelectric multiphysics in-situ X-ray diffraction testing device of this example, including: S1. The device of this embodiment is fixedly installed on the X-ray diffractometer using the docking bracket 9. The X-ray diffractometer of this embodiment is Malvern PANalytical Empyrean.

[0053] S2. Place the AIE material 1,1,2,2-tetratetra(4-methoxyphenyl)ethylene (Adamas, >98% purity) on the ITO heated glass sample stage 5, and close the main structure 1 and the upper cover 2 of the device. At this time, the temperature is room temperature, the sample is in the α state, and appears as a transparent crystalline powder to the naked eye.

[0054] S3. Turn on light source 4 to irradiate the sample with a wavelength of 365nm and a light intensity of 50 mW / cm². 2 The sample emits blue light, and the fluorescence emission spectrum of the sample is obtained by using the spectrometer 7 located below the sample. The emission spectrum is shown in the figure below. Figure 3 As shown, the peak emission value is 432 nm.

[0055] S4. XRD test before heating: XRD scan was performed in the range of 2θ = 5°–55° using an X-ray diffractometer (Cu Kα rays, λ = 1.5405 Å) to obtain the XRD diffraction pattern of the sample in the α state.

[0056] S5. Using the ITO heated glass sample stage 5, heat the sample to 200℃ at a heating rate of 15℃ per minute. After heating to 200℃, the sample undergoes a phase transition to the b state, appearing as a yellow oily substance. Under 365nm illumination, it emits green fluorescence; the emission spectrum is shown below. Figure 3 The emission peak is 500nm.

[0057] S6. XRD test after heating: XRD scan was performed in the range of 2θ = 5°–55° using an X-ray diffractometer (Cu Kα rays, λ = 1.5405 Å) to obtain the XRD diffraction pattern of the b state of the sample.

[0058] Experimental results: The sample under test was a transparent crystalline powder in its initial state (a state). After being irradiated by a 365 nm wavelength light source (light intensity 50 mW / cm²), it emitted blue fluorescence, with the emission spectrum peak located at 432 nm (see...). Figure 3 The XRD pattern of the sample showed several clear diffraction peaks in the range of 2θ = 5°–55°, indicating a highly crystalline phase (see...). Figure 4 The sample was heated to 200°C (heating rate 15°C / min) using an ITO heated glass sample stage 5. The sample changed from a crystalline state (a state) to a yellow oily substance (b state). Under 365 nm illumination, the emission color changed to green, and the emission peak red-shifted to 500 nm (see...). Figure 3 Furthermore, the luminescence intensity of the b-state was significantly enhanced compared to the a-state, indicating a significant temperature-induced phase transition in the sample. In-situ XRD results showed a significant decrease in the intensity of the b-state XRD diffraction peaks, with some peaks shifting or disappearing, indicating that the sample transitioned from an ordered crystalline phase to a disordered or liquid crystal structure. Figure 4 As shown. Throughout the entire test, the illumination, heating, and X-ray diffractometer of this invention operated in synergy without any photothermal interference or X-ray diffraction signal interference. The results demonstrate that this invention can achieve in-situ coupled testing of multiple physical fields, including illumination, heating, and electrical signal measurement, within a single device, while ensuring the stability and independence of each physical field. This experiment fully verifies the feasibility and reliability of this invention in simultaneously tracking material structure and optical properties under photothermal synergy, providing strong support for the in-situ dynamic characterization of materials coupled with multiple physical fields.

[0059] In summary, the in-situ X-ray diffraction testing device for photothermal and electrophysical multi-physics fields provided by this invention, through its ingenious main structure design and modular layout, achieves coordination and isolation between the X-ray incident and diffraction optical paths, the optical excitation source and spectrometer, the electrical probe and temperature control device. This allows each physical field to be applied synchronously without interference, thereby ensuring the stability and data reliability of testing under multi-physics field coupling conditions. Furthermore, this invention can stably load samples for extended periods under the influence of multiple physical fields such as illumination, temperature, and electric fields, while simultaneously achieving in-situ XRD measurement, optical measurement, and electrical signal acquisition. This provides a reliable technical means to reveal the structure-performance relationship and device stability of optoelectronic functional materials under actual working conditions.

[0060] The various embodiments in this specification are described in a progressive manner. Similar or identical parts between embodiments can be referred to interchangeably. Each embodiment focuses on describing the differences from other embodiments. In the description of this specification, the terms "a preferred embodiment," "furthermore," "specifically," "in this embodiment," etc., refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the embodiments in this specification. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described can be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0061] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A photothermal-electric multiphysics in-situ X-ray diffraction testing device, characterized in that, It includes a main device structure and a top cover, wherein the main device structure is connected to the top cover to form a sealed cavity; The device is equipped with a light source on the top of its cover, which is used to provide excitation irradiation for the sample to be tested; The main structure of the device is provided with a docking bracket on the outside for docking with an X-ray diffractometer to realize in-situ XRD testing of the sample to be tested. The main structure of the device includes an ITO heated glass sample stage, an ITO heated glass probe, a spectrometer, and an electrical probe, wherein: The ITO heated glass sample stage is used to place the sample to be tested, and the ITO glass heating probe is in contact with the ITO heated glass sample stage to heat and control the sample to be tested. The spectrometer is positioned below the ITO heated glass sample stage and is used to test the fluorescence emission spectrum of the sample to be tested. The electrical probe directly contacts the sample under test and is used to test the electrical signal of the sample under test and / or provide electrical excitation to the sample under test.

2. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 1, characterized in that, The main structure of the device also includes a light source shielding ring, a light source focusing ring, and a light transmission window. The light emitted by the light source passes through the light source shielding ring, the light source focusing ring, and the light transmission window in sequence to illuminate the sample to be tested, providing optical excitation to the sample.

3. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 1, characterized in that, The main structure of the device also includes a light source heat sink and a light source cooling fan. The light source uses LED beads, which are mounted on the light source heat sink. The light source cooling fan is also mounted on the side of the light source heat sink to dissipate heat for the LED beads.

4. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 1, characterized in that, The main structure of the device is also provided with a sample stage fixing frame and a fixing frame mounting support. The ITO heated glass sample stage is set on the sample stage fixing frame, and the ITO glass heating probe is also set on the sample stage fixing frame. The fixing frame mounting support is used to fix the sample stage fixing frame on the main structure of the device, keeping the position of the sample stage fixing frame and the ITO heated glass sample stage fixed.

5. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 4, characterized in that, The electrical test probe is fixed to the sample stage holder by an electrical test probe fixing stud, and is connected to the electrical test and power supply penetrator by a connecting wire. The electrical test and power supply penetrator is connected to external testing equipment through a DB9 connector.

6. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 1, characterized in that, The main structure of the device is also equipped with a temperature detector, and a thermocouple connector is provided at the bottom of the main structure of the device. The temperature detector is connected to the thermocouple connector to test the temperature of the surface of the sample to be tested.

7. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 1, characterized in that, A ball valve is also provided on the side of the main structure of the device for injecting the required gas into the main structure of the device.

8. The in-situ X-ray diffraction testing device for photothermoelectric multiphysics fields according to claim 1, characterized in that, It is also equipped with clamping screws, which are used to press the upper cover of the device onto the main structure of the device to achieve a seal for the entire device.

9. The in-situ X-ray diffraction testing device for photothermoelectric multiphysics fields according to claim 1, characterized in that, The device has a transmission window on its side cover for observing the state of the sample to be tested inside the main structure of the device.

10. The photothermal-electric multiphysics in-situ X-ray diffraction testing device according to claim 1, characterized in that, The X-ray diffractometer is provided with a slot, through which the X-ray diffractometer is connected to the main structure of the device via the docking bracket.

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