Portable in-situ XRD testing device capable of being used in continuous high-temperature and high-humidity environment

By using an integrated heating design for the cavity and gas path of a portable in-situ XRD testing device, the problem of humidity maintenance and condensation under high temperature and high humidity conditions is solved. This enables the study of material structural stability under high temperature and high humidity conditions, supports off-site aging and intermittent in-situ testing, and is suitable for the research of humidity-sensitive materials such as perovskite solar cells and flexible electronic devices.

CN121656299APending Publication Date: 2026-03-13TSINGHUA UNIVERSITY
View PDF 2 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-12-11
Publication Date
2026-03-13

AI Technical Summary

Technical Problem

Existing in-situ XRD testing equipment has difficulty maintaining humidity under high temperature and high humidity conditions, posing a risk of condensation. Furthermore, its fixed structure cannot support long-term aging and intermittent in-situ tracking, thus failing to meet the needs of material structural stability research under high temperature and high humidity conditions.

Method used

A portable in-situ XRD testing device was designed, which adopts an integrated heating design for the cavity and gas path. Combined with temperature and humidity sensors and a control system, it realizes coordinated control of humidity and temperature in the gas circulation loop, ensuring the uniformity and stability of the environment in the sealed cavity. It also achieves off-site aging and intermittent in-situ testing through a detachable modular structure.

Benefits of technology

Stable humidity control was achieved under high temperature and high humidity conditions, avoiding condensation, supporting long-term aging and intermittent in-situ testing, improving the reliability and efficiency of testing, and applicable to the structural evolution research of various humidity-sensitive materials.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN121656299A_ABST
    Figure CN121656299A_ABST
Patent Text Reader

Abstract

The invention relates to a portable in-situ XRD testing device capable of being used in a continuous high-temperature and high-humidity environment, the portable in-situ XRD testing device comprises a base and an upper cover detachably connected with the base in a sealing manner, the upper cover and the base form a sealing cavity, and the upper cover is provided with a transmission window for introducing rays; the sample table is used for bearing a sample and is arranged in the groove of the base; the heater is arranged in the base and is used as a heat source of the sealed cavity; the temperature and humidity sensor probe is arranged in the sealed cavity and is connected with the data acquisition and feedback control system; and the temperature and humidity control box is connected with the base through two gas pipes with heating and heat preservation functions to form a gas circulation loop and is used for inputting mixed moisture with preset temperature and humidity into the sealed cavity. The device can stably operate for a long time under high-temperature and high-humidity conditions such as double-85, and in-situ or off-site structural analysis of a sample in a continuous high-humidity and high-heat environment is realized.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to a portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments, belonging to the field of material environmental stability characterization and in-situ diffraction analysis technology. Background Technology

[0002] In-situ X-ray diffraction (XRD) is a crucial technique for studying the structural evolution of materials, widely applied 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 provides real-time, non-destructive crystal structure information, serving as a key tool for analyzing structure-performance relationships. In practical applications, many advanced materials (such as perovskite solar cells, polymer electrode materials, and low-dimensional nanomaterials) are extremely sensitive to environmental temperature and humidity, and their long-term stability becomes a critical factor restricting their commercialization. Therefore, research on the structural stability of materials under high temperature and high humidity conditions has significant scientific and engineering value. The "85°C, 85% RH" environmental conditions (i.e., the "double 85 test") have been widely adopted as international stability evaluation standards in fields such as solar cells and encapsulation materials, such as IEC 61215 and the ISO S-D series of test protocols.

[0003] However, currently available XRD testing devices do not effectively support the "dual 85 environment." On the one hand, traditional in-situ XRD chambers mainly focus on high temperature or atmosphere control. For example, patent CN113049618A discloses an in-situ testing system suitable for high temperature and high pressure conditions, but it does not involve a humidity control mechanism, thus failing to meet the in-situ testing requirements of materials in humid and hot environments. On the other hand, patent CN116500066A discloses a humidity-controlled in-situ measurement system for X-ray diffractometers. Although it achieves humidity control under normal temperature conditions and is suitable for testing samples such as hydrated salts, its simple structural design, limited sealing performance, and lack of overall heating function make it difficult to apply to in-situ research in high temperature and high humidity environments.

[0004] Currently, achieving in-situ XRD testing under adjustable temperature and humidity, high temperature and high humidity, and especially stable dual 85°C conditions presents multiple engineering challenges: First, high humidity gases are prone to condensation during transmission, which may lead to problems such as X-ray window shading and sample electrode short circuits; second, the humid and hot environment places higher demands on the chamber's sealing and material corrosion resistance; third, the temperature control systems of the chamber and gas channels need to work together to ensure temperature and humidity uniformity and long-term stability within the testing space.

[0005] Furthermore, current XRD testing systems generally employ fixed testing structures and are bulky. Standard damp-heat stability tests often last for hundreds to thousands of hours. Using traditional continuous in-situ testing methods would severely consume XRD instrument resources and make it difficult to maintain the airtightness, thermal stability, and system reliability required for long-term testing. Currently, no publicly available system supports the completion of the damp-heat aging process of samples in an independent chamber, and allows for both off-site environmental maintenance and intermittent in-situ XRD testing via a portable, detachable structure. Therefore, developing a compact device capable of operating under high-temperature and high-humidity conditions, maintaining a damp-heat environment, and supporting portable intermittent XRD analysis is of significant engineering importance and application potential for monitoring structural evolution under standard high-temperature and high-humidity aging conditions. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides a portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments. This device can operate stably for a long time under typical high temperature and high humidity conditions such as dual 85 (85°C, 85%RH), enabling in-situ or ex-situ structural analysis of samples in continuous high humidity and high heat environments.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: A portable in-situ XRD testing device suitable for continuous high temperature and high humidity environments, comprising: The base and the upper cover that are detachably and sealingly connected to the base, the upper cover and the base forming a sealed cavity, the upper cover being provided with a transmission window for introducing rays; A sample stage, used to hold the sample, is set in the groove of the base; A heater, disposed in the base, serves as a heat source for the sealed cavity; A temperature and humidity sensor probe is installed inside the sealed cavity and connected to the data acquisition and feedback control system. The temperature and humidity control box is connected to the base through two air pipes with heating and heat preservation functions to form a gas circulation loop, which is used to input mixed humid air with preset temperature and humidity into the sealed cavity.

[0008] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments, preferably, includes a gas tube comprising a pipe, a heating belt wrapped around the outer wall of the pipe, and an insulation layer wrapped around the heating belt.

[0009] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments, preferably, has a spiral heating belt that is spirally wound around the outer wall of the pipe.

[0010] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments, preferably, has a thermal insulation layer made of thermal insulation cotton.

[0011] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments, preferably, includes any one of rock wool insulation, glass wool insulation, mineral wool insulation, aluminum silicate insulation, asbestos and polyester fiber insulation.

[0012] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments is preferably equipped with a heating rod as the heater, which is connected to an aviation plug for connecting to an external power source.

[0013] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments is preferably configured such that the temperature and humidity sensor probe is connected to the data acquisition and feedback control system via a thermocouple connector.

[0014] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments is preferably characterized in that the sample stage is fixed to the base by a sample stage support.

[0015] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments is preferably provided in that the top cover is detachably connected to the base via a clamping screw.

[0016] The portable in-situ XRD testing device that can be used in continuous high temperature and high humidity environments is preferably equipped with a docking clamp on the base for docking with XRD.

[0017] The present invention has the following advantages due to the adoption of the above technical solutions: 1. This invention achieves thermal equilibrium under high temperature and high humidity conditions by integrating heating and temperature control of the cavity and gas pipeline. This significantly reduces the humidity gradient and condensation risk caused by temperature difference, effectively solves the problem of humidity maintenance and condensation control under high temperature and high humidity conditions, and achieves a stable and controllable humid and hot environment.

[0018] 2. The device of this invention can ensure that the test chamber maintains a stable humid and thermal environment of above 85°C and 85%RH for a long period of time, and prevents moisture from condensing at the cold walls or windows, thus avoiding interference with X-ray signals and sample condition. Compared with traditional devices that only heat the sample or a single pipeline, this invention achieves end-to-end humid and thermal control, effectively improving the uniformity and long-term stability of the humid and thermal environment, and providing reliable environmental control conditions for structural tracking of materials under complex humid and thermal stress.

[0019] 3. The test chamber of this invention adopts a compact, detachable modular structure with independent temperature and humidity control capabilities. This allows samples to maintain a high-temperature and high-humidity (dual 85%) aging environment in a sealed chamber for extended periods without occupying the XRD host, achieving a combination of off-site aging and intermittent in-situ testing. When a preset time point is reached, the sample chamber can be transferred as a whole to the XRD platform for in-situ structural characterization. After testing, it returns to the aging environment to continue operation, thus realizing a cyclical experimental mode of "aging—analysis—continued aging". This design is the first to effectively connect standard damp heat aging tests (such as IEC / ISOS standards) with in-situ XRD characterization, satisfying long-term environmental stress loading while improving the utilization efficiency of the XRD platform, providing an innovative technical approach for the structural stability study of humidity-sensitive materials.

[0020] 4. This invention overcomes several technical bottlenecks of traditional devices in high-temperature and high-humidity environments through innovative humidity-heat coupling control, condensation suppression, and a transferable cavity design, exhibiting high reliability, high repeatability, and good system compatibility. It significantly expands the application boundaries of in-situ XRD under high-temperature and high-humidity conditions. This device is particularly suitable for studying the structural evolution and degradation mechanisms of humidity-sensitive materials such as perovskite solar cells, flexible electronic devices, energy storage electrode materials, and MOFs under typical accelerated aging conditions, demonstrating significant technological innovation and broad engineering practical value. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the in-situ XRD testing device provided by the present invention when it is turned on. Figure 2 This is a schematic diagram of the in-situ XRD testing device provided by the present invention when it is sealed. Figure 3 This is a front sectional view of the in-situ XRD testing device provided by the present invention; Figure 4 This is a side sectional view of the in-situ XRD testing device provided by the present invention; Figure 5 This is a schematic diagram of the device of the present invention connected to a temperature and humidity control box via an air pipe; Figure 6 This is a cross-sectional view of the trachea structure; Figure 7 This is a temperature and humidity monitoring curve of the internal cavity of the device of the present invention; The attached figures are labeled as follows: 1-Top cover; 2-Base; 3-Sealing ring; 4-Ball valve; 5-Sample stage; 6-Transmission window; 7-Quartz window; 8-Clamping screw; 9-Sample stage support; 10-Heating rod; 11-Aviation plug; 12-Docking clamp; 13-Thermocouple connector; 14-Gas tube; 15-Insulation cotton; 16-Spiral heating belt; 17-Pipe; 18-Temperature and humidity sensor probe; 19-Temperature and humidity control box. Detailed Implementation

[0022] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention are described clearly and completely below. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0023] Unless otherwise defined, the technical or scientific terms used in this invention shall have the ordinary meaning understood by one of ordinary skill in the art to which this invention pertains. The terms "first," "second," "third," "fourth," and similar terms used in this invention do not indicate any order, quantity, or importance, but are merely used to distinguish different components. Terms such as "comprising" or "including" mean that the element or object preceding the word encompasses the elements or objects listed following the word and their equivalents, without excluding other elements or objects. Terms such as "connected" or "linked" are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect.

[0024] 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.

[0025] Current technologies have the following shortcomings: 1. Maintaining a high-humidity atmosphere in a high-temperature environment is technically challenging, and existing in-situ XRD devices have not yet effectively solved this problem: Most current in-situ XRD testing devices focus on high-temperature or specific atmosphere control, and have not yet formed a device structure that can maintain high humidity (≥85% RH) in environments above 85℃. Under high-temperature and high-humidity conditions, the water vapor content in the gas is extremely high. When there is a temperature difference between the gas path and the cavity, water vapor easily condenses on low-temperature components (such as windows, pipe walls, or connecting joints), causing a rapid drop in humidity and disrupting the stability of the testing environment. The formation of condensate not only contaminates the sample and windows but may also damage heating elements or electrical components. Existing technologies such as CN113049618A, although possessing high-temperature control functions, are only designed for high-temperature and high-pressure environments and do not address humidity maintenance and anti-condensation control mechanisms, thus failing to meet the testing requirements under conditions of humidity and heat coupling. 2. The test chamber and gas path system lack an overall thermal management design, making it impossible to achieve uniform and stable control of the humid and hot environment: Under high-temperature and high-humidity test conditions, temperature and humidity are strongly coupled variables. Once a significant temperature difference exists within the system, local temperatures below the dew point will trigger water vapor condensation, causing a decrease in the actual relative humidity in that area and resulting in a humidity gradient in the test environment. If the gas delivery pipeline is not heated, saturated moisture will condense on the inner surface of the pipe wall, leading to incomplete moisture delivery. If the temperature of the test chamber shell or window area is insufficient, condensation zones will form, affecting the consistency of the sample surface environment and the stability of the XRD signal. Existing technologies such as CN116500066A, although equipped with a humidity control module, can only operate at room temperature and lack a coordinated heating design for the chamber and pipeline, making it impossible to maintain a stable humid and hot environment under high-temperature conditions. 3. Existing in-situ XRD systems have fixed structures and are bulky, making them unsuitable for long-term aging and intermittent in-situ tracking under high temperature and humidity conditions: In stability studies, humidity-sensitive materials such as perovskite solar cells and flexible electronic devices often require long-term aging tests (lasting hundreds to thousands of hours) in an "85℃, 85% RH" (double 85) environment. Traditional in-situ XRD devices are mostly fixed structures; directly implementing such tests on an XRD platform would consume instrument resources for extended periods and compromise equipment safety. Furthermore, existing systems generally lack the ability to independently maintain a high temperature and humidity environment and lack sample sealing and transfer designs. Currently, there is no device that can achieve "long-term maintenance of a double 85 environment within an independent chamber and transfer to an XRD platform for in-situ diffraction analysis at different time points." This severely limits the tracking of structural evolution under high temperature and humidity conditions, significantly restricting the application of in-situ XRD technology in the field of damp-heat stability research.

[0026] To address the technical challenges of existing in-situ XRD testing devices, such as difficulty in maintaining humidity under high temperature and humidity conditions, easy condensation, uneven distribution of the humid and hot environment, and inability to simultaneously handle long-term aging tests and intermittent structural tracking, this invention provides a portable in-situ XRD testing device suitable for continuous high temperature and humidity environments. This device can operate stably for extended periods under typical high temperature and humidity conditions (85℃, 85%RH) (dual 85 environment), achieving precise control and reliable maintenance of the humid and hot environment. Through an integrated heating design of the cavity and gas path, the temperature and humidity gradient is effectively eliminated, preventing condensation of moisture in the XRD window, gas delivery channel, and inner wall of the cavity, thereby ensuring the uniformity of the testing environment and the stability and repeatability of the test data.

[0027] like Figure 1 , 3 As shown in Figure 5, the portable in-situ XRD testing device for continuous high temperature and high humidity environments involved in this invention includes: a base 2 and an upper cover 1 detachably and sealed to the base 2, the upper cover 1 and the base 2 forming a sealed cavity, and the upper cover 1 is provided with a transmission window 6 for introducing X-rays; a sample stage 5 for carrying samples, which is set in a groove in the base 2; a heater, which is set in the base 2 and serves as a heat source for the sealed cavity; a temperature and humidity sensor probe 18, which is set in the sealed cavity and connected to a data acquisition and feedback control system; and a temperature and humidity control box 19, which is connected to the base 2 through two gas pipes 14 with heating and heat preservation functions to form a gas circulation loop for inputting a mixed humid gas with a preset temperature and humidity into the sealed cavity.

[0028] Specifically, the test sample is placed on the sample stage 5, the upper cover 1 is closed, and the clamping screw 8 is tightened, so that the upper cover 1 and the base 2 are airtightly sealed through the sealing ring 3, forming a sealed test chamber. The entire device is made of high thermal conductivity aluminum alloy to ensure uniform temperature distribution within the chamber. The heating rod 10 embedded in the base 2 serves as a heat source, which can raise the temperature of the entire chamber to a preset high temperature environment (such as 85°C and above) through precise temperature control, and the heat is quickly conducted to the upper cover 1 and the chamber wall through the high thermal conductivity of the material, thereby eliminating the internal temperature gradient.

[0029] like Figure 6As shown, the gas tube 14 includes a pipe 17, with a spiral heating belt 16 wound around its outer wall. The spiral heating belt 16 is wrapped with insulating cotton, preferably any one of rock wool, glass wool, mineral wool, aluminum silicate, asbestos, and polyester fiber. The insulating cotton prevents condensation of hot and humid gas during transport due to temperature differences. An integrated temperature and humidity sensor probe 18 monitors and provides feedback on environmental parameters within the cavity in real time. The temperature and humidity sensor probe 18 is connected to a data acquisition and feedback control system via a thermocouple connector 13, enabling precise adjustment and long-term stable maintenance of temperature and humidity, thus ensuring the repeatability and reliability of the test sample under high temperature and high humidity conditions.

[0030] like Figure 2 , 5 As shown, the ball valve 4 on the base 2 is connected to the external temperature and humidity control box 19 via the air pipe 14. The temperature and humidity control box 19 outputs a mixture of humid air with preset temperature and humidity, which is then introduced into the cavity through the heated and insulated air pipe 14. The gas circulates through the cavity and then returns to the temperature and humidity control box 19 via the air pipe 14, realizing dynamic closed-loop regulation of humidity and air pressure.

[0031] Furthermore, such as Figure 3 As shown, the heater is a heating rod 10, which is connected to an aviation plug 11 for connecting to an external power source. The sample stage 5 is fixed to the base 2 via a sample stage support 9. The upper cover 1 is detachably connected to the base 2 via clamping screws 8. Preferably, the upper cover 1 and the base 2 are made of a high thermal conductivity metal material, not limited to aluminum alloy, etc. The transmission window 6 is made of an X-ray permeable material, not limited to quartz glass, PI, PC, PEEK, etc.

[0032] Furthermore, such as Figure 4 As shown, a docking clamp 12 is also provided on the base 2 for docking with the XRD. During XRD testing, the device is docked with the X-ray diffractometer (XRD) via the docking clamp 12 on the side of the device. During docking, the temperature and humidity inside the chamber are continuously maintained by the gas pipe 14 and the temperature and humidity control box 19, without changing the gas path or interfering with the temperature and humidity control. X-rays irradiate the sample through the transmission window 6, achieving in-situ diffraction measurement. After the XRD test is completed, the device is removed from the XRD platform and placed in the aging position. The chamber continues to maintain high temperature and high humidity conditions through the temperature and humidity control box 19 to achieve long-term aging. This process can be repeated, achieving a seamless combination of off-site aging and intermittent in-situ XRD measurement.

[0033] The technical solution of the present invention will be described in detail below with reference to specific examples.

[0034] Example 1: Maintaining a long-term, uninterrupted high temperature and high humidity (dual 85%) atmosphere when switching between in-situ and off-site environments. The experimental steps are as follows: Step 1: Place the metal-organic framework material ZIF-8 powder on the sample stage 5, close the top cover 1 and tighten the clamping screw 8 to make the whole device a sealed cavity. Step 2: Heat the heating rod 10 on the base 2 and the spiral heating strip 16 that wraps the air tube 14 to 85°C, so that the main body of the device and the air tube 14 reach 85°C; Step 3: Set the temperature and humidity control chamber 19 to 85℃ and 85%RH, and introduce high-temperature, high-humidity gas into the device cavity through the heated and insulated gas pipe 14. Monitor the temperature and humidity inside the cavity in real time using the temperature and humidity sensor probe 18; Step 4: After 50 minutes, the temperature and humidity inside the chamber reach a dual 85 state (temperature 85℃ and humidity 85%RH) and remain stable; Step 5: Transfer the device and secure it to the X-ray diffractometer (XRD, model: Malvern PANalytical Empyrean) using docking clamp 12; Step 6: Remove the device from the X-ray diffractometer and place it in the aging position; Step 7: Repeat steps 5 and 6 five times; Step 8: Throughout the above experiment, the temperature and humidity sensor probe 18 continuously monitors the temperature and humidity inside the cavity.

[0035] Experimental results: The temperature and humidity monitoring curves of the device show (see...) Figure 7 After the cavity reached a dual 85 state (temperature 85°C, humidity 85%RH), neither temperature nor humidity showed significant fluctuations. During multiple off-site and in-situ transfers (a total of five times), the internal temperature and humidity remained stable without significant fluctuations, and no environmental deviations occurred due to displacement, docking, or gas path disturbances. The entire test cycle lasted 16 hours, with internal temperature fluctuations within the cavity less than ±2°C and humidity fluctuations less than ±4%RH.

[0036] The experimental results fully verify that the device of the present invention has the performance of long-term continuous operation, environmental stability and seamless switching under high temperature and high humidity (dual 85) conditions. The device can realize convenient transfer of samples between ex-situ aging and in-situ XRD testing without shutting down the gas path or breaking the seal, ensuring that the test is conducted in a constant high temperature and high humidity environment, thereby guaranteeing the accuracy and repeatability of in-situ structural analysis data.

[0037] The above experiments demonstrate that the device of the present invention has the following advantages: 1. This invention effectively solves the problem of humidity maintenance and condensation control under high temperature and high humidity conditions, achieving a stable and controllable humid and hot environment. Specifically, the invention employs a collaborative heating design between the test chamber and the gas delivery channel to achieve overall temperature equilibrium within the chamber and the gas path. This maintains a high humidity (≥85%RH) environment for extended periods under high temperature (≥85℃) conditions, effectively preventing condensation of moisture at windows, the inner walls of the chamber, and the inner walls of the gas path. By eliminating temperature and humidity gradients, the uniformity and stability of the humid and hot environment are significantly improved, providing reliable conditions for structural characterization under high temperature and high humidity conditions.

[0038] 2. The cavity of the device of this invention adopts a compact integrated design, which has the functions of quick assembly and disassembly, independent operation and flexible movement, and can be quickly connected with various XRD testing platforms. The sample can maintain a high temperature and high humidity (dual 85) aging environment for a long time in an off-site state without occupying the host resources. At any preset time point, the cavity can be moved into the XRD instrument as a whole for in-situ diffraction testing, realizing the testing mode of off-site aging + intermittent in-situ analysis.

[0039] 3. Samples are kept in a constant humid and hot environment in an independent sealed chamber and periodically transferred to XRD equipment for diffraction analysis, without the need to occupy XRD test positions for extended periods. Structural evolution tracking can be achieved under long-term aging conditions of hundreds to thousands of hours, and it is compatible with standard humid and hot aging test procedures such as IEC / ISOS, ensuring both continuity and comparability of accelerated aging and in-situ structural characterization.

[0040] 4. High airtightness and environmental isolation design: The cavity adopts a multi-layer sealing structure and high-reliability sealing materials, which can effectively isolate external gas and humidity interference, ensure the long-term stability and test repeatability of the sample in high temperature and high humidity environment, support the safe transfer of humidity-sensitive samples, and avoid them being exposed to non-designated environments during the transfer process.

[0041] 5. It is widely applicable to a variety of humidity-sensitive materials, suitable for the study of stability and failure mechanisms of humidity-sensitive systems such as perovskite solar cells, flexible electronic devices, energy storage electrode materials, and MOFs. It can be extended to other material systems that need to carry out structural evolution and interface reaction studies in high temperature and high humidity environments, and has good versatility and engineering compatibility.

[0042] 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 portable in-situ XRD testing device suitable for continuous high temperature and high humidity environments, characterized in that, include: The base (2) and the upper cover (1) detachably and sealingly connected to the base (2) form a sealed cavity with the upper cover (1) and the base (2). The upper cover (1) is provided with a transmission window (6) for introducing rays. The sample stage (5), used to hold the sample, is set in the groove of the base (2); A heater is disposed in the base (2) and is used as a heat source for the sealed cavity; A temperature and humidity sensor probe (18) is installed in the sealed cavity and connected to the data acquisition and feedback control system. The temperature and humidity control box (19) is connected to the base (2) through two air pipes (14) with heating and heat preservation functions to form a gas circulation loop for inputting mixed moisture with preset temperature and humidity into the sealed cavity.

2. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 1, characterized in that, The air tube (14) includes a pipe (17), the outer wall of which is wrapped with a heating strip, and the heating strip is covered with an insulation layer.

3. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 2, characterized in that, The heating belt is a spiral heating belt (16), which is spirally wound around the outer wall of the pipe (17).

4. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 2, characterized in that, The insulation layer is made of insulation cotton.

5. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 4, characterized in that, The insulation cotton includes any one of rock wool insulation cotton, glass wool insulation cotton, mineral wool insulation cotton, aluminum silicate insulation cotton, asbestos and polyester fiber insulation cotton.

6. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 1, characterized in that, The heater is a heating rod (10), which is connected to an aviation plug (11) for connecting to an external power source.

7. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 1, characterized in that, The temperature and humidity sensor probe (18) is connected to the data acquisition and feedback control system via a thermocouple connector (13).

8. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 1, characterized in that, The sample stage (5) is fixed to the base (2) by the sample stage support (9).

9. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 1, characterized in that, The top cover (1) is detachably connected to the base (2) by a clamping screw (8).

10. The portable in-situ XRD testing device for continuous high temperature and high humidity environments according to claim 1, characterized in that, The base (2) is also provided with a docking clamp (12) for docking with the XRD.

Citation Information

Patent Citations

  • High-temperature and high-pressure in-situ XRD testing device

    CN113049618A

  • Humidity-controllable in-situ measurement system and method for X-ray diffractometer and application

    CN116500066A