In-situ neutron electrochemical test integrated device

Abstract

The invention relates to the technical field of in-situ neutron electrochemical testing, in particular to an in-situ neutron electrochemical testing device. The device comprises a sample cavity connecting flange, a transition cavity flange, a transition cavity, a neutron beam window, a linear manual lifting module, a handheld sample rod and the like, the vacuum of the sample cavity is maintained through the unique transition cavity design, and the air scattering influence is reduced; the hand-held sample rod realizes rapid and safe disassembly and assembly of the sample; the linear manual lifting module ensures that the position of the sample is accurate; the hollow design enables wiring to be neat; in addition, the device also has the functions of temperature control, pressure monitoring and data acquisition and processing. The problems that an existing testing device is large in air scattering influence, unsafe in sample disassembly and assembly, inaccurate in testing result and the like are solved, and a more efficient, accurate and safe testing means is provided for material science research, especially commercial battery failure mechanism research.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of in-situ neutron electrochemical testing, and particularly relates to an in-situ neutron electrochemical testing device. BACKGROUND

[0002] In the field of material science and electrochemistry research, in-situ neutron electrochemical testing technology is irreplaceable; it can monitor the structural evolution of materials in real time under working conditions, providing key information for a deep understanding of the performance change mechanism of materials, especially in the research of commercial battery failure mechanism, which can help researchers develop more efficient and safe battery systems.

[0003] Neutrons have unique physical properties, their high penetration allows them to penetrate deep into the battery, accurately capturing changes inside the battery; they are sensitive to light elements such as lithium (Li) and oxygen (O), allowing accurate monitoring of lithium insertion and extraction processes; they can also effectively distinguish between adjacent transition metals such as nickel (Ni), cobalt (Co), and manganese (Mn), helping to analyze the distribution and changes of elements in battery materials, and thus deeply exploring the charging and discharging mechanism and failure reasons of the battery.

[0004] The in-situ neutron electrochemical testing system mainly consists of an electrochemical testing device and a sample clamping and position adjustment device; the electrochemical testing device is responsible for monitoring the electrochemical performance parameters of the battery such as voltage, current, and capacity; the sample clamping and position adjustment device is responsible for fixing the sample and ensuring its accurate position in the neutron beam to obtain accurate test data.

[0005] However, the existing in-situ neutron electrochemical testing technology has obvious deficiencies; the test is usually carried out in an atmospheric environment, i.e. the sample and the detector are in a non-vacuum state; in this environment, neutrons will interact with air and scatter, forming additional background signals; although this signal does not change the sample structure information, it seriously interferes with the detection and analysis of the true structure signal of the sample, greatly affecting the data quality; especially when analyzing the dynamic evolution of lithium ion battery defects, lithium ion migration and other subtle structural changes, the air scattering signal may mask the key information, leading to deviations in the judgment of the battery failure mechanism.

[0006] The existing testing device lacks effective means to reduce air scattering, making it difficult to meet the demand for high-precision and high-accuracy test data; moreover, during the sample disassembly process, direct contact between the experimenter and the sample may pose a safety risk, and the long waiting time for sample replacement reduces the utilization efficiency of the neutron testing machine; in addition, there may be problems such as line clutter, inaccurate sample position, unstable temperature control, and missing pressure monitoring during the testing process, further affecting the reliability and accuracy of the test results.

[0007] Therefore, it is urgent to develop an in-situ neutron electrochemical testing integrated device which can effectively reduce the air scattering background, realize the rapid and safe disassembly of the sample, ensure the accurate position of the sample, have the temperature and pressure regulation and monitoring functions, and can ensure the clean test environment and reduce the stray signal sources. SUMMARY

[0008] In order to solve the above problems, the present application aims to provide an in-situ neutron electrochemical testing integrated device, which is mainly used for real-time and accurate structure evolution monitoring of materials under working conditions, especially suitable for commercial battery failure mechanism research and other related fields which have very high requirements for test data precision and accuracy, and can provide high-quality test data support for material science research by effectively reducing the influence of air scattering background.

[0009] The technical scheme adopted by the present application is: an in-situ neutron electrochemical testing integrated device, comprising: a sample cavity connecting assembly, including a sample cavity connecting flange, used for sealed connection with a neutron spectrometer sample cavity to maintain the vacuum environment of the sample cavity; a transition cavity assembly, composed of a transition cavity flange, a transition cavity barrel and a neutron beam window; the transition cavity flange is installed on the sample cavity connecting flange, the transition cavity barrel is connected below the transition cavity flange, and the neutron beam window is arranged at the lower part of the transition cavity barrel; the transition cavity barrel adopts a multi-stage design, the upper end is made of stainless steel, and the lower end of the neutron beam window is made of a special material allowing the smooth passage of neutrons; a sample position adjusting assembly, including a linear manual lifting module and a handheld sample rod; the linear manual lifting module is fixed on the transition cavity flange and connected with the handheld sample rod through a positioning block to realize the up-down movement of the handheld sample rod; the handheld sample rod is connected with the linear manual lifting module, and the sample is fixed at the lower end of the handheld sample rod; the lower end of the handheld sample rod is designed as a clamping hook, the clamping of the clamping hook is triggered by the circular ring at the upper end of the handheld sample rod, and the rapid non-contact disassembly of the sample is realized; the handheld sample rod is designed as a hollow structure, and a wire slot is arranged inside to meet the wiring requirements of the electrochemical testing device.

[0010] The transition cavity flange, the transition cavity barrel and the neutron beam window form a complete cavity, which is connected with the sample cavity through the sample cavity connecting flange to maintain the vacuum state of the sample cavity and reduce the influence of air scattering on data quality.

[0011] Further comprising a temperature control assembly, the temperature control assembly includes a temperature sensor and a heating / cooling element; the temperature sensor is arranged in the transition cavity barrel to monitor the temperature of the environment where the sample is located in real time; the heating / cooling element is installed outside the transition cavity barrel, and adjusts the temperature in the transition cavity barrel according to the feedback signal of the temperature sensor to meet the test temperature requirements of different samples.

[0012] The sealing connection mode between the sample cavity connecting flange and the sample cavity of the neutron spectrometer is sealing by a sealing ring, the material of the sealing ring is selected according to the actual working environment and sealing requirements, and the sealing property of the connection is ensured.

[0013] The wall thickness of the transition cavity cylinder is designed according to the actual working pressure and strength requirements, and when the working pressure is 0.1-0.5 MPa, the wall thickness is designed to be 2-5 mm; the inner diameter of the transition cavity cylinder is designed according to the size of the sample and the testing requirements, and the inner diameter ranges between 50-200 mm.

[0014] The special material of the neutron beam window is vanadium foil or aluminum foil; when vanadium foil material is used, the thickness is between 0.2-5 mm; when aluminum foil is used, the thickness is between 0.1-0.5 mm; the neutron beam window and the transition cavity cylinder are connected by welding or flange connection to ensure the sealing property and stability of the connection.

[0015] The adjustment principle of the linear manual lifting module adopts the cooperation mode of a lead screw and two slide rails; the lead screw adopts a trapezoidal lead screw or a ball screw, and the two slide rails are respectively installed on the two sides of the lead screw and arranged in parallel with the lead screw; the lifting range of the linear manual lifting module is between 10-50 cm, and the accuracy reaches the level of 0.1 mm.

[0016] In the temperature control assembly, the measurement accuracy of the temperature sensor is ±0.1℃; the heating power or cooling capacity of the heating / cooling element is designed according to the volume of the transition cavity cylinder and the temperature adjustment range, and the temperature adjustment range is-60℃ to 100℃.

[0017] The device also includes a pressure monitoring assembly, which contains a pressure sensor installed in the transition cavity cylinder for real-time monitoring of the pressure in the transition cavity cylinder; the measurement accuracy of the pressure sensor is ±0.01 MPa, to ensure that pressure abnormalities can be detected in time during testing.

[0018] The design of the hook of the handheld sample rod adopts a spring return mechanism, which ensures that the hook remains in the engaged state without external force when the upper end of the handheld sample rod is triggered to engage the hook; when the sample needs to be disassembled, the ring is triggered again, and the spring return mechanism releases the hook.

[0019] The device adopts an upper loading mode, which reduces the source of stray signals in the entire test environment; the reduction of stray signals helps to ensure the authenticity of the data, so that the test results can more accurately reflect the actual situation of the sample.

[0020] The device also comprises a data acquisition and processing component connected with the electrochemical testing device, for collecting electrochemical testing data and processing and analyzing the collected data in real time; the data acquisition and processing component has a data storage function and can store the processed data for subsequent review and analysis.

[0021] The in-situ neutron electrochemical testing integrated device has the following advantages:

[0022] The unique transition cavity design effectively isolates the sample from the vacuum sample cavity of the neutron spectrometer, maintains the vacuum state of the sample cavity, greatly reduces the non-vacuum environment distance between the sample and the detector, significantly reduces the influence of air scattering on data quality, and provides a strong guarantee for accurately analyzing material structure evolution, such as the dynamic evolution of anti-site defects in lithium-ion batteries and lithium-ion migration; the lower end of the portable sample rod adopts a hook design, and the upper end ring can trigger the clamping and release of the hook to realize the quick and non-contact disassembly of the sample; this design avoids direct contact between the experimenter and the sample, reduces the safety risk in the experiment process, ensures the personal safety of the experimenter, reduces the sample changing waiting time, and improves the utilization efficiency of the neutron testing machine; the linear manual lifting module is fixed on the flange of the transition cavity and connected with the portable sample rod through a positioning block, which can accurately control the up-down movement of the portable sample rod, thereby ensuring the accuracy of the test sample position and improving the reliability and repeatability of the test results; the portable sample rod is designed as a hollow structure with a wire slot inside, which can easily meet the wiring requirements of the electrochemical testing device, avoid messy wiring, ensure the cleanliness of the test environment, and reduce the influence of line interference on the test results.

[0023] In the present application, the temperature sensor in the temperature control component monitors the temperature of the environment where the sample is located in real time, and the heating / cooling element adjusts the temperature according to the feedback signal, meeting the testing requirements of different samples under different temperature conditions and expanding the application range of the device.

[0024] The pressure sensor of the pressure monitoring component can monitor the pressure in the transition cavity cylinder in real time, detect abnormal pressure conditions in time, ensure that the testing process is carried out in a stable pressure environment, and further improve the accuracy of the test data; the device adopts an upper loading method, which not only improves the efficiency of sample disassembly and assembly, but also reduces the sources of stray signals in the entire test environment, making the test results more accurately reflect the actual situation of the sample; the data acquisition and processing component can collect, process and analyze electrochemical testing data in real time, and has a data storage function, which is convenient for subsequent review and analysis and improves the efficiency of scientific research. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 is a schematic diagram of the overall structure of the present application;

[0026] Figure 2 is a cutaway perspective schematic diagram of the overall structure of the present application;

[0027] Figure 3 is a schematic diagram of the internal structure of the cavity of the present application.

[0028] BRIEF DESCRIPTION OF DRAWINGS 1 - sample cavity connecting flange, 2 - transition cavity flange, 3 - transition cavity, 4 - neutron beam window, 5 - linear manual lifting module, 6 - handheld sample rod. DETAILED DESCRIPTION

[0029] The specific embodiments of the in-situ neutron electrochemical test integrated device of the present application are described in detail below in conjunction with the accompanying drawings; as shown in Figures 1-2 the device is mainly composed of a sample cavity connecting assembly, a transition cavity assembly, a sample position adjusting assembly, a temperature control assembly, a pressure monitoring assembly, and a data acquisition and processing assembly.

[0030] EMBODIMENT

[0031] The specific structure of the in-situ neutron electrochemical test integrated device of the present embodiment is as follows:

[0032] Sample cavity connecting assembly: includes a sample cavity connecting flange 1, which is mainly used for sealed connection with the sample cavity of the neutron spectrometer; in the present embodiment, a sealing ring is used for sealing, and the sealing ring is made of rubber material that is resistant to high temperature and corrosion, to ensure the sealing of the connection under different working environments and maintain the vacuum environment of the sample cavity.

[0033] Transition cavity assembly: composed of transition cavity flange 2, transition cavity 3 and neutron beam window 4; the transition cavity flange 2 is installed on the sample cavity connecting flange 1, serving as a connection and sealing transition; the transition cavity 3 is designed in multiple stages, with the upper end made of stainless steel, the wall thickness designed to be 3mm according to the actual working pressure and strength requirements, and the inner diameter designed to be 100mm according to the sample size and testing requirements; the lower end neutron beam window 4 is made of vanadium foil with a thickness of 0.3mm, connected with the transition cavity 3 by welding to ensure the sealing and stability of the connection; the setting of the neutron beam window 4 serves the functions of maintaining the vacuum of the scattering cavity and ensuring the smooth passage of neutrons to interact with the sample.

[0034] Sample position adjustment assembly: includes a linear manual lifting module 5 and a handheld sample rod 6; the linear manual lifting module 5 is fixed on the transition cavity flange 2, and the adjustment principle adopts the cooperation mode of a lead screw and two slide rails, the lead screw is a ball screw, the lifting range is set to 20 cm, and the accuracy reaches the level of 0.1 mm; the linear manual lifting module 5 is connected with the handheld sample rod 6 through a positioning block, so as to realize the up-down movement of the handheld sample rod 6; the lower end of the handheld sample rod 6 is designed as a clamping hook, a spring return mechanism is adopted, the clamping and release of the clamping hook are triggered through the upper end ring of the handheld sample rod 6, and the rapid non-contact disassembly of the sample is realized; the handheld sample rod 6 is designed as a hollow structure, a wire slot is arranged in the hollow structure, and the wiring requirement of the electrochemical testing device is facilitated.

[0035] Temperature control assembly: includes a temperature sensor and a heating / cooling element; the temperature sensor is arranged in the transition cavity 3, has a measurement accuracy of ±0.1℃, and is used for monitoring the temperature of the environment in which the sample is located in real time; the heating / cooling element is installed outside the transition cavity 3, adjusts the temperature in the transition cavity 3 according to the feedback signal of the temperature sensor, and has a temperature adjustment range of -40℃ to 80℃, so as to meet the testing temperature requirements of different samples.

[0036] Pressure monitoring assembly: includes a pressure sensor installed in the transition cavity 3, has a measurement accuracy of ±0.01 MPa, and is used for monitoring the pressure in the transition cavity 3 in real time and discovering abnormal pressure conditions in time.

[0037] Data acquisition and processing assembly: connected with the electrochemical testing device, used for acquiring electrochemical testing data, processing and analyzing the acquired data in real time, and having a data storage function, so as to facilitate subsequent review and analysis.

[0038] Working process: when in-situ neutron electrochemical testing is performed, first, the sample is fixed at the lower end of the handheld sample rod 6, and the clamping hook design is used to ensure that the sample is firmly fixed; then, the height of the handheld sample rod 6 is adjusted through the linear manual lifting module 5, so that the sample is in a suitable position, and it is ensured that the neutrons can accurately irradiate the sample.

[0039] In the embodiment, the sample cavity connecting flange 1 is sealingly connected with the neutron spectrometer sample cavity, the transition cavity flange 2, the transition cavity 3 and the neutron beam window 4 form a complete cavity, the sample cavity is connected with the sample cavity through the sample cavity connecting flange 1, and the vacuum state of the sample cavity is maintained; at this time, the sample is placed in the cavity, the neutrons enter the cavity through the neutron beam window 4 and interact with the sample, and the generated signals are received by the detector.

[0040] The temperature sensor in the embodiment monitors the temperature of the environment where the sample is located in real time, and feeds back a signal to the heating / cooling element to adjust the temperature; the pressure sensor monitors the pressure in the transition cavity 3 in real time, to ensure that the test process is carried out in a stable pressure environment; the data acquisition and processing assembly acquires electrochemical test data in real time, and processes and analyzes the data, and stores the processed data; when the test is completed, the sample is quickly and non-contactingly disassembled by triggering the release of the hook through the circular ring at the upper end of the handheld sample rod 6.

[0041] The above embodiment effectively solves the problems in the prior art through the synergistic effect of each component, and provides a more reliable test means for material science research.

[0042] The above embodiment is only a preferred embodiment of the present application, and does not limit the present application in any form; any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. An in-situ neutron electrochemical test integrated device, characterized in that: The application relates to a neutron spectrum sample chamber, which comprises the following components: a sample chamber connecting assembly, which comprises a sample chamber connecting flange, is used for sealed connection with a neutron spectrum sample chamber to maintain the vacuum environment of the sample chamber; a transition chamber assembly, which is composed of a transition chamber flange, a transition chamber barrel and a neutron beam window; the transition chamber flange is installed on the sample chamber connecting flange, the transition chamber barrel is connected below the transition chamber flange, and the neutron beam window is arranged at the lower part of the transition chamber barrel; the transition chamber barrel adopts a multi-stage design, the upper end is made of stainless steel, and the neutron beam window at the lower end is made of special material which allows the smooth passing of neutrons; the special material is selected according to the neutron penetration and sample test requirements; a sample position adjusting assembly, which comprises a linear manual lifting module and a handheld sample rod; the linear manual lifting module is fixed on the transition chamber flange and is connected with the handheld sample rod through a positioning block to realize the up-down movement of the handheld sample rod; the handheld sample rod is connected with the linear manual lifting module, and a sample is fixed at the lower end of the handheld sample rod; the lower end of the handheld sample rod is designed as a clamping hook, the clamping hook is triggered to be clamped by a circular ring at the upper end of the handheld sample rod, and the sample is quickly and non-contactly disassembled; the handheld sample rod is designed as a hollow structure, and a wire slot is arranged in the hollow structure to meet the wiring requirement of an electrochemical test device; the transition chamber flange, the transition chamber barrel and the neutron beam window form a complete cavity, the sample chamber connecting flange is connected with the sample chamber to maintain the vacuum state of the sample chamber and reduce the influence of air scattering on data quality; a temperature control assembly is further arranged, the temperature control assembly comprises a temperature sensor and a heating / cooling element; the temperature sensor is arranged in the transition chamber barrel and is used for monitoring the temperature of the environment where the sample is located in real time; the heating / cooling element is installed outside the transition chamber barrel and adjusts the temperature in the transition chamber barrel according to the feedback signal of the temperature sensor to meet the test temperature requirement of different samples. The sealed connection mode of the sample chamber connecting flange and the neutron spectrum sample chamber is to seal by using a sealing ring, the material of the sealing ring is selected according to the actual working environment and sealing requirement to ensure the sealing property of the connection position. The wall thickness of the transition chamber barrel is designed according to the actual working pressure and strength requirement, when the working pressure is 0.1-0.5 MPa, the wall thickness is designed as 0.2-5 mm; the inner diameter of the transition chamber barrel is designed according to the size of the sample and the test requirement, and the inner diameter ranges between 50 mm and 200 mm. The special material of the neutron beam window is vanadium foil or aluminum foil; when the vanadium foil material is used, the thickness is between 0.2 mm and 5 mm; when the aluminum foil is used, the thickness is between 0.1 mm and 0.5 mm; the connection between the neutron beam window and the transition chamber barrel is achieved by welding or flange connection to ensure the sealing property and stability of the connection position. The adjustment principle of the linear manual lifting module adopts the cooperation mode of a screw rod and two slide rails; the screw rod adopts a trapezoidal screw rod or a ball screw rod, and the two slide rails are arranged on the two sides of the screw rod and are arranged in parallel with the screw rod; the lifting range of the linear manual lifting module is between 10 cm and 50 cm, and the accuracy reaches the level of 0.1 mm. ​ 2. The in-situ neutron electrochemical test integrated device according to claim 1, characterized in that: ​ 3. The in-situ neutron electrochemical test integrated device of claim 1, wherein: ​ 4. The in-situ neutron electrochemical test integrated device of claim 1, wherein: ​ 5. The in-situ neutron electrochemical test integrated device of claim 1, wherein: ​ 6. The in-situ neutron electrochemical test integrated device of claim 1, wherein: The temperature control assembly, the measurement accuracy of the temperature sensor is ± 0.1 DEG C; the heating power or cooling capacity of the heating / cooling element is designed according to the volume of the transition cavity cylinder and the temperature adjustment range, and the temperature adjustment range is-60 DEG C to 100 DEG C.

7. The in-situ neutron electrochemical test integration device of claim 1, wherein: Further comprising a pressure monitoring assembly, the pressure monitoring assembly comprises a pressure sensor installed in the transition cavity cylinder for real-time monitoring of the pressure in the transition cavity cylinder; the measurement accuracy of the pressure sensor is ± 0.01 MPa, so as to ensure that the abnormal pressure condition can be found in time during the test.

8. The in-situ neutron electrochemical test integrated device of claim 1, wherein: The hook of the hand-held sample rod is designed with a spring return mechanism, when the upper end ring of the hand-held sample rod triggers the hook to bite, the spring return mechanism ensures that the hook remains in the biting state without external force; when the sample needs to be disassembled, the ring is triggered again, and the spring return mechanism releases the hook.

9. The in-situ neutron electrochemical test integration device of claim 1, wherein: The device adopts an upper loading mode, reduces the stray signal source in the whole test environment; the reduction of stray signals helps to ensure the authenticity of the data, so that the test results can more accurately reflect the actual situation of the sample.

10. The in-situ neutron electrochemical test integrated device according to any one of claims 1-9, characterized in that: The device further comprises a data acquisition and processing assembly connected with the electrochemical test device, for acquiring electrochemical test data and processing and analyzing the acquired data in real time; the data acquisition and processing assembly has a data storage function, and can store the processed data for subsequent review and analysis.

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