Sulfide solid electrolyte air stability detection system

Abstract

The invention provides a sulfide solid electrolyte air stability detection system, which comprises a sulfide detection module, an air circulation module, a dew point and temperature control module, a detection bin, an air brake device and a data processing module, the air circulation module, the dew point and temperature control module and the air brake device are respectively connected with the detection bin; the data processing module is arranged at the bottom of the detection bin; the sulfide detection module is arranged on the inner wall of the detection bin. The system can detect the air stability of the sulfide solid electrolyte under air circulation while ensuring that the dew point and the temperature are stable, so that the accuracy and the detection efficiency are improved.

Description

Technical Field

[0001] The present application relates to the technical field of all-solid-state batteries, and in particular to a sulfide solid electrolyte air stability detection system. Background Art

[0002] At present, sulfide solid electrolytes are key components of all-solid-state batteries, and their performance has an important impact on the overall performance of the battery. However, sulfide electrolytes are very prone to hydrolysis in the air environment to generate highly toxic hydrogen sulfide (HS) gas. HS not only causes serious pollution to the environment, but also poses a health threat to workers in laboratories and industrial production lines. It also reduces the ionic conductivity of the material and affects battery performance. Therefore, the air stability detection of sulfide solid electrolytes has become an indispensable part of research and application. Traditional detection methods usually place sulfide solid electrolytes in a vacuum drying container and conduct tests in combination with HS detectors, dew point thermometers and mini fans. However, in practice, it is found that the existing methods cannot ensure the stability of dew point and temperature during the test, and are easily affected by the external environment. At the same time, there is a lack of stability tests under air circulation, which leads to deviations between the test results and the actual environmental conditions, thereby reducing the detection accuracy and efficiency. Summary of the invention

[0003] The purpose of the embodiments of the present application is to provide a sulfide solid electrolyte air stability detection system, which can perform sulfide solid electrolyte air stability detection under air circulation while ensuring the stability of dew point and temperature, thereby improving accuracy and detection efficiency.

[0004] The first aspect of the present application provides a sulfide solid electrolyte air stability detection system, comprising:

[0005] The sulfide solid electrolyte air stability detection system includes a sulfide detection module, an air circulation module, a dew point and temperature control module, a detection chamber, an airlock device and a data processing module, wherein:

[0006] The air circulation module, the dew point and temperature control module and the air brake device are respectively connected to the detection chamber;

[0007] The data processing module is arranged at the bottom of the detection chamber;

[0008] The sulfide detection module is arranged on the inner wall of the detection chamber.

[0009] In the above implementation process, the system can carry out air stability detection of sulfide solid electrolyte under air circulation while ensuring the stability of dew point and temperature, thereby improving accuracy and detection efficiency.

[0010] Furthermore, the sulfide solid electrolyte air stability detection system also includes a heating device; the heating device is arranged at the bottom of the detection chamber.

[0011] Furthermore, the sulfide solid electrolyte air stability detection system also includes a container for containing the detection sample; the container is arranged at the bottom of the detection chamber.

[0012] Furthermore, the container is a tray or a device for measuring weight.

[0013] Furthermore, the sulfide solid electrolyte air stability detection system also includes a ventilation pipe;

[0014] The ventilation pipe is arranged on the top of the detection chamber;

[0015] The air circulation module and the dew point and temperature control module are arranged on the ventilation pipe.

[0016] Furthermore, a desiccant placement area is provided on the ventilation pipe;

[0017] The desiccant is placed at both sides of the facility and the ventilation pipe.

[0018] Further, the sulfide detection module includes a dew point sensor, a temperature sensor and a plurality of sulfide sensors;

[0019] The dew point sensor and the temperature sensor are arranged on the top of the inner wall of the detection chamber;

[0020] The hydrogen sulfide sensors are respectively arranged around the inner wall of the detection chamber.

[0021] Furthermore, the air circulation module is used to start the air internal circulation function when receiving a start instruction, so as to provide stable air flow for the detection chamber.

[0022] Furthermore, the dew point and temperature control module is used to obtain the target dew point and target ambient temperature that need to be set;

[0023] The dew point and temperature control module is further used to control the dew point in the detection chamber according to the target dew point, and to control the ambient temperature in the detection chamber according to the target ambient temperature.

[0024] Further, the data processing module is used to obtain a first data set of changes in the concentration of hydrogen sulfide gas detected by the sulfide detection module over time;

[0025] The data processing module is further used to obtain the target dew point and the target ambient temperature; and to calculate a second data set of changes in the amount of hydrogen sulfide gas released over time based on the first data set;

[0026] The data processing module is further used to generate a two-dimensional point-line graph according to the second data set, and to generate a detection report according to the two-dimensional point-line graph.

[0027] The beneficial effects of the present application are: the system can detect the hydrolysis reaction occurring on the surface of the sulfide electrolyte by setting up multiple detectors, thereby avoiding the influence caused by time error, thereby improving the reliability of the detection result. At the same time, the stable dew point environment can also ensure that the detection is not affected by the external environment, thereby ensuring the reliability of the detection data.

[0028] In addition, the system is highly integrated and does not require additional gas processing or complex calibration operations, which can simplify the experimental operation process and is more suitable for laboratory and industrial applications. At the same time, in the high humidity or low temperature experimental environment of sulfide solid electrolytes and all-solid-state batteries, the system can still provide accurate HS detection, which is conducive to expanding the application range and reliability of the system. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings required for use in the embodiments of the present application will be briefly introduced below. It should be understood that the following drawings only show certain embodiments of the present application and therefore should not be regarded as limiting the scope. For ordinary technicians in this field, other related drawings can be obtained based on these drawings without paying creative work.

[0030] Figure 1 A schematic diagram of the structure of a sulfide solid electrolyte air stability detection system provided in an embodiment of the present application;

[0031] Figure 2 A schematic diagram of the structure of another sulfide solid electrolyte air stability detection system provided in an embodiment of the present application. DETAILED DESCRIPTION

[0032] The technical solutions in the embodiments of the present application will be described below in conjunction with the drawings in the embodiments of the present application.

[0033] It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in subsequent drawings. At the same time, in the description of this application, the terms "first", "second", etc. are only used to distinguish the description and cannot be understood as indicating or implying relative importance.

[0034] Example 1

[0035] Please see Figure 1 , Figure 1The schematic diagram of the structure of a sulfide solid electrolyte air stability detection system provided in this embodiment. The sulfide solid electrolyte air stability detection system includes a sulfide detection module, an air circulation module, a dew point and temperature control module, a detection chamber, an airlock device and a data processing module, wherein:

[0036] The air circulation module, the dew point and temperature control module and the air brake device are respectively connected to the detection chamber;

[0037] The data processing module is arranged at the bottom of the detection chamber;

[0038] The sulfide detection module is arranged on the inner wall of the detection chamber.

[0039] It can be seen that the sulfide solid electrolyte air stability detection system described in this embodiment can perform air stability detection of sulfide solid electrolyte under air circulation while ensuring the stability of dew point and temperature, thereby improving accuracy and detection efficiency.

[0040] Example 2

[0041] Please see Figure 2 , Figure 2 This is a schematic diagram of the structure of a sulfide solid electrolyte air stability detection system provided in this embodiment. Figure 2 As shown, the sulfide solid electrolyte air stability detection system includes a sulfide detection module, an air circulation module, a dew point and temperature control module, a detection chamber, an airlock device and a data processing module, wherein:

[0042] The air circulation module, the dew point and temperature control module and the air brake device are respectively connected to the detection chamber;

[0043] The data processing module is arranged at the bottom of the detection chamber;

[0044] The sulfide detection module is arranged on the inner wall of the detection chamber.

[0045] In this embodiment, the sulfide detection module is an H2S detection module, which is responsible for detecting the concentration of hydrogen sulfide (HS) released by the sulfide electrolyte under different dew point conditions.

[0046] In this embodiment, since the materials are very likely to react with the surrounding environment during the process of placing the materials into the device, in order to ensure the safety of the test process, the integrity of the materials and the reliability of the test, the materials will enter the device through an airlock system.

[0047] As an optional implementation, the sulfide solid electrolyte air stability detection system further includes a heating device; the heating device is disposed at the bottom of the detection chamber.

[0048] As an optional implementation, the sulfide solid electrolyte air stability detection system further includes a container for containing the detection sample; the container is arranged at the bottom of the detection chamber.

[0049] As an optional implementation, the container is a tray or a device for measuring weight.

[0050] As an optional implementation, the sulfide solid electrolyte air stability detection system further includes a ventilation pipe;

[0051] The ventilation pipe is arranged on the top of the detection chamber;

[0052] The air circulation module and the dew point and temperature control module are arranged on the ventilation pipe.

[0053] As an optional implementation, a desiccant placement area is provided on the ventilation pipe;

[0054] The desiccant is placed at both sides of the facility and the ventilation pipe.

[0055] In this embodiment, the desiccant placement is used for manually adding desiccant, and its position is located at both sides of the ventilation pipe. When performing internal circulation, the desiccant valve can be manually opened to allow all the internal circulation air to pass through the drying device.

[0056] As an optional implementation, the sulfide detection module includes a dew point sensor, a temperature sensor and a plurality of sulfide sensors;

[0057] The dew point sensor and the temperature sensor are arranged on the top of the inner wall of the detection chamber;

[0058] The hydrogen sulfide sensors are respectively arranged around the inner wall of the detection chamber.

[0059] In this embodiment, the sulfide detection module is equipped with a plurality of high-sensitivity HS sensors for detecting the environmental concentration of H2S.

[0060] As an optional implementation, the air circulation module is used to start the air internal circulation function when receiving a start instruction, so as to provide stable air flow for the detection chamber.

[0061] In this embodiment, the air circulation module can be used to provide a stable air flow, thereby ensuring that the gas in the sample environment is evenly distributed. At the same time, the air circulation module also has atmosphere circulation and exhaust functions, which can achieve rapid replacement of the atmosphere of each set of experiments and test environments.

[0062] In this embodiment, the air circulation module can be set with a specific wind speed value, so as to conduct an air stability experiment of the sulfide solid electrolyte at different wind speeds.

[0063] As an optional implementation, the dew point and temperature control module is used to obtain the target dew point and target ambient temperature that need to be set;

[0064] The dew point and temperature control module is further used to control the dew point in the detection chamber according to the target dew point, and to control the ambient temperature in the detection chamber according to the target ambient temperature.

[0065] In this embodiment, the dew point and temperature control module can precisely control the dew point and temperature in the sample environment to maintain them within a preset range.

[0066] In this embodiment, the dew point and temperature control module can control the dew point through the temperature control system and the desiccant, thereby avoiding the influence of humidity changes on the HS detection results. At the same time, the dew point and temperature control module is equipped with a manual drying box (for placing desiccant), so as to assist in controlling the dew point and temperature of the environment. Among them, the drying box should be located on both sides of the inner circulation air duct, and its opening and closing can be manually controlled. When it is opened, the air is dried, and vice versa.

[0067] As an optional implementation, the data processing module is used to obtain a first data set of changes in the concentration of hydrogen sulfide gas detected by the sulfide detection module over time;

[0068] The data processing module is further used to obtain the target dew point and the target ambient temperature; and to calculate a second data set of changes in the amount of hydrogen sulfide gas released over time based on the first data set;

[0069] The data processing module is further used to generate a two-dimensional point-line graph according to the second data set, and to generate a detection report according to the two-dimensional point-line graph.

[0070] In this embodiment, the data processing module can collect and analyze the data transmitted by each module in real time, process it through an intelligent algorithm, and then output the HS release amount of the sulfide electrolyte under different dew point conditions.

[0071] In this embodiment, the input data of the data processing module may be a dataframe, which aggregates data of multiple sensors and detection devices. Specific examples are as follows:

[0072] Time(s) Dew point(℃) Temperature(℃) <![CDATA[H2S(ppm)]]> Sample mass (g) 0 -40 25 3 0.2 1 -40 25 3.5 0.2 2 -40 25 4 0.2 … -40 25 … 0.2 20 -40 25 30 0.2 21 -40 25 31 0.2 22 -40 25 33 0.2

[0073] The Dataframe data format is for reference only. In the actual experiment, the dew point and temperature fluctuate up and down (±5 is normal).

[0074] In this embodiment, the output data of the data processing module are time, temperature and H2S (which can be displayed on the data display). Assume that the test equipment capacity is 1m 3 After the test is completed, the data output is the amount of H2S per minute (ppm / min).

[0075] For example, the application method of the sulfide solid electrolyte air stability detection system may include the following steps:

[0076] (1) The atmosphere of the device is stable: turn on the air circulation, set the device to the required temperature and dew point and let it stand for about 20 minutes.

[0077] (2) Start the detection module: Under the set dew point and temperature conditions, start the HS detection module. The sensor will measure the HS concentration released by the sample in real time, and the data will be transmitted to the data processing module for analysis.

[0078] For example, assume the temperature is 25°C and the dew point is -40°C, which is a constant value. Generally, a value greater than 10ppm is considered dangerous. The corresponding relationship between time (min) and hydrogen sulfide is:

[0079] Time - Hydrogen sulfide (ppm, dew point -28°C): 1-2.3; 2-5.9; 3-9; 4-12.1; 5-15.1; 6-18.2; 7-21.4; 8-24.6; 9-27.8; 10-31.2; 11-34.6; 12-38.2; 13-42; 14-45.6; 15-49.4; 16-53; 17-57; 18-61; 19-65.

[0080] (3) Sample placement: Place the sulfide electrolyte sample to be tested in the sample compartment of the HS detection module.

[0081] (4) Result recording and storage: After the test is completed, the data processing module records and stores all experimental data.

[0082] In this embodiment, the method can draw a two-dimensional point-line graph based on the recorded H2S (ppm) data processing module, with the horizontal axis being time (with a step length of 1 minute) and the vertical axis being ppm. At the same time, the second vertical axis plots the dew point change per minute.

[0083] In this embodiment, the following table shows the reference data that can be obtained by this method.

[0084]

[0085] Wherein, the formula V=(C×L×10 -6) / m can be used to convert ppm to cm 3 / g;

[0086] C is ppm, L is the volume of the equipment (cm 3 The test part), m is the sample mass (g).

[0087] It can be seen that the sulfide solid electrolyte air stability detection system described in this embodiment can perform air stability detection of sulfide solid electrolyte under air circulation while ensuring the stability of dew point and temperature, thereby improving accuracy and detection efficiency.

[0088] In several embodiments provided in the present application, it should be understood that the disclosed system can also be implemented in other ways. The device embodiments described above are merely schematic, for example, the flowcharts and block diagrams in the accompanying drawings show the possible architecture, functions and operations of the system according to the multiple embodiments of the present application. In this regard, each box in the flowchart or block diagram can represent a module, a program segment or a part of a code, and the module, a program segment or a part of a code contains one or more executable instructions for implementing the specified logical function. It should also be noted that in some alternative implementations, the functions marked in the box can also occur in a different order from the order marked in the accompanying drawings. For example, two consecutive boxes can actually be executed substantially in parallel, and they can sometimes be executed in the opposite order, depending on the functions involved. It should also be noted that each box in the block diagram and / or the flowchart, and the combination of boxes in the block diagram and / or the flowchart can be implemented with a dedicated hardware-based system that performs a specified function or action, or can be implemented with a combination of dedicated hardware and computer instructions.

[0089] In addition, the functional modules in the various embodiments of the present application may be integrated together to form an independent part, or each module may exist separately, or two or more modules may be integrated to form an independent part.

[0090] If the functions are implemented in the form of software function modules and sold or used as independent products, they can be stored in a computer-readable storage medium. Based on this understanding, the technical solution of the present application can be essentially or partly embodied in the form of a software product that contributes to the prior art. The computer software product is stored in a storage medium, including several instructions to enable a computer device (which can be a personal computer, a server, or a network device, etc.) to perform all or part of the steps of the methods described in each embodiment of the present application. The aforementioned storage medium includes: various media that can store program codes, such as a USB flash drive, a mobile hard disk, a read-only memory (ROM), a random access memory (RAM), a magnetic disk or an optical disk.

[0091] The above description is only an embodiment of the present application and is not intended to limit the scope of protection of the present application. For those skilled in the art, the present application may have various changes and variations. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application should be included in the scope of protection of the present application. It should be noted that similar reference numerals and letters represent similar items in the following drawings, so once an item is defined in one drawing, it does not need to be further defined and explained in the subsequent drawings.

[0092] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed in the present application, which should be included in the protection scope of the present application. Therefore, the protection scope of the present application should be based on the protection scope of the claims.

[0093] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "comprise a ..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

Claims

1. A sulfide solid electrolyte air stability detection system, characterized in that: The sulfide solid electrolyte air stability detection system includes a sulfide detection module, an air circulation module, a dew point and temperature control module, a detection chamber, an airlock device and a data processing module, wherein: The air circulation module, the dew point and temperature control module and the air brake device are respectively connected to the detection chamber; The data processing module is arranged at the bottom of the detection chamber; The sulfide detection module is arranged on the inner wall of the detection chamber.

2. The sulfide solid electrolyte air stability detection system according to claim 1, characterized in that: The sulfide solid electrolyte air stability detection system also includes a heating device; the heating device is arranged at the bottom of the detection chamber.

3. The sulfide solid electrolyte air stability detection system according to claim 1, characterized in that: The sulfide solid electrolyte air stability detection system also includes a container for containing detection samples; the container is arranged at the bottom of the detection chamber.

4. The sulfide solid electrolyte air stability detection system according to claim 3, characterized in that: The container is a tray or a device for measuring weight.

5. The sulfide solid electrolyte air stability detection system according to claim 1, characterized in that: The sulfide solid electrolyte air stability detection system also includes a ventilation pipe; The ventilation pipe is arranged on the top of the detection chamber; The air circulation module and the dew point and temperature control module are arranged on the ventilation pipe.

6. The sulfide solid electrolyte air stability detection system according to claim 5, characterized in that: The ventilation pipe is provided with a place for placing a desiccant; The desiccant is placed at both sides of the facility and the ventilation pipe.

7. The sulfide solid electrolyte air stability detection system according to claim 1, characterized in that: The sulfide detection module includes a dew point sensor, a temperature sensor and a plurality of sulfide sensors; The dew point sensor and the temperature sensor are arranged on the top of the inner wall of the detection chamber; The hydrogen sulfide sensors are respectively arranged around the inner wall of the detection chamber.

8. The sulfide solid electrolyte air stability detection system according to claim 1, characterized in that: The air circulation module is used to start the air internal circulation function when receiving a start instruction to provide stable air flow for the detection chamber.

9. The sulfide solid electrolyte air stability detection system according to claim 1, characterized in that: The dew point and temperature control module is used to obtain the target dew point and target ambient temperature that need to be set; The dew point and temperature control module is further used to control the dew point in the detection chamber according to the target dew point, and to control the ambient temperature in the detection chamber according to the target ambient temperature.

10. The sulfide solid electrolyte air stability detection system according to claim 9, characterized in that: The data processing module is used to obtain a first data set of changes in the concentration of hydrogen sulfide gas detected by the sulfide detection module over time; The data processing module is further used to obtain the target dew point and the target ambient temperature; and to calculate a second data set of changes in the amount of hydrogen sulfide gas released over time based on the first data set; The data processing module is further used to generate a two-dimensional point-line graph according to the second data set, and to generate a detection report according to the two-dimensional point-line graph.

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