Device and method for testing release rate of hydrogen sulfide

Abstract

The invention provides a hydrogen sulfide release rate testing device and testing method, and relates to the technical field of batteries. The hydrogen sulfide release rate testing device comprises a frame mechanism, a bottom plate mechanism, a movable door assembly and a testing mechanism, the movable door assembly comprises at least one movable door, the frame mechanism and the movable door are installed in a sealed mode, and the position of the movable door corresponds to a small environment room of a preset production line workshop; the bottom plate mechanism and the frame mechanism are installed in a sealed mode. The testing mechanism is installed in a closed space formed by the frame mechanism, the bottom plate mechanism and the movable door assembly, the testing mechanism comprises a testing table and a testing assembly, a sulfide solid electrolyte to be detected is placed on the testing table, and the testing assembly comprises a hydrogen sulfide gas detector. And the hydrogen sulfide gas detector is arranged on one side of the test board. The testing device can achieve the technical effect of improving the development efficiency of the sulfide solid-state battery cell.

Description

Technical Field

[0001] The present application relates to the field of battery technology, and in particular to a testing device and a testing method for hydrogen sulfide release rate. Background Art

[0002] In order to meet the technical requirements of long driving range and high safety of new energy vehicles, major car companies on the market are now planning to develop all-solid-state batteries; among them, all-solid-state batteries have the following advantages: ① High cell energy density: Compared with the energy density of traditional liquid lithium batteries of 200-300Wh / kg, solid-state batteries use solid electrolytes, which are as high as 500h / kg; ② Higher safety: Solid-state electrolytes have good thermal stability, are non-flammable and non-explosive, and have no risk of liquid leakage. In addition, since the chemical activity of solid-state electrolytes is relatively stable and is less affected by ambient temperature, they are more stable in collisions and extrusions; ③ Higher mechanical strength and stability: All-solid-state batteries upgrade all electrolytes to solid electrolytes, thus having higher mechanical strength and stability; ④ Better overall performance: Solid-state batteries can inhibit the growth of lithium dendrites to a certain extent, and at the same time have the characteristics of long cycle life, compact structure, adjustable scale, large design flexibility, and easy packaging, which are in line with the future development direction of large-capacity new chemical energy storage technologies.

[0003] Generally, there are three main technical routes for all-solid-state batteries: polymer, sulfide, and oxide. At present, the ionic conductivity of sulfide solid electrolytes has initially met the requirements, and the subsequent material modification can further improve the ionic conductivity and environmental adaptability. The sulfide system has high technical maturity, rapid development progress, and is most likely to be mass-produced in the short term. It is the best overall. Major car companies on the market have all taken sulfide as the preferred technical route for all-solid-state electrolyte materials and the main development direction. However, the sulfide solid electrolyte Li6PS5Cl will produce hydrogen sulfide (H2S) in a dry environment with moisture. Hydrogen sulfide is a colorless and highly toxic acidic gas. The existing technology has not yet provided an effective test method and process for the release rate of hydrogen sulfide. It is impossible to effectively measure the release rate of hydrogen sulfide under different dew point environments, and it is impossible to effectively guide the development and construction of sulfide all-solid-state battery production lines, resulting in low development efficiency of sulfide solid-state batteries. Summary of the invention

[0004] The purpose of the present application is to provide a test device, a test method, an electronic device and a computer-readable storage medium for the release rate of hydrogen sulfide, which can achieve the technical effect of improving the development efficiency of sulfide solid-state batteries.

[0005] In a first aspect, the present application provides a test device for hydrogen sulfide release rate, comprising a frame mechanism, a base plate mechanism, a movable door assembly and a test mechanism;

[0006] The movable door assembly includes at least one movable door, and the frame mechanism is sealed and installed with the movable door, wherein the position of the movable door is set to correspond to the small environment room of the preset production line workshop;

[0007] The bottom plate mechanism is sealed and installed with the frame mechanism;

[0008] The testing mechanism is installed in the closed space of the frame mechanism, the base plate mechanism and the movable door assembly. The testing mechanism includes a testing bench and a testing assembly. The testing bench is used to place the sulfide solid electrolyte to be tested. The testing assembly includes a hydrogen sulfide gas detector, which is arranged on one side of the testing bench.

[0009] In the above implementation process, the test device for hydrogen sulfide release rate is set to correspond to the small environment room of the preset production line workshop through the position of the movable door, and the tooling structure of the test device is proportionally reduced to the actual structure of the workshop small environment room, and the various components are sealed and installed to prevent hydrogen sulfide from escaping to the outside; thus, the tooling structure of the test device for hydrogen sulfide release rate is close to the actual state of the small environment room of the production line workshop, and the device is a proportional reduction of the real small environment room, which is convenient for assessing the anti-corrosion effect of this structure under hydrogen sulfide state, and can assess and simulate the performance requirements such as structural strength and sealing structure of small environment rooms with similar structures; moreover, the test device for hydrogen sulfide release rate can effectively guide the development and construction of sulfide all-solid-state battery production lines by effectively measuring the hydrogen sulfide release rate of the sulfide solid electrolyte to be tested, thereby achieving the technical effect of improving the development efficiency of sulfide solid-state batteries.

[0010] Furthermore, the testing mechanism also includes an air blowing mechanism, which is arranged on the other side of the testing bench, and the air blowing mechanism, the testing bench, and the hydrogen sulfide gas detector are arranged in sequence.

[0011] In the above implementation process, the testing organization configures a blower mechanism inside the tooling of the testing device, and the blower mechanism blows hydrogen sulfide released by the sulfide solid electrolyte to be tested on the test bench, which can accelerate the diffusion of hydrogen sulfide and greatly shorten the test cycle.

[0012] Furthermore, the movable door is locked and sealed by means of a fluororubber sealing gasket and a sealant, and the joint between the movable door and the frame mechanism is locked and sealed by means of a stainless steel plate and a fluororubber sealing gasket.

[0013] Furthermore, the assembly characteristic data of the testing mechanism is the same as the preset assembly characteristic data of the battery pack, and the preset assembly characteristic data of the battery pack includes one or more of the battery cell-bottom plate contact area, the battery cell layout form, and the battery cell-bottom plate glue coating amount.

[0014] In the above implementation process, the assembly feature data of the test organization is the same as the preset assembly feature data of the battery pack, that is, the assembly feature data of the test organization can meet the actual assembly characteristics of the battery pack (such as cantilever beam structure), such as the contact area between the battery cell and the base plate, the layout of the battery cell, the distance between the battery cell and various surrounding components such as the longitudinal beam, the glue coating amount control between the battery cell and the base plate, etc., to improve the effectiveness and accuracy of hydrogen sulfide release detection.

[0015] In a second aspect, the present application provides a method for testing the hydrogen sulfide release rate, which is applied to the testing device for the hydrogen sulfide release rate described in any one of the first aspects, wherein the testing device for the hydrogen sulfide release rate is arranged in a constant temperature and humidity laboratory, and the testing method comprises:

[0016] Obtaining a sulfide solid electrolyte to be tested;

[0017] Regulating the test environment of the constant temperature and humidity laboratory to a preset experimental environment;

[0018] Placing the sulfide solid electrolyte to be tested on the test bench of the testing mechanism, and sealing the test device for the hydrogen sulfide release rate;

[0019] Obtain hydrogen sulfide concentration detection data at preset intervals under multiple dew point ambient temperatures;

[0020] A hydrogen sulfide detection result is generated according to the hydrogen sulfide concentration detection data.

[0021] In the above implementation process, the test method of hydrogen sulfide release rate can accurately measure the hydrogen sulfide concentration in the closed space of the test device by using a test device, and then combine the measurement time and the net volume of the closed space in the test device to calculate the hydrogen sulfide release rate of the sulfide solid electrolyte to be tested, thereby effectively guiding the development and construction of sulfide all-solid-state battery cell production lines and achieving the technical effect of improving the development efficiency of sulfide solid-state batteries.

[0022] Furthermore, the step of obtaining the sulfide solid electrolyte to be detected includes:

[0023] Preparing a sulfide sample to be detected, wherein the sulfide sample to be detected is in the form of dry powder, slurry, or electrode;

[0024] A sulfide sample to be detected with a preset weight is weighed at a preset dew point ambient temperature, and corresponding operation adjustments are performed according to the morphology of the sulfide sample to be detected to obtain a sulfide solid electrolyte to be detected.

[0025] Furthermore, the hydrogen sulfide detection result includes mass release rate data, and the step of generating the hydrogen sulfide detection result according to the hydrogen sulfide concentration detection data includes:

[0026] Obtaining net volume data and test time data of the test device for the hydrogen sulfide release rate;

[0027] The mass release rate data is obtained according to the net volume data, the test time data and the hydrogen sulfide concentration detection data.

[0028] Furthermore, the hydrogen sulfide detection result also includes area release rate data. After the step of obtaining the mass release rate data according to the net volume data, the test time data and the hydrogen sulfide concentration detection data, the method further includes:

[0029] Acquiring surface density data of the sulfide solid electrolyte to be detected;

[0030] The areal release rate data is obtained based on the mass release rate data and the areal density data.

[0031] In a third aspect, the present application provides an electronic device, comprising: a memory, a processor, and a computer program stored in the memory and executable on the processor, wherein the processor implements the steps of the method described in any one of the first aspects when executing the computer program.

[0032] In a fourth aspect, the present application provides a computer-readable storage medium, on which instructions are stored. When the instructions are executed on a computer, the computer executes the method as described in any one of the first aspects.

[0033] In a fifth aspect, the present application provides a computer program product, which, when running on a computer, enables the computer to execute the method as described in any one of the first aspects.

[0034] Other features and advantages disclosed in the present application will be described in the following description, or some features and advantages can be inferred or determined without doubt from the description, or can be learned by implementing the above-mentioned technology disclosed in the present application.

[0035] In order to make the above-mentioned objects, features and advantages of the present application more obvious and easy to understand, preferred embodiments are specifically cited below and described in detail with reference to the attached drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0036] 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.

[0037] Figure 1 A schematic diagram of the structure of a test device for hydrogen sulfide release rate provided in an embodiment of the present application;

[0038] Figure 2 A schematic diagram of the structure of the test device and the constant temperature and humidity laboratory provided in the embodiment of the present application;

[0039] Figure 3 A schematic flow chart of a method for testing the hydrogen sulfide release rate provided in an embodiment of the present application;

[0040] Figure 4 A schematic flow chart of another method for testing the hydrogen sulfide release rate provided in an embodiment of the present application;

[0041] Figure 5 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of 25°C;

[0042] Figure 6 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -20°C;

[0043] Figure 7 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -25°C;

[0044] Figure 8 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -30°C;

[0045] Fig. 9 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -35°C;

[0046] Fig.10 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -40°C;

[0047] Fig.11 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -45°C;

[0048] Fig.12 A schematic diagram of a test of the powder provided in an embodiment of the present application at a dew point ambient temperature of -50°C;

[0049] Fig.13 A schematic diagram of a test of the slurry provided in an embodiment of the present application at a dew point ambient temperature of 25°C;

[0050] Fig.14 A schematic diagram of a test of the slurry provided in an embodiment of the present application at a dew point ambient temperature of -20°C;

[0051] Fig.15A schematic diagram of the test of the slurry provided in the embodiment of the present application at a dew point ambient temperature of -25°C;

[0052] Fig.16 A schematic diagram of the test of the slurry provided in the embodiment of the present application at a dew point ambient temperature of -30°C;

[0053] Fig.17 A schematic diagram of the test of the slurry provided in the embodiment of the present application at a dew point ambient temperature of -35°C;

[0054] Fig.18 A schematic diagram of the test of the slurry provided in the embodiment of the present application at a dew point ambient temperature of -40°C;

[0055] Fig.19 A schematic diagram of the test of the slurry provided in the embodiment of the present application at a dew point ambient temperature of -45°C;

[0056] Fig. 20 A schematic diagram of a test of the slurry provided in an embodiment of the present application at a dew point ambient temperature of -50°C;

[0057] Fig.21 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of 25°C;

[0058] Fig. 22 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -20°C;

[0059] Fig.23 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -25°C;

[0060] Fig.24 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -30°C;

[0061] Fig.25 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -35°C;

[0062] Fig.26 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -40°C;

[0063] Fig. 27 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -45°C;

[0064] Fig.28 A schematic diagram of testing the electrode provided in an embodiment of the present application at a dew point ambient temperature of -50°C;

[0065] Fig.29 A structural block diagram of an electronic device provided in an embodiment of the present application. DETAILED DESCRIPTION

[0066] 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.

[0067] 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.

[0068] Generally speaking, in order to meet the technical requirements of new energy vehicles such as long driving range and high safety, all-solid-state batteries are being developed on the market; all-solid-state batteries have the following advantages:

[0069] ① High energy density of battery cells: Compared with the energy density of traditional liquid lithium batteries of 200-300Wh / kg, solid-state batteries use solid electrolytes, which are as high as 500h / kg;

[0070] ② Higher safety: Solid electrolytes have good thermal stability, are non-flammable and non-explosive, and have no risk of liquid leakage. In addition, since the chemical activity of solid electrolytes is relatively stable and is less affected by ambient temperature, they are more stable in the event of collision and extrusion.

[0071] ③Higher mechanical strength and stability: All-solid-state batteries upgrade all electrolytes to solid electrolytes, thus having higher mechanical strength and stability;

[0072] ④ Have better comprehensive performance: solid-state batteries can inhibit the growth of lithium dendrites to a certain extent, and have the characteristics of long cycle life, compact structure, adjustable scale, large design flexibility, easy packaging, etc., which is in line with the development direction of future large-capacity new chemical energy storage technology;

[0073] Generally speaking, there are three main technical routes for all-solid-state batteries at this stage: polymer, sulfide, and oxide. At present, the ionic conductivity of sulfide solid electrolytes has initially met the requirements, and the subsequent material modification can further improve the ionic conductivity and environmental adaptability. The sulfide system has high technical maturity, rapid development progress, and is most likely to be mass-produced in the short term. It is the best overall choice. Sulfide is the preferred technical route for all-solid-state electrolyte materials on the market and is the main development direction; the chemical equation of the sulfide system is as follows:

[0074] Li6PS5Cl+6H2O→Li3PO4+5H2S+LiCl+2LiOH;

[0075] From the above formula, we can know that the sulfide solid electrolyte Li6PS5Cl will produce hydrogen sulfide H2S in a dry environment with moisture. H2S is a colorless and highly toxic acidic gas, and the occupational exposure limit of hydrogen sulfide is ≤10mg / m 3 During the development and trial production of sulfide all-solid-state batteries, for personnel safety reasons, the release of H2S needs to be specially controlled;

[0076] Existing patents and literature have not yet provided an effective test method and process for the hydrogen sulfide release rate, and are unable to effectively measure the hydrogen sulfide release rate under different dew point environments, and are unable to effectively guide the development and construction of sulfide all-solid-state battery cell production lines.

[0077] In order to solve the above-mentioned technical problems, the embodiments of the present application provide a test device, a test method, an electronic device and a computer-readable storage medium for the hydrogen sulfide release rate, which can be applied to the hydrogen sulfide release detection process of sulfide solid-state batteries; see Figure 1 and Figure 2 , Figure 1 This is a schematic diagram of the structure of a test device for the hydrogen sulfide release rate provided in an embodiment of the present application. Figure 2 A schematic diagram of the structure of a test device and a constant temperature and humidity laboratory provided in an embodiment of the present application; the test device for hydrogen sulfide release rate includes a frame mechanism 100, a base plate mechanism 200, a movable door assembly 300 and a test mechanism 400;

[0078] Optionally, the test device for the hydrogen sulfide release rate provided in the embodiment of the present application is installed in a constant temperature and humidity laboratory; Figure 2 As shown, the indoor air pressure P2 of the constant temperature and humidity laboratory is a slightly positive pressure, the internal air pressure P1 of the test device for the hydrogen sulfide release rate is a slightly negative pressure, and the air pressure P3 is the atmospheric pressure of the external environment; thereby, it is ensured that the hydrogen sulfide released by the sulfide solid electrolyte to be tested will not escape into the room of the constant temperature and humidity laboratory, and even if the hydrogen sulfide escapes into the constant temperature and humidity laboratory, it can be quickly discharged to the external environment.

[0079] Exemplarily, the movable door assembly 300 includes at least one movable door 310, and the frame mechanism 100 is sealed and installed with the movable door 310, wherein the position setting of the movable door 310 corresponds to the small environment room of the preset production line workshop;

[0080] Exemplarily, the base plate mechanism 200 is sealed and mounted with the frame mechanism 100;

[0081] Exemplarily, the test mechanism 400 is installed in the enclosed space of the frame mechanism 100, the base plate mechanism 200 and the movable door assembly 300, and the test mechanism 400 includes a test bench 410 and a test assembly 420. The test bench 410 places the sulfide solid electrolyte to be tested, and the test assembly 420 includes a hydrogen sulfide gas detector, which is arranged on one side of the test bench 410.

[0082] Illustratively, the concentration of hydrogen sulfide released by the sulfide solid electrolyte to be detected can be detected by a hydrogen sulfide gas detector, and thus the hydrogen sulfide release rate of the sulfide solid electrolyte to be detected can be calculated in combination with the detected hydrogen sulfide concentration in a closed space.

[0083] In some embodiments, the test device for hydrogen sulfide release rate is arranged to correspond to the small environment room of a preset production line workshop through the position of the movable door 310, and the tooling structure of the test device is proportionally reduced to the actual structure of the workshop small environment room, and each component is sealed and installed to prevent hydrogen sulfide from escaping to the outside; thus, the tooling structure of the test device for hydrogen sulfide release rate is close to the actual state of the small environment room of the production line workshop, and the device is a proportional reduction of the real small environment room, which is convenient for assessing the anti-corrosion effect of such structure under hydrogen sulfide state, and can assess and simulate the performance requirements such as structural strength and sealing structure of small environment rooms with similar structures; moreover, the test device for hydrogen sulfide release rate can effectively guide the development and construction of sulfide all-solid-state battery cell production lines by effectively measuring the hydrogen sulfide release rate of the sulfide solid electrolyte to be tested, thereby achieving the technical effect of improving the development efficiency of sulfide solid-state batteries.

[0084] Exemplarily, the testing mechanism 400 further includes a blower mechanism 430, which is disposed on the other side of the testing bench, and the blower mechanism 430, the testing bench 410, and the hydrogen sulfide gas detector are sequentially arranged.

[0085] Exemplarily, the testing mechanism 400 is configured with a blower mechanism 430 inside the tooling of the testing device, and the blower mechanism 430 blows hydrogen sulfide released from the sulfide solid electrolyte to be tested on the test bench 410, which can accelerate the diffusion of hydrogen sulfide and greatly shorten the test cycle.

[0086] In some embodiments, the hair blowing mechanism may be a remote-controlled variable-frequency small electric fan; it should be noted that this is only an example and not a limitation, and the hair blowing mechanism may also be other types of fans, which will not be described in detail.

[0087] Exemplarily, the movable door 310 is locked and sealed by means of a fluororubber sealing gasket and a sealant, and the joint between the movable door 310 and the frame mechanism 100 is locked and sealed by means of a stainless steel plate and a fluororubber sealing gasket.

[0088] Exemplarily, the assembly feature data of the test mechanism 400 is the same as the preset assembly feature data of the battery pack, and the preset assembly feature data of the battery pack includes one or more of the battery cell-base plate contact area, the battery cell layout form, and the battery cell-base plate glue coating amount.

[0089] Exemplarily, the assembly feature data of the test mechanism 400 is the same as the preset assembly feature data of the battery pack, that is, the assembly feature data of the test mechanism 400 can meet the actual assembly characteristics of the battery pack (such as cantilever beam structure), such as the contact area between the battery cell and the base plate, the layout of the battery cell, the distance between the battery cell and various surrounding components such as the longitudinal beam, the control of the amount of glue between the battery cell and the base plate, etc., thereby improving the effectiveness and accuracy of hydrogen sulfide release detection.

[0090] See also Figure 3 , Figure 3 A flow chart of a method for testing the release rate of hydrogen sulfide provided in an embodiment of the present application; the method for testing the release rate of hydrogen sulfide is applied to Figure 1 and Figure 2 The test device for hydrogen sulfide release rate shown in the figure, wherein the test device for hydrogen sulfide release rate is set in a constant temperature and humidity laboratory, and the test method comprises the following steps:

[0091] S100: obtaining a sulfide solid electrolyte to be tested;

[0092] The sulfide solid electrolyte to be tested is prepared, and the specific form of the sulfide solid electrolyte to be tested can be dry powder, slurry, electrode sheet and other forms.

[0093] S200: Adjust the test environment of the constant temperature and humidity laboratory to the preset experimental environment;

[0094] The test environment of the constant temperature and humidity laboratory is adjusted according to the test requirements, so that after standing for a preset time, the test device in the constant temperature and humidity laboratory reaches the preset experimental environment; wherein the preset experimental environment includes requirements such as temperature and dew point temperature.

[0095] S300: placing the sulfide solid electrolyte to be tested on a test bench of a testing organization, and sealing a test device for hydrogen sulfide release rate;

[0096] S400: obtaining hydrogen sulfide concentration detection data according to a preset interval time at multiple dew point ambient temperatures;

[0097] S500: Generate hydrogen sulfide detection results according to the hydrogen sulfide concentration detection data.

[0098] Illustratively, the test method for hydrogen sulfide release rate can accurately measure the hydrogen sulfide concentration in the enclosed space of the test device by using a test device, and then calculate the hydrogen sulfide release rate of the sulfide solid electrolyte to be tested in combination with the measurement time and the net volume of the enclosed space in the test device, thereby effectively guiding the development and construction of sulfide all-solid-state battery cell production lines and achieving the technical effect of improving the development efficiency of sulfide solid-state batteries.

[0099] Please attend Figure 4 , Figure 4 A schematic flow chart of another method for testing the hydrogen sulfide release rate provided in an embodiment of the present application.

[0100] Exemplarily, S100: the step of obtaining a sulfide solid electrolyte to be detected includes:

[0101] S110: preparing a sulfide sample to be tested, wherein the sulfide sample to be tested has a form including dry powder, slurry, and electrode;

[0102] S120: weighing a preset weight of the sulfide sample to be detected at a preset dew point ambient temperature, and performing corresponding operation adjustments according to the morphology of the sulfide sample to be detected to obtain a sulfide solid electrolyte to be detected.

[0103] Exemplarily, the hydrogen sulfide detection result includes mass release rate data. S500: the step of generating the hydrogen sulfide detection result according to the hydrogen sulfide concentration detection data includes:

[0104] S510: Obtaining net volume data and test time data of a test device for hydrogen sulfide release rate;

[0105] S520: Obtain mass release rate data according to the net volume data, the test time data and the hydrogen sulfide concentration detection data.

[0106] Exemplarily, the hydrogen sulfide detection result also includes area release rate data. S520: After the step of obtaining mass release rate data according to the net volume data, the test time data and the hydrogen sulfide concentration detection data, the method further includes:

[0107] S530: Acquire surface density data of the sulfide solid electrolyte to be tested;

[0108] S540: Obtaining area release rate data according to the mass release rate data and the surface density data.

[0109] In some implementation scenarios, combined with Figure 1 to Figure 2 The test device for the hydrogen sulfide release rate shown, and Figure 3 to Figure 4 The test method for hydrogen sulfide release rate shown in the figure, the specific process steps of the test method for hydrogen sulfide release rate are as follows:

[0110] Step 1 - Sample Preparation:

[0111] Sulfide solid electrolyte Li6PS5Cl is used, which can be in three states: dry powder (Li6PS5Cl powder), slurry (Li6PS5Cl powder + dodecane + IBIB, the slurry design solid content is 55%), pole piece (pole piece coating thickness: 70μm, the film roll is the above slurry coated and baked on the modified aluminum foil);

[0112] Step 2 - Device Layout:

[0113] Place the H2S gas detector, industrial hygrometer, and remote-controlled variable frequency small electric fan in a Figure 2 In the test device shown;

[0114] Step 3 - Environment Adjustment:

[0115] Adjust the constant temperature and humidity laboratory test environment to the required experimental environment, the temperature is: 20℃±1℃, the dew point environment temperature is: 25℃±1℃, -20℃±1℃, -30℃±1℃, -40℃±1℃, -50℃±1℃ dew point environment;

[0116] Step 4 - Sample weighing:

[0117] The test device was left to stand for a while, and the test device environment was kept consistent with the laboratory environment. 1±0.05g of sample was weighed in a -50℃ dry dew point environment. The slurry was naturally flowing in an evaporating dish, and the spreading diameter was about 2.6cm. The calculated spreading area was about 5.31cm 2 / g; the uncoated area of ​​the electrode was cut out, and the coated area was selected for testing. The powder was naturally stacked. After the sample was weighed, it was wrapped with plastic wrap to isolate the environmental water vapor;

[0118] Step 5 - Sample placement:

[0119] Place the sample in a test device with different dew point environments, seal the test device, and record the hydrogen sulfide data at regular intervals according to the hydrogen sulfide reaction rate. Record for 30 minutes or stop when the concentration exceeds the detection limit of the gas detector.

[0120] Step 6 - Post-test processing:

[0121] After the experiment is completed, take out the samples and make them harmless, evaporate the hydrogen sulfide in the test device, and then conduct the next dew point environment test;

[0122] The calculation example of hydrogen sulfide concentration and mass release rate is as follows:

[0123] The net volume inside the test device is 5066.95 cm 3, then the average mass release rate of hydrogen sulfide v m The calculation formula is:

[0124]

[0125] Wherein, a (ppm) is the reading of the hydrogen sulfide gas detector, m (g) is the actual weight of the sample, for the convenience of calculation, the test fixed mass of m can be set to 1±0.05g, and t is the test time (min); optionally, in order to reduce the effects of hydrogen sulfide desorption and volatilization under low dew point conditions, the test can be carried out at a relatively stable stage of hydrogen sulfide release;

[0126] Among them, the area release rate is calculated for the electrode, and the specific calculation method is as follows:

[0127] Use the electrode sampler to accurately cut 10cm 2 The pole piece has a weighing mass of 0.1114 g, so the surface density of the pole piece is s 0.01114 g / cm 2 ; Therefore, the average area release rate of the electrode v s for:

[0128] v s =v m ×ρ s =v m ×0.01114g / cm 2 .

[0129] In some implementation scenarios, the test device for hydrogen sulfide release rate provided in the embodiment of the present application is a first-of-its-kind test device, and its tooling structure is as follows: 1) The tooling structure is proportionally reduced to the actual structure of the workshop microenvironment room, and is mainly composed of an overall frame, a door, and a lower bottom plate, etc., and each component can be fixed together by sealing, chains, etc.; 2) A remote-controlled variable-frequency small electric fan is configured inside the tooling to accelerate the diffusion of hydrogen sulfide and shorten the test cycle; 3) The movable door is locked and sealed by a fluororubber sealing pad + sealant; 4) The joint between the door and the overall frame is locked and sealed by a stainless steel plate + fluororubber sealing pad;

[0130] The test device for hydrogen sulfide release rate has the following structural features: 1) It is closer to the actual state of the small environment room in the production line workshop. The device is a proportional reduction of the real small environment room, and the materials used are exactly the same, which makes it convenient to evaluate the anti-corrosion effect of this structure under hydrogen sulfide conditions; 2) The structure of the device is completely equivalent to the small environment room, such as the sealing structure (door hinge, door gap, door structure, rubber strip structure, etc.), which can evaluate and simulate the performance requirements of the structural strength and sealing structure of the small environment room with similar structure; 3) It meets the actual assembly characteristics of the battery pack (cantilever beam structure), such as the contact area between the battery cell and the bottom plate, the layout of the battery cell, the distance between the battery cell and various peripheral components such as the longitudinal beam, and the control of the amount of glue between the battery cell and the bottom plate; 4) The device has a simple structure and is easy to disassemble and assemble. It adopts bolt fixing method to realize hydrogen sulfide release rate test at powder level, battery cell level, and module level;

[0131] Exemplarily, the test device for the hydrogen sulfide release rate is the first tooling structure for hydrogen sulfide release rate testing, which is closer to the actual state of the small environment room in the production line workshop. Its selected materials and structural methods are equivalent to those of the small environment room, and can assess the structural strength, sealing structure, corrosion resistance and other performance requirements of the small environment room; in addition, the test device for the hydrogen sulfide release rate has the advantages of short development cycle, low cost and higher efficiency, and can realize hydrogen sulfide release rate tests at powder level, cell level, and module level, which is conducive to quickly exploring the safety boundary conditions.

[0132] In some embodiments, by Figure 1 and Figure 2 The test device for the hydrogen sulfide release rate shown, and Figure 3 and Figure 4 The test methods for hydrogen sulfide release rate shown in the figure are respectively used for powder, slurry and electrode tests, and the test results are as follows:

[0133] 1. Powder test results:

[0134] Table 1 - Powder test results

[0135]

[0136] See also Figures 5 to 12 , which are the test data of dew point ambient temperature of 25℃, -20℃, -25℃, -30℃, -35℃, -40℃, -45℃, -50℃ respectively;

[0137] Conclusion: ① From the above data, it can be seen that the dew point ambient temperature is -40℃ or above, which can effectively suppress the release of hydrogen sulfide from the powder. This is an important temperature inflection point and an important temperature reference point for guiding the design of production line equipment.

[0138] ②At a dew point of -45℃, a certain mass of sulfide will basically stabilize after half an hour of release; at a dew point of -50℃, a certain mass of sulfide will basically stabilize after nearly 10 minutes of release. This shows that for the same mass of sulfide, the lower the dew point of the environment, the shorter the release stability time. This is also an important temperature reference point to guide the design of production line equipment.

[0139] 2. Slurry test results:

[0140] Table 2 - Slurry test results

[0141]

[0142] See also Figures 13 to 20 , which are the test data of dew point ambient temperature of 25℃, -20℃, -25℃, -30℃, -35℃, -40℃, -45℃, -50℃ respectively;

[0143] Conclusion: ① From the above data, it can be seen that when the dew point ambient temperature is -40℃ or above, the release of hydrogen sulfide from the slurry can be effectively suppressed and controlled within the upper limit of occupational exposure. This is an important temperature inflection point and an important temperature reference point for guiding the design of production line equipment.

[0144] ②At a dew point of -45℃, a certain mass of sulfide will basically stabilize after half an hour of release; at a dew point of -50℃, a certain mass of sulfide will basically stabilize after nearly 10 minutes of release. This shows that for the same mass of sulfide, the lower the dew point of the environment, the shorter the release stability time. This is also an important temperature reference point for guiding the design of production line equipment.

[0145] 2. Pole piece test results:

[0146] Table 3 - Pole piece test results

[0147]

[0148] See also Figures 21 to 28 , which are the test data of dew point ambient temperature of 25℃, -20℃, -25℃, -30℃, -35℃, -40℃, -45℃, -50℃ respectively;

[0149] Conclusion: ① From the above data, it can be seen that when the dew point ambient temperature is -45℃ or above, the release of hydrogen sulfide from the electrode can be effectively suppressed and controlled within the upper limit of occupational exposure. This is an important temperature inflection point and an important temperature reference point for guiding the design of production line equipment.

[0150] ②At a dew point of -50℃, a certain mass of sulfide basically tends to be stable after being released for nearly 10 minutes; this means that for a certain mass of sulfide, the lower the dew point of the environment, the shorter the release stability time;

[0151] For example, the existing patents and literature have not yet provided an effective test method and process for the hydrogen sulfide release rate, and cannot effectively measure the hydrogen sulfide release rate under different dew point environments, and cannot effectively guide the development and construction of sulfide all-solid-state battery cell production lines; the test device and test method for the hydrogen sulfide release rate provided in the embodiment of the present application adopt the first hydrogen sulfide release rate test device structure + optimized hydrogen sulfide release rate test method and process, which can quickly explore the safe boundary state of hydrogen sulfide release of raw materials (powder, slurry, electrode) in different states at different dew point ambient temperatures, sort out its rules, and clarify -45°C as an important temperature reference point for guiding the design of production line equipment, which greatly shortens the development of the sulfide all-solid-state battery cell production line and the introduction of product development verification cycle, so that the battery cell can enter the real trial production test link as soon as possible, and truly improve the product competitiveness.

[0152] This application also provides an electronic device, see Fig.29 , Fig.29 A block diagram of an electronic device provided in an embodiment of the present application. The electronic device may include a processor 510, a communication interface 520, a memory 530, and at least one communication bus 540. The communication bus 540 is used to realize direct connection and communication between these components. The communication interface 520 of the electronic device in the embodiment of the present application is used to communicate signaling or data with other node devices. The processor 510 may be an integrated circuit chip with signal processing capabilities.

[0153] The processor 510 mentioned above can be a general-purpose processor, including a central processing unit (CPU), a network processor (NP), etc.; it can also be a digital signal processor (DSP), an application-specific integrated circuit (ASIC), a field-programmable gate array (FPGA) or other programmable logic devices, discrete gates or transistor logic devices, discrete hardware components. The methods, steps and logic block diagrams disclosed in the embodiments of the present application can be implemented or executed. The general-purpose processor can be a microprocessor or the processor 510 can also be any conventional processor, etc.

[0154] The memory 530 may be, but is not limited to, a random access memory (RAM), a read only memory (ROM), a programmable read-only memory (PROM), an erasable programmable read-only memory (EPROM), an electric erasable programmable read-only memory (EEPROM), etc. The memory 530 stores computer-readable instructions. When the computer-readable instructions are executed by the processor 510, the electronic device can execute the above-mentioned Figure 3 to Figure 4 The method embodiment involves various steps.

[0155] Optionally, the electronic device may further include a storage controller and an input / output unit.

[0156] The memory 530, storage controller, processor 510, peripheral interface, input and output unit components are directly or indirectly electrically connected to each other to achieve data transmission or interaction. For example, these components can be electrically connected to each other via one or more communication buses 540. The processor 510 is used to execute executable modules stored in the memory 530, such as software function modules or computer programs included in the electronic device.

[0157] The input and output unit is used to provide users with the task creation and to create a start optional time period or preset execution time for the task to realize the interaction between the user and the server. The input and output unit can be, but is not limited to, a mouse and a keyboard.

[0158] Understandably, Fig.29 The structure shown is for illustration only, and the electronic device may also include Fig.29 More or fewer components as shown, or with Fig.29 Different configurations shown. Fig.29 Each component shown in the figure can be implemented by hardware, software or a combination thereof.

[0159] An embodiment of the present application further provides a storage medium having instructions stored thereon. When the instructions are run on a computer, the computer program is executed by a processor to implement the method described in the method embodiment. To avoid repetition, the method will not be described here.

[0160] The present application also provides a computer program product, which, when executed on a computer, enables the computer to execute the method described in the method embodiment.

[0161] In several embodiments provided in the present application, it should be understood that the disclosed devices and methods 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 devices, methods and computer program products according to 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 flowchart, and the combination of boxes in the block diagram and / or 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.

[0162] 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.

[0163] 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.

[0164] 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.

[0165] 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.

[0166] 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 presence of other identical elements in the process, method, article or device including the elements.

Claims

1. A test device for hydrogen sulfide release rate, characterized in that: It includes a frame mechanism, a base plate mechanism, a movable door assembly and a testing mechanism; The movable door assembly includes at least one movable door, and the frame mechanism is sealed and installed with the movable door, wherein the position of the movable door is set to correspond to the small environment room of the preset production line workshop; The bottom plate mechanism is sealed and installed with the frame mechanism; The testing mechanism is installed in the closed space of the frame mechanism, the base plate mechanism and the movable door assembly. The testing mechanism includes a testing bench and a testing assembly. The testing bench is used to place the sulfide solid electrolyte to be tested. The testing assembly includes a hydrogen sulfide gas detector, which is arranged on one side of the testing bench.

2. The test device for hydrogen sulfide release rate according to claim 1, characterized in that: The testing mechanism further includes a blower mechanism, which is disposed on the other side of the testing bench, and the blower mechanism, the testing bench, and the hydrogen sulfide gas detector are sequentially arranged.

3. The test device for hydrogen sulfide release rate according to claim 1 or 2, characterized in that: The movable door is locked and sealed by means of a fluororubber sealing pad and a sealant, and the joint between the movable door and the frame mechanism is locked and sealed by means of a stainless steel plate and a fluororubber sealing pad.

4. The test device for hydrogen sulfide release rate according to claim 1, characterized in that: The assembly characteristic data of the test mechanism is the same as the preset assembly characteristic data of the battery pack, and the preset assembly characteristic data of the battery pack includes one or more of the contact area between the battery cell and the base plate, the arrangement form of the battery cell, and the glue coating amount between the battery cell and the base plate.

5. A method for testing the release rate of hydrogen sulfide, characterized in that: The test device for hydrogen sulfide release rate according to any one of claims 1 to 4 is provided in a constant temperature and humidity laboratory, and the test method comprises: Obtaining a sulfide solid electrolyte to be tested; Regulating the test environment of the constant temperature and humidity laboratory to a preset experimental environment; Placing the sulfide solid electrolyte to be tested on the test bench of the testing mechanism, and sealing the test device for the hydrogen sulfide release rate; Obtain hydrogen sulfide concentration detection data at preset intervals under multiple dew point ambient temperatures; A hydrogen sulfide detection result is generated according to the hydrogen sulfide concentration detection data.

6. The method for testing the hydrogen sulfide release rate according to claim 5, characterized in that: The steps of obtaining the sulfide solid electrolyte to be tested include: Preparing a sulfide sample to be detected, wherein the sulfide sample to be detected is in the form of dry powder, slurry, or electrode; A sulfide sample to be detected with a preset weight is weighed at a preset dew point ambient temperature, and corresponding operation adjustments are performed according to the morphology of the sulfide sample to be detected to obtain a sulfide solid electrolyte to be detected.

7. The method for testing the hydrogen sulfide release rate according to claim 5, characterized in that: The hydrogen sulfide detection result includes mass release rate data, and the step of generating the hydrogen sulfide detection result according to the hydrogen sulfide concentration detection data includes: Obtaining net volume data and test time data of the test device for the hydrogen sulfide release rate; The mass release rate data is obtained according to the net volume data, the test time data and the hydrogen sulfide concentration detection data.

8. The method for testing the hydrogen sulfide release rate according to claim 7, characterized in that: The hydrogen sulfide detection result also includes area release rate data. After the step of obtaining the mass release rate data according to the net volume data, the test time data and the hydrogen sulfide concentration detection data, the method further includes: Acquiring surface density data of the sulfide solid electrolyte to be detected; The areal release rate data is obtained based on the mass release rate data and the areal density data.

9. An electronic device, characterized in that: include: A memory, a processor, and a computer program stored in the memory and executable on the processor, wherein when the processor executes the computer program, the steps of the method for testing the hydrogen sulfide release rate according to any one of claims 5 to 8 are implemented.

10. A computer-readable storage medium, characterized in that: The computer-readable storage medium stores instructions, and when the instructions are executed on a computer, the computer is enabled to execute the method for testing the hydrogen sulfide release rate according to any one of claims 5 to 8.

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