CN114965621A - Electrochemical mass spectrum device suitable for solid-state battery gas production research - Google Patents
Electrochemical mass spectrum device suitable for solid-state battery gas production research Download PDFInfo
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- CN114965621A CN114965621A CN202210764915.4A CN202210764915A CN114965621A CN 114965621 A CN114965621 A CN 114965621A CN 202210764915 A CN202210764915 A CN 202210764915A CN 114965621 A CN114965621 A CN 114965621A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
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- G—PHYSICS
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Abstract
The invention provides an electrochemical mass spectrometry device, which comprises a battery placing sealing cavity for placing a solid-state battery; the battery placing sealing cavity is connected with a calibration system for gas quantitative calibration, a battery testing system, a mass spectrometer and a pressure difference system. The calibration system comprises a standard gas and a pressure gauge A, wherein the standard gas is communicated with the battery placing sealing cavity, the pressure gauge A can directly react the battery to place real-time pressure in the sealing cavity, a standard leak hole is formed in an air inlet pipeline of the standard gas, the standard gas enters the battery placing sealing cavity after the flow of the standard gas is controlled through the standard leak hole, and the standard gas is further connected with a pressure gauge B. The invention is suitable for direct solid-state battery gas production test and has good time resolution and test sensitivity.
Description
Technical Field
The invention relates to the technical field of battery testing, in particular to an electrochemical mass spectrometry device which can be suitable for gas production research of laboratory and commercial/industrial solid-state batteries.
Background
With the continuous improvement of energy demand of modern society, the transformation and upgrade of energy structures are imminent. New energy storage and conversion technologies typified by lithium batteries are an advanced solution strategy. Currently, organic electrolytes with high ionic conductivity and temperature use range are the mainstream electrolytes of lithium batteries. However, the lithium battery is accompanied by a large amount of heat release during its operation, such as heat generation caused by many side reactions and abuse (thermal, electrical, mechanical) of various degrees, and the organic electrolyte is flammable and is very likely to cause safety accidents. Therefore, the development of safe solid electrolyte-based lithium batteries has become a leading research field in the current academic and industrial fields. However, the interface between the solid electrolyte (including inorganic and organic polymers) and the electrode is not completely stable, and some side reactions still exist, which seriously affect the performance improvement of the solid-state battery. Therefore, developing and optimizing solid electrolyte needs to establish a set of sensitive and high-time-resolution detection method to determine its feasibility and reaction mechanism so as to further optimize and design high-performance solid lithium battery.
The differential electrochemical mass spectrum is an in-situ gas analysis technology, and can be used for in-situ qualitative and quantitative research on consumption and release conditions of battery interface reaction gases. Generally, there are two injection modes of differential electrochemical mass spectrometry: carrier gas purging sample injection and membrane sample injection. The PTFE membrane is only suitable for water system electrocatalysis/water system batteries in a membrane sample introduction mode, a special mould design is needed, and quantification is difficult; the carrier gas blowing sample injection mode refers to that the carrier gas carries the electrochemical reaction gas generated and enters a mass spectrum for analysis and detection, and the defect of film sample injection can be overcome. However, in the carrier gas purging sample injection mode, the pipeline of the sample injection system is long, the time resolution is poor, and the gas carrying amount for achieving the purging purpose is generally far larger than the gas production amount of the battery, so that the detection sensitivity is low; meanwhile, the current method is only suitable for laboratory model battery gas production research, commercial/industrial solid-state batteries are difficult to be directly coupled into a sample introduction system, and the direct coupling causes very poor time resolution, sensitivity and detection accuracy. Therefore, the application range of differential electrochemical mass spectrometry is widened to the commercial/industrial solid-state battery, and an efficient, sensitive and accurate battery testing method is provided, which has important significance for enterprise users.
Disclosure of Invention
The invention aims to provide an electrochemical mass spectrometry device which is suitable for direct gas production test of solid-state batteries (including laboratory, commercial/industrial), and improves time resolution and test sensitivity.
In order to achieve the above purpose, the invention provides the following technical scheme:
an electrochemical mass spectrometry apparatus comprising: a battery housing chamber for housing a solid-state battery; the battery is placed the seal chamber and is connected with the calibration system that is used for gaseous ration calibration, the calibration system includes places the standard gas of seal chamber intercommunication and can direct reaction battery with the battery and places the pressure gauge A of seal intracavity real-time pressure, be equipped with the standard small opening on the gaseous air inlet pipe way of standard, get into the battery after standard gas passes through standard small opening controlled flow and place the seal chamber, still be connected with pressure gauge B on the standard gas.
As an optimized alternative, the battery placing sealing cavity is also connected with: the battery test system is used for providing parameters required by the operation for the solid-state battery; a mass spectrometer for analyzing the gas generated from the solid-state battery; a pressure differential system for creating a pressure differential across the cell-receiving sealed chamber. The pressure difference system is matched with the calibration system to finish calibration before mass spectrometer detection, the battery test system can control and adjust the solid-state battery under the target detection condition, and high-sensitivity detection is finished by matching with the device state after calibration.
As an optimized alternative, the battery testing system, the mass spectrometer and the differential pressure system are respectively communicated with the battery placing sealing cavity directly or through one or more solenoid valves in the valve group. Profile complexity and tubing length are reduced.
As an optimized alternative, the differential pressure system comprises a suction device, preferably a vacuum pump.
As an optimized alternative, the battery placing sealing cavity is provided with an interface used for connecting with other components. Specifically, the battery placing sealing cavity is respectively provided with an interface a and an interface e for connecting with a battery testing system, an interface c for connecting with a pressure gauge A, an interface d for connecting with a pressure difference system, and an interface b for connecting with a calibration system. Each interface can set up respectively on the sealed lid body of sealed chamber is placed to the battery, and the setting up of interface has made things convenient for the connection between the part and has guaranteed sealing stability.
As an optimized alternative, electromagnetic valves for controlling the opening and closing of the communication state of each pipeline and the battery placement sealing cavity are respectively arranged on the pipelines of the differential pressure system, the mass spectrometer and the calibration system.
The invention also provides a battery placing sealed cavity structure which is provided with a sealed cavity capable of being opened and closed for placing the solid battery, wherein a wall body for enclosing to form the sealed cavity is provided with an interface, and the sealed cavity structure comprises an interface a and an interface e which are used for being connected with a battery testing system for providing parameters required by the work of the solid battery, an interface c which is used for being connected with a pressure gauge A for reacting the real-time pressure in the battery placing sealed cavity, an interface d which is used for being connected with a pressure difference system for generating the pressure difference in the battery placing sealed cavity, and an interface b which is used for being connected with a calibration system for quantitatively calibrating the gas.
As an optimized alternative, the sealed cavity is enclosed by a hollow cavity body and a cover body, and the interfaces are respectively arranged on the cavity body and/or the cover body.
As an optimized alternative, a sealing gasket is arranged at the covering part between the cavity and the cover body, and fixing holes respectively corresponding to the upper positioning hole on the cover body and the lower positioning hole on the cavity are formed in the sealing gasket.
The invention also provides a method for carrying out gas production test on the solid-state battery by adopting the electrochemical mass spectrometry device, which comprises the following steps:
s1: placing the solid-state battery in a battery placing sealing cavity, well connecting the solid-state battery with a battery testing system, and closing the battery placing sealing cavity to finish sealing;
s2: a differential pressure system is adopted to remove air or impure gas in a battery placing sealing cavity and a pipeline including a calibration system and form differential pressure;
s3: opening a pipeline where the calibration system, the pressure gauge A and the mass spectrometer are located, closing other pipelines, determining the leakage rate of a standard leak hole in the calibration system through the pressure gauge A and a pressure gauge B in the calibration system, and establishing a standard curve between the flow rate of standard gas components and the ion current of the mass spectrometer;
s4: and starting a battery testing system and a pipeline where a mass spectrometer is located, and closing other pipelines to enable the solid-state battery to start to operate under the condition of target working parameters, and performing electrochemical mass spectrometry on the generated gas generated in the operation process.
As an optimized alternative, in step S1, the solid-state battery is placed in front of the battery placement sealing cavity, and a gas outlet is reserved to facilitate gas collection.
As an optimized alternative, in step S2, the solenoid valve B is closed, the solenoid valve C and the solenoid valve a are opened, the vacuum pump is opened to pump air, and whether the pressure gauge a is reduced to a vacuum state is observed, and then the solenoid valve a and the vacuum pump are closed, the solenoid valve B is opened, and the corresponding response signal of the mass spectrometer is observed to determine whether the content of air or impure gas in the whole system is reduced to a desired value and reaches a steady state.
As an optimized alternative, in step S2, closing the electromagnetic valve a and the electromagnetic valve B, opening the electromagnetic valve C, allowing the standard gas to flow through the standard leak hole and the electromagnetic valve C, reach the battery placement sealing cavity, and then rapidly diffuse into the mass spectrometer through the electromagnetic valve B under the pressure difference of the battery placement sealing cavity, so that the mass spectrometer can obtain the corresponding mass spectrum ion current of the standard gas component at the standard gas flow rate; and changing the standard gas pressure to change the leak rate of the standard leak hole, namely changing the flow rate of the standard gas, and repeating the steps to establish a standard curve between the flow rate of the standard gas component and the ion current of the mass spectrum.
The electrochemical mass spectrometer device suitable for solid-state battery gas production research/test provided by the invention meets the direct gas production test of various types (laboratory, commercial/industrial) of solid-state batteries. The standard leak hole is matched with the two pressure gauges to carry out gas quantification calibration, so that the detection accuracy is greatly improved; the vacuum pump is matched with the battery to place the impure gas in the sealing cavity and pump out the impure gas, the battery gas is directly diffused into the mass spectrometer through the pressure difference, the mass spectrometer is directly connected with the battery sealing cavity, the use of complex pipelines is reduced, the time resolution is effectively improved, the battery gas with less integral gas amount almost enters the mass spectrometer by 100 percent, the influence of a partial solid-state battery carrier gas blowing and sampling mode on the detection sensitivity and reliability is overcome, and the time resolution and the test sensitivity are ensured.
Drawings
FIG. 1 is a schematic diagram of an electrochemical mass spectrometer for gas production research of a solid-state battery according to an embodiment of the present invention;
fig. 2 is a schematic diagram of a cell-housing sealed chamber structure of an electrochemical mass spectrometry apparatus according to an embodiment of the present invention.
Detailed Description
In order that the invention may be more fully understood, preferred embodiments of the invention are now described. It should be understood that these examples are for illustrative purposes only and are not to be construed as limiting the invention in any way, i.e., not intended to limit the scope of the invention.
An exemplary junction structure of an electrochemical mass spectrometry apparatus of the invention is shown in FIG. 1, comprising:
a battery housing seal chamber 9 for housing the solid-state battery 8;
a battery test system 10 for providing parameters required for operation of the solid-state battery 8;
a calibration system for gas quantitative calibration;
a mass spectrometer 12 for analyzing the gas generated from the solid-state battery 8; the mass spectrometer 12 can carry out in-situ qualitative and quantitative analysis on the gas generated by the solid-state battery 8;
a differential pressure system for causing a pressure drop to the cell placement capsule 9 to bring the solid-state cell 8 gas to the mass spectrometer 12 by differential pressure action;
a valve group for controlling the on-off of each pipeline;
the battery test system 10, the mass spectrometer 12 and the differential pressure system are communicated with the battery placing sealing cavity 9 directly or through one or more solenoid valves in a valve group.
A plurality of interfaces for connecting with other components can be arranged on the battery placing sealing cavity 9 according to the requirement; as shown in fig. 2, an exemplary battery placing sealed cavity structure is shown, which has a hollow cavity j and a cover g, the cavity j and the cover g can form a sealed cavity for placing a solid battery 8 through a sealed cover, the cover g is provided with an interface a, an interface b, an interface c, an interface d, and an interface e for connection, the covered part between the cavity j and the cover g is further provided with a sealing gasket h, which can improve the sealing effect, and the sealing gasket h can be provided with fixing holes corresponding to an upper positioning hole f on the cover g and a lower positioning hole i on the cavity j, respectively, for installing and positioning the sealing gasket h.
The battery testing system 10 can be respectively communicated with the battery placing sealing cavity 9 through the interface a and the interface e, so that the pipelines are connected with the anode and the cathode of the solid-state battery 8, and the control and adjustment of the working parameters and the state of the solid-state battery 8 are realized.
The calibration system is an important part for realizing high-sensitivity detection, and comprises standard gas 2 communicated with the battery placing sealing cavity 9 and a pressure gauge A7 capable of directly reflecting real-time pressure in the battery placing sealing cavity 9, wherein a standard leak hole 3 is formed in an air inlet pipeline of the standard gas 2, the standard gas 2 enters the battery placing sealing cavity 9 after controlling flow through the standard leak hole 3, and the standard gas 2 is also connected with a pressure gauge B1. By comparing the pressure gauge A7 with the pressure gauge B1, the leakage rate of the standard leak hole 3 can be determined, and the standard leak hole is used for gas quantitative calibration. The invention creatively adopts the standard leak hole 3 to match with the two pressure gauges to carry out gas quantitative comparison, and because the leak rate of the standard leak hole 3 is stable and can provide the gas flow with the same magnitude as the gas production of the solid-state battery, the detection sensitivity is greatly improved, and the dilution of a large amount of carrier gas to the gas production is avoided. Meanwhile, the leakage rate of the standard leakage hole 3 can be stably changed along with the air inlet pressure, and the leakage rate of the standard leakage hole 3 can be easily adjusted by changing the pressure of the standard gas 2, so that different gas production detection requirements can be met. In addition, the standard gas 2 can be detachably connected to the gas inlet pipeline in the form of a gas tank and the like, and the requirements of different standard gas types can be met by replacing different standard gases 2.
The pressure gauge A7 is arranged in various ways, for example, the pressure gauge A7 can be communicated with the battery placing sealing cavity 9 through the interface c, and also can be arranged in the battery placing sealing cavity 9 and can display the pressure result through a display device integrally arranged on the battery placing sealing cavity 9.
The pressure difference system comprises an air exhaust device, and the air exhaust device can be a vacuum pump. The air extractor is communicated with the battery placing sealing cavity 9 through the interface d, so that air in the battery placing sealing cavity 9 is extracted to form negative pressure (differential pressure), and when pipelines of other parts such as the calibration system are in an opening state communicated with the battery placing sealing cavity 9, the air in connecting pipelines of other parts can be extracted simultaneously, and miscellaneous gas is fully discharged. The working pressure of the mass spectrometer 12 is generally in a vacuum state, when the battery placing sealing cavity 9 generates negative pressure through a pressure difference system to form pressure difference, the standard gas entering the battery placing sealing cavity 9 through the standard leak hole 3 and/or the reaction generated gas generated by the solid-state battery 8 through operation can rapidly diffuse into the mass spectrometer 12 through the pressure difference, and the generated gas completely enters the mass spectrometer at a ratio of almost 100% because the amount of the standard gas and the reaction generated gas is controlled at a low level, thereby ensuring the detection accuracy and improving the time resolution.
The valve group comprises electromagnetic valves respectively arranged on pipelines of the differential pressure system, the mass spectrometer 12 and the calibration system, and specifically can be an electromagnetic valve A5 connected with an interface d on a pipeline of the differential pressure system (vacuum pump 6), an electromagnetic valve B11 connected with an interface C on a pipeline of the mass spectrometer 12 and an electromagnetic valve C4 connected with an interface B on a pipeline of the calibration system respectively. Each pipeline is directly placed the seal chamber 9 with the battery through the solenoid valve respectively and is communicate, has reduced the use of complicacy and branch pipeline, has reduced gas diffusion path length, helps further to improve time resolution and detectivity. Each solenoid valve may be a manual valve, and is not particularly limited thereto. The port size of the valve may also be adaptively selected, such as preferably 1/8 inches or 1/16 inches, although not limited thereto.
The size of the battery housing seal chamber 9 can be modified adaptively according to the structure and size of the solid-state battery 8 to be tested.
It should be noted that the main structure and operation principle of the mass spectrometer 12 and the battery test system 10 can refer to the conventional battery test system and mass spectrometer in the prior art, and the detailed description is omitted here.
To more specifically illustrate the operation of this embodiment, the following detailed description of the test operation steps is provided with reference to the electrochemical mass spectrometer system shown in FIG. 1, as follows:
before testing, the solid-state battery 8 is generally provided with a gas outlet, so that the generated gas of the solid-state battery can be conveniently dissipated to the battery placing sealing cavity 9 to facilitate the collection of the generated gas; then, the solid-state battery 8 is placed in the battery placing sealing cavity 9 and is well connected with the battery testing system 10, and the battery placing sealing cavity 9 is covered to complete sealing connection.
Before testing, the solid-state battery 8 and the battery are placed in the sealed cavity 9, and residual air or impure gas in pipelines of the calibration system, the differential pressure system and the like is removed. Specifically, the solenoid valve B11 was closed, the solenoid valve C4 and the solenoid valve A5 were opened, the vacuum pump 6 was opened to evacuate air, and the pressure gauge A7 was observed to be lowered to a vacuum state, whereby impure gas or air in the entire apparatus was discharged. Subsequently, solenoid valve A5 and vacuum pump 6 are closed, solenoid valve B11 is opened, and the corresponding response signal of mass spectrometer 12 is observed to further determine whether the air or impurity content of the whole system has been reduced to the desired value and reaches a steady state.
After the above steps are completed, the battery placing sealing chamber 9 is in a vacuum state, and then a gas calibration step can be started to obtain a calibration factor of the tested gas. The standard gas 2 depends on the experimental test gas, and the standard leak hole 3 can determine the standard leak rate under the condition that the pressure on two sides (the pressure gauge B1 and the pressure gauge A7) is definite. Specifically, the electromagnetic valve A5 and the electromagnetic valve B11 are closed, the electromagnetic valve C4 is opened, the standard gas 2 flows through the standard leak hole 3 and the electromagnetic valve C4, reaches the battery placement sealing cavity 9, and then rapidly diffuses into the mass spectrometer 12 through the electromagnetic valve B11 under the pressure difference of the battery placement sealing cavity 9, and at this time, the mass spectrometer can obtain the corresponding mass spectrum ion current of the standard gas component at a certain standard gas flow rate; the standard gas pressure is changed to change the leak rate of the standard leak hole 3, namely the standard gas flow rate is changed, and the steps are repeated, so that a standard curve between the standard gas component flow rate (such as mu L/min) and the mass spectrum ion current can be established. Accordingly, the generation rate (mol/s, which is converted according to the standard gas molar volume) of the gas-generating component of the solid-state battery 8 can be obtained in situ according to the magnitude of the ion current, and the total output (mol) of the gas-generating component can be obtained after integration.
After the above steps are completed, the electromagnetic valve C4 is closed. And starting the battery test system 10 to connect the solid-state battery 8, so that the solid-state battery 8 starts to operate under the condition of target working parameters, and the generated gas generated in the operation process is dissipated to the battery placing sealing cavity 9 and further quickly diffused to enter the mass spectrometer 12 completely, so that the generated gas of the solid-state battery can be subjected to electrochemical mass spectrometry.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An electrochemical mass spectrometry apparatus, comprising: a battery placing sealing cavity (9) for placing the solid-state battery (8); the battery is placed sealed chamber (9) and is connected with the calibration system who is used for gaseous ration calibration, the calibration system includes places standard gas (2) of sealed chamber (9) intercommunication and can direct reaction battery and place pressure gauge A (7) of the interior real time pressure of sealed chamber (9) with the battery, be equipped with standard small opening (3) on the air inlet pipeline of standard gas (2), get into the battery after standard gas (2) pass through standard small opening (3) controlled flow and place sealed chamber (9), still be connected with pressure gauge B (1) on standard gas (2).
2. The electrochemical mass spectrometry apparatus according to claim 1, wherein the cell housing seal chamber (9) is further connected to: a battery test system (10) for providing parameters required for operation of the solid-state battery (8); a mass spectrometer (12) for analyzing the gas generated by the solid-state battery (8); a differential pressure system for generating a differential pressure to the cell placement seal chamber (9).
3. The electrochemical mass spectrometry apparatus according to claim 2, wherein the cell test system (10), the mass spectrometer (12), and the differential pressure system are each in communication with the cell placement capsule (9) either directly or indirectly through one or more solenoid valves in a valve stack.
4. The electrochemical mass spectrometry apparatus according to claim 2, wherein the pressure differential system comprises a gas evacuation device, preferably a vacuum pump (6).
5. The electrochemical mass spectrometry apparatus according to claim 2, wherein the cell placement confinement (9) is provided with an interface for connection with other components;
preferably, the battery placing sealing cavity (9) is respectively provided with an interface a and an interface e for connecting with a battery testing system (10), an interface c for connecting with a pressure gauge A (7), an interface d for connecting with a differential pressure system and an interface b for connecting with a calibration system.
6. The electrochemical mass spectrometry apparatus according to claim 2, wherein the conduits of the pressure difference system, the mass spectrometer (12) and the calibration system are respectively provided with solenoid valves for controlling the opening and closing of the communication state of each conduit with the cell placement seal chamber (9).
7. The method of performing solid state battery gassing tests of an electrochemical mass spectrometry apparatus according to any of claims 1 to 6, comprising the steps of:
s1: placing the solid-state battery (8) in a battery placing sealing cavity (9), well connecting the solid-state battery with a battery testing system (10), and closing the battery placing sealing cavity (9) to finish sealing;
s2: a differential pressure system is adopted to remove air or impure gas in a battery placing sealing cavity (9) and a pipeline including a calibration system and form differential pressure;
s3: opening a pipeline where the calibration system, the pressure gauge A (7) and the mass spectrometer (12) are located, closing other pipelines, determining the leakage rate of a standard leak hole (3) in the calibration system through the pressure gauge A (7) and a pressure gauge B (1) in the calibration system, and establishing a standard curve between the flow rate of standard gas components and the ion current of the mass spectrometer;
s4: and (3) starting a pipeline where the battery test system (10) and the mass spectrometer (12) are located, and closing other pipelines to enable the solid-state battery (8) to start to operate under the condition of target working parameters, so as to carry out electrochemical mass spectrometry on the generated gas generated in the operation process.
8. The method for performing solid-state battery gassing test according to claim 7 wherein in step S1, the solid-state battery (8) is placed in front of the battery placement chamber (9) with a vent opening reserved to facilitate gassing collection.
9. The method for performing solid-state battery gassing test on electrochemical mass spectrometry apparatus according to claim 7, wherein in step S2, solenoid valve B (11) is closed, solenoid valve C (4) and solenoid valve a (5) are opened, vacuum pump (6) is opened to draw air, pressure gauge a (7) is observed to be lowered to vacuum state, then solenoid valve a (5) and vacuum pump (6) are closed, solenoid valve B (11) is opened, and the corresponding response signal of mass spectrometer (12) is observed to determine whether the content of air or impure gas in the whole system is lowered to the desired value and reaches the steady state.
10. The method for performing the solid-state battery gas production test by using the electrochemical mass spectrometry device according to claim 7, wherein in the step S2, the electromagnetic valve A (5) and the electromagnetic valve B (11) are closed, the electromagnetic valve C (4) is opened, the standard gas (2) flows through the standard leak hole (3) and the electromagnetic valve C (4) to reach the battery placement sealing cavity (9), and then rapidly diffuses into the mass spectrometer (12) through the electromagnetic valve B (11) under the pressure difference of the battery placement sealing cavity (9), so that the mass spectrometer can obtain the corresponding mass spectrum ion current of the standard gas component at the standard gas flow rate; and changing the standard gas pressure to change the leak rate of the standard leak hole (3), namely changing the standard gas flow rate, and repeating the steps to establish a standard curve between the standard gas component flow rate and the mass spectrum ion current.
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CN116358796A (en) * | 2023-05-18 | 2023-06-30 | 天津博益气动股份有限公司 | Leakage detection method and leakage detection system for new energy power battery box |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN116358796A (en) * | 2023-05-18 | 2023-06-30 | 天津博益气动股份有限公司 | Leakage detection method and leakage detection system for new energy power battery box |
CN116358796B (en) * | 2023-05-18 | 2023-08-01 | 天津博益气动股份有限公司 | Leakage detection method and leakage detection system for new energy power battery box |
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