CN112285194B - Battery mass spectrum sampling system and battery testing device - Google Patents
Battery mass spectrum sampling system and battery testing device Download PDFInfo
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- CN112285194B CN112285194B CN202011116176.5A CN202011116176A CN112285194B CN 112285194 B CN112285194 B CN 112285194B CN 202011116176 A CN202011116176 A CN 202011116176A CN 112285194 B CN112285194 B CN 112285194B
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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
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/385—Arrangements for measuring battery or accumulator variables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0422—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for gaseous samples
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a battery mass spectrum sampling system and a battery testing device, wherein the battery mass spectrum sampling system comprises: the device comprises a battery testing device for placing a battery, a battery testing system for providing working parameters required by the battery for working, a mass spectrometer for performing mass spectrometry on the generated gas of the battery, and a carrier gas sampling system capable of bringing the generated gas of the battery to the mass spectrometer under the combined action of pressure difference and carrier gas; the battery testing device is communicated with the carrier gas sampling system only through outlet gas of the battery testing device, and the carrier gas and the produced gas are mixed in the carrier gas sampling system. The battery testing device is communicated with the carrier gas sampling system only through the gas outlet of the battery testing device, the carrier gas and the generated gas are mixed in the carrier gas sampling system, and the carrier gas sampling system brings the generated gas to the mass spectrometer through the combined action of differential pressure and the carrier gas. The battery mass spectrum sample introduction system can directly carry out differential electrochemical mass spectrum technical qualitative and quantitative in-situ analysis on high-capacity batteries such as commercial soft packages, columnar batteries and the like, and ensures the accuracy of test results.
Description
Technical Field
The invention relates to the technical field of battery testing, in particular to a battery mass spectrum sample introduction system and a battery testing device.
Background
In the working process of the battery, an electrode interface is easy to generate irreversible reaction, and combustible gases such as methane, ethylene, hydrogen and the like are released, so that the battery is failed, even is ignited and exploded, and the safety problem exists. In order to solve the safety problem caused by battery failure, the gas production condition of the battery electrode interface needs to be researched on line and the root cause of gas release needs to be analyzed.
The differential electrochemical mass spectrum is used as an online electrochemical analysis technology, and can be used for in-situ qualitative and quantitative research on consumption and release conditions of gaseous products at the battery electrode interface. The differential electrochemical mass spectrum mainly has two sample injection modes of membrane sample injection and carrier gas purging sample injection. The carrier gas purging and sample injection means that the carrier gas directly carries the electrochemical reaction generated gas to enter a mass spectrum for analysis, and is suitable for direct gas generation analysis of small model batteries suitable for laboratory scientific research.
And for carrier gas purging sample introduction, the battery is placed in the battery testing device, and carrier gas enters from the gas inlet of the battery testing device and then is discharged from the gas outlet of the battery testing device, so that the generated gas of the battery in the battery testing device is carried to enter mass spectrometry. However, the carrier gas is liable to generate eddy current in the battery test device, which results in that part of the generated gas cannot be completely carried into the mass spectrometer by the carrier gas, especially for the battery test device with large dead volume, which results in low accuracy of the test result.
In addition, if the fluctuation of the gas production rate in the unit time of the battery is larger than the fluctuation of the flow rate of the carrier gas, especially for large-capacity batteries such as commercial soft package batteries and cylindrical batteries, the gas calibration coefficient cannot be regarded as a constant, so that the test result has larger error and lower accuracy; moreover, the electrolyte consumption of large-capacity batteries such as commercial soft package batteries and columnar batteries is large, and volatile electrolyte easily enters and pollutes a mass spectrometer, so that the service life of the mass spectrometer is influenced.
In summary, how to directly perform qualitative and quantitative in-situ analysis on a battery by using a differential electrochemical mass spectrometry technology so as to be suitable for large-capacity batteries such as commercial soft-package batteries and cylindrical batteries and ensure the accuracy of a test result is a problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a battery mass spectrum sampling system which can be suitable for high-capacity batteries such as commercial soft package batteries and columnar batteries and can improve the accuracy of a test result. The invention also aims to provide a battery testing device applied to the battery mass spectrum sampling system.
In order to achieve the above purpose, the invention provides the following technical scheme:
a battery mass spectrometry sample introduction system, comprising:
a battery testing device for placing a battery,
a battery test system for providing operating parameters required for operation of the battery,
a mass spectrometer for mass spectrometric analysis of the gas produced by the cell,
a carrier gas sample injection system capable of bringing the gas produced by the cell to the mass spectrometer by the combined action of a differential pressure and a carrier gas;
wherein, carrier gas sampling system includes: the gas source, a first sample introduction pipeline communicated with the gas source and the gas outlet, a second sample introduction pipeline communicated with the mass spectrometer, an exhaust branch capable of being communicated with the first sample introduction pipeline, and an exhaust device arranged on the exhaust branch;
the second sample introduction pipeline can be communicated with the first sample introduction pipeline, and the communication position of the exhaust branch and the first sample introduction pipeline is positioned between the communication position of the second sample introduction pipeline and the first sample introduction pipeline and the gas outlet; and the carrier gas and the produced gas are mixed in the carrier gas sampling system.
Preferably, the carrier gas injection system further comprises: the first pressure gauge is connected in series with the first sample introduction pipeline, and the second pressure gauge is connected in series with the second sample introduction pipeline; wherein, the gas outlet, first pressure gauge, the second advance a kind pipeline with the intercommunication position of first advance a kind pipeline, and the mass spectrograph distributes in proper order.
Preferably, the second sample introduction pipeline is communicated with the first sample introduction pipeline through a first three-way valve, and the exhaust branch is communicated with the first sample introduction pipeline through a second three-way valve.
Preferably, the exhaust means is a vacuum pump.
Preferably, a flow regulating valve is connected in series to the exhaust branch, and the flow regulating valve is located between the exhaust branch and the first sample introduction pipeline and the exhaust device.
Preferably, the flow regulating valve is a needle valve.
Preferably, a first filter and a flowmeter are sequentially connected in series to the first sample inlet pipeline, the first filter is located at the downstream of the gas source, the flowmeter is located at the downstream of the first filter, and the flowmeter is located at the upstream of a communication position of the second sample inlet pipeline and the first sample inlet pipeline;
the second advances appearance pipeline and has concatenated second filter and cold hydrazine in proper order, the second filter is located the upper reaches of mass spectrograph, the cold hydrazine is located the second advances appearance pipeline with the low reaches of the intercommunication position of first appearance pipeline.
Based on the battery mass spectrum sample introduction system, the invention also provides a battery testing device, which is provided with: the battery testing system comprises a cavity for placing a battery, a gas outlet which is communicated with the cavity and is used for discharging gas in the cavity, and a positive electrode wiring interface and a negative electrode wiring interface which are used for realizing the electric connection of the battery and the battery testing system; wherein, the battery testing device is only communicated with the carrier gas sampling system through the gas outlet.
In the battery mass spectrum sampling system provided by the invention, the battery testing device is communicated with the carrier gas sampling system only through the gas outlet of the battery testing device, and the carrier gas and the generated gas are mixed in the carrier gas sampling system, so that the carrier gas is prevented from entering the battery testing device and generating eddy current in the battery testing device, the condition that the generated gas is not completely removed is avoided, and the accuracy of a testing result is effectively improved; in addition, the carrier gas sample introduction system brings part of the produced gas to the mass spectrometer through the combined action of the pressure difference and the carrier gas, and part of the produced gas is taken away by the exhaust device, so that the fluctuation of the produced gas of the battery is smaller relative to the flow rate of the carrier gas, and the produced gas brought into the mass spectrometer can be accurately quantified and can be extrapolated to obtain the gas production condition of the battery in unit time, thus being applicable to high-capacity batteries such as commercial soft package batteries, columnar batteries and the like, and improving the accuracy of the gas production test result of the battery; at the same time, the chance of volatile electrolyte entering and contaminating the mass spectrometer is also greatly reduced.
Meanwhile, in the battery mass spectrum sampling system provided by the invention, the carrier gas sampling system brings part of the gas generated by the carrier gas sampling system to the mass spectrometer under the combined action of the pressure difference and the carrier gas, so that continuous sampling is realized; meanwhile, under the action of negative pressure, the device can accelerate the discharge of the produced gas in the battery testing device and accelerate the produced gas to reach a mass spectrometer, thereby effectively improving the time resolution.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic diagram of a mass spectrometry sample injection system of a battery provided in an embodiment of the present invention;
fig. 2 is an exploded view of a cell testing device in a cell mass spectrometry sampling system according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, a mass spectrometry sample injection system of a battery provided by the embodiment of the present invention includes: a battery test device 114, a battery test system 115, a mass spectrometer 107, and a carrier gas injection system; the battery testing device 114 is used for placing the battery 113, the battery testing system 115 is used for providing working parameters required by the work of the battery 113, the mass spectrometer 107 is used for performing mass spectrometry on the produced gas of the battery 113, and the carrier gas sampling system can bring the produced gas of the battery 113 to the mass spectrometer 107 through the combined action of pressure difference and carrier gas.
The battery test apparatus 114 is connected to the carrier gas injection system only through the outlet gas g, and the carrier gas and the generated gas are mixed in the carrier gas injection system.
The size of the battery test apparatus 114 may be adaptively modified according to the structure and size of the battery 113 to which it is applied.
The mass spectrometer 107 performs a qualitative and quantitative differential electrochemical mass spectrometry on the gas produced by the battery 113.
It should be noted that, the main structures of the battery test device 114 and the mass spectrometer 107 and the working principles thereof can be referred to the conventional battery test device 114 and the mass spectrometer 107 respectively; the battery test system 115 is a conventional battery test system, and is not described in detail herein.
It will be appreciated that the above-described battery testing apparatus 114 is not provided with an air inlet and that the carrier gas does not enter the battery testing apparatus 114. The gas outlet g is used for discharging gas in the battery test device 114.
The carrier gas injection system brings the gas produced by the battery 113 to the mass spectrometer 107 through the combined action of the pressure difference and the carrier gas, and the carrier gas and the gas produced are mixed in the carrier gas injection system, which indicates that the carrier gas injection system has a position where the carrier gas and the gas produced are mixed.
Specifically, the carrier gas sampling system comprises: the gas source 101, a first sample introduction pipeline 116 for communicating a gas outlet g of the battery testing device 114 with the gas source 101, a second sample introduction pipeline 117 for communicating with the mass spectrometer 107, an exhaust branch 118 capable of communicating with the first sample introduction pipeline 116, and an exhaust device arranged on the exhaust branch 118;
the second sample introduction pipeline 117 can be communicated with the first sample introduction pipeline 116, and the communication position of the exhaust branch 118 and the first sample introduction pipeline 116 is located between the communication position of the second sample introduction pipeline 117 and the first sample introduction pipeline 116 and the gas outlet g.
The gas source 101 may be an argon gas source, or may be a gas source of other gases, which is not limited in this embodiment.
Specifically, the first sample introduction pipeline 116 includes: the air outlet pipeline and the air supply pipeline are communicated; wherein, the gas outlet pipeline is communicated with the gas outlet g, and the gas supply pipeline is communicated with the gas source 101; the second sample feeding pipeline 116 is connected to the communication position of the gas outlet pipeline and the gas supply pipeline, namely, both the gas outlet pipeline and the gas supply pipeline can be communicated with the second sample feeding pipeline 116; the exhaust branch 118 is disposed on the exhaust line and is in communication with the exhaust line.
It will be appreciated that the carrier gas and the generated gas begin to mix at the connection between the gas outlet line and the gas supply line, thereby enabling the carrier gas to carry the generated gas into the second sample inlet line 117 and thus into the mass spectrometer 107.
The exhaust device generates a negative pressure by exhausting air, so that the first sample introduction pipe 116 can be conducted to the second sample introduction pipe 117. Specifically, by adjusting the exhaust device, the pressure in the exhaust branch 118 and the gas outlet pipeline communicated with the exhaust branch 118 is changed, so that the pressure in the gas outlet pipeline is greater than the pressure in the second sample inlet pipeline 116, so that the gas in the battery testing device 114 enters the second sample inlet pipeline 116, and the gas in the gas supply pipeline enters the second sample inlet pipeline 116.
In the battery mass spectrum sampling system provided by the invention, the battery testing device 114 is communicated with the carrier gas sampling system only through the gas outlet g of the battery testing device, and the carrier gas and the generated gas are mixed in the carrier gas sampling system, so that the carrier gas is prevented from entering the battery testing device 114 and generating eddy current in the battery testing device 114, the condition that the generated gas is not completely eliminated is avoided, and the accuracy of a testing result is effectively improved; moreover, the carrier gas sample introduction system brings part of the produced gas to the mass spectrometer 107 through the combined action of differential pressure and carrier gas, the produced gas brought to the mass spectrometer 107 can be accurately quantified and can be extrapolated to obtain the gas production condition of the soft package battery in unit time, the gas production system can be suitable for large-capacity batteries such as commercial soft package batteries and columnar batteries, and the accuracy of the gas production test result of the battery is improved; the chance of volatile electrolyte entering and contaminating mass spectrometer 107 is also greatly reduced.
The large-capacity battery is a battery having a capacity not smaller than the capacity of a commercial pouch battery and the capacity of a cylindrical battery.
Meanwhile, in the battery mass spectrum sampling system, the carrier gas sampling system brings part of the generated gas to the mass spectrometer 107 through the combined action of the pressure difference and the carrier gas, so that continuous sampling is realized; meanwhile, under the action of negative pressure, the discharge of the produced gas in the battery testing device 114 can be accelerated, the produced gas can be accelerated to reach a mass spectrometer, and the time resolution is effectively improved.
Meanwhile, in the cell mass spectrum sample introduction system, the cell testing device 114 is only provided with the gas outlet g to be communicated with the carrier gas sample introduction system, so that the structure of the cell testing device is simplified, corresponding pipelines are reduced, the whole cell mass spectrum sample introduction system is simplified, and the cost is reduced.
The battery mass spectrum sample introduction system can effectively couple the gas generated by the battery 113 into the mass spectrum gas circuit through the battery testing device 114, so that the gas generation condition of the battery can be directly subjected to online qualitative and quantitative analysis by adopting a differential electrochemical mass spectrum technology. Preferably, the battery 113 is a commercial pouch battery or a cylindrical battery. Specifically, the battery mass spectrum sampling system can perform online qualitative and quantitative analysis on the gas production condition of commercial soft package batteries or cylindrical batteries which are commercially available and suitable for research and development in the market.
In order to facilitate pressure acquisition, the carrier gas injection system further comprises: a first pressure gauge 109 connected in series to the first sample introduction pipe 116, and a second pressure gauge 108 connected in series to the second sample introduction pipe 117; the gas outlet g, the first pressure gauge 109, the communication position of the second sample inlet pipeline 117 and the first sample inlet pipeline 116, and the mass spectrometer 107 are distributed in sequence.
In the application process, the pressure value detected by the first pressure gauge 109 is greater than the pressure value detected by the second pressure gauge 108 by exhausting through the exhaust device, so that the gas in the battery testing device 114 is discharged from the gas outlet g to enter the first sample inlet pipeline 116, and then enters the second sample inlet pipeline 117.
The types of the first pressure gauge 109 and the second pressure gauge 108 are selected according to actual needs, and this embodiment does not limit this.
To facilitate the communication of the lines and reduce the number of valves, the second sample line 117 is communicated with the first sample line 116 through the first three-way valve 104, and the exhaust branch 118 is communicated with the first sample line 116 through the second three-way valve 110.
Specifically, the first three-way valve 104 is connected in series to the first sample introduction pipeline 116 through a first inlet port and a second inlet port thereof, the first inlet port is close to the gas source 101, the second inlet port is close to the gas outlet g, an outlet port of the first three-way valve 104 is communicated with the second sample introduction pipeline 117, when the first three-way valve 104 is at the first valve position, a pipeline through which the first inlet ports of the first sample introduction pipeline 116 and the first three-way valve 104 are communicated is communicated with the second sample introduction pipeline 117, and a pipeline through which the second inlet ports of the first sample introduction pipeline 116 and the first three-way valve 104 are communicated is communicated with the second sample introduction pipeline 117.
For example, when the first sample inlet pipeline 116 includes an air outlet pipeline and an air inlet pipeline which are communicated with each other, the air inlet pipeline is communicated with the first inlet valve port of the first three-way valve 104, the air outlet pipeline is communicated with the second inlet valve port of the first three-way valve 104, and when the first three-way valve 104 is at the first valve position, both the air outlet pipeline and the air inlet pipeline are communicated with the second sample inlet pipeline 117.
The second three-way valve 110 has an inlet port, a first outlet port, and a second outlet port, the second three-way valve 110 is connected in series to the first sample line 116 through the inlet port and the first outlet port, and the second outlet port of the second three-way valve 110 is communicated with the exhaust branch 118. When the second three-way valve 110 is at the first valve position, the inlet port of the second three-way valve 110 is communicated with the first outlet port, and the inlet port of the second three-way valve 110 is communicated with the second outlet port.
The first three-way valve 104 and the second three-way valve 110 may have other valve positions, and are not limited to the first valve position described in the above embodiment.
The pressure in the air outlet pipeline can be adjusted through air exhaust by the exhaust device, and the specific type of the exhaust device is selected according to actual needs. Specifically, the exhaust device exhausts air to the external environment.
Meanwhile, the battery mass spectrum sampling system can discharge part of the generated gas by using the exhaust branch 118 and the exhaust device, so that the fluctuation of the gas flow entering the second sampling pipeline 117 is small, namely the fluctuation of the gas flow entering the mass spectrometer 107 is small relative to the fluctuation of the carrier gas, and meanwhile, the gas brought into the mass spectrometer 107 can be accurately quantified and extrapolated to obtain the battery gas generation condition in unit time, thereby improving the accuracy of the battery gas generation test result and greatly reducing the possibility that volatile electrolyte enters and pollutes the mass spectrometer 107.
It should be noted that the proportion of the gas generated by the battery 113 and carried away by the exhaust device can be calibrated by the standard gas. The calibration procedure may refer to prior art differential electrochemical mass spectrometry calibration procedures. Therefore, the gas ratio of the generated gas of the battery 113 entering the mass spectrometer 107 can be known, and the gas generation amount of the battery 113 per unit time can be calculated according to the effective volume V of the battery testing device 114. The effective volume V is the difference between the volume of the battery test apparatus 114 and the volume of the battery 113.
Further, the exhaust and exhaust device is a vacuum pump 112. Of course, the exhaust device may be other devices or structures, such as an exhaust valve, and is not limited to the above embodiment.
For convenience of adjustment, a flow regulating valve is connected in series on the exhaust branch 118, and the flow regulating valve is located between the exhaust branch 118 and the first sample introduction pipeline 116 and the exhaust device.
In the mass spectrum sample introduction system for the battery, the flow in the exhaust branch 118 is adjusted through the flow adjusting valve, so that the generated gas is convenient to enter the second sample introduction pipeline 117, the flow of the generated gas entering the second sample introduction pipeline 117 is convenient to keep stable, and the fluctuation of the gas flow is reduced; meanwhile, the gas production rate entering the second sample inlet pipeline 117 is also reduced, so that the amount of electrolyte entering the mass spectrometer 107 is reduced, the damage to the mass spectrometer 107 is reduced, and the service life of the mass spectrometer 107 is prolonged.
Preferably, the flow rate control valve is a needle valve 111. Of course, the flow regulating valve may also be another type of valve, which is not limited in this embodiment.
Preferably, the first sample introduction pipeline 116 is connected in series with a first filter 102 and a flow meter 103 in sequence, the first filter 102 is located downstream of the gas source 101, the flow meter 103 is located downstream of the first filter 102, and the flow meter 103 is located upstream of a communication position of the second sample introduction pipeline 117 and the first sample introduction pipeline 116. In this way, the carrier gas is filtered by the first filter 102, and the flow of the carrier gas is adjusted by the flow meter 103, so that the carrier gas is carried with the generated gas and enters the mass spectrometer 107.
It will be appreciated that the gas source 101, the first filter 102 and the flow meter 103 are arranged in sequence.
Preferably, the second sample introduction pipeline 117 is connected in series with a second filter 106 and a cold trap 105 in sequence, the second filter 106 is located upstream of the mass spectrometer 107, and the cold trap 105 is located downstream of a communication position of the second sample introduction pipeline 117 and the first sample introduction pipeline 116.
It will be appreciated that the cold trap 105, the second filter 106 and the mass spectrometer 107 are arranged in sequence.
In practical applications, other components may be connected in series to the first sample inlet line 116, the second sample inlet line 117, and the exhaust branch 118, and are not limited to the above embodiments.
In each of the above embodiments, the size of the interface of the first filter 102 and the second filter 106 is not particularly limited, for example, the size of the interface of the first filter 102 and the second filter 106 may be preferably 1/8 inches or 1/16 inches, and the filter element pore size of the first filter 102 and the second filter 106 may be preferably 2 μm.
In addition, the needle valve 111 may be a solenoid valve or a manual valve, which is not particularly limited. The port size of the needle valve 111 is preferably 1/8 inches or 1/16 inches. Of course, the port size of the needle valve 111 may be selected to be other, and is not limited thereto.
Accordingly, the interface size of the flow meter 103 is preferably 1/8 inches or 1/16 inches. The flow rate of the flow meter 103 preferably ranges from 0 to 500 mL/min. Of course, the port size and flow range of the flow meter 103 may be selected to be other, and is not limited thereto.
The refrigeration mode of the cold trap 105 is electric refrigeration, liquid nitrogen refrigeration or dry ice refrigeration, and the refrigeration temperature of the cold trap 105 is less than-20 ℃.
To illustrate the present embodiment more specifically, the following describes the testing steps according to the mass spectrometer sample injection system of the battery shown in fig. 1, specifically, the testing steps are as follows:
before testing, a small opening is cut on the battery 113, so that the produced gas can be conveniently collected; then, placing the battery 113 with the cut in a battery testing device 114, assembling the battery testing device 114, and connecting the assembled battery testing device 114 to a carrier gas sample injection system;
before the test, the air or impure gas remaining in each line of the battery test device 114 and the carrier gas sampling system is removed, and specifically, the opening degree of the needle valve 111 is adjusted to a proper position to ensure that the pressure of the second pressure gauge 108 is lower than that of the first pressure gauge 109. Thus, the air and impure gas in the battery test equipment 114 and the outlet line will flow to the first three-way valve 104 by the pressure differential. The carrier gas provided by the gas source 101 sequentially passes through the first filter 102, the flowmeter 103 and the first three-way valve 104, and carries residual air and impure gas discharged from the battery testing device 114 and the gas outlet pipeline 116 to continuously flow to the cold trap 105 and the second filter 106, and finally reaches the mass spectrometer 107; observing a corresponding response signal of the mass spectrometer 107 until the components of the residual air and the impure gas in the gas circuit are reduced to ideal values and reach a stable state, and considering that the residual air and the impure gas in the battery mass spectrum sampling system are removed;
after the above steps are completed, the battery test system 115 may be started to perform electrochemical mass spectrometry on the produced gas of the battery 113.
Based on the battery mass spectrum sample introduction system provided by the above embodiment, the embodiment of the present invention further provides a battery testing device, as shown in fig. 1 and fig. 2, the battery testing device is provided with: the battery testing system comprises a cavity for placing the battery 113, a gas outlet g which is communicated with the cavity and is used for exhausting gas in the cavity, and a positive electrode wiring interface e and a negative electrode wiring interface f which are used for realizing the electric connection between the battery 113 and the battery testing system 115; wherein, the battery testing device is only communicated with the carrier gas sampling system through the gas outlet g.
It will be appreciated that the above described cell testing device is not provided with an air inlet and that the carrier gas does not enter the cell testing device. The battery testing device provided by the embodiment is communicated with the carrier gas sampling system by only arranging the gas outlet g, and only part of battery gas production is carried into the mass spectrometer for analysis, so that the large fluctuation of the battery gas production relative to the carrier gas flow is reduced, the battery gas production condition in unit time can be extrapolated, the accuracy of the battery gas production testing result is improved, and the opportunity that volatile electrolyte enters and pollutes the mass spectrum is greatly reduced; meanwhile, the battery testing device is only provided with the air outlet g to be communicated with the carrier gas sampling system, so that the structure of the battery testing device is simplified, and the cost is reduced. Specifically, the battery test apparatus includes: a shell j for placing the battery 113, and a cover plate i detachably connected with the shell j in a sealing way; wherein, the air outlet g is arranged on the shell j and/or the cover plate i; the positive wiring interface e is arranged on the shell j and/or the cover plate i, and the negative wiring interface f is arranged on the shell j and/or the cover plate i.
In order to facilitate installation and disassembly, the cover plate i is positioned at the top end of the shell j, and the air outlet g, the positive wiring interface e and the negative wiring interface f are all arranged on the cover plate i.
In order to facilitate the sealing connection between the cover plate i and the shell j, the cover plate i and the shell j are preferably connected in a sealing manner through a sealing ring h. The type of the sealing ring h is selected according to actual needs, and this embodiment does not limit this.
Of course, the cover plate i and the housing j may be connected by other components or structures, and are not limited to the above limitation.
The cover plate i is detachably connected with the shell j in a sealing mode, and the specific structure of the detachable connection is selected according to actual needs. For the convenience of mounting and dismounting, the cover plate i is preferably detachably connected with the shell j through a threaded connector. Specifically, the threaded connector is a bolt. And threaded holes d matched with the bolts in a threaded manner are respectively arranged at the positions of the cover plate i corresponding to the shell j. The number and distribution of the bolts are selected according to actual needs, and this embodiment does not limit this.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A battery mass spectrometry sample introduction system is characterized by comprising:
a battery test device (114) for placing a battery (113),
a battery test system (115) for providing the battery (113) with operating parameters required for operation,
a mass spectrometer (107) for mass spectrometric analysis of the gas produced by the battery (113),
a carrier gas injection system capable of bringing the gas output of the cell (113) to the mass spectrometer (107) by the combined action of a pressure differential and a carrier gas;
wherein, carrier gas sampling system includes: the device comprises a gas source (101), a first sample inlet pipeline (116) which is communicated with a gas outlet (g) of the battery testing device (114) and the gas source (101), a second sample inlet pipeline (117) which is communicated with the mass spectrometer (107), an exhaust branch (118) which can be communicated with the first sample inlet pipeline (116), and an exhaust device which is arranged on the exhaust branch (118);
the second sample feeding pipeline (117) can be communicated with the first sample feeding pipeline (116), and the communication position of the exhaust branch (118) and the first sample feeding pipeline (116) is positioned between the communication position of the second sample feeding pipeline (117) and the first sample feeding pipeline (116) and the gas outlet (g); the carrier gas and the produced gas are mixed in the carrier gas sampling system;
the communication position of the second sample feeding pipeline (117) and the first sample feeding pipeline (116) is positioned between the communication position of the exhaust branch (118) and the first sample feeding pipeline (116) and the gas source (101);
the first sample introduction line (116) comprises: the air outlet pipeline and the air supply pipeline are communicated; wherein the gas outlet pipeline is communicated with the gas outlet (g), and the gas supply pipeline is communicated with the gas source (101); the second sample injection pipeline (117) is connected to the communication position of the gas outlet pipeline and the gas supply pipeline, and both the gas outlet pipeline and the gas supply pipeline can be communicated with the second sample injection pipeline (117); the exhaust branch (118) is arranged on the air outlet pipeline and communicated with the air outlet pipeline;
partial produced gas can be discharged by using the exhaust branch (118) and the exhaust device, and the pressure in the gas outlet pipeline can be adjusted by the exhaust device through exhaust;
the battery (113) is a commercial soft package battery or a cylindrical battery.
2. The battery mass spectrometry sample introduction system of claim 1, wherein the carrier gas sample introduction system further comprises: a first pressure gauge (109) connected in series to the first sample introduction pipe (116), and a second pressure gauge (108) connected in series to the second sample introduction pipe (117); wherein, the gas outlet (g), the first pressure gauge (109), the second sample pipeline (117) and the communicating position of the first sample pipeline (116) and the mass spectrometer (107) are distributed in sequence.
3. The battery mass spectrometry sample introduction system according to claim 1, wherein the second sample introduction line (117) is communicated with the first sample introduction line (116) through a first three-way valve (104), and the exhaust branch (118) is communicated with the first sample introduction line (116) through a second three-way valve (110).
4. The battery mass spectrometry sample introduction system of claim 1, wherein the exhaust device is a vacuum pump (112).
5. The battery mass spectrometry sample introduction system according to claim 1, wherein a flow regulating valve is connected in series to the exhaust branch (118), and the flow regulating valve is located between a communication position of the exhaust branch (118) and the first sample introduction pipeline (116) and the exhaust device.
6. The system of claim 5, wherein the flow regulating valve is a needle valve (111).
7. The battery mass spectrometry sample introduction system of any one of claims 1-6,
a first filter (102) and a flow meter (103) are sequentially connected to the first sample feeding pipeline (116) in series, the first filter (102) is located at the downstream of the gas source (101), the flow meter (103) is located at the downstream of the first filter (102), and the flow meter (103) is located at the upstream of the communication position of the second sample feeding pipeline (117) and the first sample feeding pipeline (116);
second filter (106) and cold hydrazine (105) have concatenated in proper order on second appearance pipeline (117), second filter (106) are located the upper reaches of mass spectrograph (107), cold hydrazine (105) are located second appearance pipeline (117) with the low reaches of the intercommunication position of first appearance pipeline (116).
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| CN113433192B (en) * | 2021-06-23 | 2023-06-02 | 天目湖先进储能技术研究院有限公司 | Full-automatic electrochemical mass spectrometry system |
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