CN112285193B - Battery mass spectrum sampling system - Google Patents
Battery mass spectrum sampling system Download PDFInfo
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- CN112285193B CN112285193B CN202011116172.7A CN202011116172A CN112285193B CN 112285193 B CN112285193 B CN 112285193B CN 202011116172 A CN202011116172 A CN 202011116172A CN 112285193 B CN112285193 B CN 112285193B
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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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- 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
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Abstract
The invention discloses a battery mass spectrum sample introduction system, which comprises: the battery testing device is used for placing a battery, the battery testing system is used for providing working parameters required by the work of the battery, the mass spectrometer is used for performing mass spectrum analysis on the produced gas of the battery, the exhaust device can exhaust the produced gas of the battery, and the carrier gas sampling system can carry the produced gas of the battery to the mass spectrometer and the exhaust device through carrier gas; wherein, carrier gas sampling system includes: the valve assembly is a first sample introduction pipeline communicated with the gas outlet of the battery testing device; the first sample introduction pipeline comprises a first branch and a second branch, the first branch is communicated with the mass spectrometer, the second branch is communicated with the exhaust device, and the valve assembly is used for controlling the on-off and the flow of the first branch and the second branch. The battery mass spectrum sampling system can be suitable for high-capacity batteries such as commercial soft package batteries and columnar batteries, and the accuracy of a battery gas production test result is ensured.
Description
Technical Field
The invention relates to the technical field of battery testing, in particular to a battery mass spectrum sampling system which can be suitable for high-capacity batteries such as commercial soft package batteries and columnar batteries.
Background
In the working process of the battery, an electrode/electrolyte 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 subjected to fire explosion, 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/in-situ 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 introduction modes of membrane sample introduction and carrier gas purging. The membrane sample introduction requires that an electrochemical device is directly connected to a mass spectrum sample introduction port through a flange, a polytetrafluoroethylene membrane is used for separating an electrolyte from the mass spectrum vacuum sample introduction port, and generated gas/volatile products are diffused into a mass spectrum through pressure difference for analysis. Therefore, the battery needs special design to meet the use requirement, and the polytetrafluoroethylene membrane can not effectively isolate the organic electrolyte from the mass spectrum vacuum injection port. The carrier gas purging can directly carry the electrochemical reaction generated gas to enter a mass spectrum for analysis, and an electrochemical system and a sample injection system are relatively independent, so the carrier gas purging sample injection mode is often used for the analysis of the generated gas of the battery.
The existing carrier gas purging and sampling system is only suitable for small model batteries suitable for laboratory scientific research and cannot be directly coupled with actual batteries, particularly large-capacity batteries such as commercial soft package batteries and columnar batteries. In addition, if the high-capacity batteries such as commercial soft package batteries and columnar batteries are directly coupled on the premise of not changing a carrier gas purging and sampling system, the fluctuation of the gas production rate of the high-capacity batteries in unit time is larger than the carrier gas flow, and the accuracy of a test result cannot be ensured if a gas calibration coefficient cannot be regarded as a constant. In addition, the electrolyte consumption of large-capacity batteries such as commercial soft packages and columnar batteries is large, and the carrier gas purging is easy to carry volatilized electrolyte to enter and pollute the mass spectrometer.
In summary, a problem to be solved by those skilled in the art is how to provide a mass spectrometry sample injection system for a battery, which is suitable for a large-capacity battery such as a commercial pouch battery and a cylindrical battery, and ensures accuracy of a test result.
Disclosure of Invention
The invention aims to provide a battery mass spectrum sampling system which is suitable for large-capacity batteries such as commercial soft package batteries and columnar batteries and ensures the accuracy of a test result.
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 gas produced by a battery,
an exhaust device capable of exhausting the gas generated by the battery,
a carrier gas injection system capable of carrying the cell gas production to the mass spectrometer and the exhaust;
wherein, carrier gas sampling system includes: the valve assembly is a first sample feeding pipeline communicated with the gas outlet of the battery testing device; the first sample introduction pipeline comprises a first branch and a second branch, the first branch is communicated with the mass spectrometer, the second branch is communicated with the exhaust device, and the valve assembly is used for controlling the on-off and flow of the first branch and the second branch.
Preferably, the exhaust means is a vacuum pump.
Preferably, the valve assembly comprises: the three-way valve is connected in series with a first valve on the first branch and a second valve on the second branch; the inlet valve port of the three-way valve is communicated with the air outlet, and the two outlet valve ports of the three-way valve are respectively communicated with the first branch and the second branch.
Preferably, the second valve is a needle valve.
Preferably, the first valve is a leakage valve, the first branch is connected in series with a first pressure gauge and a second pressure gauge, the first pressure gauge is located at the upstream of the leakage valve, and the second pressure gauge is located at the downstream of the leakage valve.
Preferably, the first branch is connected in series with a cold trap and a first filter in sequence; wherein the cold trap is located downstream of the three-way valve, the first filter is located downstream of the cold trap, the first valve is located downstream of the first filter, and the mass spectrometer is located downstream of the first valve.
Preferably, the battery mass spectrometry sample introduction system further comprises: and the second sample inlet pipeline is communicated with the air inlet of the battery testing device, and an air source, a second filter and a flowmeter are sequentially connected in series on the second sample inlet pipeline, wherein the flowmeter is close to the air inlet of the battery testing device.
Preferably, the battery mass spectrometry sample introduction system further comprises a fan arranged in the battery testing device.
Preferably, the number of the fans is at least two, and the fans are uniformly distributed in the battery testing device;
and/or the fan is an electric fan, the battery testing device is provided with a wire passing hole for allowing a power wire of the power supply fan to penetrate out, and the power wire is hermetically connected with the wire passing hole.
Preferably, the battery test apparatus includes: the battery cover comprises a shell for placing a battery and a cover plate which is detachably connected with the shell in a sealing manner;
wherein, the air outlet of the battery testing device is arranged on the shell and/or the cover plate;
the shell and/or the cover plate are/is provided with a positive electrode wiring interface and a negative electrode wiring interface which are used for realizing the electric connection between the battery and the battery testing system.
According to the battery mass spectrum sample introduction system provided by the invention, the first sample introduction pipeline communicated with the gas outlet of the battery testing device is divided into the first branch and the second branch, the exhaust device is arranged, so that the first branch is communicated with the mass spectrometer, the second branch is communicated with the exhaust device, and the valve assembly is utilized to control the on-off and flow of the first branch and the second branch. Therefore, partial produced gas can be discharged by utilizing the second branch and the exhaust device, so that only partial produced gas enters the mass spectrometer, and the fluctuation of the produced gas entering the mass spectrometer can be reduced; moreover, the flow rate of the produced gas entering the mass spectrometer can be controlled, so that the fluctuation of the produced gas entering the mass spectrometer can be reduced. Therefore, the battery mass spectrum sampling system can be suitable for large-capacity batteries such as commercial soft package batteries and cylindrical batteries, and the accuracy of a test result is ensured.
Meanwhile, the battery mass spectrum sample introduction system provided by the invention can accelerate the produced gas to enter a mass spectrometer by regulating the flow and discharging part of the produced gas, so that the time resolution is improved; the discharged part of the produced gas also reduces the chance of the electrolyte volatilization to pollute the mass spectrometer, and prolongs the service life of the mass spectrometer.
In addition, according to the battery mass spectrum sample introduction system provided by the invention, the first pressure gauge, the second pressure gauge and the leakage valve are adopted to accurately control the gas flow entering the mass spectrometer, so that the fluctuation of the gas flow flowing through the second branch is further small, the influence on the quantitative analysis of the gas of the mass spectrometer caused by the large gas production rate of the battery in unit time is avoided, and meanwhile, the accurate gas production rate of the battery in unit time can be extrapolated by analyzing the gas flow entering the mass spectrometer. Therefore, the battery mass spectrum sampling system not only protects the mass spectrometer, but also reduces the error of the test result and improves the accuracy of the test result. And moreover, by adopting the leakage valve, continuous sample introduction is realized, the test continuity is ensured, and the time resolution and the accuracy of a test result are improved.
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 a schematic structural diagram of a battery testing device in a battery mass spectrometry sampling system provided in an embodiment of the present invention;
fig. 3 is a sectional view of a housing of the battery test apparatus shown in fig. 2.
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, the system for sampling a mass spectrum of a battery provided by the embodiment of the present invention includes: battery test equipment 105, battery test system 106, mass spectrometer 115, exhaust, and carrier gas injection system.
The battery testing device 105 is used for placing the battery 104, the battery testing system 106 is used for providing working parameters required by the operation of the battery 104, the mass spectrometer 115 is used for performing mass spectrometry on the generated gas of the battery 104, the exhaust device can exhaust the generated gas of the battery 104, and the carrier gas sampling system can bring the generated gas of the battery 104 to the mass spectrometer 115 and the exhaust device through carrier gas.
Specifically, the carrier gas sampling system comprises: a valve assembly, a first sample inlet pipeline 116 communicated with the gas outlet e of the battery testing device 105; the first sample inlet line 116 includes a first branch 117 and a second branch 118, the first branch 117 is communicated with the mass spectrometer 115, the second branch 118 is communicated with the exhaust device, and the valve assembly is used for controlling the on-off and flow of the first branch 117 and the second branch 118.
The size of the battery test apparatus 105 may be adaptively modified according to the structure and size of the battery 104 to which it is applied.
The mass spectrometer 115 performs a differential electrochemical mass spectrometry qualitative and quantitative analysis on the gas produced by the battery 104.
It should be noted that, the main structures of the battery test apparatus 105 and the mass spectrometer 115 and the working principle thereof may refer to the structures of the conventional battery test apparatus 105 and the mass spectrometer 115 in the prior art, respectively, and are not described herein again.
The battery mass spectrum sample introduction system can effectively couple the gas generated by the battery 104 into the mass spectrum gas path through the battery test device 105, 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 104 is a commercial pouch battery or a cylindrical battery.
According to the sample injection system for the battery mass spectrometry provided by the embodiment of the invention, the first sample injection pipeline 116 communicated with the gas outlet e of the battery testing device 105 is divided into the first branch 117 and the second branch 118, and the exhaust device is arranged, so that the first branch 117 is communicated with the mass spectrometer 115, the second branch 118 is communicated with the exhaust device, and the valve assembly is used for controlling the make-and-break and the flow of the first branch 117 and the second branch 118. Therefore, partial generated gas can be discharged by using the second branch 118 and the exhaust device, so that only partial generated gas enters the mass spectrometer 115, and fluctuation of the generated gas entering the mass spectrometer 115 can be reduced; furthermore, the flow rate of the produced gas into the mass spectrometer 115 can be controlled, so that fluctuations in the gas production into the mass spectrometer 115 can be reduced. Therefore, the battery mass spectrum sampling system can be suitable for large-capacity batteries such as commercial soft package batteries and cylindrical batteries, and the accuracy of a test result is ensured.
Meanwhile, the battery mass spectrum sample introduction system provided by the embodiment can accelerate the produced gas to enter the mass spectrometer 115 by adjusting the flow and discharging part of the produced gas, so that the time resolution is improved; the discharged portion of the gas also reduces the chance of electrolyte volatilization contaminating the mass spectrometer 115, extending the life of the mass spectrometer 115.
The battery mass spectrum sampling system can perform online qualitative and quantitative analysis on the gas production condition of the commercial and developed and applicable soft package battery or cylindrical battery in the market.
The exhaust device may be an exhaust port or an exhaust pump. For the convenience of evacuation, the evacuation device is preferably a vacuum pump 109. The type of the vacuum pump 109 is selected according to actual needs, and this embodiment is not limited to this.
The above valve assembly is used to control the opening and closing of the first branch 117 and the second branch 118, and the flow rate, it can be understood that the first branch 117 can be opened and closed independently, and the second branch 118 can be opened and closed independently.
The specific type and construction of the valve assembly is selected according to the actual needs. To facilitate adjustment of the first branch 117 and the second branch 118, it is preferred that the valve assembly comprises: a three-way valve 107, a first valve connected in series to the first branch 117, and a second valve connected in series to the second branch 118; the inlet port a of the three-way valve 107 is communicated with the outlet port e of the battery testing device 105, and the three-way valve 107 is communicated with the first branch 117 and the second branch 118 respectively.
The two outlet ports are respectively a first outlet port c and a second outlet port b, the first outlet port c is communicated with the first branch 117, and the second outlet port b is communicated with the second branch 118.
Specifically, when the three-way valve 107 is in the first valve position, the three-way valve 107 connects the air outlet e of the battery testing device 105 and the first branch 117, and the air outlet e of the battery testing device 105 and the second branch 118; when the three-way valve 107 is in the second valve position, the three-way valve 107 disconnects the air outlet e of the battery test device 105 from the first branch 117 and disconnects the air outlet e of the battery test device 105 from the second branch 118. Of course, the three-way valve 107 may also have a third valve position and a fourth valve position, and when the three-way valve 107 is in the third valve position, the three-way valve 107 connects the air outlet e of the battery testing apparatus 105 and the first branch 117, and disconnects the air outlet e of the battery testing apparatus 105 and the second branch 118; when the three-way valve 107 is in the fourth valve position, the three-way valve 107 connects the air outlet e of the battery testing device 105 with the first branch 117 and connects the air outlet e of the battery testing device 105 with the second branch 118.
The specific type of the three-way valve 107 is selected according to actual needs, and this embodiment is not limited to this.
The three-way valve 107 controls the opening and closing of the first branch 117 and the second branch 118, and the flow rate.
The first valve is used to control the flow rate of the first branch 117, and the second valve is used to control the flow rate of the second branch 118. The specific types of the first valve and the second valve are selected according to actual needs.
Preferably, the second valve is a needle valve 108, which accelerates the gas flow, thereby accelerating the gas generation into the mass spectrometer 115, and further improving the time resolution. Of course, the second valve may be of other types, which is not limited in this embodiment.
Preferably, the first valve is a leakage valve 113, the first branch 117 is connected in series with a first pressure gauge 112 and a second pressure gauge 114, the first pressure gauge 112 is located upstream of the leakage valve 113, and the second pressure gauge 114 is located downstream of the leakage valve 113.
It should be noted that, the remaining volume after the battery testing apparatus 105 is placed into the battery 104 is defined as V, and the leak rate of the leak valve 113 is known, for example, the leak rate of the leak valve 113 is 10uL/min, so that the proportion of the generated gas of the battery 104 entering the mass spectrum can be inferred, and the gas generation rate of the battery 104 per unit time can be further deduced.
In the battery mass spectrum sampling system, the flow of gas entering the mass spectrometer 115 is accurately controlled by using the first pressure gauge 112, the second pressure gauge 114 and the leakage valve 113, and residual gas is discharged by carrier gas through the second branch 118 and the exhaust device, so that the problem of mass spectrum pollution caused by electrolyte volatilization is reduced. Thus, the gas flow entering the mass spectrometer 115 is precisely controlled, the gas flow is not fluctuated basically, so that the gas calibration coefficient can be regarded as a constant, the gas production condition of the battery can be extrapolated by quantitatively introducing the gas production into the mass spectrometer 115, the error of the test result is reduced, the accuracy of the test result is improved, and the mass spectrometer 115 is protected. Moreover, the leakage valve 113 is adopted, so that continuous sample introduction is realized, the test continuity is ensured, and the time resolution and the accuracy of a test result are improved.
In the sample introduction system for the battery mass spectrum, part of gas generated by the battery 104 is taken away from the carrier gas system through the needle valve 108 and the vacuum pump 109, and part of generated gas enters the mass spectrometer 115 through the leakage valve 113, so that the increase of quantitative errors caused by the large fluctuation range of the gas generated in unit time of the battery can be effectively avoided; at the same time, because less gas enters mass spectrometer 115 through leak valve 113, the chance of volatile electrolyte entering and contaminating mass spectrometer 115 is reduced.
In the above-mentioned sample introduction system for mass spectrometry of battery, the opening degree of the needle valve 108 is adjusted, the pressure reading before entering the leakage valve 113, that is, the reading of the first pressure gauge 112, can adjust the leakage rate of the leakage valve 113, thereby controlling the gas flow entering the mass spectrometer 115.
In addition, the needle valve 108 and the leak valve 113 may be solenoid valves or manual valves, which are not particularly limited. The port size of the needle valve 108 and the leak valve 113 is preferably 1/8 inches or 1/16 inches. The leakage rate of the leakage valve 113 is preferably 1uL/min to 50 uL/min. Of course, other values of the above parameters of the needle valve 108 and the leak valve 113 may be selected, and are not limited to the above embodiments.
The first branch 117 is connected in series with a cold trap 110 and a first filter 111 in sequence; wherein the cold trap 110 is located downstream of the three-way valve 107, the first filter 111 is located downstream of the cold trap 110, the first valve is located downstream of the first filter 111, and the mass spectrometer 115 is located downstream of the first valve.
The refrigeration mode of the cold trap is electric refrigeration, liquid nitrogen refrigeration or dry ice refrigeration, and the refrigeration temperature is less than-20 ℃.
In order to facilitate the carrier gas sample injection, the carrier gas sample injection system further comprises: and the second sample introduction pipeline 119 is communicated with the gas inlet h of the battery testing device 105, and the gas source 101 is connected to the second sample introduction pipeline 119 in series.
In the above-mentioned sample injection system for battery mass spectrum, the gas inlet h and the gas outlet e of the battery test device 105 are connected with the carrier gas sample injection system, so that the gas generated by the battery 104 in the battery test device 105 is brought into the mass spectrometer 115 by the carrier gas, and the gas generated by the battery can be analyzed by the mass spectrometer 115.
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.
Preferably, the second filter 102 and the flow meter 103 are connected in series to the second sample inlet line 119 in sequence, wherein the flow meter 103 is close to the gas inlet h of the battery testing device 105.
It is to be understood that, in the above-described embodiment, the size of the interface of the first filter 111 and the second filter 102 is not particularly limited, for example, the size of the interface of the first filter 111 and the second filter 102 may be preferably 1/8 inches or 1/16 inches, and the filter element pore size thereof may be preferably 2 μm.
Likewise, 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 is preferably in the range of 0-500 mL/min.
The gas generated by the battery is distributed in the battery testing device 105, and in order to improve the mixing uniformity of the gas generated and the carrier and bring the gas generated out by the carrier gas, the battery mass spectrum sample injection system further comprises a fan p arranged in the battery testing device 105. Therefore, the generated gas and the carrier gas are uniformly mixed by blowing the fan p, the generated gas is conveniently brought out, and the accuracy of a test result is improved.
In order to reduce the influence of the fan p on the carrier gas carrying away the produced gas, the fan p is a small fan. The specific size of the fan p is selected according to actual needs, which is not limited in this embodiment.
The number of the fans p can be one, or more than two, and the fans p can be selected according to actual needs. In order to improve the effect of the fans p, at least two fans p are uniformly distributed in the battery testing apparatus 105.
Specifically, there are two fans p, which are respectively located on two sides of the battery 104.
The type of the fan p is selected according to actual needs. Preferably, the fan p is an electric fan, and the battery testing apparatus 105 is provided with a wire hole q through which a power line k of the electric fan passes. A power supply 120 for supplying power to the fan p is provided outside the battery test apparatus 105.
In the practical application process, the power line k is hermetically connected with the wire through hole q so as to ensure that the produced gas is taken away by the carrier gas. Specifically, the power line k and the line through hole q are hermetically connected by a sealing element, and the specific type of the sealing element is selected according to actual needs, which is not limited in this embodiment.
Preferably, as shown in fig. 2, the battery test apparatus 105 includes: a case n for placing the battery 104, and a cover plate m detachably and hermetically connected with the case n. It will be appreciated that the housing n and cover plate m described above form a closed chamber.
Wherein, the air outlet e of the battery testing device 105 is arranged on the shell n and/or the cover plate m; the housing n and/or the cover plate m are provided with a positive wiring interface f and a negative wiring interface g for electrically connecting the battery 104 and the battery test system 106. It is understood that the battery test system 106 is located outside of the battery test apparatus 105.
When the second sample inlet pipeline 119 is communicated with the gas inlet h of the battery testing device 105, the gas inlet h is arranged on the shell n and/or the cover plate m.
In order to facilitate installation and disassembly, the cover plate m is positioned at the top end of the shell n, and the air inlet h, the air outlet e, the positive wiring interface f and the negative wiring interface g are all arranged on the cover plate m.
In order to facilitate the sealing connection, the housing n and the cover m are hermetically connected by a sealing gasket i. The type of the sealing gasket i is selected according to actual needs, and this embodiment is not limited to this.
The shell n and the cover plate m are detachably connected in a sealing mode, and specific structures of the detachable connection are selected according to actual needs. For the convenience of mounting and dismounting, the housing n and the cover plate m are preferably detachably connected by a screw coupling. Specifically, the threaded connector is a bolt. The housing n and the cover plate m are respectively provided with a threaded hole d corresponding to the bolt, as shown in fig. 2 and 3. The number and distribution of the bolts are selected according to actual needs, and this embodiment does not limit this.
In order to more specifically describe the battery mass spectrometry sampling system provided in this embodiment, a specific testing procedure is described below according to the battery mass spectrometry sampling system shown in fig. 1 as an example.
The test steps of the battery mass spectrum sample injection system shown in the figure 1 are as follows:
before testing, a small opening is cut in the battery 104, so that the gas generation of the battery can be detected; the clipped batteries 104 are then placed in the battery test apparatus 105, and the battery test apparatus 105 is assembled, and then the assembled battery test apparatus 105 is connected to a carrier gas sampling system;
before testing, removing the residual air or impure gas in each pipeline channel of the carrier gas sampling system and the battery testing device 105 by using carrier gas, specifically, firstly opening a power supply 120 for supplying power to a fan p, secondly opening a gas source 101, and adjusting a flow meter 103 to a set flow rate, so that the carrier gas passes through a second filter 102, the flow meter 103 and the battery testing device 105 in sequence, and a part of gas discharged from the battery testing device 105 passes through a valve inlet port a of a three-way valve 107 to a first valve outlet port c, a cold trap 110, a first filter 111, a leakage valve 113 and a mass spectrometer 115; another part of the gas discharged from the battery test device 105 passes through the inlet port a of the three-way valve 107 to the second outlet port b, and is pumped away by the vacuum pump 109; observing the corresponding response signal of the mass spectrometer 115 until the gas components in the gas path, such as nitrogen, oxygen, water, carbon dioxide, etc., decrease to the ideal value and reach a stable state, indicating that the residual air or impure gas in each pipeline channel of the carrier gas injection system and the cell testing device 105 is completely removed; finally, the needle valve 108 is adjusted to a proper opening degree, and the reading of a first pressure gauge 112 in front of a leakage valve 113 is controlled to be a proper working value;
after the above process is completed, the battery test system 106 may be activated to perform direct electrochemical mass spectrometry on the gas produced by the battery 104.
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 (10)
1. A battery mass spectrometry sample introduction system is characterized by comprising:
a battery test device (105) for placing a battery (104),
a battery test system (106) for providing operating parameters required for operation of the battery (104),
a mass spectrometer (115) for mass spectrometric analysis of the gas produced by the battery (104),
an exhaust device capable of exhausting the gas generated by the battery (104),
a carrier gas injection system capable of carrying the gas produced by the cell (104) to the mass spectrometer (115) and the exhaust by a carrier gas;
wherein, carrier gas sampling system includes: a valve assembly, a first sample inlet pipeline (116) communicated with the gas outlet (e) of the battery testing device (105); the first sample inlet pipeline (116) comprises a first branch (117) and a second branch (118), the first branch (117) is communicated with the mass spectrometer (115), the second branch (118) is communicated with the exhaust device, and the valve assembly is used for controlling the on-off and flow of the first branch (117) and the second branch (118);
partial generated gas can be discharged by utilizing the second branch (118) and the exhaust device, so that only partial generated gas enters the mass spectrometer (115), and fluctuation of the generated gas entering the mass spectrometer (115) can be reduced;
the battery (104) is a commercial soft package battery or a cylindrical battery.
2. The battery mass spectrometry sample introduction system of claim 1, wherein the exhaust device is a vacuum pump (109).
3. The battery mass spectrometry sample introduction system of claim 1, wherein the valve assembly comprises: a three-way valve (107), a first valve in series on the first branch (117), and a second valve in series on the second branch (118); the inlet port of the three-way valve (107) is communicated with the outlet port (e), and the two outlet ports of the three-way valve (107) are respectively communicated with the first branch (117) and the second branch (118).
4. The battery mass spectrometry sample introduction system of claim 3, wherein the second valve is a needle valve (108).
5. The battery mass spectrometry sample introduction system of claim 3,
the first valve is a leakage valve (113), a first pressure gauge (112) and a second pressure gauge (114) are connected to the first branch (117) in series, the first pressure gauge (112) is located on the upstream of the leakage valve (113), and the second pressure gauge (114) is located on the downstream of the leakage valve (113).
6. The battery mass spectrometry sample introduction system of claim 3, wherein the first branch (117) is connected with a cold trap (110) and a first filter (111) in series; wherein the cold trap (110) is located downstream of the three-way valve (107), the first filter (111) is located downstream of the cold trap (110), the first valve is located downstream of the first filter (111), and the mass spectrometer (115) is located downstream of the first valve.
7. The system of claim 1, further comprising: and the second sample introduction pipeline (119) is communicated with the gas inlet (h) of the battery testing device (105), and a gas source (101), a second filter (102) and a flow meter (103) are sequentially connected onto the second sample introduction pipeline (119) in series, wherein the flow meter (103) is close to the gas inlet (h) of the battery testing device (105).
8. The battery mass spectrometry sample introduction system of claim 1, further comprising a fan (p) disposed within the battery testing device (105).
9. The battery mass spectrometry sample introduction system of claim 8, wherein the number of the fans (p) is at least two and is uniformly distributed in the battery test device (105);
and/or the fan (p) is an electric fan, the battery testing device (105) is provided with a wire passing hole (q) through which a power wire (k) of the power fan (p) penetrates, and the power wire (k) is hermetically connected with the wire passing hole (q).
10. The battery mass spectrometry sample introduction system according to any one of claims 1-9, wherein the battery testing device (105) comprises: a shell (n) used for placing a battery (104), and a cover plate (m) detachably connected with the shell (n) in a sealing way;
wherein the air outlet of the battery testing device (105) is arranged on the housing (n) and/or the cover plate (m);
the housing (n) and/or the cover plate (m) are provided with a positive connection interface (f) and a negative connection interface (g) for electrically connecting the battery (104) and the battery test system (106).
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| CN113340967A (en) * | 2021-05-19 | 2021-09-03 | 上海大学 | Device and method for analyzing gas production components of battery through electrochemistry-gas chromatography-mass spectrometry |
| 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 |
| CN113376243B (en) * | 2021-06-23 | 2023-07-21 | 天目湖先进储能技术研究院有限公司 | Full-automatic multichannel battery mass spectrometry system |
| CN116572747B (en) * | 2023-07-13 | 2023-12-22 | 宁德时代新能源科技股份有限公司 | Battery fault detection method, device, computer equipment and storage medium |
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| CN106353462B (en) * | 2016-11-18 | 2019-07-09 | 宁德时代新能源科技股份有限公司 | Battery cell gas production detection device and detection method |
| CN108802276A (en) * | 2017-05-03 | 2018-11-13 | 宁德时代新能源科技股份有限公司 | Gas production test system for battery cell |
| CN108333244A (en) * | 2018-02-11 | 2018-07-27 | 上海零露仪器设备有限公司 | A kind of electrochemistry mass spectrometer |
| CN108548874A (en) * | 2018-04-02 | 2018-09-18 | 东莞塔菲尔新能源科技有限公司 | A kind of shell with square aluminum lithium battery interior gas collection detection device and method |
| CN109752139B (en) * | 2018-12-14 | 2020-08-18 | 兰州空间技术物理研究所 | Device and method for calibrating vacuum leak of nitrogen-hydrogen mixed gas |
| CN209342441U (en) * | 2018-12-29 | 2019-09-03 | 天目湖先进储能技术研究院有限公司 | A kind of battery core electrolyte inside sampling analysis device |
| CN210948653U (en) * | 2019-11-01 | 2020-07-07 | 苏州冠德能源科技有限公司 | Device for rapidly evaluating shale gas well productivity |
| CN110808203B (en) * | 2019-11-12 | 2022-03-18 | 北京中计新科仪器有限公司 | Device and method for quickly and accurately detecting impurities in high-purity hydrogen for hydrogen fuel cell |
| CN111562500B (en) * | 2020-05-22 | 2021-09-21 | 中国科学院长春应用化学研究所 | Battery test box and battery mass spectrum sampling system |
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