CN112213406A - Method and system for measuring amount of gas in battery cell - Google Patents
Method and system for measuring amount of gas in battery cell Download PDFInfo
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- CN112213406A CN112213406A CN201911150407.1A CN201911150407A CN112213406A CN 112213406 A CN112213406 A CN 112213406A CN 201911150407 A CN201911150407 A CN 201911150407A CN 112213406 A CN112213406 A CN 112213406A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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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 provides a method and a system for measuring the amount of gas in a battery cell, and belongs to the technical field of batteries. A method for measuring an amount of gas within a cell, the method comprising: communicating a sampling device filled with reference gas with a preset volume in advance with a space where to-be-detected gas in the electric core is located, wherein the reference gas and the to-be-detected gas do not have the same gas components and do not react; mixing the reference gas with the gas to be detected to obtain a mixed gas; measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas; and calculating the volume of each gas component in the gas to be detected according to the volume ratio and the preset volume of the reference gas. A system for measuring the amount of gas in the battery cell is also provided. The method has the advantages of simplicity, effectiveness and capability of measuring the gas production volume of the gas.
Description
Technical Field
The invention relates to the technical field of batteries, in particular to a method and a system for measuring the amount of gas in a battery core.
Background
In recent years, lithium ion batteries have been rapidly developed as power batteries. The lithium ion battery can generate a large amount of gas in the processes of storage and long-term charge-discharge circulation, and is particularly more obvious at high temperature, a large amount of electrolyte is consumed in the gas generation process of the battery, materials and current collectors are separated from each other, the contact interface between pole pieces is poor, and the transmission of ions and electrons is difficult, so that the impedance of the battery is increased, the polarization phenomenon is serious, even lithium is separated, the battery fails, the performance of the battery is influenced, a great potential safety hazard is caused, the service life and the power performance of the battery are influenced, and the like.
The gas generation of the lithium ion battery occurs in the whole life cycle, the gas generation in the formation process mainly comes from the generation of a negative electrode SEI (solid electrolyte interface) film, and a large amount of gas is also generated in the subsequent storage and circulation processes. In the circulation process of negative electrode materials such as graphite, silicon and the like, along with the desorption of lithium ions, the volume shrinkage and expansion phenomena can occur, so that the graphite is separated and shed, and the stripped graphite generates new active sites and continues to react with electrolyte to generate gas, thereby causing the battery to swell. Particularly, in an electric automobile, the battery core generates gas to expand and deform, the pressure between the battery cores is increased, and the module is in a high-risk state, so that the research on the gas generation mechanism of the battery core has very important reference value on the safety and the electrochemical performance of the power battery.
Generally, GC (Gas Chromatography) is mostly used to measure Gas production components and their ratios, but this method has many disadvantages:
1. the amount of gas required is greater. When GC is used for measurement, a certain amount of gas needs to be extracted and injected into an instrument to measure, but when the gas production of a battery at certain stages is researched, only a small amount of gas is remained, and the minimum amount required by the test cannot be met.
2. The gas production of each gas cannot be measured. GC can only measure the percentage of each gas, and cannot calculate the gas yield of each gas in the cell without knowing the total cell gas yield. And different gas yields in the battery cell have important value for researching the gas production reaction and side reaction mechanism in the battery cell.
Disclosure of Invention
The invention aims to provide a method and a system for measuring the amount of gas in a battery cell, and aims to solve the technical problems that the amount of gas to be measured in the existing battery cell gas production measurement is small and the specific volume cannot be obtained.
In order to achieve the above object, an embodiment of the present invention provides a method for measuring an amount of gas in a battery cell, where the method includes:
communicating a sampling device filled with reference gas with a preset volume in advance with a space where to-be-detected gas in the electric core is located, wherein the reference gas and the to-be-detected gas do not have the same gas components and do not react;
mixing the reference gas with the gas to be detected to obtain a mixed gas;
measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas;
and calculating the volume of each gas component in the gas to be detected according to the volume ratio and the preset volume of the reference gas.
Optionally, the measuring of the volume ratio of the gas component of the mixed gas to each gas component specifically comprises:
sampling the mixed gas, and measuring the sampled gas by a gas chromatograph to obtain the gas components of the mixed gas and the volume ratio of each gas component.
Optionally, the mixing the reference gas and the gas to be detected includes:
and sealing the communication part of the sampling device and the battery cell, and standing for a preset time.
Optionally, the method further includes:
and acquiring the gas pressure in the sampling device, and correcting the volume of each gas component according to the change of the gas pressure.
Optionally, the method further includes: and acquiring the temperature in the sampling device, and correcting the volume of each gas component according to the change of the temperature.
In a second aspect of the present invention, there is also provided a system for measuring an amount of gas within a cell, the system comprising:
the sampling device is used for mixing reference gas with a preset volume with gas to be detected in the electric core to obtain mixed gas; the reference gas and the gas to be detected do not have the same gas components and do not react;
a measuring device for measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas; and
and the calculating device is used for calculating the volume of each gas component in the gas to be measured according to the volume ratio and the preset volume of the reference gas.
Optionally, the measuring device is a gas chromatograph; the gas chromatograph obtains the gas components of the mixed gas and the volume ratio of each gas component by measuring a sampled gas sampled from the mixed gas.
Optionally, the system further includes: and the negative pressure generator is connected with the sampling device or arranged in the sampling device.
Optionally, the system further includes: a gas pressure measuring device for obtaining a gas pressure within the sampling device, the gas pressure being used to correct the volume of each gas component according to a change in the gas pressure.
Optionally, the system further includes: a temperature measuring device for acquiring a temperature within the sampling device, the temperature being used to correct the volume of each gas component in accordance with a change in the temperature.
The invention adopts the reference gas and the gas to be measured to be mixed and then to be measured, thereby not only overcoming the measurement difficulty caused by too small volume of the gas to be measured, but also obtaining the volume of each gas in the gas to be measured. The method provided by the invention is simple and effective and is convenient to implement.
Additional features and advantages of embodiments of the invention will be set forth in the detailed description which follows.
Drawings
The accompanying drawings, which are included to provide a further understanding of the embodiments of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the embodiments of the invention without limiting the embodiments of the invention. In the drawings:
fig. 1 is a schematic flow chart of a method for measuring an amount of gas in a battery cell according to an embodiment of the present invention;
fig. 2 is a first schematic structural diagram of a system for measuring an amount of gas in a cell according to an embodiment of the present invention;
fig. 3 is a second schematic structural diagram of a system for measuring the amount of gas in the battery cell according to an embodiment of the present invention.
Detailed Description
The following detailed description of embodiments of the invention refers to the accompanying drawings. It should be understood that the detailed description and specific examples, while indicating embodiments of the invention, are given by way of illustration and explanation only, not limitation.
Fig. 1 is a schematic flow chart of a method for measuring an amount of gas in a cell according to an embodiment of the present invention, and as shown in fig. 1, the method for measuring an amount of gas in a cell includes:
communicating a sampling device filled with reference gas with a preset volume in advance with a space where to-be-detected gas in the electric core is located, wherein the reference gas and the to-be-detected gas do not have the same gas components and do not react; mixing the reference gas with the gas to be detected to obtain a mixed gas; measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas; and calculating the volume of each gas component in the mixed gas according to the volume ratio and the preset volume of the reference gas.
So, through the mode of adding the reference gas of predetermineeing the volume, increased the volume of mist, avoided the quantity of gas to be measured too little and lead to the drawback that can not satisfy the test demand. Meanwhile, the volume of the gas to be measured can be obtained under the condition of not measuring the volume by determining the volume of the reference gas and directly according to the volume ratio of each gas, so that the volume can be obtained more simply.
Specifically, the sampling device is first filled with a reference gas, preferably nitrogen N2Or a rare gas such as Ar, He, or the like, which is required to satisfy the following conditions: 1. the same gas components in the gas to be measured need not be contained, otherwise the measurement result will be affected; 2. the stability is good, and the electric core can not react with other gases in the electric core during standing and testing, otherwise, the measurement result can be influenced. Filling the sampling device with the reference gas may be performed by: filling the sampling device with reference gas, and discharging part of the reference gas to obtain the residual reference gas injection amount V1; the reference gas injection amount V1 should be ensured to satisfy the requirement of the sample amount required by the GC test when the sampling test is performed. And through the mode of taking out full again earlier, can guarantee that reference gas receives the influence minimum of former residual gas in the sampling device. And inserting a sampling device into the electric core, and mixing the reference gas with the gas to be detected to obtain mixed gas. After the liquid injection port is sealed, the mixture is left standing for a certain period of time, preferably more than 24 hours, so that the gases are uniformly mixed. Taking a sample of the gas in the core, where it has been thoroughly mixed, measuring the gas of the sample using GCAnd (4) obtaining the measurement result according to the components and the proportion. Such as: there were 4 sample gases, A, B, C and reference gas (R), measured by GC, corresponding to a volume percentage of MA，MB，MC，MR；
And calculating the volume of each gas component in the mixed gas according to the volume ratio and the preset volume of the reference gas. The calculation method is as follows: volume of gas a: vA＝V1/MR*MAVolume of gas B: vB＝V1/MR*MBVolume of gas C: vC＝V1/MR*MC. From this, the components of the gas to be measured and the volume occupied by each component are obtained.
In one embodiment of the present invention, the volume ratio of the gas component of the mixed gas to each gas component is measured, specifically: sampling the mixed gas, and measuring the sampled gas by a gas chromatograph to obtain the gas components of the mixed gas and the volume ratio of each gas component. The gas chromatograph has the advantages of high sensitivity, high analysis speed, wide application range and the like, so accurate results can be obtained in a short time by adopting the GC to test the gas components in the mixed gas.
In one embodiment, the mixing the reference gas and the gas to be measured includes: and sealing the communication part of the sampling device and the battery cell, and standing for a preset time. In order to achieve better test results, it is necessary to mix the reference gas and the gas to be tested thoroughly and prevent gas leakage and overflow or other gas infiltration, and the preset time period is preferably about 24 hours. There is another embodiment of the intensive mixing, namely, after the reference gas in the sampling device is injected into the electric core through the injection port, the injection port is closed and left standing for a preset time. The mixing position here is within the cell, unlike the mixing position described above in the region of the cell and the sampling device. But the reference gas and the gas to be measured need to be fully mixed, so that a better measurement effect is achieved.
In one embodiment provided by the present invention, the method further comprises: and acquiring the gas pressure in the sampling device, and correcting the volume of each gas component according to the change of the gas pressure. And the method further comprises: and acquiring the temperature in the sampling device, and correcting the volume of each gas component according to the change of the temperature.
According to the ideal gas state equation, the equation is PV ═ nRT, P refers to the pressure of the ideal gas, V is the volume of the ideal gas, n represents the amount of gas species, and T represents the thermodynamic temperature of the ideal gas; there is also a constant: r is an ideal gas constant. It can be seen that the volume of a certain amount of gaseous matter is closely related to pressure and temperature. Therefore, in order to accurately obtain the volumes of the respective gases in the gas to be measured, it is necessary to measure the temperature and pressure of the volumes at the corresponding times. The obtained volume can be converted or corrected by measuring the temperature and the pressure corresponding to the volume so as to achieve the aim of accurate measurement.
An embodiment of the present invention further provides a system for measuring an amount of gas in a battery cell, fig. 2 is a first schematic structural diagram of the system for measuring an amount of gas in a battery cell according to an embodiment of the present invention, as shown in fig. 2, the system includes:
the sampling device is used for mixing reference gas with a preset volume with gas to be detected in the electric core to obtain mixed gas; the reference gas and the gas to be detected do not have the same gas components and do not react;
a measuring device for measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas; and
and the calculating device is used for calculating the volume of each gas component in the gas to be measured according to the volume ratio and the preset volume of the reference gas.
The sampling device, the measuring device and the calculating device in the embodiment are relatively independent devices, and the sampling device, the measuring device and the calculating device can finish the gas measurement work together. Wherein sampling device is used for the gas that awaits measuring in the sample electric core to will predetermine reference gas of volume and the gas that awaits measuring and carry out intensive mixing, in order to reach the effect that increases gas volume and measure the gas volume in the gas that awaits measuring. The measuring device provides calculation basis for subsequent calculation by measuring the volume ratio of the gas component of the mixed gas and each gas component. The measuring device herein may be a gas component analyzer or the like, depending on the composition of the gas to be measured. The computing device may preferably be a PC, which outputs the final computation result via an output device.
In an alternative embodiment of the present invention, the measuring device is a gas chromatograph; the gas chromatograph obtains the gas components of the mixed gas and the volume ratio of each gas component by measuring a sampled gas sampled from the mixed gas. The advantages of using a gas chromatograph are as described above and will not be repeated here.
In an optional embodiment of the invention, the system further comprises: and the negative pressure generator is connected with the sampling device or arranged in the sampling device. The negative pressure generator may be, but is not limited to, a commonly used electric pump, and may also be a manual pump, such as a syringe-type suction pump. Therefore, a certain negative pressure is kept in the sampling device filled with the reference gas, so that more volume of gas to be measured can be sucked into the sampling device, and meanwhile, leakage caused by overlarge gas pressure is avoided. The negative pressure generator may be arranged in communication with the sampling device, where the connection comprises a connection by a hard or flexible tube; the sampling device can also be arranged in the sampling device, and the integrated design is adopted, so that the sampling device is more convenient to use.
In an optional embodiment of the invention, the system further comprises: a gas pressure measuring device for obtaining a gas pressure within the sampling device, the gas pressure being used to correct the volume of each gas component according to a change in the gas pressure. Since the volume of the gas and the gas pressure are related to each other, when the gas pressure in the sampling device changes, the volume of the mixed gas in the device also changes accordingly, and therefore, by measuring the gas pressure value in the sampling device, the volume of the gas obtained by measurement can be converted or corrected correspondingly.
In an optional embodiment of the invention, the system further comprises: a temperature measuring device for acquiring a temperature within the sampling device, the temperature being used to correct the volume of each gas component in accordance with a change in the temperature. As described above, since the temperature of the gas and the gas pressure are also related to each other, when the temperature in the sampling device changes, the volume of the mixed gas in the device also changes accordingly, and therefore, by measuring the temperature value in the sampling device, the volume of the gas obtained by measurement can be converted or corrected correspondingly.
Fig. 3 is a structural schematic diagram of a system for measuring the amount of gas in the battery cell according to an embodiment of the present invention, and the structure of the apparatus is shown in fig. 3. The following calculation method is exemplified by a specific measurement procedure and numerical values as follows:
extracting 0.5ml of reference gas helium by using a sampling device, injecting the reference gas helium into the cell, standing for 24H, extracting the gas in the cell, and performing GC test to obtain a mixed gas which contains other four gases besides helium: methane, ethane, carbon dioxide and carbon monoxide in respective volume contents of 2.31%, 0.42%, 44.66%, 19.15%, helium content 30.00%, and 96.54% after the sum of all gas contents, where the sum of the contents is not equal to 100%, indicating that part of the electrolyte may be carried in during sampling. The gas production rate of each gas can be calculated:
v (methane) ═ 0.5 ml/30.00%. 2.31%. 0.0385 ml;
v (ethane) ═ 0.5 ml/30.00%. 0.42%. 0.007 ml;
V(CO2)＝0.5ml/30.00％*44.66％＝0.7443ml；
V(CO)＝0.5ml/30.00％*19.15％＝0.3192ml；
thereby, the volume of gas generated in the electric core is measured.
According to the embodiment of the invention, the volume of the mixed gas is increased by adding the reference gas with the preset volume, so that the defect that the test requirement cannot be met due to too small gas to be tested is avoided. The embodiment of the invention simplifies the volume measurement of the gas to be measured, considers the influence of temperature and air pressure and ensures that the volume measurement of the gas is more accurate.
Although the embodiments of the present invention have been described in detail with reference to the accompanying drawings, the embodiments of the present invention are not limited to the details of the above embodiments, and various simple modifications can be made to the technical solutions of the embodiments of the present invention within the technical idea of the embodiments of the present invention, and the simple modifications all belong to the protection scope of the embodiments of the present invention.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention. In order to avoid unnecessary repetition, the embodiments of the present invention do not describe every possible combination.
Those skilled in the art will understand that all or part of the steps in the method according to the above embodiments may be implemented by a program, which is stored in a storage medium and includes several instructions to enable a single chip, a chip, or a processor (processor) to execute all or part of the steps in the method according to the embodiments of the present application. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-Only Memory (ROM), a Random Access Memory (RAM), a magnetic disk or an optical disk, and other various media capable of storing program codes.
In addition, any combination of various different implementation manners of the embodiments of the present invention is also possible, and the embodiments of the present invention should be considered as disclosed in the embodiments of the present invention as long as the combination does not depart from the spirit of the embodiments of the present invention.
Claims (10)
1. A method for measuring an amount of gas within a cell, the method comprising:
communicating a sampling device filled with reference gas with a preset volume in advance with a space where to-be-detected gas in the electric core is located, wherein the reference gas and the to-be-detected gas do not have the same gas components and do not react;
mixing the reference gas with the gas to be detected to obtain a mixed gas;
measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas;
and calculating the volume of each gas component in the gas to be detected according to the volume ratio and the preset volume of the reference gas.
2. The method according to claim 1, wherein the volume ratio of the gas component of the gas mixture to each gas component is measured, specifically:
sampling the mixed gas, and measuring the sampled gas by a gas chromatograph to obtain the gas components of the mixed gas and the volume ratio of each gas component.
3. The method of claim 1 or 2, wherein the mixing the reference gas with the gas to be measured comprises:
and sealing the communication part of the sampling device and the battery cell, and standing for a preset time.
4. The method for measuring the amount of gas within a cell of claim 1, further comprising:
and acquiring the gas pressure in the sampling device, and correcting the volume of each gas component according to the change of the gas pressure.
5. The method for measuring the amount of gas within a cell of claim 1, further comprising:
and acquiring the temperature in the sampling device, and correcting the volume of each gas component according to the change of the temperature.
6. A system for measuring an amount of gas within a cell, the system comprising:
the sampling device is used for mixing reference gas with a preset volume with gas to be detected in the electric core to obtain mixed gas; the reference gas and the gas to be detected do not have the same gas components and do not react;
a measuring device for measuring the gas components of the mixed gas and the volume ratio of each gas component in the mixed gas; and
and the calculating device is used for calculating the volume of each gas component in the gas to be measured according to the volume ratio and the preset volume of the reference gas.
7. The system for measuring an amount of gas within a cell of claim 6, wherein,
the measuring device is a gas chromatograph; the gas chromatograph obtains the gas components of the mixed gas and the volume ratio of each gas component by measuring a sampled gas sampled from the mixed gas.
8. The system for measuring the amount of gas within a cell of claim 6, further comprising: and the negative pressure generator is connected with the sampling device or arranged in the sampling device.
9. The system for measuring the amount of gas within a cell of claim 6, further comprising:
a gas pressure measuring device for obtaining a gas pressure within the sampling device, the gas pressure being used to correct the volume of each gas component according to a change in the gas pressure.
10. The system for measuring the amount of gas within a cell of claim 6, further comprising:
a temperature measuring device for acquiring a temperature within the sampling device, the temperature being used to correct the volume of each gas component in accordance with a change in the temperature.
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