CN116243180A - In-situ test method for charge-discharge gas production of soft-packaged battery - Google Patents
In-situ test method for charge-discharge gas production of soft-packaged battery Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 20
- 238000010998 test method Methods 0.000 title claims abstract description 15
- 239000007789 gas Substances 0.000 claims abstract description 74
- 238000012360 testing method Methods 0.000 claims abstract description 55
- 238000000034 method Methods 0.000 claims abstract description 21
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001819 mass spectrum Methods 0.000 claims abstract description 14
- 238000001514 detection method Methods 0.000 claims abstract description 12
- 229910052786 argon Inorganic materials 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 238000007600 charging Methods 0.000 claims abstract description 6
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000004080 punching Methods 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004949 mass spectrometry Methods 0.000 abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002985 plastic film Substances 0.000 abstract description 2
- 229920006255 plastic film Polymers 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 7
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- 238000005452 bending Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 125000004122 cyclic group Chemical group 0.000 description 1
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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]
- G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
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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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- 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 belongs to the field of battery detection, and particularly relates to an in-situ test method for charge, discharge and gas production of a soft package battery. The method for testing the gas production of the soft package battery is simple and can be used for testing in a simple die pool. In addition, the innovation points of the testing means of the invention are as follows: pricking a plurality of small holes on the edge of the aluminum plastic film on one side of the soft package battery; placing the punched battery in a simple soft package battery test mould prepared in advance and sealing; charging and discharging the battery and simultaneously taking out the gas in the sealed die by adopting inert carrier gas such as argon and the like; and analyzing the carried gas in real time by adopting mass spectrometry. The modified effect is as follows: the soft package battery with the holes is free from influencing the normal charge and discharge and long circulation of the battery, and gas generated in the reaction process can smoothly escape through the pinholes and can be detected by carrying the carrier gas into the mass spectrum, so that the electrochemical differential mass spectrum curve has obvious display effect.
Description
Technical Field
The invention belongs to the field of battery detection, and particularly relates to an in-situ test method for charge, discharge and gas production of a soft package battery.
Background
With the continuous emission of carbon dioxide worldwide, greenhouse gases have proliferated, posing a threat to the life system. In this context, energy resource shortage is the primary problem. The battery is attracting attention as a new energy device capable of mutually converting electric energy and chemical energy, wherein commercial lithium ion batteries are widely applied to the fields of electric automobiles, electronic devices and energy storage due to the advantages of high energy density, long service life, no pollution and the like. At present, more and more battery systems are proposed, such as sodium ion batteries, zinc ion batteries and the like, however, the batteries are usually accompanied by gas generation during charging and discharging due to complex chemical reactions, so that the gas pressure in the batteries is increased to generate a gas expansion phenomenon, thereby negatively affecting the performance of the batteries. In addition, a large amount of gas existing in the battery can cause structural change of electrode materials, so that the spacing between the positive electrode plate and the negative electrode plate is increased, and the cycle performance of the battery is obviously reduced. Even under the high temperature condition, the combustible gas in the battery escapes and burns to cause fire disaster, and great potential safety hazards exist, so the method is particularly important for observing and solving the gas production of the battery.
Researchers have made a great deal of research on gas production inside commercial lithium ion batteries. The formation of gas inside the battery is affected by various factors, and mainly comes from two stages of battery formation and charge-discharge cycle test, wherein the gas generated in the charge-discharge cycle test stage has a great influence on the battery. Research shows that in the cyclic test process, the generation of gas inside the battery is closely related to the ambient temperature and the charge and discharge modes. The types of the gas generated in the interior at different temperatures are not obviously changed, but the gas production rate is obviously increased; the gas types are partially changed under different cut-off voltages, and obviously, when the upper voltage limit is exceeded, gases such as oxygen, methane, ethylene and the like are generated.
The existing method for detecting the gas in the battery comprises a gas chromatography, a spectrum method, an optical fiber sensor, an electrochemical differential mass spectrometry and the like, and the spectrum type gas detection method mostly adopts in-situ Raman analysis, wherein the method and the optical fiber sensor both adopt laser as a gas detection light source, and have great influence on the working state and the performance of the battery in the analysis and test process, and belong to lossy detection; in addition, the spectrometry detection is commonly used for qualitative analysis of gas, and the quantitative analysis capability is weak; fiber optic sensors can be used for quantitative analysis, but at a higher cost. The electrochemical differential mass spectrometry method is to extract gas in the battery and perform qualitative and quantitative analysis on the gas after the gas enters mass spectrometer equipment, and the gas is pumped into the analysis equipment under the condition of negative pressure of mass spectrum by carrier gas, so that a relatively ideal monitoring signal can be obtained.
The existing soft package battery gas production test technology mainly comprises 1) extracting gas in a gas expansion battery through an injector, and injecting the gas into gas chromatography or mass spectrum for detection; 2) Embedding a capillary tube in the soft package battery and taking out the gas generated by charge and discharge through carrier gas; the disadvantages are as follows:
1. the common soft-package battery is completely closed, so that the reaction gas cannot escape and cannot be detected;
2. the air component is very easy to be introduced into the syringe for sampling, and the result is disturbed;
3. the preset capillary tube often affects the normal operation of the battery, and has great operation difficulty, so that a meaningful result cannot be obtained;
4. the gas produced by the soft package battery cannot escape, so that the gas is expanded, the performance of the battery is further influenced, and the battery is inaccurately evaluated;
5. the prior methods are difficult to quantify the produced gas and can not realize in-situ real-time observation;
6. the current method is usually only operated in a laboratory and cannot be applied under the working condition of a production scene.
Disclosure of Invention
The technical problem in the prior art is that the conventional soft package battery testing method is mainly to reform and design the air circuit on the soft package and the testing mold, but the methods have complex processes and high requirements on equipment. The operation difficulty is big when the mould is made, and cost is with high costs to comparatively complicacy when assembling the soft packet of battery, and the survival rate of soft packet of battery is low, can not directly feed back the original problem of using plastic-aluminum membrane equipment soft packet of battery moreover.
In order to solve the technical problems, the application provides the following technical scheme:
an in-situ test method for charge-discharge gas production of a soft package battery comprises the following steps:
s1: sealing the soft package battery in a soft package battery test mould after punching holes; the soft package battery test die is provided with an air inlet, an air outlet, a positive electrode lead and a negative electrode lead;
s2: the method comprises the steps that a positive electrode and a negative electrode of the soft package battery are connected with an external battery test system through a positive electrode lead and a negative electrode lead respectively, and an air inlet of a soft package battery test die is connected with a flow controller;
s3: the soft package battery is subjected to charge and discharge test through an external battery test system, meanwhile, inert gas is introduced into the air inlet through the flow controller, and is discharged through the air outlet;
s4: and carrying out mass spectrum detection on the gas discharged from the gas outlet to obtain a charge-discharge curve and a mass spectrum detection curve.
Preferably, in the step S1, a hole is punched at an edge of one side surface of the soft pack battery.
Preferably, in the step S1, the sealing method is screw fixation.
Further, a syringe needle is used for puncturing.
Further, the number of the pricking holes is 3-5.
Preferably, in the step S3, the inert gas is argon.
Preferably, in the step S3, the flow rate of the inert gas is 2-4sccm.
Preferably, in the step S3, the temperature of the charge and discharge test is 25-210 ℃.
Preferably, in the step S3, the voltage range of the charge-discharge test is 2-4.5V.
Preferably, in the step S3, the charge duration of the charge-discharge test is 2-4h, and the discharge duration is 0.5-1.5h.
Preferably, in the step S3, the current level of the charge-discharge test is 20mA.
The invention has the advantages that the testing method for the gas production of the soft package battery is particularly simple, the gas production of the soft package battery can be tested in a very simple die pool, and in addition, the innovation points of the testing means of the invention are as follows: pricking a plurality of small holes on the edge of the aluminum plastic film on one side of the soft package battery; placing the punched battery in a simple soft package battery test mould prepared in advance and sealing; charging and discharging the battery and simultaneously taking out the gas in the sealed die by adopting inert carrier gas; and analyzing the carried gas in real time by adopting mass spectrometry. The modified effect is as follows: the soft package battery with the holes is free from influencing the normal charge and discharge and long circulation of the battery, and gas generated in the reaction process can smoothly escape through the pinholes and can be detected by carrying the carrier gas into the mass spectrum, so that the electrochemical differential mass spectrum curve has obvious display effect.
Compared with the prior art, the technical scheme of the invention has the following advantages:
(1) The gas produced by the traditional commercial soft package battery cannot escape and cannot be detected, and the gas produced after hole punching can smoothly escape;
(2) The problem of gas escape is solved, and the finished soft package battery is placed in a simple die and can be detected only by punching holes, so that the difficulty in assembling the soft package battery in the die with a complex structure can be reduced;
(3) Experimental tests show that the soft package battery after hole punching does not influence the charge and discharge of the soft package battery, and the gas production of the battery can be detected in real time and quantitatively;
(4) The method can be quickly and conveniently implemented in a battery factory production workshop.
Drawings
Fig. 1 is a schematic view of a bundle Kong Ruanbao cell placed in a simple mold.
Fig. 2 is a view showing a soft pack battery placed in a simple mold.
Fig. 3 is a side view of the mold.
Fig. 4 is a graph of voltage test of a bundle Kong Ruanbao cell placed in a mold sealed and open circuit.
FIG. 5 is a diagram of an in situ cell connection with a LAND control system and flow controller.
Fig. 6 is a diagram of a detection result of the charge-discharge in situ mass spectrum of the soft package battery.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific examples, which are not intended to be limiting, so that those skilled in the art will better understand the invention and practice it.
Example 1
The prepared soft package battery is placed in a simple airtight and breathable soft package battery test mold after being punched, the size of the soft package battery is 6cm long, the width of the soft package battery is 4.5cm, the width of a tab is 0.6cm, the length of the tab after bending is 1cm, as shown in fig. 2, the bottom of the soft package battery test mold is arranged on the left side, and the top cover of the soft package battery test mold is arranged on the right side.
The soft package battery is placed in a die, the soft package battery is punched by a syringe needle, the soft package battery is in a sealed state by fastening with a screw, the open circuit voltage of the soft package battery is tested after the soft package battery is connected with positive and negative wires on the die, the normal open circuit voltage of the punched soft package battery is maintained to be 0.2V, and the result shows that the punched soft package battery has no negative influence on the soft package battery.
After the pouch cell and the pouch cell test mold were assembled in the glove box, they were taken out and connected with the LAND control system (cell test system) and the gas inlet to the flow controller (as shown in fig. 3, a is the gas inlet, b is the gas outlet), the flow controller was set to 3sccm, high purity argon was used as a carrier gas, and the high purity argon was continuously used as a flowing gas in the pouch cell mold pool during charge and discharge. Then, a charge and discharge program is applied to the battery by using the LAND control system, and during the charge and discharge process, the gas generated by the battery is detected along with the pumping of carrier gas (high-purity Ar) into a mass spectrum, and the charge and discharge test conditions are as follows: the room temperature is 25 ℃, the first charge and discharge is carried out, the voltage range is 2-4.5V, the charge and discharge program is limited by voltage conditions, the charge duration is 55 minutes and 25 seconds, the discharge duration is 58 minutes and 17 seconds, the charge and discharge current is 20mA, and the test result is shown in figure 6.
Example 2
And (3) placing the manufactured soft package battery in a soft package battery test mold which is simple and airtight and can be ventilated after punching, wherein the size of the soft package battery is 6cm long, the width of the soft package battery is 4.5cm, the width of a tab is 0.6cm, the length of the tab after bending is 1cm, the left side is the bottom of the soft package battery test mold, and the right side is the top cover of the soft package battery test mold.
The soft package battery is placed in a die, the soft package battery is punched by a syringe needle, the soft package battery is in a sealed state by fastening with a screw, the open circuit voltage of the soft package battery is tested after the soft package battery is connected with positive and negative wires on the die, the normal open circuit voltage of the punched soft package battery is maintained to be 0.2V, and the result shows that the punched soft package battery has no negative influence on the soft package battery.
After the soft battery and the soft battery test mold were assembled in the glove box, they were taken out and connected with a LAND control system (battery test system) and a flow controller, the flow controller was set to 2sccm, high-purity argon was used as a carrier gas, and the carrier gas was continuously used as a flowing gas in the soft battery mold pool during charge and discharge. Then, a charge and discharge program is applied to the battery by using the LAND control system, and during the charge and discharge process, the gas generated by the battery is detected along with the pumping of carrier gas (high-purity Ar) into a mass spectrum, and the charge and discharge test conditions are as follows: the temperature is 100 ℃, the first charge and discharge is carried out, the voltage range is 2-4.5V, the charge and discharge program is limited by voltage conditions, the charge duration is 2h, the discharge duration is 0.5h, and the charge and discharge current is 20mA.
Example 3
And (3) placing the manufactured soft package battery in a soft package battery test mold which is simple and airtight and can be ventilated after punching, wherein the size of the soft package battery is 6cm long, the width of the soft package battery is 4.5cm, the width of a tab is 0.6cm, the length of the tab after bending is 1cm, the left side is the bottom of the soft package battery test mold, and the right side is the top cover of the soft package battery test mold.
The soft package battery is placed in a die, the soft package battery is punched by a syringe needle, the soft package battery is in a sealed state by fastening with a screw, the open circuit voltage of the soft package battery is tested after the soft package battery is connected with positive and negative wires on the die, the normal open circuit voltage of the punched soft package battery is maintained to be 0.2V, and the result shows that the punched soft package battery has no negative influence on the soft package battery.
After the soft battery and the soft battery test mold are assembled in the glove box, the soft battery and the soft battery test mold are taken out and connected with a LAND control system (battery test system) and a flow controller, the flow controller is set to be 4sccm, high-purity argon is used as carrier gas, and the carrier gas is continuously used as flowing gas in the soft battery mold pool in the charge and discharge period. Then, a charge and discharge program is applied to the battery by using the LAND control system, and during the charge and discharge process, the gas generated by the battery is detected along with the pumping of carrier gas (high-purity Ar) into a mass spectrum, and the charge and discharge test conditions are as follows: the temperature is 210 ℃, the first charge and discharge is carried out, the voltage range is 2-4.5V, the charge and discharge program is limited by voltage conditions, the charge duration is 4h, the discharge duration is 1.5h, and the charge and discharge current is 20mA.
FIG. 6 is a plot of the first charge and discharge of the soft pack cell at room temperature (25deg.C) and a plot of differential electrochemical mass spectrometry monitoring for example 1, wherein a is the charge and discharge plot; b is the ion current curve of the corresponding gas; c is the concentration content percentage of the corresponding gas. It can be seen that the gas generation of the battery is serious at the beginning and ending time of charging and in the discharging process, and the CO can be monitored in situ 2 、H 2 And CH (CH) 4 Generating, wherein the comparative gases Ar and O 2 The content hardly changed at all.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations and modifications of the present invention will be apparent to those of ordinary skill in the art in light of the foregoing description. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (10)
1. The in-situ test method for the charge and discharge gas production of the soft package battery is characterized by comprising the following steps of:
s1: sealing the soft package battery in a soft package battery test mould after punching holes; the soft package battery test die is provided with an air inlet, an air outlet, a positive electrode lead and a negative electrode lead;
s2: the method comprises the steps that a positive electrode and a negative electrode of the soft package battery are connected with an external battery test system through a positive electrode lead and a negative electrode lead respectively, and an air inlet of a soft package battery test die is connected with a flow controller;
s3: the soft package battery is subjected to charge and discharge test through an external battery test system, meanwhile, inert gas is introduced into the air inlet through the flow controller, and is discharged through the air outlet;
s4: and carrying out mass spectrum detection on the gas discharged from the gas outlet to obtain a charge-discharge curve and a mass spectrum detection curve.
2. The in-situ test method of generating gas by charging and discharging a soft battery according to claim 1, wherein in the step S1, holes are punched at an edge of a side surface of the soft battery.
3. The in situ test method of soft pack battery charge-discharge gas production of claim 2, wherein the puncturing is performed by using a syringe needle.
4. The in situ test method of soft pack battery charge-discharge gas production of claim 2, wherein the number of holes is 3-5.
5. The in-situ test method for generating gas by charging, discharging and discharging a soft package battery according to claim 1, wherein in the step S1, the sealing method is screw fixing.
6. The in-situ test method for generating gas during charge and discharge of a soft pack battery according to claim 1, wherein in the step S3, the inert gas is argon.
7. The in-situ test method of soft pack battery charge-discharge gas production according to claim 1, wherein in the step S3, the flow rate of the inert gas is 2-4sccm.
8. The in-situ test method for charge-discharge gas production of a soft pack battery according to claim 1, wherein in the step S3, the temperature of the charge-discharge test is 25-210 ℃.
9. The in-situ test method for charge-discharge gas production of a soft pack battery according to claim 1, wherein in the step S3, the voltage range of the charge-discharge test is 2-4.5V.
10. The in-situ test method for charge, discharge and gas production of a soft pack battery according to claim 1, wherein in the step S3, the charge duration of the charge and discharge test is 2-4h, and the discharge duration is 0.5-1.5h.
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2023
- 2023-02-08 CN CN202310080114.0A patent/CN116243180A/en active Pending
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|---|---|---|---|---|
| CN111413635A (en) * | 2020-03-04 | 2020-07-14 | 合肥国轩高科动力能源有限公司 | Soft package lithium ion battery failure analysis method |
| EP3736903A2 (en) * | 2020-07-15 | 2020-11-11 | Marposs | Method for leak testing a battery cell |
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