CN110333455B - Method for separating gas production from positive electrode and negative electrode through charge and discharge of symmetrical battery and application of method - Google Patents
Method for separating gas production from positive electrode and negative electrode through charge and discharge of symmetrical battery and application of method Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000007599 discharging Methods 0.000 claims abstract description 22
- 238000012360 testing method Methods 0.000 claims abstract description 16
- 238000004817 gas chromatography Methods 0.000 claims abstract description 8
- 241000208340 Araliaceae Species 0.000 claims description 18
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims description 18
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 18
- 235000008434 ginseng Nutrition 0.000 claims description 18
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- 239000003792 electrolyte Substances 0.000 claims description 8
- 235000002789 Panax ginseng Nutrition 0.000 claims description 6
- 208000032953 Device battery issue Diseases 0.000 claims description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052744 lithium Inorganic materials 0.000 abstract description 4
- 238000004458 analytical method Methods 0.000 abstract description 2
- 230000002687 intercalation Effects 0.000 abstract description 2
- 238000009830 intercalation Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 34
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- 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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- 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
- G01R31/387—Determining ampere-hour charge capacity or SoC
- G01R31/388—Determining ampere-hour charge capacity or SoC involving voltage measurements
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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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Abstract
The invention discloses a method for separating gas generation of positive and negative electrodes by charging and discharging symmetrical batteries, which comprises the following steps: s1, testing an SOC-Voltage curve; s2, charging and discharging the full battery; s3, detecting positive reference voltage and negative reference voltage; s4, preparing a symmetrical battery; s5, detecting the voltage range of the symmetrical battery; s6, separating the anode and the cathode to generate gas. The invention also provides the application of the method for separating gas generation of the positive electrode and the negative electrode by charging and discharging the symmetrical battery in analyzing the failure types of the battery. The positive plate and the negative plate in different lithium intercalation states are assembled into the positive symmetric battery and the negative symmetric battery for charging and discharging, the gas generation types are tested through the gas chromatography, the gas generation types of the positive plate and the negative plate are further separated, and are compared with the gas generation type of the full battery, so that the failure type of the full battery is determined, and a foundation is laid for the failure analysis of the battery.
Description
Technical Field
The invention relates to the technical field of gas component testing of lithium ion batteries, in particular to a method for separating gas generation of a positive electrode and a negative electrode by charging and discharging of a symmetrical battery and application thereof.
Background
The conventional gas generating components in the lithium battery mainly comprise oxygen, hydrogen, carbon dioxide, carbon monoxide, methane, ethane, ethylene, propane, propylene and other gases. Wherein the oxygen is mainly caused by the over-charge and oxygen release of the ternary cathode material and the decomposition of the negative electrode SEI film; carbon dioxide is mainly generated by anode failure; and hydrocarbon gases such as methane, ethane and the like are mainly caused by decomposition failure of the electrolyte due to extremely strong negative reducibility.
At present, the method adopted in the existing literature is mainly to disassemble the battery in a certain state, respectively encapsulate positive and negative pole pieces at high temperature for gas production, and represent and separate failure gas production types of the positive and negative poles in a state without electron participation, while the gas production of the lithium battery is mainly caused by redox decomposition of electrolyte at the positive and negative poles and cannot separate the electron participation.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for separating gas generation of a positive electrode and a negative electrode by charging and discharging of a symmetrical battery and an application thereof.
The invention provides a method for separating gas generation from positive and negative electrodes by charging and discharging symmetrical batteries, which comprises the following steps:
s1, testing an SOC-Voltage curve: manufacturing three electrodes of the ternary laminated battery and testing the SOC-Voltage curves of the positive reference and the negative reference of the ternary laminated battery;
s2, full battery charging and discharging: charging and discharging the full cell A to SOC1, and charging and discharging the full cell B to SOC2, wherein the positive and negative pole pieces, the diaphragm and the electrolyte in the three electrodes of the ternary laminated cell, the full cell A and the full cell B are the same, the capacity of the full cell A is QA at nC multiplying power, and the difference between the capacity of the three electrodes of the ternary laminated cell and the capacity of the full cell B and the QA is within-5% QA;
s3, detecting positive reference voltage and negative reference voltage: according to the SOC-Voltage curves of the positive reference and the negative reference in the S1, the corresponding positive reference Voltage V1 of the full-cell A in the SOC1 state can be obtainedRoot of red ginsengAnd a negative reference voltage V1Ginseng radix (radix Ginseng)Positive reference voltage V2 corresponding to the state of SOC2 of full battery BRoot of red ginsengAnd a negative reference voltage V2Ginseng radix (radix Ginseng)；
S4, preparing a symmetrical battery: disassembling the full battery A and the full battery B to obtain 2 positive plates and 2 negative plates, and assembling the positive symmetric battery and the negative symmetric battery, wherein the initial voltage range of the positive symmetric battery is-V2Root of red ginseng-V1Root of red ginseng∣～∣V2Root of red ginseng-V1Root of red ginseng| the initial voltage range of the cathode symmetrical battery is- | V2Ginseng radix (radix Ginseng)-V1Ginseng radix (radix Ginseng)∣～∣V2Ginseng radix (radix Ginseng)-V1Ginseng radix (radix Ginseng)∣；
S5, detecting the voltage range of the symmetrical battery: when the current is nC multiplying power, the initial voltage range is taken as reference, the voltage range is adjusted, so that the difference between the capacities of the positive electrode symmetrical battery and the negative electrode symmetrical battery and QA is within-5% QA to 5% QA, and the corresponding voltage ranges are respectively the voltage range of the positive electrode symmetrical battery and the voltage range of the negative electrode symmetrical battery at the moment;
s6, separating the anode and the cathode to generate gas: and (3) taking the positive electrode symmetric battery and the negative electrode symmetric battery within respective voltage ranges, carrying out electrical property test by taking nC multiplying power as current, and then detecting gas components generated by each battery through gas chromatography to realize gas generation of the separated positive electrode and the negative electrode.
The three electrodes, the positive electrode, the negative electrode, the full cell and the symmetrical cell of the ternary laminated battery are common terms in the field.
Preferably, SOC1+ SOC2 is 100%.
Preferably, SOC1 is more than or equal to 0% and less than or equal to 100%, and SOC2 is more than or equal to 0% and less than or equal to 100%.
Preferably, 0.01< n <1 in nC.
Preferably, in S1, the Voltage range of the measured SOC-Voltage curve is 3-4.2V.
Preferably, in S5, when adjusting the voltage range, the voltage across the symmetrical battery needs to be adjusted symmetrically.
The invention also provides the application of the method for separating gas generation of the positive electrode and the negative electrode by charging and discharging the symmetrical battery in analyzing the failure types of the battery.
Preferably, the specific application method is as follows: taking the full cell C for electrical property test, and then detecting gas components generated by the full cell C through gas chromatography; and then comparing the generated gas with the positive electrode symmetrical battery and the negative electrode symmetrical battery, and finally determining the failure type of the full battery C.
Preferably, the positive and negative electrode plates, the diaphragm and the electrolyte of the full battery C are the same as those of the full battery A.
Preferably, the capacity of the full cell C is within-5% QA to 5% QA from QA.
Preferably, the full cell C has the same electrical property test and the same multiplying power as the positive electrode symmetric cell and the negative electrode symmetric cell.
Preferably, the full cell C is subjected to an electrical property test at a voltage ranging from 3 to 4.2V.
The invention manufactures the symmetrical batteries with different SOC, namely different lithium intercalation states, and carries out charge and discharge, separates the anode and the cathode, simultaneously has the participation of electrochemical reaction, namely electrons, and further can more truly separate the gas generation types of the anode and the cathode, and the gas generation types are tested by gas chromatography; and comparing the type of the generated gas with the type of the generated gas of the full battery, thereby determining the failure type of the full battery and laying a foundation for the failure analysis of the battery.
Drawings
Fig. 1 is a SOC-Voltage curve of three electrodes of the ternary laminated battery in example 1.
FIG. 2 is a 0.1C charge-discharge curve of the symmetric positive electrode in example 1 at-1 to 1V.
FIG. 3 is a 0.1C charge-discharge curve of the symmetric negative electrode cell of example 1 at-2V.
Fig. 4 is a comparison of gas compositions collected after three cycles of 0.1C for all cell C, positive symmetric cell and negative symmetric cell in example 2.
Fig. 5 is a schematic diagram of a positive symmetric cell structure.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A method for separating gas generation from positive and negative electrodes by charging and discharging of a symmetrical battery comprises the following steps:
s1, testing an SOC-Voltage curve: manufacturing three electrodes of the ternary laminated battery, and testing the SOC-Voltage curves of the positive reference and the negative reference of the ternary laminated battery under the conditions of 0.1C multiplying power and 3-4.2V, specifically referring to FIG. 1;
s2, full battery charging and discharging: charging a full battery A0.1C to 4.2V at constant current and constant voltage, wherein the cut-off current is 0.05C, the SOC1 is 100%, discharging a full battery B0.1C to 3V, and the SOC2 is 0%, wherein the three electrodes of the ternary laminated battery, the positive and negative pole pieces, the diaphragm and the electrolyte in the full battery A and the full battery B are the same, the capacity of the full battery A0.1C is 60mAh, and the capacity of the full battery B0.1C is 61 mAh;
s3, detecting positive reference voltage and negative reference voltage: according to the SOC-Voltage curves of the positive reference and the negative reference in the S1 (namely, the SOC-Voltage curve in the S1), the corresponding positive reference Voltage V1 of the full-cell A in the SOC1 state can be obtainedRoot of red ginsengAnd a negative reference voltage V1Ginseng radix (radix Ginseng)Positive reference voltage V2 corresponding to the state of SOC2 of full battery BRoot of red ginsengAnd a negative reference voltage V2Ginseng radix (radix Ginseng)(ii) a See table 1 for details:
table 10% and 100% SOC states corresponding to the voltages of the full cell, the positive reference, and the negative reference, respectively.
S4, preparing a symmetrical battery: disassembling the full battery A and the full battery B to obtain 2 positive plates and 2 negative plates, and assembling the positive symmetric battery and the negative symmetric battery, wherein the initial voltage range of the positive symmetric battery is-V2Root of red ginseng-V1Root of red ginseng∣～∣V2Root of red ginseng-V1Root of red ginseng| 0.7-0.7V, and the initial voltage range of the symmetric-cathode battery is | V2Ginseng radix (radix Ginseng)-V1Ginseng radix (radix Ginseng)∣～∣V2Ginseng radix (radix Ginseng)-V1Ginseng radix (radix Ginseng)| is-0.3 to 0.3V;
s5, detecting the voltage range of the symmetrical battery: the positive electrode symmetrical battery has a 0.1C multiplying power of 50mAh under-0.7V, and the negative electrode symmetrical battery has a 0.1C multiplying power of 30mAh under-0.3V; the total battery capacity of 60mAh is taken as a reference, the positive and negative symmetric batteries have 0.1C multiplying power, and the voltage ranges are symmetrically widened at two ends to obtain: when the voltage of the positive electrode symmetrical battery is-1V, the 0.1C capacity exertion is 63mAh, see figure 2, and when the voltage of the negative electrode symmetrical battery is-2V, the capacity exertion is 57mAh, see figure 3; compared with 60mAh, the capacity errors of the positive and negative symmetric batteries are controlled to be within 5 percent, so that the voltage range of the positive symmetric battery is-1V, and the voltage range of the negative symmetric battery is-2V;
s6, separating the anode and the cathode to generate gas: and (3) taking the positive electrode symmetrical battery and the negative electrode symmetrical battery within respective voltage ranges, circulating for three weeks at 0.1 ℃, and then detecting gas components generated by each battery through gas chromatography to realize gas generation of the positive electrode and the negative electrode.
Example 2
The application of a method for separating gas generated by positive and negative electrodes by charging and discharging symmetrical batteries in analyzing the types of battery failure is as follows:
the specific application method comprises the following steps: taking a full battery C, wherein the 0.1C capacity is 63mAh, and the positive and negative pole pieces, the diaphragm and the electrolyte of the full battery C are the same as those of the full battery A; taking a full battery C, circulating for three weeks at 3-4.2V under 0.1C, and detecting gas components generated by the full battery by gas chromatography; then comparing the gas production with positive electrode symmetrical batteries and negative electrode symmetrical batteries, and obtaining the result shown in figure 4;
FIG. 4 shows the comparison results of the gas components collected after the full cell C, the positive symmetric cell and the negative symmetric cell are cycled for three weeks at 0.1C; FIG. 4 shows that the gas production component of the whole battery is mainly generated by the negative electrode and CO is mainly generated by the positive electrode2Gas, negative electrode formation of H2CO and hydrocarbon gas (CH)4、C2H4、C2H6) The symmetric battery effectively separates the gas production components of the positive electrode and the negative electrode.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for separating gas generation from positive and negative electrodes by charging and discharging of a symmetrical battery is characterized by comprising the following steps:
s1, testing an SOC-Voltage curve: manufacturing three electrodes of the ternary laminated battery and testing the SOC-Voltage curves of the positive reference and the negative reference of the ternary laminated battery;
s2, full battery charging and discharging: charging and discharging the full cell A to SOC1, and charging and discharging the full cell B to SOC2, wherein the positive and negative pole pieces, the diaphragm and the electrolyte in the three electrodes of the ternary laminated cell, the full cell A and the full cell B are the same, the capacity of the full cell A is QA at nC multiplying power, and the difference between the capacity of the three electrodes of the ternary laminated cell and the capacity of the full cell B and the QA is within-5% QA;
s3, detecting positive reference voltage and negative reference voltage: according to the SOC-Voltage curves of the positive reference and the negative reference in the S1, the corresponding positive reference Voltage V1 of the full-cell A in the SOC1 state can be obtainedRoot of red ginsengAnd a negative reference voltage V1Ginseng radix (radix Ginseng)Positive reference voltage V2 corresponding to the state of SOC2 of full battery BRoot of red ginsengAnd a negative reference voltage V2Ginseng radix (radix Ginseng)；
S4, preparing a symmetrical battery: disassembling the full battery A and the full battery B to obtain 2 positive plates and 2 negative plates, and assembling the positive symmetric battery and the negative symmetric battery, wherein the initial voltage range of the positive symmetric battery is-V2Root of red ginseng-V1Root of red ginseng∣～∣V2Root of red ginseng-V1Root of red ginseng| the initial voltage range of the cathode symmetrical battery is- | V2Ginseng radix (radix Ginseng)-V1Ginseng radix (radix Ginseng)∣～∣V2Ginseng radix (radix Ginseng)-V1Ginseng radix (radix Ginseng)∣；
S5, detecting the voltage range of the symmetrical battery: when the current is nC multiplying power, the initial voltage range is taken as reference, the voltage range is adjusted, so that the difference between the capacities of the positive electrode symmetrical battery and the negative electrode symmetrical battery and QA is within-5% QA to 5% QA, and the corresponding voltage ranges are respectively the voltage range of the positive electrode symmetrical battery and the voltage range of the negative electrode symmetrical battery at the moment;
s6, separating the anode and the cathode to generate gas: and (3) taking the positive electrode symmetric battery and the negative electrode symmetric battery within respective voltage ranges, carrying out electrical property test by taking nC multiplying power as current, and then detecting gas components generated by each battery through gas chromatography to realize gas generation of the separated positive electrode and the negative electrode.
2. The method for separating gas generation from positive and negative electrodes through charge and discharge of the symmetrical battery as claimed in claim 1, wherein SOC1+ SOC2 is 100%.
3. The method for separating gas generation from positive and negative electrodes of a symmetric battery in charge and discharge according to claim 1 or 2, wherein SOC1 is between 0% and 100%, and SOC2 is between 0% and 100%.
4. The method for separating gas generation of positive and negative electrodes by charging and discharging of the symmetrical battery according to claim 1, wherein 0.01< n <1 in nC.
5. The method for separating gas generation of the positive electrode and the negative electrode through charge and discharge of the symmetrical battery according to claim 1, wherein in S1, the Voltage range of the SOC-Voltage curve is 3-4.2V; in S5, when adjusting the voltage range, the voltages at the two ends of the symmetrical battery need to be adjusted symmetrically.
6. Use of a method for separating gas from positive and negative electrodes of a symmetrical battery according to any one of claims 1 to 5 for analyzing battery failure types.
7. The application of the method for separating gas generation of positive and negative electrodes by charging and discharging of the symmetrical battery in analyzing the failure types of the battery according to claim 6 is characterized in that the specific application method is as follows: taking the full cell C for electrical property test, and then detecting gas components generated by the full cell C through gas chromatography; and then comparing the generated gas with the positive electrode symmetrical battery and the negative electrode symmetrical battery, and finally determining the failure type of the full battery C.
8. The application of the method for separating gas production from positive and negative electrodes through charge and discharge of the symmetrical battery in analyzing the failure types of the battery according to claim 7 is characterized in that the positive and negative electrode plates, the diaphragm and the electrolyte of the full battery C are the same as those of the full battery A.
9. The application of the method for separating gas generated by positive and negative electrodes through charge and discharge of the symmetrical battery in analyzing the failure types of the battery according to claim 7 or 8 is characterized in that the difference between the capacity of the full battery C and QA is within-5% QA to 5% QA.
10. The application of the method for separating gas generation of positive and negative electrodes by charging and discharging of the symmetrical battery in analyzing the failure types of the battery according to claim 7 is characterized in that the full battery C is the same as the positive electrode symmetrical battery and the negative electrode symmetrical battery in electrical property tests and has the same multiplying power; the voltage range of the full cell C subjected to the electrical property test was 3-4.2V.
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| CN109342952A (en) * | 2018-09-26 | 2019-02-15 | 合肥国轩高科动力能源有限公司 | Lithium ion battery electrode and electrolyte interface evaluation method |
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