CN114527172B - Evaluation method for stability of battery anode material - Google Patents
Evaluation method for stability of battery anode material Download PDFInfo
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- CN114527172B CN114527172B CN202210155965.2A CN202210155965A CN114527172B CN 114527172 B CN114527172 B CN 114527172B CN 202210155965 A CN202210155965 A CN 202210155965A CN 114527172 B CN114527172 B CN 114527172B
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- 238000011156 evaluation Methods 0.000 title claims abstract description 36
- 239000010405 anode material Substances 0.000 title abstract description 14
- 239000007774 positive electrode material Substances 0.000 claims abstract description 65
- 238000000034 method Methods 0.000 claims abstract description 38
- 230000008859 change Effects 0.000 claims abstract description 30
- 238000012360 testing method Methods 0.000 claims description 22
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 18
- 229910052744 lithium Inorganic materials 0.000 claims description 13
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 10
- 239000010406 cathode material Substances 0.000 claims description 9
- 239000011888 foil Substances 0.000 claims description 7
- 238000013461 design Methods 0.000 claims description 6
- 238000010277 constant-current charging Methods 0.000 claims description 5
- 125000004122 cyclic group Chemical group 0.000 claims description 5
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 47
- 238000011056 performance test Methods 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 description 10
- 229910001416 lithium ion Inorganic materials 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 239000011230 binding agent Substances 0.000 description 8
- 239000011248 coating agent Substances 0.000 description 8
- 239000006258 conductive agent Substances 0.000 description 8
- 239000011267 electrode slurry Substances 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 7
- 230000001351 cycling effect Effects 0.000 description 7
- 239000003792 electrolyte Substances 0.000 description 7
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- -1 nickel aluminum cobalt Chemical compound 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 5
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 5
- 239000002033 PVDF binder Substances 0.000 description 4
- 239000006230 acetylene black Substances 0.000 description 4
- 238000007600 charging Methods 0.000 description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 4
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 4
- 239000007773 negative electrode material Substances 0.000 description 4
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000002562 thickening agent Substances 0.000 description 4
- HFCVPDYCRZVZDF-UHFFFAOYSA-N [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O Chemical compound [Li+].[Co+2].[Ni+2].[O-][Mn]([O-])(=O)=O HFCVPDYCRZVZDF-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 239000011889 copper foil Substances 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 229910003002 lithium salt Inorganic materials 0.000 description 3
- 159000000002 lithium salts Chemical class 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 229920003048 styrene butadiene rubber Polymers 0.000 description 3
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 2
- 239000006256 anode slurry Substances 0.000 description 2
- 239000001768 carboxy methyl cellulose Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- IGILRSKEFZLPKG-UHFFFAOYSA-M lithium;difluorophosphinate Chemical compound [Li+].[O-]P(F)(F)=O IGILRSKEFZLPKG-UHFFFAOYSA-M 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- ZPFAVCIQZKRBGF-UHFFFAOYSA-N 1,3,2-dioxathiolane 2,2-dioxide Chemical compound O=S1(=O)OCCO1 ZPFAVCIQZKRBGF-UHFFFAOYSA-N 0.000 description 1
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- QTHKJEYUQSLYTH-UHFFFAOYSA-N [Co]=O.[Ni].[Li] Chemical compound [Co]=O.[Ni].[Li] QTHKJEYUQSLYTH-UHFFFAOYSA-N 0.000 description 1
- LTHNASGMNUUKRZ-UHFFFAOYSA-N [Mg].[Mn].[Ni] Chemical compound [Mg].[Mn].[Ni] LTHNASGMNUUKRZ-UHFFFAOYSA-N 0.000 description 1
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- VEWLDLAARDMXSB-UHFFFAOYSA-N ethenyl sulfate;hydron Chemical compound OS(=O)(=O)OC=C VEWLDLAARDMXSB-UHFFFAOYSA-N 0.000 description 1
- 229910021385 hard carbon Inorganic materials 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910000625 lithium cobalt oxide Inorganic materials 0.000 description 1
- FRMOHNDAXZZWQI-UHFFFAOYSA-N lithium manganese(2+) nickel(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Ni+2].[Li+] FRMOHNDAXZZWQI-UHFFFAOYSA-N 0.000 description 1
- 229910001496 lithium tetrafluoroborate Inorganic materials 0.000 description 1
- DVATZODUVBMYHN-UHFFFAOYSA-K lithium;iron(2+);manganese(2+);phosphate Chemical compound [Li+].[Mn+2].[Fe+2].[O-]P([O-])([O-])=O DVATZODUVBMYHN-UHFFFAOYSA-K 0.000 description 1
- VGYDTVNNDKLMHX-UHFFFAOYSA-N lithium;manganese;nickel;oxocobalt Chemical compound [Li].[Mn].[Ni].[Co]=O VGYDTVNNDKLMHX-UHFFFAOYSA-N 0.000 description 1
- BFZPBUKRYWOWDV-UHFFFAOYSA-N lithium;oxido(oxo)cobalt Chemical compound [Li+].[O-][Co]=O BFZPBUKRYWOWDV-UHFFFAOYSA-N 0.000 description 1
- URIIGZKXFBNRAU-UHFFFAOYSA-N lithium;oxonickel Chemical compound [Li].[Ni]=O URIIGZKXFBNRAU-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- ZAUUZASCMSWKGX-UHFFFAOYSA-N manganese nickel Chemical compound [Mn].[Ni] ZAUUZASCMSWKGX-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 229910021384 soft carbon Inorganic materials 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 230000007847 structural defect Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
-
- 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
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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 belongs to the technical field of battery material performance test, and particularly relates to an evaluation method of stability of a battery anode material. The evaluation method provided by the invention takes the positive reference potential change rate as an evaluation index, has the characteristics of rapid evaluation and comprehensive evaluation of the positive electrode material, and is different from the existing single evaluation based on a material level or comprehensive long-cycle evaluation based on a battery level. Compared with material level evaluation, the method has comprehensive consideration and higher evaluation accuracy; compared with the evaluation of the battery level, the method can accurately evaluate the difference of the cycle performance of a plurality of positive electrode materials in a short time on the premise of taking the comprehensive evaluation of the materials into consideration and without expensive instruments and equipment.
Description
Technical Field
The invention belongs to the technical field of battery material performance test, and particularly relates to an evaluation method of stability of a battery anode material.
Background
Lithium ion batteries are widely used in mobile phones, tablet computers, and power equipment because of their high energy density and long cycle life. The cycle performance of lithium ion batteries is critical to their life and conservation capability. The performance of the positive electrode material is a key point affecting the cycling stability of the lithium ion battery, such as the crystal structure, doping coating and structural defects of the positive electrode material, residual alkali in the preparation process of the material, the grain distribution and primary grain size of the material and the like can directly affect the performance of the positive electrode material. However, the positive electrode materials provided by various companies are good and bad, and positive electrode materials with reliable performances need to be screened in advance.
The evaluation method of the battery material performance in the prior art mainly comprises the following steps: firstly, based on the material or pole piece level, discussing some or some characteristics of the material, lacking in evaluation of the overall performance of the battery, and having low evaluation comprehensiveness and accuracy; secondly, based on longer circulation of the battery, compared with capacity attenuation in the circulation process of a plurality of materials, the method is comprehensive, has higher evaluation accuracy, but has larger long-term circulation time consumption, slower evaluation speed and higher resource consumption. For example, current evaluation of ternary cathode materials requires cycling greater than 1000 times, about 4 months. However, in the context of high-speed update iterations of lithium ion batteries, a rapid evaluation of the performance of the positive electrode material means whether the product can preempt the market. Therefore, it is important to develop a reliable and rapid cathode material evaluation method. For example, there is a dQ/dV test method in the prior art, but the method needs to rely on an ultra-high precision coulombmeter (UHPC) for testing, and although the number of cycles can be reduced to less than 200, the cycle rate is small, the actual time consumption is relatively long, and the equipment is expensive and has no popularity.
In view of the foregoing, there is a need to develop a method for evaluating the stability of a battery positive electrode material in a short-term cycle based on battery level without expensive instrumentation.
Disclosure of Invention
Therefore, the invention aims to overcome the defects of long testing time, expensive instrument and equipment dependence and the like of the testing method of the anode material in the prior art, thereby providing an evaluation method of the stability of the battery anode material.
The test principle of the invention is as follows: ideally, in a battery, lithium ions extracted from the positive electrode during charging should be fully intercalated back into the positive electrode during discharging. The active sites of the positive electrode material are reduced due to irreversible phase change and anisotropic volume expansion of the positive electrode material, so that Li ions embedded into the negative electrode cannot be embedded back into the positive electrode in the discharge process, and the positive electrode potential is changed.
The invention utilizes the phenomenon that the potential of the positive electrode changes along with the cycling process, and monitors the potential change of the positive electrode to the reference electrode (hereinafter referred to as positive reference potential) in the cycling process through a three-electrode battery. Generally, the positive electrode material with stable structure and good cycle performance has smaller fluctuation of positive reference potential in the cycle process; the positive electrode material with poor structural stability and poor cycle performance has larger positive reference potential change due to more structural collapse or irreversible phase change in the cycle process. Therefore, the stability of the positive electrode material in the cycling process can be determined by comparing the change rate of the positive reference potential under the same cycle times, and preferably, the positive reference potential change rate under the state of a full-charge battery of 100% SoC (state of charge) under the same cycle times is compared, because the positive electrode potential is high in full charge, has a maximum value, and is easy to determine and accurately compare.
Therefore, the invention provides the following technical scheme:
the invention provides a method for evaluating stability of a battery anode material, which comprises the following steps:
s1, preparing a positive electrode material to be detected into a three-electrode battery;
Specifically, the preparation method of the three-electrode battery is a standard method in the field, and reference is made to patent CN107293778A, CN108987836A, CN108630980A, CN203562453U. Typically, but not by way of limitation, the three electrode cell is fabricated by placing a copper wire between the positive and negative electrodes of the cell, separating the electrodes with a separator, drawing the copper wire out of the cell as one electrode, and then constant current charging (with the copper wire as the negative electrode, with a current of 0.1mA or otherwise) the positive/copper wire electrode pair until the voltage is 0V (e.g., 0.1mA charge for 2 hours). Then constant current charging (copper wire is used as a negative electrode, current is 0.1mA or other) is carried out on the negative electrode/copper wire electrode pair until the voltage is 0V, and the three-electrode battery is obtained after stopping charging (for example, 0.1mA for 2 h); the copper wire can also be a lithium metal electrode such as a porous lithium foil, a lithium belt and the like (when the lithium metal reference electrode is applied, the reference electrode does not need to be charged, and the three-electrode battery is obtained after the preparation is completed).
S2, setting circulation parameters according to the design requirements and the evaluation requirements of the three-electrode battery, circulating the three-electrode battery, and monitoring the positive reference potential;
Specifically, the circulation parameter setting is determined according to the evaluated materials and the design requirements of the battery (meeting the requirements of quick charge or long service life, and the like), the experimental targets are different, the parameters are different, and the use purpose of the battery to be evaluated can be determined by a person skilled in the art.
And S3, plotting by taking the positive reference potential as an ordinate and the cycle times as an abscissa, comparing the change rate of the positive reference potential of the positive electrode material to be tested compared with the initial state at the same cycle times, and determining the cycle stability of the positive electrode material.
Specifically, the initial positive reference potential is V 0, the positive reference potential after a certain cycle is V x, and the rate of change (positive reference potential rate of change) = (V x-V0)/V0).
Optionally, the loop parameters in step S2 include: testing temperature, cyclic voltage, cyclic multiplying power and number of cycles.
Alternatively, the test may be a constant temperature test or a variable temperature test, with a test temperature between-20 ℃ and 60 ℃. Alternatively, the test temperature is from 30℃to 55℃and preferably, the test temperature is 45 ℃.
Optionally, the cyclic voltage is a discharge cutoff voltage to a charge cutoff voltage V; for example, the cycling voltage of the lithium iron phosphate battery is 2.5-3.65V; the cycling voltage of the NCM cell is 2.8-4.35V.
Optionally, the number of circulation turns is less than or equal to 500; alternatively, the number of cycles is 100-350.
Optionally, in step S1, the reference electrode of the three-electrode battery is a conventional worn coin electrode in the field, which is typically, but not limited to, a copper wire, a lithium-plated electrode, or a lithium metal electrode such as a porous lithium foil, a lithium tape, or the like, which is directly implanted.
Optionally, the positive electrode material is a binary positive electrode material, a ternary positive electrode material or a lithium iron phosphate positive electrode material. Wherein the binary positive electrode material is at least one of nickel-manganese-based materials; the ternary positive electrode material is at least one of nickel cobalt manganese base, nickel aluminum cobalt base and nickel magnesium manganese base.
For a specific three-electrode battery, a typical and non-limiting method is a conventional method in the art, reference may be made to patent CN107293778A, CN108987836A, CN108630980A, CN203562453U, as long as it is ensured that the three-electrode battery prepared from the positive electrode material to be tested has the same parameters (including but not limited to, homogenization, coating, electrolyte, separator, negative electrode, etc.) except for the positive electrode material itself.
Typically, but not limited to, the positive electrode of the three-electrode battery includes a current collector and a positive electrode active material coated on the current collector, the positive electrode active material being selected from at least one of lithium iron phosphate, lithium manganese iron phosphate, lithium nickel manganese oxide material, lithium nickel oxide material, lithium cobalt oxide material, lithium nickel cobalt oxide material, and lithium nickel manganese cobalt oxide material. The coating process can be performed by using existing coating and cold pressing processes. Specifically, uniformly mixing an anode active material, a conductive agent and a binder according to a conventional proportion, and adding the mixture into a solvent to prepare anode slurry; and uniformly coating the positive electrode slurry on a positive electrode current collector aluminum foil, drying, cold pressing, and carrying out die cutting and slitting to prepare the positive electrode plate. Wherein the solid content of the positive electrode slurry may be 70-75%, the conductive agent may be a conventional conductive agent such as acetylene black, the binder may be a conventional binder such as styrene-butadiene rubber or vinylidene fluoride PVDF, and the solvent may be a conventional organic solvent such as N-methylpyrrolidone NMP.
The negative electrode of the three-electrode battery comprises a current collector and a negative electrode active material coated on the current collector, wherein the negative electrode active material is at least one selected from graphite, hard carbon, soft carbon and mesophase carbon microspheres. The coating process can be performed by using existing coating and cold pressing processes. Specifically, mixing a negative electrode active material, a conductive agent, a thickening agent and a binder according to a conventional proportion, adding the mixture into solvent water, uniformly mixing, and preparing negative electrode slurry; and uniformly coating the negative electrode slurry on a negative electrode current collector copper foil, drying, and then cold pressing to prepare a negative electrode plate. Wherein the solid content of the anode slurry may be 50-55%, the conductive agent may be a conventional conductive agent such as acetylene black, the binder may be a conventional binder such as styrene-butadiene rubber or vinylidene fluoride PVDF, and the thickener may be a conventional thickener such as sodium hydroxymethyl cellulose.
The reference electrode of the three-electrode battery comprises any form of metal lithium electrode such as copper wire plating lithium, porous lithium foil, lithium belt and the like.
The electrolyte of the invention can be made of conventional commercial lithium ion electrolyte or conventional materials, for example, electrolyte comprising solvent, lithium salt and additive, wherein the solvent is at least one of ethylene carbonate, dimethyl carbonate and ethylmethyl carbonate. The lithium salt is selected from lithium hexafluorophosphate and/or lithium tetrafluoroborate; the additive is at least one selected from vinylene carbonate, propylene carbonate, vinyl sulfate and lithium difluorophosphate. The molar concentration of the lithium salt is 0.8-1.2mol/L, and the mixed solution of Ethylene Carbonate (EC), dimethyl carbonate (DEC) and methyl ethyl carbonate (EMC) with the volume ratio of 1:1:1-1:2:2 can be adopted as the solvent. The volume percent of the additive may be 0.5-5%. The present invention may employ existing conventional membranes such as PE membranes, PP/PE composite films, or other commercially available membranes.
Optionally, in step S3, the positive reference potential is cycled at a certain required temperature compared with the initial state change rate, and the smaller the positive reference potential change rate corresponding to 100% soc at the same cycle number, the better the stability of the positive electrode material.
Preferably, the circulation temperature is set at 30-55 ℃ (preferably 45 ℃), and the circulation times are 100-500 circles (preferably within 350 circles).
The technical scheme of the invention has the following advantages:
the invention provides a method for evaluating the stability of a battery anode material, which comprises the following steps: s1, preparing a positive electrode material to be detected into a three-electrode battery; s2, setting circulation parameters according to the design requirements and the evaluation requirements of the three-electrode battery, circulating the three-electrode battery, and monitoring the positive reference potential; and S3, plotting by taking the positive reference potential as an ordinate and the cycle times as an abscissa, comparing the change rate of the positive reference potential of the positive electrode material to be tested compared with the initial state, and determining the cycle stability of the positive electrode material. The invention has the characteristics of rapid evaluation and comprehensive evaluation of the positive electrode material, and is different from the existing single evaluation based on material level or comprehensive long-cycle evaluation based on battery level. Compared with material level evaluation, the method has comprehensive consideration and higher evaluation accuracy; compared with the evaluation of the battery level, the method can accurately evaluate the difference of the cycle performance of a plurality of positive electrode materials in a short time on the premise of taking the comprehensive evaluation of the materials into consideration and without expensive instruments and equipment. This is because the degradation of the battery capacity is affected by multiple factors such as the positive electrode, the negative electrode, and the electrolyte, and the degradation of the capacity is not necessarily caused by the positive electrode material at a small number of cycles, which results in that the capacity retention rate is in a fluctuating state within a short number of cycles, and the difference in the cycle performance of a plurality of positive electrode materials cannot be distinguished. However, the positive reference potential is used for directly detecting the performance change of the positive electrode material, the tiny positive voltage change is captured by the positive reference potential, and the positive reference potential is continuously increased along with the accumulation of the positive electrode structure change in the circulation process, so that the difference of the circulation performances of various positive electrode materials can be easily distinguished.
According to the method for evaluating the stability of the battery anode material, provided by the invention, the degradation rate of the anode material can be accelerated by further limiting the test temperature, but the change of other materials and performances of the battery is not influenced, so that the cycle period can be greatly shortened, and the difference of the positive reference potential of a plurality of anode materials can be more obviously shown under the same cycle period.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing the variation of the positive reference potential of the positive electrode material lithium nickel cobalt manganese oxide (model: NCM613, named material 1) in example 1 of the present invention;
FIG. 2 is a graph showing the variation of the positive reference potential of the positive electrode material lithium nickel cobalt manganese oxide (model: NCM613, named material 2) in example 1 of the present invention;
FIG. 3 is a graph showing the variation of the positive reference potential of the positive electrode material lithium nickel cobalt manganese oxide (model: NCM613, named material 1) in example 2 of the present invention;
FIG. 4 is a graph showing the variation of the positive reference potential of the positive electrode material lithium nickel cobalt manganese oxide (model: NCM613, named material 2) in example 2 of the present invention;
FIG. 5 is a graph of the conventional cycle capacity retention (25 ℃) for the positive electrode material lithium nickel cobalt manganese oxide (model: NCM613, named Material 2) in the comparative example of the invention.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
The three-electrode batteries in the embodiment of the invention are all prepared by the following method: the preparation of the three-electrode battery comprises the following steps:
(1) Preparation of a positive plate: respectively taking an anode material, a conductive agent acetylene black and a binder polyvinylidene fluoride PVDF according to the mass ratio of 96:2:2, mixing uniformly to obtain a mixture, adding the mixture into a solvent N-methyl-2-pyrrolidone (NMP) to prepare positive electrode slurry (the solid content is 70%), uniformly coating the positive electrode slurry on a positive electrode current collector aluminum foil according to the surface density of 19mg/cm 2, drying the aluminum foil at the temperature of 100 ℃ and then cold pressing, and then carrying out die cutting and strip cutting to prepare the positive electrode plate of the lithium ion battery.
(2) Preparing a negative plate: taking negative electrode active material graphite, conductive agent acetylene black, thickener sodium carboxymethylcellulose (CMC) and binder Styrene Butadiene Rubber (SBR) according to the mass ratio of 95:1.5:1.5:2, mixing to obtain a mixture, adding the mixture into solvent water, uniformly mixing and preparing negative electrode slurry (the solid content is 50 percent); and uniformly coating the negative electrode slurry on a negative electrode current collector copper foil according to the surface density of 11mg/cm 2, wherein the thickness of the copper foil is 6 mu m, drying at 90 ℃, and then cold pressing to prepare the negative electrode plate of the lithium ion battery to be manufactured.
(3) Preparation of reference electrode sheet: a 0.2 micron copper wire was placed between the positive and negative electrodes and separated by a separator, the copper wire was led out of the cell as one electrode, and then the positive/copper wire electrode pair was subjected to constant current charging to a voltage of 0V and stopped (0.1 mA charging for 2 h). And then constant current charging is carried out on the cathode/copper wire electrode pair until the voltage is 0V, and the three-electrode battery is obtained after stopping charging for 2 hours at 0.1 mA.
(4) Preparation of electrolyte: and dissolving lithium hexafluorophosphate in a mixed solvent of ethylene carbonate, dimethyl carbonate and methyl ethyl carbonate in a volume ratio of 5:3:2 to obtain a lithium hexafluorophosphate solution with a concentration of 1.15mol/L, and adding 1vt% of ethylene carbonate, 0.5vt% of lithium difluorophosphate and 0.5vt% of ethylene sulfate DTD to obtain the lithium ion battery electrode liquid.
(5) And assembling the positive plate, the PE diaphragm (purchased from Enjetsche, model: SV 12) and the negative plate in a lamination mode to obtain a battery electrode group, drying in a vacuum drying oven, injecting electrolyte, and sealing to obtain the battery (model 33220102, thickness 33mm, width 220mm, height 102mm and nominal voltage 3.72V).
The preparation method of the battery in the comparative example of the present invention was different from the preparation method of the three-electrode battery described above in that the reference electrode was not included.
Example 1
The embodiment provides a method for evaluating stability of a battery anode material, which comprises the following steps:
step one: preparing two positive electrode materials to be evaluated, wherein the materials belong to nickel cobalt lithium manganate, the model is NCM613, and the materials are from different manufacturers, so that other manufacturing technical parameters and material parameters are the same except for the positive electrode materials to be evaluated, and preparing a three-electrode battery according to the method;
Step two: selecting a proper temperature T according to design parameters and evaluation requirements of the battery, placing the battery in a target temperature environment, circulating the battery for n times in a proper voltage circulation interval by proper multiplying power, and recording potential change of a positive electrode to a reference electrode; in the embodiment, the temperature is 45 ℃, the circulating voltage interval is 2.8V-4.35V, constant-current constant-voltage (4.35) charge/constant-current discharge is adopted, the multiplying power is 1C/1C, and the circulating frequency is 350.
Step three: and (3) plotting the positive reference potential against the cycle times, comparing the positive reference potential change rate (compared with an initial state) of a battery prepared by the target positive electrode material to be tested by taking the positive reference potential at 100% of SoC as an analysis object, and determining the cycle stability of the material.
The method for calculating the positive reference potential change rate comprises the following steps: c= (V x-V0)/V0, where c is the positive reference potential change rate, V x is the positive reference potential after x cycles (100% soc), and V 0 is the initial positive reference potential (100% soc).
After the three-electrode battery made of the two positive electrode materials is circulated for 350 circles at 45 ℃, the positive parameter change rate of the material 1 (figure 1) with poor performance is 0.502%, and the positive parameter change rate of the material 2 (figure 2) with good performance is 0.235%.
Example 2
The embodiment provides a method for evaluating stability of a battery anode material, which comprises the following steps:
Step one: preparing two positive electrode materials to be evaluated, wherein the materials belong to nickel cobalt lithium manganate, the model is NCM613, and the materials are from different manufacturers (same as in example 1), so that the manufacturing technical parameters and the material parameters are the same except that the positive electrode materials to be evaluated are different, and preparing a three-electrode battery according to the method;
Step two: selecting a proper temperature T according to design parameters and evaluation requirements of the battery, placing the battery in a target temperature environment, circulating the battery for n times in a proper voltage circulation interval by proper multiplying power, and recording potential change of a positive electrode to a reference electrode; in the embodiment, the temperature is-15 ℃, the circulating voltage interval is 2.8V-4.35V, constant-current constant-voltage charge/constant-current discharge is adopted, the multiplying power is 1C/1C, and the circulating times are 350.
Step three: and (3) plotting the positive reference potential against the cycle times, taking 100% SoC as an analysis object, comparing the positive reference potential change rate (compared with an initial state) of a battery prepared by the target positive electrode material to be detected, and determining the cycle stability of the material.
After the three-electrode battery made of the two positive electrode materials is circulated for about 350 circles at the temperature of minus 15 ℃, the positive parameter change rate of the material 1 (figure 3) with poor performance is 0.04%, and the positive parameter change rate of the material 2 (figure 4) with good performance is 0.02%.
Comparative example 1
The comparative example provides a method for evaluating the stability of a battery cathode material, comprising the following steps:
Two positive electrode materials to be evaluated are prepared, the materials belong to nickel cobalt lithium manganate, the model is NCM613, the batteries prepared by the materials 1 and 2 are subjected to constant-current constant-voltage charge/constant-current discharge at 25 ℃ from different manufacturers (same example 1), the multiplying power is 1C/1C, the capacity retention rate is shown in figure 5, and after 1500 times of circulation, the circulation stability of the material 1 is superior to that of the material 2 through linear prediction. However, after the actual recycling to about 2600 times, the disadvantage of the recycling stability of the material 1 is only apparent, and when the material 1 is attenuated to 80% of the capacity retention, the capacity retention of the material 2 is 86%.
As can be seen from the test results, compared with the comparative example, the test method provided by the embodiment of the invention can test the advantages and disadvantages of different positive electrode materials in the cycle of 350 circles, and the test results are consistent with the test results of the cycle of 2600 circles of the comparative example, thereby proving the accuracy of the test results. According to the data comparison between the embodiments of the invention, the decay rate of the positive electrode material can be accelerated at the preferable test temperature, so that the cycle period can be greatly shortened, and the difference of positive reference potentials of a plurality of positive electrode materials can be more obviously shown under the same cycle period.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. 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 method for evaluating the stability of the battery cathode material is characterized by comprising the following steps of:
s1, preparing a positive electrode material to be detected into a three-electrode battery;
S2, setting circulation parameters according to the design requirements and the evaluation requirements of the three-electrode battery, circulating the three-electrode battery, wherein the number of circulation turns is less than or equal to 500, the circulation multiplying power is 1C/1C, and monitoring the positive reference potential;
And S3, plotting by taking the positive reference potential as an ordinate and the cycle times as an abscissa, and comparing the change rate of the positive reference potential of the positive electrode material to be tested compared with the initial state on the premise of consistent cycle times to determine the cycle stability of the positive electrode material.
2. The method for evaluating the stability of a battery cathode material according to claim 1, wherein the cycle parameters in step S2 include: testing temperature, cyclic voltage, cyclic multiplying power and number of cycles.
3. The method for evaluating the stability of a battery cathode material according to claim 2, wherein the test temperature is-20 ℃ to 60 ℃.
4. The method for evaluating the stability of a battery cathode material according to claim 3, wherein the test temperature is 30 ℃ to 55 ℃;
alternatively, the test temperature is 45 ℃.
5. The method according to claim 2, wherein in the step S3, the smaller the rate of change of the positive reference potential compared to the initial state is, the better the stability of the positive electrode material is.
6. The method for evaluating the stability of a battery cathode material according to any one of claims 1 to 5, wherein the three-electrode battery uses a copper wire, a lithium foil or a lithium tape as a reference electrode.
7. The method of claim 6, wherein the positive electrode material is at least one of a binary positive electrode material, a ternary positive electrode material, or a lithium iron phosphate positive electrode material.
8. The method for evaluating the stability of a battery positive electrode material according to claim 6, wherein when the copper wire is used as the reference electrode, the positive electrode/reference electrode and the negative electrode/reference electrode are respectively subjected to constant current charging after the three-electrode battery is assembled.
9. The method for evaluating the stability of a battery cathode material according to claim 8, wherein the constant current is charged to a voltage of 0V.
10. The method for evaluating the stability of a positive electrode material for a battery according to claim 5, wherein a rate of change of a positive reference potential after being cycled 350 times at 45 ℃ of 0.5% or less from an initial state represents good stability of the positive electrode material.
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