CN114094043A - Method for evaluating cycle performance of lithium battery positive electrode material - Google Patents
Method for evaluating cycle performance of lithium battery positive electrode material Download PDFInfo
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- CN114094043A CN114094043A CN202111340544.9A CN202111340544A CN114094043A CN 114094043 A CN114094043 A CN 114094043A CN 202111340544 A CN202111340544 A CN 202111340544A CN 114094043 A CN114094043 A CN 114094043A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4285—Testing apparatus
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/48—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte
- H01M10/482—Accumulators combined with arrangements for measuring, testing or indicating the condition of cells, e.g. the level or density of the electrolyte for several batteries or cells simultaneously or sequentially
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a method for evaluating the cycle life of a lithium battery anode material, which comprises the following steps: step S1, preparing at least two anode materials to be evaluated; step S2, making each positive electrode material to be evaluated into a positive electrode; step S3, assembling each positive electrode with the same negative electrode and the same electrolyte into a battery cell; step S4, measuring the charging capacity Q of each battery cell from the charge-discharge cycle to the nth circle under the same multiplying powercCharging energy EcDischarge capacity QdAnd discharge energy EdN is any integer between 1 and 145; step S5, acquiring the average charging voltage V of each battery cell according to the following formulacAnd discharge average voltage Vd: step S6, acquiring the average charge-discharge voltage difference value delta V of each battery cell; step S7, comparing average charge-discharge voltage difference values delta V of each battery cell, wherein delta V is smallerThe cycle life of the positive electrode material to be evaluated corresponding to the battery core is longer. The evaluation method is convenient, rapid, low in cost and accurate.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a method for evaluating the cycle performance of a lithium battery positive electrode material.
Background
In order to solve the problem of environmental pollution caused by using traditional energy, the state advocates clean energy energetically, and then, the lithium battery technology is developed at a rapid speed. The performance of the anode material as an important raw material in the lithium battery is good and bad, and particularly the cycle life directly determines the performance index of the final lithium battery product. The proportion of the anode material in the lithium battery cost is as high as about 40%, so that the safety performance of the battery is determined, and the cost of the anode material directly determines the cost of the battery. Therefore, the anode material is subjected to model selection before large-scale production, and the cycle life of different anode materials is compared, so that the method has very important significance for predicting the performance of the lithium battery.
In the prior art, a positive electrode material to be evaluated is generally made into an electric core, then long circulation (the number of circulation circles is more than 500 circles) is carried out on the electric core until the battery capacity reaches an SOC state of 80% of the initial capacity, the positive electrode material with long circulation life is considered to be better by comparing the circulation life of the battery, or the long circulation is carried out, more than one month is usually needed, the rate of capacity attenuation is compared, and the quality of the positive electrode material is judged. In addition, few methods such as high-low temperature cycling and impedance testing are used to evaluate the positive electrode material.
However, the existing evaluation method usually needs to consume a large amount of test cost, and particularly, in the evaluation period, more than one month is often needed, which often causes project delay, low efficiency and missing business opportunity.
Disclosure of Invention
The invention mainly aims to provide a method for evaluating the cycle performance of a lithium battery anode material, and aims to solve the problems of long cycle and high test cost existing in the process of evaluating the cycle life of the anode material in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method of evaluating cycle life of a positive electrode material for a lithium battery, comprising the steps of: step S1, preparing at least two anode materials to be evaluated; step S2, the positive electrode materials to be evaluated are respectively mixed with the same conductive agent and the sameThe binder is mixed according to the same proportion to prepare anode slurry, and then the anode slurry is coated on the same anode current collector to form an anode; step S3, assembling the positive electrode made of each positive electrode material to be evaluated, the same negative electrode and the same electrolyte into a battery cell; step S4, measuring the charging capacity Q of each battery cell from the charge-discharge cycle to the nth circle under the same multiplying powercCharging energy EcDischarge capacity QdAnd discharge energy EdN is any integer between 1 and 145; step S5, acquiring the average charging voltage V of each battery cell according to the following formulacAnd discharge average voltage Vd：
Vc＝Ec/Qc
Vd＝Qd/Qc
Step S6, obtaining a charge-discharge average voltage difference Δ V of each battery cell, where Δ V is Vc－Vd(ii) a Step S7, comparing the average charge-discharge voltage difference Δ V of each cell, where the cycle life of the positive electrode material to be evaluated corresponding to the cell with the smaller average charge-discharge voltage difference Δ V is longer.
Further, n is any integer between 20 and 80.
Further, in step S3, the capacity C of each cell is measured, and then the charge capacity Q of each cell in the cycle from charge and discharge to the nth cycle under the magnification of 0.1-5C is measuredcCharging energy EcDischarge capacity QdAnd discharge energy Ed。
Further, at least two groups of positive electrode materials to be evaluated are prepared respectively, and the steps S2 to S5 are performed on each group of positive electrode materials to be evaluated respectively; and in step S5, the average charging voltage V of the battery cell corresponding to each positive electrode material to be evaluatedcTaking the average value of the corresponding groups, and the average discharge voltage V of the battery cell corresponding to each anode material to be evaluateddThe average value of each group is taken.
Further, in step S2, the conductive agent is one or more of conductive carbon black, carbon nanotubes, and graphene, and the binder is one or more of Kynar761A, PVDF, and HSV 900.
Furthermore, the weight ratio of the anode material to the conductive agent to the binder is (95-97): (1.2-1.8): 2-3.
Further, the positive current collector is an aluminum foil, a carbon-coated aluminum foil or a composite polyimide aluminum foil.
Further, the positive electrode material is lithium iron phosphate, lithium nickelate or lithium nickel cobalt manganese oxide.
The method can quickly evaluate the cycle life of different anode materials in a short time, can correspondingly quickly read and judge the advantages and disadvantages of the cycle performance of different anode materials, and can finish evaluation in a few cycles more accurately. Compared with the traditional test method, the method is convenient and quick, low in cost and accurate in result.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a variation curve of a charge-discharge average voltage difference Δ V after different cycles of a battery cell corresponding to each group of positive electrode materials in embodiment 1 of the present invention; and
fig. 2 shows the capacity retention rate of the cells corresponding to different cathode materials according to example 1 of the present invention as a function of the number of cycles.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As described in the background section, the current methods for evaluating the cycle life of the positive electrode material often consume a large amount of test cost, and particularly, the evaluation period often requires more than one month, which often results in delayed project, low efficiency and lost business opportunity.
In order to solve the above problems, the present invention provides a method for evaluating cycle life of a positive electrode material for a lithium battery, comprising the steps of: in the step of S1,preparing at least two anode materials to be evaluated; step S2, mixing each positive electrode material to be evaluated with the same conductive agent and the same binder according to the same proportion to prepare positive electrode slurry, and coating the positive electrode slurry on the same positive electrode current collector to form a positive electrode; step S3, assembling the positive electrode made of each positive electrode material to be evaluated, the same negative electrode and the same electrolyte into a battery cell; step S4, measuring the charging capacity Q of each battery cell from the charge-discharge cycle to the nth circle under the same multiplying powercCharging energy EcDischarge capacity QdAnd discharge energy EdN is any integer between 1 and 145; step S5, acquiring the average charging voltage V of each battery cell according to the following formulacAnd discharge average voltage Vd：
Vc＝Ec/Qc
Vd＝Qd/Qc
Step S6, obtaining a charge-discharge average voltage difference Δ V of each battery cell, where Δ V is Vc－Vd(ii) a Step S7, comparing the average charge-discharge voltage difference Δ V of each cell, where the cycle life of the positive electrode material to be evaluated corresponding to the cell with the smaller average charge-discharge voltage difference Δ V is longer.
The Δ V value is an average pressure difference during charging and discharging of the battery cell, and can comprehensively reflect adverse factors such as polarization internal resistance, SEI film resistance, electrolyte consumption, resistance caused by dissolution and precipitation of transition metal and loss of active lithium generated by the battery cell in a cyclic process, so that the quality of different anode materials can be accurately evaluated, and particularly the cycle life of the anode material can be directly reflected to be short or long.
The invention mixes different anode materials with the same conductive agent, binder and other materials according to the same proportion, then prepares the anode and assembles the anode with other same cathode, electrolyte and so on. Therefore, except for the anode material, the other materials and the proportion of the battery core are the same, so that the evaluation result is more accurate. After the battery cells are assembled, different battery cells are subjected to charge-discharge circulation under the same multiplying power, and the charge-discharge circulation is measured to obtain the circulation n-th circle (n is any integer between 1 and 145)Number of different cells, and the same number of cycles, as compared to the charge capacity Q of the same 5 th or 80 th cycle)cCharging energy EcDischarge capacity QdAnd discharge energy EdAnd further obtaining the average charge-discharge voltage difference value delta V of each battery cell. By comparing the delta V of the battery cores of different anode materials, the long cycle life of which anode material can be qualitatively judged.
The method can judge more accurately only by cycling the battery cells with different anode materials for a few times, thereby having the advantages of convenience, rapidness and low test cost.
In a preferred embodiment, n is any integer between 20 and 80. Therefore, the number of the circulating circles can be further reduced, the evaluation efficiency is improved, and the evaluation is relatively accurate.
Preferably, in step S3, the capacity C of each cell is measured, and then the charge capacity Q of each cell in the charge-discharge cycle to the nth cycle at a rate of 0.1-5C is measuredcCharging energy EcDischarge capacity QdAnd discharge energy Ed. Therefore, when the charge and discharge circulation of each battery cell is actually carried out, each battery cell is tested under the multiplying power of 0.1-5C, for example, the charge and discharge tests are carried out according to 0.1 time of the respective capacity, and the result is more accurate and more efficient.
In order to further improve the accuracy of comparing the cycle lives of different cathode materials, more preferably, at least two groups of cathode materials to be evaluated are respectively prepared, and the steps S2 to S5 are respectively performed on each group of cathode materials to be evaluated; and in step S5, the average charging voltage V of the battery cell corresponding to each positive electrode material to be evaluatedcTaking the average value of the corresponding groups, and the average discharge voltage V of the battery cell corresponding to each anode material to be evaluateddThe average value of each group is taken. Therefore, a plurality of parallel samples such as 2 samples and 3 samples are arranged on each anode material, and the average charge-discharge voltage difference value delta V of the anode material is calculated according to the average value of the cell test results of all the parallel samples of each anode material, so that the test result is more accurate.
As mentioned above, in order to improve the accuracy of the result, it is necessary to assemble different cathode materials according to the rest materials for the same cell, and the rest materials for the specific cell may be conventional materials in the art, for example, in step S2, the conductive agent is one or more of conductive carbon black, carbon nanotube, and graphene, and the binder is one or more of Kynar761A, PVDF, and HSV 900.
Similarly, the proportion of the materials in the assembling process is the same, and preferably, the weight ratio of the positive electrode material to the conductive agent to the binder is (95-97): (1.2-1.8): 2-3. The ratio was as 96:1.5:2.5.
The positive electrode current collector includes, but is not limited to, an aluminum foil, a carbon-coated aluminum foil, or a composite polyimide aluminum foil. Negative electrode materials include, but are not limited to, artificial graphite, natural graphite, or mesocarbon microbeads. The negative current collector includes, but is not limited to, copper foil, carbon-coated copper foil, or aluminum foil. The electrolyte includes, but is not limited to, lithium hexafluorophosphate, a mixed solvent of ethylene carbonate and diethyl carbonate, lithium hexafluorophosphate, an ethylene carbonate solvent or a lithium tetrafluoroborate salt, a mixed solvent of dimethyl carbonate and ethylene carbonate.
The above evaluation method is suitable for the qualitative comparison of the cycle life of various cathode materials, preferably, the cathode material includes, but is not limited to, lithium iron phosphate, lithium nickelate or lithium nickel cobalt manganese oxide.
In the process of specifically assembling the battery core, the whole manufacturing and process can be controlled to be the same, which is understood by those skilled in the art and will not be described herein again.
In a word, the method can judge the cycle life difference between the anode materials through data processing after a few cycles, can greatly shorten the evaluation time compared with the traditional evaluation methods such as long cycle and the like, reduces the evaluation period from several months to several days, greatly improves the evaluation efficiency, saves huge evaluation and manufacturing cost, has the advantage of strong repeatability, and provides a favorable evaluation tool for the development of the anode materials.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
1. LiNi as a positive electrode material was prepared from A and B6CoMn3O2；
2. LiNi of positive electrode materials of manufacturers A and B to be evaluated6CoMn3O2Mixing the conductive carbon black and the PVDF according to the weight ratio of 96:1.5:2.5, stirring in NMP to form slurry, and coating the slurry on a conductive aluminum foil; the negative electrode keeps the same type of artificial graphite, and the artificial graphite, the conductive carbon black and the CMC are mixed according to the weight ratio of 96:1:3, and are uniformly mixed with deionized water to be coated on the copper foil; the battery cell is assembled by the procedures of drying, die cutting, assembling, 1 mol of lithium hexafluorophosphate, ethylene carbonate and diethyl carbonate in the volume ratio of 1:2, formation and the like. Only the positive electrode material is changed in the period, the other materials and the manufacturing process are kept unchanged, the 5.2Ah soft package battery cell is manufactured, the battery cell of the positive electrode material of the manufacturer A is marked as A, and three parallel samples are manufactured, namely A1, A2 and A3. The cell of the anode material of manufacturer B was marked as B, and three parallel samples were made, B1, B2, and B3.
3. Respectively calibrating the capacity of the A sample and the B sample as CaAnd CbThen using 1C respectivelyaAnd 1CbThe cells of the samples a and B are subjected to 25 ℃ cycling for 145 circles (it should be noted that, in actual judgment, the following data of any circle within 145 circles, for example, the following data of only the 20 th circle, are used to calculate Δ V of each cell, where the 145 circles are cycled to calculate the following Δ V at different cycles, so as to prove that the evaluation of the invention performed at any number of circles within 1 to 145 has accuracy and reliability).
4. And (3) respectively processing data of the sample A and the sample B: extraction of all turns of the charge capacity Q of the two sample testscCharging energy EcDischarge capacity QdEnergy of discharge Ed. For A sample Vac＝Ea c/Qa cTo obtain Vac is the average voltage of charge; vad＝Ea d/Qa dTo obtain Vad is the average discharge voltage; Δ Va＝Va c—Va d. For B sample Vbc＝Eb c/Qb cTo obtain Vbc is the average voltage of charge; vbd＝Eb d/Qb dTo obtain Vbd is the average discharge voltage; Δ Vb＝Vbc-Vb d. (the Δ V values for the different groups of samples A1, A2, A3, B1, B2, B3 were all passed through V herec－VdAnd calculating to prove that the delta V between the parallel sample A and the parallel sample B is stable under different cycle numbers of 1-145, and the comparison between the quality and the quality can be realized only by calculating the delta V average value of the parallel samples under the fixed cycle number, particularly the V of the sample AcV for samples A1, A2, A3cMean value, V of BcV of samples B1, B2, B3cAverage value, then comparison, where Δ V is small the longer the cycle life).
5. Comparison of Δ V by calculation or mappingaAnd Δ VbThe size of (A), as shown in FIG. 1, Δ V of the sampleaAll three parallel samples of (2) are less than the DeltaV of the B sampleb. This resulted in a longer cycle life for the anode material from manufacturer a than that from manufacturer B.
In order to verify the accuracy, the present embodiment further tests the variation curve of the capacity retention rate of the battery cell a1 and the battery cell B1 along with the cycle life, and the result is shown in fig. 2, which indicates that the actual cycle life of the battery cell a1 is actually longer than that of the battery cell B1, and the positive electrode material of the manufacturer a is better than that of the manufacturer B, and is consistent with the above evaluation result.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for evaluating the cycle life of a lithium battery positive electrode material is characterized by comprising the following steps:
step S1, preparing at least two anode materials to be evaluated;
step S2, mixing each positive electrode material to be evaluated with the same conductive agent and the same binder according to the same proportion to prepare positive electrode slurry, and coating the positive electrode slurry on the same positive electrode current collector to form a positive electrode;
step S3, assembling the positive electrode made of each positive electrode material to be evaluated, the same negative electrode and the same electrolyte into a battery cell;
step S4, measuring the charging capacity Q of each battery cell under the same multiplying power in the charging and discharging circulation to the nth circlecCharging energy EcDischarge capacity QdAnd discharge energy EdN is any integer between 1 and 145;
step S5, acquiring the average charging voltage V of each battery cell according to the following formulacAnd discharge average voltage Vd：
Vc＝Ec/Qc
Vd＝Qd/Qc
Step S6, obtaining a charge-discharge average voltage difference Δ V between the battery cells, where Δ V is Vc－Vd；
Step S7, comparing the average charge-discharge voltage difference Δ V of each of the battery cells, where the battery cells with smaller average charge-discharge voltage difference Δ V have longer cycle life of the positive electrode material to be evaluated.
2. The method according to claim 1, wherein n is any integer between 20 and 80.
3. The method of claim 1, wherein in the step S3, the capacity C of each cell is measured, and then the charging capacity Q of each cell in a charge-discharge cycle to the nth circle under a multiplying power of 0.1-5C is measuredcThe charging energy EcThe discharge capacity QdAnd said discharge energy Ed。
4. The method according to any one of claims 1 to 3, characterized in that at least two sets of each of the positive electrode materials to be evaluated are prepared, respectively, and the steps S2 to S5 are performed for each set of the positive electrode materials to be evaluated, respectively;
and in the step S5, the average charging voltage V of the battery cell corresponding to each positive electrode material to be evaluatedcTaking the average value of the corresponding groups, and obtaining the average discharge voltage V of the battery cell corresponding to each anode material to be evaluateddThe average value of each group is taken.
5. The method according to any one of claims 1 to 3, wherein in the step S2, the conductive agent is one or more of conductive carbon black, carbon nanotubes and graphene, and the binder is one or more of Kynar761A, PVDF and HSV 900.
6. The method of claim 5, wherein the weight ratio of the positive electrode material to the conductive agent to the binder is (95-97): 1.2-1.8: 2-3.
7. The method according to any one of claims 1 to 3, wherein the positive electrode current collector is an aluminum foil, a carbon-coated aluminum foil, or a composite polyimide aluminum foil.
8. The method according to any one of claims 1 to 3, wherein the positive electrode material is lithium iron phosphate, lithium nickelate or lithium nickel cobalt manganese.
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