CN112984963B - Lithium ion battery cell drying method capable of improving battery cell consistency - Google Patents
Lithium ion battery cell drying method capable of improving battery cell consistency Download PDFInfo
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/04—Heating arrangements using electric heating
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B25/00—Details of general application not covered by group F26B21/00 or F26B23/00
- F26B25/06—Chambers, containers, or receptacles
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B9/00—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards
- F26B9/06—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards in stationary drums or chambers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a lithium ion battery core drying method capable of improving battery core consistency, which is characterized in that a freeze drying method is adopted to dry a lithium ion battery core, and the freeze dehydration method is used for replacing a traditional high-temperature drying method, so that the battery core drying consistency can be improved, the battery core drying time can be greatly shortened, and the battery core competitiveness can be improved.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a lithium ion battery drying method capable of improving battery cell consistency.
Background
The lithium ion cell is a secondary cell capable of being repeatedly charged and discharged and is composed of main components such as cathode and anode plates, a separation film, electrolyte, mechanical parts and the like. In the whole life cycle process of the lithium ion battery cell, particularly in the process of researching the production and manufacturing of the battery cell, the influence of the water content on the quality of the battery cell is great, and the water content is not easy to remove.
At present, the lithium battery industry basically uses high temperature to bake the battery cell so as to achieve the purpose of drying and dewatering, but has several great disadvantages: 1. high temperature and large energy consumption, which basically exceeds 100 ℃; 2. the time is long, the efficiency is low, and generally exceeds 20 h. Due to long-time high-temperature baking, on one hand, the isolating film is easy to shrink or close the holes, and the safety of the battery cell is reduced; on the other hand, the uniformity of water removal of the battery core is poor;
disclosure of Invention
In order to solve the technical problems, the invention provides a lithium ion battery cell drying method capable of improving the consistency of a battery cell, and a freeze dehydration method is used for replacing the traditional high-temperature drying method. The consistency of drying the battery cell is improved, the drying time of the battery cell is greatly shortened, and the competitiveness of the battery cell is improved.
The technical scheme adopted by the invention is as follows:
a lithium ion battery core drying method capable of improving battery core consistency adopts a freeze drying method to dry a lithium ion battery core.
Further, the drying method of the lithium ion battery cell comprises the following steps:
(1) pre-cooling: firstly, cooling the battery cell to 0 +/-5 ℃ at a cooling rate of 0.2 +/-0.05 ℃/min, and preserving heat; then cooling the battery cell to-30 +/-5 ℃ at a cooling rate of 1 +/-0.05 ℃/min, and preserving heat;
(2) vacuum pumping to <200 Pa;
(3) sublimation drying: firstly, heating the battery cell to-15 +/-5 ℃ at a heating rate of 0.2 +/-0.05 ℃/min, and preserving heat; then heating the battery cell to 0 +/-5 ℃ at a heating rate of 1 +/-0.05 ℃/min, and preserving heat;
(4) and (3) resolving and drying: firstly, heating the battery cell to 20 +/-5 ℃ at a heating rate of 1 +/-0.05 ℃/min, and preserving heat; and then heating the battery cell to 45 +/-5 ℃ at a heating rate of 1 +/-0.05 ℃/min, and preserving the temperature.
In the step (1), the time for keeping the temperature of the battery cell at 0 +/-5 ℃ is 1 +/-0.5 h; the heat preservation time at minus 30 plus or minus 5 ℃ is 2 plus or minus 0.5 h.
In the step (3), the heat preservation time is 1 plus or minus 0.5 h.
In the step (3), the vacuum degree is controlled to be less than 50Pa during sublimation drying.
In the step (4), the heat preservation time is 1 plus or minus 0.5 h.
In the step (4), the vacuum degree is controlled to be less than 20Pa during analysis and drying.
According to the invention, the drying of the lithium ion battery cell is realized by controlling the temperature rise and fall speed, the precooling temperature, the sublimation drying temperature and the vacuum degree, and the analysis drying temperature and the vacuum degree in the drying process, the average time consumed in the drying process is about 12.5h, the time is shortened by about half compared with the conventional high-temperature baking process, and no bubbles or bulges appear on the surface of the pole piece in the drying process; the temperature range in the drying process is controlled to be-30-45 ℃, the chemical property and the physical structure of the battery cell are basically not changed, and the water removal consistency is good.
Compared with the prior art, the invention has the following beneficial effects:
1. the dried product keeps the original chemical composition and physical properties;
2. the electrolyte has excellent rehydration property, and is beneficial to the infiltration of subsequent electrolyte;
3. the heat consumption is less at higher temperature;
4. the efficiency is high, and the dewatering time is greatly reduced by a high-temperature method;
5. the dewatering uniformity is high, the consistency of the battery cell is greatly improved, and the matching success rate of the battery cell is improved.
Drawings
Fig. 1 is a data distribution graph of the water content of the cells in example 1 and comparative example 1;
fig. 2 is a data distribution graph of the water content of the cells in example 2 and comparative example 2;
fig. 3 is an SEM image of the positive electrode material before and after freeze-drying of the cell in example 1;
fig. 4 is an SEM image of the negative electrode material before and after freeze-drying of the cell in example 1;
fig. 5 is a data distribution diagram of the capacities of the cells in example 1 and comparative example 1;
fig. 6 is a data distribution diagram of the capacities of the cells in example 2 and comparative example 2;
fig. 7 is a photograph of a cell in example 2;
fig. 8 is a photograph of a cell in comparative example 3.
Detailed Description
The present invention will be described in detail with reference to examples.
The drying equipment is Shanghai leaf Tuotuo YTLG-100F.
The method for measuring the water content of the pole piece by using the Karl Fischer moisture tester comprises the following steps: cutting a sample pole piece into a small sample, sending the small sample into a penicillin bottle, weighing again (weighing an empty bottle before sampling) to obtain the weight of the sample, inputting the weight of the sample into an instrument, and setting parameters: the deviant value is less than or equal to 20ug/min, the extraction time is 400s, and the heating temperature of the card furnace is 170 ℃; and (4) testing standard: the water content is less than 400 ppm.
Example 1: 200Ah lithium iron phosphate hard shell battery cell (freezing dehydration)
A drying method of a 200Ah lithium iron phosphate hard shell battery cell selects 48 assembled battery cells for drying at one time, and comprises the following steps:
(1) putting 48 electric cores into a clamp and a precooling cabin, and setting a precooling flow: firstly, cooling the battery cell to 0 +/-5 ℃ at a cooling rate of 0.2 ℃/min, and preserving heat for 1 +/-0.5 h; then cooling the battery cell to-30 +/-5 ℃ at a cooling rate of 1.05 ℃/min, and preserving heat for 2 +/-0.5 h;
(2) after the pre-cooling is finished, starting a vacuum pump, and vacuumizing to less than 100 Pa; then setting sublimation drying and desorption drying procedures;
(3) sublimation drying is carried out, the temperature rise rate of 0.25 ℃/min is used, the temperature of the battery cell is raised to-15 +/-5 ℃, and the temperature is kept for 1 +/-0.5 h; then heating the battery cell to 0 +/-5 ℃ at the heating rate of 1 ℃/min, and preserving the heat for 1 +/-0.5 h; the vacuum degree is kept to be less than 50Pa in the two temperature rising processes;
(4) analyzing and drying, and then heating the battery cell to 20 +/-5 ℃ at the heating rate of 1.05 ℃/min, and keeping the temperature for 1 +/-0.5 h; the temperature of the battery cell is raised to 45 plus or minus 5 ℃ at the temperature raising rate of 1.05 ℃/min, and the temperature is kept for 1 plus or minus 0.5 h.
And (3) respectively testing the water content data of the anode and cathode pole piece mixed sample at the innermost layer of each battery cell, wherein the data distribution is shown in the attached figure 1, and the related statistical data are shown in the table 1. The total elapsed time for the drying process of this example averaged 13 hours, which was about 60% of the time consumed for the drying process of comparative example 1, with an average water content of 299.6ppm and a standard deviation of 29.89, which is significantly less than that of comparative example 1, and the relevant statistical data are shown in table 1.
And taking the positive and negative electrode plates of the naked electric core before freeze drying and the positive and negative electrode plates of the naked electric core after freeze drying to measure SEM, and finding out that the appearance of the positive and negative electrode materials is not changed through an SEM comparison graph, wherein the relevant data are shown in the attached figures 3 and 4.
The infiltration effect of the battery core is represented by the infiltration time of the electrolyte, and the infiltration effect experiment specifically comprises the following operations: the dried cell of 3ea example 1 and the dried cell of 3ea comparative example 1 were filled with the same amount of electrolyte solution 600 ± 3g, and after standing for 10h, the free electrolyte solution was poured out, and the wetting effect of drying and removing water was found to be significantly better than that of the high temperature drying in comparative example 1 by comparing the amount of free electrolyte solution (the less free electrolyte solution, the better the wetting effect), and the experimental data are shown in table 1.
By comparing the chemical performances of the two drying modes in a normal-temperature capacity test (namely a 1C charging and 1C discharging test), the battery cell capacity performance and the high-temperature dewatering have no obvious difference, and the related data are shown in an attached figure 5.
Example 2: 40Ah lithium iron phosphate aluminum shell battery cell (freezing dehydration)
A drying method for 40Ah lithium iron phosphate aluminum shell battery cells selects 48 assembled battery cells for drying at one time, and comprises the following steps:
(1) putting 48 electric cores into a clamp and a precooling cabin, and setting a precooling flow: firstly, cooling the battery cell to 0 +/-5 ℃ at a cooling rate of 0.15 ℃/min, and preserving heat for 1 +/-0.5 h; then cooling the battery cell to-30 +/-5 ℃ at a cooling rate of 0.95 ℃/min, and preserving heat for 2 +/-0.5 h;
(2) after the pre-cooling is finished, transferring the battery cell to a vacuum freeze drying box, and vacuumizing to less than 100 Pa; then setting sublimation drying and desorption drying procedures;
(3) heating the battery cell to-15 +/-5 ℃ at a heating rate of 0.2 ℃/min, and keeping the temperature for 1 +/-0.5 h; then heating the battery cell to 0 +/-5 ℃ at the heating rate of 1 ℃/min, and preserving the heat for 1 +/-0.5 h; the vacuum degree is kept to be less than 50Pa in the two temperature rising processes;
(4) then heating the battery cell to 20 +/-5 ℃ at the heating rate of 1 ℃/min, and keeping the temperature for 1 +/-0.5 h; the temperature of the battery cell is raised to 45 +/-5 ℃ at the temperature raising rate of 1 ℃/min, and the temperature is kept for 1 +/-0.5 h.
And (3) respectively testing the water content data of the anode and cathode pole piece mixed sample at the innermost layer of each battery cell, wherein the data distribution is shown in the attached figure 2, and the related statistical data are shown in a table 1. The average time consumption of the drying process of this example was 10 hours in total, which is about 50% of the time consumption of the drying process of comparative example 2, and the average time consumption was 21 hours in total, with an average water content of 180.3ppm and a standard deviation of 17.88, which is significantly smaller than that of comparative example 2, and the relevant statistical data are shown in table 1.
3ea dried cell is taken to test the infiltration effect (the liquid injection amount is 120 +/-3 g), and the related data are shown in table 1.
And taking 1ea cell to test the capacity performance, wherein the related data is shown in the attached figure 6.
Comparative example 1: 200Ah lithium iron phosphate hard shell battery cell (high temperature baking)
200Ah lithium iron phosphate hard shell battery cells in the same batch as that in example 1 were used as experimental sample battery cells, and 48 assembled battery cells were selected at a time for experiments.
The experiment comprises the following specific steps:
putting 48 electric cores into a clamp, putting the electric cores into a vacuum baking box, firstly vacuumizing to less than 500Pa, setting the temperature to be 100 +/-5 ℃, baking for 24-48 h, and testing the water content data of the anode and cathode pole piece mixed sample at the innermost layer of each electric core after the completion, wherein the data distribution is shown in the attached figure 1. The average time consumption is 21h, the average water content is 329.4ppm, the standard deviation is 46.76, and relevant statistical data are shown in Table 1.
3ea dried electric core is taken to test infiltration effect (the liquid injection amount is 600 +/-3 g), and relevant data are shown in table 1.
And taking 1ea cell to test the capacity performance, wherein the related data is shown in the attached figure 5.
Comparative example 2: 40Ah lithium iron phosphate aluminum shell battery cell (high temperature baking)
The same batch of 40Ah lithium iron phosphate hard shell cells as in example 2 were used as the experimental sample cells, and 48 assembled cells were selected at a time for the experiment.
The experiment comprises the following specific steps:
putting 48 electric cores into a clamp, putting the electric cores into a vacuum baking box, firstly vacuumizing to less than 1kPa, setting the temperature to be 90 +/-5 ℃, baking for 20-48 h, and testing the water content data of the anode and cathode pole piece mixed sample at the innermost layer of each electric core after the completion, wherein the data distribution is shown in the attached figure 2. The average time consumption is 20h, the average water content is 241.6ppm, the standard deviation is 89.96, and relevant statistical data are shown in Table 1.
3ea dried cell is taken to test the infiltration effect (the liquid injection amount is 120 +/-3 g), and the related data are shown in table 1.
And taking 1ea cell to test the capacity performance, wherein the related data is shown in the attached figure 6.
Comparative example 3: 40Ah lithium iron phosphate aluminum shell battery cell (Freeze drying)
A drying method for 40Ah lithium iron phosphate aluminum shell battery cells selects 48 assembled battery cells for drying at one time, and comprises the following steps:
(1) putting 48 electric cores into a clamp and a precooling cabin, and setting a precooling flow: firstly, cooling the battery cell to 0 +/-5 ℃ at a cooling rate of 1.5 ℃/min, and preserving heat for 1 +/-0.5 h; then cooling the battery cell to-30 +/-5 ℃ at a cooling rate of 5 ℃/min, and preserving heat for 2 +/-0.5 h;
(2) after the pre-cooling is finished, transferring the battery cell to a vacuum freeze drying box, and vacuumizing to less than 100 Pa; subsequently, sublimation drying and desorption drying procedures are set
(3) Heating the battery cell to-15 +/-5 ℃ at a heating rate of 2 ℃/min, and keeping the temperature for 1 +/-0.5 h; then heating the battery cell to 0 +/-5 ℃ at a heating rate of 5 ℃/min, and preserving heat for 1 +/-0.5 h; the vacuum degree is kept to be less than 50Pa in the two temperature rising processes;
(4) then heating the battery cell to 20 +/-5 ℃ at a heating rate of 10 ℃/min, and preserving heat for 1 +/-0.5 h; the temperature of the battery cell is raised to 45 plus or minus 5 ℃ at the heating rate of 10 ℃/min, and the temperature is kept for 1 plus or minus 0.5 h.
Disassemble electric core again after electric core preparation is accomplished, find naked electric core deformation serious, embodiment 2 is more level and more smooth than the naked electric core of comparative example 3. The naked electric core of embodiment 2 is seen in fig. 7, and the naked electric core of comparative example 3 is seen in fig. 8.
TABLE 1
The above detailed description of a method for drying a lithium ion battery capable of improving cell consistency with reference to the embodiments is illustrative and not restrictive, and several embodiments may be enumerated within the scope of the limitations, so that changes and modifications may be made without departing from the spirit of the present invention.
Claims (6)
1. A lithium ion battery cell drying method capable of improving battery cell consistency is characterized by comprising the following steps:
(1) pre-cooling: firstly, cooling the battery cell to 0 +/-5 ℃ at a cooling rate of 0.2 +/-0.05 ℃/min, and preserving heat; then cooling the battery cell to-30 +/-5 ℃ at a cooling rate of 1 +/-0.05 ℃/min, and preserving heat;
(2) vacuum pumping to <200 Pa;
(3) sublimation drying: firstly, heating the battery cell to-15 +/-5 ℃ at a heating rate of 0.2 +/-0.05 ℃/min, and preserving heat; then heating the battery cell to 0 +/-5 ℃ at a heating rate of 1 +/-0.05 ℃/min, and preserving heat;
(4) and (3) resolving and drying: firstly, heating the battery cell to 20 +/-5 ℃ at a heating rate of 1 +/-0.05 ℃/min, and preserving heat; and then heating the battery cell to 45 +/-5 ℃ at a heating rate of 1 +/-0.05 ℃/min, and preserving the temperature.
2. The drying method for the lithium ion battery cell according to claim 1, wherein in the step (1), the cell is kept at 0 ± 5 ℃ for 1 ± 0.5 h; the heat preservation time at minus 30 plus or minus 5 ℃ is 2 plus or minus 0.5 h.
3. The method for drying the lithium ion battery cell according to claim 1, wherein in the step (3), the holding time is 1 ± 0.5 h.
4. The method for drying a lithium ion battery cell according to claim 1, wherein in the step (3), the degree of vacuum is controlled to be <50Pa during sublimation drying.
5. The method for drying the lithium ion battery cell according to claim 1, wherein in the step (4), the holding time is 1 ± 0.5 h.
6. The method for drying a lithium ion battery cell according to claim 1, wherein in the step (4), the degree of vacuum is controlled to be less than 20Pa during the desorption drying.
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| CN104061766B (en) * | 2014-03-27 | 2016-08-24 | 张建岗 | A kind of drying equipment |
| SG11201700725TA (en) * | 2014-07-29 | 2017-02-27 | Agency Science Tech & Res | Method of preparing a porous carbon material |
| CN106310217A (en) * | 2015-06-16 | 2017-01-11 | 北京济美堂医药研究有限公司 | Freeze-drying process for preparation of bortezomib for injection |
| CN105020988A (en) * | 2015-07-27 | 2015-11-04 | 丹东君澳食品有限公司 | Vacuum freeze-drying technological method |
| CN206094751U (en) * | 2016-05-31 | 2017-04-12 | 东莞阿李自动化股份有限公司 | Vacuum drying oven and vacuum chamber |
| CN107195974A (en) * | 2017-05-13 | 2017-09-22 | 合肥国轩高科动力能源有限公司 | Method for improving capacity consistency of lithium ion battery cell |
| CN107546368A (en) * | 2017-09-05 | 2018-01-05 | 沈阳理工大学 | Nickle cobalt lithium manganate ternary based lithium-ion battery positive plate preparation method |
| CN207585232U (en) * | 2017-12-04 | 2018-07-06 | 自贡朗星达科技有限公司 | A kind of battery core drying shed and its system |
| CN108375285B (en) * | 2018-02-10 | 2020-07-31 | 嘉兴晟源工业设计有限公司 | Drying device and drying method for lithium ion power battery |
| CN208254074U (en) * | 2018-04-08 | 2018-12-18 | 深圳市众创赢科技有限公司 | A kind of full-automatic low-temperature high-vacuum baking line |
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| CN110375521A (en) * | 2019-07-24 | 2019-10-25 | 维卡新能源科技(南通)有限公司 | A kind of drying lithium ion battery method |
| CN211782555U (en) * | 2019-12-18 | 2020-10-27 | 慧湿环境科技（上海）有限公司 | High performance lithium cell dewatering drying equipment |
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