CN104880384A - Evaluation method for lithium ion battery anode paste stability - Google Patents
Evaluation method for lithium ion battery anode paste stability Download PDFInfo
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- CN104880384A CN104880384A CN201510242986.8A CN201510242986A CN104880384A CN 104880384 A CN104880384 A CN 104880384A CN 201510242986 A CN201510242986 A CN 201510242986A CN 104880384 A CN104880384 A CN 104880384A
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Abstract
The invention discloses an evaluation method for lithium ion battery anode paste stability. An acid type burette is filled with anode paste, after vertical standing is carried out for 1-5 hours, the paste is measured from the upper end part and the lower end part of the burette respectively, a shear rate-viscosity curve of the paste is measured by using a rheometer, when the coincidence of the shear rate-viscosity curves of the paste on the upper end part and the lower end part is good, the paste stability is shown to be good, otherwise, the paste stability is shown to be poor. According to the evaluation method disclosed by the invention, operation steps are simple and quick, the practicability is high, test results are accurate, the reproducibility is good, and accurate reference can be provided for the evaluation of the paste stability.
Description
Technical field
The present invention relates to technical field of lithium-ion battery, be specifically related to a kind of evaluation method of lithium ion battery anode glue size stability.
Background technology
Along with the exhaustion of traditional energy and becoming increasingly conspicuous of environmental problem, lithium ion battery is more and more subject to the attention of national governments and scientist as the developing direction of new cleaning fuel, is constantly devoted to the lithium ion battery of development research practicality and high efficiency more.Anode sizing agent is the key factor determining performance of lithium ion battery, normally after stirring, is scattered in the solution dispersion system formed in solvent by active substance, cementing agent, conductive agent.But current practical active material such as LiFePO4 dispersiveness is in a solvent all very bad, and in order to pursue excellent chemical property, less to the Particle size requirements of electrode material, but along with diminishing of particle diameter, easily secondary aggregate is formed between active substance and other materials particle, it is uneven, very unstable that serious agglomeration makes slurry disperse equally.The instability of slurry can make the consistance of final battery performance poor, reversible capacity reduces, and therefore forming potential safety hazard with the super-charge super-discharge phenomenon of local, the stability of test evaluation anode sizing agent is most important to guarantee performance of lithium ion battery in process of production as seen.
Although at present about the research of Stability of Slurry is a lot, but still lack very much the method for testing of Stability of Slurry being carried out to science accurate evaluation, after patent CN102539294A proposes to utilize test cathode size to leave standstill in separating funnel, levels slurry particles size difference evaluates cathode size stability, the good stability of slurry.This method has its limitation, be only applicable to test evaluation cathode size, although cathode size stability is relevant with graphite particle diameter, but it is more relevant with particle dispersiveness in a solvent, if even the graphite of same particle size disperses the uneven instability that also can cause slurry, but can not embody this difference on grain graininess rate of change.Patent CN101382489A proposes to utilize the difference of testing size levels slurry backward scattering intensity after centrifugation to evaluate Stability of Slurry.Although this method is convenient but also have its limitation, first on centrifugal rotational speed and centrifugation time, there is no choice criteria, because different slurries has without viscosity, need different centrifugal conditions; Secondly the backward scattering strength difference obtained in the different observed altitude of centrifuge tube is also different, and the repeatability of test result and accuracy are not high.
Summary of the invention
The object of the invention is for Existing Defects, provide a kind of operation steps simple and fast, practical, test result is accurate, and favorable reproducibility, can evaluate the method for lithium ion battery anode glue size stability.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
An evaluation method for lithium ion battery anode glue size stability, comprises the following steps:
(1) get the anode sizing agent after closing slurry, be loaded in acid buret, vertical time of repose is 1-5 hour;
(2) measure the anode sizing agent at position, acid buret top and bottom respectively, use rheometry shear rate-viscosity B coefficent curve;
(3) compare the repeatability of the shear rate-viscosity B coefficent curve at position, top and bottom, when the shear rate-viscograph repeatability of position, top and bottom anode sizing agent is good time, show that this Stability of Slurry is good, otherwise, show the poor stability of this slurry.
Preferably, in the acid buret described in step (1), in standing process, use sealing-plug tight closure upper end open.
Preferably, in step (2), the anode sizing agent of upper-end part of driving can use the sucking-off of glue head dropper, and the anode sizing agent of lower end part can directly be released by rotary glass piston.
Preferably, when measuring in step (2), the flat-disc of diameter 35 mm selected by mould, and disk and sample stage clearance distance are set as 1mm, and during measurement, range of shear rate is set as 0.1-600 1/s, and each measurement uses now gets fresh anode sizing agent.
Beneficial effect of the present invention is: operation steps simple and fast of the present invention, practical, and test result is accurate, favorable reproducibility, can provide accurate reference for the stability evaluating slurry.
Accompanying drawing explanation
Fig. 1 is the shear rate-viscosity B coefficent curve map of anode sizing agent after leaving standstill 1 hour in embodiment 1, and wherein, a1 and a2 is the shear rate-viscosity B coefficent curve of position, buret top and bottom slurry respectively;
Fig. 2 is the shear rate-viscosity B coefficent curve map of anode sizing agent after leaving standstill 3 hours in embodiment 2, and wherein, b1 and b2 is the shear rate-viscosity B coefficent curve of position, buret top and bottom slurry respectively;
Fig. 3 is the shear rate-viscosity B coefficent curve map of anode sizing agent after leaving standstill 5 hours in embodiment 3, and wherein, c1 and c2 is the shear rate-viscosity B coefficent curve of position, buret top and bottom slurry respectively.
Embodiment
Below by embodiment, the present invention will be further described, but embodiment does not limit the scope of the invention.
embodiment 1
Take LiFePO4, SP, KS-6 and PVDF, mass percent is 90:4:1:5, and use NMP as dispersion solvent, theoretical solid content is set as 45%, uses XFZH planetary dispersion stirring vacuum mixer high speed dispersion to stir 2 hours according to technological requirement.Get 100 ml close the anode sizing agent after starching and be loaded in 50 ml acid burets, upper end open position uses sealing-plug tight seal and vertically leaves standstill under being placed in room temperature, glue head dropper sucking-off upper-end part of driving slurry is used respectively after leaving standstill 1 hour, release lower end part slurry by rotary glass piston, measure solid content and the shear rate-viscograph of slurry.
Fig. 1 is the shear rate-viscosity B coefficent curve map of anode sizing agent after leaving standstill 1 hour in embodiment 1, wherein a1 and a2 is the shear rate-viscosity B coefficent curve of position, buret top and bottom slurry respectively, although slurry curve in position, top and bottom is not obvious in low shear rate district viscosity differences as can be seen from this figure, but lower end part viscosity is apparently higher than upper-end part of driving viscosity, illustrate that this slurry only disperses after 2 hours stir uneven, poor stability.
embodiment 2
Take LiFePO4, SP, KS-6 and PVDF, mass percent is 90:4:1:5, and use NMP as dispersion solvent, theoretical solid content is set as 45%, uses XFZH planetary dispersion stirring vacuum mixer high speed dispersion to stir 4 hours according to technological requirement.Get 100 ml close the anode sizing agent after starching and be loaded in 50 ml acid burets, upper end open position uses sealing-plug tight seal and vertically leaves standstill under being placed in room temperature, glue head dropper sucking-off upper-end part of driving slurry is used respectively after leaving standstill 3 hours, release lower end part slurry by rotary glass piston, measure solid content and the shear rate-viscograph of slurry.
Fig. 2 is the shear rate-viscosity B coefficent curve map of anode sizing agent after leaving standstill 3 hours in embodiment 2, wherein b1 and b2 is the shear rate-viscosity B coefficent curve of position, buret top and bottom slurry respectively, the curve of position, top and bottom slurry has minor differences as can be seen from this figure, lower end part viscosity is a little more than upper-end part of driving viscosity, illustrate that this slurry disperses after 4 hours stir comparatively even, stability is better than the slurry in embodiment 1.
embodiment 3
Take LiFePO4, SP, KS-6 and PVDF, mass percent is 90:4:1:5, and use NMP as dispersion solvent, theoretical solid content is set as 45%, uses XFZH planetary dispersion stirring vacuum mixer high speed dispersion to stir 6 hours according to technological requirement.Get 100 ml close the anode sizing agent after starching and be loaded in 50 ml acid burets, upper end open position uses sealing-plug tight seal and vertically leaves standstill under being placed in room temperature, glue head dropper sucking-off upper-end part of driving slurry is used respectively respectively after leaving standstill 5 hours, release lower end part slurry by rotary glass piston, measure solid content and the shear rate-viscograph of slurry.
Fig. 3 is the shear rate-viscosity B coefficent curve map of anode sizing agent after leaving standstill 5 hours in embodiment 3, wherein c1 and c2 is the shear rate-viscosity B coefficent curve of position, buret top and bottom slurry respectively, the curve co-insides of position, top and bottom slurry is good as can be seen from this figure, lower end part viscosity is almost consistent with upper-end part of driving viscosity, illustrate that this slurry disperses after 6 hours stir very even, stability is all better than the slurry in embodiment 1 and embodiment 2.
Claims (4)
1. an evaluation method for lithium ion battery anode glue size stability, is characterized in that, comprises the following steps:
(1) get the anode sizing agent after closing slurry, be loaded in acid buret, vertical time of repose is 1-5 hour;
(2) measure the anode sizing agent at position, acid buret top and bottom respectively, use rheometry shear rate-viscosity B coefficent curve;
(3) compare the repeatability of the shear rate-viscosity B coefficent curve at position, top and bottom, when the shear rate-viscograph repeatability of position, top and bottom anode sizing agent is good time, show that this Stability of Slurry is good, otherwise, show the poor stability of this slurry.
2. the evaluation method of lithium ion battery anode glue size stability according to claim 1, is characterized in that: in the acid buret described in step (1), uses sealing-plug tight closure upper end open in standing process.
3. the evaluation method of lithium ion battery anode glue size stability according to claim 1, it is characterized in that: in step (2), the anode sizing agent of upper-end part of driving can use the sucking-off of glue head dropper, and the anode sizing agent of lower end part can directly be released by rotary glass piston.
4. the evaluation method of lithium ion battery anode glue size stability according to claim 1, it is characterized in that: when measuring in step (2), the flat-disc of diameter 35 mm selected by mould, disk and sample stage clearance distance are set as 1mm, during measurement, range of shear rate is set as 0.1-600 1/s, and each measurement uses now gets fresh anode sizing agent.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105738827A (en) * | 2016-03-28 | 2016-07-06 | 合肥国轩高科动力能源有限公司 | Comprehensive performance evaluation method for conductive slurry of lithium ion battery |
| CN105758766A (en) * | 2016-03-15 | 2016-07-13 | 廊坊立邦涂料有限公司 | Method measuring inter-batch stability of latex paint by using rotational rheometer |
| CN106124363A (en) * | 2016-07-14 | 2016-11-16 | 曙鹏科技（深圳）有限公司 | A kind of evaluating method of lithium ion battery plus-negative plate Stability of Slurry |
| CN107185421A (en) * | 2017-07-18 | 2017-09-22 | 汇森生物设备镇江有限公司 | A kind of accurate liquid mixing system for high viscosity feed liquid |
| CN108169057A (en) * | 2017-12-07 | 2018-06-15 | 惠州拓邦电气技术有限公司 | Pulp of lithium ion battery stability test method and device |
| CN109142149A (en) * | 2018-09-04 | 2019-01-04 | 陕西煤业化工技术研究院有限责任公司 | A method of detection battery slurry dispersion stabilization |
| CN110095380A (en) * | 2019-03-28 | 2019-08-06 | 合肥国轩高科动力能源有限公司 | A kind of method of Fast Evaluation lithium ion battery electrode sizing agent stability |
| CN110296916A (en) * | 2019-05-29 | 2019-10-01 | 合肥国轩高科动力能源有限公司 | A kind of method that the detection of high-pressure solid LiFePO 4 material batch compaction stability determines |
| CN110346243A (en) * | 2019-06-13 | 2019-10-18 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery anode glue size Detection of Stability method |
| CN110869737A (en) * | 2018-02-23 | 2020-03-06 | 株式会社Lg化学 | Method and apparatus for evaluating phase stability of electrode mixture slurry |
| CN111024552A (en) * | 2019-12-25 | 2020-04-17 | 四川新巩固建材有限公司 | Method for detecting viscosity difference of asphalt warm-mixing modifier |
| CN111624136A (en) * | 2020-06-18 | 2020-09-04 | 合肥国轩高科动力能源有限公司 | Method for detecting stability and viscosity of battery slurry |
| CN112014265A (en) * | 2020-08-05 | 2020-12-01 | 中国铝业股份有限公司 | Continuous anode aluminum cell anode paste performance evaluation device and evaluation method |
| CN112198092A (en) * | 2020-08-24 | 2021-01-08 | 浙江南都电源动力股份有限公司 | Method for testing stability of battery slurry |
| CN113075087A (en) * | 2021-04-09 | 2021-07-06 | 芜湖天弋能源科技有限公司 | Electrode paste performance testing device and testing method thereof |
| CN114235902A (en) * | 2021-11-15 | 2022-03-25 | 湖北亿纬动力有限公司 | Method for testing dispersion stability of carbon black |
| US11735735B2 (en) | 2017-09-28 | 2023-08-22 | Lg Energy Solution, Ltd. | Method for predicting processability of electrode slurry and selecting electrode binder |
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| CN105758766A (en) * | 2016-03-15 | 2016-07-13 | 廊坊立邦涂料有限公司 | Method measuring inter-batch stability of latex paint by using rotational rheometer |
| CN105738827B (en) * | 2016-03-28 | 2018-11-02 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery electrocondution slurry comprehensive performance evaluation method |
| CN105738827A (en) * | 2016-03-28 | 2016-07-06 | 合肥国轩高科动力能源有限公司 | Comprehensive performance evaluation method for conductive slurry of lithium ion battery |
| CN106124363A (en) * | 2016-07-14 | 2016-11-16 | 曙鹏科技（深圳）有限公司 | A kind of evaluating method of lithium ion battery plus-negative plate Stability of Slurry |
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| CN108169057B (en) * | 2017-12-07 | 2020-05-22 | 惠州拓邦电气技术有限公司 | Lithium ion battery slurry stability testing method and device |
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| CN110869737B (en) * | 2018-02-23 | 2022-04-19 | 株式会社Lg新能源 | Method and apparatus for evaluating phase stability of electrode mixture slurry |
| CN110869737A (en) * | 2018-02-23 | 2020-03-06 | 株式会社Lg化学 | Method and apparatus for evaluating phase stability of electrode mixture slurry |
| US11456450B2 (en) | 2018-02-23 | 2022-09-27 | Lg Energy Solution, Ltd. | Method and apparatus for evaluating phase stability of electrode mixture slurry |
| CN109142149A (en) * | 2018-09-04 | 2019-01-04 | 陕西煤业化工技术研究院有限责任公司 | A method of detection battery slurry dispersion stabilization |
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| CN110296916A (en) * | 2019-05-29 | 2019-10-01 | 合肥国轩高科动力能源有限公司 | A kind of method that the detection of high-pressure solid LiFePO 4 material batch compaction stability determines |
| CN110346243A (en) * | 2019-06-13 | 2019-10-18 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery anode glue size Detection of Stability method |
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| CN112014265A (en) * | 2020-08-05 | 2020-12-01 | 中国铝业股份有限公司 | Continuous anode aluminum cell anode paste performance evaluation device and evaluation method |
| CN112014265B (en) * | 2020-08-05 | 2024-01-23 | 中国铝业股份有限公司 | Device and method for evaluating anode paste performance of continuous anode aluminum electrolysis cell |
| CN112198092A (en) * | 2020-08-24 | 2021-01-08 | 浙江南都电源动力股份有限公司 | Method for testing stability of battery slurry |
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