CN106018699B - A kind of method of rapid evaluation pulp of lithium ion battery dispersibility - Google Patents
A kind of method of rapid evaluation pulp of lithium ion battery dispersibility Download PDFInfo
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Abstract
The invention discloses a kind of methods of rapid evaluation pulp of lithium ion battery dispersibility, compare step through over sampling, drying test and with Duplicate Samples, complete the dispersibility of rapid evaluation pulp of lithium ion battery.The present invention has the advantages that the present invention is not limited to single carbon to evaluate slurry dispersibility, this method is suitable for the detection of slurry dispersing uniformity and proportioning process optimization containing other any easy blending processes for surveying element.This method is suitable for the slurry dispersibility evaluation of the blending process of multiple material, particularly such as: the slurry uniformity detection and feed proportioning optimization technique of LiFePO4, iron manganese phosphate for lithium, nickel cobalt aluminium ternary material, nickel-cobalt-manganese ternary material, rich lithium material and the ingredient of negative electrode materials multiple material such as their blend positive electrode and lithium titanate, silicon oxygen, alloy anode;This method is not limited to lithium ion battery industry, and this method is suitble to the detection and proportioning process optimization of the blending process slurry uniformity of any industry.
Description
Technical field
The invention belongs to lithium ion battery production technical fields, and in particular to a kind of rapid evaluation pulp of lithium ion battery point
Dissipate the method for property.
Background technique
Recently as the increasingly serious of environmental problem, new energy technology has welcome the spring of development, in numerous new energy
In source technology, lithium ion battery is flourished due to many advantages such as high-energy-density, long-lives.And in lithium
In the practical manufacture of ion battery, many urgent problems to be solved are still faced with, the safety of battery, consistency are always to perplex
The difficulties of battery industry.Solve the problems, such as that battery consistency will be done from the source ingredient of battery production, ingredient is lithium ion
The first step of battery production, and guarantee the basic of battery consistency.It, can be to cell performance if the poor dispersion of cell size
Performance can be caused to cause following influence: (1) battery capacity is inconsistent;(2) internal resistance of cell is inconsistent;(3) battery safety is poor.
So slurry dispersing uniformity directly influences battery with two side terminals and security performance.Literature survey discovery, it is existing
The method about dispersing uniformity of lithium ion battery slurry evaluation registered all exists: (1) time cost is long, cannot supervise in real time
It surveys;(2) uncontrollable factor for evaluating and testing data is more, and data reliability is poor;(3) experience dependence is strong, and slurry can not be uniformly dispersed
Property with one quantify index evaluated.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to which now providing one kind quickly has
The method of effect, the rapid evaluation pulp of lithium ion battery dispersibility of quantifiable index.
In order to solve the above technical problems, the technical solution adopted by the present invention are as follows: a kind of rapid evaluation pulp of lithium ion battery
The method of dispersibility, innovative point are: comparing step through over sampling, drying test and with Duplicate Samples, completion is quickly commented
Estimate the dispersibility of pulp of lithium ion battery;Specific step is as follows:
(1) it samples: being carried out at different jitter times, different location separately sampled;
(2) drying test: being placed in 120 DEG C of baking oven and carry out drying, and the criteria thus the drying time is 2 hours, after drying
It takes out, carries out the test of carbon content;
(3) it compares: being compared by comparison between the data measured and with theoretical carbon content, then with Duplicate Samples
Using standard deviation of the theoretical carbon content between mean value calculation institute measured data, can be commented with the size of standard deviation and variation tendency
The dispersing uniformity of valence slurry.
Further, the carbon content detection method is the analysis of other carbon contents such as carbon and sulfur analytical instrument detection, thermogravimetric analysis
Method.
Further, the theoretical carbon content is during main active material, conductive agent, binder and conjunction are starched
The sum of phosphorus content of all materials such as other additives.
Further, the main active material includes: LiFePO4, iron manganese phosphate for lithium, nickel cobalt aluminium ternary material, nickel
Cobalt-manganese ternary material, the rich cathode material such as the positive electrodes such as lithium material and their blend and lithium titanate, silicon oxygen, alloy anode
Material.
Further, the conductive agent is acetylene black, electrically conductive graphite, conductive black, Super-P, KS-6, VGCF or CNT.
Further, the binder is PVDF5130, PVDFHSV900 or LA133.
Beneficial effects of the present invention are as follows:
(1) present invention is not limited to single carbon to evaluate slurry dispersibility, and this method is suitable for any containing other
Easily survey the detection of slurry dispersing uniformity and proportioning process optimization of the blending process of element.
(2), this method is suitable for the slurry dispersibility evaluation of the blending process of multiple material, particularly such as: LiFePO4,
Iron manganese phosphate for lithium, nickel cobalt aluminium ternary material, nickel-cobalt-manganese ternary material, the rich positive electrodes such as lithium material and their blend and
The slurry uniformity of the ingredients of negative electrode materials multiple material such as lithium titanate, silicon oxygen, alloy anode detects and feed proportioning optimization technique;
(3) this method is not limited to lithium ion battery industry, and this method is suitble to the blending process slurry of any industry uniform
Property detection and proportioning process optimization.
Specific embodiment
Embodiments of the present invention are illustrated by particular specific embodiment below, those skilled in the art can be by this explanation
Content disclosed by book is understood other advantages and efficacy of the present invention easily.
Invention applies the differences of the dispersing uniformity of material carbon elements in the slurry to lead to the carbon containing of samples taken
Measure difference.If carbon has aggregate not to be dispersed in the slurry, carbon content of slurry is necessarily higher at this;Similarly, no group
The phosphorus content of mer portion slurry is necessarily relatively low.The dispersibility of slurry is converted into a quantifiable slurry carbon content by this method
It is evaluated, rapidly and reliably property is high for method.
A kind of method of rapid evaluation pulp of lithium ion battery dispersibility, through over sampling, drying test and and Duplicate Samples into
Row comparison step, completes the dispersibility of rapid evaluation pulp of lithium ion battery;Specific step is as follows:
(1) it samples: being carried out at different jitter times, different location separately sampled;
(2) drying test: being placed in 120 DEG C of baking oven and carry out drying, and criteria thus the drying time is 2 hours, takes out after drying,
Carry out the test of carbon content;
(2) it compares: being compared by comparison between the data measured and with theoretical carbon content, then with Duplicate Samples
Using standard deviation of the theoretical carbon content between mean value calculation institute measured data, can be commented with the size of standard deviation and variation tendency
The dispersing uniformity of valence slurry.
Embodiment 1
For assessing the dispersibility of certain capacity type LiFePO4, the phosphorus content of LiFePO4 is 1.4%, formula are as follows: ferric phosphate
Lithium: Kynoar: conductive black: electrically conductive graphite=93:3:3:1, the finely dispersed theoretical carbon content of slurry are as follows: 6.39%
To the slurry sampling and testing of 2 hours of dispersion: respectively taking four samples at three layers of the upper, middle and lower of size barrel respectively, so
It is dried afterwards according to above-mentioned steps, and carries out carbon content test, test data is as follows:
Above data can be seen that be clearly present in data carbon content be higher than, the data lower than 6.39%, can prove this
There are SP, KS-6 for much reuniting not to be dispersed in slurry, causes the carbon content of the slurry in different location widely different.
Embodiment 2
For assessing the dispersibility of certain capacity type LiFePO4, the phosphorus content of LiFePO4 is 1.4%, formula are as follows: ferric phosphate
Lithium: Kynoar: conductive black: electrically conductive graphite=93:3:3:1, the finely dispersed theoretical carbon content of slurry are as follows: 6.39%
Test is sampled to the slurry after 6 hours of dispersion, data are as follows:
As can be seen that the gap between the carbon content of the slurry after 6 hours of dispersion and theoretical carbon content becomes smaller, and between data
Dispersibility be also improved, standard deviation reduce, but it is pure with the theoretical biggish data of carbon content gap, illustrate disperse 4 hours
The dispersibility of slurry be improved, but there are still the agglomerations of conductive agent for regional area.
Embodiment 3
For assessing the dispersibility of certain capacity type LiFePO4, the phosphorus content of LiFePO4 is 1.4%, formula are as follows: ferric phosphate
Lithium: Kynoar: conductive black: electrically conductive graphite=93:3:3:1, the finely dispersed theoretical carbon content of slurry are as follows: 6.39%
Test is sampled to the slurry after 8 hours of dispersion, data are as follows:
The carbon content of the slurry after dispersing 8 hours be can be seen that substantially close to theoretical carbon content, and consistent between data
Property it is also fine, standard deviation significantly reduce, slurry dispersion it is substantially uniform.
Embodiment 4
For assessing the dispersibility of certain capacity type LiFePO4, the phosphorus content of LiFePO4 is 1.4%, formula are as follows: ferric phosphate
Lithium: Kynoar: conductive black: electrically conductive graphite=93:3:3:1, the finely dispersed theoretical carbon content of slurry are as follows: 6.39%
Test is sampled to the slurry after 10 hours of dispersion, data are as follows:
As can be seen that the carbon content of the slurry after 10 hours of dispersion and the test number of the carbon content of 8 small time of dispersion
It is good close to the consistency between theory carbon content and data according to substantially unchanged.
By above data as can be seen that the optimal decentralized time of the LiFePO 4 material system is 8 hours.
The present invention is not limited to single carbon to evaluate slurry dispersibility, and this method is suitable for containing other any easy surveys
The slurry dispersing uniformity of the blending process of element detects and proportioning process optimization.This method is suitable for the ingredient mistake of multiple material
The slurry dispersibility of journey is evaluated, particularly such as: LiFePO4, iron manganese phosphate for lithium, nickel cobalt aluminium ternary material, nickel-cobalt-manganese ternary material
Material, the rich negative electrode materials multiple material such as the positive electrodes such as lithium material and their blend and lithium titanate, silicon oxygen, alloy anode
Ingredient slurry uniformity detection and feed proportioning optimization technique;This method is not limited to lithium ion battery industry, and this method is suitble to
The detection of the blending process slurry uniformity of any industry and proportioning process optimization.
Above-described embodiment is presently preferred embodiments of the present invention, is not a limitation on the technical scheme of the present invention, as long as
Without the technical solution that creative work can be realized on the basis of the above embodiments, it is regarded as falling into the invention patent
Rights protection scope in.
Claims (6)
1. a kind of method of rapid evaluation pulp of lithium ion battery dispersibility, it is characterised in that: through over sampling, drying test and with
Duplicate Samples compare step, complete the dispersibility of rapid evaluation pulp of lithium ion battery;Specific step is as follows:
Sampling: it is carried out at different jitter times, different location separately sampled;
Drying test: being placed in 120 DEG C of baking oven and carry out drying, and the criteria thus the drying time is 2 hours, takes out after drying, into
The test of row carbon content;
It compares: being compared by comparison between the data measured and with theoretical carbon content, then with theoretical carbon with Duplicate Samples
Content is the standard deviation under the same jitter time of mean value calculation between the carbon determination content data of different location place, when with different dispersions
Between lower standard deviation size and variation tendency can carry out the dispersing uniformity of evaluation slurry.
2. a kind of method of rapid evaluation pulp of lithium ion battery dispersibility according to claim 1, it is characterised in that: institute
The method for stating the test of carbon content is carbon and sulfur analytical instrument detection, thermogravimetric analysis carbon content analysis method.
3. a kind of method of rapid evaluation pulp of lithium ion battery dispersibility according to claim 1, it is characterised in that: institute
Stating theoretical carbon content is the sum of main active material, conductive agent, the phosphorus content of binder.
4. a kind of method of rapid evaluation pulp of lithium ion battery dispersibility according to claim 3, it is characterised in that: institute
Stating main active material includes: LiFePO4, iron manganese phosphate for lithium, nickel cobalt aluminium ternary material, nickel-cobalt-manganese ternary material, rich lithium material
Material and their blend and lithium titanate, silicon oxygen, alloy anode.
5. a kind of method of rapid evaluation pulp of lithium ion battery dispersibility according to claim 3, it is characterised in that: institute
Stating conductive agent is acetylene black, electrically conductive graphite, conductive black, Super-P, KS-6, VGCF or CNT.
6. a kind of method of rapid evaluation pulp of lithium ion battery dispersibility according to claim 3, it is characterised in that: institute
Stating binder is PVDF5130, PVDFHSV900 or LA133.
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CN112285066A (en) * | 2019-07-24 | 2021-01-29 | 天津工业大学 | Method for quantitatively evaluating distribution uniformity degree of titanium powder added into low-solid-phase-content zirconia slurry by laser transmission method |
CN112945791A (en) * | 2021-02-18 | 2021-06-11 | 大连中比动力电池有限公司 | Evaluation method for dispersibility of lithium ion secondary battery slurry |
CN113138138A (en) * | 2021-03-25 | 2021-07-20 | 万向一二三股份公司 | Method for testing mobility of binder in lithium ion battery pole piece |
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CN102207479A (en) * | 2010-03-31 | 2011-10-05 | 深圳市比克电池有限公司 | Method for detecting dispersing uniformity of lithium ion battery slurry |
CN102305812B (en) * | 2011-05-25 | 2013-03-27 | 天津力神电池股份有限公司 | Method for detecting dispersion effect of lithium ion battery slurry on line |
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