CN106404584A - Evaluation method for dry mixing uniformity of admixture slurry powder used for lithium ion battery - Google Patents
Evaluation method for dry mixing uniformity of admixture slurry powder used for lithium ion battery Download PDFInfo
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Abstract
The invention discloses an evaluation method for the dry mixing uniformity of admixture slurry powder used for a lithium ion battery. The method comprises the following concrete steps: successively adding a dry powder material and magnetic iron powder in lithium ion battery slurry into a stirrer for stirring; randomly taking n powder samples, separately weighing each powder sample, removing magnetic iron powder in each powder sample through suction by a Gauss magnetic bar, then weighing the left samples and calculating the coefficient of variation of material mixing uniformity according to a formula; and determining the dry mixing uniformity of the admixture slurry powder according to the coefficient of variation, wherein the dry mixing uniformity of the admixture slurry powder is good if the coefficient of variation is less than 10%, and the smaller the coefficient of variation is, the more uniform the dry mixing of the admixture slurry powder is. According to the invention, the coefficients of variation of the magnetic iron powder in mixed materials with different stirring parameters are tested, so stirring parameters for more uniform mixing of different lithium ion battery materials can be accurately and efficiently evaluated; and thus, reliability in the consistency of the electrochemical performance like internal resistance and capacity of lithium ion batteries is guaranteed.
Description
Technical field
The present invention relates to lithium ion battery processing technique field, more particular to one kind are made using magnetic material removal method
Evaluation method for powder uniformity in lithium ion battery powder dry mixing process.
Background technology
Have been widely used because lithium ion battery has high-energy-density, wide temperature working range and superior cycle performance
On portable computer, camera, video camera, electric tool, pure battery and hybrid vehicle, and will be in artificial satellite, boat
Empty space flight and energy storage aspect find application, and to solve the problems such as international energy resource consumption occurring at present and environmental pollution.
Lithium ion battery most important step in process for making is slurry mixing, agitating procedure, lithium ion battery
Slurry include solvent (deionized water, N methyl pyrrolidone), active material (positive electrode active materials be LiFePO4, cobalt acid
Lithium, LiMn2O4 etc.；Negative active core-shell material is graphite, silica-base material etc.), conductive agent, binding agent etc., usually first by active material
The dry powder materials such as material, binding agent and conductive agent are dry mixed, and then add solvent and make cell size.But if dry powder material
It is dry mixed uneven, then can affect the uniformity of the chemical properties such as internal resistance, the capacity of battery, thus causing electrokinetic cell electronic
The problems such as automobile application field pressure reduction uniformity is poor.And the uniformity not being directed to cell size mixing at present is judged
Or evaluation method.
Content of the invention
The purpose of the present invention is for above-mentioned technical problem, and spy provides a kind of lithium ion battery dry powder blend stirring
The evaluation method of the process uniformity, provides reliable foundation for different material slurry-stirring process parameter.
Technical scheme is as follows：A kind of lithium ion battery closes the evaluation method that starch material is dry mixed uniformity, its bag
Include following steps：
(1) dry powder material in pulp of lithium ion battery and magnetic powder are sequentially added in mixer；
(2) open mixing and blending machine stirring 10-15min, obtain mixture；
(3) take out n part powder sample at random from the diverse location of mixture, wherein n is more than 2；
(4) every part of powder sample is weighed respectively,
(5) more remaining sample is claimed after the magnetic powder in every part of powder sample being absorbed using Gauss magnetically attractive rod
Weight, then show that in every part of powder sample, the mass ratio shared by magnetic powder is ω1, ω2, ω3……ωn；Then magnetic powder institute
The mean value of the mass ratio accounting for is
(6) standard deviation S and coefficient of variation CV of material mixture homogeneity is calculated respectively by following formula：
Standard deviation：
The coefficient of variation：
If coefficient of variation CV drawing is less than 10%, it is good that lithium ion battery conjunction starch material is dry mixed uniformity；And make a variation
Coefficient is less, and lithium ion battery conjunction starch material is dry mixed more uniform.
Scheme further, in described pulp of lithium ion battery, dry powder material includes active material, conductive agent and binding agent powder
Material, wherein active material includes graphite, LiFePO4, cobalt acid lithium or LiMn2O4；Conductive agent include conductive black, superconduction carbon black,
Gas-phase growth of carbon fibre (VGCF) or Graphene；Binding agent powder includes sodium carboxymethylcellulose (CMC) or Kynoar
(PVDF).
The addition of described magnetic powder accounts for the 2%～5% of dry powder material gross mass.
Granularity D50 of described magnetic powder is 0.5～2um.
Described mixing and blending machine is double-planet power mixer, and it revolves round the sun as 5～25rpm, certainly switchs to 100～1000rpm.
The magnetic field intensity of described Gauss magnetically attractive rod is 8000～12000GS.
The present invention adopts magnetic material removal method as the evaluation side of the lithium ion battery dry powder blend whipping process uniformity
Method, because in lithium ion battery powder, magnetic metal impurity has considerable influence, therefore lithium battery to self-discharge of battery, security performance
Close very strict to magnetic metal impurity control in slurry powder.Therefore we can be miscellaneous using a small amount of magnetic metal of artificial interpolation
Plasmid (as iron oxide etc.) carries out closing slurry batch mixing, then removes magnetic metal impurity using Gauss magnetically attractive rod again.Closing
Sample contained by the magnetic of parameter, diverse location sampling in slurry dry mixing process, if sample mixed is not uniform, is dry mixed for difference
The ratio of impurity differs.The method invented using this can effectively judge that heterogeneity lithium battery powder closes slurry batch mixing mistake
The device parameter of journey, the uniformity for chemical properties such as the internal resistance of lithium ion battery, capacity provides basic basis.
Magnetic powder is added in lithium ion battery dry powder material by way of artificial interpolation by invention, then passes through setting
Different mixing parametric are blended in the side of the calculating in lithium ion battery dry powder material, providing by the present invention making magnetic powder
Method, test magnetic powder, in the mixovariation coefficient of different stirring arrange parameters, evaluates difference such that it is able to accurate and effective
It is more uniform that lithium ion battery material can mix under which kind of mixing parametric, thus in postorder processing, process for making
The uniformity of the chemical properties such as the internal resistance of lithium ion battery, capacity provides guaranteed reliability.
Specific embodiment：
The present invention is described further with the following Examples, and embodiment respectively comprises the following steps that：
Embodiment 1：
Choose lithium ion battery dry powder material, its name of material and design proportioning are as follows, LiFePO4：Superconduction carbon black：Poly-
Vinylidene binding agent=94:2:4, the gross weight of solid mixture is 2kg, i.e. LiFePO4 1.88kg, superconduction carbon black
0.04kg, binding agent 0.08kg；Weigh 4 parts as dry powder raw material by aforementioned proportioning respectively, then respectively it is carried out being dry mixed all
The evaluation test of even property, specific as follows：
1st, in 4 parts of dry powder raw material being separately added in four double-planet power mixers；
2nd, weigh the magnetic powder that four parts of D50 are 0.5um to be separately added in aforementioned four mixer, every part of magnetic powder institute
Account for the 3% of dry powder material quality, that is, magnetic powder quality is 0.06kg；
3rd, it is respectively provided with the stirring hybrid parameter of four mixers, respectively：
Group A：Revolution 15rpm, rotation 300rpm, stir incorporation time t=10min；
Group B：Revolution 15rpm, rotation 500rpm, stir incorporation time t=10min；
Group C：Revolution 20rpm, rotation 500rpm, stir incorporation time t=15min；
Group D：Revolution 20rpm, rotation 800rpm, stir incorporation time t=15min；
4th, stop after stirring mixing, 10 samples are taken respectively to four groups of mixtures；M is designated as to each samples weighing, then
Absorb the magnetic powder in sample using the Gauss magnetically attractive rod for 10000GS for the magnetic field intensity, then weigh again and be designated as m '；
5th, calculate the mass ratio ω shared by magnetic powder in every part of sample；In every group, the mass ratio shared by magnetic powder is flat
Average is；
6th, standard deviation S and coefficient of variation CV of material mixture homogeneity is calculated respectively by following formula：
Standard deviation：
The coefficient of variation：
Then specific experiment data is as shown in the table：
Organize other coefficient of variation for four kinds to be analyzed as follows：
Can be seen that from upper table data：1st, being directed to lithium ion battery dry powder material is LiFePO4：Superconduction carbon black：Gather inclined fluorine
Ethene binding agent=94:2:4, using the mixing parametric of group B, C, D, its coefficient of variation CV is respectively less than 10%, all can reach lithium from
Sub- battery closes starch material and uniformity good purpose is dry mixed.
2nd, the coefficient of variation is less, and lithium ion battery conjunction starch material is dry mixed more uniform, using revolution 20rpm, rotation in group C
The powder that 500rpm, the mixing parametric of stirring incorporation time t=15min are mixed, its coefficient of variation CV is 1.66%, explanation
The mixing uniformity being dry mixed of group C is best.
Embodiment 2：
Choose lithium ion battery dry powder material, graphite：Superconduction carbon black (SP)：Sodium cellulose glycolate (CMC)=96:2:2,
The gross weight of solid mixture is 3kg, weighs 3 parts as dry powder raw material by aforementioned proportioning respectively, then respectively it is done
Mixed uniformity evaluation test, specific as follows：
1st, in 3 parts of dry powder raw material being separately added in four double-planet power mixers；
2nd, weigh the magnetic powder that three parts of D50 are 1.0um to be separately added in above three mixer, every part of magnetic powder institute
Account for the 2% of dry powder material quality, that is, magnetic powder quality is 0.06kg；
3rd, it is respectively provided with the stirring hybrid parameter of three mixers, it is respectively：
Group A：Revolution 10rpm, rotation 300rpm, stir incorporation time t=10min；
Group B：Revolution 15rpm, rotation 300rpm, stir incorporation time t=10min；
Group C：Revolution 15rpm, rotation 500rpm, stir incorporation time t=10min；
4th, stop after stirring mixing, 5 samples are taken respectively to three groups of mixtures；M is designated as to each samples weighing, then adopts
The magnetic powder in sample absorbed by the Gauss magnetically attractive being 12000GS with magnetic field intensity rod, then weighs again and is designated as m '；
5th, calculate the mass ratio ω shared by magnetic powder in every part of sample；In every group, the mass ratio shared by magnetic powder is flat
Average is；
6th, standard deviation S and coefficient of variation CV of material mixture homogeneity is calculated respectively by following formula：
Standard deviation：
The coefficient of variation：
Then specific experiment data is as shown in the table：
Can be seen that from upper table data：For negative pole graphite：Superconduction carbon black (SP)：Sodium cellulose glycolate (CMC)=96:
2:2 formulas, the mixing parametric using group B carries out dry powder blend, and the material mixture homogeneity coefficient of variation is minimum, is 2.27%, from
And illustrate using component B：Revolution 15rpm, rotation 300rpm, its powder of mixing parametric mixing of stirring incorporation time t=10min
Uniformity is best.
Above content is only to patent example of the present invention and explanation, affiliated those skilled in the art couple
Described specific embodiment is made various modifications or supplements or substituted using similar mode, without departing from the present invention
Or surmount scope defined in the claims, the protection domain of patent of the present invention all should be belonged to.
Claims (6)
1. a kind of lithium ion battery close starch material be dry mixed uniformity evaluation method it is characterised in that：Comprise the following steps：
(1) dry powder material in pulp of lithium ion battery and magnetic powder are sequentially added in mixer；
(2) open mixing and blending machine stirring 10-15min, obtain mixture；
(3) take out n part powder sample at random from the diverse location of mixture, wherein n is more than 2；
(4) every part of powder sample is weighed respectively；
(5) more remaining sample is weighed after the magnetic powder in every part of powder sample being absorbed using Gauss magnetically attractive rod,
Then show that in every part of powder sample, the mass ratio shared by magnetic powder is ω1, ω2, ω3……ωn；Then shared by magnetic powder
The mean value of mass ratio be
(6) standard deviation S and coefficient of variation CV of material mixture homogeneity is calculated respectively by following formula：
Standard deviation：
The coefficient of variation：
If coefficient of variation CV drawing is less than 10%, illustrate that lithium ion battery conjunction starch material is dry mixed uniformity good；And make a variation
Coefficient is less, and lithium ion battery conjunction starch material is dry mixed more uniform.
2. evaluation method according to claim 1 it is characterised in that：In described pulp of lithium ion battery, dry powder material includes
Active material, conductive agent and binding agent powder, wherein active material include graphite, LiFePO4, cobalt acid lithium or LiMn2O4；Conductive
Agent includes conductive black, superconduction carbon black, gas-phase growth of carbon fibre or Graphene；Binding agent powder include sodium carboxymethylcellulose or
Kynoar.
3. evaluation method according to claim 1 it is characterised in that：It is total that the addition of described magnetic powder accounts for dry powder material
The 2%～5% of quality.
4. evaluation method according to claim 1 it is characterised in that：Granularity D50 of described magnetic powder is 0.5～2um.
5. evaluation method according to claim 1 it is characterised in that：Described mixing and blending machine stirs for double-planet power
Machine, it revolves round the sun as 5～25rpm, certainly switchs to 100～1000rpm.
6. evaluation method according to claim 1 it is characterised in that：The magnetic field intensity of described Gauss magnetically attractive rod is 8000～
12000GS.
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| CN109211714A (en) * | 2018-10-31 | 2019-01-15 | 桑顿新能源科技有限公司 | A kind of evaluation method of pulp of lithium ion battery stability |
| CN109374467A (en) * | 2018-12-29 | 2019-02-22 | 无锡威孚环保催化剂有限公司 | The method for measuring auto-exhaust catalyst coating uniformity |
| CN109612871A (en) * | 2019-01-15 | 2019-04-12 | 东莞维科电池有限公司 | A kind of test method of lithium cell cathode material mixing uniformity |
| CN109752286A (en) * | 2018-11-20 | 2019-05-14 | 浙江南都电源动力股份有限公司 | Pulp of lithium ion battery disperses homogeneity on-line measuring device and method |
| CN109765139A (en) * | 2019-01-15 | 2019-05-17 | 东莞维科电池有限公司 | A kind of test method of anode material of lithium battery mixing uniformity |
| CN112255560A (en) * | 2020-10-19 | 2021-01-22 | 奇瑞商用车（安徽）有限公司 | Battery core health degree prediction method |
| CN112414898A (en) * | 2020-11-10 | 2021-02-26 | 中国农业科学院农产品加工研究所 | Method for evaluating mixing uniformity of composite powder |
| CN114029334A (en) * | 2021-12-03 | 2022-02-11 | 上海康恒环境修复有限公司 | Method for rapidly measuring mixing uniformity of medicament in contaminated soil remediation construction site |
| CN118113000A (en) * | 2024-01-31 | 2024-05-31 | 成都数智碳合科技有限公司 | Method for realizing automatic compound in intelligent manufacturing |
| CN118113000B (en) * | 2024-01-31 | 2024-11-15 | 成都数智碳合科技有限公司 | Method for realizing automatic compound in intelligent manufacturing |
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Cited By (17)
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| CN108152161A (en) * | 2017-12-13 | 2018-06-12 | 桑顿新能源科技有限公司 | A kind of evaluation method of pulp of lithium ion battery stability |
| CN109211714A (en) * | 2018-10-31 | 2019-01-15 | 桑顿新能源科技有限公司 | A kind of evaluation method of pulp of lithium ion battery stability |
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| CN109752286A (en) * | 2018-11-20 | 2019-05-14 | 浙江南都电源动力股份有限公司 | Pulp of lithium ion battery disperses homogeneity on-line measuring device and method |
| CN109374467A (en) * | 2018-12-29 | 2019-02-22 | 无锡威孚环保催化剂有限公司 | The method for measuring auto-exhaust catalyst coating uniformity |
| CN109765139B (en) * | 2019-01-15 | 2021-08-06 | 东莞维科电池有限公司 | Method for testing mixing uniformity of lithium battery positive electrode material |
| CN109765139A (en) * | 2019-01-15 | 2019-05-17 | 东莞维科电池有限公司 | A kind of test method of anode material of lithium battery mixing uniformity |
| CN109612871A (en) * | 2019-01-15 | 2019-04-12 | 东莞维科电池有限公司 | A kind of test method of lithium cell cathode material mixing uniformity |
| CN109612871B (en) * | 2019-01-15 | 2021-09-21 | 东莞维科电池有限公司 | Method for testing mixing uniformity of lithium battery negative electrode material |
| CN112255560A (en) * | 2020-10-19 | 2021-01-22 | 奇瑞商用车（安徽）有限公司 | Battery core health degree prediction method |
| CN112255560B (en) * | 2020-10-19 | 2024-05-10 | 奇瑞商用车（安徽）有限公司 | Battery cell health degree prediction method |
| CN112414898A (en) * | 2020-11-10 | 2021-02-26 | 中国农业科学院农产品加工研究所 | Method for evaluating mixing uniformity of composite powder |
| CN112414898B (en) * | 2020-11-10 | 2021-12-21 | 中国农业科学院农产品加工研究所 | Method for evaluating mixing uniformity of composite powder |
| US11892384B2 (en) | 2020-11-10 | 2024-02-06 | Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences | Evaluation method of mixing uniformity of composite powder |
| CN114029334A (en) * | 2021-12-03 | 2022-02-11 | 上海康恒环境修复有限公司 | Method for rapidly measuring mixing uniformity of medicament in contaminated soil remediation construction site |
| CN118113000A (en) * | 2024-01-31 | 2024-05-31 | 成都数智碳合科技有限公司 | Method for realizing automatic compound in intelligent manufacturing |
| CN118113000B (en) * | 2024-01-31 | 2024-11-15 | 成都数智碳合科技有限公司 | Method for realizing automatic compound in intelligent manufacturing |
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Application publication date: 20170215 |