CN102368544A - Preparation method of lithium ion battery anode slurry - Google Patents
Preparation method of lithium ion battery anode slurry Download PDFInfo
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- CN102368544A CN102368544A CN201110333459XA CN201110333459A CN102368544A CN 102368544 A CN102368544 A CN 102368544A CN 201110333459X A CN201110333459X A CN 201110333459XA CN 201110333459 A CN201110333459 A CN 201110333459A CN 102368544 A CN102368544 A CN 102368544A
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- Prior art keywords
- slurry
- ion battery
- lithium ion
- solvent
- battery anode
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000006256 anode slurry Substances 0.000 title abstract 4
- 239000002002 slurry Substances 0.000 claims abstract description 42
- 239000002904 solvent Substances 0.000 claims abstract description 31
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000006258 conductive agent Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims description 30
- 239000003292 glue Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- -1 Kynoar Substances 0.000 claims description 6
- 239000011343 solid material Substances 0.000 claims description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 5
- 230000014759 maintenance of location Effects 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 230000033001 locomotion Effects 0.000 abstract description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 abstract description 3
- 239000011267 electrode slurry Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 239000010405 anode material Substances 0.000 abstract 2
- 239000007767 bonding agent Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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 preparation method of lithium ion battery anode slurry with which effective control can be taken upon the consistency of a lithium ion battery in a micro perspective. The lithium ion battery anode slurry is prepared from mixed materials of a solvent, polyvinylidene difluoride, a conductive agent, and a lithium iron phosphate anode material. The preparation method comprises steps that: the solvent, polyvinylidene difluoride, the conductive agent, and the lithium iron phosphate anode material are well mixed under a temperature environment of 65 to 70 DEG C, such that the lithium ion battery anode slurry is prepared. According to the invention, during the whole slurry preparation procedure, the whole slurry system is maintained to be in a constant high temperature; with a method wherein the raw materials and the solvent are added to the slurry system in batches, the viscosity of the slurry system is controlled within a certain range; before a bonding agent is added, all solid powders are premixed by using the solvent, such that the components of the slurry are subject to more severe molecular motions under a temperature higher than that of a common slurry mixing technology. Therefore, electrode slurry with a better consistency in the micro perspective is obtained.
Description
Technical field
The invention belongs to technical field of lithium-ion battery, be specifically related to a kind of preparation method of lithium ion battery anode glue size.
Background technology
Electric automobile has characteristics such as low-carbon environment-friendly, is automobile development in future direction, and along with the development of electric vehicle engineering, and automobile vendor is also urgent day by day to the requirement that the performance of used for electric vehicle lithium-ion-power cell improves.The consistency problem of used for electric vehicle lithium-ion-power cell is the maximum bottleneck of restriction whole electric automobile technical development.
Solve the conforming method of cell at present and mainly concentrate on following several kinds of modes: 1, adopt high-precision coating machine to improve consistency and the smear left-right symmetric property that battery pole piece laterally reaches dressing amount on the longitudinal direction; 2, take the production facility of various precisions to improve the consistency between single pole piece; 3, adopt high accuracy chip select equipment that pole piece weight is selected, to satisfy the consistency of battery pole piece.Said method is only controlled the battery pole piece consistency from macroscopical aspect; And can not solve the problem on the microcosmic such as the dispersiveness of electrode material and conductive agent, binding agent, and the consistency on the electrode microcosmic influences the most directly key factor of battery consistency exactly.
The consistency of electrode is by the character decision of slurry.Traditional slurry-stirring process is in manufacturing process; Whole system is in lower temperature; Under this low-temperature condition, the molecular diffusion of components such as positive electrode, PVDF, conductive agent (SP or CNT), solvent is slow, only relies on machinery that above-mentioned substance is mixed each other when closing slurry; The effect of disperseing like this is poor, causes the consistency of microcosmic spreading mass very undesirable.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of the lithium ion battery anode glue size that can aspect microcosmic, control effectively to battery consistency.
The preparation method of lithium ion battery anode glue size of the present invention; This lithium ion battery anode glue size is mixed by solvent, Kynoar, conductive agent, lithium iron phosphate positive material; The key of its preparation method is that said solvent, Kynoar, conductive agent, lithium iron phosphate positive material are in 65 ℃～70 ℃ temperature environment, to stir, and processes lithium ion battery anode glue size.
Adopt and to close the mode that slurry stirs under the hot conditions, under high temperature (65 ℃～70 ℃) condition, can make the diffusion motion of each component molecule of slurry more violent, thereby it is more even to impel component to disperse, and then guarantees the consistency of battery pole piece from microcosmic.
Further, said solvent is the N-methyl pyrrolidone.
Further, said conductive agent is one or several in conductive black, the electrically conductive graphite.
Further, the weight proportion of said Kynoar, conductive agent, lithium iron phosphate positive material is a Kynoar: conductive agent: lithium iron phosphate positive material=3%～4%:2～4%:92%～95%; Said solvent quality: solid material quality=45%～55%, said solid material quality are the gross mass of Kynoar, conductive agent and lithium iron phosphate positive material.
Specifically, the preparation method of above-mentioned lithium ion battery anode glue size comprises the steps:
A: in the planet agitator, add the solvent of 20～30Wt%, in 65 ℃～70 ℃ temperature environment, stir, solvent temperature is promoted to 65～68 ℃;
B: stop to stir, Kynoar is all added in the planet agitator, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the first order slurry of 2000～3500mpa.s;
C: in the first order slurry that makes, add the solvent of 20%～30Wt% and whole conductive agents, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the second level slurry of 4300～5500mpa.s;
D: in the second level slurry that makes, add solvent and the lithium iron phosphate positive material of 20%～30Wt%, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the third level slurry of 5500～7000mpa.s; The lithium iron phosphate positive material that adds accounts for 50% of whole lithium iron phosphate positive materials;
E: in the third level slurry that makes, add solvent and the 50% remaining lithium iron phosphate positive material of 10%～40Wt%, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the fourth stage slurry of 6500～7500mpa.s;
F: the fourth stage slurry that makes is cooled off in 18 ℃～20 ℃ temperature environment, and when the temperature of fourth stage slurry drops to below 45 ℃, begin to vacuumize, make the lithium ion battery anode glue size that viscosity is 7800～8300mpa.s.
In the said F step, vacuum degree require for-0.08MPa～-0.1MPa, the vacuum retention time is not less than 1 hour.
In said each step, be that utilization is controlled the stirring ambient temperature to the method that the planet agitator feeds the thermostatical circulating water of relevant temperature.
The preparation method of lithium ion battery anode glue size of the present invention is in whole slurry manufacturing process; Make whole slurry system be in the temperature constant state under the higher temperature through control slurry system temperature; Utilize viscosity Control that the method that in slurry system, drops into raw material and solvent in batches makes slurry system within the specific limits simultaneously; And all solid powders will use solvent to carry out premix before dropping into glue; Make the more violent motion of carrying out molecular level under of each component of slurry, thereby obtain the more outstanding electrode slurry of consistency of microcosmic aspect than the higher temperature conditions of conventional slurry-stirring process.
Embodiment
Below through to the description of embodiment, the effect of mutual alignment between the shape of specific embodiments of the invention such as related each member, structure, the each several part and annexation, each several part and operation principle etc. are done further to specify.
Embodiment 1:
The lithium ion battery anode glue size of present embodiment is by as the N-methyl pyrrolidone of solvent, Kynoar, mix as conductive black, the lithium iron phosphate positive material of conductive agent; The weight proportion of Kynoar, conductive agent, lithium iron phosphate positive material is a Kynoar: conductive agent: lithium iron phosphate positive material=4%:4%:92%; Solvent quality: solid material quality=50%, said solid material quality are the gross mass of Kynoar, conductive agent and lithium iron phosphate positive material.
The preparation method's of the lithium ion battery anode glue size of present embodiment key is that said solvent, Kynoar, conductive agent, lithium iron phosphate positive material are in 65 ℃～70 ℃ temperature environment, to stir; Process lithium ion battery anode glue size, comprise the steps: specifically
A: in the planet agitator, add the N-methyl pyrrolidone of 25Wt%, logical 65 ℃～70 ℃ thermostatical circulating water, the flow velocity of water is 2.5～3.5m
3/ min open to stir, and sets revolution 5HZ～10HZ, disperses 5HZ～10HZ, with N-methyl pyrrolidone temperature increase to 65～68 ℃;
B: stop to stir, Kynoar is all added in the planet agitator, logical 65 ℃～70 ℃ thermostatical circulating water, the flow velocity of water is 2.5～3.5m
3/ min opens and stirs, and sets revolution 30HZ～40HZ, disperses 30HZ～40HZ, stirs 3～5 hours, and making temperature is 65～68 ℃, and viscosity is the first order slurry of 2000～3500mpa.s;
C: in the first order slurry that makes, add the solvent of 25Wt% and whole conductive agents, logical 65 ℃～70 ℃ thermostatical circulating water, the flow velocity of water is 1.8～2.2m
3/ min opens and stirs, and sets revolution 30～35HZ, disperses 30～35HZ, stirs 1～3 hour, and making temperature is 65～68 ℃, and viscosity is the second level slurry of 4300～5500mpa.s;
D: in the second level slurry that makes, add solvent and the lithium iron phosphate positive material of 25Wt%, logical 65 ℃～70 ℃ thermostatical circulating water, the flow velocity of water is 1.8～2.2m
3/ min opens and stirs, and sets revolution 30～35HZ, disperses 30～35HZ, stirs 1～1.5 hour, and making temperature is 65～68 ℃, and viscosity is the third level slurry of 5500～7000mpa.s; The lithium iron phosphate positive material that adds accounts for 50% of whole lithium iron phosphate positive materials;
E: in the third level slurry that makes, add solvent and the 50% remaining lithium iron phosphate positive material of 10%～40Wt%, logical 65 ℃～70 ℃ thermostatical circulating water, the flow velocity of water is 2.0～2.4m
3/ min opens and stirs, and sets revolution 30～35HZ, disperses 30～35HZ, stirs 2～2.5 hours, and making temperature is 65～68 ℃, and viscosity is the fourth stage slurry of 6500～7500mpa.s;
F: with the thermostatical circulating water of logical 18 ℃～20 ℃ of planet agitator, the flow velocity of water is 3.0～3.5m
3/ min begins to vacuumize when the temperature of fourth stage slurry drops to below 45 ℃, vacuum degree require for-0.08MPa～-0.1MPa, the vacuum retention time is not less than 1 hour, makes the lithium ion battery anode glue size that viscosity is 7800～8300mpa.s.
Claims (7)
1. the preparation method of a lithium ion battery anode glue size; This lithium ion battery anode glue size is mixed by solvent, Kynoar, conductive agent, lithium iron phosphate positive material; Its preparation method is characterised in that said solvent, Kynoar, conductive agent, lithium iron phosphate positive material are in 65 ℃～70 ℃ temperature environment, to stir, and processes lithium ion battery anode glue size.
2. the preparation method of lithium ion battery anode glue size according to claim 1 is characterized in that said solvent is the N-methyl pyrrolidone.
3. the preparation method of lithium ion battery anode glue size according to claim 1 is characterized in that said conductive agent is one or several in conductive black, the electrically conductive graphite.
4. according to the preparation method of claim 1 or 2 or 3 described lithium ion battery anode glue sizes, the weight proportion that it is characterized in that said Kynoar, conductive agent, lithium iron phosphate positive material is a Kynoar: conductive agent: lithium iron phosphate positive material=3%～4%:2～4%:92%～95%; Said solvent quality: solid material quality=45%～55%, said solid material quality are the gross mass of Kynoar, conductive agent and lithium iron phosphate positive material.
5. the preparation method of lithium ion battery anode glue size according to claim 1 is characterized in that comprising the steps:
A: in the planet agitator, add the solvent of 20～30Wt%, in 65 ℃～70 ℃ temperature environment, stir, solvent temperature is promoted to 65～68 ℃;
B: stop to stir, Kynoar is all added in the planet agitator, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the first order slurry of 2000～3500mpa.s;
C: in the first order slurry that makes, add the solvent of 20%～30Wt% and whole conductive agents, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the second level slurry of 4300～5500mpa.s;
D: in the second level slurry that makes, add solvent and the lithium iron phosphate positive material of 20%～30Wt%, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the third level slurry of 5500～7000mpa.s; The lithium iron phosphate positive material that adds accounts for 50% of whole lithium iron phosphate positive materials;
E: in the third level slurry that makes, add solvent and the 50% remaining lithium iron phosphate positive material of 10%～40Wt%, in 65 ℃～70 ℃ temperature environment, stir, making temperature is 65～68 ℃, and viscosity is the fourth stage slurry of 6500～7500mpa.s;
F: the fourth stage slurry that makes is cooled off in 18 ℃～20 ℃ temperature environment, and when the temperature of fourth stage slurry drops to below 45 ℃, begin to vacuumize, make the lithium ion battery anode glue size that viscosity is 7800～8300mpa.s.
6. the preparation method of lithium ion battery anode glue size according to claim 5 is characterized in that in the said F step, vacuum degree require for-0.08MPa～-0.1MPa, the vacuum retention time is not less than 1 hour.
7. according to the preparation method of claim 5 or 6 described lithium ion battery anode glue sizes, it is characterized in that in said each step, is that utilization is controlled the stirring ambient temperature to the method that the planet agitator feeds the thermostatical circulating water of relevant temperature.
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| CN201110333459A CN102368544B (en) | 2011-10-28 | 2011-10-28 | Preparation method of lithium ion battery anode slurry |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103094556A (en) * | 2013-01-30 | 2013-05-08 | 浙江超威创元实业有限公司 | Method for preparing positive electrode slurry of lithium ion battery |
| CN103545487A (en) * | 2013-10-28 | 2014-01-29 | 深圳格林德能源有限公司 | Preparation method of high-viscosity ultra-fine dispersion anode slurry of lithium ion battery |
| CN103618063A (en) * | 2013-09-26 | 2014-03-05 | 奇瑞汽车股份有限公司 | Lithium ion power battery positive electrode slurry and slurry mixing method |
| CN103887556A (en) * | 2014-03-13 | 2014-06-25 | 深圳格林德能源有限公司 | Power energy storage polymer lithium ion battery and preparation method thereof |
| CN106159270A (en) * | 2015-03-25 | 2016-11-23 | 北京波士顿动力电池有限公司 | A kind of power lithium-ion battery pair conductive agent negative poles |
| CN109786740A (en) * | 2018-12-20 | 2019-05-21 | 惠州亿纬锂能股份有限公司 | The preparation method of lithium battery anode slurry |
| CN111883738A (en) * | 2020-08-02 | 2020-11-03 | 江西安驰新能源科技有限公司 | High-temperature low-energy-consumption positive pole slurry mixing process |
| CN112179894A (en) * | 2019-07-03 | 2021-01-05 | 万向一二三股份公司 | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery |
| CN112952090A (en) * | 2021-01-26 | 2021-06-11 | 惠州亿纬锂能股份有限公司 | Preparation method of lithium battery positive electrode slurry and lithium battery positive electrode slurry prepared by same |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103094556A (en) * | 2013-01-30 | 2013-05-08 | 浙江超威创元实业有限公司 | Method for preparing positive electrode slurry of lithium ion battery |
| CN103618063A (en) * | 2013-09-26 | 2014-03-05 | 奇瑞汽车股份有限公司 | Lithium ion power battery positive electrode slurry and slurry mixing method |
| CN103618063B (en) * | 2013-09-26 | 2016-05-11 | 奇瑞新能源汽车技术有限公司 | A kind of lithium ion power battery cathode slurry and close paste-making method |
| CN103545487A (en) * | 2013-10-28 | 2014-01-29 | 深圳格林德能源有限公司 | Preparation method of high-viscosity ultra-fine dispersion anode slurry of lithium ion battery |
| CN103545487B (en) * | 2013-10-28 | 2014-09-17 | 深圳格林德能源有限公司 | Preparation method of high-viscosity ultra-fine dispersion anode slurry of lithium ion battery |
| CN103887556A (en) * | 2014-03-13 | 2014-06-25 | 深圳格林德能源有限公司 | Power energy storage polymer lithium ion battery and preparation method thereof |
| CN103887556B (en) * | 2014-03-13 | 2015-08-19 | 深圳格林德能源有限公司 | A kind of power energy storage polymer Li-ion battery and preparation method |
| CN106159270A (en) * | 2015-03-25 | 2016-11-23 | 北京波士顿动力电池有限公司 | A kind of power lithium-ion battery pair conductive agent negative poles |
| CN109786740A (en) * | 2018-12-20 | 2019-05-21 | 惠州亿纬锂能股份有限公司 | The preparation method of lithium battery anode slurry |
| CN112179894A (en) * | 2019-07-03 | 2021-01-05 | 万向一二三股份公司 | Method for detecting free iron in lithium iron phosphate anode slurry of lithium ion battery |
| CN111883738A (en) * | 2020-08-02 | 2020-11-03 | 江西安驰新能源科技有限公司 | High-temperature low-energy-consumption positive pole slurry mixing process |
| CN112952090A (en) * | 2021-01-26 | 2021-06-11 | 惠州亿纬锂能股份有限公司 | Preparation method of lithium battery positive electrode slurry and lithium battery positive electrode slurry prepared by same |
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