CN104733689A - Preparation method for lithium iron phosphate positive electrode of lithium ion battery - Google Patents
Preparation method for lithium iron phosphate positive electrode of lithium ion battery Download PDFInfo
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- CN104733689A CN104733689A CN201310710453.9A CN201310710453A CN104733689A CN 104733689 A CN104733689 A CN 104733689A CN 201310710453 A CN201310710453 A CN 201310710453A CN 104733689 A CN104733689 A CN 104733689A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
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Abstract
The invention discloses a preparation method for a lithium iron phosphate positive electrode of a lithium ion battery. The preparation method overcomes the problems of uneasy dispersion of solid components and hard thorough drying of positive electrodes in preparation of lithium iron phosphate positive electrodes of lithium ion batteries in the prior art. The preparation method mainly comprises the following steps: (1) weighing materials; (2) preparation of a premix; (3) primary dispersion; (4) secondary dispersion; (5) slow stirring; (6) coating; and (7) drying in segments. The preparation method provided by the invention has the advantages of simple steps, uniform dispersion of each solid component in the process of preparation and thorough drying of pole pieces; and the battery prepared from the positive electrode has good electrochemical performance.
Description
Technical field
The present invention relates to technical field of lithium ion, especially relate to a kind of preparation method of cathode of lithium iron phosphate lithium ion battery.
Background technology
At present according to kind and the processing technology of solvent in lithium iron phosphate battery anode formula slurry, anode sizing agent can divide oil system's (NMP is as solvent) slurry and water system (deionized water is as solvent) slurry, aqueous slurry is not owing to relating to solvent recovery and problem of environmental pollution, and low price, homogenate is subject to large how many lithium cell factory by advantages such as environmental constraints are less and favors, but the conductive agent in aqueous positive-pole slurry, the solid matters such as positive active material are not easily dispersed, make the consistency of aqueous positive-pole slurry poor, stability is not high, easy generation sedimentation, thus cause battery reversible capacity less, cycle performance is not good, greatly have impact on battery capacity and cycle life, therefore be badly in need of solving the scattering problem of solid matter in aqueous positive-pole slurry in water paste, in addition, when preparing the lithium iron phosphate battery anode adopting water paste, usually be all freeze-day with constant temperature, cause positive pole not easily bone dry.
Such as, Chinese patent application publication No.: CN102306782A, Shen Qing Publication day: on January 4th, 2012, disclose a kind of lithium iron phosphate battery anode and preparation method thereof, this positive pole comprises the component of following weight percents: aqueous binders 0.5% ~ 1%; Conductive agent 1% ~ 3%; Crystalline flake graphite 0.5% ~ 2%; LiFePO4 90% ~ 97%; Water-base cement 1% ~ 3%, the preparation method of this positive pole is mixed by high speed and stirring at low speed for each component being put into mixer.Its weak point is, first, the binding agent in this anode formula is modification polyethylene glycol oxide, and modification polyethylene glycol oxide adhesion strength is inadequate, therefore need to improve adhesion strength by adding water-base cement, and after adding water-base cement, in slurry, each solid constituent is more not easily disperseed, and the stability of slurry is not high, easy generation sedimentation, cause battery reversible capacity less, cycle performance is not good, greatly have impact on battery capacity and cycle life.
Summary of the invention
The present invention is that the cathode of lithium iron phosphate lithium ion battery each solid constituent in preparation process in order to solve prior art is not easily disperseed, the problem of positive pole not easily bone dry, provide a kind of preparation method of cathode of lithium iron phosphate lithium ion battery, this preparation method's processing step is simple, in preparation process, each solid constituent is uniformly dispersed, pole piece is thoroughly dry, and the battery performance that the positive pole utilizing the present invention to obtain is made is good.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for cathode of lithium iron phosphate lithium ion battery, comprises the following steps:
(1) weighing: in the gross mass of anode sizing agent, takes each component by following mass percentage: LiFePO4 45 ~ 50%, conductive agent 2 ~ 3%, aqueous binders 2 ~ 3%, ethanol 3 ~ 5%, and surplus is deionized water.Adopt water paste in the present invention, this cost of sizing agent is low, stability and excellent dispersion, and obtained battery performance is good.
(2) premix preparation: after being mixed with conductive agent by ethanol, add aqueous binders and portions of de-ionized water, being milled to fineness of materials is 5 ~ 10 μm, obtains premix.In the present invention, the step of batch mixing is very crucial, first ethanol must be mixed with conductive agent in the present invention, because conductive agent is difficult in water dispersed, first ethanol is mixed with conductive agent, the moistening conductive agent of ethanol can be made, be conducive to conductive agent in the slurry dispersed, thus be evenly wrapped in lithium iron phosphate particles surface, and add ethanol in slurry, in the process of high-speed stirred, slurry not easily produces bubble, without the need to carrying out vacuum defoamation process to slurry in subsequent process, technique is simplified, ethanol also plays the effect of anti-settling simultaneously, stability and the consistency of slurry can be improved.
(3) once disperse: being milled to fineness of materials add LiFePO4 in premix after is 5 ~ 10 μm.Once dispersion adopts the mode of ball milling, particle is fully pulverized and becomes granule, otherwise in follow-up twice dispersing process, material is still bulky grain.
(4) twice dispersing: the material in step (3) is added the deionized water adding surplus in planetary pulp blender, high-speed stirred to fineness is 10 ~ 30 μm.First add remaining deionized water during twice dispersing with diluted material, then make each component quick in aqueous phase, dispersed by high-speed stirred, the Stability of Slurry obtained like this and consistency good.
(5) stir slowly: cross 120 ~ 200 mesh sieves by after the material stirring at low speed 20 ~ 30min in step (4), obtain LiFePO4 aqueous positive-pole slurry.
(6) be coated with: LiFePO4 aqueous positive-pole slurry is evenly coated in positive collection liquid surface.
(7) segmentation is dried: at the positive collector that step (6) obtains is placed in 85 ~ 90 DEG C after dry 5 ~ 7h, under room temperature, naturally cool 30 ~ 60min, then at 70 ~ 80 DEG C drying 12 ~ 14h, after pressure roller, namely obtain cathode of lithium iron phosphate lithium ion battery.The mode that the present invention adopts segmentation to dry carries out drying to pole piece, in earlier stage in pole piece, moisture is more, therefore can adopt the mode of high temperature and rapid drying that moisture is evaporated rapidly, but baking temperature is too high, drying time is long, the drying of pole piece can be caused excessive, coating is made to occur crackle, dry linting phenomenon can be caused, dry linting phenomenon can be caused, after pole piece high temperature drying premenstruum (premenstrua), pole piece is hardening, the moisture of pole piece inside can be stoped to discharge, therefore moisture slowing to external migration, rate of drying is more and more slower, be unfavorable for the bone dry of pole piece, pole piece is at room temperature cooled 30 ~ 60min by mid-term naturally, pole piece internal moisture can be made externally to transmit, be conducive to the bone dry of pole piece, later stage carries out low temperature drying, moisture in pole piece is fully removed.Stage drying can bone dry pole piece, can improve the chemical property of battery.
As preferably, described conductive agent is one or more in conductive black, superconduction carbon, electrically conductive graphite, crystalline flake graphite, carbon nano-tube.
As preferably, described aqueous binders is mixed 3:5 ~ 7 in mass ratio by sodium alginate and acrylonitrile multiple copolymer LA133.Sodium alginate and acrylonitrile multiple copolymer LA133 coordinated, bond effect is good, and cost is low, sodium alginate, except cementation, also can be filled in the gap between LiFePO4, for LiFePO4 provides support and buffering, there is fragmentation in the aggregate effectively avoiding LiFePO4 to be formed, thus improve the processing characteristics of electrode slice in roll-in, and sodium alginate can also make close contact between LiFePO4 and binding agent, conductive agent simultaneously, avoid the polarization of pole piece, be conducive to improving chemical property.
As preferably, in step (2), the quality of portions of de-ionized water is 30 ~ 40% of deionized water gross mass.
As preferably, the process conditions that step (4) high speed stirs are: revolution 20 ~ 50r/min, rotation 1800 ~ 2500r/min.
As preferably, in step (5), the process conditions of stirring at low speed are: revolution 20 ~ 50r/min, rotation 1000 ~ 1500r/min.
As preferably, when in step (7), segmentation is dried, front 5 ~ 8h vacuumizes once every 1 ~ 2h, vacuumizes once afterwards every 3 ~ 4h.Vacuumize the moisture removed in dry environment when stage drying, can drying effect be improved.
Therefore, the invention has the beneficial effects as follows:
(1) mode adopting ball milling and high-speed stirred to disperse, and formula of size is optimized, the Stability of Slurry obtained, consistency are good;
(2) adopt the drying mode of stage drying, pole piece is completely dry.
Accompanying drawing explanation
Fig. 1 to be capacity that positive pole that embodiment 1 obtains is made be lithium ion battery of 1500mAh at 20 ± 5 DEG C, with the loop test figure of 1C/1C charge-discharge magnification in the voltage range of 3.0 ~ 4.2V.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
In the present invention, if not refer in particular to, all percentage is unit of weight, and all devices and raw material all can be buied from market or the industry is conventional, and the method in following embodiment, if no special instructions, is this area conventional method.
Embodiment 1
(1) weighing: in the gross mass of anode sizing agent, each component is taken: LiFePO4 45% by following mass percentage, conductive agent 2%, aqueous binders 2%, ethanol 3%, deionized water 48%, wherein conductive agent is conductive carbon black, aqueous binders by sodium alginate and acrylonitrile multiple copolymer LA133 in mass ratio 3:5 mix.
(2) premix preparation: after being mixed with conductive agent by ethanol, add aqueous binders and portions of de-ionized water, being milled to fineness of materials is 5 μm, obtains premix, and wherein, the quality of portions of de-ionized water is 40% of deionized water gross mass.
(3) once disperse: being milled to fineness of materials add LiFePO4 in premix after is 5 μm.
(4) twice dispersing: the material in step (3) is added the deionized water adding surplus in planetary pulp blender, high-speed stirred to fineness is 10 μm, and the process conditions of high-speed stirred are: revolution 20r/min, rotation 1800r/min.
(5) stir slowly: cross 200 mesh sieves by after the material stirring at low speed 20min in step (4), obtain LiFePO4 aqueous positive-pole slurry.
(6) be coated with: LiFePO4 aqueous positive-pole slurry is evenly coated in positive collection liquid surface.
(7) segmentation is dried: at the positive collector that step (6) obtains is placed in 85 DEG C after dry h, naturally 30min is cooled under room temperature, dry 14h at 70 DEG C again, namely cathode of lithium iron phosphate lithium ion battery is obtained after pressure roller, when segmentation is dried, front 8h vacuumizes once every 2h, vacuumizes once afterwards every 4h.
The positive pole obtained being made model is 495148, and nominal capacity is the lithium ion battery of 1500mAh, at 20 ± 5 DEG C, carries out loop test with 1C/1C charge-discharge magnification in the voltage range of 3.0 ~ 4.2V, and the loop test figure obtained as shown in Figure 1.
As can be seen from Figure 1, battery is in the voltage range of 3.0 ~ 4.2V, can remain on about 89% of initial capacity with the capability retention after 1C circulation 300 times, illustrate that the cycle performance of battery is good, what that is obtained by the present invention just has excellent chemical property.
Embodiment 2
(1) weighing: in the gross mass of anode sizing agent, each component is taken: LiFePO4 47% by following mass percentage, conductive agent 2.7%, aqueous binders 2.6%, ethanol 4%, deionized water 43.7%, wherein conductive agent is conductive carbon black and carbon nano-tube (mass ratio 1:2), aqueous binders by sodium alginate and acrylonitrile multiple copolymer LA133 in mass ratio 3:6 mix.
(2) premix preparation: after being mixed with conductive agent by ethanol, add aqueous binders and portions of de-ionized water, being milled to fineness of materials is 7 μm, obtains premix, and wherein, the quality of portions of de-ionized water is 35% of deionized water gross mass.
(3) once disperse: being milled to fineness of materials add LiFePO4 in premix after is 6 μm.
(4) twice dispersing: the material in step (3) is added the deionized water adding surplus in planetary pulp blender, high-speed stirred to fineness is 15 μm, and the process conditions of high-speed stirred are: revolution 25r/min, rotation 2000r/min.
(5) stir slowly: cross 150 mesh sieves by after the material stirring at low speed 25min in step (4), obtain LiFePO4 aqueous positive-pole slurry.
(6) be coated with: LiFePO4 aqueous positive-pole slurry is evenly coated in positive collection liquid surface.
(7) segmentation is dried: at the positive collector that step (6) obtains is placed in 87 DEG C after dry 6h, naturally 35min is cooled under room temperature, dry 13h at 75 DEG C again, namely cathode of lithium iron phosphate lithium ion battery is obtained after pressure roller, when segmentation is dried, front 6h vacuumizes once every 1.5h, vacuumizes once afterwards every 3.5h.
The positive pole obtained being made model is 495148, nominal capacity is the lithium ion battery of 1500mAh, at 20 ± 5 DEG C, carries out loop test with 1C/1C charge-discharge magnification in the voltage range of 3.0 ~ 4.2V, loop test figure and the Fig. 1 obtained is similar, therefore does not repeat at this.
Embodiment 3
(1) weighing: in the gross mass of anode sizing agent, each component is taken: LiFePO4 50% by following mass percentage, conductive agent 3%, aqueous binders 3%, ethanol 5%, deionized water 39%, wherein conductive agent is conductive carbon black, carbon nano-tube and crystalline flake graphite (mass ratio 1:2:1), aqueous binders by sodium alginate and acrylonitrile multiple copolymer LA133 in mass ratio 3:2 mix.
(2) premix preparation: after being mixed with conductive agent by ethanol, add aqueous binders and portions of de-ionized water, being milled to fineness of materials is 10 μm, obtains premix, and wherein, the quality of portions of de-ionized water is 30% of deionized water gross mass.
(3) once disperse: being milled to fineness of materials add LiFePO4 in premix after is 10 μm.
(4) twice dispersing: the material in step (3) is added the deionized water adding surplus in planetary pulp blender, high-speed stirred to fineness is 10 μm, and the process conditions of high-speed stirred are: revolution 50r/min, rotation 2500r/min.
(5) stir slowly: cross 120 mesh sieves by after the material stirring at low speed 30min in step (4), obtain LiFePO4 aqueous positive-pole slurry.
(6) be coated with: LiFePO4 aqueous positive-pole slurry is evenly coated in positive collection liquid surface.
(7) segmentation is dried: at the positive collector that step (6) obtains is placed in 90 DEG C after dry 5h, naturally 60min is cooled under room temperature, dry 12h at 80 DEG C again, namely cathode of lithium iron phosphate lithium ion battery is obtained after pressure roller, when segmentation is dried, front 5h vacuumizes once every 1h, vacuumizes once afterwards every 3h.
The positive pole obtained being made model is 495148, nominal capacity is the lithium ion battery of 1500mAh, at 20 ± 5 DEG C, carries out loop test with 1C/1C charge-discharge magnification in the voltage range of 3.0 ~ 4.2V, loop test figure and the Fig. 1 obtained is similar, therefore does not repeat at this.
Above-described embodiment is one of the present invention preferably scheme, not does any pro forma restriction to the present invention, also has other variant and remodeling under the prerequisite not exceeding the technical scheme described in claim.
Claims (7)
1. a preparation method for cathode of lithium iron phosphate lithium ion battery, is characterized in that, comprises the following steps:
(1) weighing: in the gross mass of anode sizing agent, takes each component by following mass percentage: LiFePO4 45 ~ 50%, conductive agent 2 ~ 3%, aqueous binders 2 ~ 3%, ethanol 3 ~ 5%, and surplus is deionized water;
(2) premix preparation: after being mixed with conductive agent by ethanol, add aqueous binders and portions of de-ionized water, being milled to fineness of materials is 5 ~ 10 μm, obtains premix;
(3) once disperse: being milled to fineness of materials add LiFePO4 in premix after is 5 ~ 10 μm;
(4) twice dispersing: the material in step (3) is added the deionized water adding surplus in planetary pulp blender, high-speed stirred to fineness is 10 ~ 30 μm;
(5) stir slowly: cross 120 ~ 200 mesh sieves by after the material stirring at low speed 20 ~ 30min in step (4), obtain LiFePO4 aqueous positive-pole slurry;
(6) be coated with: LiFePO4 aqueous positive-pole slurry is evenly coated in positive collection liquid surface;
(7) segmentation is dried: at the positive collector that step (6) obtains is placed in 85 ~ 90 DEG C after dry 5 ~ 7h, under room temperature, naturally cool 30 ~ 60min, then at 70 ~ 80 DEG C drying 12 ~ 14h, after pressure roller, namely obtain cathode of lithium iron phosphate lithium ion battery.
2. preparation method according to claim 1, is characterized in that, described conductive agent is one or more in conductive black, superconduction carbon, electrically conductive graphite, crystalline flake graphite, carbon nano-tube.
3. preparation method according to claim 1, is characterized in that, described aqueous binders is mixed 3:5 ~ 7 in mass ratio by sodium alginate and acrylonitrile multiple copolymer LA133.
4. preparation method according to claim 1, is characterized in that, in step (2), the quality of portions of de-ionized water is 30 ~ 40% of deionized water gross mass.
5. preparation method according to claim 1, is characterized in that, the process conditions that step (4) high speed stirs are: revolution 20 ~ 50r/min, rotation 1800 ~ 2500r/min.
6. preparation method according to claim 1, is characterized in that, in step (5), the process conditions of stirring at low speed are: revolution 20 ~ 50r/min, rotation 1000 ~ 1500r/min.
7. preparation method according to claim 1, is characterized in that, when in step (7), segmentation is dried, front 5 ~ 8h vacuumizes once every 1 ~ 2h, vacuumizes once afterwards every 3 ~ 4h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106981623A (en) * | 2017-04-25 | 2017-07-25 | 河北工业大学 | A kind of power lithium ion battery pole piece slurry production line |
| CN106981685A (en) * | 2016-12-11 | 2017-07-25 | 长兴天晟能源科技有限公司 | A kind of lithium ion cell electrode piece baking process containing aqueous binders |
| CN109560246A (en) * | 2018-11-27 | 2019-04-02 | 惠州亿纬锂能股份有限公司 | A kind of lithium battery and its method of preparation |
| CN109698338A (en) * | 2018-12-26 | 2019-04-30 | 湖北锂诺新能源科技有限公司 | A kind of powerful graphene-based LiFePO4 pole piece of low cost and preparation method |
| CN112259717A (en) * | 2020-10-14 | 2021-01-22 | 安徽益佳通电池有限公司 | Dry-mixing preparation method of lithium ion battery anode slurry |
| CN113809322A (en) * | 2021-08-10 | 2021-12-17 | 福建巨电新能源股份有限公司 | Water-based lithium iron phosphate battery, positive electrode slurry thereof and preparation method of positive electrode slurry |
| CN114361714A (en) * | 2021-12-06 | 2022-04-15 | 惠州市旭然新能源有限公司 | Coating slurry, preparation method thereof, composite porous diaphragm prepared from coating slurry and lithium ion battery |
| CN114614007A (en) * | 2022-02-17 | 2022-06-10 | 东莞凯德新能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN114682349A (en) * | 2022-03-14 | 2022-07-01 | 广西燚能新能源有限公司 | Manufacturing method for improving water system lithium iron phosphate battery positive plate |
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| CN1734825A (en) * | 2005-08-08 | 2006-02-15 | 河南环宇集团有限公司 | Preparation method for high rate phosphate lithium ion battery and battery prepared thereby |
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Cited By (11)
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| CN106981685A (en) * | 2016-12-11 | 2017-07-25 | 长兴天晟能源科技有限公司 | A kind of lithium ion cell electrode piece baking process containing aqueous binders |
| CN106981623A (en) * | 2017-04-25 | 2017-07-25 | 河北工业大学 | A kind of power lithium ion battery pole piece slurry production line |
| CN109560246A (en) * | 2018-11-27 | 2019-04-02 | 惠州亿纬锂能股份有限公司 | A kind of lithium battery and its method of preparation |
| CN109560246B (en) * | 2018-11-27 | 2021-12-14 | 惠州亿纬锂能股份有限公司 | Lithium battery and preparation method thereof |
| CN109698338A (en) * | 2018-12-26 | 2019-04-30 | 湖北锂诺新能源科技有限公司 | A kind of powerful graphene-based LiFePO4 pole piece of low cost and preparation method |
| CN112259717A (en) * | 2020-10-14 | 2021-01-22 | 安徽益佳通电池有限公司 | Dry-mixing preparation method of lithium ion battery anode slurry |
| CN113809322A (en) * | 2021-08-10 | 2021-12-17 | 福建巨电新能源股份有限公司 | Water-based lithium iron phosphate battery, positive electrode slurry thereof and preparation method of positive electrode slurry |
| CN114361714A (en) * | 2021-12-06 | 2022-04-15 | 惠州市旭然新能源有限公司 | Coating slurry, preparation method thereof, composite porous diaphragm prepared from coating slurry and lithium ion battery |
| CN114614007A (en) * | 2022-02-17 | 2022-06-10 | 东莞凯德新能源有限公司 | Lithium ion battery anode slurry and preparation method thereof |
| CN114614007B (en) * | 2022-02-17 | 2023-07-21 | 东莞凯德新能源有限公司 | Positive electrode slurry of lithium ion battery and preparation method thereof |
| CN114682349A (en) * | 2022-03-14 | 2022-07-01 | 广西燚能新能源有限公司 | Manufacturing method for improving water system lithium iron phosphate battery positive plate |
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Address after: 315800 standard workshop No. 2 of the 0212 massif in the West Zone of the Ningbo Free Trade Zone, Zhejiang Patentee after: Ningbo Veken Battery Co., Ltd. Address before: 315800 No. 5 West Avenue, Beilun Free Trade Zone, Ningbo, Zhejiang Patentee before: Ningbo Veken Battery Co., Ltd. |
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Effective date of registration: 20190402 Address after: 315800 Factory Building-1 North Side of No.3 Gangxi Avenue, Ningbo Bonded West District, Zhejiang Province Patentee after: Ningbo Vico Amperex Technology Limited Address before: 315800 Standard Workshop No. 2, 0212 Block, West Ningbo Free Trade Zone, Zhejiang Province Patentee before: Ningbo Veken Battery Co., Ltd. |