CN102637847B - Method for preparing high-dispersity lithium battery anode and cathode slurry - Google Patents

Method for preparing high-dispersity lithium battery anode and cathode slurry Download PDF

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Publication number
CN102637847B
CN102637847B CN201210125678.3A CN201210125678A CN102637847B CN 102637847 B CN102637847 B CN 102637847B CN 201210125678 A CN201210125678 A CN 201210125678A CN 102637847 B CN102637847 B CN 102637847B
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stirring
speed
mixing time
carry
slurry
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CN201210125678.3A
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CN102637847A (en
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张宏立
李海望
宗煜钦
费松庭
陆钥飞
陈洁
郑旭芳
张永学
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宁波世捷新能源科技有限公司
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention relates to a technology for preparing anode and cathode slurry of a rechargeable secondary lithium ion battery, and provides a method for realizing uniform dispersion of the anode and cathode slurry of the lithium battery through optimized stirring. The core of the invention is that: the turbulent loss state of the slurry is increased and the range of 'dead areas' in the slurry is reduced by adopting a 'fluctuated stirring' method, so that the dispersity of the slurry is improved. The 'fluctuated stirring' is characterized in that: the slurry is stirred at low speed at first (the stirring intensity is S1 and the stirring time is t1), then the stirring speed is slowly promoted (the stirring intensities are S2 and S3 and the stirring times are t2 and t3) until the speed is high (the stirring intensity is S4 and the stirring time is t4), and the stirring speed is reduced to medium speed (the stirring intensity is S2 and the stirring time is t2). The 'fluctuated stirring' unit is repeatedly performed until the stirring time is over. By adopting the method, a lithium battery manufacturing enterprise can conveniently obtain the highly dispersed anode and cathode slurry under the condition that a conventional stirring machine is used.

Description

A kind of method of preparing polymolecularity lithium battery anode and cathode slurry
Technical field
The present invention relates to a kind of method of preparing lithium battery anode and cathode slurry.
Background technology
Lithium rechargeable battery because monomer whose voltage is high, energy and power density is large, long-life, quality are gently little, memory-less effect, the advantage such as pollution-free, become current widely used power supply product.Its application mainly comprises all kinds of portable electronic consumer goods (as smart mobile phone, panel computer, digital camera etc.); The supporting energy storage in solar energy/wind energy power station; Electric motor car (EV) and hybrid electric vehicle (HEV); Military weaponry; Space industry etc.Especially in recent years along with the application in electric motor car, people have proposed higher performance requirement to lithium ion battery.And the raising of performance of lithium ion battery is except being limited by the performance improvement of various battery materials (as positive electrode, negative material, electrolyte, barrier film), also depend on to a great extent the preparation of the anode and cathode slurry of the control of each link of battery production technology process, particularly initial stage.
Lithium battery anode and cathode slurry consists of components such as active material (positive pole and negative pole), conductive additive (as carbon black, graphite, Graphene, carbon nano-fiber, carbon nano-tube), binding agent, solvent (water system or oil system), additives (as defoamer, thickener, dispersant) conventionally, this comprising mutual between liquid and liquid, liquid and solid mix, a series of processes such as dissolving, dispersion.The final dispersity of each component directly affects capacity performance, high rate performance, cycle life, internal resistance consistency and the security performance of lithium battery.Therefore, how realizing the dispersed of anode and cathode slurry is the most important thing of the whole production process of lithium battery.At present, applied for that patent great majority with disclosed lithium battery slurry aspect all concentrate on the improvement to each component relative amount and hybrid mode (be dry mixed, wet mixing), " Recipe " is upper, as CN102148369A, and CN101740757A, CN101609882A, CN1626603A, CN101414694A, CN102280612A, CN101752550A, CN102148363A; In addition, also have report to adopt additional dispersion means to improve the dispersion effect of slurry as ultrasonic dispersion (CN102145329A), planetary ball mill (CN101232091A) etc., but adopt these means to need extra increase equipment, cost is high, complex process.
Summary of the invention
In order to overcome the existing above-mentioned deficiency of preparing the method for lithium battery anode and cathode slurry, the invention provides a kind of method of preparing polymolecularity lithium battery anode and cathode slurry that just can conveniently obtain the anode and cathode slurry of high degree of dispersion under conventional mixer condition of using.
The technical scheme that the present invention solves its technical problem is: a kind of method of preparing polymolecularity lithium battery anode and cathode slurry, adopt conventional mixer, and loop the operation of fluctuation-type agitating unit, the operating procedure of each fluctuation-type agitating unit is:
A. first carry out stirring at low speed, stirring intensity is S1, mixing time t1;
B. carry out middling speed stirring, stirring intensity is S2 again, and mixing time is t2;
C. carry out high speed stirring, stirring intensity is S3 again, and mixing time is t3;
D. carry out high-speed stirred, stirring intensity is S4 again, and mixing time is t4;
E. carry out middling speed stirring, stirring intensity is S2 again, and mixing time is t2;
In above-mentioned steps, stirring intensity is measured with the speed of agitator of mixer, stirring intensity S1 < S2 < S3 < S4.
Recommend, stirring intensity S1 is 10% ~ 20% of mixer maximum speed, and stirring intensity S2 is 30% ~ 40% of mixer maximum speed, and stirring intensity S3 is 50% ~ 60% of mixer maximum speed; Stirring intensity S4 is 70% ~ 90% of mixer maximum speed.
Recommend, mixing time t1 is 1min ~ 20min, and mixing time t2 is 5 min ~ 30min, and mixing time t3 is 10min ~ 40min, and mixing time t4 is 20 min ~ 60min.
Recommend, the number of times of fluctuation-type agitating unit operation is 2 ~ 20 times.
Because lithium battery slurry belongs to non-Newtonian fluid, the present invention proposes the disorderly state of mistake of the method increase slurry of employing " fluctuation-type stirring ", reduces " dead band " scope in slurry (stirring, the impalpable region of dispersion force), to improve dispersiveness.
In the inventive method, anode sizing agent system is optional: LiFePO4 (LiFePO4), LiMn2O4 (LiMn2O4), cobalt acid lithium (LiCoO2), ternary material (LiNi xmn yco zo 2) in one or more as positive electrode active materials, in carbon black, electrically conductive graphite, Graphene, carbon nano-fiber, carbon nano-tube, one or more are as conductive additive, Kynoar (PVDF), butadiene-styrene rubber (SBR) or polyacrylonitrile (PAN) are as binding agent, 1-METHYLPYRROLIDONE (NMP) or water are as solvent, and sodium carboxymethylcellulose (CMC) is as thickener.
In the inventive method, cathode size system is optional: native graphite, Delanium, MCMB, hard charcoal, lithium titanate (Li 4ti 5o 12), in tin/carbon composite, silicon/carbon composite one or more as negative active core-shell material, in carbon black, electrically conductive graphite, Graphene, carbon nano-fiber, carbon nano-tube, one or more are as conductive additive, Kynoar (PVDF), butadiene-styrene rubber (SBR) or polyacrylonitrile (PAN) are as binding agent, 1-METHYLPYRROLIDONE (NMP) or water are as solvent, sodium carboxymethylcellulose (CMC) is as thickener, and ethanol is as defoamer.
Beneficial effect of the present invention is: by adopting fluctuation-type to stir, and can be so that each component materials infiltrates fully, mixes and disperses in anode and cathode slurry.Comparing traditional fixed (constant speed) stirs, the present invention has that efficiency is high, dispersion effect good, to advantages such as equipment impact wear are little, the present invention can significantly improve uniformity and the stability of slurry in lithium battery production, and then the controllability of raising lithium ion battery production process and the consistency of properties of product, and in equipment utilization, use conventional mixer, do not increase new equipment completely, greatly saved cost.
Accompanying drawing explanation
Fig. 1 is technical process schematic diagram of the present invention.
Fig. 2 is the optical photograph that adopts technique cathode size dispersion effect of the present invention.
Fig. 3 is the stereoscan photograph that adopts technique cathode size dispersion effect of the present invention.
Fig. 4 is the optical photograph that adopts the technique cathode size dispersion effect of traditional stirring means.
Fig. 5 is the stereoscan photograph that adopts the technique cathode size dispersion effect of traditional stirring means.
Fig. 6 is the optical photograph that adopts technique anode sizing agent dispersion effect of the present invention.
Fig. 7 is the stereoscan photograph that adopts technique anode sizing agent dispersion effect of the present invention.
Fig. 8 is the optical photograph that adopts the technique anode sizing agent dispersion effect of traditional stirring means
Fig. 9 is the stereoscan photograph that adopts the technique anode sizing agent dispersion effect of traditional stirring means.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in further detail.
Embodiment mono-
The conventional formulation technique of preparing according to cathode of lithium battery slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), graphite cathode powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 20% of mixer maximum speed, mixing time t1, and t1 is 5 minutes; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 40% of mixer maximum speed, and mixing time is t2, and t2 is 10 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 50% of mixer maximum speed, and mixing time is t3, and t3 is 15 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 80% of mixer maximum speed, and mixing time is t4, and t4 is 20 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 40% of mixer maximum speed, and mixing time is t2, and t2 is 10 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " unit 5 times, stir and finish.From Fig. 2, Fig. 3, can see, it is very even that slurry disperses, and do not have big particle agglomerate to occur.
Comparative example one
The conventional formulation technique of preparing according to cathode of lithium battery slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), graphite cathode powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring according to constant speed stir mode: stirring intensity is 80% of mixer maximum speed, and mixing time is 5 hours.From Fig. 4, Fig. 5, can see in slurry, having a lot of bulky grains not to be dispersed out, mixing effect is undesirable.
Embodiment bis-
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 15% of mixer maximum speed, mixing time t1, and t1 is 5 minutes; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 35% of mixer maximum speed, and mixing time is t2, and t2 is 10 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 60% of mixer maximum speed, and mixing time is t3, and t3 is 15 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 90% of mixer maximum speed, and mixing time is t4, and t4 is 20 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 35% of mixer maximum speed, and mixing time is t2, and t2 is 10 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " unit 7 times, stir and finish.From Fig. 6, Fig. 7, can see, it is very even that slurry disperses, and do not have big particle agglomerate to occur.
Comparative example two
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring according to constant speed stir mode: stirring intensity is 90% of mixer maximum speed, and mixing time is 7 hours.From Fig. 8, Fig. 9, can see in slurry, there are a lot of island particles, dispersion effect is undesirable.
Embodiment tri-
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 10% of mixer maximum speed, mixing time t1, and t1 is 5 minutes; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 40% of mixer maximum speed, and mixing time is t2, and t2 is 20 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 52% of mixer maximum speed, and mixing time is t3, and t3 is 10 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 83% of mixer maximum speed, and mixing time is t4, and t4 is 20 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 40% of mixer maximum speed, and mixing time is t2, and t2 is 20 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " single
Unit 2 times, stirs and finishes.
Embodiment tetra-
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 20% of mixer maximum speed, mixing time t1, and t1 is 11 minutes; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 30% of mixer maximum speed, and mixing time is t2, and t2 is 5 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 60% of mixer maximum speed, and mixing time is t3, and t3 is 40 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 70% of mixer maximum speed, and mixing time is t4, and t4 is 48 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 30% of mixer maximum speed, and mixing time is t2, and t2 is 5 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " single
Unit 15 times, stirs and finishes.
Embodiment five
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 17% of mixer maximum speed, mixing time t1, and t1 is 1 minute; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 33% of mixer maximum speed, and mixing time is t2, and t2 is 10 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 59% of mixer maximum speed, and mixing time is t3, and t3 is 23 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 90% of mixer maximum speed, and mixing time is t4, and t4 is 35 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 33% of mixer maximum speed, and mixing time is t2, and t2 is 10 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " single
Unit 18 times, stirs and finishes.
Embodiment six
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 12% of mixer maximum speed, mixing time t1, and t1 is 20 minutes; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 38% of mixer maximum speed, and mixing time is t2, and t2 is 26 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 50% of mixer maximum speed, and mixing time is t3, and t3 is 35 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 86% of mixer maximum speed, and mixing time is t4, and t4 is 56 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 38% of mixer maximum speed, and mixing time is t2, and t2 is 26 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " single
Unit 20 times, stirs and finishes.
Embodiment seven
The conventional formulation technique of preparing according to lithium battery anode slurry, with certain proportion, take sodium carboxymethylcellulose (CMC) and water is played glue, then in batches, gradation adds conductive additive (Super P carbon black and KS-6 electrically conductive graphite), iron phosphate lithium positive pole powder and binding agent SBR; Use the conventional mixing plant of lithium battery manufacturing enterprise to carry out dispersed with stirring: A. according to following " fluctuation-type stirring " unit and first carry out stirring at low speed, stirring intensity is S1, and S1 is 15% of mixer maximum speed, mixing time t1, and t1 is 18 minutes; B. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 35% of mixer maximum speed, and mixing time is t2, and t2 is 30 minutes; C. carry out high speed stirring, stirring intensity is S3 again, and S3 is 57% of mixer maximum speed, and mixing time is t3, and t3 is 15 minutes; D. carry out high-speed stirred, stirring intensity is S4 again, and S4 is 75% of mixer maximum speed, and mixing time is t4, and t4 is 60 minutes; E. carry out middling speed stirring, stirring intensity is S2 again, and S2 is 35% of mixer maximum speed, and mixing time is t2, and t2 is 30 minutes.Above-mentioned A, B, C, D step form " fluctuation-type stirring " unit, repeat this " fluctuation-type stirring " unit 8 times, stir and finish.

Claims (4)

1. a method of preparing polymolecularity lithium battery anode and cathode slurry, is characterized in that: adopt conventional mixer, loop the operation of fluctuation-type agitating unit, the operating procedure of each fluctuation-type agitating unit is:
A. first carry out stirring at low speed, stirring intensity is S1, mixing time t1;
B. carry out middling speed stirring, stirring intensity is S2 again, and mixing time is t2;
C. carry out high speed stirring, stirring intensity is S3 again, and mixing time is t3;
D. carry out high-speed stirred, stirring intensity is S4 again, and mixing time is t4;
E. carry out middling speed stirring, stirring intensity is S2 again, and mixing time is t2;
In above-mentioned steps, stirring intensity is measured with the speed of agitator of mixer, stirring intensity S1 < S2 < S3 < S4.
2. the method for preparing polymolecularity lithium battery anode and cathode slurry as claimed in claim 1, it is characterized in that: stirring intensity S1 is 10% ~ 20% of mixer maximum speed, stirring intensity S2 is 30% ~ 40% of mixer maximum speed, and stirring intensity S3 is 50% ~ 60% of mixer maximum speed; Stirring intensity S4 is 70% ~ 90% of mixer maximum speed.
3. the method for preparing polymolecularity lithium battery anode and cathode slurry as claimed in claim 2, it is characterized in that: mixing time t1 is 1min ~ 20min, mixing time t2 is 5 min ~ 30min, and mixing time t3 is 10min ~ 40min, and mixing time t4 is 20 min ~ 60min.
4. the method for preparing polymolecularity lithium battery anode and cathode slurry as described in one of claim 1 ~ 3, is characterized in that: the number of times of fluctuation-type agitating unit operation is 2 ~ 20 times.
CN201210125678.3A 2012-04-26 2012-04-26 Method for preparing high-dispersity lithium battery anode and cathode slurry CN102637847B (en)

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CN104993135A (en) * 2015-06-13 2015-10-21 田东 Lithium ion battery with long cycle performance
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