CN102891282A - Cathode preparation technique of lithium ion battery - Google Patents

Cathode preparation technique of lithium ion battery Download PDF

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Publication number
CN102891282A
CN102891282A CN2011102053828A CN201110205382A CN102891282A CN 102891282 A CN102891282 A CN 102891282A CN 2011102053828 A CN2011102053828 A CN 2011102053828A CN 201110205382 A CN201110205382 A CN 201110205382A CN 102891282 A CN102891282 A CN 102891282A
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slurry
minutes
lithium ion
stirring
ion battery
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CN102891282B (en
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娄勇刚
闻涛
吕循峰
刘勇
沈成龙
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HUBEI CAMEL SPECIAL POWER SUPPLY CO Ltd
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HUBEI CAMEL SPECIAL POWER SUPPLY CO Ltd
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    • 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 relates to a cathode preparation technique of a lithium ion battery, which comprises the following steps: adding a thickening agent, a conductive agent and 1/2 cathode active matter in an agitating cylinder according to the prescription, and stirring for 30+/-15 minutes; adding the remaining 1/2 cathode active matter and stirring at a low speed for 10+/-5 minutes; scrapping materials after stirring, then stirring for 30+/-15 minutes at a high speed until the slurry is uniform; adding the solvent, stirring for 10+/-5 minutes at a low speed; scrapping materials, then stirring for 30+/-15 minutes at a high speed again, and storing; then raising temperature to 80+/-5 DEG C, stirring for 45+/-5 minutes at a high speed; reducing temperature; adding the bonding agent according to the prescription ratio, stirring for 60+/-15 minutes at a high speed; reducing temperature and cooling the slurry to 25-45 DEG C, and storing. By adopting the invention, the problems of long preparation technique time of the lithium ion battery, low equipment utilization rate and low production volume at present are solved; the preparation technique time of the lithium ion battery is controlled to be within about 5 hours, so that the equipment utilization rate is improved, the cost is reduced, and the battery performance is not affected.

Description

The lithium ion battery negative proportioning process
Technical field
The invention belongs to the lithium ion battery distributing production technology, be specifically related to cathode blending and be dry mixed the improvement of processing and the interpolation of high-temperature process.
Background technology
Development along with science and technology such as electronics, aviation and automobiles, oil, the global problems such as the exhaustion of the non-renewable fossil fuel such as natural gas, air pollution and greenhouse effect receive publicity day by day, development level based on energy technology, in order to alleviate even to solve these global problems, at present to the demand rapid growth of energy-conserving and environment-protective portable power source.Because lithium ion battery has advantages of high voltage, high power capacity, and have extended cycle life, security performance is good, it is had broad application prospects in many-sides such as portable electric appts, electric automobile, space technology, national defense industry, become the study hotspot of widely paying close attention in recent years.
The mechanism generality of lithium ion battery is thought, lithium ion battery refers to respectively with two secondary cells of consisting of as both positive and negative polarity of the compound of Infix and desfix lithium ion reversibly as a kind of chemical power source, when battery charges, lithium ion takes off embedding from positive pole, in negative pole, embed, otherwise during discharge.The Physical Mechanism that lithium ion battery is related, explain to embed physics in the solid-state physics at present, embed (intercalation) and refer to that object particle (molecule, atom, ion) movably reversibly is embedded on the network lattice vacancy in the host lattice with suitable dimension.
Good distribution can guarantee that battery lithium ion when charging can normally embed the graphite-structure layer, and lithium ion can normally take off and imbed into positive pole during discharge, guarantees that not stopping for a long time to discharge and recharge the positive and negative pole material lattice does not subside, and guarantees that battery can the long-life normal operation.
In the prior art lithium ion battery negative batching production technology time long, needs about ten hours, utilization rate of equipment and installations is low.Because the demand of lithium ion battery in continuous growth, therefore under the prerequisite that guarantees battery performance, is sought new production technology and is improved production output and shorten the both positive and negative polarity proportioning process time particularly important.
Summary of the invention
The object of the present invention is to provide a kind of batching time short, utilization rate of equipment and installations height and the low lithium ion battery negative proportioning process of cost rate.
Technical solution of the present invention is: a kind of lithium ion battery negative proportioning process, and its parts by weight of raw materials proportioning is:
Binding agent: 0.5～1.7;
Thickener: 0～1.3;
Conductive agent: 0.5～0.7;
Negative electrode active material: 44.0～51.0;
Solvent: 45.3～55.0;
Described thickener comprises: sodium carboxymethylcellulose (CMC);
Described binding agent comprises: the PVA(polyvinyl alcohol), the PTFE(polytetrafluoroethylene), the CMC(sodium carboxymethylcellulose), the PVDF(Kynoar), SBR(butadiene-styrene rubber), Viton, polyurethane, LA(polyacrylonitrile copolymer);
Described conductive agent: the agent of KS(graphite), the agent of SP(carbon black conductive);
Described negative electrode active material: the NG(native graphite), the AG(Delanium), the CG(composite graphite);
Described solvent: deionized water, NMP(N-methyl pyrrolidone);
Its operation is:
Figure 295996DEST_PATH_IMAGE001
Siccative mixes one: add the negative electrode active material of thickener, conductive agent and 1/2 recipe ratio weight by recipe ratio in a mixing bowl, stirred 30 ± 15 minutes;
Figure 412988DEST_PATH_IMAGE002
Siccative mixes two: rise a mixing bowl, in operation The negative electrode active material that adds residue 1/2 recipe ratio weight in the slurry that makes carried out stirring at low speed 10 ± 5 minutes, stirred complete rear scraper, and high-speed stirred 30 ± 15 minutes is even to slurry again;
Adding solvent disperses: in operation
Figure 178666DEST_PATH_IMAGE002
Add described solvent in the slurry that makes, stirring at low speed 10 ± 5 minutes, scraper, high-speed stirred is 30 ± 15 minutes again, preserves;
Figure 15909DEST_PATH_IMAGE004
High-temperature process: in the chuck of mixing plant (carry and add circulating water device), pass into 80 ± 5 ℃ of recirculated waters and make operation
Figure 235669DEST_PATH_IMAGE003
The slurry that makes is warming up to 80 ± 5 ℃, high-speed stirred 45 ± 5 minutes; Perhaps with operation
Figure 48161DEST_PATH_IMAGE003
The slurry that makes toasted 45 ± 5 minutes under 80 ± 5 ℃ of high temperature, continued high-speed stirred 60 ± 15 minutes again, passed into cooling water in the chuck to a mixing bowl and made slurry be cooled to 45 ~ 60 ℃, preserved;
Figure 616546DEST_PATH_IMAGE005
Add binding agent: get operation
Figure 708129DEST_PATH_IMAGE004
The slurry that makes adds recipe ratio weight binding agent, and high-speed stirred 60 ± 15 minutes passes into water and makes slurry be cooled to 25 ~ 45 ℃ in the chuck to a mixing bowl, preserves.
Described operation also comprises
Figure 964536DEST_PATH_IMAGE006
Particle screen selecting: to operation
Figure 130069DEST_PATH_IMAGE005
The slurry that makes carries out viscosity test, and viscosity is qualified sieves afterwards to slurry, removes bulky grain in case cause broken belt during coating.
Thickener consumption of the present invention is 0.5～1.0 part, weight portion.
When raw material binding agent of the present invention was the polyacrylonitrile copolymer, the thickener consumption can be 0.
Stirring at low speed speed of the present invention is revolution 15 ± 5HZ, rotation 10 ± 2HZ; High-speed stirred speed is revolution 35 ± 5HZ, rotation 30 ± 5 HZ.
Operation of the present invention
Figure 615945DEST_PATH_IMAGE003
Described in the scraper concrete operations be to scrape in a mixing bowl with material scraping plate stirring the remaining slurry that casing wall splashes on slurry and the mixer.
The present invention removes
Figure 364458DEST_PATH_IMAGE001
Figure 384498DEST_PATH_IMAGE002
Outer other operations of siccative mixed processes stir and leave standstill preservation all carries out under vacuum.
The sodium salt of carboxymethyl cellulose ether belongs to the anionic cellulose ether, is white or milky fibrous powder or particle, density 0.5-0.7g/cm 3, almost odorless, tasteless has moisture absorption, be easy to be dispersed in water into transparent colloidal solution, insoluble in the organic solvents such as ethanol, rise rapidly 20 ℃ of following viscosity, change slowlyer in the time of 45 ℃, long-time heating can make its colloid sex change and viscosity and performance obviously descend more than 85 ℃.Design philosophy of the present invention is that temperature is controlled at below 80 ℃, guarantees the consistency of sodium carboxymethylcellulose, improves his activity, can dissolve fast.
The polyacrylonitrile outward appearance is white powder, and density is 1.14 ~ 1.15g/cm 3Softening concurrent solution estranged when being heated to 220 ~ 300 ℃, approximately 90 ℃ of vitrification points, it is dissolved in dimethyl formamide, dimethyl sulfoxide (DMSO), sulfolane, nitric acid ethylidene ester isopolarity organic solvent, can also be dissolved in the special solvents such as the fortified aqueous of the inorganic salts such as rhodanate, perchlorate, zinc chloride, lithium bromide and red fuming nitric acid (RFNA).So the temperature of batching and binding agent dissolving preferably is controlled at below 90 ℃.
The invention solves that the present lithium ion battery distributing process time is long, utilization rate of equipment and installations is low and low these three problems of output.The lithium ion battery distributing process time was controlled at about five hours, roughly was 1/2nd of the prior art batching time, had so both improved utilization rate of equipment and installations, had reduced again cost, and had not affected battery performance.
Embodiment
Embodiment 1
Thickener: the CMC(sodium carboxymethylcellulose) 0.5 wt%;
Binding agent: SBR(butadiene-styrene rubber) 1.2 wt%;
Conductive agent: the agent of SP(carbon black conductive) 0.5 wt%;
Negative electrode active material: the AG(Delanium) 44.4 wt%;
Solvent: H 2The O(deionized water) 53.4 wt%;
Siccative mixes: pill tank adds above-mentioned formula rate: thickener CMC, conductive agent SP and inventory 50.0wt% negative electrode active material AG stirring at low speed 30 minutes, preserve;
Figure 797079DEST_PATH_IMAGE002
In above-mentioned slurry, added again other 50.0wt% negative electrode active material AG elder generation stirring at low speed 10 minutes, scraper, high-speed stirred 30 minutes is even to slurry again, preserves;
Figure 83704DEST_PATH_IMAGE003
Add solvent H 2O dispersed paste: add solvent H in the slurry above-mentioned finishing 2O, stirring at low speed 10 minutes, scraper, then high-speed stirred is 30 minutes, preserves;
Figure 223829DEST_PATH_IMAGE004
High-temperature process: in mixing plant (carry and add circulating water device), add heat recirculated water and make slurry be warming up to 80 ℃, carried out again high-speed stirred 45 minutes, perhaps slurry is carried out 80 ℃ of high-temperature bakings processed in 45 minutes, scraper, continuation was carried out high-speed stirred 60 minutes to slurry, a mixing bowl is added recirculated water make slurry be cooled to 35 ℃, preserve;
Figure 885011DEST_PATH_IMAGE005
Add binding agent: in the above-mentioned slurry of finishing, add recipe ratio weight binding agent SBR and carried out high-speed stirred 60 minutes, a mixing bowl is added recirculated water make slurry be cooled to 25 ℃, preserve;
Figure 94276DEST_PATH_IMAGE006
Particle screen selecting: the slurry of finishing is above carried out viscosity test, and viscosity is qualified sieves afterwards to slurry, removes bulky grain in case cause broken belt during coating.
Embodiment 2
Binding agent: LA (polyacrylonitrile copolymer) 1.6 wt%;
Conductive agent: the agent of SP(carbon black conductive) 0.5 wt%;
Negative electrode active material: the AG(Delanium) 50.5 wt%
Solvent: H 2The O(deionized water) 47.4 wt%
Figure 935324DEST_PATH_IMAGE001
Siccative mixes: pill tank adds above-mentioned recipe ratio weight: binding agent LA, conductive agent SP and 50.0wt% negative electrode active material AG stirring at low speed 30 minutes, preserve;
Figure 179223DEST_PATH_IMAGE002
In above-mentioned slurry, add again other 50.0wt% negative electrode active material AG, first stirring at low speed 10 minutes, scraper, even to slurry to slurry high-speed stirred 30 minutes again, preserve;
Figure 946060DEST_PATH_IMAGE003
Add solvent H 2O dispersed paste: add solvent H in the slurry above-mentioned finishing 2O, stirring at low speed 10 minutes, scraper, then high-speed stirred is 30 minutes, preserves;
Figure 908200DEST_PATH_IMAGE004
High-temperature process: slurry is warming up to 80 ℃ of high-speed stirred 45 minutes by mixing plant recirculated water, and scraper was carried out high-speed stirred 120 minutes to slurry again, and a mixing bowl is added recirculated water make slurry be cooled to 40 ℃,
Preserve;
5. particle screen selecting: the slurry of finishing is above carried out viscosity test, and viscosity is qualified sieves afterwards to slurry, removes bulky grain in case cause broken belt during coating.
Embodiment 3
Binding agent: PVDF (Kynoar) 1.5 wt%
Conductive agent: the agent of SP(carbon black conductive) 0.7 wt%;
Negative electrode active material: CG (composite graphite) 47.7 wt%
Solvent: the NMP(N-methyl pyrrolidone) 50.0 wt%
Figure 287360DEST_PATH_IMAGE001
Siccative mixes: pill tank adds above-mentioned recipe ratio weight: binding agent PVDF, conductive agent SP and 50.0wt% negative electrode active material CG low speed 30 minutes, preserve;
Figure 385766DEST_PATH_IMAGE002
In above-mentioned slurry, added again other 50.0wt% negative electrode active material CG elder generation stirring at low speed 5 minutes, scraper, even to slurry to slurry high-speed stirred 40 minutes again, preserve;
Figure 344011DEST_PATH_IMAGE003
Add solvent NMP dispersed paste: add solvent NMP in the slurry above-mentioned finishing, stirring at low speed 10 minutes, scraper, then high-speed stirred is 30 minutes, preserves;
Figure 340917DEST_PATH_IMAGE004
High-temperature process: slurry is carried out 40 minutes processing of 80 ℃ of high-temperature bakings, and scraper was carried out high-speed stirred 120 minutes to slurry again, a mixing bowl is added recirculated water make slurry be cooled to 45 ℃, preserved;
5. particle screen selecting: the slurry of finishing is above carried out viscosity test, and viscosity is qualified sieves afterwards to slurry, removes bulky grain in case cause broken belt during coating.

Claims (7)

1. lithium ion battery negative proportioning process, its parts by weight of raw materials proportioning is:
Binding agent: 0.5～1.7;
Thickener: 0～1.3;
Conductive agent: 0.5～0.7;
Negative electrode active material: 44.0～51.0;
Solvent: 45.3～55.0;
Described thickener comprises sodium carboxymethylcellulose;
Described binding agent comprises polyvinyl alcohol, polytetrafluoroethylene, sodium carboxymethylcellulose, polyolefin, Kynoar, butadiene-styrene rubber, Viton, polyurethane, polyacrylonitrile copolymer;
Described conductive agent comprises the graphite agent, the carbon black conductive agent;
Described negative electrode active material comprises native graphite, Delanium, composite graphite;
Described solvent comprises deionized water, 1-METHYLPYRROLIDONE;
Its operation comprises:
Figure 2011102053828100001DEST_PATH_IMAGE001
Siccative mixes one: add the negative electrode active material of thickener, conductive agent and 1/2 recipe ratio weight by recipe ratio in a mixing bowl, stirred 30 ± 15 minutes;
Figure 446366DEST_PATH_IMAGE002
Siccative mixes two: in operation The negative electrode active material that adds residue 1/2 recipe ratio weight in the slurry that makes carried out stirring at low speed 10 ± 5 minutes, stirred complete rear scraper, and high-speed stirred 30 ± 15 minutes is even to slurry again;
Figure 2011102053828100001DEST_PATH_IMAGE003
Adding solvent disperses: in operation Add described solvent in the slurry that makes, stirring at low speed 10 ± 5 minutes, scraper, high-speed stirred is 30 ± 15 minutes again, preserves;
Figure 511121DEST_PATH_IMAGE004
High-temperature process: heat up, make operation
Figure 883197DEST_PATH_IMAGE003
The slurry that makes is warming up to 80 ± 5 ℃, high-speed stirred 45 ± 5 minutes; Perhaps with operation
Figure 999926DEST_PATH_IMAGE003
The slurry that makes toasted 45 ± 5 minutes under 80 ± 5 ℃ of high temperature, continued high-speed stirred 60 ± 15 minutes again, then made slurry be cooled to 45 ~ 60 ℃, preserved;
Figure 2011102053828100001DEST_PATH_IMAGE005
Add binding agent: get operation
Figure 928699DEST_PATH_IMAGE004
The slurry that makes adds recipe ratio weight binding agent, and then high-speed stirred 60 ± 15 minutes makes slurry be cooled to 25 ~ 45 ℃, preserves.
2. lithium ion battery negative proportioning process according to claim 1, it is characterized in that: described operation also comprises
Figure 145310DEST_PATH_IMAGE006
Particle screen selecting: to operation
Figure 688287DEST_PATH_IMAGE005
The slurry that makes carries out viscosity test, and viscosity is qualified sieves afterwards to slurry, removes bulky grain in case cause broken belt during coating.
3. lithium ion battery negative proportioning process according to claim 1, it is characterized in that: described thickener consumption is 0.5～1.0 part, weight portion.
4. lithium ion battery negative proportioning process according to claim 1, it is characterized in that: when described raw material binding agent was the polyacrylonitrile copolymer, the thickener consumption was 0.
5. lithium ion battery negative proportioning process according to claim 1 is characterized in that: described stirring at low speed speed is revolution 15 ± 5HZ, rotation 10 ± 2HZ; High-speed stirred speed is revolution 35 ± 5HZ, rotation 30 ± 5 HZ.
6. lithium ion battery negative proportioning process according to claim 1 is characterized in that: operation
Figure 59357DEST_PATH_IMAGE002
, operation
Figure 713192DEST_PATH_IMAGE003
Described in the scraper concrete operations be to scrape in a mixing bowl with material scraping plate stirring the remaining slurry that casing wall splashes on slurry and the mixer.
7. lithium ion battery negative proportioning process according to claim 1 is characterized in that: remove
Figure 984642DEST_PATH_IMAGE001
,
Figure 698520DEST_PATH_IMAGE002
Outer other operations of siccative mixed processes stir and leave standstill preservation all carries out under vacuum.
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Cited By (11)

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CN103296254A (en) * 2013-04-16 2013-09-11 江苏力天新能源科技有限公司 Preparation method for lithium ion battery negative pole slurry
CN104409736A (en) * 2014-11-14 2015-03-11 无锡信大气象传感网科技有限公司 Lithium ion battery anode material and manufacturing method thereof
CN105047854A (en) * 2015-06-30 2015-11-11 保定风帆新能源有限公司 Preparation method for anode material of lithium ion battery
CN106486643A (en) * 2015-11-25 2017-03-08 上海杉杉科技有限公司 A kind of preparation technology of lithium cell cathode material
CN108305987A (en) * 2018-01-31 2018-07-20 北京国能电池科技股份有限公司 Proportioning process, anode plate for lithium ionic cell and the lithium ion battery of lithium ion battery anode slurry
CN108539121A (en) * 2018-04-16 2018-09-14 江西迪芯能源科技有限公司 A kind of lithium ion battery anode slurry and lithium ion battery
CN109768253A (en) * 2019-01-11 2019-05-17 合肥国轩高科动力能源有限公司 A kind of proportioning process of lithium ion battery negative material
CN111554937A (en) * 2020-05-26 2020-08-18 苏州凌威新能源科技有限公司 Negative electrode slurry, negative electrode sheet and preparation method thereof
CN111725508A (en) * 2020-06-22 2020-09-29 湖北亿纬动力有限公司 Preparation method of negative electrode slurry without glue solution, obtained negative electrode slurry and application
CN112072093A (en) * 2020-09-18 2020-12-11 天科新能源有限责任公司 Lithium battery negative electrode slurry with good dispersion effect and preparation method thereof
CN115602807A (en) * 2022-09-08 2023-01-13 中国新型建材设计研究院有限公司（Cn） Industrial preparation method of carbon-coated silicon monoxide negative electrode material

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Publication number Priority date Publication date Assignee Title
CN103296254A (en) * 2013-04-16 2013-09-11 江苏力天新能源科技有限公司 Preparation method for lithium ion battery negative pole slurry
CN104409736A (en) * 2014-11-14 2015-03-11 无锡信大气象传感网科技有限公司 Lithium ion battery anode material and manufacturing method thereof
CN105047854A (en) * 2015-06-30 2015-11-11 保定风帆新能源有限公司 Preparation method for anode material of lithium ion battery
CN105047854B (en) * 2015-06-30 2017-11-10 保定风帆新能源有限公司 A kind of lithium ion battery cathode slurry preparation method
CN106486643A (en) * 2015-11-25 2017-03-08 上海杉杉科技有限公司 A kind of preparation technology of lithium cell cathode material
CN108305987B (en) * 2018-01-31 2021-02-09 北京国能电池科技股份有限公司 Proportioning process of lithium ion battery negative electrode slurry, lithium ion battery negative electrode sheet and lithium ion battery
CN108305987A (en) * 2018-01-31 2018-07-20 北京国能电池科技股份有限公司 Proportioning process, anode plate for lithium ionic cell and the lithium ion battery of lithium ion battery anode slurry
CN108539121A (en) * 2018-04-16 2018-09-14 江西迪芯能源科技有限公司 A kind of lithium ion battery anode slurry and lithium ion battery
CN109768253A (en) * 2019-01-11 2019-05-17 合肥国轩高科动力能源有限公司 A kind of proportioning process of lithium ion battery negative material
CN111554937A (en) * 2020-05-26 2020-08-18 苏州凌威新能源科技有限公司 Negative electrode slurry, negative electrode sheet and preparation method thereof
CN111725508A (en) * 2020-06-22 2020-09-29 湖北亿纬动力有限公司 Preparation method of negative electrode slurry without glue solution, obtained negative electrode slurry and application
CN112072093A (en) * 2020-09-18 2020-12-11 天科新能源有限责任公司 Lithium battery negative electrode slurry with good dispersion effect and preparation method thereof
CN115602807A (en) * 2022-09-08 2023-01-13 中国新型建材设计研究院有限公司（Cn） Industrial preparation method of carbon-coated silicon monoxide negative electrode material
CN115602807B (en) * 2022-09-08 2023-10-31 中国新型建材设计研究院有限公司 Industrial preparation method of carbon-coated silicon oxide negative electrode material

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