CN105185951A - Preparation method of lithium battery cathode slurry - Google Patents
Preparation method of lithium battery cathode slurry Download PDFInfo
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- CN105185951A CN105185951A CN201510523079.0A CN201510523079A CN105185951A CN 105185951 A CN105185951 A CN 105185951A CN 201510523079 A CN201510523079 A CN 201510523079A CN 105185951 A CN105185951 A CN 105185951A
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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
- H01M4/04—Processes of manufacture in general
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
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Abstract
The invention provides a preparation method of lithium battery cathode slurry. The method comprises the following steps: (A) adding a cathode active material, a conductive agent, a binder and a solvent to an agitating vessel at the ratio, and stirring and dispersing the raw materials; (B) adding 55%-60% of solvent to the stirred powder, and stirring and dispersing the powder, wherein the slurry temperature is 25-35 DEG C; (C) adding 35%-30% of solvent to the slurry obtained in the step (B), stirring and dispersing the slurry, wherein the slurry temperature is 25-35 DEG C; (D) carrying out a viscosity test on the viscosity of the slurry stirred in the step (B), if the viscosity is 3,000MPa.S to 8,000MPa.S, directly entering the next step; and (E) carrying out vacuum supply on the vessel body in a low-speed stirring state, wherein the vacuum degree is minus 0.09MPa to minus 0.1MPa and the time is 15-30 minutes, thus obtaining the cathode slurry. A lithium battery prepared from the lithium battery cathode slurry provided by the invention is low in internal resistance, not easy to heat, high in energy density, good in cycle performance and long in service life.
Description
Technical field
The present invention relates to field of lithium ion battery, be specially a kind of preparation technology and method of positive electrode slurry.
Background technology
At present continuous deterioration with climatic environment in short supply along with global petroleum resources, human social development is faced with stern challenge.The new-energy automobile of development clean energy-saving is subject to the great attention of countries in the world.The development of new-energy automobile, crucial in its electrical source of power.Lithium ion battery has the advantages such as energy density is large, self discharge is little, memory-less effect, operating voltage range are wide, long service life, non-environmental-pollution, is the main electrical source of power of current new-energy automobile.
Lithium ion battery generally comprises positive plate, negative plate, is interval in barrier film between positive plate and negative plate.Anode pole piece comprises plus plate current-collecting body and is coated on the positive pole diaphragm on plus plate current-collecting body, and negative plate comprises negative current collector and is coated on the cathode membrane on negative current collector.Time prepared by electrode plates, first by active material (as cobalt acid lithium, graphite etc.), conductive agent is (as acetylene black, carbon nano-tube, carbon fiber etc.), bonding agent (as Kynoar, PVP, sodium carboxymethylcellulose, SBR emulsion etc.) and solvent (as 1-METHYLPYRROLIDONE, water etc.) make electrode slurry together, again it is coated in collection liquid surface on request, then carry out drying, obtain battery pole piece.
Wherein the performance of performance on lithium ion battery of electrode slurry has important impact.In electrode slurry, each component disperses must be more even, the processing characteristics that pole piece has just had, and electrode distribution of impedance is everywhere even, when discharge and recharge, the effect of active material can play larger, its average gram volume plays and will promote to some extent, thus promotes the performance of full battery.
In practical application, conductive agent binder solution is carried out high-revolving double planetary dispersion by traditional anode sizing agent preparation method, then adds positive active material, obtains final anode sizing agent after carrying out the stirring of certain hour.First this kind of method need long time treatment to the dispersion of conductive agent, length consuming time and dispersity is unsatisfactory, especially for adopting carbon nano-tube (CNT), Graphene etc. be prepared by the slurry of conductive agent; Secondly traditional handicraft needs in slurry preparation process, keeps vacuumizing state always, cause slurry system internal temperature easily to raise to stirring system, adds recirculated water again simultaneously cool in outside, therefore all very high with wearing and tearing to the requirement of equipment.More than cause that slurry preparation efficiency is low, poor stability, effect are undesirable, all can impact the preparation of follow-up pole piece, the performance of lithium battery.
Summary of the invention
In order to overcome problems of the prior art, the object of this invention is to provide a kind of preparation method of lithium battery anode slurry, dispersed to each component of slurry to realize within a short period of time, its slurry uniformity prepared is good, excellent in stability, its battery pole piece adhesion prepared is improved simultaneously, and therefore improves the chemical property of battery with two side terminals and battery thereof.
In order to realize foregoing invention object, the present invention adopts technical scheme as described below:
Step 1, dispersion powder: positive active material, conductive agent, binding agent are added agitator dispersed with stirring in proportion, the time is 30 ~ 40 minutes, and time 1/2 and at the end of, scrape the powder on paddle and staving;
Step 2, high-viscosity stirring: add in 55% ~ 60% powder after above-mentioned stirring of solvent total amount, dispersed with stirring, the time is 60 ~ 70 minutes, and the time 1/3,2/3 and at the end of, scrape the slurry on paddle and staving, slurry temperature controls between 25 ~ 35 DEG C;
Step 3, low viscosity stir: add in 35 ~ 30% slurries after above-mentioned high-viscosity stirring of solvent total amount, dispersed with stirring, the time is 60 ~ 70 minutes, and the time 1/3,2/3 and at the end of, scrape the slurry on paddle and staving, slurry temperature controls between 25 ~ 35 DEG C;
Step 4, viscosity test: the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, as at normal range (NR) 3000 ~ 8000MpaS, directly enters next step vacuum froth breaking; As exceeded above-mentioned scope, then add 5% ~ 10% of solvent total amount, then dispersed with stirring, time is 30 ~ 40 minutes, and time 1/2 and at the end of, scrape the slurry on paddle and staving, detect a slurry viscosity again, reaching range of viscosities requirement can enter next step;
Step 5, vacuum froth breaking: under stirring at low speed state, vacuumize staving, vacuum degree is-0.09 ~-0.1MPa, and the time is 15 ~ 30 minutes, namely obtains the anode sizing agent prepared by the inventive method.
Preferably, in above-mentioned steps 1, positive active material is LiCoO
2, LiNiO
2, LiMn
2o
4, LiNi
xco
ymn
(1-x-y)o
2one or more mixtures in (0 < x < 1,0 < y < 1,0 < x+y < 1) and LiFePO4.
Preferably, in above-mentioned steps 1, conductive agent is one or more mixtures in conductive black, electrically conductive graphite, carbon nano-tube, carbon fiber, Graphene.
Preferably, in above-mentioned steps 1, binding agent is Kynoar (PVDF).
Preferably, in above-mentioned steps 2, solvent is 1-METHYLPYRROLIDONE (NMP).
Preferably, in above-mentioned steps 1 and step 2, the mass ratio of each component of positive active material, conductive agent, binding agent is followed successively by (90-97): (1-4): (1-5), and solvent is 50% ~ 100% of above-mentioned each component total amount.
Preferably, in above steps, mixing plant is double-planet de-airing mixer, and slurry temperature is that the method that utilization passes into the thermostatical circulating water of relevant temperature to planet stirring bucket controls.
Owing to adopting technique scheme, present invention offers following beneficial effect:
1, preparation time is short: anode sizing agent preparation time whole process of the present invention is about 195 ~ 250 minutes, and in subsequent preparation process, by the accumulation of practical experience several times, viscosity test step can be omitted, directly enter last vacuum defoaming process, 30 ~ 40 minutes can be saved again thus, compare the conventional fabrication process preparation time of about 5 ~ 8 hours, substantially increase production efficiency;
2, equipment attrition is little: the present invention only in the end just needs to vacuumize staving in vacuum defoaming process, compare traditional handicraft to need in slurry preparation process, keep vacuumizing state to stirring system always, heat difficulty in whipping process is caused to distribute, the drawback that slurry temperature easily raises, have substance and improve effect, the short time vacuumizes process and reduces facility load, reduces equipment attrition;
3, energy consumption is low: the anode sizing agent solid content obtained by the present invention is about 50 ~ 65%, compare conventional fabrication process, have high solids content, low viscous feature, the quantity of solvent therefore used is corresponding minimizing also, reduces in subsequent coating processes the energy consumption needed for solvent evaporation and recovery;
4, dispersion effect is good: positive active material, conductive agent, binding agent are first carried out dispersed with stirring by the present invention, avoid conductive agent and produce reunion in the slurry, adopt high-viscosity stirring dispersion early stage, the mechanicals efforts (extruding, collision, friction) of paddle to slurry is large, good dispersion effect can be played, adopt low viscosity to stir again, each component is thoroughly scatter.
Adopt the lithium battery obtained by lithium battery anode slurry provided by the invention, internal resistance is low, not easily generates heat, and energy density is high, good cycle, long service life.
Accompanying drawing explanation
Fig. 1 is the loop test capability retention comparison diagram of embodiment 1 and comparative example 1.
Fig. 2 is the loop test capability retention comparison diagram of embodiment 2 and comparative example 2.
Embodiment
Below in conjunction with accompanying drawing, preferably embodiment of the present invention is described in further detail:
Embodiment 1
Take LiFePO4 as positive active material, SP is conductive agent, and PVDF is binding agent, according to LiFePO
4: the mass ratio of SP:PVDF=95.7:2.3:2.0, solvent NMP is 100% of above-mentioned each component total amount.Preparation process is as follows:
1, each component is added agitator dispersed with stirring, the time is 40 minutes, and when 20 minutes time and 40 minutes, scrapes the powder on paddle and staving;
2, add in 55% powder after above-mentioned stirring of NMP total amount, dispersed with stirring, the time is 70 minutes, and when 20 minutes time, 40 minutes and 60 minutes, scrapes the slurry on paddle and staving, and slurry temperature controls between 25 ~ 35 DEG C;
3, add in 35% slurry after above-mentioned high-viscosity stirring of solvent total amount, dispersed with stirring, the time is 60 minutes, and when 23 minutes time, 46 minutes and 70 minutes, scrapes the slurry on paddle and staving, and slurry temperature controls between 25 ~ 35 DEG C;
4, the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, test result is 8514MpaS, super normal range value, adds 5% of solvent total amount, then dispersed with stirring, time is 40 minutes, and when 20 minutes time and 40 minutes, scrape the slurry on paddle and staving, then detect a slurry viscosity, test result is 7627MpaS, reaches range of viscosities requirement;
5, under stirring at low speed state, vacuumize staving, vacuum degree is-0.09 ~-0.1MPa, and the time is 30 minutes, namely obtains the anode sizing agent prepared by the inventive method, about 250 minutes consuming time altogether.
According to lithium battery conventional production process, by anode sizing agent through coating, dry, roll film, point cut into positive plate, then be assembled into negative plate, barrier film, electrolyte, battery case, after discharge and recharge activation, obtained 18650 types, initial designs capacity are the cylinder ferric phosphate lithium cell of 1350mA.
Comparative example 1
Lithium iron phosphate cathode slurry production technology conveniently, prepares about 7 hours consuming time, and according to lithium battery conventional production process, obtained 18650 types, initial designs capacity are the cylinder LiFePO4 power type battery of 1350mA.
Electrical performance testing is carried out to 18650 type cylinder ferric phosphate lithium cells obtained by embodiment 1 and comparative example 1, its charge and discharge under 1C, the circulation volume conservation rate of 1000 times, embodiment 1 is 97.92%, comparative example 1 is 95.23%, comparing result as shown in Figure 1, energy density and inner walkway comparing result as shown in table 1.
Embodiment 2
With cobalt acid lithium for positive active material, SP and KS-6 is conductive agent, and PVDF is binding agent, according to LiCoO
2: the mass ratio of SP:KS-6:PVDF=93:2.2:1.3:3.5, solvent NMP is 60% of above-mentioned each component total amount.Preparation process is as follows:
1, each component is added agitator dispersed with stirring, the time is 30 minutes, and when 15 minutes time and 30 minutes, scrapes the powder on paddle and staving;
2, add in 60% powder after above-mentioned stirring of NMP total amount, dispersed with stirring, the time is 60 minutes, and when 20 minutes time, 40 minutes and 60 minutes, scrapes the slurry on paddle and staving, and slurry temperature controls between 25 ~ 35 DEG C;
3, add in 30% slurry after above-mentioned high-viscosity stirring of solvent total amount, dispersed with stirring, the time is 60 minutes, and when 20 minutes time, 40 minutes and 60 minutes, scrapes the slurry on paddle and staving, and slurry temperature controls between 25 ~ 35 DEG C;
4, the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, test result is 6149MpaS, belongs to normal range value, reaches requirement;
5, under stirring at low speed state, vacuumize staving, vacuum degree is-0.09 ~-0.1MPa, and the time is 15 minutes, namely obtains the anode sizing agent prepared by the inventive method, about 165 minutes consuming time altogether.
According to lithium battery conventional production process, by anode sizing agent through coating, dry, roll film, point cut into positive plate, then be assembled into negative plate, barrier film, electrolyte, battery case, after discharge and recharge activation, obtained 18650 types, initial designs capacity are the cylindrical battery of 2000mA.
Comparative example 2
Lithium cobaltate cathode slurry production process conveniently, prepares about 6.5 hours consuming time, and according to lithium battery conventional production process, obtained 18650 types, initial designs capacity are the cylindrical battery of 2000mA.
Electrical performance testing is carried out to 18650 type cylindrical batteries obtained by embodiment 1 and comparative example 1, its charge and discharge under 1C, the circulation volume conservation rate of 1000 times, embodiment 1 is 97.23%, comparative example 1 is 93.23%, comparing result as shown in Figure 2, energy density and inner walkway comparing result as shown in table 1.
The energy density of each embodiment of table 1 and comparative example and inner walkway comparing result
| Project | Energy density (Wh/L) | Internal resistance (m Ω) |
| Embodiment 1 | 127.6 | 45.1 |
| Comparative example 1 | 118.4 | 49.3 |
| Embodiment 2 | 154.7 | 37.5 |
| Comparative example 2 | 142.9 | 40.8 |
As can be seen from the above table, adopt the lithium battery obtained by anode sizing agent prepared by the inventive method, all higher than the lithium battery obtained by conventional cathode slurry production process in energy density, all lower than the lithium battery obtained by conventional cathode slurry production process in internal resistance.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (9)
1. a preparation method for lithium battery anode slurry, is characterized in that, comprising:
Steps A: positive active material, conductive agent, binding agent and solvent are added agitator dispersed with stirring in proportion;
Step B: add in 55% ~ 60% powder after above-mentioned stirring of solvent total amount, dispersed with stirring, slurry temperature is 25 ~ 35 DEG C;
Step C: add in 35 ~ 30% to the step B slurries obtained of solvent total amount, dispersed with stirring, slurry temperature is 25 ~ 35 DEG C;
Step D: the slurry viscosity that above-mentioned steps B stirs is carried out viscosity test, if scope 3000 ~ 8000MpaS, directly enters next step; If exceed above-mentioned scope, then
Step D1: add 5% ~ 10% of solvent total weight, then dispersed with stirring, test slurry viscosity reaches range of viscosities requirement can enter next step;
Step e: under stirring, vacuumize staving, vacuum degree is-0.09 ~-0.1MPa, and the time is 15 ~ 30 minutes, namely obtains anode sizing agent.
2. preparation method as claimed in claim 1, it is characterized in that, in described steps A, the mass ratio of each component of positive active material, conductive agent and binding agent is followed successively by (90-97): (1-4): (1-5), solvent is 50% ~ 100% of positive active material, conductive agent and binding agent total amount, and mixing time is 30 ~ 40 minutes.
3. preparation method as claimed in claim 1, it is characterized in that, in described step B and C, the time of dispersion is 60 ~ 70 minutes.
4. preparation method as claimed in claim 1, it is characterized in that, in described steps A, positive active material is LiCoO
2, LiNiO
2, LiMn
2o
4, LiNi
xco
ymn
(1-x-y)o
2(0 < x < 1,0 < y < 1,0 < x+y < 1) and LiFePO
4in one or more mixtures, conductive agent adopts conductive black, electrically conductive graphite, carbon nano-tube, carbon fiber, one or more mixtures in Graphene, and binding agent adopts Kynoar, and solvent adopts 1-METHYLPYRROLIDONE.
5. preparation method as claimed in claim 1, it is characterized in that, in described step e, vacuum degree is-0.09 ~-0.1MPa, and the time is 15 ~ 30 minutes.
6. preparation method as claimed in claim 1, is characterized in that, in described steps A, the time 1/2 and at the end of, scrape the powder on paddle and staving.
7. preparation method as claimed in claim 1, is characterized in that, described step B and C and the time 1/3,2/3 and at the end of, scrape the slurry on paddle and staving.
8. preparation method as claimed in claim 1, is characterized in that, in described step D1, dispersed with stirring, the time is 30 ~ 40 minutes, and the time 1/2 and at the end of, scrape the slurry on paddle and staving, then test slurry viscosity.
9. preparation method as claimed in claim 1, is characterized in that, in above steps, mixing plant adopts double-planet de-airing mixer, and slurry temperature is that the method that utilization passes into the thermostatical circulating water of relevant temperature to planet stirring bucket controls.
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| CN201510523079.0A CN105185951A (en) | 2015-08-24 | 2015-08-24 | Preparation method of lithium battery cathode slurry |
| PCT/CN2015/098767 WO2017031884A1 (en) | 2015-08-24 | 2015-12-24 | Preparation method for lithium battery positive-electrode slurry |
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| CN105047858A (en) * | 2015-08-25 | 2015-11-11 | 田东 | Preparation method for lithium cobalt oxide cathode slurry |
| CN105161709A (en) * | 2015-08-25 | 2015-12-16 | 田东 | Preparation method of lithium manganate cathode slurry |
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| CN109244373A (en) * | 2018-11-08 | 2019-01-18 | 上海电气国轩新能源科技有限公司 | A kind of anode sizing agent and preparation method, lithium ion battery |
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| CN105161709A (en) * | 2015-08-25 | 2015-12-16 | 田东 | Preparation method of lithium manganate cathode slurry |
| CN105047858A (en) * | 2015-08-25 | 2015-11-11 | 田东 | Preparation method for lithium cobalt oxide cathode slurry |
| WO2017032165A1 (en) * | 2015-08-25 | 2017-03-02 | 田东 | Preparation method for lithium manganate positive-electrode slurry |
| WO2017032167A1 (en) * | 2015-08-25 | 2017-03-02 | 田东 | Preparation method for lithium cobalt oxide positive-electrode slurry |
| CN105514417A (en) * | 2016-01-28 | 2016-04-20 | 先进储能材料国家工程研究中心有限责任公司 | High-safety lithium ion battery cathode paste and preparation method thereof |
| WO2017206307A1 (en) * | 2016-06-03 | 2017-12-07 | 田东 | Method for applying graphene as conductive agent to anode slurry for lithium-ion batteries |
| CN106099029A (en) * | 2016-07-04 | 2016-11-09 | 金龙联合汽车工业（苏州）有限公司 | A kind of lithium ion battery electrode sizing agent process for dispersing |
| CN107617351A (en) * | 2017-07-31 | 2018-01-23 | 珠海格力电器股份有限公司 | A kind of negative electrode of lithium ion battery stirring means, purposes and lithium ion battery |
| CN107579205A (en) * | 2017-08-21 | 2018-01-12 | 江苏东汛锂业有限公司 | The formula and preparation technology of a kind of positive plate of lithium battery |
| CN108400287A (en) * | 2018-02-23 | 2018-08-14 | 安徽益佳通电池有限公司 | The method that lithium ion battery electrode sizing agent is prepared using vibration-mechanical agitation combination |
| CN109192941A (en) * | 2018-08-10 | 2019-01-11 | 欣旺达电子股份有限公司 | Lithium ion battery, positive plate, lithium ion battery anode glue size and preparation method thereof |
| CN109244373A (en) * | 2018-11-08 | 2019-01-18 | 上海电气国轩新能源科技有限公司 | A kind of anode sizing agent and preparation method, lithium ion battery |
| CN109244373B (en) * | 2018-11-08 | 2021-09-03 | 上海电气国轩新能源科技有限公司 | Positive electrode slurry, preparation method and lithium ion battery |
| CN110380015B (en) * | 2019-05-27 | 2020-09-29 | 合山市华美新能源科技有限公司 | Preparation method of lithium battery positive electrode slurry |
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