CN105024044A - Preparation method of high-capacity silica-powder-doped lithium battery anode slurry - Google Patents
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Abstract
The invention discloses a preparation method of high-capacity silica-powder-doped lithium battery anode slurry. Nanometer silica powder is added in the conventional anode slurry preparation process, so that the capacity playing performance of the material is improved and the requirement of lithium-ion batteries for high energy density can be met; besides, through steps of thickening agent solution preparation, powder dispersion, high-viscosity stirring, low-viscosity stirring, viscosity testing, vacuum foam removal and the like, all components, particularly the nanometer silica powder, are fully dispersed into an anode system, agglomeration of the nanometer silica powder is avoided, and the cycle stability is guaranteed. The method has the advantages that the preparation time is short, the equipment abrasion is low, the production energy consumption is low, the dispersion effect is good, and the like. The lithium batteries prepared from the provided anode slurry have low internal resistance, the volume energy density is obviously increased, and the cycle performance of the batteries is good.
Description
Technical field
This patent relates to field of lithium ion battery, is specially a kind of preparation method of nano silica fume elements doped lithium battery cathode 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.
The develop rapidly of lithium ion battery mainly has benefited from the contribution of electrode material, the particularly progress of negative material.What current commercial Li-ion battery negative material adopted is graphite-like material with carbon element, and having lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, is more satisfactory lithium ion battery negative material.Graphite-like material with carbon element, having lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, is more satisfactory lithium ion battery negative material.But its theoretical specific capacity only has 372mAh/g, thus limit the further raising of lithium ion battery specific energy, the demand of growing high-energy Portable power source can not be met.
Silicon is a kind of negative material being hopeful to replace material with carbon element most, this is because silicon has the peak capacity up to 4200mAh/g; And there is the stable discharge platform being similar to graphite.But with other high power capacity Metal Phase seemingly, the non-constant of cycle performance of silicon, can not carry out normal charge and discharge cycles.When silicon uses as negative material, in charge and discharge cycles process, the reversible generation of Li2Si alloy and decomposition are along with huge change in volume, the mechanical disintegration of alloy (producing crack and efflorescence) can be caused, cause the avalanche of material structure and peeling off of electrode material and make electrode material lose electrical contact, thus cause the cycle performance of electrode sharply to decline, finally cause electrode failure, therefore in lithium-ions battery, be difficult to practical application.Research shows, the silicon of small particle diameter or its alloy all improve a lot on capacity or on cycle performance, when the particle of alloy material reaches nanoscale, volumetric expansion in charge and discharge process can alleviate greatly, performance also can increase, but nano material has larger surface energy, easily reunites, efficiency for charge-discharge can be made on the contrary to reduce and accelerate the decay of capacity, thus counteract the advantage of nano particle.
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 thickener soln is carried out high-revolving double planetary dispersion by traditional cathode size preparation method, then add negative electrode active material, after carrying out the stirring of certain hour, then stirring obtains final cathode size through the row short time to add binding agent.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 high power capacity silica flour elements doped lithium battery cathode slurry, to realize within a short period of time to each component of slurry, especially nano silica fume is dispersed, its slurry uniformity prepared is good, excellent in stability, its battery pole piece adhesion prepared and gram volume are improved simultaneously, and therefore improve energy density and the cyclical stability of battery.
In order to realize foregoing invention object, the present invention adopts technical scheme as described below:
1, thickener soln preparation: added by a certain percentage in deionized water solvent by thickener sodium carboxymethylcellulose (CMC), be uniformly dissolved with mixer, take out for subsequent use, the time is 60 ~ 100 minutes;
2, dispersion powder: negative electrode active material, nano silica fume, conductive 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;
3, high-viscosity stirring: add in 55% ~ 60% powder after above-mentioned stirring of thickener soln 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;
4, low viscosity stirs: add in 35 ~ 30% slurries after above-mentioned high-viscosity stirring of thickener soln 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;
5, viscosity test: the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, as at normal range (NR) 2000 ~ 5000MpaS, directly enters next step; As exceeded above-mentioned scope, then add 5% ~ 10% of thickener soln 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;
6, binding agent adds: add binding agent SBR, dispersed with stirring, the time is 10 ~ 30 minutes;
7, 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 cathode size prepared by the inventive method.
In above-mentioned steps 2, negative electrode active material is one or more mixtures in Delanium, native graphite, lithium titanate, hard carbon, carbonaceous mesophase spherules.
In above-mentioned steps 2, the particle diameter of nano silica fume is not more than 70nm.
In above-mentioned steps 2, conductive agent is one or more mixtures in conductive black, electrically conductive graphite, carbon nano-tube, carbon fiber, Graphene.
In above-mentioned steps 1 and step 2, the mass ratio of each component of negative electrode active material, nano silica fume, conductive agent, thickener, binding agent is followed successively by (90-97): (1-10): (1-4): (1-5): (1-3), and solvent is 80% ~ 120% of above-mentioned each component total amount.
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.
Secondly, the present invention also has following characteristics:
1, gram specific capacity is high: the present invention is because of in traditional cathode size, add nano silica fume, the capacity that improve material plays performance, the requirement of lithium ion battery to high-energy-density can be met, and nano silica fume has fully disperseed in negative pole system, avoid the reunion of nano silica fume, ensure cyclical stability;
2, preparation time is short: cathode size preparation time whole process of the present invention is about 265 ~ 380 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 thus, first thickener soln is prepared if any multiple devices, 60 ~ 100 minutes can be saved again, compare the conventional anode blank preparation technics time of about 7 ~ 9 hours, substantially increase production efficiency;
3, 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;
4, energy consumption is low: the cathode size solid content obtained by the present invention is about 45 ~ 55%, compare conventional fabrication process, there is high solids content, low viscous feature, the ratio also corresponding minimizing of the water therefore used, reduce in subsequent coating processes the energy consumption needed for moisture evaporation.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1
Take Delanium as negative electrode active material, SP is conductive agent, and nano Si particle diameter is 50nm, by graphite: the mass ratio of Si:CMC:SBR=94.0:3.0:1.5:2.0:2.5, and solvent deionized water is 100% of above-mentioned each component total amount.Preparation process is as follows:
1, add in deionized water solvent by thickener CMC, be uniformly dissolved with mixer, take out for subsequent use, the time is 60 minutes;
2, negative electrode active material, nano-silicon, conductive agent are 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;
3, add in 55% powder after above-mentioned stirring of thickener soln 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, add in 35% slurry after above-mentioned high-viscosity stirring of thickener soln 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;
5, the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, test result is 5332MpaS, super normal range value, adds 5% of solvent total amount, then dispersed with stirring, time is 30 minutes, and when 15 minutes time and 30 minutes, scrape the slurry on paddle and staving, then detect a slurry viscosity, test result is 4215MpaS, reaches range of viscosities requirement;
6, add binding agent SBR, dispersed with stirring, the time is 10 minutes;
7, under stirring at low speed state, vacuumize staving, vacuum degree is-0.09 ~-0.1MPa, and the time is 15 minutes, namely obtains the cathode size prepared by the inventive method, about 265 minutes consuming time altogether.
According to lithium battery conventional production process, by cathode size through coating, dry, roll film, point cut into negative plate, then be assembled into iron phosphate lithium positive pole sheet, barrier film, electrolyte, battery case, obtained 18650 type cylinder ferric phosphate lithium cells after discharge and recharge activation.
Comparative example 1
Artificial plumbago negative pole slurry production process conveniently, prepares about 7 hours consuming time, according to lithium battery conventional production process, and obtained 18650 type cylinder ferric phosphate lithium cells.
Carry out electrical performance testing to 18650 type cylinder ferric phosphate lithium cells obtained by embodiment 1 and comparative example 1, the total capacity of battery, volume energy density, 500 circulation conservation rates and internal resistance of cell test comparison result are as shown in table 1.
Embodiment 2
Take native graphite as negative electrode active material, SP is conductive agent, and nano Si particle diameter is 50nm, by graphite: the mass ratio of Si:SP:CMC:SBR=94.5:7.0:2.0:1.6:1.9, and solvent deionized water is 80% of above-mentioned each component total amount.Preparation process is as follows:
1, add in deionized water solvent by thickener CMC, be uniformly dissolved with mixer, take out for subsequent use, the time is 120 minutes;
2, negative electrode active material, conductive agent are 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;
3, add in 60% powder after above-mentioned stirring of thickener soln total amount, dispersed with stirring, the time is 70 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, add in 35% slurry after above-mentioned high-viscosity stirring of thickener soln total amount, dispersed with stirring, the time is 70 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;
5, the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, test result is 4578MpaS, belongs to normal range value, reaches requirement;
6, add binding agent SBR, dispersed with stirring, the time is 30 minutes;
7, under stirring at low speed state, vacuumize staving, vacuum degree is-0.09 ~-0.1MPa, and the time is 30 minutes, namely obtains the cathode size prepared by the inventive method, about 360 minutes consuming time altogether.
According to lithium battery conventional production process, by cathode size through coating, dry, roll film, point cut into negative plate, then be assembled into lithium cobaltate cathode sheet, barrier film, electrolyte, battery case, the obtained stacked soft-package battery of 4244130 type after discharge and recharge activation.
Comparative example 1
Natural graphite cathode slurry production process conveniently, prepares about 7.5 hours consuming time, according to lithium battery conventional production process, and the obtained stacked soft-package battery of 4244130 type.
Carry out electrical performance testing to the stacked soft-package battery of 4244130 type obtained by embodiment 2 and comparative example 2, the total capacity of battery, volume energy density, 500 circulation conservation rates and internal resistance of cell test comparison result are as shown in table 1.
The circulation of each embodiment of table 1 and comparative example, multiplying power discharging and inner walkway comparing result
As can be seen from the above table, adopt the lithium battery obtained by cathode size prepared by the inventive method, all lower than the lithium battery obtained by conventional anode slurry production process in internal resistance, all higher than the lithium battery obtained by conventional anode slurry production process in battery capacity and volume energy density, 500 circulation volume conservation rates are lower than conventional anode, still there is the problem of decay mainly due to silica flour, but compare the behavior pattern of single silica flour, tool has greatly improved and improves.
Claims (6)
1. a preparation method for high power capacity silica flour elements doped lithium battery cathode slurry, its by the following technical solutions:,
(1) thickener soln preparation: added by a certain percentage in deionized water solvent by thickener sodium carboxymethylcellulose (CMC), be uniformly dissolved with mixer, take out for subsequent use, the time is 60 ~ 100 minutes;
(2) dispersion powder: negative electrode active material, nano silica fume, conductive 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;
(3) high-viscosity stirring: add in 55% ~ 60% powder after above-mentioned stirring of thickener soln 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;
(4) low viscosity stirs: add in 35 ~ 30% slurries after above-mentioned high-viscosity stirring of thickener soln 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;
(5) viscosity test: the slurry viscosity that above-mentioned steps low viscosity stirs is carried out viscosity test, as at normal range (NR) 2000 ~ 5000MpaS, directly enters next step; As exceeded above-mentioned scope, then add 5% ~ 10% of thickener soln 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;
(6) binding agent adds: add binding agent SBR, dispersed with stirring, the time is 10 ~ 30 minutes;
(7) 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 cathode size prepared by the inventive method.
2. the preparation method of a kind of high power capacity silica flour elements doped lithium battery cathode slurry according to claim 1, it is characterized in that, in above-mentioned steps (2), negative electrode active material is one or more mixtures in Delanium, native graphite, lithium titanate, hard carbon, carbonaceous mesophase spherules.
3. the preparation method of a kind of high power capacity silica flour elements doped lithium battery cathode slurry according to claim 1, is characterized in that, in above-mentioned steps (2), the particle diameter of nano silica fume is not more than 70nm.
4. the preparation method of a kind of high power capacity silica flour elements doped lithium battery cathode slurry according to claim 1, it is characterized in that, in above-mentioned steps (2), conductive agent is one or more mixtures in conductive black, electrically conductive graphite, carbon nano-tube, carbon fiber, Graphene.
5. the preparation method of a kind of high power capacity silica flour elements doped lithium battery cathode slurry according to claim 1, it is characterized in that, in above-mentioned steps (1), step (2), step (6), the mass ratio of each component of negative electrode active material, nano silica fume, conductive agent, thickener, binding agent is followed successively by (90-97): (1-10): (1-4): (1-5): (1-3), and solvent is 80% ~ 120% of above-mentioned each component total amount.
6. the preparation method of a kind of high power capacity silica flour elements doped lithium battery cathode slurry according to claim 1, it is characterized in that, 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.
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| CN201510524533.4A CN105024044A (en) | 2015-08-25 | 2015-08-25 | Preparation method of high-capacity silica-powder-doped lithium battery anode slurry |
| PCT/CN2016/071966 WO2017031943A1 (en) | 2015-08-25 | 2016-01-25 | Method for preparing negative electrode paste for high-capacity silica-powder-doped lithium battery |
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| CN106299272A (en) * | 2016-08-22 | 2017-01-04 | 浙江金开来新能源科技有限公司 | A kind of preparation method of silica flour doped lithium ion power battery cathode slurry |
| WO2017031943A1 (en) * | 2015-08-25 | 2017-03-02 | 田东 | Method for preparing negative electrode paste for high-capacity silica-powder-doped lithium battery |
| CN106784609A (en) * | 2017-03-10 | 2017-05-31 | 江西佳沃新能源有限公司 | A kind of cathode of lithium battery blank preparation technicses |
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| CN108390095A (en) * | 2018-02-11 | 2018-08-10 | 三门峡速达交通节能科技股份有限公司 | A kind of lithium battery material and preparation method thereof |
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| CN111697217A (en) * | 2020-06-15 | 2020-09-22 | 中国检验检疫科学研究院 | Preparation method of silicon/graphite composite cathode of lithium ion battery |
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