CN103280566A - Preparation methods of positive and negative pole pastes for lithium ion batteries - Google Patents
Preparation methods of positive and negative pole pastes for lithium ion batteries Download PDFInfo
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Abstract
The invention belongs to the technical field of pastes for lithium ion batteries and in particular relates to preparation methods of positive and negative pole pastes for lithium ion batteries. The preparation method of the negative pole paste comprises the following steps of: mixing an anti-sedimentation dispersing agent, a negative pole conductive agent and a negative pole active substance, then adding a solvent for stirring, and finally, adding water-based cement for uniformly stirring to obtain the negative pole paste. The preparation method of the positive pole paste comprises the following steps of: mixing a macromolecular adhesive, a positive pole conductive agent and an active substance, then adding a solvent and sufficiently and uniformly stirring the materials to obtain the positive pole paste. The preparation methods of the positive and negative pole pastes for the lithium ion batteries are simple and feasible, are short in production period and low in comprehensive cost and has a good dispersion effect; the production efficiency is greatly improved, and the stirring time is shortened by half compared with that of a traditional process; and the produced lithium battery has excellent battery core multiplying power, circulating property and high-temperature storage property.
Description
Technical field
The invention belongs to the pulp of lithium ion battery technical field, be specifically related to a kind of preparation method of lithium ion battery plus-negative plate slurry.
Background technology
When at present making lithium ion battery, anodal agitating procedure is generally binding agent is dissolved in the organic solvent, adds conductive agent then and stirs, and adds active material at last and stirs, can discharging after viscosity regulates, and its technological process is as shown in Figure 1.The negative pole agitating procedure is generally and earlier the anti-settling dispersant is dissolved in the solvent, adds conductive agent then and stirs, and adds active material again and stirs, and adds water-base cement at last and stirs, can discharging after viscosity regulates, and its technological process part Fig. 2.This agitating mode is because whenever a reinforced step all need be opened agitator tank, especially need to vacuumize stirring, need to stop vacuumizing earlier, open jar then, reinforced again, and then open vacuum stirring again, therefore this process need flower at least 15 to 20 minutes can extend manufacture cycle inefficiency greatly, energy consumption is big, the integrated cost height.
China Patent No. is: 200810008359.8, the preparation method of a kind of lithium ion battery cathode slurry of denomination of invention and negative pole, the method that discloses comprises thickener, negative electrode active material and solvent, wherein, described method with thickener, electrode active material and solvent comprises thickener and partial solvent mixed and is made into colloidal solution; This colloidal solution, negative active core-shell material and partial solvent are put into duplicate rows star mixer, stir; Add adhesive and remaining solvent then, stir again.Can make not only that according to preparation cathode size method provided by the invention preparation time shortens greatly, and homogeneity and stability that slurry disperses all improve greatly, the cycle performance of the battery of being made by this kind slurry also greatly improves, but the method with thickener and active material and solvent, be made in the process of colloid, because the viscosity of colloid is very big, pulverous negative electrode active material is difficult to scatter equably, cause the time of stirring to lengthen, and dispersion effect is bad.And should invent a preparation method at cathode size, and anode sizing agent still adopts traditional stirring technique equally, and the preparation technology of integral battery door is difficult to reach quick minimizing the time, and 300 circulation volume conservation rates of the battery for preparing are the highest can only to arrive 89%.
Another patent 201010258975.6 of China discloses a kind of lithium ion battery, cathode size and preparation method thereof, and this method may further comprise the steps: (1) is mixed back adding lubricant with negative electrode active material and cathode conductive agent and is stirred in blender; (2) will stir in the additive sodium carboxymethylcellulose CMC adding blender; (3) material in the above-mentioned blender is added in the blend glue stuff of negative pole aqueous solvent and negative pole binding agent, mixing and stirring is made cathode size.Described lubricant is the mixture of alcohol, ketone or alcohol and ketone.The present invention can effectively shorten wetting time owing to adopt wetting agent to mix with graphite and conductive agent, shortens the pulp preparation time, improves uniformity and the stability of cathode size.Be to take first that liquid adds fixing hybrid mode equally, dispersion effect is not good, and 300 capability retentions of the battery for preparing are the highest to have only 88.9%, and battery performance is not good.
Summary of the invention
The objective of the invention is at above-mentioned deficiency of the prior art, a kind of preparation method of lithium ion battery plus-negative plate slurry is provided, it has the characteristics simple, that mixing cycle is short, dispersion effect good, energy consumption is little and cost is low of producing, the lithium ion battery for preparing, it is big that it has the battery power output, battery high-temperature stable storing performance is good, the characteristics that battery circulation volume conservation rate is high.
Purpose of the present invention is achieved through the following technical solutions:
A kind of preparation method of lithium ion battery plus-negative plate slurry is characterized in that: cathode size comprises following preparation process:
A. cathode conductive agent, negative electrode active material and the anti-settling dispersant of powdery being put into agitator tank successively stirs;
B. after treating that each powder in the steps A mixes, add solvent, continue to stir, each powder is soaked into fully;
C. continue to stir after adding water-base cement in the agitator tank;
D. after treating that material among the step C stirs, regulate viscosity;
Anode sizing agent comprises following preparation process:
1) stirs in anodal conductive agent, positive active material and the high polymer binder adding agitator tank with powdery;
2) in agitator tank, add organic solvent then, stir, soak into fully until flour;
3) regulate viscosity.
Wherein, described cathode size comprises following preparation process:
A. earlier cathode conductive agent, negative electrode active material and the anti-settling dispersant of powdery are put into agitator tank successively, do not open vacuum, open revolution and rotation simultaneously and carry out dry powder stirring 15～90min, the rotating speed of revolution is 15～30 rev/mins, and the rotating speed of rotation is 500～1000 rev/mins; Revolution herein is used for mixing, so rotating speed need not be too fast, is diverted to the granular powder of chopping certainly, makes mixing more even, therefore needs bigger rotating speed.
B. after treating that each powder mixes in the steps A, in agitator tank, add solvent, setting the revolution rotating speed is 15～30 rev/mins, the rotation rotating speed is 500～1000 rev/mins, continue to stir 10～30min, to revolve round the sun during this time and the rotation paddle on dry powder scrape in the agitator tank, confirm that each powder soaks into fully;
C. be evacuated to-99kPa～-90kPa, setting the revolution rotating speed is 25～35 rev/mins, the rotation rotating speed is 1000～1500 rev/mins, after stirring 120～240min, add water-base cement, setting the revolution rotating speed again is 15～25 rev/mins, the rotation rotating speed is 500～800 rev/mins, adjust rotating speed to revolving round the sun 20～35 rev/mins after stirring 5～15min, 40～90min is stirred in 1000～1500 rev/mins of rotations; Just added water-base cement, prevented that rotating speed is excessive, water-base cement is splashed the agitator tank top, therefore when adding water-base cement rotating speed is suitably reduced.
D. add organic solvent, adjust rotating speed to revolving round the sun 15～25 rev/mins, 10～30min is stirred in 500～800 rev/mins of rotations, utilizes solvent adjustment slurry viscosity at 1500-4000 mPas.Concrete, organic solvent is the N-methyl pyrrolidone, and it can effectively reduce the surface tension of slurry, reduces the generation of cathode size bubble, filters more smooth and easyly, and the negative plate after coating is dried is more soft, and pole piece is difficult for dry linting behind the pair roller, and the surface is more level and smooth.
The mixer that the present invention uses is duplicate rows star mixer, can revolve round the sun simultaneously and the rotation stirring.
Wherein, among the described step D, after viscosity mixes up, open vacuum and continue revolution stirring 10-30min, 15～35 rev/mins of revolution speeds,, use 150 purpose steel sieve to filter discharging.After only opening revolution vacuum stirring slowly, can farthest remove bubble, preventing that coating from producing because bubble breaks reveals the Copper Foil phenomenon.
Wherein, described cathode conductive agent comprises conductive carbon black, electrically conductive graphite, carbon fiber and carbon nano-tube any or several mixtures, described negative electrode active material comprises any or several mixture wherein in Delanium, native graphite, soft carbon and the hard carbon, described anti-settling dispersant is that the described water-base cement of sodium carboxymethylcellulose is SBR emulsion, concrete, the solid content of SBR emulsion is 50%.Its dielectric property are better, and ease of solubility is strong, and the solution viscosity is improved, and form colloid substance, are easy to coating.
Wherein, the slurry of described positive pole comprises following preparation process:
1) anodal conductive agent, positive active material and the high polymer binder of powdery are put into agitator tank successively, do not open vacuum, open revolution and rotation simultaneously and carry out dry powder stirring 15～90min, the revolution rotating speed is 15～30 rev/mins, and the rotation rotating speed is 500～1000 rev/mins; The material that this step stirs is powder entirely, does not vacuumize, and prevents that powder from flying upward.The purpose of revolution is to mix, and the purpose of rotation is to provide shearing force that particle is shredded, and makes mixing more fully with even.
2) treat that each powder mixes in the step 1) after, add the N-methyl pyrrolidone, setting the revolution rotating speed is 15～30 rev/mins, and the rotation rotating speed is 500～1000 rev/mins, continues to stir 10～30min, to revolve round the sun during this time and the rotation paddle on dry powder scrape in the agitator tank, after treating that each powder soaks into fully, be evacuated to-99kPa～-90kPa, adjusting the revolution rotating speed is 25～35 rev/mins, the rotation rotating speed is 1000～1500 rev/mins, stirs 120～240min.
3) utilize organic solvent to regulate the slurry viscosity at 3000-6000 mPas, after viscosity mixes up, only open the revolution vacuum and stir 30min slowly, use 150 order steel screen filtration dischargings.Later stage only opens the revolution vacuum and stirs slowly, prevents the slurry layering.
Wherein, before step 1), earlier anodal conductive agent, positive active material and high polymer binder are contained in respectively in the pallet, are put in the baking oven 100～150 ℃ of bakings 1～5 hour, guarantee that its powder is in drying regime, makes dry powder blend more abundant.
Wherein, described solvent has deionized water, and described organic solvent is the N-methyl pyrrolidone.
Wherein, the slurry of described positive pole is made up of the material of following weight ratio: positive active material: anodal conductive agent: high polymer binder: N-methyl pyrrolidone=100:0.05～15:0.2～10:60～160.
Wherein, the slurry of described negative pole is made up of the material of following weight ratio: negative electrode active material: cathode conductive agent: anti-settling dispersant: water-base cement: deionized water: N-methyl pyrrolidone=100:0.05-10:0.05-8:0.3-10:100-200:0.5-10.
Wherein, described anodal conductive agent comprises any or several mixture wherein in conductive carbon black, electrically conductive graphite, carbon fiber and the carbon nano-tube, described positive active material is any or several mixture wherein in the lithium intercalation compounds such as cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate and LiFePO4, and described high polymer binder is polyvinylidene fluoride.
Cobalt acid lithium has the following advantages as positive electrode:
1. operating voltage height;
2. charging/discharging voltage is steady;
3. be fit to high current charge-discharge;
4. specific energy height;
5. conductivity height;
6. production technology is simple.
Nickle cobalt lithium manganate has the following advantages as positive electrode:
1, energy density height;
2. operating voltage range is wide, can be in the 2.5-4.5V voltage range stable circulation;
3. good cycle under normal temperature and the high temperature;
4. Heat stability is good;
5. the crystal structure ideal that has extended cycle life, self discharge is little.
LiFePO4 has the following advantages as positive electrode:
1. environmental protection does not contain any harmful heavy metal element;
2. cycle performance is long, under the 100%DOD condition, discharges and recharges more than 2000 times capability retention more than 80%;
3. high-temperature stability is good, and security performance is good;
4. aboundresources.
LiMn2O4 has the following advantages as positive electrode:
1. aboundresources;
2. low price;
3. safe;
4. operating voltage height;
5. preparation is simple.
Carbon fiber powder be with the high-strength high-modules carbon fibre long filament through special technique surface treatment, grinding,
Behind micro-examination, screening, the hyperthermia drying and obtain etc. the elongated cylindrical particulate, it has kept numerous premium properties of carbon fiber, and shape is tiny, the surface is pure, specific area is big, be easy to by resin wetted by dispersion, and be the composite material filler of function admirable.Can carry out compound with materials such as resin, plastics, metal, rubber, with the intensity that increases material and wear-resisting, ni-mh, NI-G and lithium ion battery plus-negative plate material conductive additive, electronic chip, conductive plate, electrically-conducting floor, electric mechanical, antistatic industry (coating, terrace, paint, printing ink), antistatic filter core, defence and military, building heat preservation have been widely used in, chemical industry food is slightly imitated fields such as filtration, noise eliminator of motorcycle, the air filtration of paint drying room, polytetrafluoroethylene.
Carbon nano-tube is a kind of One-dimensional Quantum material with special construction (radial dimension is nanometer scale, and axial dimension can reach micron dimension), has typical stratiform hollow structure feature, and the two ends of general pipe have end cap to seal.The pipe shaft of carbon nano-tube is the director circle tubular construction, is made up of hexagonal carbon ring structure unit, and terminal cap moiety is the polygonized structure that contains pentagon and hexagonal carbocyclic ring composition.Carbon nano-tube can have only one deck also multilayer can be arranged, and is called single-layer carbon nano-tube and multilayer carbon nanotube, and its diameter is generally 2～20nm, and the spacing between the synusia of formation carbon nano-tube is about 0.34nm.Carbon nano-tube has excellent conducting performance, because the structure of carbon nano-tube is identical with the lamellar structure of graphite, so have good electric property.
As preferred embodiment, anodal conductive agent is the mixture of electrically conductive graphite and conductive carbon black, electrically conductive graphite is the important component that plays electric action in the positive electrode, its conductive capability has determined the discharge performance of lithium ion battery, the particle of electrically conductive graphite is bigger, the composition conductive path that is superimposed together, lithium ion be mobile discharge in conductive path.Conductive carbon black is nano level fine-grained particles, can be filled in the slit between the electrically conductive graphite, strengthens conductive capability, improves the electrical property of lithium ion battery.
Beneficial effect of the present invention: lithium ion battery plus-negative plate slurry preparation method of the present invention, at first the material with all powderies carries out premix earlier, again with liquid solvent, reduce step, the shutdown of needs when saving adds material, reinforced, operating time such as start again, compare the traditional handicraft mixing time and shorten half, therefore can save power cost and enhance productivity; The present invention can make each mixing of materials more abundant, stock quality is stable, be difficult for layering, simple for process, with short production cycle, dispersion effect is good and integrated cost is low, lithium ion battery cell multiplying power, circulation and the high-temperature storage performance of utilizing the preparation technology of anode and cathode slurry of the present invention to prepare are good.
Description of drawings
Utilize accompanying drawing that invention is described further, but the embodiment in the accompanying drawing does not constitute any limitation of the invention, for those of ordinary skill in the art, under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to the following drawings.
Fig. 1 is the stirring technique flow chart of traditional lithium ion battery anode glue size;
Fig. 2 is the stirring technique flow chart of traditional lithium ion battery cathode slurry;
Fig. 3 is the stirring technique flow chart of anode sizing agent of the present invention;
Fig. 4 is the stirring technique flow chart of cathode size of the present invention;
The cyclic curve figure of the electric core 5C charging 10C discharge that Fig. 5 makes for Comparative Examples and embodiment.
Embodiment
With the following Examples the present invention is further described.
Embodiment 1:
As shown in Figure 3, anodal stirring technique: polyvinylidene fluoride, conductive carbon black, electrically conductive graphite and nickel-cobalt-manganese ternary material are contained in respectively in the pallet, are put in the baking oven in 120 ℃ of baking coolings after 2 hours down.To toast 2 hours cooled 210g polyvinylidene fluoride down in 120 ℃ successively, the 210g conductive carbon black, 90g electrically conductive graphite and 5.5kg nickel-cobalt-manganese ternary material, be put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, after adding the N-methyl pyrrolidone of 4.5kg, revolution and rotation mixing speed are constant, continue to stir slowly 30min, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 33 rev/mins, 210min is stirred in 1300 rev/mins of rotations.The slurry viscosity gets final product at 3000-6000 mPas, before the discharging, after only opening revolution vacuum stirring 30min slowly, uses 150 purpose steel screen filtration dischargings.
As shown in Figure 4, negative pole stirring technique: successively with the 79g sodium carboxymethylcellulose, 158g conductive carbon black and 3.6kg Delanium are put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, the deionized water that adds 6.1kg, revolution and rotation mixing speed are constant, do not open vacuum and stir 30min slowly, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 30 rev/mins, 1200 rev/mins of rotations are behind the stirring 210min, once add SBR emulsion 204g, revolve round the sun 20 rev/mins, 600 rev/mins of rotations are stirred slowly and are adjusted rotating speed behind the 10min to revolving round the sun 30 rev/mins, 1200 rev/mins of rotations, stir 60min, add 150g N-methyl pyrrolidone, adjust rotating speed to revolving round the sun 20 rev/mins, 600 rev/mins of rotations, slowly survey the slurry viscosity after mixing 30min, viscosity is adjusted to 1500-4500 mPas and gets final product, before the discharging, after only opening revolution vacuum stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
Embodiment 2:
As shown in Figure 3, anodal stirring technique: polyvinylidene fluoride, conductive carbon black, electrically conductive graphite and nickel-cobalt-manganese ternary material are contained in respectively in the pallet, are put in the baking oven in 120 ℃ of baking coolings after 2 hours down.Successively with the 178g polyvinylidene fluoride, the 208g conductive carbon black, 59g electrically conductive graphite and 5.5kg nickel-cobalt-manganese ternary material, be put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, after adding the N-methyl pyrrolidone of 4.2kg, revolution and rotation mixing speed are constant, continue to stir slowly 30min, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 33 rev/mins, 210min is stirred in 1300 rev/mins of rotations.The slurry viscosity gets final product at 3000-6000 mPas, before the discharging, after only opening revolution vacuum stirring 30min slowly, uses 150 purpose steel screen filtration dischargings.
As shown in Figure 4, negative pole stirring technique: successively with the 70g sodium carboxymethylcellulose, 116g conductive carbon black and 3.6kg Delanium are put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, the deionized water that adds 5.8kg, revolution and rotation mixing speed are constant, do not open vacuum and stir 30min slowly, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 30 rev/mins, 1200 rev/mins of rotations are behind the stirring 210min, once add SBR emulsion 178g, revolve round the sun 20 rev/mins, 600 rev/mins of rotations are stirred slowly and are adjusted rotating speed behind the 10min to revolving round the sun 30 rev/mins, 1200 rev/mins of rotations, stir 60min, add 150g N-methyl pyrrolidone, adjust rotating speed to revolving round the sun 20 rev/mins, 600 rev/mins of rotations, slowly survey the slurry viscosity after mixing 30min, viscosity is adjusted to 1500-4500 mPas and gets final product, before the discharging, after only opening revolution vacuum stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
Embodiment 3:
As shown in Figure 3, anodal stirring technique: polyvinylidene fluoride, conductive carbon black, electrically conductive graphite and nickel-cobalt-manganese ternary material are contained in respectively in the pallet, are put in the baking oven in 120 ℃ of baking coolings after 2 hours down.Successively with the 147g polyvinylidene fluoride, the 176g conductive carbon black, 59g electrically conductive graphite and 5.5kg nickel-cobalt-manganese ternary material, be put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, after adding the N-methyl pyrrolidone of 3.8kg, revolution and rotation mixing speed are constant, continue to stir slowly 30min, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 33 rev/mins, 210min is stirred in 1300 rev/mins of rotations.The slurry viscosity gets final product at 3000-6000 mPas, before the discharging, after only opening revolution vacuum stirring 30min slowly, uses 150 purpose steel screen filtration dischargings.
As shown in Figure 4, negative pole stirring technique: successively with the 57g sodium carboxymethylcellulose, 96g conductive carbon black and 3.6kg Delanium are put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, the deionized water that adds 5.4kg, revolution and rotation mixing speed are constant, do not open vacuum and stir 30min slowly, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 30 rev/mins, 1200 rev/mins of rotations are behind the stirring 210min, once add SBR emulsion 154g, revolve round the sun 20 rev/mins, 600 rev/mins of rotations are stirred slowly and are adjusted rotating speed behind the 10min to revolving round the sun 30 rev/mins, 1200 rev/mins of rotations, stir 60min, add 150g N-methyl pyrrolidone, adjust rotating speed to revolving round the sun 20 rev/mins, 600 rev/mins of rotations, slowly survey the slurry viscosity after mixing 30min, viscosity is adjusted to 1500-4500 mPas and gets final product, before the discharging, after only opening revolution vacuum stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
Embodiment 4:
As shown in Figure 3, anodal stirring technique: polyvinylidene fluoride, conductive carbon black, electrically conductive graphite and nickel-cobalt-manganese ternary material are contained in respectively in the pallet, are put in the baking oven in 120 ℃ of baking coolings after 2 hours down.Successively with the 128g polyvinylidene fluoride, the 145g conductive carbon black, 29g electrically conductive graphite and 5.5kg nickel-cobalt-manganese ternary material, be put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, after adding the N-methyl pyrrolidone of 3.5kg, revolution and rotation mixing speed are constant, continue to stir slowly 30min, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 33 rev/mins, 210min is stirred in 1300 rev/mins of rotations.The slurry viscosity gets final product at 3000-6000 mPas, before the discharging, after only opening revolution vacuum stirring 30min slowly, uses 150 purpose steel screen filtration dischargings.
As shown in Figure 4, negative pole stirring technique: successively with 50 sodium carboxymethylcellulose pyces, 76g conductive carbon black and 3.6kg Delanium are put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, the deionized water that adds 5.1kg, revolution and rotation mixing speed are constant, do not open vacuum and stir 30min slowly, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 30 rev/mins, 1200 rev/mins of rotations are behind the stirring 210min, once add SBR emulsion 137g, revolve round the sun 20 rev/mins, 600 rev/mins of rotations are stirred slowly and are adjusted rotating speed behind the 10min to revolving round the sun 30 rev/mins, 1200 rev/mins of rotations, stir 60min, add 150g N-methyl pyrrolidone, adjust rotating speed to revolving round the sun 20 rev/mins, 600 rev/mins of rotations, slowly survey the slurry viscosity after mixing 30min, viscosity is adjusted to 1500-4500 mPas and gets final product, before the discharging, after only opening revolution vacuum stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
Embodiment 5:
As shown in Figure 3, anodal stirring technique: polyvinylidene fluoride, conductive carbon black, electrically conductive graphite and nickel-cobalt-manganese ternary material are contained in respectively in the pallet, are put in the baking oven in 120 ℃ of baking coolings after 2 hours down.Successively with the 103g polyvinylidene fluoride, the 115g conductive carbon black, 29g electrically conductive graphite and 5.5kg nickel-cobalt-manganese ternary material, be put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, after adding the N-methyl pyrrolidone of 3.3kg, revolution and rotation mixing speed are constant, continue to stir slowly 30min, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 33 rev/mins, 210min is stirred in 1300 rev/mins of rotations.The slurry viscosity gets final product at 3000-6000 mPas, before the discharging, after only opening revolution vacuum stirring 30min slowly, uses 150 purpose steel screen filtration dischargings.
As shown in Figure 4, negative pole stirring technique: successively with the 38g sodium carboxymethylcellulose, 56g conductive carbon black and 3.6kg Delanium are put in the agitator tank of 10L, do not open vacuum and stir 30min slowly, revolve round the sun 20 rev/mins, 600 rev/mins of rotations, after treating that each powder mixes, the deionized water that adds 4.8kg, revolution and rotation mixing speed are constant, do not open vacuum and stir 30min slowly, need during this time the dry powder on revolution and the rotation paddle is scraped in the agitator tank, after confirming that each powder soaks into fully, be evacuated to-90kPa, revolve round the sun 30 rev/mins, 1200 rev/mins of rotations are behind the stirring 210min, once add SBR emulsion 112g, revolve round the sun 20 rev/mins, 600 rev/mins of rotations are stirred slowly and are adjusted rotating speed behind the 10min to revolving round the sun 30 rev/mins, 1200 rev/mins of rotations, stir 60min, add 150g N-methyl pyrrolidone, adjust rotating speed to revolving round the sun 20 rev/mins, 600 rev/mins of rotations, slowly survey the slurry viscosity after mixing 30min, viscosity is adjusted to 1500-4500 mPas and gets final product, before the discharging, after only opening revolution vacuum stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
Comparative Examples 1:
Anodal stirring technique: polyvinylidene fluoride, conductive carbon black, electrically conductive graphite and nickel-cobalt-manganese ternary material are contained in respectively in the pallet, are put in the baking oven in 120 ℃ of baking coolings after 2 hours down.The 147g polyvinylidene fluoride is put in the agitator tank of 10L, adds the N-methyl pyrrolidone of 3.8kg, do not open vacuum and stir slowly, treat that polyvinylidene fluoride soaks into fully after, be evacuated to-90kPa, revolve round the sun 30 rev/mins 800 rev/mins of rotations, stirring 360min.59g electrically conductive graphite and 176g conductive carbon black are added in the agitator tank, revolve round the sun 20 rev/mins, 10min is stirred in 500 rev/mins of rotations, treat that anodal conductive agent soaks into fully after, adjust rotating speed to revolving round the sun 33 rev/mins, 1300 rev/mins of rotations, stirring 120min.Add 5.5kg nickel-cobalt-manganese ternary material in the agitator tank at twice, each 50% of total amount that adds, need stir 10min slowly after each the feeding in raw material, revolve round the sun 20 rev/mins, 500 rev/mins of rotations after the affirmation powder soaks into fully, are adjusted rotating speed to revolving round the sun 33 rev/mins, 180min is stirred in 1300 rev/mins of rotations.The slurry viscosity gets final product at 3000-6000 mPas, before the discharging, after only opening revolution vacuum stirring 30min slowly, uses 150 purpose steel screen filtration dischargings.
Negative pole stirring technique: the 57g sodium carboxymethylcellulose is put in the agitator tank of 10L, adds the deionized water of 5.4kg, do not open vacuum and stir slowly, after treating that sodium carboxymethylcellulose soaks into fully, be evacuated to-90kPa, revolve round the sun 30 rev/mins, 360min is stirred in 800 rev/mins of rotations.The 96g conductive carbon black is added in the agitator tank at twice, add 50% of total amount at every turn, revolve round the sun 20 rev/mins, 10min is stirred in 500 rev/mins of rotations, treat that conductive carbon black soaks into fully after, adjust rotating speed to revolving round the sun 30 rev/mins, 120min is stirred in 1200 rev/mins of rotations.3.6kg Delanium average mark is added for three times in the agitator tank, need stir 10min slowly after each the feeding in raw material, revolve round the sun 20 rev/mins, 500 rev/mins of rotations after the affirmation powder soaks into fully, are adjusted rotating speed to revolving round the sun 30 rev/mins, 180min is stirred in 1200 rev/mins of rotations.Once add SBR emulsion 154g, revolve round the sun 20 rev/mins, 600 rev/mins of rotations are stirred slowly and are adjusted rotating speed behind the 10min to revolving round the sun 30 rev/mins, 1200 rev/mins of rotations, stir 60min, add 150g N-methyl pyrrolidone, adjust rotating speed to revolving round the sun 20 rev/mins, 600 rev/mins of rotations, slowly survey the slurry viscosity after mixing 30min, viscosity gets final product for 1500-4500 mPas.Before the discharging, after only opening revolution vacuum stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
After anode and cathode slurry is ready to, produce electric core through following operation more respectively.Operation is as follows: put in storage after stirring pulping-coating-pair roller-itemize-welding rubberizing-coiling-survey short circuit-back welding-slot rolling-survey short circuit-baking-fluid injection-shelve-change into-shelve-partial volume-shelve-voltage internal resistance grouping, also can be by other operation preparations, its preparation method is as well known to those skilled in the art.
Test the comprehensive electrochemical of the electric core that different pulping process make.
1. high rate performance
1. the 1C constant current constant voltage is charged to 4.2V, by electric current 0.05C
2. shelve 5min
3. use 1C/5C/10C/15C/20C/25C/30C to be discharged to 2.75V respectively, shelve after the different multiplying discharge
Time unification is 20min.Table 1 is that the different high rate performance of embodiment under identical discharge system compares with table 2.
The electric core normal temperature of table 1 high rate performance contrast tabulation
| Electric current | Comparative Examples 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
|
|
100% | 100% | 100% | 100% | 100% | 100% |
| 5C | 95% | 96% | 96% | 97% | 95% | 94% |
| 10C | 98% | 99% | 99% | 101% | 99% | 97% |
| 15C | 99% | 100% | 100% | 101% | 100% | 98% |
| 20C | 98% | 99% | 100% | 101% | 98% | 96% |
| 25C | 96% | 98% | 99% | 102% | 90% | 77% |
| 30C | 93% | 94% | 95% | 98% | 82% | 50% |
The electric core normal temperature discharge of table 2 intermediate value voltage-contrast
| Electric current | Comparative Examples 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| 1C | 3.655 | 3.665 | 3.668 | 3.67 | 3.666 | 3.663 |
| 5C | 3.541 | 3.558 | 3.56 | 3.572 | 3.563 | 3.559 |
| 10C | 3.441 | 3.452 | 3.458 | 3.465 | 3.456 | 3.451 |
| 15C | 3.350 | 3.371 | 3.376 | 3.385 | 3.374 | 3.372 |
| 20C | 3.264 | 3.291 | 3.294 | 3.301 | 3.294 | 3.287 |
| 25C | 3.181 | 3.21 | 3.214 | 3.221 | 3.172 | 3.151 |
| 30C | 3.087 | 3.108 | 3.116 | 3.127 | 3.056 | 3.02 |
By table 1 and table 2 as can be seen, both positive and negative polarity adopts different proportionings, and the consumption of conductive agent directly influence makes high rate performance and the discharge intermediate value voltage platform of electric core.The electric core multiplying power discharging capability retention maximum that wherein adopts embodiment 3 to make, the intermediate value voltage platform of discharge is the highest, and namely electric core has stronger power output.
2. 60 ℃ of 7 days high-temperature storage performances experiments
1. the 1C constant-current constant-voltage charging is to 4.2V, cut-off current 0.05C;
2. shelve 5min;
3. the 1C constant-current discharge is to 2.75V;
4. shelve 5min;
5. the 1C constant-current constant-voltage charging is to 4.2V, cut-off current 0.05C;
6. the baking oven of putting into temperature and be 60 ± 2 ℃ stores 7 days;
7. the battery normal temperature that will take out from baking oven was shelved 4 hours;
8. the 1C constant-current discharge is to 2.75V (residual capacity; )
9. shelve 5min;
10. the 1C constant-current constant-voltage charging is to 4.2V, cut-off current 0.05C;
Shelve 5min;
The 1C constant-current discharge is to 2.75V (recovery capacity).
The capability retention of electric core after high-temperature storage that table 3 embodiment and Comparative Examples make
| Different embodiment and Comparative Examples | The remaining rate of capacity | The capacity restoration rate |
| Comparative Examples 1 | 88% | 96% |
| Embodiment 1 | 91% | 98% |
| Embodiment 2 | 91% | 99% |
| Embodiment 3 | 92% | 99% |
| Embodiment 4 | 91% | 99% |
| Embodiment 5 | 91% | 98% |
As can be seen from Table 3, the electric core that employing embodiment makes is after 60 ℃ of storages in 7 days, and capability retention is higher than Comparative Examples, and the high-temperature storage performance is better.Wherein adopt electric core that embodiment 3 makes through 60 ℃ stored in 7 days after, the remaining rate of capacity is 92%, the capacity restoration rate is 99%.
3. cycle performance
Test adopts embodiment 3 and Comparative Examples to make the cycle performance of electric core respectively
1. the 5C constant current constant voltage is charged to 4.2V, by electric current 0.05C
2. shelve 30min
3. 10C is discharged to 2.75V
4. shelve 30min
5. circulate 600 times, initial work step is for 1.
As shown in Figure 5, the electric core that top curve representative adopts embodiment 3 to make, the electric core that following curve representative adopts the method for Comparative Examples to make, the cyclic curves of 5C charging 10 discharges of the electric core that employing embodiment 3 makes are more level and smooth, show thus, the charge-discharge performance that is prepared lithium ion battery by anode and cathode slurry of the present invention is more stable, and 600 times the circulation volume conservation rate can remain on more than 92%.
4. the dispersive property of cathode size
Use Hegman grind gage that the slurry of different embodiment and Comparative Examples is carried out the fineness grade test, judge that with the dispersion effect to this method the result is as shown in table 4.
Make with the following method the slurry to different embodiment and Comparative Examples carry out the solid content test:
Different slurries are respectively charged in the 100ml graduated cylinder, placing temperature is that 23 ℃, relative humidity are 45% climatic chamber, place after 24 hours and again 15mm place, graduated cylinder top layer slurry is carried out the solid content test, come stability of slurry is passed judgment on the situation of change of placing 24 hours front and back slurry solid contents, test result is as shown in table 4 below.
Table 4 slurry curing amount contrast table
| Different embodiment and Comparative Examples | The slurry numbering | Fineness/micron | Place solid content (%) before 24 hours | Place solid content (%) after 24 hours |
| Embodiment 1 | S1 | 30 | 38.9 | 38.5 |
| Embodiment 2 | S2 | 30 | 39.9 | 39.4 |
| Embodiment 3 | S3 | 35 | 41.3 | 40.9 |
| Embodiment 4 | S4 | 35 | 42.4 | 42.0 |
| Embodiment 5 | S5 | 35 | 43.8 | 43.3 |
| Comparative Examples 1 | D1 | 45 | 41.2 | 35.6 |
As can be seen from Table 4, the slurry fineness that is made by embodiment is little, shelve 24h under certain humiture after, the slurry solid content changes very little.
In sum, adopt anode and cathode slurry dispersion stabilization of the present invention good, the electric core high rate performance height that makes, good cycle, the high-temperature storage performance is good, and production efficiency is greatly improved, and mixing time shortens over half.
Should be noted that at last; above embodiment is only in order to illustrate technical scheme of the present invention; but not limiting the scope of the invention; although with reference to preferred embodiment the present invention has been done to explain; those of ordinary skill in the art is to be understood that; can make amendment or be equal to replacement technical scheme of the present invention, and not break away from essence and the scope of technical solution of the present invention.
Claims (10)
1. the preparation method of a lithium ion battery plus-negative plate slurry, it is characterized in that: cathode size comprises following preparation process:
Cathode conductive agent, negative electrode active material and the anti-settling dispersant of powdery are put into agitator tank successively to stir;
After treating that each powder in the steps A mixes, add solvent, continue to stir, each powder is soaked into fully;
Continue to stir after adding water-base cement in the agitator tank;
After treating that material among the step C stirs, regulate viscosity;
Wherein, anode sizing agent comprises following preparation process:
1) stirs in anodal conductive agent, positive active material and the high polymer binder adding agitator tank with powdery;
2) in agitator tank, add organic solvent then, stir, soak into fully until flour;
3) regulate viscosity.
2. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 1, it is characterized in that: described cathode size comprises following preparation process:
Earlier cathode conductive agent, negative electrode active material and the anti-settling dispersant of powdery are put into agitator tank successively, do not open vacuum, open revolution and rotation simultaneously and carry out dry powder stirring 15～90min, the rotating speed of revolution is 15～30 rev/mins, and the rotating speed of rotation is 500～1000 rev/mins;
After treating that each powder mixes in the steps A, in agitator tank, add solvent, setting the revolution rotating speed is 15～30 rev/mins, the rotation rotating speed is 500～1000 rev/mins, continue to stir 10～30min, to revolve round the sun during this time and the rotation paddle on dry powder scrape in the agitator tank, confirm that each powder soaks into fully;
Be evacuated to-99kPa～-90kPa, setting the revolution rotating speed is 25～35 rev/mins, the rotation rotating speed is 1000～1500 rev/mins, after stirring 120～240min, add water-base cement, setting the revolution rotating speed again is 15～25 rev/mins, the rotation rotating speed is 500～800 rev/mins, adjust rotating speed to revolving round the sun 20～35 rev/mins after stirring 5～15min, 40～90min is stirred in 1000～1500 rev/mins of rotations;
Add organic solvent, adjust rotating speed to revolving round the sun 15～25 rev/mins, 10～30min is stirred in 500～800 rev/mins of rotations, utilizes solvent adjustment slurry viscosity at 1500-4000 mPas.
3. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 2 is characterized in that: among the described step D, after viscosity mixes up, continue out the vacuum revolution and stir 10-30min for 10～30 rev/mins, cross 150 order steel sieve then and filter discharging.
4. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 1, it is characterized in that: cathode conductive agent comprises any or several mixture wherein in conductive carbon black, electrically conductive graphite, carbon fiber and the carbon nano-tube in the described steps A, described negative electrode active material comprises any or several mixture wherein in Delanium, native graphite, soft carbon and the hard carbon, described anti-settling dispersant is sodium carboxymethylcellulose, and water-base cement is SBR emulsion among the described step C.
5. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 1, it is characterized in that: anode sizing agent comprises following preparation process:
Anodal conductive agent, positive active material and the high polymer binder of powdery are put into agitator tank successively, do not open vacuum, open revolution and rotation simultaneously and carry out dry powder stirring 15～90min, the revolution rotating speed is 15～30 rev/mins, and the rotation rotating speed is 500～1000 rev/mins;
After treating that each powder mixes in the step 1), add organic solvent, setting the revolution rotating speed is 15～30 rev/mins, and the rotation rotating speed is 500～1000 rev/mins, continues to stir 10～30min, to revolve round the sun during this time and the rotation paddle on dry powder scrape in the agitator tank, after treating that each powder soaks into fully, be evacuated to-99kPa～-90kPa, adjusting the revolution rotating speed is 25～35 rev/mins, the rotation rotating speed is 1000～1500 rev/mins, stirs 120～240min;
Utilize organic solvent to regulate the slurry viscosity at 3000-6000 mPas, after only opening the revolution vacuum and stirring 30min slowly, use 150 purpose steel screen filtration dischargings.
6. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 1, it is characterized in that: the preparation process 1 of described anode sizing agent) before, earlier anodal conductive agent, positive active material and high polymer binder are contained in respectively in the pallet, are put in the baking oven 100～150 ℃ of bakings 1～5 hour.
7. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 1, it is characterized in that: anodal conductive agent comprises any or several mixture wherein in conductive carbon black, electrically conductive graphite, carbon fiber and the carbon nano-tube in the described step 1), described positive active material is any or several mixture wherein in cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate and the LiFePO4, and described high polymer binder is polyvinylidene fluoride.
8. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 1, it is characterized in that: described solvent is deionized water, described organic solvent is the N-methyl pyrrolidone.
9. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 8, it is characterized in that: the slurry of described positive pole is made up of the material of following weight ratio: positive active material: anodal conductive agent: high polymer binder: N-methyl pyrrolidone=100:0.05～15:0.2～10:60～160.
10. the preparation method of a kind of lithium ion battery plus-negative plate slurry according to claim 8, it is characterized in that: the slurry of described negative pole is made up of the material of following weight ratio: negative electrode active material: cathode conductive agent: anti-settling dispersant: water-base cement: deionized water: N-methyl pyrrolidone=100:0.05-10:0.05-8:0.3-10:100-200:0.5-10.
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