CN102329538B - Water-based conductive ink of a lithium-ion battery - Google Patents
Water-based conductive ink of a lithium-ion battery Download PDFInfo
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- CN102329538B CN102329538B CN2011100262602A CN201110026260A CN102329538B CN 102329538 B CN102329538 B CN 102329538B CN 2011100262602 A CN2011100262602 A CN 2011100262602A CN 201110026260 A CN201110026260 A CN 201110026260A CN 102329538 B CN102329538 B CN 102329538B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the technical field of a lithium-ion battery, in particular to water-based conductive ink of the lithium-ion battery. Dry materials mainly comprise (by weight percentage): 0.2-2 percent of water-soluble polymer thickener, 5-25 percent of water-based dispersant, 30-70 percent of conductive carbon black and 20-50 percent of non-polar high polymer water-based latex with the solubility parameter delta less than or equal to 18(J/cm3)1/2. The solvent adopts water and accounts for 60-90 percent of the total weight of the pulp. The adhesive properties of the adhesive can be enhanced, the adhesive also has the characteristics of water resistance, NMP (nuclear matrix protein) resistance and electrolyte resistance, a conductive network is formed on a current collector under the effect of the adhesive after adding the conductive carbon black, the contact area between the current collector and a film is increased, and the effect of reducing the contact resistance can be achieved. The current collector after printing of the water-based conductive ink is not only suitable for pulp coating of water-based systems, but also suitable for pulp coating of NMP systems. Moreover, the lithium-ion battery has lower internal resistance and longer cycle life.
Description
Technical field
The present invention relates to technical field of lithium ion, especially a kind of lithium ion battery use electrically conductive ink.
Background technology
Lithium ion battery is owing to having the advantages such as energy density is high, operating voltage is high, temperature limit is wide, have extended cycle life, and is widely used as the power supply of various mobile devices.In existing production technology, the battery core of lithium ion battery is generally to adopt active material first to be modulated into to take 1-METHYLPYRROLIDONE (NMP) be solvent, the oiliness slurry that Kynoar (PVDF) is bonding agent, perhaps take water as solvent; then the water paste that butadiene-styrene latex (SBR) is bonding agent; make the diaphragm slurry is coated on collector and makes pole piece.Positive active material has cobalt acid lithium, LiFePO4, LiMn2O4, nickel LiMn2O4 and other ternarys or polynary material, and negative electrode active material has graphite (electrographite and native graphite), petroleum coke, carbon fiber, pyrolytic carbon, mesophase pitch based carbon microsphere (MCMB), glass charcoal, CNT (carbon nano-tube) etc.The electrolyte of lithium ion battery is generally to take lithium hexafluoro phosphate as lithium salts, the organic bath that carbonic ester is solvent.All substances in positive and negative pole material comprise before bonding agent all it must being electrolyte resistance, are not dissolved in the organic carbonate ester solvent.
It is little that high performance lithium ion battery requires to possess internal resistance, have extended cycle life, large cell discharge performance excellence, but lithium ion battery in cyclic process, the internal resistance meeting increases, capacity attenuation.The internal resistance meeting increases, and the reason of circulating battery decay is more.It is generally acknowledged that it is a major reason that causes the cyclic process capacity to reduce that active material and collector are peeled off, and the method that increases at present the cementability between active material and collector probably there are three kinds.
The first is by punch to increase the cementability between active material and collector at collection liquid surface, but the collector of this punching can cause the surface of active material rete to be uneven, easily cause the inside lithium ion cell micro-short circuit to cause self discharge serious.
The second is that collector is carried out to surface treatment, the surface treatment method of the affluxion body in lithium ion batteries of openly inventing as patent CN00117142.9, the method is first carried out on Passivation Treatment 5-20 minute collector with the copper ammon solution of 1%-5%, with the dichromic acid aqueous solution of 5%-20% concentration, collector is carried out to further Passivation Treatment 1-5 minute again, finally on collector, apply the 0.5-1.5% coupling agent at 150 ℃ of dry 10-100 minute.The method complex procedures, and used the noxious substances such as dichromic acid water, can only produce effect by the anticathode copper foil of affluxion body.The method also has a shortcoming, and because coupling agent is non-conductive, this method must increase the contact resistance of active material rete and collector, affects performance of lithium ion battery.
The third is first on collector, to print one deck active material slurry, applies active material slurry after oven dry again, is equal to twice coating.Because all contain active material in two coatings, so active material must be the same, be unfavorable for the switching of different formulations, increase operation, and for the DeGrain that strengthens the bonding of collector and reduction internal resistance.Also some is first to print the slurry that there is no active material, but this kind of coating is can not be water-fast or be ability NMP not, and the working procedure of coating that can't take into account aqueous systems slurry and NMP system slurry is complicated.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, and provide a kind of lithium ion battery use electrically conductive ink, it is printed on positive pole or negative current collector, operation is simple, the adhesive property of enhanced activity material rete and collector significantly, reduce the internal resistance of cell and extend battery cycle life, and this water-soluble conducting ink bonding agent used is nonpolar and solubility parameters<18 (J/cm
3)
1/2high molecular polymer, make this printed layers be not dissolved in water, NMP, carbonic ester isopolarity solvent, the collector after printing is not only applicable to the slurry coating of water-based system, is applicable to the slurry coating of NMP system yet, there is good versatility, greatly enhance productivity.
To achieve these goals, the technical solution used in the present invention is:
A kind of lithium ion battery use electrically conductive ink, siccative mainly contains by weight percentage:
Water soluble polymer thickener 0.2～2%,
Aqueous dispersion 5～25%,
Conductive carbon black 30～70%,
Water based emulsion 20～50%,
Described water based emulsion is nonpolar and solubility parameters δ≤18 (J/cm
3)
1/2high molecular polymer,
Solvent for use is water, and the content of solvent accounts for the 60-90% of slurry gross weight.
With respect to prior art, the water soluble polymer thickener and the aqueous dispersion that in the present invention, add, the interface that can improve active material rete and collector, play the effect of auxiliary bonding, added and had nonpolar and solubility parameters δ≤18 (J/cm
3)
1/2the water based emulsion of high molecular polymer, as main bonding agent, according to rule of similarity, this type of water based emulsion is non-polar polymer, is not dissolved in water, NMP, carbonic ester isopolarity solvent; According to this solubility parameters δ of solubility parameters phase approximately principle≤18 (J/cm
3)
1/2the solubility parameters of polymer and water, NMP, carbonic ester equal solvent is made poor absolute value all much larger than 2, so it both had been not dissolved in water (δ ≈ 47.3 (J/cm3)
1/2), also be not dissolved in NMP (δ ≈ 11.3 (J/cm3)
1/2), carbonic ester (δ ≈ 29 (J/cm3)
1/2) the isopolarity solvent, this bonding agent can strengthen adhesive property, the characteristic that there is again water-fast anti-NMP, electrolyte resistance, add conductive carbon black to form conductive network under the effect of bonding agent on collector, and the contact area of increase collector and diaphragm, play the effect that reduces contact resistance, so the collector after this water-soluble conducting ink printing is not only applicable to the slurry coating of water-based system, also be applicable to the slurry coating of NMP system, and make lithium ion battery there is low internal resistance, higher cycle life.
Collector after printing is not only applicable to the slurry coating of water-based system, is applicable to the slurry coating of NMP system yet, has good versatility, greatly enhances productivity.
A kind of lithium ion battery use electrically conductive ink, further preferably, siccative mainly contains by weight percentage:
Water soluble polymer thickener 0.2～1%,
Aqueous dispersion 5～10%,
Conductive carbon black 45～65%,
Water based emulsion 30～45%,
Described water based emulsion is nonpolar and solubility parameters δ≤17 (J/cm
3)
1/2high molecular polymer.
A kind of lithium ion battery use electrically conductive ink, further preferably, siccative mainly contains by weight percentage:
Water soluble polymer thickener 0.2%,
Aqueous dispersion 9.8%,
Conductive carbon black 50%,
Water based emulsion 40%,
Described water based emulsion is nonpolar and solubility parameters δ is 17 (J/cm
3)
1/2high molecular polymer.
Wherein, limitation of the invention further, described water based emulsion is PTFE emulsion (PTFE, δ ≈ 12.7 (J/cm
3)
1/2), butadiene-styrene latex (SBR, δ ≈ 16.6 (J/cm
3)
1/2), polyethylene latex (PE, δ ≈ 16.5 (J/cm3)
1/2) in one or more, water based emulsion of the present invention does not limit above several, can also be the polybutadiene latex, polyethylene propylene latex, Polybutadiene Acrylonitrile latex, styrene-acrylic latex etc.
Wherein, limitation of the invention further, described water soluble polymer thickener is one or more in hydroxyethylcellulose, sodium carboxymethylcellulose (CMC-Na), polyacrylamide (PAM).
Wherein, limitation of the invention further, aqueous dispersion can be polyacrylic acid (PAA) or polyacrylate (PAE), or their mixture.
Wherein, limitation of the invention further, conductive carbon black is acetylene carbon black (SP), one or more in conduction charcoal fiber (CNT), electrically conductive graphite.
Described a kind of lithium ion battery use electrically conductive ink makes by following steps:
A, fill a prescription by weight percentage water and water soluble polymer thickener and aqueous dispersion are first joined in mixer grinder by siccative, dissolve complete.
B, by siccative, fill a prescription by weight percentage conductive carbon black is added in the solution of steps A, it is below 5 μ m that rapid stirring is ground to particle diameter.
C, add water based emulsion by formula again, low rate mixing evenly after, filter and make required printing ink.
A kind of lithium ion battery use electrically conductive ink, on collector, be prepared into electrodes of lithium-ion batteries by press printing.
Described collector is aluminium foil, Copper Foil, aluminium net, copper mesh, nickel sheet or stainless steel substrates.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment 1:
The preparation of water-soluble conducting ink:
The water-soluble conducting ink slurry is pressed the siccative weight percent meter, 0.2% sodium carboxymethylcellulose (CMC-Na) as water soluble polymer thickener, 9.8% polyacrylic acid (PAA) as aqueous dispersion, 50% butadiene-styrene latex (SBR) as water based emulsion, its solubility parameters is 17 (J/cm3)
1/2, 40% acetylene carbon black (SP) is as conductive carbon black, solvent is water, water accounts for 85% of total slurry.At first press above formula by water, sodium carboxymethylcellulose, polyacrylic acid, join in mixer grinder, dissolve complete under vacuum state, by formula, conductive carbon black is added and has in the aqueous high molecular solution dissolved again, it is below 5 μ m that rapid stirring is ground to particle diameter, finally by formula, adds butadiene-styrene latex, and the vacuum low rate mixing is evenly (for preventing the butadiene-styrene latex breakdown of emulsion, can not rapid stirring), make required printing ink slurry with 200 order stainless steel sift net filtrations.
The preparation of positive collector:
The plus plate current-collecting body body is selected the aluminium foil that 16um is thick, by the water-soluble conducting ink prepared, be printed on equably the aluminium foil two sides with intaglio press, print speed printing speed is 5m/min, and bake out temperature is under 80～110 ℃, the printing aluminium foil that the layer thickness that obtains being printed on one side is 3um, its rough surface is network-like, conductive carbon forms good conductive network, can not only strengthen bondingly also can reduce contact resistance, and the printed layers after printing both had been not dissolved in water and also has been not dissolved in NMP, carbonic ester electrolyte.
The making of anode pole piece:
The anodal LiFePO4 (LiFePO4) that uses is as active material.The anode sizing agent that contains this active material according to the formula modulation, the solid constituent of this slurry comprises this positive active material of 90%, and 5% PVDF (Kynoar) is as bonding agent, and 5% conductive carbon is as the conductivity auxiliary agent.This slurry is used NMP as solvent, and the solids content of slurry is 40%.This slurry is coated in equably to the aluminium foil two sides of having handled well, then with roll squeezer by the pole piece compacting, obtain the oiliness anode pole piece.
The making of cathode pole piece:
Negative pole is used Delanium as active material.The anode sizing agent that contains this active material according to the formula modulation, the solid constituent of this slurry comprises this negative electrode active material of 95%, 1.5% sodium carboxymethylcellulose, 1.5% conductive carbon black is as the conductivity auxiliary agent, and 2% butadiene-styrene latex is as bonding agent.This slurry makes water as solvent, and the solids content of slurry is 50%.This slurry is coated in equably to the aluminium foil two sides of having handled well, then with roll squeezer by the pole piece compacting, obtain the aqueous positive-pole pole piece.
The assembling of battery:
Welding conduction lug on anodal and cathode pole piece, make anodal and negative pole centre accompany the PP/PE composite isolated film of 20um and overlapping, be wound into cubic shape, use again in the aluminum plastic film packaging bag, inject nonaqueous electrolytic solution, the LiPF6 solution that the electrolyte of battery is 1mol/L, primary solvent is mixed by EC, PC, DMC, after encapsulation, battery is changed into and burn-in test, obtaining length and width thick is the square flexible-packed battery of 109mm * 101mm * 3mm.
Embodiment 2
Difference from Example 1 is: the water-soluble conducting ink slurry is pressed the siccative weight percent meter, 0.2% hydroxyethylcellulose and 0.8% sodium carboxymethylcellulose (CMC-Na) are as the water soluble polymer thickener, 5% polyacrylic acid (PAA) as aqueous dispersion, 45% butadiene-styrene latex (SBR) as water based emulsion, 49% conductive carbon fibre as conductive carbon black, solvent is water, and water accounts for 75% of total slurry weight.In addition, other is identical with embodiment 1, repeats no more here.
Embodiment 3
Difference from Example 1 is: the water-soluble conducting ink slurry is pressed the siccative weight percent meter, 2% sodium carboxymethylcellulose (CMC-Na) is as the water soluble polymer thickener, 22.5% polyacrylic acid (PAA) and 0.5% polyacrylate (PAE) as aqueous dispersion, 30% butadiene-styrene latex (SBR) and 10% polyethylene latex (PE) as water based emulsion, 30% acetylene carbon black and 5% conductive carbon fibre as conductive carbon black, solvent is water, and water accounts for 85% of total slurry weight.In addition, other is identical with embodiment 1, repeats no more here.
Embodiment 4
Difference from Example 1 is: the water-soluble conducting ink slurry is pressed the siccative weight percent meter, 0.5% sodium carboxymethylcellulose (CMC-Na) is as the water soluble polymer thickener, 19.5% polyacrylic acid (PAA) is conductive carbon black as aqueous dispersion, 30% polyethylene latex (PE) as water based emulsion, 50% acetylene carbon black, solvent is water, and water accounts for 85% of total slurry weight.In addition, other is identical with embodiment 1, repeats no more here.
Embodiment 5
Difference from Example 4 is: the making of anode pole piece is to take the water paste that water is solvent, the solids content of slurry is 40%, the solid constituent of this slurry comprises 90% LiFePO4 (LiFePO4) positive active material, 1% sodium carboxymethylcellulose is as thickener, 5% acetylene carbon black is as conductive carbon black, 4% aqueous adhesive.In addition, other is identical with embodiment 4, repeats no more here.
Embodiment 6
Difference from Example 1 is: the water-soluble conducting ink slurry is pressed the siccative weight percent meter, by 2% hydroxyethylcellulose, 5% polyacrylate (PAE), 28% polyethylene latex (PE), 65%, formed, solvent is water, and water accounts for 60% of total slurry weight.In addition, other is identical with embodiment 1, repeats no more here.
Embodiment 7
Difference from Example 1 is: the negative current collector body is selected the Copper Foil that 12um is thick, by the water-soluble conducting ink prepared, be printed on equably the Copper Foil two sides with intaglio press, print speed printing speed is 5m/min, bake out temperature is under 80～110 ℃, the printing aluminium foil that the layer thickness that obtains being printed on one side is 3um, its rough surface is network-like, conductive carbon forms good conductive network, can not only strengthen and bondingly also can reduce contact resistance, the printed layers after printing both had been not dissolved in water and also had been not dissolved in NMP, carbonic ester electrolyte.In addition, other is identical with embodiment 1, repeats no more here.
Comparative Examples 1
Difference from Example 1 is: do not have the use electrically conductive ink to process collector, other is identical with embodiment 1, repeats no more here.
Diaphragm and battery that above 6 embodiment and 1 Comparative Examples are prepared are tested, and obtain following result:
The anode pole piece that above-described embodiment is done carries out adhesive property test and resistance test, the results are shown in following table:
Table 1 anode pole piece adhesive property and resistance test data
Carry out adhesive property and resistance test data (as shown in table 1) by anode pole piece and can illustrate that the collector of having used after water-soluble conducting ink printing of the present invention can be used for water-based and the oiliness anode pole piece of preparation, the water-based obtained and oiliness anode pole piece are compared with Comparative Examples, there is bonding force strong, and the characteristics such as membrane resistance is little.
The full battery that above-described embodiment is done carries out internal resistance, capacity, power density test comparison, the results are shown in following table:
The full internal resistance of cell of table 2, capacity, power density test data
Can illustrate that by the full internal resistance of cell, capacity, power density test data (as shown in table 2) water-based of having used the collector after water-soluble conducting ink printing of the present invention to prepare and the full battery of oiliness positive pole compare with Comparative Examples, internal resistance obviously reduces, power density is greatly improved, if both positive and negative polarity is all used water-soluble conducting ink to process collector, effect can be better.
Comprehensive upper data, can show that water-soluble conducting ink of the present invention can strengthen the adhesive property of collector and active material rete really, reduces the effect of contact resistance.Collector after this water-soluble conducting ink printing is not only applicable to the slurry coating of water-based system, is applicable to the slurry coating of NMP system yet, and the lithium ion battery of manufacture has low internal resistance, high power density, the long characteristics such as cycle life.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also carry out suitable change and modification to above-mentioned execution mode.Therefore, the present invention is not limited to embodiment disclosed and described above, to modifications and changes more of the present invention, also should fall in the protection range of claim of the present invention.In addition, although used some specific terms in this specification, these terms just for convenience of description, do not form any restriction to the present invention.
Claims (9)
1. a lithium ion battery use electrically conductive ink, it is characterized in that: siccative mainly contains by weight percentage:
Described water based emulsion is nonpolar and solubility parameters δ≤18 (J/cm
3)
1/2high molecular polymer, solvent for use is water, the content of solvent accounts for 60～90% of slurry gross weight; Described water based emulsion is PTFE emulsion, δ ≈ 12.7 (J/cm
3)
1/2, butadiene-styrene latex, δ ≈ 16.6J/cm
3)
1/2, the polyethylene latex, δ ≈ 17 (J/cm
3)
1/2in one or more.
2. a kind of lithium ion battery use electrically conductive ink according to claim 1, it is characterized in that: siccative mainly contains by weight percentage:
Described water based emulsion is nonpolar and solubility parameters δ≤17 (J/cm
3)
1/2high molecular polymer.
3. a kind of lithium ion battery use electrically conductive ink according to claim 2, it is characterized in that: siccative mainly contains by weight percentage:
Described water based emulsion is nonpolar and solubility parameters δ is 17 (J/cm
3)
1/2high molecular polymer.
4. according to the described a kind of lithium ion battery use electrically conductive ink of claim 1-3 any one, it is characterized in that: described water soluble polymer thickener is hydroxyethylcellulose, sodium carboxymethylcellulose, one or more in polyacrylamide.
5. according to the described a kind of lithium ion battery use electrically conductive ink of claim 1-3 any one, it is characterized in that: aqueous dispersion is polyacrylic acid or polyacrylate, or their mixture.
6. according to the described a kind of lithium ion battery use electrically conductive ink of claim 1-3 any one, it is characterized in that: conductive carbon black is acetylene carbon black, one or more in conduction charcoal fiber, electrically conductive graphite.
7. according to the described a kind of lithium ion battery use electrically conductive ink of claim 1-3 any one, it is characterized in that: by following steps, make:
A, fill a prescription by weight percentage water and water soluble polymer thickener and aqueous dispersion are first joined in mixer grinder by siccative, dissolve complete;
B, by siccative, fill a prescription by weight percentage conductive carbon black is added in the solution of steps A, it is below 5 μ m that rapid stirring is ground to particle diameter;
C, add water based emulsion by formula again, low rate mixing evenly after, filter and make required printing ink.
8. a kind of lithium ion battery use electrically conductive ink according to claim 7, is characterized in that: by press printing, on collector, be prepared into electrodes of lithium-ion batteries.
9. a kind of lithium ion battery use electrically conductive ink according to claim 8, it is characterized in that: described collector is aluminium foil, Copper Foil, aluminium net, copper mesh, nickel sheet or stainless steel substrates.
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| CN2011100262602A CN102329538B (en) | 2011-01-25 | 2011-01-25 | Water-based conductive ink of a lithium-ion battery |
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| CN103102717B (en) * | 2012-12-18 | 2015-06-03 | 东莞市易威科电子科技有限公司 | Water-based ceramic coating for lithium ion battery and application thereof |
| CN103073953A (en) * | 2013-02-07 | 2013-05-01 | 苏州牛剑新材料有限公司 | Waterborne conductive ink and preparation method thereof |
| CN103450737B (en) * | 2013-08-30 | 2015-07-15 | 深圳市凯力诚实业发展有限公司 | Printing ink as well asand preparation method and application thereof |
| CN104130625A (en) * | 2014-08-14 | 2014-11-05 | 朱寰 | Conductive ink |
| CN104821403A (en) * | 2015-03-17 | 2015-08-05 | 江苏乐能电池股份有限公司 | Preparation method for lithium ion battery |
| CN105024082A (en) * | 2015-06-19 | 2015-11-04 | 东莞市翔丰华电池材料有限公司 | Water-based conductive ink for lithium ion battery and preparation method thereof |
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| JP7021641B2 (en) * | 2016-12-02 | 2022-02-17 | 日産化学株式会社 | Method for manufacturing thin film containing conductive carbon material |
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| KR102555665B1 (en) | 2017-11-03 | 2023-07-14 | 체에스에엠 센트레 스위쎄 데 엘렉트로니크 에트 데 미크로테크니크 에스아-르쉐르슈 에트 데블로프망 | Foldable flexible cell assembly for lithium-ion battery and current collector with carbon-based conductive material |
| CN110341261A (en) * | 2019-07-09 | 2019-10-18 | 惠州市广麟材耀科技有限公司 | A kind of lithium battery aluminum-plastic film and preparation method thereof of surface coloring |
| CN112409858B (en) * | 2020-11-10 | 2022-06-07 | 横店集团东磁股份有限公司 | Conductive coating for battery case, preparation method and application thereof |
| CN113921895A (en) * | 2021-09-29 | 2022-01-11 | 东方电气集团科学技术研究院有限公司 | Lithium iron phosphate battery and preparation method thereof |
| CN115588748B (en) * | 2022-12-07 | 2023-04-11 | 四川启睿克科技有限公司 | Battery and circuit board integrated device and preparation method thereof |
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