CN102368543A - Lithium ion battery cathode and lithium ion battery therewith - Google Patents
Lithium ion battery cathode and lithium ion battery therewith Download PDFInfo
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- CN102368543A CN102368543A CN2011103389944A CN201110338994A CN102368543A CN 102368543 A CN102368543 A CN 102368543A CN 2011103389944 A CN2011103389944 A CN 2011103389944A CN 201110338994 A CN201110338994 A CN 201110338994A CN 102368543 A CN102368543 A CN 102368543A
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Abstract
The invention belongs to the field of lithium ion battery materials, and provides a lithium ion battery cathode comprising a current collector and a cathode material coated on eth current collector. The cathode material comprises a carbon material or an alloy material. An adopted binder is carboxymethylcellulose sodium. The carboxymethylcellulose sodium has a substitution degree of 0.6 to 1.2, and a number-average molecular weight of 50 thousands to 1 million. The viscosity of a 1% aqueous solution of carboxymethylcellulose sodium under a temperature of 25 DEG C is 50-1200mPa*s. The mass percentage of carboxymethylcellulose sodium in the cathode material is 1% to 5%. With a lithium ion battery employing the cathode, a defect of over-expended thickness during a battery circulation process is solved. Also, the produced battery is safe, reliable, and has a long circulation life.
Description
Technical field
The invention belongs to the lithium ion battery material field, more specifically relate to a kind of composition and method of having improved the lithium ion battery of performance.
Background technology
Lithium ion battery is since commercialization, because its energy density is high, operating voltage is high, memory-less effect, and the power supply that have extended cycle life, plurality of advantages such as environmentally safe is widely used as various mobile devices also makes it get into the large-scale practical stage.
The lithium ion battery characteristic can develop through the parts that improve battery; The performance of battery depends on electrode, electrolyte and comprises battery material wherein; And characteristic of electrode depends on active material, collector and the binding agent of battery; Binding agent provides the bonding force of cell active materials and collector, when binding agent provide between the active material or active material and collector between strong cohesive force the time, electronics and lithium ion move in electrode and electrode internal resistance reduction reposefully.
At present lithium ion battery water-base cathode pole piece generally adopts SBR styrene butadiene rubbers (SBR) as binding agent; But this type of binding agent modulus is less; Cause in the cyclic process; Cell thickness changes greatly, and this point performance is more obvious in square soft-package battery, has limited the application of lithium battery significantly; On the other hand, the SBR electrolyte resistance is relatively poor, in case through after the electrolyte immersion, cohesive force obviously weakens, so anode strip poor adhesion in the cyclic process, causes lithium battery to demonstrate bad cycle life characteristics.
Summary of the invention
The invention reside in the deficiency that is directed against prior art and provide a kind of rigidity stronger, the bonding agent of the lithium ion battery of low bulk performance uses the lithium ion battery of this bonding agent to have the good resistance expansion character.
In order to reach above-mentioned requirements, the present invention adopts following technical scheme:
The invention provides a kind of lithium ion battery negative; This negative pole comprises collector, is coated in the negative material on the collector; Negative material mainly comprises active material, conductive agent and binding agent; Wherein, binding agent adopts cellulosic binder, and the binding agent consumption accounts for the 1%-5%wt% of negative material total weight.
In the formula of size, content of binder very few (mass fraction is less than 1%), active material dispersion effect in slurry is poor; The slurry less stable of making causes the skewness of the active material in the pole piece, thus cause the part active material overcharge with crossing and put; And then have influence on the cycle performance of battery, in addition, binding agent is very few; The pole piece bonding is relatively poor, and in the pole piece manufacturing process, negative material comes off easily.(otherwise mass fraction is greater than 5%), binding agent possibly cover most of active material surface, cause anode impedance to increase, and analyse lithium in the battery charging process easily, influence battery performance.
Described cellulosic binder is a sodium carboxymethylcellulose, xanthans and hydroxyethylcellulose, because these materials have than higher modulus, lower ductility in the cyclic process, can suppress the expansion of graphite effectively.On the other hand, active SBR relatively between binding agent and the electrolyte, PVDF is lower, thereby has guaranteed the long cycle performance of battery, in addition, owing on its molecular structure a certain amount of carboxyl is arranged, significantly the bonding of improvement and active material and collector.
The concentration of aqueous solution of described cellulosic binder is 1% o'clock, and the viscosity under 25 ℃ is 50-1200mPa.s.Binding agent viscosity is too high, and solid content is lower in the preparation slurry process, causes in the pole piece dry run load bigger, wastes energy.
Find in the research that the substitution value that sodium carboxymethylcellulose is suitable is 0.6-1.2, substitution value is unsuitable excessive; Otherwise viscosity is too high; Cause the caking property variation, even have influence on the capacity performance of battery, substitution value is crossed to hang down and can be caused sodium carboxymethylcellulose hydrophily variation; Insoluble matter can significantly increase, and influences the slurry dispersion effect.Discover that in a large number the suitable number-average molecular weight of sodium carboxymethylcellulose is 50,000-1,000,000, it is more moderate to bond, and the battery performance of preparation is best.
The present invention also provides a kind of lithium ion battery negative; Comprise collector, active material, conductive agent, cellulose family bonding agent attached on the collector; Described bonding agent is above-mentioned bonding agent; Wherein, active material: conductive agent: cellulosic binder=92～99: 0～3: 1～5.Said active material is material with carbon element or alloy material.
The present invention also provides a kind of lithium ion battery in addition, comprises positive pole, negative pole, barrier film and electrolyte, and wherein, described negative pole is above-mentioned negative pole.
Beneficial effect of the present invention:
After the present invention adopts cellulosic binder to replace traditional sodium carboxymethylcellulose and butadiene-styrene rubber as the lithium battery binding agent; Realized the adhesive property more more superior than conventional binders; The battery of preparation has outstanding premium properties simultaneously, is mainly reflected in the following aspects:
The first, low cell expansion rate.Because cellulosic binder has high-modulus, the good characteristic of low bulk elongation can suppress the expansion of battery anode strip in cyclic process significantly, thereby reduces the cell expansion rate.
The second, Low ESR, high efficiency.In the pulp preparation process, because it has improved the dispersive property of active material and conductive carbon significantly, make that active material and the conductive carbon dispersion in the electrode is more even, reduce the electronic conductivity of battery, thereby improved the efficient of battery.
The 3rd, good long cycle characteristics.On the one hand; Carboxyl in the cellulosic binder can form chemical bond with the hydroxyl of active material, conductive carbon; Thereby strengthened the adhesion of active material and conductive carbon; When the electrode part was destroyed, the carboxyl of this strong polarity and the hydroxyl of active material showed good self-repair effect, thereby had guaranteed the stability of electrode.On the other hand; Since low reaction activity between binding agent and the electrolyte, and have good high electrolyte resistance characteristic, in the cyclic process; The part surface of active material covers for bonded dose preferably; Surface in feasible the exposure in the electrolyte significantly reduces, thereby has reduced the irreversible consumption of electrolyte on the active material particle surface, has guaranteed the long cycle performance of battery.
Description of drawings
Fig. 1 is the bounce-back curve chart of negative plate in the embodiment of the invention 1 and the Comparative Examples 1 electric core manufacturing process;
Fig. 2 is the AC impedance spectrogram of the battery of the embodiment of the invention 1 and Comparative Examples 1 preparation;
Fig. 3 embodiment 1 of the present invention and 2 and Comparative Examples 1 process lithium ion battery at 45 ℃ of cycle graphs that discharge with 0.7C charging and 0.5C.
Fig. 4 embodiment 1 of the present invention is processed lithium ion battery in 45 ℃ of cyclic processes with 0.7C charging and 0.5C discharge, cell expansion rate variation diagram with Comparative Examples 1.
Embodiment
Come content of the present invention is further specified below in conjunction with concrete embodiment and accompanying drawing, but invention protection range of the present invention is not limited only to the described content of embodiment.
Embodiment 1
The preparation process of negative plate
The cathode size prescription is pressed the siccative weight percent meter; Form by 2.5% sodium carboxymethylcellulose (CMC-Na), 1.5% conductive black, 96% negative electrode active material, three parts; Wherein negative electrode active material adopts Delanium, sodium carboxymethylcellulose, and its number-average molecular weight is about 500,000; 25 ℃ of viscosity 150mPa.s of its 1% aqueous solution, substitution value is 0.8.In the slurry layoutprocedure, solvent is a water, and water accounts for 60% of total slurry.
At first press above prescription with water, sodium carboxymethylcellulose; Join in the mixer grinder; Dissolving adds conductive black to have had by prescription again and dissolves in the good aqueous high molecular solution fully under vacuum state, and agitation grinding to fineness is below the 5 μ m fast; Add Delanium by prescription at last, vacuum stirs at a slow speed.Promptly make required cathode size with 150 order stainless steel sift net filtrations.
This slurry is coated in the Copper Foil two sides of 8 μ m equably, again with roll squeezer with the pole piece compacting, obtain the water-base cathode pole piece.
The preparation process of positive plate
The anodal cobalt acid lithium (LiCoO that uses
2) as active material.Modulate the anode sizing agent that contains this active material according to prescription, the solid constituent of this slurry comprises this positive active material of 90%, and 5% PVDF (Kynoar) is as bonding agent, and 5% conduction charcoal is as the conductivity auxiliary agent.This slurry uses NMP as solvent, and the solids content of slurry is 40%.
Press above prescription with N-methyl pyrrolidone (NMP), PVDF; Join in the mixer grinder; Dissolving joins conductive black by prescription and dissolves in the good oiliness Polymer Solution fully under vacuum state, and agitation grinding to fineness is below the 5 μ m fast; Add cobalt acid lithium by prescription at last, vacuum stirring is even.Promptly make required anode sizing agent with 200 order stainless steel sift net filtrations.
This slurry is coated in 12 μ m aluminium foil two sides equably, again with roll squeezer with the pole piece compacting, obtain the oiliness anode pole piece.
The assembling of battery:
Welding conduction lug on anodal and cathode pole piece makes the PP/PE composite isolated film that accompanies 14um in the middle of anodal and the negative pole and overlapping, and it is reeled forms naked electric core, encapsulate with aluminum plastic film again, and the injection nonaqueous electrolytic solution, the electrolyte of battery is the LiPF of 1mol/L
6Solution, primary solvent is mixed by EC, PC, DMC, and encapsulation back changes into and burn-in test battery, obtains that length and width are thick to be the square flexible-packed battery of 32mm * 82mm * 42mm.
Be with embodiment 1 difference: this negative electrode active material of cathode formula 97.5%, 1% sodium carboxymethylcellulose, 1.5% conductive black is as the conductivity auxiliary agent.The sodium carboxymethylcellulose substitution value that is wherein adopted is 1.0, molecular weight 1,000,000, and 25 ℃ of viscosity 1200mPa.s of its 1% aqueous solution, other is identical with embodiment 1, repeats no more here.
Embodiment 3
Be with embodiment 1 difference: this negative electrode active material of cathode formula 93.5%, 5% sodium carboxymethylcellulose, 1.5% conductive black is as the conductivity auxiliary agent.The sodium carboxymethylcellulose substitution value that is wherein adopted is 0.6, molecular weight 50,000, and 25 ℃ of viscosity 50mPa.s of its 1% aqueous solution, other is identical with embodiment 1, repeats no more here.
Be with embodiment 1 difference: this negative electrode active material of cathode formula 96.5%, 1% sodium carboxymethylcellulose, 1% xanthans, 1.5% conductive black is as the conductivity auxiliary agent.Other is identical with embodiment 1, repeats no more here.
Be with embodiment 1 difference: this negative electrode active material of cathode formula 96.5%, 1% sodium carboxymethylcellulose, 1% sodium hydroxyethyl cellulose, 1.5% conductive black is as the conductivity auxiliary agent.Other is identical with embodiment 1, repeats no more here.
Be with embodiment 1 difference: adopt alloy as active material, contain this negative electrode active material of 93.5% in the solid constituent of slurry, 5% sodium carboxymethylcellulose, 1.5% conductive black is as the conductivity auxiliary agent.Other is identical with embodiment 1, repeats no more here.
Comparative Examples 1
The cathode size prescription is pressed the siccative weight percent meter; By 1.0% sodium carboxymethylcellulose (CMC-Na), 1.5% conductive carbon, 96.0% Delanium, 1.5% butadiene-styrene rubber (SBR), four parts are formed, and wherein negative electrode active material adopts Delanium; Sodium carboxymethylcellulose; Its number-average molecular weight is about 500,000,25 ℃ of viscosity 150mPa.s of its 1% aqueous solution, and substitution value is 0.8.In the slurry layoutprocedure, solvent is a water, and water accounts for 60% of total slurry.
Press above prescription with water, sodium carboxymethylcellulose; Join in the mixer grinder; Dissolving joins conductive black by prescription and dissolves in the good aqueous high molecular solution fully under vacuum state, and agitation grinding to fineness is below the 5 μ m fast; Add Delanium by prescription at last, vacuum stirs at a slow speed.Filter with the examination of 150 order stainless steel mesh, after strainability is good, transfer slow mixing speed, add butadiene-styrene rubber again, vacuum slowly stirs to prevent the butadiene-styrene rubber breakdown of emulsion, after being uniformly dispersed, promptly makes required cathode size.
All the other adopt with embodiment 1 said same way as electrode are provided.
Performance test methods:
The test of pole piece cohesive force:
Get the anode diaphragm after colding pressing, be cut into the rectangle small pieces of 20mm*10cm size, with the wide two-sided gluing of 20mm on the corrosion resistant plate of cleaning.Adopt puller system test pole piece 180 degree peeling forces, the puller system draw speed is 50mm/min.Be to characterize the pole piece electrolyte resistance and soak performance, get the anode strip after the cutting, be placed in the electrolyte, airtight being placed in the 60 degree baking ovens taken out diaphragm after 96 hours, adopted same procedure test pole piece cohesive force.
Pole piece bounce-back test:
After pole piece is colded pressing, with micrometer test pole piece thickness, as the pole piece initial thickness.In the electric subsequently core manufacturing process, before toasting afterwards, reel at anode strip successively, the shaping of electric core anchor clamps; Battery completely fills 4.2V for the first time; The battery 3.0V that discharges for the first time, and voltage is several stages test anode strip thickness such as 3.8V, calculates different conditions inferior pole piece bounce-back rate.
The test of battery circulation expansion rate:
Before the battery circulation, adopt height gage test 3.8V cell thickness, note is made the battery original thickness.In the cyclic process, the test battery that uses the same method is the 10th, 20, and battery 4.2V completely fills thickness after 30,40,60,80,100,200,300,400 circulations.
Cell expansion rate=(4.2V cell thickness/3.8V battery original thickness-1) * 100%
After the negative plate of the foregoing description preparation is colded pressing and after soaking electrolyte, pole piece cohesive force test result is seen table 1:
The pole piece cohesive force and the resistance of the different embodiment/Comparative Examples of table 1
Pole piece cohesive force test result explanation, the cathode pole piece that the carboxymethyl cellulose adhesive preparation obtains is compared with the pole piece of butadiene-styrene rubber preparation in the Comparative Examples, and it is strong to have a bonding force, and characteristics such as membrane resistance is little.And under the same terms, after the pole piece of patent preparation of the present invention soaked through electrolyte, cohesive force was apparently higher than Comparative Examples.
In order to contrast sodium carboxymethylcellulose and conventional SBR binding agent performance, in battery manufacturing process, monitored the rebound of cathode pole piece in the manufacturing process, the result sees Fig. 1.The cathode pole piece same phase bounce-back that the sodium carboxymethylcellulose binding agent is made is starkly lower than the SBR binding agent.
The ac impedance spectroscopy of test implementation example 1 and battery normal temperature under 3.85V voltage of Comparative Examples 1 preparation, the result sees Fig. 2, the battery impedance of carboxymethyl cellulose adhesive preparation is starkly lower than conventional SBR battery.
To embodiment 1, embodiment 2 systems full battery 45 ℃ with the charging of 0.7 multiplying power, after the 0.5C multiplying power discharging circulation 400 times, capability retention is higher than Comparative Examples 1 still 88%, sees Fig. 3, has characteristics safe and reliable, that have extended cycle life.
Fig. 4 be embodiment 1 with Comparative Examples 1 under 45 ℃ of conditions, with the charging of 0.7 multiplying power, in the cyclic process of 0.5C multiplying power discharging, cell thickness expansion variation diagram, same loop number down, the battery of pure sodium carboxymethylcellulose preparation is starkly lower than the battery of traditional SBR preparation.
The comprehensive data that go up, sodium carboxymethylcellulose can strengthen the adhesive property of collector and active material rete really as binding agent, reduces contact resistance, suppresses the effect of battery bounce-back in the cyclic process.The lithium ion battery of making has low internal resistance, long characteristics such as cycle life.
Need to prove that according to the announcement and the elaboration of above-mentioned specification, those skilled in the art in the invention can also change and revise above-mentioned execution mode.Therefore, the embodiment that discloses and describe above the present invention is not limited to also should be in the protection range of claim of the present invention to equivalent modifications more of the present invention and change.In addition, although used some specific terms in this specification, these terms are explanation for ease just, the present invention is not constituted any restriction.
Claims (9)
1. lithium ion battery negative; Comprise collector, be coated in the negative material on the collector; Described negative material comprises active material, conductive agent and binding agent; It is characterized in that: described binding agent is a cellulosic binder, and said cellulose family bonding agent accounts for the 1%-5%wt of negative material total weight.
2. lithium ion battery negative according to claim 1 is characterized in that: described cellulosic binder is at least a in sodium carboxymethylcellulose, xanthans or the hydroxyethylcellulose.
3. lithium ion battery negative according to claim 1 and 2 is characterized in that: the concentration of aqueous solution of described cellulosic binder is 1% o'clock, and the viscosity under 25 ℃ is 50-1200mPa.s.
4. lithium ion battery negative according to claim 2 is characterized in that: the substitution value of said sodium carboxymethylcellulose is 0.6-1.2.
5. lithium ion battery negative according to claim 2 is characterized in that: the number-average molecular weight of said sodium carboxymethylcellulose is 50,000-1,000,000.
6. lithium ion battery negative according to claim 1 is characterized in that: the mass ratio of said active material, conductive agent, cellulosic binder is 92～99: 0～3: 1～5.
7. according to claim 1 or 6 described lithium ion battery negatives, it is characterized in that: said active material is material with carbon element or alloy material.
8. lithium ion battery negative according to claim 1 is characterized in that: said conductive agent is a conductive black.
9. a lithium ion battery comprises positive pole, negative pole, barrier film and electrolyte, it is characterized in that: described negative pole is each described negative pole of claim 1 to 8.
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| CN105655627A (en) * | 2016-01-03 | 2016-06-08 | 天津中科锂能科技发展有限公司 | Rapid preparation method of lithium battery slurry |
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| CN108183215A (en) * | 2017-12-27 | 2018-06-19 | 广州鸿森材料有限公司 | Ion secondary battery cathode material lithium and preparation method thereof |
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| CN112345139A (en) * | 2020-10-13 | 2021-02-09 | 安普瑞斯(南京)航运动力有限公司 | Pressure detection method based on battery box |
| CN112345139B (en) * | 2020-10-13 | 2022-02-08 | 安普瑞斯(南京)航运动力有限公司 | Pressure detection method based on battery box |
| CN113363589A (en) * | 2021-05-19 | 2021-09-07 | 东莞维科电池有限公司 | Lithium ion battery and preparation method thereof |
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