CN102637903A - Formation method of lithium ion battery - Google Patents
Formation method of lithium ion battery Download PDFInfo
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- CN102637903A CN102637903A CN2012100983831A CN201210098383A CN102637903A CN 102637903 A CN102637903 A CN 102637903A CN 2012100983831 A CN2012100983831 A CN 2012100983831A CN 201210098383 A CN201210098383 A CN 201210098383A CN 102637903 A CN102637903 A CN 102637903A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
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Abstract
The invention belongs to the technical field of lithium ion batteries and particularly relates to a formation method of a lithium ion battery. The formation method comprises the following steps of: vacuumizing a battery to be injected and performing first injection on the battery; performing opening formation on the battery subjected to the first injection, wherein a formation current ranges from 0.1C to 1.5C; and performing second injection and encapsulation on the battery subjected to the formation, wherein electrolyte for the second injection comprises high-temperature additives including at least one of trimethylene sulfite, ethylene sulfate, succinonitrile and adiponitrile. Compared with the prior art, the formation method disclosed by the invention avoids the electrolyte leakage caused by quick gas production during deformation with a large current by virtue of the way of twice injection, and avoids the influence on the components of an SEI (Solid Electrolyte Interface) membrane due to adding the electrolyte additives once, thereby improving the low temperature performance of a battery cell; and as the battery cell has high temperature performance by virtue of the additives injected after the formation, and the formation time is shortened greatly, the process efficiency is enhanced greatly, and the production cost is reduced.
Description
Technical field
The invention belongs to technical field of lithium ion, relate in particular to a kind of big electric current chemical synthesizing method of lithium ion battery.
Background technology
Lithium rechargeable battery is as a kind of environmental protection battery; Have advantages such as operating voltage height, specific energy is high and have extended cycle life; Obtained in recent years developing rapidly, the application in mobile devices such as mobile phone, ups power, notebook computer, electric bicycle and electric automobile more and more widely.The increase of the expansion in battery applications field and battery requirements amount impels the battery production merchant must simplify technological process, and the reduction activity time is enhanced productivity to satisfy market demands, and the comprehensive electrochemical of constantly improving battery simultaneously satisfies application requirements.Along with the lifting of the production mechanization degree of battery industry, formation process has become the important step of present restriction lithium ion battery production efficiency.
The step that changes into of lithium ion battery is the important procedure that battery is made, and is related to the performance of the aspects such as capacity height, cycle life length and high temperature storage of battery.In the formation process of battery, organic electrolyte can reduce, decompose in negative terminal surface, forms SEI (Solid Electrolyte Interface, solid electrolyte) film in negative terminal surface.Formation is even, stable SEI film all is favourable to the various chemical properties of battery.And the composition of electrolyte directly influences the film formed quality of SEI: when containing the additive of difference in functionality in the electrolyte, be not easy to form desirable SEI film when changing into.
In order to obtain SEI film preferably, it is to adopt little electric current to reach tens of hours charging that tradition changes into, and production efficiency is extremely low.
In order to improve the efficient of formation process, quicken to produce side reaction gas and shorten and change into the time through introducing big pre-charge electricity thereby notification number is the world patent of WO2010/081422A1.But this process using is the identical electrolyte of twice injection before and after changing into, the influencing each other of each additive of electrolyte when not considering large current charge, so charging effect is unsatisfactory, electric core cryogenic property is relatively poor relatively.
And in order to improve the quality and the battery performance of the SEI film that forms in the formation process, publication number is that the Chinese patent of CN101640285A is through pouring into different electrolyte respectively, with low temperature and the cycle performance that improves battery before and after changing into.But need leave standstill 2～3 days after this technology fluid injection, and adopt little electric current to change into, the whole formation process time is long, needs the sealing liquid injection hole to prevent that electrolyte from leaking because of long-time the exposure, need open liquid injection hole after changing into again and carry out the secondary fluid injection, and production efficiency is low.
In view of this, necessary a kind of compound method for lithium ion battery that can greatly shorten the time of changing into, increase substantially production capacity is provided, guarantees that simultaneously battery has excellent high and cryogenic property.
Summary of the invention
The objective of the invention is to: to the deficiency of prior art, and a kind of compound method for lithium ion battery that can greatly shorten the time of changing into, increase substantially production capacity is provided, guarantees that simultaneously battery has excellent high and cryogenic property.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of chemical synthesizing method of lithium ion battery comprises the steps:
Treat that intercell vacuumizes and carry out the fluid injection first time; Vacuumizing before the fluid injection, is to guarantee that the gas in the pole piece hole is removed, and is beneficial to the quick infiltration of the electrolyte of the injection of fluid injection for the first time, shortens time of repose.
Battery after the fluid injection first time is carried out opening change into, forming current is 0.1C～1.5C; In the formation process, adopt the extremely certain electric weight of large current charge of 0.1C～1.5C, thereby form the SEI film in negative terminal surface.Opening changes into the quick discharge of the gas that conveniently changes into generation, avoids gas to gather at inside battery and causes cell expansion, shell swell, distortion.Opening changes into and also is convenient to electrolyte adding for the second time in addition, shortens activity time.
Battery after changing into is carried out the fluid injection second time and encapsulation, contain high temperature additive in the electrolyte of the said fluid injection second time, said high temperature additive is at least a in propylene sulfite, sulfuric acid vinyl ester, succinonitrile and the adiponitrile.Additive can form protective layer at negative pole or anodal surface, prevents decomposition or the positive electrode active materials oxidation electrolyte of SEI film under the high temperature and causes electric core flatulence.
The adding of high temperature additive can improve the high-temperature behavior of battery.The present invention injects the electrolyte that contains high temperature additive after being chosen in formation process, is because if before changing into, inject the electrolyte that contains high temperature additive, can influence the quality of SEI film, makes electric core deteriorated low temperature performance.Therefore, adopt chemical synthesizing method of the present invention, both can shorten the time of changing into, guarantee that electric core forms the SEI film than homogeneous when big electric current changes into, can improve the comprehensive electrochemical (comprising high-temperature behavior and cryogenic property) of electric core again.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, be benchmark with the electrolyte total weight, the weight content of said high temperature additive is 0.1～5wt%.Experimental result is found high temperature additive amount in the electrolyte if surpass 5%, and the discharge performance of battery and electric core cycle performance can variation.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, be benchmark with the electrolyte total weight, the weight content of said high temperature additive is 0.5～3wt%.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, be benchmark with the electrolyte total weight, the weight content of said high temperature additive is 2wt%.
A kind of improvement as the chemical synthesizing method of lithium ion battery of the present invention; The said vacuum magnitude that vacuumizes for-0.01Mpa～-0.1Mpa; To guarantee that the gas in the pole piece hole is drawn out of, be beneficial to the quick infiltration of the electrolyte of the injection of fluid injection for the first time, shorten changing into preceding time of repose.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, the electrolyte content that fluid injection is for the first time injected is 65～85% of the total consumption of electrolyte.Carry electrolyte secretly when electrolyte content too much can cause changing into the generation gaseous emission and overflow, cause damage, also influence the battery outward appearance.If electrolyte content is not enough, owing to there is not enough electrolyte, ion channel is obstructed when changing into, the formation effect variation in the pole piece.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, the electrolyte content that fluid injection is for the second time injected is 15～35% of the total consumption of electrolyte.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, the charging interval that opening changes into is 3～60Min.This chemical synthesizing method will change into time decreased to 60Min under the situation that guarantees electric core performance, overcome the long-time opening of traditional little electric current and change into the volatilization that causes electrolyte, be beneficial to the production process clean environment firendly.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, priming volume is 8%～60% of a battery rated capacity in the opening formation process.Experiment is found to reach about 10% of battery total current when the preliminary filling electric weight, and it is maximum that formation gas reaches, and formed the SEI film.
As a kind of improvement of the chemical synthesizing method of lithium ion battery of the present invention, said forming current is 0.5C～1.5C.
In addition, whole formation process carries out in drying shed or glove box.Avoid moisture and other impurity in the external environment condition to the negative effect that battery causes, guarantee electric core performance.
With respect to prior art, beneficial effect of the present invention:
Utilize chemical synthesizing method of the present invention, treat intercell earlier and vacuumize, can the gas in the pole piece hole be discharged, the electrolyte that is beneficial to injection soaks into the pole piece of loose structure fast, shortens to change into preceding time of repose; The problem that quick aerogenesis causes electrolyte to leak when having overcome big electric current and change into through twice fluid injection mode; Add the influence of high temperature additive before also having avoided changing into to the SEI membrane component; Thereby improved the cryogenic property of electric core, changed into the high temperature additive of injecting the back simultaneously and make electric core have high-temperature behavior concurrently.The method that changes into through big electric current in addition can obtain the similar even better electrical property of electric core that changes into for a long time with traditional little electric current, shortens changing into the time simultaneously greatly.Conventional method needs the formation process of ability completion in to several days, as long as just can accomplish in one or two hour, has greatly improved process efficiency through the method, has reduced production cost, has important economic implications.
Embodiment
Embodiment 1
The preparation of anode pole piece: with LiCoO
2(cobalt acid lithium), Super-P (conductive carbon black), PVDF (gathering inclined to one side fluorine resin) mix and stir with NMP (N, N-dimethyl pyrrolidone) according to mass ratio 95: 2: 3 and obtain the slurry of anode pole piece coating.Regulate viscosity through NMP in the whipping process.Then slurry is uniformly coated on the two sides of the plus plate current-collecting body (aluminium foil) of 14 micron thick according to certain width, through colding pressing, cutting into slices, makes anode pole piece at last.
The preparation of cathode pole piece: with MCMB (anode graphite a kind of; The mesophase pitch based carbon microsphere), Super-P (conductive carbon black), CMC (water based adhesive, carboxymethyl cellulose), SBR (Styrene Butadiene Rubber rubber) were according to mass ratio 94: 1: 2: 3 mix and stir with deionized water and obtain the negative pole coating sizing-agent.Regulate viscosity through deionized water in the whipping process.Then slurry is coated on the two sides of the negative current collector (Copper Foil) of 9 micron thick according to certain width, through colding pressing, cutting into slices makes cathode pole piece.
The preparation of battery: the polyethylene barrier film of the above-mentioned positive pole that obtains, negative pole and 16 micron thick is wound into electric core, electric core is put into battery case (aluminum-plastic composite membrane).Electrolyte prescription is the LiPF of 1mol/L
6Solution, its solvent are the mixed solvent of EC, PC and DEC, and wherein the volume ratio of ethylene carbonate (EC), propene carbonate (PC), diethyl carbonate (DEC) is 1: 1: 1.In drying shed, the above-mentioned electrolyte vacuum of 3.0 grams is injected battery case carry out the fluid injection first time.Leave standstill and carry out opening with 0.5C current charges 15min after half an hour and change into, charging capacity is 12.5% of a battery rated capacity.Then 0.038 dintrile (AN) of restraining oneself is added in the above-mentioned electrolyte of 0.762 gram and mixes, the electrolyte that will contain the AN additive then injects the electric core shell body and carries out the fluid injection second time, and fast sealing is processed 053450 type lithium ion battery.
Embodiment 2
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 2.47 grams, leaves standstill to carry out opening with 0.1C current charges 60min after half an hour and change into, and charging capacity is 10% of a battery rated capacity.Then with mixing in the above-mentioned electrolyte of 0.19 gram succinonitrile (SN) adding, 1.14 grams, the electrolyte that will contain the SN additive then injects the electric core shell body and carries out the fluid injection second time, and fast sealing is processed 053450 type lithium ion battery.
Embodiment 3
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 3.23 grams, leaves standstill to carry out opening with 1.5C current charges 3min after half an hour and change into, and charging capacity is 8% of a battery rated capacity.Then with mixing in the above-mentioned electrolyte of 0.038 gram sulfuric acid vinyl ester (DTD) adding, 0.532 gram, the electrolyte that will contain the DTD additive then injects the electric core shell body and carries out the fluid injection second time, and fast sealing is processed 053450 type lithium ion battery.
Embodiment 4
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 3.04 grams, leaves standstill to carry out opening with 1C current charges 30min after half an hour and change into, and charging capacity is 50% of a battery rated capacity.Then with mixing in the above-mentioned electrolyte of 0.114 gram propylene sulfite (PS) adding, 0.646 gram, the electrolyte that will contain the PS additive then injects the electric core shell body and carries out the fluid injection second time, and fast sealing is processed 053450 type lithium ion battery.
Embodiment 5
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 2.85 grams, leaves standstill to carry out opening with 0.5C current charges 30min after half an hour and change into, and charging capacity is 25% of a battery rated capacity.Then with mixing in 0.114 gram propylene sulfite (PS) and the above-mentioned electrolyte of 0.038 gram succinonitrile (SN) adding, 0.798 gram; The electrolyte that will contain PS and SN additive then injects the electric core shell body and carries out the fluid injection second time; Fast sealing is processed 053450 type lithium ion battery.
Embodiment 6
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 2.85 grams, leaves standstill to carry out opening with 0.5C current charges 30min after half an hour and change into, and charging capacity is 45% of a battery rated capacity.Then 0.114 gram propylene sulfite (PS) and 0.038 dintrile (AN) of restraining oneself is added 0.798 and restrains in the above-mentioned electrolyte and mix; The electrolyte that will contain PS and AN additive then injects the electric core shell body and carries out the fluid injection second time; Fast sealing is processed 053450 type lithium ion battery.
Embodiment 7
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 2.85 grams, leaves standstill to carry out opening with 0.5C current charges 30min after half an hour and change into, and charging capacity is 35% of a battery rated capacity.Then with mixing in 0.076 gram sulfuric acid vinyl ester (DTD) and the above-mentioned electrolyte of 0.038 gram succinonitrile (SN) adding, 0.836 gram; The electrolyte that will contain DTD and SN additive then injects the electric core shell body and carries out the fluid injection second time; Fast sealing is processed 053450 type lithium ion battery.
Embodiment 8
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, the electrolyte content that when first time fluid injection, injects is 2.85 grams, leaves standstill to carry out opening with 0.5C current charges 30min after half an hour and change into, and charging capacity is 60% of a battery rated capacity.Then 0.076 gram sulfuric acid vinyl ester (DTD) and 0.038 dintrile (AN) of restraining oneself is added 0.836 and restrains in the above-mentioned electrolyte and mix; The electrolyte that will contain DTD and AN additive then injects the electric core shell body and carries out the fluid injection second time; Fast sealing is processed 053450 type lithium ion battery.
Comparative example 1
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is that the electrolyte that secondary injects does not contain high temperature additive with for the first time identical.
Comparative example 2
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, will contain 0.038 restrain oneself dintrile (AN) the disposable injection battery case of electrolyte, the weight of electrolyte is 3.8 grams.
Comparative example 3
The mode of describing according to embodiment 1 prepares lithium ion battery, and different is, changes into and adopts traditional little electric current chemical synthesizing method, and with the 0.035C 800min that charges, charging capacity is 50% of a battery rated capacity.
Battery performance relatively
Battery to embodiment 1 to 8 and comparative example 1 to 3 is tested as follows:
(1) low temperature loop test
The battery of embodiment 1 to 8 and comparative example 1 to 3 is placed in the low temperature environment (10 ℃) carries out the capacity loop test, method of testing: the discharge capacity first of first test battery.To 4.2V, change constant voltage charge with the 0.8C constant current charge then, to electric current be 0.05C, be discharged to 3V with 0.5C then, and repeat 200 circulations, the discharge capacity of test this moment, and the capability retention of counting cell, the computing formula of capability retention is following:
Capability retention=(C1-C2)/C1 * 100%
The result sees table 1.Can find out that from table 1 cryogenic property of the battery of embodiment 1 to 8 is similar with the cryogenic property of the battery of the comparative example that does not increase temperature additive 1, and obviously be superior to the cryogenic property that comparative example 2 disposable addings contain the battery of additive.Embodiment 1 battery that adopts battery that big electric current changes into and the little electric current of comparative example 3 usefulness to change into has suitable cryogenic property in addition.
(2) normal temperature and high temperature circulation test
The battery of embodiment 1 to 8 and comparative example 1 to 3 preparation is placed in normal temperature environment (25 ℃) and the hot environment (45 ℃) carries out the capacity loop test, method of testing: the discharge capacity first of test battery at first, to 4.2V, change constant voltage charge with the 1C constant current charge then; To electric current 0.05C; Be discharged to 3V with 1C then, and repeat 500 circulations, test discharge capacity at this moment; And the capability retention of counting cell, the computing formula of capability retention is following:
Capability retention=(C1-C2)/C1 * 100%
The result sees table 1.Can find out that from table 1 high-temperature behavior of the battery of embodiment 1 to 8 contains additive than disposable adding the high-temperature behavior of battery of comparative example 2 is good, and the high-temperature behavior of the battery of not additivated comparative example 1 is very poor.Embodiment 1 battery that adopts battery that big electric current changes into and the little electric current of comparative example 3 usefulness to change into has suitable high-temperature behavior in addition.
Table 1: embodiment 1 to 8, and the cycle performance of comparative example 1 to 3 relatively
In sum; Utilize chemical synthesizing method of the present invention,, overcome big electric current and changed into the defective that is difficult for forming desirable SEI film and causes electric core Cycle Difference through twice fluid injection mode; Both guaranteed the good high temperature performance of lithium ion battery tool; Shorten changing into the time simultaneously greatly, increase substantially production capacity, reduce production costs.
Need to prove that according to other execution modes of the present invention, positive active material also can be Li
zCoO
2, Li
zNiO
2, Li
zMnO
2, Li
zCo
1-(x+y)Ni
xMn
yO
2, Li
zNi
xMn
1-xO
2, Li
zCo
xNi
1 -xO
2, LiVPO
4, Li
2MnO
3Or Li
zMn
xM
1-xO
4Deng in (wherein: x, y, x+y＜1, z>=1) one or several.Negative electrode active material also can be hard carbon, soft carbon, Li
4Ti
5O
12, Sn, Si or its arbitrary proportion mixture.Barrier film can be the polypropylene barrier film; The polyethylene barrier film; Or polypropylene and polyethylene composite high-molecular barrier film; Or the polymer gel attitude barrier film that forms of polyvinylidene fluoride, vinylidene difluoride-hexafluoropropylene copolymer, polymethyl methacrylate, polyethylene glycol, or the composite isolated film of aforementioned composite high-molecular barrier film and aforementioned gel state barrier film.Electrolytic salt in the electrolyte can be LiPF
6, LiClO
4, LiBF
4, LiAsF
6, LiCl, LiBr, LiBOB, CF
3SO
3Li, CH
3SO
3Li, LiB (C
6H
5)
4Or its combination.Organic solvent in the electrolyte can be EC, PC, DEC, DMC, FEC, VC, oxolane, gamma-butyrolacton, diethyl ethyl phosphonate, methyl sulfoxide, dioxolane, acetonitrile or its combination.
Need to prove that according to the announcement and the instruction 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 fall in the protection range of claim of the present invention 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 (10)
1. the chemical synthesizing method of a lithium ion battery is characterized in that, comprises the steps:
Treat that intercell vacuumizes and carry out the fluid injection first time;
Battery after the fluid injection first time is carried out opening change into, forming current is 0.1C～1.5C;
Battery after changing into is carried out the fluid injection second time and encapsulation, contain high temperature additive in the electrolyte of the said fluid injection second time, said high temperature additive is at least a in propylene sulfite, sulfuric acid vinyl ester, succinonitrile and the adiponitrile.
2. the chemical synthesizing method of lithium ion battery according to claim 1, it is characterized in that: with the electrolyte total weight is benchmark, the weight content of said high temperature additive is 0.1～5wt%.
3. the chemical synthesizing method of lithium ion battery according to claim 2, it is characterized in that: with the electrolyte total weight is benchmark, the weight content of said high temperature additive is 0.5～3wt%.
4. the chemical synthesizing method of lithium ion battery according to claim 3, it is characterized in that: with the electrolyte total weight is benchmark, the weight content of said high temperature additive is 2wt%.
5. the chemical synthesizing method of lithium ion battery according to claim 1 is characterized in that: the said vacuum magnitude that vacuumizes for-0.01Mpa～-0.1Mpa.
6. the chemical synthesizing method of lithium ion battery according to claim 1 is characterized in that: the electrolyte content that fluid injection is for the first time injected is 65～85% of the total consumption of electrolyte.
7. the chemical synthesizing method of lithium ion battery according to claim 1 is characterized in that: the electrolyte content that fluid injection is for the second time injected is 15～35% of the total consumption of electrolyte.
8. the chemical synthesizing method of lithium ion battery according to claim 1, it is characterized in that: the charging interval that opening changes into is 3～60Min.
9. the chemical synthesizing method of lithium ion battery according to claim 1, it is characterized in that: priming volume is 8%～60% of a battery rated capacity in the opening formation process.
10. the chemical synthesizing method of lithium ion battery according to claim 1, it is characterized in that: said forming current is 0.5C～1.5C.
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