CN101944585B - Injection method for lithium battery - Google Patents
Injection method for lithium battery Download PDFInfo
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- CN101944585B CN101944585B CN2010102671873A CN201010267187A CN101944585B CN 101944585 B CN101944585 B CN 101944585B CN 2010102671873 A CN2010102671873 A CN 2010102671873A CN 201010267187 A CN201010267187 A CN 201010267187A CN 101944585 B CN101944585 B CN 101944585B
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Abstract
The invention discloses an injection method for a lithium battery. The method comprises a step of injecting electrolyte into a vacuumized battery shell. In the method, repeated vacuumization is performed in the presence of inert gas so that the electrolyte is completely absorbed in the battery and the electrolyte is supplemented finally. In the method, the original pressurizing process is canceled, the influence of gas on the electrolyte absorption is avoided, the exposure time of the battery in the air is shortened and the battery capacity is improved.
Description
Technical field
The invention relates to a kind of lithium battery manufacture method, electrolyte filling method, relate in particular to the electrolyte filling method of lithium battery.
Technical background
Along with science and technology and rapid economic development, the function of market electronic product from strength to strength, and the shape molded dimension requires more and more littler, weight to require more and more lighter.The lithium ion battery volume is little, the energy height, high working voltage, non-environmental-pollution, have extended cycle life, advantage such as operating temperature range is wide, be widely used in the electronic products such as mobile manual phone, notebook computer, digital camera, even be applied on the automobile.Therefore little, the lightweight requirement of electronic product volume is reflected on one's body the lithium battery that power is provided, and just has requirement more and more higher to lithium ion battery, particularly needs the lithium ion battery product that the capacity performance is higher, volume is littler, performance is listed as.
Lithium ion battery generally comprises battery case and is contained in battery container interior electric core and nonaqueous electrolytic solution, and described electric core comprises positive pole, negative pole and the barrier film between positive pole and negative pole.The preparation method of this battery makes electric core with positive pole, negative pole and barrier film, then electric core is placed in the battery case, and nonaqueous electrolytic solution injects in the battery case.Described nonaqueous electrolytic solution generally contains organic solvent and lithium salts.Therefore the uptake of electrolyte how much be related to battery capacity and cycle life, the incomplete absorption of electrolyte can cause battery to hold decline, the increase of the internal resistance of cell and the rapid decay of cycle life of reason.Lithium ion battery constantly reduces volume, high-octane direction develops, and is very limited for the space that holds electrolyte in the battery.Therefore must absorb as much as possible in limited space may many electrolyte, provide battery institute must electrolyte, the cycle life of raising battery.
The master operation flow process of existing lithium ion battery fluid injection is as follows: vacuumize → fluid injection → pressurize → vacuumize pressurize → leave standstill → secondary fluid injection district → battery discharges, therefore, three districts of whole fluid injection flow process: fluid injection district, leave standstill district, secondary fluid injection district.Be not difficult to find out thus, leave standstill the district and play a very important operation, the time length that leaves standstill concerns the absorbing state of electrolyte, the battery time that Electolyte-absorptive is good is short, and it is long to absorb bad battery time, thus one, and battery is exposed in the air for a long time, absorbed a large amount of moisture content and impurity, this fail safe to battery brings very big influence.This process of pressurization is particularly arranged in the fluid injection process flow, and there is certain defective in this method, and pressurization must have gas to enter in the battery case, and this part air has reduced the finite volume in the battery case, makes to absorb more electrolyte content in battery.
Summary of the invention
The objective of the invention is in order to overcome in the prior art the few defective of reservoir quantity in the battery liquid-filling process, for a kind of lithium battery electrolyte filling method, this method can effectively provide the fluid injection efficient of lithium battery, promotes the absorption of electrolyte.
The present invention adopts following technical scheme:
A kind of electrolyte filling method of lithium battery, this method are included in and inject electrolyte in the battery case that vacuumizes, and it is characterized in that this method repeats to vacuumize under the condition of inert gas, cause abundant Electolyte-absorptive in the battery, in the end carry out replenishing of electrolyte.In the method, cancelled original pressure process, avoided gas to the influence that electrolyte absorbs, shortened battery and be exposed to the airborne time, the capacity of battery is improved.
Described inert gas is any one of nitrogen, argon gas etc.
Specifically, this method comprises the steps:
(1), lithium ion battery is inserted in the good fluid injection district of sealing;
(2), battery is weighed;
(3), battery port is installed priming device;
(4), battery is vacuumized, and keep certain hour;
(5), to injecting nonaqueous electrolytic solution behind the battery vacuum-pumping;
(6), battery is charged into nitrogen and recover atmospheric pressure;
(7), repeat battery vacuum-pumping is charged into nitrogen at same station;
(8), battery is discharged;
(9), battery is carried out weighing the second time;
(10), battery is replenished electrolyte;
(11), battery is sealed.
The electrolyte filling method of above-mentioned lithium ion battery is inserted battery in the seal area earlier, and battery is carried out weighing before the fluid injection, priming device is installed is vacuumized, and again battery is injected nonaqueous electrolytic solution, and nonaqueous electrolytic solution can be divided equally injection several times.In the electrolyte filling method of described lithium ion battery, battery is charged into nitrogen recover atmospheric pressure, charge into nitrogen recover atmospheric pressure can at least twice, be preferably 3-5 time, the described nitrogen that charges into recovers atmospheric pressure, nitrogen must be dry gas, otherwise can introduce moisture, causes degradation of cell performance.
The electrolyte filling method of described lithium ion battery, battery carry out the good fluid injection district of sealing, will carry out being weighed as for the first time the dry weight W1 of battery to battery, behind the vacuum pumping liquid injection, advance to be weighed as for the second time dry weight and the electrolyte weight W2 of battery, and it is as follows to calculate worker's formula:
Electrolyte weight: W=W2-W1
After said method is weighed, calculate the weight of inside battery electrolyte effectively, the battery not enough to electrolyte content replenishes electrolyte content, will solve the electrolyte content of battery effectively.
Nonaqueous electrolytic solution of the present invention can be normally used various nonaqueous electrolytic solutions in the lithium ion battery, and described electrolyte contains electrolyte lithium salt and organic solvent (additive) and mixed.Lithium salts as: (Chinese name of LiPF6: the Chinese name of lithium hexafluoro phosphate, LiBF4: LiBF4) etc., organic solvent is as EC, the DMC (Chinese name of EC: ethylene carbonate, the Chinese name of DMC: the dimethyl cyclosiloxane) etc. for LiPF6, LiBF4.(mixed proportion is weight ratio: 1: 1--1: 2)
The electrolyte filling method of lithium ion battery of the present invention, the air pressure that wherein vacuumizes is 30mPa-60mPa, is preferably 40mPa.Time is maintained 40-60S, is preferably 45S.It is 1 standard atmospheric pressure that inflated with nitrogen recovers atmospheric pressure, can repeat to charge into nitrogen and return to atmospheric pressure at least twice.
Fluid injection of the present invention is for vacuumizing simultaneously of fluid injection carried out, so the fluid injection machine adopts vacuum fluid injection machine.
Adopt the electrolyte filling method of lithium battery of the present invention, Construction Bank original technology, the flow process of fluid injection will be shortened greatly, shorten battery divides contact in water in air time, effectively the control battery is to the absorption of electrolyte, electrolyte content to inside battery guarantees simultaneously, has improved capacity and the cycle life of battery.
Description of drawings
Fig. 1 is the loop test curve chart of institute of the present invention implementation result.
Embodiment
Be described in detail below by concrete enforcement of the present invention of embodiment.
Embodiment 1
This example explanation the invention provides a kind of electrolyte filling method of lithium ion battery
1, the preparation of battery
(1) Zheng Ji preparation
The anodal active component LiFePO4 of 143 grams, 6.4 gram conductive agent SP, 9.55 gram binding agent polyvinylidene fluoride PVDF, 262 gram N-methyl pyrrolidones are mixed, in de-airing mixer, stir then and form uniform anode sizing agent.
This slurry is evenly coated on the 18um aluminium foil, makes the positive pole that is of a size of 1540 * 55 * 0.167mm in 120 ℃ of oven dry, roll-in, itemize cutting then, wherein contain 26.4 gram active component LiFePO4 (LiFePO 4).
(2) preparation of negative pole
Sodium polydithio-dipropyl sulfonate), 2.65 gram binding agent polyvinylidene fluoride (PVDF), 64.5 gram N-N-methyl 2-pyrrolidone N-s, 0.04 gram additive oxalic acid mix with 53.2 gram active component native graphites, 1.48 gram acetylene blacks, the 1.77 gram conductive agent SP (Chinese name of SP:, in de-airing mixer, stir then and form uniform cathode size.
This slurry is evenly coated on the 10um Copper Foil, makes the negative pole that is of a size of 1576 * 57 * 0.82mm in 110 ℃ of oven dry, roll-in, itemize cutting then, wherein contain 9.9 gram active component native graphites.
(3) preparation of electrolyte
LiPF6 (lithium hexafluoro phosphate) is dissolved in EC/DMC=1 by the concentration of 1 mol: form nonaqueous electrolytic solution in 1 the mixed solvent.
(4) assembling of battery
The electric core that anodal, three layers of barrier film and negative plate are wound into a cylindrical lithium ion battery places the box hat of 26 series, and making cylindrical battery and taking by weighing weight is W1.It is W2 that fluid injection vacuumizes back weight.
Electrolyte filling method by above-mentioned a kind of lithium ion battery will carry out fluid injection to battery, (59.5g) carries out vacuum pumping liquid injection with battery weight, earlier be evacuated to air pressure 40mPa with described vacuum fluid injection machine, keep 45S, inject electrolyte 20.5g, charge into nitrogen then and recover straight atmospheric pressure, same station repeats 3 days, carry out then weigh the second time (78.5g), wherein obtaining electrolyte content is 19g, will mend into electrolyte 2g, vacuum-pumping and sealing, claim to such an extent that battery weight is 80g, the electrolyte total weight is 20.5g, injects the electrolyte rate each time to be: 92.7%.
Comparison example 2
Do not contain the battery of electrolyte and take by weighing weight W 1 (59.9g) according to embodiment 1 described preparation method's preparation, different is that the fluid injection mode is by existing electrolyte filling method, electrolyte is the electrolyte that described embodiment 1 makes, vacuumizing the injection electrolyte content is 21g, pressurization vacuumizes pressurization, wipe clean the electrolyte that spills, and battery is weighed as 77.2g, electrolyte content is 17.3g, enters to mend electrolyte 3g for the second time, vacuum-pumping and sealing is wiped clean and is claimed to such an extent that weight is 79.8g, the electrolyte total weight is 19.9g, finds that time of repose is long in this process, account for the time 70% of whole fluid injection flow process, the electrolyte absorptivity is for the first time: 86.9%.
The effect contrast:
Battery after the fluid injection among the embodiment 1 is changed into, and the cell voltage after changing into is not less than 3.33V, carries out Performance Detection then:
(1) discharge capacity test
With the battery that above-mentioned example 1 makes, use detecting box to carry out discharge test, test environment is 25 ℃, method for testing is as follows:
Current charges to voltage with 0.5C is 3.65V, left standstill 5 minutes, then with the 0.5C current discharge to 2.5V, the record gained discharge capacity of the cell.
(2) cycle performance test
Get the above-mentioned battery that makes, use detecting box to carry out the cycle performance test, test environment is 25 ℃, and relative humidity is 25%, and method of testing is as follows:
To 3.65V, it is 0.03C that constant voltage 3.65V charges to cut-off current, shelves 5 minutes with the electric current constant current charge of 0.5C, with the electric current constant current discharge of 0.5C to 2.5V, test obtains the initial discharge capacity of battery, finishes first loop test, repeats above test work step, record 50,100,200,300, discharge capacity after 400,500 circulations.Press column count worker formula then and calculate discharge capacitance:
Discharge capacitance=circulation back discharge capacity/initial discharge capacity * 100%
Test result such as table 1, shown in Figure 1.
Table 1
| The embodiment numbering | Embodiment 1 | Comparative Examples 1 |
| Discharge capacity (MAH) first | 3002 | 2989 |
| 50 circulation volume conservation rates (%) | 99.2 | 97.4 |
| 100 circulation volume conservation rates (%) | 98.3 | 96.6 |
| 200 circulation volume conservation rates (%) | 97.8 | 95.9 |
| 300 circulation volume conservation rates (%) | 97.3 | 94.9 |
| 400 circulation volume conservation rates (%) | 95.7 | 93.5 |
| 500 circulation volume conservation rates (%) | 94.8 | 91.6 |
From table 1 and Fig. 1 as can be seen, adopt electrolyte filling method of the present invention, the Capacity Ratio comparative example's 1 who discharges first on the embodiment discharge capacity first exceeds about 10mAh, also be not difficult to find out from the loop test data, adopt electrolyte filling method of the present invention, the battery cycle life performance specific absorption rate that the electrolyte absorptivity is high hangs down.
Claims (3)
1. the electrolyte filling method of a lithium battery, this method comprises the steps:
(1), lithium ion battery is inserted in the good fluid injection district of sealing;
(2), battery is weighed;
(3), battery port is installed priming device;
(4), battery is vacuumized, and keep certain hour;
(5), to injecting nonaqueous electrolytic solution behind the battery vacuum-pumping;
(6), battery is charged into nitrogen and recover atmospheric pressure;
(7), repeat battery vacuum-pumping is charged into nitrogen at same station;
(8), battery is discharged;
(9), battery is carried out weighing the second time;
(10), battery is replenished electrolyte;
(11), battery is sealed;
Charging into nitrogen recovery atmospheric pressure is 3-5 time, and described nitrogen must be dry gas; The air pressure that vacuumizes is 30mPa-60mPa, and the time is maintained 40-60s, and it is 1 standard atmospheric pressure that inflated with nitrogen recovers atmospheric pressure.
2. the electrolyte filling method of lithium battery according to claim 1 is characterized in that described electrolyte by electrolyte lithium salt and organic solvent and mixed.
3. the electrolyte filling method of lithium battery according to claim 1 is characterized in that electrolyte divides 2-5 time and divides equally injection.
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| CN2010102671873A CN101944585B (en) | 2010-08-23 | 2010-08-23 | Injection method for lithium battery |
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| CN2010102671873A CN101944585B (en) | 2010-08-23 | 2010-08-23 | Injection method for lithium battery |
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| CN101944585B true CN101944585B (en) | 2013-07-03 |
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| CN102122706B (en) * | 2011-01-28 | 2013-06-05 | 福建南平南孚电池有限公司 | Method for injecting electrolyte into housing of battery |
| CN102738438B (en) * | 2012-07-17 | 2014-08-27 | 宁波超霸能源有限公司 | Vacuum filling device of cylindrical lithium battery |
| CN103872381B (en) * | 2012-12-17 | 2015-12-09 | 北汽福田汽车股份有限公司 | A kind of fluid injection of electrokinetic cell leaves standstill method |
| CN104253262B (en) * | 2014-08-12 | 2016-09-14 | 中天储能科技有限公司 | A kind of electrolyte filling method of lithium ion battery |
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| CN109461877A (en) * | 2018-08-14 | 2019-03-12 | 银隆新能源股份有限公司 | Standing method and battery after a kind of battery liquid-filling |
| CN109273663A (en) * | 2018-11-21 | 2019-01-25 | 惠州亿纬锂能股份有限公司 | A kind of battery electrolyte injection method |
| CN109755654A (en) * | 2018-12-04 | 2019-05-14 | 惠州锂威新能源科技有限公司 | A kind of system and method for managing battery core standing time |
| CN109830755A (en) * | 2019-01-11 | 2019-05-31 | 深圳吉阳智能科技有限公司 | A kind of electrolyte wetting method for lithium battery |
| CN110160915A (en) * | 2019-05-22 | 2019-08-23 | 苏州宇量电池有限公司 | A kind of test method of battery electrolyte infiltration consistency |
| CN110661050B (en) * | 2019-09-27 | 2021-03-23 | 安徽益佳通电池有限公司 | Method for improving formation interface of lithium ion battery |
| CN110993881A (en) * | 2019-12-23 | 2020-04-10 | 天能电池(芜湖)有限公司 | Efficient acid adding process |
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