CN101170200A - Mixed non water electrolyte additive for improving battery high-temperature performance - Google Patents
Mixed non water electrolyte additive for improving battery high-temperature performance Download PDFInfo
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- CN101170200A CN101170200A CNA2007101503629A CN200710150362A CN101170200A CN 101170200 A CN101170200 A CN 101170200A CN A2007101503629 A CNA2007101503629 A CN A2007101503629A CN 200710150362 A CN200710150362 A CN 200710150362A CN 101170200 A CN101170200 A CN 101170200A
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Abstract
The invention relates to a mixed type non-water electrolytic solution additive used for improving high temperature performance of a cell, which is characterized in that the additive comprises mixture of 1-propenyl phosphonic cyclic acid anhydride, ethyl acetate, as well as vinyl enthylene elayl carbonic ester, and is dissolved in the non-water electrolytic solution; the ratio of addition of the 1-propenyl phosphonic cyclic acid anhydride and the weight share of the non-water electrolytic solution is 0.05-5.0:100; the ratio of weight shares of the ethyl acetate and the non-water electrolytic solution is 0.05-5.0:100; the ratio of addition of the vinyl enthylene elayl carbonic ester and the non-water electrolytic solution is 0.05-5.0:100. The 1-propenyl phosphonic cyclic acid anhydride in the component of the invention can effectively inhibit expansion in the process of high-temperature storage and circulation through inhibit CO2 generated effect; at the same time, the vinyl enthylene elayl carbonic ester can improve the cell capacity under the conditions of high-temperature storage and circulation through effectively protecting SEI membrane. The addition agent can effectively improve the cell performance on high-temperature storage and high-temperature circulation, as well as make the cell maintain good low-temperature electric discharge characteristic.
Description
Technical field
The present invention relates to a kind of nonaqueous electrolytic solution additive package, particularly a kind of mixed non water electrolyte additive that is used to improve battery high-temperature behavior.
Background technology
Nonaqueous electrolytic solution is as the carrier of ion motion in the lithium ion battery, its composition is basicly stable, be mainly EC, PC, EMC, DEC etc., continuous popularization along with battery applications, for the Study on Additive that satisfies the different performance requirement gets more and more, the additive that wherein especially is used for improving cell safety characteristic aspect is in the majority, as prevent over-charging of battery additive, prevent that additive that the hot case of battery lost efficacy or the like from having made huge contribution for the security performance that improves lithium battery.In recent years, along with people deepen continuously to the understanding of battery service condition, find that the use of battery under a lot of situations all is being higher than under the condition of normal temperature, when moving as cells in notebook computer, battery can generate heat, about about 45 ℃ of its temperature; When MP3, MP4 play for a long time, the temperature of battery can rise to about 40 ℃; Mobile phone is in charging process, and the temperature of battery also can be near 40 ℃; The GPS battery is more arranged, because long term exposure in the sun, temperature tends to reach about 80 ℃ or the like, make battery consumer and manufacturing commercial city cause attention at the electrical property under the hot conditions to improving battery, a lot of battery manufacturers have all been carried out the test of aspects such as high-temperature storage performance and high temperature cyclic performance to battery, and improve to a certain extent.Yet many electrolyte improve prescription often all starts with from the solvent of electrolyte, has improved high-temperature behavior, has but lost cryogenic property, still can not satisfy the demand that battery is used well.Therefore, set about, improve the battery high-temperature characteristic, become one of present important topic of improving the battery high-temperature characteristic from additive.
Summary of the invention
The objective of the invention is to overcome the deficiency of above-mentioned technology, a kind of mixed non water electrolyte additive that is used to improve battery high-temperature behavior is provided.
The technical solution adopted in the present invention is for achieving the above object: a kind of mixed non water electrolyte additive that is used to improve battery high-temperature behavior is characterized in that (Vinylethylene carbonate, molecular formula is C by 1-propylene phosphonic acid cyclic acid anhydrides
5H
6O
3, be called for short VEC), (1-propanephosphonic acid cyclic anhydride, molecular formula is C for ethyl acetate and vinyl ethylidene carbonic ester
9H
21O
6P
3, be called for short PPACA) mix and form, and be dissolved in the nonaqueous electrolytic solution; Described 1-propylene phosphonic acid cyclic acid anhydrides addition is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100; Described ethyl acetate is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100; Described vinyl ethylidene carbonic ester addition is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100.
The nonaqueous electrolytic solution that the present invention uses mainly is made up of methyl ethyl carbonate (EMC), vinyl carbonate (EC) and propylene carbonate (PC), prescription is in detail: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute is LiPF6, concentration is 1mol/l, universal additive is 3 part 1,3-N-morpholinopropanesulfonic acid lactone (PS), 1 part of vinylene carbonate (VC), they form nonaqueous electrolytic solution stoste jointly.Additive of the present invention is PPACA, ethyl acetate and VEC, and the ratio of weight and number of its relative nonaqueous electrolytic solution all is that 0.05-5 part is not waited, and joins in the nonaqueous electrolytic solution according to described ratio, is made into the electrolyte of battery.The positive electrode of battery is a cobalt acid lithium, and negative material is a modified graphite, and barrier film is a Celgard 20um barrier film, and lug is the wide lug of the 3mm of Sumitomo Electric Industries, is packaged as plastic-aluminum encapsulation bag.According to the manufacture craft of polymer battery, be assembled into battery 032220, do performance test.
The invention has the beneficial effects as follows: the 1-propylene phosphonic acid cyclic acid anhydrides in this additive can be by suppressing CO
2The effect that generates effectively suppresses the expansion of battery in high temperature storage and cyclic process; Vinyl ethylidene carbonic ester can improve the capacity of battery under high temperature storage and cycling condition by effective protection SEI film simultaneously.The present invention by a large amount of experiments, develops a kind of functional additive package that can effectively improve battery high-temperature storage and cycle performance just from starting with in this respect, has both effectively guaranteed the high-temperature behavior of battery, has effectively guaranteed the cryogenic property of battery again; Its reasonable mixture ratio, preparation is simple, and effect is remarkable, is widely used, and can well satisfy the demand of consumer to battery performance.
Embodiment
Below in conjunction with preferred embodiment, to details are as follows according to embodiment provided by the invention:
A kind of mixed non water electrolyte additive that is used to improve battery high-temperature behavior is characterized in that being made up of 1-propylene phosphonic acid cyclic acid anhydrides, ethyl acetate and the mixing of vinyl ethylidene carbonic ester, and is dissolved in the nonaqueous electrolytic solution; Described 1-propylene phosphonic acid cyclic acid anhydrides addition is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100; Described ethyl acetate is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100; Described vinyl ethylidene carbonic ester addition is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100.
The used non-aqueous solvent electrolyte additive package of the present invention is mainly mixed by PPACA and VEC to be formed.They can be used in combination in described ratio according to the demand of battery performance.It is to be noted especially that wherein PPACA generally can not individualism, and its cosolvent kind also seldom, therefore use ethyl acetate as its cosolvent, add by 1: 1 weight ratio with PPACA, when promptly in electrolyte, adding this additive, also add ethyl acetate simultaneously.
At battery performance, do following comparative example and embodiment experiment, comparative analysis nonaqueous electrolytic solution additive package is to the influence of battery high-temperature storage and cycle performance:
Comparative example 1
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC.
Embodiment 1
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC forms universal additive.Then to wherein adding 0.5 part of VEC and respectively being 0.1 part PPACA and ethyl acetate.
Embodiment 2
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC forms universal additive.Then to wherein adding 1.0 parts of VEC and respectively being 0.1 part PPACA and ethyl acetate.
Embodiment 3
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC forms universal additive.Then to wherein adding 1.0 parts of VEC and respectively being 0.2 part PPACA and ethyl acetate.
Embodiment 4
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC forms universal additive.Then to wherein adding 2.0 parts of VEC and respectively being 0.4 part PPACA and ethyl acetate.
Embodiment 5
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC forms universal additive.Then to wherein adding 2.0 parts of VEC and respectively being 0.8 part PPACA and ethyl acetate.
Embodiment 6
Nonaqueous electrolytic solution is formed: EMC/EC/PC=55: 40: 5 (ratio of weight and number), solute are LiPF6, and concentration is 1mol/L.In the nonaqueous electrolytic solution of 100 parts of weight, add 3 parts of PS, 1 part of VC forms universal additive.Then to wherein adding 3.0 parts of VEC and respectively being 3.0 parts PPACA and ethyl acetate.
Use comparative example 1 respectively, the electrolyte of embodiment 1-6 is made into 032220 battery, and its lowest capacity is 95mAh, investigates the influence of electrolysis additive to battery high-temperature storage, high temperature circulation and cryogenic discharging characteristic.
Charge condition: the 0.5C constant current charge is to 4.2V, and constant voltage charge is to 5mAh.
Dormancy: 10 minutes.
The discharge standard: the 0.5C constant-current discharge is to 3.0V.
85 ℃ of I high temperature, the test of 4h memory property
Battery after comparative example 1, embodiment 1-6 experiment test adopt reprocessing intact.Fill/put once electricity earlier, record discharge capacity of the cell, and be full of electricity is put into battery in 85 ℃ the baking oven then, deposit 4 hours after, hot test battery thickness; After the storage at room temperature 2 hours, the thickness of test battery and internal resistance; Discharge and recharge with 0.5C, do 4 times then and charge and discharge, get that discharge capacity is as the recovery capacity for the third time, detailed data sees Table 1.
Comparative example 1, after 85 ℃ of embodiment 1-6 high temperature, the 4h storage, under the hot condition, with the gas in the needle tubing extraction battery, the composition and the relative amount of utilization gas chromatograph GC analytical gas, detailed data is as shown in table 2.Wherein the gas chromatograph model is GC6890N-MS5973N, and chromatogram is the GS-GASPRO post mutually.
45 ℃ of cycle performance tests of II high temperature
Battery after comparative example 1, the battery that embodiment 1-6 uses finish as reprocessing is full of electricity afterwards initial internal resistance, the thickness of test battery.Then, battery is carried out 45 ℃ of cycle performance tests, circulation ratio is that 0.5C charges and discharge, the variation of thickness, internal resistance and the capacity of wherein per 100 measurement batteries in cyclic process.Detailed data is as shown in table 3.
The test of III temperature discharge performance
Comparative example 1, embodiment 1-6 adopt is battery after the reprocessing.Under the normal temperature condition, battery is full of electricity after, be placed on the temperature environment that needs discharge and keep after 3 hours battery being discharged the capacity of record battery.Charge and discharge/discharging current is 0.5C, main investigate add the nonaqueous electrolytic solution additive package after, whether the cryogenic property of battery can remain unchanged.Detailed data is as shown in table 4.
Temperature is respectively-10 ℃, and 0 ℃, 25 ℃, 60 ℃.
85 ℃ of 4h memory property tests of table 1 high temperature
The test of 85 ℃ of 4h storages of table 2 high temperature gas componant
45 ℃ of cycle performance tests of table 3 high temperature
The test of table 4 temperature discharge performance
As can be seen from Table 1, embodiment 1 compares with 2, and VEC content increases, and residue and recovery capacity after latter's storage in 85 ℃/4 hours all are higher than the former by a relatively large margin, show that the adding of VEC can improve remaining battery and recovery capacity; Embodiment 2 compares with 3, after the storage in 85 ℃/4 hours, the thickness swelling of latter's battery obviously descends, proof PPACA content increases, expanded thickness in the time of can reducing the battery high-temperature storage, simultaneously, the latter is with respect to the relative reduction with the recovery capacity of the former residue, prove the increase of PPACA content, can reduce the residue and the recovery capacity of battery under the high temperature storage condition.Comparative example 1, with respect to embodiment 1-6, after the storage in 85 ℃/4 hours, the latter's thickness swelling is all much smaller, further proves the adding of PPACA and contain to measure increase, can effectively suppress the expansion of battery under the high temperature storage condition.Comparative example 1, for embodiment 1-4, after the storage in 85 ℃/4 hours, the latter's recovery capacity and residual capacity all are higher than the former, the expansion ratio all is lower than the former, the mixed solvent concentration of prove out both can improve residue and the recovery capacity of battery under the high temperature storage condition, can effectively suppress the thickness swelling of battery under the high temperature storage condition again.Comparative example 1, for embodiment 5-6, after the storage in 85 ℃/4 hours, the residue of latter's battery is relative with the recovery capacity, and the former decreases, but thickness swelling is still less, still can effectively suppress the expansion of thickness under the battery high-temperature storage condition though prove excessive PPACA, can reduce the residue and the recovery capacity of battery to a certain extent.
As can be seen from Table 2, comparative example 1 is compared with embodiment 1-6, and latter's aerogenesis is less than the former, shows as the CO that air-blowing produces
2Content reduces, and proves that PPACA can effectively suppress CO under the high temperature storage condition
2Generation, simultaneously because the increase of PPACA content, CO
2Reduce gradually, show that within the specific limits PPACA content is many more, can effectively suppress CO under the high temperature storage condition more
2Generation, protection SEI film, thus reach the purpose that effective inhibition cell thickness expands.Embodiment 1 compares with 2, along with VEC content increases, and latter CO
2Content does not obviously reduce, and proves that VEC can not effectively suppress the CO under the high temperature storage condition
2Generate, simultaneously to suppressing not contribution of thickness swelling.Embodiment 2 compares with 3, and PPACA content increases, latter CO
2Content obviously reduces, and proves that PPACA can effectively suppress CO under the high temperature storage condition
2Generation.
As can be seen from Table 3, embodiment 1 compares with 2, and VEC content increases, and the former increases the residual capacity in 45 ℃ of cyclic processes of the latter to some extent relatively, shows that VEC can improve the circulation volume in the battery high-temperature cyclic process.Embodiment 2 compares with 3, and the thickness swelling in 45 ℃ of cyclic processes of the latter is starkly lower than the former, proves that the increase of PPACA content can effectively reduce the thickness swelling of battery in the high temperature circulation process.Comparative example 1, with respect to embodiment 1-6, the thickness swelling of battery all will prove that further PPACA can effectively reduce the thickness swelling of battery under the high temperature circulation condition far below the former in 45 ℃ of cyclic processes of the latter; Comparative example 1, for embodiment 1-4, the capacity of battery all is higher than the former in 45 ℃ of cyclic processes of the latter, thickness swelling is lower than the former, the further capacity of proof VEC when adding the high temperature circulation that can improve battery, PPACA can effectively reduce the thickness swelling of battery high-temperature circulation time, under suitable mixed solvent proportioning, can obtain high power capacity and low expansion character simultaneously; For embodiment 5-6, the latter's circulation volume shows as not as the former, and thickness swelling still can reduce the thickness swelling of battery in the high temperature circulation process though prove excessive PPACA, but can reduce the circulation volume of battery less than the former.
As can be seen from Table 4, comparative example 1 is compared with embodiment 1-6, and both 0 ℃ and-10 ℃ of low temperature performances are basic identical; 60 ℃ of discharge performances, latter embodiment 1-4 omits, but difference is very little, and 5-6 is almost identical with comparative example 1; Therefore, total relatively, the adding of PPACA and VEC does not have influence substantially to low temperature performance.
The analysis showed that from comparative example 1 and embodiment 1-6 PPACA and VEC play a different role respectively in the additive package.The former can reduce the thickness swelling when battery uses under the hot conditions, and content is many more within the specific limits, and the cell thickness expansion is more little, but the adding of PPACA simultaneously and content increase the capacity in the time of can reducing the battery use; Capacity when the latter can improve battery under the hot conditions and uses, within the specific limits, content is many more, and effect is obvious more, but does not excessively just have an effect; Therefore, the mixing of this additive is used, and can effectively solve the demand of and the high power capacity low to thickness swelling in the use of current battery high temperature, can also be by the adjustment of additive package proportioning being satisfied the specific (special) requirements of single money battery.
Above-mentioned detailed description of this mixed non water electrolyte additive that is used to improve battery high-temperature behavior being carried out with reference to embodiment; be illustrative rather than determinate; can list several embodiment according to institute's limited range; therefore in the variation and the modification that do not break away under the general plotting of the present invention, should belong within protection scope of the present invention.
Claims (1)
1. a mixed non water electrolyte additive that is used to improve battery high-temperature behavior is characterized in that being made up of 1-propylene phosphonic acid cyclic acid anhydrides, ethyl acetate and the mixing of vinyl ethylidene carbonic ester, and is dissolved in the nonaqueous electrolytic solution; Described 1-propylene phosphonic acid cyclic acid anhydrides addition is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100; Described ethyl acetate is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100; Described vinyl ethylidene carbonic ester addition is 0.05-5.0 with nonaqueous electrolytic solution ratio by weight: 100.
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|---|---|---|---|
| CN2007101503629A CN101170200B (en) | 2007-11-23 | 2007-11-23 | Mixed non water electrolyte additive for improving lithium battery high-temperature performance |
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| CN2007101503629A CN101170200B (en) | 2007-11-23 | 2007-11-23 | Mixed non water electrolyte additive for improving lithium battery high-temperature performance |
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| CN101170200B CN101170200B (en) | 2012-02-22 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101593851B (en) * | 2008-05-29 | 2012-05-23 | 比亚迪股份有限公司 | Additive composition, electrolyte containing same and lithium ion secondary battery |
| CN104332653A (en) * | 2014-09-01 | 2015-02-04 | 东莞新能源科技有限公司 | Non-aqueous electrolyte and lithium ion battery using the same |
-
2007
- 2007-11-23 CN CN2007101503629A patent/CN101170200B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101593851B (en) * | 2008-05-29 | 2012-05-23 | 比亚迪股份有限公司 | Additive composition, electrolyte containing same and lithium ion secondary battery |
| CN104332653A (en) * | 2014-09-01 | 2015-02-04 | 东莞新能源科技有限公司 | Non-aqueous electrolyte and lithium ion battery using the same |
| CN104332653B (en) * | 2014-09-01 | 2017-03-01 | 东莞新能源科技有限公司 | A kind of nonaqueous electrolytic solution and the lithium ion battery using this electrolyte |
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|---|---|
| CN101170200B (en) | 2012-02-22 |
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