CN104701571B - A kind of lithium ion battery high-temperature-resistant high-pressure-resistant electrolyte - Google Patents

A kind of lithium ion battery high-temperature-resistant high-pressure-resistant electrolyte Download PDF

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CN104701571B
CN104701571B CN201510143570.0A CN201510143570A CN104701571B CN 104701571 B CN104701571 B CN 104701571B CN 201510143570 A CN201510143570 A CN 201510143570A CN 104701571 B CN104701571 B CN 104701571B
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lithium
electrolyte
ion battery
lithium ion
additive
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CN104701571A (en
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闫春凤
许莹
夏建荣
黄当睦
刘新平
祖利洲
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Fujian Institute of Research on the Structure of Matter of CAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
    • H01M10/0566—Liquid materials
    • H01M10/0567—Liquid materials characterised by the additives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
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  • Condensed Matter Physics & Semiconductors (AREA)
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  • Inorganic Chemistry (AREA)
  • Secondary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The present invention relates to a kind of electrolyte for lithium ion battery, described electrolyte contains lithium salts, organic solvent and additive, and the additive is boric acid three (trimethylsilyl) ester.The electrolyte is applied in lithium ion battery, its operating voltage is 4.5~4.7V, and operating temperature range is room temperature~60 DEG C, has good high-temperature-resistant high-pressure-resistant cycle performance, is a HTHP functional form nonaqueous electrolytic solution simple and easy to get.

Description

A kind of lithium ion battery high-temperature-resistant high-pressure-resistant electrolyte
Technical field
The invention belongs to lithium-ion battery electrolytes technical field, and in particular to a kind of resistance to height of lithium ion battery high temperature resistant Mobyneb electrolyte is pressed, the high temperature high voltage resistant cycle performance suitable for improving lithium ion battery.
Background technology
Lithium ion battery produces because energy density is big, voltage platform is high, long lifespan and the advantages that environmental protection in electronic energy The fields such as product, electric tool and electric automobile have a wide range of applications.In recent years, due to intelligent, mobile and high power consumption The development of electronic equipment, people require to improve the energy density of lithium ion battery, the current work for improving lithium ion battery in a hurry Magnitude of voltage is considered as a kind of effective way for improving its energy density.Can be under higher temperature environment efficiently in addition, obtaining The lithium ion battery of work is also one of the important research content in the field.
The operating voltage of lithium ion battery is determined by the positive electrode of battery, has been obtained operating voltage in the market and has been existed 4.35-5.0V high-voltage anode material；But existing carbonate group electrolyte can not meet the lithium ion battery under this high voltage Charge-discharge power demand, therefore, the performance of existing carbonate group electrolyte is lifted, develop the high voltage matched with high-voltage anode material Type electrolyte is one of key issue in the urgent need to address.In addition, lithium ion battery applications temperature is narrower, generally 55 DEG C with Upper battery capacity decay is quickly, in some instances it may even be possible to burning and blast occurs, which limit its application, therefore studies lithium ion The high-temperature behavior of battery equally has great importance.
It is to improve battery work by adding a variety of additives acted on different efficacies into lithium-ion battery electrolytes Make one of important means of efficiency, particularly add additive some while that there are multiple functions, such as with being lifted simultaneously The additive of high temperature resistant and high voltage performance.
Solid State Ionics, Vol.263, P.146, higher operating voltage, the document are reported in (2014) It is middle using dioxalic acid lithium borate (LiBOB) and difluorine oxalic acid boracic acid lithium (LiDFOB) as additive application in LiCo1/3Ni1/3Mn1/ 3O2In battery, the heat endurance of electrode material can be improved under the conditions of normal temperature 3.0-4.6V operating voltages, is followed for 60 times by 0.6C After ring, battery capacity still keeps 88.2% and 91.8%.Electrochemical and Solid-State Letters, Vol.10, P.A45 (2007) report improves MCMB/LiCo using additive1/3Ni1/3Mn1/3O2Service behaviour under battery high-temperature Work, such battery is improved under 3.0-4.0V scopes as additive by using difluorine oxalic acid boracic acid lithium (LiDFOB) Cycle performance during 55 DEG C of 0.5C, only 6% capacitance loss after 100 circulations.Journal of Power Sources Vol.268, P.37, in (2014) will difluorine oxalic acid boracic acid lithium (LiDFOB) be used as additive, LiCo can be improved1/3Ni1/ 3Mn1/3O2The electrolyte stability of-graphite cell at 60 DEG C, there is preferable capability retention, after 100 circulations, battery Capacity still keeps 60%.Journal of Power Sources Vol.208, P.67, by methylene ethylene carbonate in (2012) After ester (MEC) is used as additive, LiCo can be made1/3Ni1/3Mn1/3O2(NMC)/graphite soft-package battery is under 55 DEG C and 3.0-4.2V Cycle performance with brilliance.South China Normal University was once used for LiCo using (trimethylsilyl) ester of boric acid three as additive1/ 3Ni1/3Mn1/3O2In/graphite cell, the battery cycle performance of operating voltage in 3.0-4.2V at 60 DEG C can be improved, is passed through After 270 circulations, battery capacity still keeps~80%.
The progress in terms of Li-Co-Ni-Mn series lithium ion batteries high temperature resistant and high voltage performance is at present：In room The lower maximum operating voltage of temperature reaches 4.6V, and maximum operating voltage reaches 4.2V at 60 DEG C.Patent CN1840550A is pointed out boron Sour three (trimethylsilyl) esters can suppress the internal resistance of cell as additive application into lithium battery to be increased and can suppress battery appearance The reduction of amount.Shanghai Communications University's correlative study group report applies boric acid three (trimethylsilyl) ester in LiFePO4/Li (2.5-4.2V) and LiMn2O4In/Li (3.0-4.5V) battery, this two classes battery following under 55 DEG C of operating temperatures can be improved Ring performance (Journal of Power Sources Vol.202, P.341, (2012)；Journal of Power Sources Vol.221,P.90,(2013)。
The content of the invention
It is an object of the invention to relatively low for current lithium-ion battery electrolytes operating voltage, Applicable temperature scope compared with It is narrow, a kind of non-aqueous electrolyte for lithium ion cell with high-temperature-resistant high-pressure-resistant Mobyneb is proposed hereby.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of electrolyte for lithium ion battery, described electrolyte contain lithium salts, organic solvent and additive, the addition Agent is boric acid three (trimethylsilyl) ester.
According to the present invention, the lithium ion battery is Li-Co-Ni-Mn systems, preferably LiCo1/3Ni1/3Mn1/3O2Type.
According to the present invention, the additive can make lithium ion battery high temperature resistant and high pressure resistant.The electrolyte can be Used under HTHP, its operating temperature can be from room temperature to 60 DEG C, and operating voltage can be from 4.5V to 4.7V.Preferably, 1C 100 Capacity is more than or equal to 75% after secondary circulation.
According to the present invention, wherein the boric acid three (trimethylsilyl) ester accounts for 0.1~5wt% of electrolyte gross mass.
According to the present invention, described organic solvent is linear carbonate or cyclic carbonate, preferably ethylene carbonate (EC), propene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), methyl ethyl carbonate Any one or more in ester (DMC), dimethoxy-ethane (DME), two or three in preferably above-mentioned organic solvent.It is excellent Choosing, the organic solvent accounts for 10~90wt% of lithium-ion battery electrolytes gross mass.
According to the present invention, the lithium salts in the electrolyte is lithium hexafluoro phosphate (LiPF6), LiBF4 (LiBF4), it is double Lithium bis (oxalate) borate (LiBOB), difluorine oxalic acid boracic acid lithium (LiODFB), lithium perchlorate (LiClO4) in one or more.It is preferred that , the amount total concentration of the material of the lithium salts in the electrolytic solution is 0.8~1.4molL-1.
The present invention also provides a kind of method for preparing the lithium-ion battery electrolytes, including：By organic solvent, lithium salts and Additive boric acid three (trimethylsilyl) ester is mixed.
Present invention also offers a kind of purposes of above-mentioned lithium-ion battery electrolytes, it is used for lithium ion battery.Particularly, For making lithium-ion electric pool high temperature resistant and high pressure resistant.
According to the present invention, the lithium ion battery is Li-Co-Ni-Mn systems, preferably LiCo1/3Ni1/3Mn1/3O2Type.
Further, present invention also offers a kind of lithium ion battery, it includes positive plate, negative plate, barrier film, and Electrolyte, wherein, the electrolyte is lithium-ion battery electrolytes of the present invention.
According to the present invention, the lithium ion battery is Li-Co-Ni-Mn systems, preferably LiCo1/3Ni1/3Mn1/3O2Type.
The present invention using boric acid three (trimethylsilyl) ester as additive application in Organic Electrolyte Solutions for Li-Ion Batteries, by It can suppress the decomposition of solvent with the lithium salts anion binding in electrolyte in boric acid three (trimethylsilyl) ester and improve interface resistance It is anti-, cycle performance of the lithium ion battery under high voltage (4.5~4.7V) can be improved.Boric acid three (trimethylsilyl) ester simultaneously The heat endurance of lithium salts in electrolyte can be improved, further improves the high-temperature behavior of lithium ion battery.Just because of basic electricity Solve the cooperation synergy of liquid and additive so that lithium ion battery has preferable chemical property.
The beneficial effects of the present invention are：
1. boric acid three (trimethylsilyl) ester is used as improving lithium-ion electric pool high temperature resistant and Nai Gao simultaneously first by the present invention The Mobyneb electrolysis additive of voltage performance, make lithium ion battery when maximum operating temperature reaches 60 DEG C, highest work Voltage reaches 4.7V, and after 100 circulations, battery can be remained above or the capacity equal to 70%, less adds the addition Such battery of agent cycle life under the conditions of identical operating temperature and operating voltage improves a lot.
2. the material of the present invention is easy to get, preparation technology is simple, easy to implement.
Brief description of the drawings
Fig. 1 is the LiCo of embodiment 11/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.5V Capacitance conservation rate figure (room temperature).
Fig. 2 is the LiCo of comparative example 11/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.5V Capacitance conservation rate figure (room temperature).
Fig. 3 is the LiCo of embodiment 21/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.6V Capacitance conservation rate figure (room temperature).
Fig. 4 is the LiCo of comparative example 21/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.6V Capacitance conservation rate figure (room temperature).
Fig. 5 is the LiCo of embodiment 31/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.7V Capacitance conservation rate figure (room temperature).
Fig. 6 is the LiCo of comparative example 31/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.7V Capacitance conservation rate figure (room temperature).
Fig. 7 is the LiCo of embodiment 41/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.6V Capacitance conservation rate figure (55 DEG C).
Fig. 8 is the LiCo of comparative example 41/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.6V Capacitance conservation rate figure (55 DEG C).
Fig. 9 is the LiCo of embodiment 51/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is putting for 3.0-4.7V Capacitance conservation rate figure (60 DEG C).
Figure 10 is the LiCo of comparative example 51/3Ni1/3Mn1/3O2/ Li lithium ion batteries discharge voltage range is 3.0-4.7V's Discharge capacitance figure (60 DEG C).
Embodiment
The present invention is described in detail by following embodiments.But skilled in the art realises that following embodiments are not Limiting the scope of the invention.Any improvement and change made on the basis of the present invention, all the protection model in the present invention Within enclosing.
In the specific comparative example and embodiment of the present invention, organic solvent selection ethylene carbonate (EC), dimethyl carbonate (DMC) two kinds, the mass ratio of two kinds of solvents is EC:DMC=1:1.
Conventional button cell manufacture craft, by mixing LiCo1/3Ni1/3Mn1/3O2Powder (80 weight %), carbon black (10 Weight %), polyvinylidene fluoride (the weight % of PVDF 10) and 1-METHYLPYRROLIDONE (NMP) anode sizing agent is made, by mixing slurry Hand coatings are expected on the aluminium flake of the 16mm sizes cut out, and 12 hours pole pieces for being made dry are dried at 120 DEG C.At room temperature The pole piece of above-mentioned drying is compacted with infrared tablet press machine again.(the moisture in the glove box full of argon gas<1ppm, oxygen<1ppm), Above-mentioned 16mm pole piece, barrier film, lithium piece, both positive and negative polarity shell are assembled into 2025 type button cells.
The electrolyte prepared as follows is added in button cell.
Electrolyte composition is as follows：
Embodiment：Lithium salts LiPF6Concentration 1.0molL-1, organic solvent EC:DMC=1:1 (mass ratio), additive boric acid Three (trimethylsilyl) esters, it accounts for the 1% of electrolyte gross mass；It is defined as ref+1%TMSB；
Comparative example：Lithium salts LiPF6Concentration 1.0molL-1, organic solvent EC:DMC=1:1 (mass ratio), is defined as ref。
(1) normal-temperature circulating performance is evaluated
Embodiment 1：
The present embodiment adds boric acid three (trimethylsilyl) ester.Electrolyte composition is ref+1%TMSB.By above-mentioned preparation Electrolyte is added in button cell.
Battery carries out cycle performance test according to following flow, as a result such as Fig. 1.
0.2C constant-current charges 0.2C constant-current discharges to 3.0V, circulate 3 weeks, 0.5C constant-current charges to 4.5V, 0.5C to 4.5V Constant-current discharge is circulated 3 weeks, 1C constant-current charges to 4.5V, 1C constant-current discharges to 4.5V, circulated 150 weeks to 4.5V.
Comparative example 1：
Electrolyte composition is ref.The electrolyte of above-mentioned preparation is added in button cell.
Battery carries out cycle performance test according to the flow of above-described embodiment 1：As a result such as Fig. 2.
Embodiment 2：
The present embodiment adds boric acid three (trimethylsilyl) ester.Electrolyte composition is ref+1%TMSB.By above-mentioned preparation Electrolyte is added in button cell.
Battery carries out cycle performance test according to following flow, as a result such as Fig. 3.
0.2C constant-current charges 0.2C constant-current discharges to 3.0V, circulate 3 weeks, 0.5C constant-current charges to 4.6V, 0.5C to 4.6V Constant-current discharge is circulated 3 weeks, 1C constant-current charges to 4.6V, 1C constant-current discharges to 4.6V, circulated 150 weeks to 4.6V.
Comparative example 2：
Electrolyte composition is ref, and the electrolyte of above-mentioned preparation is added in button cell.
Battery carries out cycle performance test according to the flow of above-described embodiment 2：As a result such as Fig. 4.
Embodiment 3：
The present embodiment adds boric acid three (trimethylsilyl) ester.Electrolyte composition is ref+1%TMSB.By above-mentioned preparation Electrolyte is added in button cell.
Battery carries out cycle performance test according to following flow, as a result such as Fig. 5.
0.2C constant-current charges 0.2C constant-current discharges to 3.0V, circulate 3 weeks, 0.5C constant-current charges to 4.7V, 0.5C to 4.7V Constant-current discharge is circulated 3 weeks, 1C constant-current charges to 4.7V, 1C constant-current discharges to 4.7V, circulated 100 weeks to 4.7V.
Comparative example 3：
Electrolyte composition is ref, and the electrolyte of above-mentioned preparation is added in button cell.
Battery carries out cycle performance test according to the flow of above-described embodiment 3, as a result such as Fig. 6.
(2) high temperature cyclic performance is evaluated
Embodiment 4：
The present embodiment adds boric acid three (trimethylsilyl) ester.Electrolyte composition is ref+1%TMSB.By above-mentioned preparation Electrolyte is added in button cell.
Battery carries out cycle performance test according to following flow：As a result such as Fig. 7.
Battery is shelved in insulating box, it is 55 DEG C to control temperature, shelves time 240min.0.2C constant-current charges are extremely 4.6V, 0.2C constant-current discharge circulate 3 weeks, 0.5C constant-current charges to 4.6V, 0.5C constant-current discharges to 4.6V, circulation 3 to 3.0V In week, 1C constant-current charges to 4.6V, 1C constant-current discharges to 4.6V, circulate 100 weeks.
Comparative example 4：
Electrolyte composition is ref.The electrolyte of above-mentioned preparation is added in button cell.
Battery carries out cycle performance test according to the flow of above-described embodiment 4：As a result such as Fig. 8.
Embodiment 5：
The present embodiment adds boric acid three (trimethylsilyl) ester.Electrolyte composition is ref+1%TMSB.By above-mentioned preparation Electrolyte is added in button cell.
Battery carries out cycle performance test according to following flows：As a result such as Fig. 9.
Battery is shelved in insulating box, it is 60 DEG C to control temperature, shelves time 240min.0.2C constant-current charges are extremely 4.7V, 0.2C constant-current discharge circulate 3 weeks, 0.5C constant-current charges to 4.7V, 0.5C constant-current discharges to 4.7V, circulation 3 to 3.0V In week, 1C constant-current charges to 4.6V, 1C constant-current discharges to 4.7V, circulate 100 weeks.
Comparative example 5：
Electrolyte composition is ref.The electrolyte of above-mentioned preparation is added in button cell.
Battery carries out cycle performance test according to the flow of above-described embodiment 5：As a result such as Figure 10.
During 1~10 result with reference to the accompanying drawings, normal temperature and high temperature cyclic performance are evaluated, from comparative example compared with embodiment, In above-mentioned 1C tests, comparative example 1-5 battery capacity decay is rapid, and especially voltage increases to 4.7V from 4.5V, and capacity declines Subtract degree progressively to increase.And the battery capacity decay that with the addition of boric acid three (trimethylsilyl) ester is slow, as embodiment 1-5 ought be incited somebody to action Temperature from normal temperature be added to 55 DEG C when, high pressure 4.6V test show, the cycle life of embodiment 4 has clear improvement compared with comparative example 4.Again Temperature and pressure is improved to 60 DEG C simultaneously, during 3.0-4.7V, the cycle life of embodiment 5 (76.3%) is compared with comparative example 5 (52.5%) greatly improve.Illustrate that additive boric acid three (trimethylsilyl) ester is added in electrolyte to be advantageous to improve battery Active material stability, electrolyte side reaction is reduced, improve LiCo1/3Ni1/3Mn1/3O2/ Li batteries are in wide temperature range and height Cycle performance under voltage.
In a word, from the test result of above example, it can be seen that (trimethylsilyl) ester of boric acid three has as additive Beneficial to raising LiCo1/3Ni1/3Mn1/3O2Cycle of higher pressure performance under the wide temperature range of/Li batteries.
The foregoing is only presently preferred embodiments of the present invention, all equivalent variations done according to scope of the present invention patent with Modification, it should all belong to the covering scope of the present invention.

Claims (6)

1. a kind of lithium-ion battery electrolytes are used to make LiCo1/3Ni1/3Mn1/3O2Type lithium-ion electric pool high temperature resistant and high voltage bearing use On the way, described electrolyte contains lithium salts, organic solvent and additive, and the additive is boric acid three (trimethylsilyl) ester, institute The 1wt% that boric acid three (trimethylsilyl) ester accounts for electrolyte gross mass is stated, described organic solvent is ethylene carbonate（EC）And carbon Dimethyl phthalate（DMC）, the maximum operating temperature of the lithium ion battery reaches 60 DEG C, and maximum operating voltage reaches 4.7 V, described Capacity is more than or equal to 70% after 100 circulations of lithium ion battery 1C.
2. purposes according to claim 1, wherein, the lithium salts in the electrolyte is lithium hexafluoro phosphate（LiPF6）, tetrafluoro Lithium borate（LiBF4）, di-oxalate lithium borate（LiBOB）, difluorine oxalic acid boracic acid lithium（LiODFB）, lithium perchlorate (LiClO4) in It is one or more.
3. purposes according to claim 2, wherein, the amount total concentration of the material of the lithium salts in the electrolytic solution for 0.8 ~ 1.4 mol·L-1。
A kind of 4. LiCo1/3Ni1/3Mn1/3O2Type lithium ion battery, including positive plate, negative plate, barrier film, and electrolyte, its In, the electrolyte contains lithium salts, organic solvent and additive, and the additive is boric acid three (trimethylsilyl) ester, described Boric acid three (trimethylsilyl) ester accounts for the 1wt% of electrolyte gross mass, and described organic solvent is ethylene carbonate（EC）And carbonic acid Dimethyl ester（DMC）, the maximum operating temperature of the lithium ion battery reaches 60 DEG C, and maximum operating voltage reaches 4.7 V, the lithium Capacity is more than or equal to 70% after 100 circulations of ion battery 1C.
5. lithium ion battery according to claim 4, wherein, the lithium salts in the electrolyte is lithium hexafluoro phosphate （LiPF6）, LiBF4（LiBF4）, di-oxalate lithium borate（LiBOB）, difluorine oxalic acid boracic acid lithium（LiODFB）, lithium perchlorate (LiClO4) in one or more.
6. lithium ion battery according to claim 5, wherein, the amount total concentration of the material of the lithium salts in the electrolytic solution is 0.8~1.4 mol·L-1。
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CN101188313A (en) * 2006-11-20 2008-05-28 三星Sdi株式会社 Electrolyte for rechargeable lithium battery, and rechargeable lithium battery including same

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Title
Effect of tris(trimethylsilyl)borate on the high voltage capacity retention of LiNi0.5Co0.2Mn0.3O2/graphite cells;Xiaoxi Zuo等;《Journal of Power Sources》;20121222;第229卷;第308-312页 *
Tris(trimethylsilyl) borate as an electrolyte additive to improve the cyclability of LiMn2O4 cathode for lithium-ion battery;Yanbo Liu;《Journal of Power Sources》;20120821;第221卷;第60-69页 *

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