CN103762384B - A kind of battery safety-type nonaqueous electrolytic solution - Google Patents
A kind of battery safety-type nonaqueous electrolytic solution Download PDFInfo
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- CN103762384B CN103762384B CN201410035305.6A CN201410035305A CN103762384B CN 103762384 B CN103762384 B CN 103762384B CN 201410035305 A CN201410035305 A CN 201410035305A CN 103762384 B CN103762384 B CN 103762384B
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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
- H01M10/0569—Liquid materials characterised by the solvents
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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
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion 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
- 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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Abstract
The invention discloses a kind of battery safety-type nonaqueous electrolytic solution, described electrolyte contains lithium salts, organic solvent and additive; Described organic solvent comprises cyclic compound and linear carbonate, and described cyclic compound comprises propene carbonate and cyclic phosphazene compound. It is solvent that this electrolyte uses flame retardant type compound, has good security performance, cryogenic property and high temperature cyclic performance, is a kind of safety-type electrolysis liquid that can use in wide temperature range. The cooperation of solvent and additive synergy, makes battery have good chemical property simultaneously, uses the lithium ion battery of electrolyte of the present invention can give full play to capacity, has excellent security performance, high-temperature behavior, cryogenic property and cycle life.
Description
Technical field
The present invention relates to the electrolyte technical field of battery, be specifically related to a kind of battery safety-type non-aqueous solution electrolysisLiquid.
Background technology
Lithium ion battery is with its high-energy-density, high voltage, memory-less effect, environmental protection and the advantage such as the life-span is long, as canThe energy leaning on has been widely used in portable type electronic product, as mobile phone, notebook computer and Miniature Power Unit driving arrangementPower supply. But in recent years, a lot of cell safety accidents had all occurred in each state, this is mainly because battery is in abuse (thermal shock, mistakeFill, short circuit etc.) cause thermal runaway under state and the safety issue that causes, particularly in large capacity power source application sides such as electric motor carsFace, safety problem is even more important. At present, the electrolyte of lithium ion battery is mostly liquid organic electrolyte, by organic solvent andElectric conducting lithium salt composition. Conventional organic solvent is alkyl carbonate compounds, as ethylene carbonate (EC), diethyl carbonateAnd methyl ethyl carbonate (EMC) etc. (DEC). Because the flash-point of these organic solvents is all very low, make the electrolyte of lithium ion battery moltenLiquid (electrolyte) very easily burns. In the time of the safety problems such as battery is short-circuited, overcharges, battery abnormal heating, gasification or decomposition are producedRaw a large amount of gas causes cell fracture on fire. Although battery is furnished with holding circuit, safety valve and semistorEtc., but can not avoid that leaking appears in these organic solvents, the even situation of blast of burning completely (PTC). At present relevant electrolysisThe research discovery of liquid combustibility, though alkyl phosphate has certain flame retardant effect, but severe exacerbation battery performance; And containNitrogen compound is little on battery performance impact, but their flame retarding efficiency is not high, and toxicity is larger. In addition, along with electronicThe development of the key areas such as car, space technology, the serviceability temperature scope of lithium ion battery also become battery researcher pay close attention toOne of Important Problems. Ethylene carbonate (EC) is current the most frequently used cyclic carbonate ester solvent. But solidifying of ethylene carbonatePoint high (39 DEG C), is solid-state under normal temperature, and under low temperature, electrolyte solidifies, and electrical conductivity reduces, and greatly affects the cryogenic property of battery.
As mentioned above, improve the security of battery, give electrolyte noninflammability and the serviceability temperature scope of widening electrolyteImportant.
For the problems referred to above, phosphazene compound is added in nonaqueous electrolytic solution, give nonaqueous electrolytic solution from putting out characteristic, largeAmplitude reduces battery short circuit, cell fracture danger on fire while overcharging. The freezing point of phosphazene compound, can below-5 DEG CImprove the cryogenic property of battery. Simultaneously preferably propene carbonate (PC), as one of solvent composition of electrolyte, further improvesThe cryogenic property of battery.
Summary of the invention
The object of the present invention is to provide the safety-type electrolysis liquid that a kind of serviceability temperature scope is wide, short circuit, break while overchargingHazard of catch fire is little, and high temperature cyclic performance is good, and low temperature performance is good, has the nonaqueous electrolytic solution of good battery performance.
For achieving the above object, the present invention adopts following technical scheme:
A kind of battery safety-type nonaqueous electrolytic solution, described electrolyte contains lithium salts, organic solvent and additive; DescribedOrganic solvent comprise cyclic compound and linear carbonate, described cyclic compound comprises propene carbonate and cyclic phosphazeneCompound; The structural formula of described cyclic phosphazene compound is:
, wherein, R1~R6In optional two groups be fluorine, alkyl, alkoxyl, aryl, virtueOne in oxygen base, all the other four groups are fluorine.
Described propene carbonate consumption accounts for 10% ~ 70% of organic solvent gross mass in electrolyte.
Described cyclic phosphazene compound consumption accounts for 5% ~ 50% of organic solvent gross mass in electrolyte.
Described lithium salts is selected from one in lithium hexafluoro phosphate, LiBF4, di-oxalate lithium borate, difluorine oxalic acid boracic acid lithiumKind or several; The mass concentration of described lithium salts in electrolyte is 0.8～1.3molL-1。
Described lithium salts is lithium hexafluoro phosphate.
Described linear carbonate solvent is selected from dimethyl carbonate, diethyl carbonate, Methylethyl carbonic ester, methylOne or more in propyl carbonate, butylene.
Described additive is selected from vinylene carbonate, fluorinated ethylene carbonate, vinyl vinylene carbonate, sulfurous acidOne or more in vinyl acetate, vinyl ethylene sulfite, propylene sulfite, dimethyl suflfate, sulfuric acid propylene; InstituteStating additive amount is 0.5～10% of electrolyte gross mass.
The mass ratio that described organic solvent consists of cyclic compound and linear carbonate is 30:70～75:25.
Beneficial effect of the present invention is:
In electrolyte, use phosphonitrile analog derivative as one of electrolyte organic solvent component, due to phosphonitrile analog derivativeThere is flame retardant effect, can solve the safety problem of battery under abuse state (overcharge, short circuit etc.); Use propylene carbonate simultaneouslyEster, as electrolyte organic solvent component, because the fusing point of propene carbonate is lower, has improved the cryogenic property of battery; Use intoFilm additive can form SEI film in the surface of active material of battery, suppresses the decomposition of electrolyte in surface of active material, improvesThe stability of battery. The cooperation of solvent and additive synergy, makes battery have good chemical property simultaneously, usesThe lithium ion battery of electrolyte of the present invention can be given full play to capacity, has excellent security performance, high-temperature behavior, cryogenic propertyAnd cycle life.
Detailed description of the invention
The present invention further illustrates the present invention with the following example, but protection scope of the present invention is not limited to following realityExecute example.
In specific embodiments of the invention, affiliated linear carbonate is selected from and well known to a person skilled in the art organic solvent,In order to facilitate elaboration of the present invention, linear carbonate is selected diethyl carbonate (DEC).
Embodiment 1
Electrolyte is composed as follows: lithium salts LiPF6Mass concentration 1.0molL-1, organic solvent propene carbonate, structural formulaCyclic phosphazene compound (the wherein R that (I) represents1~R5For fluorine, R6For ethyoxyl) and diethyl carbonate (mass ratio 20:20:60),Additive vinyl ethylene sulfite (VES) accounts for 3% of electrolyte gross mass, and additive VC accounts for 2% of electrolyte gross mass.
By the electrolyte preparing, according to conventional cell making process, injecting just very cobalt acid lithium, negative pole is graphiteFlexible-packed battery in. Battery design capacity is 1000mAh. Battery changes into according to following flow process: 0.02C constant-current charge extremely2.8V, 0.05C constant-current charge is to 3.3V, and 0.1C constant-current charge is to 4.2V, 4.2V constant-voltage charge, cut-off current 0.033C. Change intoAfter battery vacuum-pumping again seal, carry out partial volume according to following flow process: 0.2C constant-current discharge is to 2.5V, and 0.2C constant-current charge is extremely4.2V, 4.2V constant-voltage charge, cut-off current 0.05C, charge and discharge cycles 2 times.
(1) electrolyte flame-retardant is evaluated
According to the UL94 horizontal firing method of UL standard measure the flame of lighting in atmospheric environment burning length andBurning time, and evaluate. Particularly, based on UL94HB experimental standard, glass fibre long 13cm is soaked in configuration24h at least in electrolyte, then takes out and is placed in combustion test instrument, with gas lamp, it is executed to flame 15s, then removes gas lamp,Record the residual flame time, be self-extinguishing time.
(2) over-charging of battery evaluation
Detection battery core is shelved to 24h. Connect constant current constant voltage source and set output voltage 10V, it is 5.5 little that output current 0.5C chargesTime, battery should not explode, not on fire.
(3) battery short circuit evaluation
Battery core full charging, to 4.2V, is shelved to 24h. Be not more than the short-circuiting device of 50m Ω by circuit all-in resistance, short circuit battery core justNegative pole, finishes test when battery temperature drops to than low approximately 10 DEG C of peak value. In process of the test battery should be not on fire, do not explode, electricityThe external temperature in pond must not be higher than 150 DEG C.
(4) battery low temperature performance is evaluated
Battery in room temperature with 0.5C multiplying power constant-current constant-voltage charging, blanking voltage 4.2V. Battery is shelved in cryogenic box to controlTemperature processed is-30 DEG C, shelves time 120min. End to voltage 2.5V with 0.2C multiplying power discharging. Record charge/discharge capacity.
(5) 50 DEG C of cycle performance evaluations of battery
Battery is shelved in insulating box, and controlling temperature is 50 DEG C, shelves time 120min. Fill with 1C multiplying power constant current constant voltageElectricity, blanking voltage 4.2V; End to voltage 2.75V with 1C multiplying power discharging again. Circulate 300 times. Record charge/discharge capacity.
The test result of electrolyte and battery is in table 1.
Embodiment 2
Electrolyte is composed as follows: lithium salts LiPF6Concentration 1.0molL-1, organic solvent propene carbonate, general formula (I) tableCyclic phosphazene compound (the wherein R showing1~R5For fluorine, R6For methoxyl group) and diethyl carbonate (mass ratio 25:5:70), additiveThe quality percentage composition that vinyl ethylene sulfite (VES) accounts for electrolyte total amount is 3%, and additive VC accounts for electrolyte total amountQuality percentage composition is 2%.
Embodiment 3
Electrolyte is composed as follows: lithium salts LiPF6Concentration 0.8molL-1, organic solvent propene carbonate, general formula (I) tableCyclic phosphazene compound (the wherein R showing1~R6For fluorine) and diethyl carbonate (mass ratio 20:10:70), additive vinyl sulfurousThe quality percentage composition that vinyl acetate (VES) accounts for electrolyte total amount is 3%, and the quality percentage that additive VC accounts for electrolyte total amount containsAmount is 2%.
Embodiment 4
Electrolyte is composed as follows: lithium salts LiPF6Concentration 1.3molL-1, organic solvent propene carbonate, general formula (I) tableCyclic phosphazene compound (the wherein R showing1~R5For fluorine, R6For trifluoro ethoxy) and diethyl carbonate (mass ratio 45:15:40),The quality percentage composition that additive vinyl ethylene sulfite (VES) accounts for electrolyte total amount is 3%, and additive VC accounts for electrolyteThe quality percentage composition of total amount is 2%.
Embodiment 5
Electrolyte is composed as follows: lithium salts LiPF6Concentration 1.0molL-1, organic solvent propene carbonate, general formula (I) representCyclic phosphazene compound (wherein R1~R5For fluorine, R6For ethyoxyl) and diethyl carbonate (mass ratio 70:5:25), additive secondThe quality percentage composition that thiazolinyl ethylene sulfite (VES) accounts for electrolyte total amount is 3%, and additive VC accounts for the matter of electrolyte total amountAmount percentage composition is 2%.
Embodiment 6
Electrolyte is composed as follows: lithium salts LiPF6Concentration 1.0molL-1, organic solvent propene carbonate, general formula (I) representCyclic phosphazene compound (wherein R1~R5For fluorine, R6For ethyoxyl) and diethyl carbonate (mass ratio 10:50:40), additiveThe quality percentage composition that vinyl ethylene sulfite (VES) accounts for electrolyte total amount is 3%, and additive VC accounts for electrolyte total amountQuality percentage composition is 2%.
Embodiment 7
As a comparison, the present embodiment does not add cyclic phosphazene compound, and electrolyte is composed as follows: lithium salts LiPF6Concentration1.0mol·L-1, organic solvent propene carbonate and diethyl carbonate (mass ratio 30:70), additive vinyl sulfurous acid etheneThe quality percentage composition that ester (VES) accounts for electrolyte total amount is 3%, and the quality percentage composition that additive VC accounts for electrolyte total amount is 2%.
Embodiment 8
As a comparison, the present embodiment does not add propene carbonate, and electrolyte is composed as follows: lithium salts LiPF6Concentration1.0mol·L-1, cyclic phosphazene compound (the wherein R that general formula (I) represents1~R5For fluorine, R6For ethyoxyl) and diethyl carbonate(mass ratio 30:70), the quality percentage composition that additive vinyl ethylene sulfite (VES) accounts for electrolyte total amount is 3%, addsAdding the quality percentage composition that agent VC accounts for electrolyte total amount is 2%.
Table 1 electrolyte and battery performance evaluation
According to the data in table 1, the electrolyte of embodiment 7 is long burning time, does not possess fire resistance, phosphonitrile analog derivativeAdd the anti-flammability that can significantly improve electrolyte. Meanwhile, the over-charging of battery short circuit of being made by the electrolyte of embodiment 7 all onlyClose, phosphazene derivative can significantly improve the security performance of battery. The battery of being made by the electrolyte of embodiment 8, low temperature dischargeCapacity is lower, and the cryogenic property that can improve electrolyte that adds of PC is described. By the relatively discovery of embodiment 1 ~ 6 and embodiment 7, phosphorusNitrile derivative is improved the high temperature circulation of battery. The electrolyte of the present invention's design has good security performance, low temperature propertiesEnergy and high temperature cyclic performance are a kind of safety-type electrolysis liquid that can use in wide temperature range.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change withModify, all should belong to covering scope of the present invention.
Claims (6)
1. a battery safety-type nonaqueous electrolytic solution, is characterized in that: described electrolyte contains lithium salts, organic solvent and addsAdd agent; Described organic solvent comprises cyclic compound and linear carbonate, the consisting of of described cyclic compound: carbonic acid thirdAlkene ester and cyclic phosphazene compound; The structural formula of described cyclic phosphazene compound is:
, wherein, R1~R6In optional two groups be fluorine, alkyl, alkoxyl, aryl, aryloxy groupIn one, all the other four groups are fluorine;
Described propene carbonate consumption accounts for 10% ~ 70% of organic solvent gross mass in electrolyte; Described cyclic phosphazene chemical combinationThing consumption accounts for 5% ~ 50% of organic solvent gross mass in electrolyte.
2. battery according to claim 1 safety-type nonaqueous electrolytic solution, is characterized in that: described lithium salts is selected from hexafluoroOne or more in lithium phosphate, LiBF4, di-oxalate lithium borate, difluorine oxalic acid boracic acid lithium; Described lithium salts is in electrolysisMass concentration in liquid is 0.8～1.3molL-1。
3. battery according to claim 2 safety-type nonaqueous electrolytic solution, is characterized in that: described lithium salts is hexafluoro phosphorusAcid lithium.
4. battery according to claim 1 safety-type nonaqueous electrolytic solution, is characterized in that: described linear carbonate is moltenAgent is selected from dimethyl carbonate, diethyl carbonate, Methylethyl carbonic ester, methyl-propyl carbonic ester, butyleneOne or more.
5. battery according to claim 1 safety-type nonaqueous electrolytic solution, is characterized in that: described additive is selected from carbonAcid vinylene, fluorinated ethylene carbonate, vinyl vinylene carbonate, ethylene sulfite, vinyl ethylene sulfite,One or more in propylene sulfite, dimethyl suflfate, sulfuric acid propylene; Described additive amount is electrolyte gross mass0.5～10%.
6. battery according to claim 1 safety-type nonaqueous electrolytic solution, is characterized in that: described organic solvent compositionFor the mass ratio of cyclic compound and linear carbonate is 30:70～75:25.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104218258A (en) * | 2014-09-17 | 2014-12-17 | 宜春金晖新能源材料有限公司 | Over-charging prevention flame-retardant battery electrolyte |
| CN106207263B (en) * | 2015-05-25 | 2021-01-15 | 松下知识产权经营株式会社 | Electrolyte solution and battery |
| CN104900879B (en) * | 2015-06-01 | 2018-02-23 | 山东大学 | A kind of flame retardant type sodium-ion battery electrolyte and its application |
| CN105789683A (en) * | 2016-03-22 | 2016-07-20 | 山东大学 | Non-combustible lithium-sulfur or sodium-sulfur cell electrolyte solution and preparation method therefor |
| CN107305963A (en) * | 2016-04-25 | 2017-10-31 | 上海交通大学 | Electrolyte for lithium-sulfur cell and preparation method thereof |
| CN106450454A (en) * | 2016-10-19 | 2017-02-22 | 中航锂电（洛阳）有限公司 | Electrolyte and lithium ion battery using electrolyte |
| CN106935909A (en) * | 2017-05-08 | 2017-07-07 | 山东大学 | A kind of flame retardant type kalium ion battery electrolyte and preparation method thereof |
| CN108963337B (en) | 2017-05-26 | 2020-05-05 | 宁德时代新能源科技股份有限公司 | Lithium ion battery and electrolyte thereof |
| HUE064146T2 (en) * | 2018-07-04 | 2024-02-28 | Lg Energy Solution Ltd | Electrolyte for lithium secondary battery and lithium secondary battery including same |
| CN111082146A (en) * | 2020-01-21 | 2020-04-28 | 大同新成新材料股份有限公司 | Electrolyte taking propylene carbonate as main solvent |
| CN111943219B (en) * | 2020-08-24 | 2021-11-16 | 厦门大学 | Inorganic salt and preparation method thereof, lithium ion battery electrolyte additive, lithium ion battery electrolyte and lithium ion battery |
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