CN103000942A - Additive promoting graphite cathode to generate solid electrolyte interfacial film, and application thereof - Google Patents
Additive promoting graphite cathode to generate solid electrolyte interfacial film, and application thereof Download PDFInfo
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- CN103000942A CN103000942A CN2011102726211A CN201110272621A CN103000942A CN 103000942 A CN103000942 A CN 103000942A CN 2011102726211 A CN2011102726211 A CN 2011102726211A CN 201110272621 A CN201110272621 A CN 201110272621A CN 103000942 A CN103000942 A CN 103000942A
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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
Abstract
The invention provides an additive used for promoting a graphite cathode to generate a solid electrolyte interfacial film. The additive is characterized in that the additive has a structural formula below. The structure is a nitrogen-site unitary substitution on an imidazole ring (X). The invention also provides a propylene carbonate electrolyte containing the additive, and an application of the additive-containing propylene carbonate electrolyte in lithium ion batteries. The melting point of the electrolyte system is greatly reduced, such that lithium ion batteries employing the additive-containing propylene carbonate electrolyte has good low-temperature performance.
Description
Technical field
The present invention relates to a kind of additive and application, specifically relate to a kind of graphite cathode material that promotes and in cyclic process, generate the electrolysis additive of solid electrolyte interface film, and the application in lithium ion battery.The invention belongs to electrochemical field.
Background technology
Lithium ion battery is as a kind of energy density is high, output voltage is high, memory-less effect, eco-friendly Green Chemistry power supply, have good economic benefit, social benefit and strategic importance, be widely used in the every field such as mobile communication, digital product.
At present the electrolyte solvent that uses of lithium ion battery almost all is to add some linear carbonate with ethylene carbonate (EC) as key component, the solvent mixture that forms such as dimethyl carbonate (DMC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC) etc.The sharpest edges of ethylene carbonate are and can form form compact and stable solid electrolyte interface film (SEI film) at high-graphitized carbon material surface, because formed passivating film is comparatively fine and close, can effectively prevent further decomposition and the altogether embedding of ethylene carbonate, thereby guarantee the normal chemical property of carbon negative pole material.But the fusing point of EC higher (about 36oC) itself, although can reduce by adding the cosolvent such as DEC, DMC the fusing point of electrolyte, but its minimum serviceability temperature also only is-20oC usually, and this has limited the performance of lithium ion battery under cryogenic conditions significantly.Present fast development along with high-technology fields such as military affairs, polar region scientific investigation and Aero-Space, the low temperature scope of application and performance to lithium ion battery have proposed very high requirement, therefore the cryogenic property of lithium ion battery is one of pressing issues that must solve, and the chief component of electrolyte is especially important to the expansion of performance of lithium ion battery.Wherein the electrolyte take propene carbonate (PC) as solvent is that a kind of feasible approach that provides is provided.
The fusing point of propene carbonate is more much lower than EC, is about-49oC, has good cryogenic property, and its conductivity is higher, and price is also cheap, therefore is considered to only solvent for low-temperature electrolyte.But the compatibility of the electrolyte take propene carbonate as the primary solvent component and high-graphitized carbon electrode material is poor, efficiency for charge-discharge is low, its main cause is that propene carbonate decomposes on the surface of graphite electrode, can not form densification, effective SEI film, present corresponding to the platform about the 0.7-0.8V (with respect to Li/Li+) of the common embedding of solvation Li+ at discharge curve, finally cause peeling off of graphite electrode, efflorescence occurs, cause completely losing of the obvious decline of graphite electrode reversible capacity or even cycle performance, therefore it is generally acknowledged that propene carbonate electrolyte is not suitable in the lithium ion battery of graphitized material as negative pole.
Film for additive is that it preferentially reduces on the negative materials such as graphite surface, forms a class electrolysis additive of SEI film.By in propylene carbonate ester group electrolyte, adding film for additive, can make graphitized carbon material in propylene carbonate ester group electrolyte, have good chemical property, improve the lithium ion battery cryogenic property thereby play, the effect of the expansion lithium ion battery scope of application.At present, the film for additive that uses of research mainly contains: with CO2, SO2 as the gas of representative, reach with the liquid additive as representative such as vinylene carbonate (VC), benzimidazole, ethylene sulfite, cyano group furans as the solid of representative with LiCO3.But there are the low problem of solubility in solid and additives gas, have therefore limited the performance of its effect.Liquid additive is the problem of existence and stability and toxicity aspect often then, and these problems have limited graphite electrode in the PC base electrolyte, thereby have finally limited the application of lithium ion battery under cryogenic conditions.
Summary of the invention
An object of the present invention is to provide a kind of graphite cathode that promotes and generate the additive of SEI film in PC base electrolyte, another object of the present invention provides the lithium ion battery that a kind of employing contains the electrolyte assembling of this additive.
The invention provides a kind of graphite cathode that promotes and generate the additive of solid electrolyte interface film, it is characterized in that: described additive is following structural formula,
The said structure formula is that the monobasic of nitrogen position on the imidazole ring replaces (X), wherein X must be the functional group of containing unsaturated bond, particularly, X be carbon number between 2-10, contain thiazolinyl, alkenylene, alkynyl, aldehyde radical, ester group, ketone group, cyano group, azo-compound, phenyl and the phenyl substituted thing of the two keys of carbon-to-carbon double bond, carbon-to-carbon triple bond, carbon-oxygen, carbon-nitrogen triple bond, the two keys of nitrogen-nitrogen; Additive is to have a kind of of above structural formula or its combination; The mass fraction of additive in propylene carbonate ester group electrolyte is 0.5%-10%.
The described propylene carbonate ester group electrolyte that contains additive refers to take propene carbonate as electrolyte system unique or that primary solvent forms, namely can be with the electrolyte of pure propene carbonate as solvent, also can be binary or the multiple mixed solvent of propene carbonate and ethylene carbonate, diethyl carbonate, dimethyl carbonate, methyl ethyl carbonate ester solvent, wherein the mass fraction of propene carbonate in solvent be 50%-99.5%.
The described used electrolytic salt of propylene carbonate ester group electrolyte that contains additive is electrolytic salt commonly used in the present commercialization electrolyte system, is lithium hexafluoro phosphate (LiPF
6), lithium perchlorate (LiClO
4), di-oxalate lithium borate (LiBC
4O
8, LiBOB), LiBF4 (LiBF
4), trifluoromethyl sulfonic acid lithium (LiCF
3SO
3), tetraethyl ammonium tetrafluoroborate ((C
2H
5)
4NBF
4), two (trifluoromethane sulfonic acid acyl) imine lithium (LiN (CF
3SO
2)
2), methyltriethylammonitetrafluoroborate tetrafluoroborate (CH
3(C
2H
5)
3NBF
4) in a kind of or its combination.
The invention provides a kind of propylene carbonate ester group electrolyte that contains additive.
The invention provides a kind of application of propylene carbonate ester group electrolyte in lithium ion battery that contains additive.
The invention provides the lithium ion battery that a kind of employing contains the propylene carbonate ester group electrolyte assembling of additive, because the adding of additive can make graphite form the SEI film in PC base electrolyte, and PC is the main or unique composition in the electrolyte solvent, the fusing point decrease of electrolyte system, thereby adopt this lithium ion battery that contains the PC base electrolyte assembling of additive to have preferably cryogenic property.
Description of drawings
Fig. 1 is the cycle performance curve of graphite electrode in the electrolyte that adopts embodiment 1, Comparative Examples 1, Comparative Examples 2 gained.
Stereoscan photograph after Fig. 2 circulation that is graphite electrode in adopting the PC base electrolyte of embodiment 1 gained 20 times.
FT-IR spectrogram after Fig. 3 circulation that is graphite electrode in adopting the PC base electrolyte of embodiment 1 gained 20 times.
Embodiment
The below will be described in more detail by embodiment, but protection scope of the present invention is not limited to these embodiment.
Preparation PC and DMC mass ratio are that 1: 1 LiPF6 concentration is the PC base electrolyte 500ml of 1mol/L in glove box, and mixing leaves standstill.Add 0.5 gram 1-vinyl imidazole (structural formula is as follows, and X is vinyl) in 9.5 this kind of gram electrolyte, mixing leaves standstill.Obtain containing the PC base electrolyte of additive, the content of additive is 5wt%.
The preparation of graphite electrode: after a certain amount of MCMB graphite cathode material (CMS), conductive agent acetylene black and binding agent Kynoar (PVDF) be ground according to a certain percentage, add a certain amount of 1-METHYLPYRROLIDONE (NMP), obtain uniform slurry, be coated on the Copper Foil and under the 120oC vacuum condition, dried by the fire 12 hours, obtain cathode pole piece after rolling.
Cycle performance of lithium ion battery test: adopt the cylindrical simulated battery of stainless steel, with graphite electrode as Electrode, with lithium metal as to electrode, take the basic electrolyte of the PC that contains additive that makes as electrolyte, with Celgard 2325 perforated membranes as barrier film, with battery mould, after the barrier film drying, in glove box, be assembled into simulated battery.The voltage range that discharges and recharges is 0.001-2V (with respect to Li/Li+), and charge-discharge velocity is 0.2C.Gained cycle performance curve is shown in Fig. 1 (▲).Discharge capacity is 208.2mAh/g first, and after 20 circulations, discharge capacity is 194.6mAh/g, and capability retention is 93.5%.Illustrate that graphite electrode has preferably cycle performance in containing the PC base electrolyte of additive.
Microscopic appearance and FT-IR test: in glove box, take simulated battery apart, 20 times graphite cathode material of circulation is stripped down from Copper Foil, with the DMC eluent solvent of LITHIUM BATTERY several times, after under vacuum condition, DMC being volatilized fully, put into rapidly respectively that scanning electron microscope example chamber and infrared spectrometer carry out the microscopic appearance test and FT-IR tests.Spherical CMS surface is covered by the skin covering of the surface of one deck densification as can see from Figure 2, this one deck skin covering of the surface is the SEI film that is formed at the CMS Surface disintegration by additive, it can effectively suppress decomposition and the common embedding of PC solvent molecule, makes graphite material have normal chemical property in PC base electrolyte.FT-IR test result (Fig. 3) then belongs to the infrared absorption peak of lithium alkylide and lithium carbonate in the SEI film of additives decompose formation, has confirmed the formation of graphite electrode surface SEI.
Embodiment 2
Preparation LiPF6 concentration is the pure PC electrolyte 500ml of 1mol/L in glove box, and mixing leaves standstill.Add 1 gram 1-vinyl imidazole in 9 this kind of gram electrolyte, mixing leaves standstill.Obtain containing the PC base electrolyte of additive, the content of additive is 10wt%.
Embodiment 3
The LiBF4 concentration of preparing PC, DMC, DEC mass ratio be in glove box 2: 1: 1 is the PC base electrolyte 500ml of 1mol/L, and mixing leaves standstill.Add 0.2 gram N-allyl imidazole (structural formula is as follows, and X is pi-allyl) in 9.8 this kind of gram electrolyte, mixing leaves standstill.Obtain containing the PC base electrolyte of additive, the content of additive is 2wt%.
Embodiment 4
LiN (CF3SO2) 2 concentration of preparing PC, DMC, DEC mass ratio be in glove box 4: 1: 1 are the PC base electrolyte 500ml of 1mol/L, and mixing leaves standstill.Add 0.4 gram 1-to Methyl benzenesulfonyl imidazoles (structural formula such as figure below, X are to Methyl benzenesulfonyl) in 9.6 this kind of gram electrolyte, mixing leaves standstill.Obtain containing the PC base electrolyte of additive, the content of additive is 4wt%.
Preparation PC and EC mass ratio are that 2: 1 LiCF3SO3 concentration is the PC base electrolyte 500ml of 1mol/L in glove box, and mixing leaves standstill.Add 0.5 gram 1-acetyl imidazole (structural formula such as figure below, X are acetyl group) in 9.5 this kind of gram electrolyte, mixing leaves standstill.Obtain containing the PC base electrolyte of additive, the content of additive is 5wt%.
Comparative Examples
LiPF6 take the pure PC of 1mol/L as solvent studies the cycle performance of CMS graphite electrode as electrolyte.The preparation of graphite electrode and the test of cycle performance of lithium ion battery such as embodiment 1.The cycle performance curve is such as Fig. 1 (●) shown in, because PC electrolyte is decomposing on the surface of graphite electrode in the discharge process first, can not form densification, effective SEI film, the constantly altogether embedding of solvation Li+ occurs, finally cause peeling off of graphite electrode, efflorescence occurs, thereby can not discharge and recharge normally by graphite electrode, its follow-up discharge capacity is almost 0.
Claims (5)
1. the invention provides a kind of graphite cathode that promotes and generate the additive of solid electrolyte interface film, it is characterized in that: described additive is following structural formula,
The said structure formula is that the monobasic of nitrogen position on the imidazole ring replaces (X), wherein X must be the functional group of containing unsaturated bond, particularly, X be carbon number between 2-10, contain thiazolinyl, alkenylene, alkynyl, aldehyde radical, ester group, ketone group, cyano group, azo-compound, phenyl and the phenyl substituted thing of the two keys of carbon-to-carbon double bond, carbon-to-carbon triple bond, carbon-oxygen, carbon-nitrogen triple bond, the two keys of nitrogen-nitrogen; Additive is to have a kind of of above structural formula or its combination; The mass fraction of additive in propylene carbonate ester group electrolyte is 0.5%-10%.
2. described promotion graphite cathode generates the additive of solid electrolyte interface film according to claim 1, it is characterized in that: the described propylene carbonate ester group electrolyte that contains additive refers to take propene carbonate as electrolyte system unique or that primary solvent forms, namely can be with the electrolyte of pure propene carbonate as solvent, also can be binary or the multiple mixed solvent of propene carbonate and ethylene carbonate, diethyl carbonate, dimethyl carbonate, methyl ethyl carbonate ester solvent, wherein the mass fraction of propene carbonate in solvent be 50%-99.5%.
3. described graphite cathode generates the additive of solid electrolyte interface film according to claim 1, it is characterized in that: the described used electrolytic salt of propylene carbonate ester group electrolyte that contains additive is electrolytic salt commonly used in the present commercialization electrolyte system, is lithium hexafluoro phosphate (LiPF
6), lithium perchlorate (LiClO
4), di-oxalate lithium borate (LiBC
4O
8, LiBOB), LiBF4 (LiBF
4), trifluoromethyl sulfonic acid lithium (LiCF
3SO
3), tetraethyl ammonium tetrafluoroborate ((C
2H
5)
4NBF
4), two (trifluoromethane sulfonic acid acyl) imine lithium (LiN (CF
3SO
2)
2), methyltriethylammonitetrafluoroborate tetrafluoroborate (CH
3(C
2H
5)
3NBF
4) in a kind of or its combination.
4. one kind by the described propylene carbonate ester group electrolyte that contains additive of one of claim 1-3.
5. by the application of propylene carbonate ester group electrolyte in lithium ion battery that contains additive claimed in claim 4.
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|---|---|---|---|
| CN2011102726211A CN103000942A (en) | 2011-09-15 | 2011-09-15 | Additive promoting graphite cathode to generate solid electrolyte interfacial film, and application thereof |
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|---|---|---|---|
| CN2011102726211A CN103000942A (en) | 2011-09-15 | 2011-09-15 | Additive promoting graphite cathode to generate solid electrolyte interfacial film, and application thereof |
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|---|---|
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Family
ID=47929250
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| CN108390096A (en) * | 2018-03-01 | 2018-08-10 | 中南大学 | A kind of application of tetrafluoroborate, composite electrolyte and composite positive pole comprising tetrafluoroborate |
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Application publication date: 20130327 |