CN103326065B - Lithium titanate battery and electrolyte thereof - Google Patents
Lithium titanate battery and electrolyte thereof Download PDFInfo
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- CN103326065B CN103326065B CN201310227365.3A CN201310227365A CN103326065B CN 103326065 B CN103326065 B CN 103326065B CN 201310227365 A CN201310227365 A CN 201310227365A CN 103326065 B CN103326065 B CN 103326065B
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- lithium titanate
- titanate battery
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- lithium
- ketone
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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 present invention provides a lithium titanate battery and electrolyte thereof. The electrolyte of the lithium titanate battery comprises lithium salt, non-aqueous solvent and an additive which is a compound with the structure of R-CO-CH=N2, wherein R is the alkyl group or phenyl group from C1-C8. The lithium titanate battery comprises an anode pole piece; a cathode pole piece, of which the cathode active substance is pure titanic acid lithium, impure titanic acid lithium or surface-covered titanic acid lithium; a diaphragm, between the adjacent anode and cathode pole pieces; and an electrolyte; the said electrolyte is the electrolyte of the lithium titanate battery. The electrolyte of the lithium titanate battery provided by the invention is able to reduce the aerogenesis of the titanic acid lithium battery, thus improving the performance in high-temperature storage and cycle of the titanic acid lithium battery.
Description
Technical field
The present invention relates to field of lithium ion battery, particularly relate to a kind of lithium titanate battery and electrolyte thereof.
Background technology
Lithium titanate is as a kind of lithium ion battery negative material, and owing to being zero strain material, have the features such as cycle performance is good, long service life, therefore it has good application prospect in lithium ion battery.When lithium titanate is as negative material, its cycle life can reach more than 20000 times at normal temperatures.In addition, lithium titanate also has discharging voltage balance, high rate performance is superior, voltage platform is high, can not produce advantages such as analysing lithium phenomenon, therefore has very high fail safe, has very large application advantage in electric automobile.But unfortunately because lithium titanate can cause electrolyte decomposition at high temperature, produce more gas, therefore lithium titanate as its high temperature cyclic performance of battery of negative material and memory property poor.
Summary of the invention
In view of background technology Problems existing, the object of the present invention is to provide a kind of lithium titanate battery and electrolyte thereof, it can reduce the aerogenesis of lithium titanate battery, and then improves high temperature storage and the cycle performance of lithium titanate battery.
To achieve these goals, in a first aspect of the present invention, the invention provides a kind of lithium titanate battery electrolyte, it comprises Li Yan ﹑ nonaqueous solvents and R-CO-CH=N
2the additive of structural compounds, wherein R is the alkyl or phenyl of C1 ~ C8.
In a second aspect of the present invention, the invention provides a kind of lithium titanate battery, it comprises: anode pole piece; Cathode pole piece, the negative electrode active material contained is pure lithium titanate, the lithium titanate of doping or surface coated lithium titanate; Barrier film, is interval between adjacent positive/negative plate; And electrolyte; Described electrolyte is described lithium titanate battery electrolyte according to a first aspect of the present invention.
Beneficial effect of the present invention is as follows:
Lithium titanate battery electrolyte provided by the invention can suppress lithium titanate battery air-generating reaction at high temperature, improves high temperature cyclic performance and the memory property of lithium titanate battery.
Embodiment
The following detailed description of according to lithium titanate battery of the present invention and electrolyte thereof and embodiment.
First lithium titanate battery electrolyte is according to a first aspect of the present invention described.
Lithium titanate battery electrolyte according to a first aspect of the present invention comprises Li Yan ﹑ nonaqueous solvents and R-CO-CH=N
2the additive of structural compounds, wherein R is the alkyl or phenyl of C1 ~ C8.R-CO-CH=N
2the structural formula of structural compounds is as follows:
Research finds that the gas production of size on lithium titanate battery of water content has vital impact, and when water content increases, gas production can the increase sharply along with the increase of water content.Therefore, how to reduce the water content of lithium titanate particle, on the high temperature storage and high temperature cyclic performance etc. of lithium titanate battery, there is vital impact.
Contained R-CO-CH=N in the lithium titanate battery electrolyte of first aspect present invention
2the additive of structural compounds effectively can remove the moisture of lithium titanate in cathode pole piece, thus decreases gas production, significantly reduces expansion during high temperature storage, improves lithium titanate battery high-temperature cycle life.
Because lithium titanate easily absorbs water, lithium titanate particle surface is made to have Ti-OH and the method that hydroxyl is difficult to be toasted by conventional heating is thoroughly removed, the existence of hydroxyl often impels the generation of some catalytic reactions, result in lithium titanate aerogenesis phenomenon in the electrolytic solution.In the present invention, R-CO-CH=N
2the Ti-OH key generation hydrolysis on structural compounds and lithium titanate particle surface, and generate R-CO-CH
2-O-Ti-key, eliminates the hydroxyl in Ti-OH, effectively avoids some catalytic reactions occurred because hydroxyl exists, further increases high temperature storage and the high temperature cyclic performance of lithium titanate battery.
In lithium titanate battery electrolyte described according to a first aspect of the present invention, alkyl can be alkyl group or cycloalkyl.
In lithium titanate battery electrolyte described according to a first aspect of the present invention, R-CO-CH=N
2structural compounds can comprise dizaomethyl ketone CH
3-CO-CH=N
2, benzene diazonium ketone C
6h
5-CO-CH=N
2, diazonium ethyl ketone CH
3cH
2-CO-CH=N
2, diazonium cyclopropyl ketone (CH
2)
3-CO-CH=N
2, diazonium n-octyl ketone CH
3(CH
2)
7-CO-CH=N
2.
In lithium titanate battery electrolyte described according to a first aspect of the present invention, described R-CO-CH=N
2structural compounds mass percentage is in the electrolytic solution 0.001% ~ 5%.When mass percentage lower than 0.001% time, the quantity not sufficient of additive is all to remove moisture (hydroxyl namely in Ti-OH) wherein; When additive amount higher than 5% time, the safety problem of lithium titanate battery may be caused.Preferably, described R-CO-CH=N
2structural compounds mass percentage is in the electrolytic solution 0.01% ~ 3%; More preferably, described R-CO-CH=N
2structural compounds mass percentage is in the electrolytic solution 0.1%.
In lithium titanate battery electrolyte described according to a first aspect of the present invention, solvent comprises cyclic carbonate and chain titanate esters.Cyclic carbonate can be selected from least one in ethylene carbonate (EC), propene carbonate (PC), gamma-butyrolacton (γ-BL), butylene (BC); Linear carbonate is selected from least one in dimethyl carbonate (DMC), diethyl carbonate (DEC), methyl ethyl carbonate (EMC), methyl propyl carbonate (MPC), dipropyl carbonate (DPC).
In lithium titanate battery electrolyte described according to a first aspect of the present invention, described lithium salts can be selected from LiN (C
xf
2x+1sO
2) (C
yf
2y+1sO
2) (wherein, x, y are positive integer), LiPF
6, LiBF
4, LiBOB, LiAsF
6, Li (CF
3sO
2)
2n, LiCF
3sO
3, LiClO
4or its combination.
Secondly lithium titanate battery is according to a second aspect of the present invention described.
Lithium titanate battery according to a second aspect of the present invention comprises: anode pole piece; Cathode pole piece, the negative electrode active material contained is pure lithium titanate, the lithium titanate of doping or surface coated lithium titanate; Barrier film, is interval between adjacent positive/negative plate; And electrolyte; Described electrolyte is described lithium titanate battery electrolyte according to a first aspect of the present invention.
In lithium titanate battery described according to a second aspect of the present invention, the positive active material of the positive plate of lithium titanate battery can be cobalt acid lithium, ternary material, LiFePO4, LiMn2O4, nickel ion doped.
In lithium titanate battery described according to a second aspect of the present invention, the Surface coating material of described surface coated lithium titanate can be metal oxide or its composite oxides or is selected from aluminum phosphate, magnesium phosphate, lithium fluoride, lithium phosphate, LiMPO
4in one or more.
In lithium titanate battery described according to a second aspect of the present invention, the metal in described metal oxide or its composite oxides can be selected from Mg, Al, Ti, V, Zr, Sc, Mn, Cr, Co, Ni, Zn or Ce; LiMPO
4in M be selected from Mg, Fe, Co, Ni, Cr, Ti or V.
In lithium titanate battery described according to a second aspect of the present invention, what the lithium titanate of described doping adulterated can be in Nb, Mg, Zn, La, Zr, N, Al and Y ion one or more.
Following explanation is according to the embodiment of lithium titanate battery of the present invention and electrolyte thereof.
Embodiment 1
Prepare lithium titanate battery anode pole piece: using ternary material (nickle cobalt lithium manganate) as positive active material, mix with 1-METHYLPYRROLIDONE (NMP) according to mass ratio 93:2:5 with Kynoar (PVDF), conductive carbon black (SP), slurry is obtained by stirring, coating machine coated current collector aluminum foil post-drying, is colded pressing, obtained anode pole piece after itemize;
Preparation lithium titanate battery negative pole piece: using lithium titanate as negative electrode active material, mix with 1-METHYLPYRROLIDONE (NMP) according to mass ratio 93:2:5 with Kynoar (PVDF), conductive carbon black (SP), slurry is obtained by stirring, coating machine coated current collector aluminum foil post-drying, is colded pressing, obtained cathode pole piece after itemize;
Prepare lithium titanate battery electrolyte: electrolyte take concentration as 1M lithium hexafluoro phosphate (LiPF
6) be lithium salts, with the mixture of the ethylene carbonate of mass ratio EC/DMC/EMC=1:1:1 (EC), dimethyl carbonate (DMC) and methyl ethyl carbonate (EMC) for non-aqueous organic solvent.Also containing additive in electrolyte, additive to be mass percentage be 0.1% dizaomethyl ketone CH
3-CO-CH=N
2;
Prepare lithium titanate battery: the lithium titanate anode pole piece of preparation, cathode pole piece (respectively the upper lug of welding) and barrier film (using polyethylene film as barrier film) are made lithium titanate battery through winding process; Then the lithium titanate battery electrolyte of above-mentioned preparation is injected; And change into, bled afterwards and Vacuum Package, the gas produced is discharged, completes the preparation of lithium titanate battery.
Embodiment 2
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the dizaomethyl ketone CH of 0.01% with mass percentage
3-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 3
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the dizaomethyl ketone CH of 0.05% with mass percentage
3-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 4
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the dizaomethyl ketone CH of 1% with mass percentage
3-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 5
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the benzene diazonium ketone C of 0.5% with mass percentage
6h
5-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 6
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the diazonium ethyl ketone CH of 1% with mass percentage
3cH
2-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1, and all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 7
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the diazonium ethyl ketone CH of 3% with mass percentage
3cH
2-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1, and all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 8
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1, wherein negative electrode active material is the Li doped with Nb
4ti
4.95nb
0.05o
12particle;
Prepare lithium titanate battery electrolyte: be the diazonium cyclopropyl ketone (CH of 0.1% with mass percentage
2)
3-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1, and all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 9
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1, wherein negative electrode active material is that Surface coating has 1% magnesian lithium titanate particle;
Prepare lithium titanate battery electrolyte: be the diazonium octyl group ketone CH of 0.1% with mass percentage
3(CH
2)
7-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1, and all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Embodiment 10
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: be the diazonium octyl group ketone CH of 5% with mass percentage
3(CH
2)
7-CO-CH=N
2mass percentage in replacement embodiment 1 is the dizaomethyl ketone CH of 0.1%
3-CO-CH=N
2, all the other are with embodiment 1, and all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
Comparative example 1
Prepare lithium titanate battery anode pole piece: with embodiment 1;
Preparation lithium titanate battery negative pole piece: with embodiment 1;
Prepare lithium titanate battery electrolyte: additive-free, all the other are with embodiment 1;
Prepare lithium titanate battery: with embodiment 1.
The embodiment 1-10 and the comparative example 1 that finally provide lithium titanate battery of the present invention detect and result.
High temperature cyclic performance test is carried out to the lithium titanate battery of embodiment 1-10 and comparative example 1: the first thickness d 1 of the front battery of record circulation, then at 60 DEG C 1.5 ~ 2.8V voltage range in, charge with the multiplying power of 0.5C, the multiplying power discharging of 0.5C carries out loop test, circulate and again record the thickness d 2 of battery after 500 times, calculate its thickness swelling (d2-d1)/d1, acquired results is in table 1.
High-temperature storage performance test is carried out to the lithium titanate battery of embodiment 1-10 and comparative example 1: first record stores the thickness d 3 of front battery, then at 85 DEG C, 4h is stored, the thickness d 4 of battery after record stores, calculate its thickness swelling (d4-d3)/d3, acquired results is in table 1.
The electrochemical property test of the lithium titanate battery of table 1 embodiment 1-10 and comparative example 1
As can be seen from Table 1, embodiment 1-10(compares ratio 1) lithium titanate battery add the additive containing R-CO-CH=N2 compounds in the electrolytic solution after, its high temperature storage and high temperature cyclic performance are obtained for very large improvement.This is because R-CO-CH=N2 compounds in lithium titanate battery can with the hydroxyl reaction on lithium titanate surface, generate R-CO-CH2-O-Ti-key, eliminate the hydroxyl on lithium titanate surface, thus avoid the catalytic reaction that hydroxyl causes, decrease the decomposition of electrolyte, reduce the probability of lithium titanate aerogenesis, decrease the flatulence phenomenon in lithium titanate battery, reduce the thickness that battery core expands when high temperature storage and high temperature circulation, and then improve high-temperature storage performance and the high temperature cyclic performance of lithium titanate battery.
Claims (9)
1. a lithium titanate battery electrolyte, comprising: lithium salt ﹑ nonaqueous solvents, is characterized in that, described lithium titanate battery electrolyte also comprises R-CO-CH=N
2the additive of structural compounds, wherein R is the alkyl or phenyl of C1 ~ C8, described R-CO-CH=N
2structural compounds mass percentage is in the electrolytic solution 0.001% ~ 5%.
2. lithium titanate battery electrolyte according to claim 1, is characterized in that,
R-CO-CH=N
2structural compounds comprises dizaomethyl ketone CH
3-CO-CH=N
2, benzene diazonium ketone C
6h
5-CO-CH=N
2, diazonium ethyl ketone CH
3cH
2-CO-CH=N
2, diazonium cyclopropyl ketone (CH
2)
3-CO-CH=N
2, diazonium n-octyl ketone CH
3(CH
2)
7-CO-CH=N
2.
3. lithium titanate battery electrolyte according to claim 1, is characterized in that,
Described R-CO-CH=N
2structural compounds mass percentage is in the electrolytic solution 0.01% ~ 3%.
4. lithium titanate battery electrolyte according to claim 3, is characterized in that,
Described R-CO-CH=N
2structural compounds mass percentage is in the electrolytic solution 0.1%.
5. a lithium titanate battery, comprising:
Positive plate;
Negative plate, the negative electrode active material contained is pure lithium titanate, the lithium titanate of doping or surface coated lithium titanate;
Barrier film, is interval between adjacent positive/negative plate; And
Electrolyte;
It is characterized in that, the lithium titanate battery electrolyte of described electrolyte according to any one of claim 1-4.
6. lithium titanate battery according to claim 5, is characterized in that, the positive active material of the positive plate of lithium titanate battery is selected from least one in cobalt acid lithium, ternary material, LiFePO4, LiMn2O4, nickel ion doped.
7. lithium titanate battery according to claim 5, is characterized in that, the Surface coating material of described surface coated lithium titanate is metal oxide or its composite oxides or is selected from aluminum phosphate, magnesium phosphate, lithium fluoride, lithium phosphate, LiMPO
4in one or more.
8. lithium titanate battery according to claim 7, is characterized in that, the metal in described metal oxide or its composite oxides is selected from Mg, Al, Ti, V, Zr, Sc, Mn, Cr, Co, Ni, Zn or Ce; LiMPO
4in M be selected from Mg, Fe, Co, Ni, Cr, Ti or V.
9. lithium titanate battery according to claim 5, is characterized in that, what the lithium titanate of described doping adulterated is one or more in Nb, Mg, Zn, La, Zr, N, Al and Y ion.
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|---|---|---|---|
| CN201310227365.3A CN103326065B (en) | 2013-06-08 | 2013-06-08 | Lithium titanate battery and electrolyte thereof |
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| CN103326065B true CN103326065B (en) | 2015-06-03 |
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| CN107293720B (en) * | 2017-06-28 | 2019-12-10 | 合肥国轩高科动力能源有限公司 | Zirconium-scandium composite oxide coated lithium titanate negative electrode material and preparation method thereof |
| CN111063932B (en) * | 2018-10-17 | 2021-06-29 | 宁德时代新能源科技股份有限公司 | Electrolyte solution and secondary battery |
| CN115207467A (en) * | 2022-07-27 | 2022-10-18 | 合肥国轩高科动力能源有限公司 | High-temperature lithium ion battery electrolyte and lithium ion battery |
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|---|---|---|---|---|
| CN101958428A (en) * | 2010-09-15 | 2011-01-26 | 东莞新能源科技有限公司 | Lithium ion secondary battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101958428A (en) * | 2010-09-15 | 2011-01-26 | 东莞新能源科技有限公司 | Lithium ion secondary battery |
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