CN103117414B - A kind of negative pole lithium titanate battery electrolyte, lithium ion battery and preparation method thereof - Google Patents
A kind of negative pole lithium titanate battery electrolyte, lithium ion battery and preparation method thereof Download PDFInfo
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- CN103117414B CN103117414B CN201310034975.1A CN201310034975A CN103117414B CN 103117414 B CN103117414 B CN 103117414B CN 201310034975 A CN201310034975 A CN 201310034975A CN 103117414 B CN103117414 B CN 103117414B
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- Y02E60/10—Energy storage using 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
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a kind of negative pole lithium titanate battery electrolyte, lithium ion battery and preparation method thereof, this electrolyte take lithium hexafluoro phosphate as electrolyte, with ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate for solvent, with in fluorinated ethylene carbonate, di-oxalate lithium borate, PS or vinylene carbonate one or more for film for additive.The present invention adopts the lithium ion battery of this electrolyte to comprise positive pole, negative pole and electrolyte.The present invention discloses the preparation method of this battery.The present invention to strengthen by adding film for additive in the electrolytic solution and changing in conjunction with high temperature lithium titanate anode to form passivating film stability in pre-charging stage with aging techniques, efficiently solve the problem adopting aqueous binders to replace the easier flatulence of lithium titanate battery of organic binder bond, ensure that the cycle performance that lithium titanate battery is superior and good fail safe, be conducive to applying of lithium titanate battery.
Description
Technical field
The present invention relates to a kind of take lithium titanate as the electrolyte for lithium ion battery of negative pole, relates to lithium ion battery adopting this electrolyte and preparation method thereof simultaneously, belongs to lithium-ion battery energy technical field.
Background technology
Along with continuous progress and the development of lithium ion battery technology, life-span and the safety of battery more and more get more and more people's extensive concerning.In recent years, spinel lithium titanate (Li
4ti
5o
12) owing to having higher doff lithium current potential (1.55Vvs.Li
+/ Li) and higher lithium ion diffusion coefficient (2 × 10
-8cm
2/ s), battery can be avoided overcharging, large current charge or low temperature time the deposition of lithium ion on Carbon anode surface, be thus that the lithium ion battery of negative pole has higher fail safe with lithium titanate, be expected to be applied to electrokinetic cell; Meanwhile, lithium titanate, as a kind of " zero strain material ", can avoid the structural change of battery in charge and discharge process, and thus lithium titanate battery has excellent cyclicity, is potentially applied to energy-storage battery.But, be that the lithium ion battery of negative pole also exists serious flatulence problem with lithium titanate, this seriously inhibits its commercialization process.
At present, the industrial Kynoar (PVDF) that generally adopts is as lithium ion battery binding agent, and organic solvent 1-METHYLPYRROLIDONE (NMP), DMF (DMF) etc. make dispersant.The method organic solvent use amount is large, and production cost is high, contaminated environment, infringement health.Therefore, lithium ion battery plus-negative plate material all adopts aqueous binders to become a kind of trend, compared with lithium ion battery prepared by the lithium ion battery adopting aqueous binders to prepare and organic bond, there is superior fail safe and good social benefit, but adopt the lithium ion battery of aqueous binders compared to the lithium ion battery adopting organic bond, owing to containing a large amount of polar group in aqueous binders, such pole piece compares and is difficult to dewater, therefore the easier aerogenesis of battery, this not only has influence on the chemical property of battery, also potential safety hazard is brought to battery.
Summary of the invention
The object of this invention is to provide a kind of take lithium titanate as the electrolyte for lithium ion battery of negative pole.
In order to realize above object, it take lithium titanate as the electrolyte for lithium ion battery of negative pole that the technical solution adopted in the present invention is to provide a kind of, comprises the component of following percetage by weight: electrolyte 10% ~ 15%, solvent 80% ~ 88% and film for additive 2% ~ 5%; Film for additive is one or more in fluorinated ethylene carbonate, di-oxalate lithium borate, PS or vinylene carbonate.
Described electrolyte is lithium hexafluoro phosphate.
Described solvent is mixed according to volume ratio 1:1:1:0.5 ~ 3 by ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate.
The present invention enhances the stability of lithium titanate anode at pre-charging stage formation passivating film by adding film for additive in the electrolytic solution, efficiently solves the problem of the easy flatulence of lithium titanate battery.
The present invention also aims to provide a kind of lithium ion battery adopting this electrolyte.
The technical solution adopted in the present invention is also to provide a kind of lithium ion battery adopting this electrolyte, comprises positive pole, negative pole and electrolyte; Described negative pole comprises negative electrode active material lithium titanate 85wt.% ~ 94wt.%, conductive agent 3wt.% ~ 10wt.%, negative pole aqueous binders 3wt.% ~ 5wt.% and additive for electrode 0wt.% ~ 1wt.%; Described positive pole comprises positive active material 90wt.% ~ 95wt.%, conductive agent 2wt.% ~ 5wt.%, positive pole aqueous binders 3wt.% ~ 5wt.% and additive for electrode 0wt.% ~ 1wt.%.
Described lithium titanate is the modified lithium titanate of single-phase lithium titanate or coated with carbon, and its primary particle is nanoscale.
Described negative pole aqueous binders is the combination in any of sodium carboxymethylcellulose and butadiene-styrene rubber, LA132 or LA133 tri-kinds, at least one in butadiene-styrene rubber, LA132 or LA133.
Described additive for electrode is oxalic acid or hydrochloric acid.
Described positive active material is LiFePO4 LiFePO
4, ternary material LiNi
xmn
yco
(1-x-y)o
2or lithium-rich manganese base material zLi
2mnO
3(1-z) LiMO
2in one or more; Wherein, ternary material LiNi
xmn
yco
(1-x-y)o
2in, 0 < x < 1, y < 0.5, x+y < 1; Lithium-rich manganese base material zLi
2mnO
3(1-z) LiMO
2in, 0 < z < 1, M=Ni
0.5mn
0.5or Ni
xmn
yco
(1-x-y)o
2, 0 < x < 1, y < 0.5, x+y < 1.
Described positive pole aqueous binders is the combination in any of sodium carboxymethylcellulose and LA132 or LA133 two kinds, at least one in LA132 or LA133.
The shortcomings such as the present invention replaces organic binder bond with aqueous binders, and overcome organic binder bond use amount large, production cost is high, contaminated environment, infringement health.
The present invention also aims to provide a kind of preparation method adopting the lithium ion battery of this electrolyte.
The technical solution adopted in the present invention is also to provide a kind of preparation method adopting the lithium ion battery of this electrolyte, comprises the following steps:
1) preparation of material:
A) negative electrode active material lithium titanate, conductive agent, negative pole aqueous binders and additive for electrode are joined in pure water by formula ratio make cathode size and be coated on aluminium collector, then dry, shear, be rolled into negative plate;
B) positive active material, conductive agent, positive pole aqueous binders and additive for electrode are joined in pure water by formula ratio make anode sizing agent and be coated on aluminium collector, then dry, shear, be rolled into positive plate;
C) ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate are pressed formula ratio mixing, preparation solvent, then electrolyte and film for additive are joined in solvent by formula ratio and form electrolyte;
2) adopt polyalkene diaphragm, by lamination process, positive plate and negative plate are made aluminum plastic film flexible packaged battery core, then drying, injection electrolyte, sealing, obtained soft-package battery;
3) soft-package battery is changed into constant volume, obtain lithium ion battery.
In described step 3), environment residing for soft-package battery is 30 ~ 60 DEG C, and carries out changing into process with 0.01C ~ 0.2C electric current.
The present invention is simple to operate, raw material sources are extensive, is convenient to industrialization promotion.
The present invention increases lithium titanate anode while pre-charging stage forms Stability of Passive Film; change in conjunction with high temperature, with aging techniques, reconstruction is carried out to passivating film; reach the protective effect to deep layer passivating film; further increase the stability of passivating film; thus inhibit electrolyte and the continuous reduction reaction of lithium titanate anode; efficiently solve the problem adopting aqueous binders to replace the easier flatulence of lithium titanate battery of organic binder bond; ensure that the cycle performance that lithium titanate battery is superior and good fail safe, be conducive to applying of lithium titanate battery.
Accompanying drawing explanation
Fig. 1 is 1000 cycle performances of embodiment 1 battery;
Fig. 2 is the discharge curve of embodiment 1 battery under different cycles;
Fig. 3 is 1000 cycle performances of embodiment 2 battery;
Fig. 4 is the discharge curve of embodiment 2 battery under different cycles;
Fig. 5 is 1000 cycle performances of embodiment 3 battery;
Fig. 6 is the discharge curve of embodiment 3 battery under different cycles:
Fig. 7 is 1000 cycle performances of embodiment 4 battery;
Fig. 8 is the discharge curve of embodiment 4 battery under different cycles.
Embodiment
Embodiment 1
The present embodiment take lithium titanate as the electrolyte for lithium ion battery of negative pole, comprises the component of following percetage by weight: lithium hexafluoro phosphate 15%, fluorinated ethylene carbonate 3%, vinylene carbonate 2% and solvent 80%; Wherein solvent is mixed according to volume ratio 1:1:1:0.5 by ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate.
The present embodiment adopts the lithium ion battery of this electrolyte, comprise positive pole, negative pole and electrolyte, wherein, negative pole comprises the oxalic acid of the single-phase lithium titanate (primary particle is nanoscale) of 85wt.%, the carbon nano-tube of 4wt.%, the conductive black of 6wt.%, the sodium carboxymethylcellulose of 1.5wt.%, the butadiene-styrene rubber of 2.5wt.% and 1wt.%; Positive pole comprises the LiFePO of 92.5wt.%
4, the carbon nano-tube of 1wt.%, the conductive black of 2.5wt.% and 4wt.% LA132.
The present embodiment adopts the preparation method of the lithium ion battery of this electrolyte, comprises the following steps:
1) preparation of material:
A) single-phase lithium titanate, carbon nano-tube, conductive black, sodium carboxymethylcellulose, butadiene-styrene rubber and oxalic acid are joined in pure water by formula ratio, after mix and blend, make cathode size, and cathode size be uniformly coated on aluminium collector, then dry, shear, be rolled into negative plate;
B) by LiFePO
4, carbon nano-tube, conductive black and LA132 join in pure water by formula ratio, after mix and blend, make anode sizing agent, and anode sizing agent be uniformly coated on aluminium collector, then dry, shear, be rolled into positive plate;
C) ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate are pressed formula ratio mixing, obtained solvent, then by formula ratio lithium hexafluoro phosphate, fluorinated ethylene carbonate and vinylene carbonate joined in solvent and form electrolyte;
2) adopt polyalkene diaphragm, by lamination process, positive plate and negative plate are made aluminum plastic film flexible packaged battery core, then drying, injection electrolyte, sealing, obtained soft-package battery;
3) by soft-package battery under 30 DEG C of environment, that carries out 0.01C electric current changes into process, obtains lithium ion battery.
1000 cycle performance results of the present embodiment battery, as shown in Figure 1.
The discharge curve of the present embodiment battery under different cycles, as shown in Figure 2.
Embodiment 2
The present embodiment take lithium titanate as the electrolyte for lithium ion battery of negative pole, comprises the component of following percetage by weight: lithium hexafluoro phosphate 10%, di-oxalate lithium borate 2% and solvent 88%; Wherein solvent is mixed according to volume ratio 1:1:1:1 by ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate.
The present embodiment adopts the lithium ion battery of this electrolyte, comprise positive pole, negative pole and electrolyte, wherein, negative pole comprises the modified lithium titanate (primary particle is nanoscale) of the coated with carbon of 94wt.%, the sodium carboxymethylcellulose of the conductive black of 3wt.%, LA132 and 0.5wt.% of 2.5wt.%; Positive pole comprises the 0.5Li of 95wt.%
2mnO
30.5LiNi
0.5mn
0.5o
2, the conductive black of 1wt.%, the electrically conductive graphite of 1wt.%, LA132 and 1wt.% of 2wt.% sodium carboxymethylcellulose.
The present embodiment adopts the preparation method of the lithium ion battery of this electrolyte, comprises the following steps:
A) modified lithium titanate of coated with carbon, conductive black, LA132 and sodium carboxymethylcellulose are joined in pure water by formula ratio, after mix and blend, make cathode size, and cathode size be uniformly coated on aluminium collector, then dry, shear, be rolled into negative plate;
B) by 0.5Li
2mnO
30.5LiNi
0.5mn
0.5o
2, conductive black, electrically conductive graphite, LA132 and sodium carboxymethylcellulose join in pure water by formula ratio, after mix and blend, make anode sizing agent, and anode sizing agent be uniformly coated on aluminium collector, then dry, shear, be rolled into positive plate;
C) ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate are pressed formula ratio mixing, obtained solvent, then by formula ratio lithium hexafluoro phosphate and di-oxalate lithium borate joined in solvent and form electrolyte;
2) adopt polyalkene diaphragm, by lamination process, positive plate and negative plate are made aluminum plastic film flexible packaged battery core, then drying, injection electrolyte, sealing, obtained soft-package battery;
3) by soft-package battery under 40 DEG C of environment, that carries out 0.05C electric current changes into process, obtains lithium ion battery.
1000 cycle performance results of the present embodiment battery, as shown in Figure 3.
The discharge curve of the present embodiment battery under different cycles, as shown in Figure 4.
Embodiment 3
The present embodiment take lithium titanate as the electrolyte for lithium ion battery of negative pole, comprises the component of following percetage by weight: lithium hexafluoro phosphate 12.5%, di-oxalate lithium borate 1.5%, PS 1%, vinylene carbonate 1% and solvent 84%; Wherein solvent is mixed according to volume ratio 1:1:1:2 by ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate.
The present embodiment adopts the lithium ion battery of this electrolyte, comprise positive pole, negative pole and electrolyte, wherein, negative pole comprises the oxalic acid of the conductive black of the modified lithium titanate of the coated with carbon of 89.5wt.% (primary particle is nanoscale), 3wt.%, the electrically conductive graphite of 2wt.%, LA133 and 0.5wt.% of 5wt.%; Positive pole comprises the LiNi of 90wt.%
1/3mn
1/3co
1/3o
2, the conductive black of 3wt.%, the electrically conductive graphite of 2wt.%, LA133 and 1wt.% of 4wt.% oxalic acid.
The present embodiment adopts the preparation method of the lithium ion battery of this electrolyte, comprises the following steps:
1) preparation of material:
A) modified lithium titanate of coated with carbon, conductive black, electrically conductive graphite, LA133 and oxalic acid are joined in pure water by formula ratio, after mix and blend, make cathode size, and cathode size be uniformly coated on aluminium collector, then dry, shear, be rolled into negative plate;
B) by LiNi
1/3mn
1/3co
1/3o
2, conductive black, electrically conductive graphite, LA133 and oxalic acid joins in pure water by formula ratio, after mix and blend, make anode sizing agent, and anode sizing agent be uniformly coated on aluminium collector, then dry, shear, be rolled into positive plate;
C) ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate are pressed formula ratio mixing, obtained solvent, then by formula ratio lithium hexafluoro phosphate, di-oxalate lithium borate, PS and vinylene carbonate joined in solvent and form electrolyte:
2) adopt polyalkene diaphragm, by lamination process, positive plate and negative plate are made aluminum plastic film flexible packaged battery core, then drying, injection electrolyte, sealing, obtained soft-package battery;
3) by soft-package battery under 50 DEG C of environment, that carries out 0.1C electric current changes into process, obtains lithium ion battery.
1000 cycle performance results of the present embodiment battery, as shown in Figure 5.
The discharge curve of the present embodiment battery under different cycles, as shown in Figure 6.
Embodiment 4
The present embodiment take lithium titanate as the electrolyte for lithium ion battery of negative pole, comprises the component of following percetage by weight: lithium hexafluoro phosphate 13%, vinylene carbonate 2% and solvent 85%; Wherein solvent is mixed according to volume ratio 1:1:1:3 by ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate.
The present embodiment adopts the lithium ion battery of this electrolyte, comprise positive pole, negative pole and electrolyte, wherein, negative pole comprises the hydrochloric acid of LA133 and 1wt.% of the conductive black of the single-phase lithium titanate of 88wt.% (primary particle is nanoscale), 3wt.%, the electrically conductive graphite of 3wt.%, LA132,3wt.% of 2wt.%; Positive pole comprises the LiFePO of 42.5wt.%
4, 50wt.% LiNi
1/3mn
1/3co
1/3o
2, the electrically conductive graphite of 2wt.%, LA132,3wt.% of 2wt.% the hydrochloric acid of LA133 and 0.5wt.%.
The present embodiment adopts the preparation method of the lithium ion battery of this electrolyte, comprises the following steps:
1) preparation of material:
A) single-phase lithium titanate, conductive black, electrically conductive graphite, LA132, LA133 and hydrochloric acid are joined in pure water by formula ratio, after mix and blend, make cathode size, and cathode size be uniformly coated on aluminium collector, then dry, shear, be rolled into negative plate;
B) by LiFePO
4, LiNi
1/3mn
1/3co
1/3o
2, electrically conductive graphite, LA132, LA133 and hydrochloric acid joins in pure water by formula ratio, after mix and blend, make anode sizing agent, and anode sizing agent be uniformly coated on aluminium collector, then dry, shear, be rolled into positive plate;
C) ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate are pressed formula ratio mixing, obtained solvent, then joins in solvent by formula ratio form electrolyte by lithium hexafluoro phosphate, vinylene carbonate:
2) adopt polyalkene diaphragm, by lamination process, positive plate and negative plate are made aluminum plastic film flexible packaged battery core, then drying, injection electrolyte, sealing, obtained soft-package battery;
3) by soft-package battery under 60 DEG C of environment, that carries out 0.2C electric current changes into process, obtains lithium ion battery.
1000 cycle performance results of the present embodiment battery, as shown in Figure 7.
The discharge curve of the present embodiment battery under different cycles, as shown in Figure 8.
Comparative example 1
In this comparative example, the step implemented is identical with embodiment 3, and difference is: the soft-package battery of preparation carries out changing into process under normal temperature 25 DEG C of environment.
Comparative example 2
In this comparative example, the step implemented is identical with embodiment 3, and difference is: electrolyte is the lithium-ion electrolyte not adding film for additive.The soft-package battery of preparation carries out changing into process under normal temperature 25 DEG C of environment.
Experimental example
Before and after the capability retention of each embodiment battery under different cycle period and circulation, cell thickness change is as shown in table 1, can be found out: after adding film for additive in the electrolytic solution, obviously can suppress lithium titanate battery flatulence problem by contrast.Change into and aging techniques in conjunction with high temperature while adding film for additive, effectively can solve the problem adopting aqueous binders to replace the easier flatulence of lithium titanate battery of organic binder bond, ensure that the cycle performance that lithium titanate battery is superior and good fail safe.
Capability retention under table 1 embodiment 1-4 cycle period different from comparative example 1-2 and the cell thickness change of circulation front and back
Note: cell thickness × 100% before thickness change=(after circulation the front cell thickness of cell thickness-circulation)/circulation
Claims (7)
1. a lithium ion battery, is characterized in that, comprises positive pole, negative pole and electrolyte; Described negative pole comprises negative electrode active material lithium titanate 85wt.% ~ 89.5wt.%, conductive agent 5wt.% ~ 10wt.%, negative pole aqueous binders 3wt.% ~ 5wt.% and additive for electrode 0.5wt.% ~ 1wt.%; Described positive pole comprises positive active material 90wt.% ~ 95wt.%, conductive agent 2wt.% ~ 5wt.%, positive pole aqueous binders 4wt.% ~ 5wt.% and additive for electrode 0wt.% ~ 1wt.%;
Described additive for electrode is oxalic acid or hydrochloric acid;
Described electrolyte comprises the component of following percetage by weight: electrolyte 12.5% ~ 15%, solvent 80% ~ 85% and film for additive 2% ~ 5%; Film for additive is one or more in fluorinated ethylene carbonate, di-oxalate lithium borate, PS or vinylene carbonate;
Described solvent is mixed according to volume ratio 1:1:1:0.5 ~ 3 by ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate;
Described electrolyte is lithium hexafluoro phosphate.
2. a kind of lithium ion battery according to claim 1, is characterized in that, described lithium titanate is the modified lithium titanate of single-phase lithium titanate or coated with carbon, and its primary particle is nanoscale.
3. a kind of lithium ion battery according to claim 1, it is characterized in that, described negative pole aqueous binders is at least one in butadiene-styrene rubber, LA132 or LA133, or is any one the combination in sodium carboxymethylcellulose and butadiene-styrene rubber, LA132 or LA133 tri-kinds.
4. a kind of lithium ion battery according to claim 1, is characterized in that, described positive active material is LiFePO4 LiFePO
4, ternary material LiNi
xmn
yco
(1-x-y)o
2or lithium-rich manganese base material zLi
2mnO
3(1-z) LiMO
2in one or more; Wherein, ternary material LiNi
xmn
yco
(1-x-y)o
2in, 0 < x < 1, y < 0.5, x+y < 1; Lithium-rich manganese base material zLi
2mnO
3(1-z) LiMO
2in, 0 < z < 1, M=Ni
0.5mn
0.5or Ni
xmn
yco
(1-x-y)o
2, 0 < x < 1, y < 0.5, x+y < 1.
5. a kind of lithium ion battery according to claim 1, is characterized in that, described positive pole aqueous binders is at least one in LA132 or LA133, or is any one the combination in sodium carboxymethylcellulose and LA132 or LA133 two kinds.
6. a preparation method for lithium ion battery as claimed in claim 1, is characterized in that, comprises the following steps:
1) preparation of material:
A) negative electrode active material lithium titanate, conductive agent, negative pole aqueous binders and additive for electrode are joined in pure water by formula ratio make cathode size and be coated on aluminium collector, then dry, shear, be rolled into negative plate;
B) positive active material, conductive agent, positive pole aqueous binders and additive for electrode are joined in pure water by formula ratio make anode sizing agent and be coated on aluminium collector, then dry, shear, be rolled into positive plate;
C) ethylene carbonate, methyl ethyl carbonate, diethyl carbonate and propene carbonate are pressed formula ratio mixing, preparation solvent, then electrolyte and film for additive are joined in solvent by formula ratio and form electrolyte;
2) adopt polyalkene diaphragm, by lamination process, positive plate and negative plate are made aluminum plastic film flexible packaged battery core, then drying, injection electrolyte, sealing, obtained soft-package battery;
3) soft-package battery is changed into constant volume, obtain lithium ion battery.
7. the preparation method of a kind of lithium ion battery according to claim 6, is characterized in that, described step 3) in environment residing for soft-package battery be 30 ~ 60 DEG C, and carry out changing into process with 0.01C ~ 0.2C electric current.
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| JP6319305B2 (en) | 2012-06-01 | 2018-05-09 | ソルベー エスアー | Lithium ion battery |
| US10044066B2 (en) | 2012-06-01 | 2018-08-07 | Solvary SA | Fluorinated electrolyte compositions |
| CA2908044C (en) | 2013-04-04 | 2022-08-23 | E. I. Du Pont De Nemours And Company | Nonaqueous electrolyte compositions |
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| CN109273763A (en) * | 2018-09-06 | 2019-01-25 | 贵州兴锂新能源科技有限公司 | It is a kind of using lithium titanate as the lithium-ion battery electrolytes of cathode |
| CN109244530A (en) * | 2018-09-21 | 2019-01-18 | 深圳市卓能新能源股份有限公司 | A kind of lithium ion battery and preparation method |
| CN111029559A (en) * | 2019-12-16 | 2020-04-17 | 银隆新能源股份有限公司 | Lithium titanate battery and preparation method thereof |
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