CN102774891A - Method for improving electrochemical performance of spinel (LiNi0.5 Mn1.5O4) - Google Patents
Method for improving electrochemical performance of spinel (LiNi0.5 Mn1.5O4) Download PDFInfo
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- CN102774891A CN102774891A CN2012102814804A CN201210281480A CN102774891A CN 102774891 A CN102774891 A CN 102774891A CN 2012102814804 A CN2012102814804 A CN 2012102814804A CN 201210281480 A CN201210281480 A CN 201210281480A CN 102774891 A CN102774891 A CN 102774891A
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- spinel
- lini
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- raising
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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 discloses a method for improving the electrochemical performance of the spinel (LiNi0.5 Mn1.5O4), which is characterized by adopting the multi-step calcination to control the content of trivalent manganese ion in the spinel (LiNi0.5Mn1.5O4). As the cathode material of the lithium battery, the LiNi0.5Mn1.5O4 has good magnification performance and a very stable cycle performance and has the discharge capacity of 108mAhg<-1>, 108mAhg<-1>, 106mAhg<-1>, 102mAhg<-1> and 98mAhg<-1> under the magnification of 1C, 2C, 5C, 10C and 20C and can be circularly charged and discharged for 100 times under the magnification of 10C without being changed in capacity. The method is simple in process, low in requirement for the equipment and good in reproducibility and complies with the environmental requirements.
Description
Technical field
The invention belongs to and belong to battery material and learn the field, be specifically related to a kind of raising spinel LiNi
0.5Mn
1.5O
4The method of chemical property.
Background technology
Spinel LiNi
0.5Mn
1.5O
4Because of its output voltage is high, cost is low, environmental friendliness has received extensive studies.The pertinent literature report that the control of the contained manganic pair ion of control spinel chemical property is not also arranged at present.
Summary of the invention
The object of the present invention is to provide a kind of raising spinel LiNi
0.5Mn
1.5O
4The method of chemical property, LiNi of the present invention
0.5Mn
1.5O
4Show good high rate performance and highly stable cycle performance as anode material of lithium battery.Technology is simple, and is low for equipment requirements, and favorable reproducibility meets environmental requirement.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of raising spinel LiNi
0.5Mn
1.5O
4The method of chemical property is calcined through multistep and to be controlled spinel LiNi
0.5Mn
1.5O
4Material manganic ionic content.
With lithium salts, nickel salt and manganese salt molar ratio ingredient according to 2:1:3; Put into the ball grinder ball milling 6-10 hour; Temperature rise rate with 1-10 ℃/min is heated to 800 ℃, and temperature is controlled at 800 ℃ of calcinings 8-20 hour, and the cooling back is taken out and ground; Temperature rise rate with 1-10 ℃/min is heated to 800 ℃ again, and temperature is controlled at 800 ℃ and calcines the spinel LiNi that promptly obtained disordered structure in 8-20 hour once more
0.5Mn
1.5O
4
Described lithium salts is a Lithium Hydroxide MonoHydrate.
Described nickel salt is a nickelous acetate.
Described manganese salt is manganous carbonate.
Lithium cell assembling: press mass ratio LiNi
0.5Mn
1.5O
4: acetylene black: be coated in 0.25 cm equably behind tetrafluoroethylene=80:15:5 mixed grinding
2Aluminium flake on do positive pole, reference electrode and counter electrode are metallic lithium, ionogen is by 1M LiPF
6EC+DMC (EC/DMC=1/1 v/v) solution.All assemblings are all carried out in glove box.
Beneficial effect of the present invention: LiNi of the present invention
0.5Mn
1.5O
4Show good high rate performance and highly stable cycle performance as anode material of lithium battery.Loading capacity is respectively 108mAhg under 1C, 2C, 5C, 10C, 20C multiplying power
-1, 108 mAhg
-1, 106 mAhg
-1, 102 mAhg
-1, 98 mAhg
-1Charge and discharge cycles 100 circles under the 10C multiplying power, capacity does not have to change basically.This method technology is simple, low for equipment requirements, and favorable reproducibility meets environmental requirement.
Description of drawings
Fig. 1 is spinel LiNi
0.5Mn
1.5O
4Sem photograph.
Fig. 2 is spinel LiNi
0.5Mn
1.5O
4Different multiplying discharge performance figure.
Fig. 3 is spinel LiNi
0.5Mn
1.5O
4Charging and discharging curve figure.
Fig. 4 is spinel LiNi
0.5Mn
1.5O
4Stable circulation performance figure.
Embodiment
With Lithium Hydroxide MonoHydrate, nickelous acetate and manganous carbonate molar ratio ingredient according to 2:1:3; Put into the ball grinder ball milling 6 hours; Temperature rise rate with 3 ℃/min is heated to 800 ℃, and temperature is controlled at 800 ℃ of calcinings 8 hours, and the cooling back is taken out and ground; Temperature rise rate with 3 ℃/min is heated to 800 ℃ again, and temperature is controlled at 800 ℃ and calcines the spinel LiNi that promptly obtained disordered structure in 8 hours once more
0.5Mn
1.5O
4Lithium cell assembling: press mass ratio LiNi
0.5Mn
1.5O
4: acetylene black: be coated in 0.25 cm equably behind tetrafluoroethylene=80:15:5 mixed grinding
2Aluminium flake on do positive pole, reference electrode and counter electrode are metallic lithium, ionogen is by 1M LiPF
6EC+DMC (EC/DMC=1/1 v/v) solution.All assemblings are all carried out in glove box.
Embodiment 2
With Lithium Hydroxide MonoHydrate, nickelous acetate and manganous carbonate molar ratio ingredient according to 2:1:3; Put into the ball grinder ball milling 6 hours; Temperature rise rate with 5 ℃/min is heated to 800 ℃, and temperature is controlled at 800 ℃ of calcinings 8 hours, and the cooling back is taken out and ground; Temperature rise rate with 5 ℃/min is heated to 800 ℃ again, and temperature is controlled at 800 ℃ and calcines the spinel LiNi that promptly obtained disordered structure in 12 hours once more
0.5Mn
1.5O
4Lithium cell assembling: press mass ratio LiNi
0.5Mn
1.5O
4: acetylene black: be coated in 0.25 cm equably behind tetrafluoroethylene=80:15:5 mixed grinding
2Aluminium flake on do positive pole, reference electrode and counter electrode are metallic lithium, ionogen is by 1M LiPF
6EC+DMC (EC/DMC=1/1 v/v) solution.All assemblings are all carried out in glove box.
With Lithium Hydroxide MonoHydrate, nickelous acetate and manganous carbonate molar ratio ingredient according to 2:1:3; Put into the ball grinder ball milling 6 hours; Temperature rise rate with 5 ℃/min is heated to 800 ℃, and temperature is controlled at 800 ℃ of calcinings 20 hours, and the cooling back is taken out and ground; Temperature rise rate with 5 ℃/min is heated to 800 ℃ again, and temperature is controlled at 800 ℃ and calcines the spinel LiNi that promptly obtained disordered structure in 20 hours once more
0.5Mn
1.5O
4Lithium cell assembling: press mass ratio LiNi
0.5Mn
1.5O
4: acetylene black: be coated in 0.25 cm equably behind tetrafluoroethylene=80:15:5 mixed grinding
2Aluminium flake on do positive pole, reference electrode and counter electrode are metallic lithium, ionogen is by 1M LiPF
6EC+DMC (EC/DMC=1/1 v/v) solution.All assemblings are all carried out in glove box.
Fig. 1 is spinel LiNi
0.5Mn
1.5O
4Sem photograph.From Electronic Speculum figure, the size of particles of the mangaic acid nickel lithium that we synthesized at 500nm between the 2um.Fig. 2 is spinel LiNi
0.5Mn
1.5O
4Different multiplying discharge performance figure.Figure sees from high rate performance, and the mangaic acid nickel lithium that we were synthesized has extraordinary high rate performance.Fig. 3 is spinel LiNi
0.5Mn
1.5O
4Charging and discharging curve figure.The voltage platform of spinel mangaic acid nickel lithium has a platform in addition at 4.7V about 4.0V, the capacity contribution is mainly derived from the manganic ion, and we can control manganic ionic content through the control of temperature rise rate and calcining temperature.Manganic ionic content is different, and the length of 4.0V left and right sides platform, obliquity all are different.Fig. 4 is spinel LiNi
0.5Mn
1.5O
4Stable circulation performance figure.Charge and discharge cycles 100 circles under the 10C multiplying power, capacity does not have to change basically, and stability is fine.
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (5)
1. one kind is improved spinel LiNi
0.5Mn
1.5O
4The method of chemical property is characterized in that: calcine through multistep and control spinel LiNi
0.5Mn
1.5O
4Material manganic ionic content.
2. raising spinel LiNi according to claim 1
0.5Mn
1.5O
4The method of chemical property; It is characterized in that: with lithium salts, nickel salt and manganese salt molar ratio ingredient, put into the ball grinder ball milling 6-10 hour, be heated to 800 ℃ with the temperature rise rate of 1-10 ℃/min according to 2:1:3; Temperature is controlled at 800 ℃ of calcinings 8-20 hour; The cooling back is taken out and is ground, and the temperature rise rate with 1-10 ℃/min is heated to 800 ℃ again, and temperature is controlled at 800 ℃ and calcines the spinel LiNi that promptly obtained disordered structure in 8-20 hour once more
0.5Mn
1.5O
4
3. raising spinel LiNi according to claim 2
0.5Mn
1.5O
4The method of chemical property is characterized in that: described lithium salts is a Lithium Hydroxide MonoHydrate.
4. raising spinel LiNi according to claim 2
0.5Mn
1.5O
4The method of chemical property is characterized in that: described nickel salt is a nickelous acetate.
5. raising spinel LiNi according to claim 2
0.5Mn
1.5O
4The method of chemical property is characterized in that: described manganese salt is manganous carbonate.
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|---|---|---|---|
| CN2012102814804A CN102774891A (en) | 2012-08-09 | 2012-08-09 | Method for improving electrochemical performance of spinel (LiNi0.5 Mn1.5O4) |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103762354A (en) * | 2014-01-22 | 2014-04-30 | 中南大学 | LiNi0.5Mn1.5O4 material, preparation method thereof as well as lithium ion battery |
| CN103972494A (en) * | 2014-04-17 | 2014-08-06 | 山东精工电子科技有限公司 | Synthesizing method for dual anode material |
| CN104900865A (en) * | 2015-04-10 | 2015-09-09 | 合肥国轩高科动力能源股份公司 | High practicality lithium nickel manganese oxide and preparation method thereof |
| CN106430314A (en) * | 2016-09-20 | 2017-02-22 | 北京工业大学 | Method for preparing molten salt of hollow spherical LiNi<0.5>Mn<1.5>O<4> high-voltage anode material |
| US10651467B2 (en) | 2015-08-27 | 2020-05-12 | Haldor Topsøe A/S | High tap density lithium positive electrode active material, intermediate and process of preparation |
-
2012
- 2012-08-09 CN CN2012102814804A patent/CN102774891A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103762354A (en) * | 2014-01-22 | 2014-04-30 | 中南大学 | LiNi0.5Mn1.5O4 material, preparation method thereof as well as lithium ion battery |
| CN103762354B (en) * | 2014-01-22 | 2016-10-05 | 中南大学 | A kind of LiNi0.5Mn1.5O4 material, its preparation method and lithium ion battery |
| CN103972494A (en) * | 2014-04-17 | 2014-08-06 | 山东精工电子科技有限公司 | Synthesizing method for dual anode material |
| CN104900865A (en) * | 2015-04-10 | 2015-09-09 | 合肥国轩高科动力能源股份公司 | High practicality lithium nickel manganese oxide and preparation method thereof |
| US10651467B2 (en) | 2015-08-27 | 2020-05-12 | Haldor Topsøe A/S | High tap density lithium positive electrode active material, intermediate and process of preparation |
| US11444279B2 (en) | 2015-08-27 | 2022-09-13 | Haldor Topsøe A/S | High tap density lithium positive electrode active material, intermediate and process of preparation |
| CN106430314A (en) * | 2016-09-20 | 2017-02-22 | 北京工业大学 | Method for preparing molten salt of hollow spherical LiNi<0.5>Mn<1.5>O<4> high-voltage anode material |
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Application publication date: 20121114 |