CN102738463A - Surface coating modification method of lithium vanadium phosphate cathode material by use of EDTA as carbon source - Google Patents
Surface coating modification method of lithium vanadium phosphate cathode material by use of EDTA as carbon source Download PDFInfo
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- CN102738463A CN102738463A CN2012102244548A CN201210224454A CN102738463A CN 102738463 A CN102738463 A CN 102738463A CN 2012102244548 A CN2012102244548 A CN 2012102244548A CN 201210224454 A CN201210224454 A CN 201210224454A CN 102738463 A CN102738463 A CN 102738463A
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- edta
- lithium
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- carbon source
- phosphoric acid
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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 surface coating modification method of a lithium vanadium phosphate cathode material by the use of EDTA as a carbon source and belongs to the field of chemical power source materials and lithium ion batteries. The method comprises the following steps of: mixing a lithium source, a vanadium source, a phosphorus source and EDTA, adding water, grinding to obtain a solid-liquid mixture, and sintering for two times to obtain the carbon source EDTA coated and modified lithium vanadium phosphate cathode material. The method requires low synthesis temperature and short calcining time, and is suitable for large-scale industrial production. The obtained carbon source EDTA coated and modified lithium vanadium phosphate cathode material has fine particles, is uniformly distributed and has high electrochemical performance.
Description
Technical field
The present invention relates to a kind of EDTA of employing is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, belongs to chemical power source material and lithium ion battery field.
Background technology
Lithium ion battery has that specific energy is big, self discharge is little, has extended cycle life, in light weight and advantages of environment protection, becomes the strong competitor of electric automobile and hybrid vehicle power supply.Common power lithium-ion battery positive electrode has spinel lithium manganate (LiMn
2O
4), nickel-cobalt-manganese ternary material (LiNi
1-x-yCo
xMn
yO
2) and polyanion type positive electrode (LiMPO
4, M=Mn, Fe, V etc.).Wherein, polyanion type LiFePO4 (LiFePO
4, having extended cycle life LFP), safe, cheap, but have the electronic and ionic poorly conductive, defective such as the lithium ion diffusion coefficient is low and the heavy-current discharge characteristic is relatively poor.Be all the phosphoric acid vanadium lithium (Li of polyanion type structure
3V
2(PO
4)
3LVP) theoretical energy density reaches 500mWh/g; Compare LFP and have higher electronic and ionic conductivity, theoretical charge/discharge capacity and charging/discharging voltage platform; And under the high charge voltage of 4.8V, still can keep rock-steady structure, therefore have more application prospect as the power lithium-ion battery positive electrode.
But phosphoric acid vanadium lithium has the total shortcoming of phosphate cathode material too, and promptly electronic conductivity is low.Need carry out material modification to phosphoric acid vanadium lithium.At present, the method for modifying of phosphoric acid vanadium lithium mainly contains the carbon coating, metal oxide coats and metal cation mixes, and is wherein common with the coated modified carbon method again.Adopt LiH like people such as Jiawei Wang
2PO
4Be phosphorus source and lithium source, V
2O
5Be the vanadium source, polyethylene glycol obtains the Li that carbon coats as carbon source through solid phase reaction
3V
2(PO
4)
3/ C positive electrode, said positive electrode capacity under the charge-discharge magnification of 1C remains on 110 ~ 120mAh/g.In addition, sucrose, maltose, polystyrene, citric acid also can be used in the coated modified carbon of this material.
EDTA (EDTA) is a kind of chelating agent; Have six coordination atoms; Can with the stable water soluble complexs of formation such as alkali gold rare earth element and transition metal, in the synthesizing of anode material for lithium-ion batteries, can be used as complexing agent, but at present not with EDTA as carbon source; Phosphoric acid vanadium lithium is carried out coating modification, prepare the report of phosphoric acid vanadium lithium positive electrode.
Summary of the invention
It is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode that the object of the invention has been to provide a kind of EDTA of employing; After said method is mixed lithium source, vanadium source, phosphorus source and EDTA; Add the water grinding and obtain solidliquid mixture, obtaining adopting EDTA through twice sintering is carbon source coating modification phosphoric acid vanadium lithium positive electrode.Said method synthesis temperature is low, calcination time is short, the employing EDTA that obtains be carbon source coating modification phosphoric acid vanadium lithium positive electrode particle thin, be evenly distributed, chemical property is high, is suitable for large-scale industrial production.
For realizing above-mentioned purpose, technical scheme of the present invention is following:
A kind of EDTA of employing is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, and said method step is following:
(1) with after lithium source, vanadium source, phosphorus source and the EDTA mixing, adds the water grinding and obtain solidliquid mixture;
Wherein, the consumption of said lithium source, vanadium source, phosphorus source, EDTA and water is Li:V:P:EDTA: water=(3.0~3.3) mol:2mol:3mol: (0.8~1.6) mol: (400 ~ 600) ml;
(2) solidliquid mixture is moved in the airtight container,, obtain presoma at 70~90 ℃ of reaction 8~15h;
(3) with presoma at 300 ~ 400 ℃ of sintering 3~5h, obtain material previously treated behind the natural cooling;
(4) with material previously treated at 700~850 ℃ of sintering 6~10h, obtain black solid behind the natural cooling, said black solid is a carbon source coating modification phosphoric acid vanadium lithium positive electrode for adopting EDTA.
Wherein, in the step (1), said lithium source, vanadium source and phosphorus source are the conventional material in anode material for lithium-ion batteries field, and preferred said lithium source is lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate, lithium fluoride or lithium oxalate; Said vanadium source is vanadic oxide or ammonium metavanadate; Said phosphorus source is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate.
In step (3), (4), sintering carries out under inert gas shielding, like argon gas, helium or nitrogen.
In the preferred steps (1), after lithium source, vanadium source, phosphorus source and EDTA mixing, add entry and grind, obtain uniform solidliquid mixture.
In the preferred steps (4), after the material previously treated grinding,, obtain the solid sheet that thickness is 0.5 ~ 1cm, carry out sintering then at 5 ~ 15MPa compacting, 5 ~ 10min.
Beneficial effect
The invention provides a kind of EDTA of employing is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode; EDTA makes as chelating agent and carries out coordination more fully between the raw material in the said method; EDTA improves the chemical property of material again as the carbon source that is coated on the phosphoric acid vanadium lithium surface simultaneously.The employing EDTA that obtains is that the discharge capacity first of carbon source coating modification phosphoric acid vanadium lithium positive electrode is 129mAh/g, near the theoretical capacity of phosphoric acid vanadium lithium.
Description of drawings
Fig. 1 is X-ray diffraction (XRD) figure of carbon source coating modification phosphoric acid vanadium lithium positive electrode for the employing EDTA of embodiment 1 preparation;
Fig. 2 is ESEM (SEM) figure of carbon source coating modification phosphoric acid vanadium lithium positive electrode for the employing EDTA of embodiment 1 preparation;
Fig. 3 is transmission electron microscope (TEM) figure of carbon source coating modification phosphoric acid vanadium lithium positive electrode for the employing EDTA of embodiment 1 preparation;
When Fig. 4 was 0.1C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the first charge-discharge curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode;
When Fig. 5 was 0.1C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the cycle performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode;
When Fig. 6 was 2C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the cycle performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode;
When Fig. 7 was respectively 0.1C, 1C, 2C and 3C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the high rate performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode;
When Fig. 8 was 0.1C for charge-discharge magnification, the employing EDTA of embodiment 2 preparations was the cycle performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode;
When Fig. 9 was respectively 0.1C, 1C, 2C and 3C for charge-discharge magnification, the employing EDTA of embodiment 3 preparations was the high rate performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode.
Embodiment
Embodiment 1
A kind of employing EDTA of the present invention is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, and said method step is following:
(1) with lithium source 0.0079mol Li
2CO
3, vanadium source 0.005mol V
2O
5, phosphorus source 0.015molNH
4H
2PO
4Grind in mortar with 0.006mol EDTA, after mixing, drip adding 2ml deionized water, grind and obtain uniform solidliquid mixture;
(2) be lined with in solidliquid mixture is moved in the agitated reactor of polytetrafluoroethylene cover,, obtain presoma at 80 ℃ of reaction 12h;
(3) with presoma in argon gas, 350 ℃ of following sintering 3h obtain material previously treated behind the natural cooling;
(4) material previously treated is ground, behind 10MPa compacting 5min, obtain the solid sheet that thickness is 0.5 ~ 1cm; In argon gas; 800 ℃ of following sintering 8h obtain black solid behind the natural cooling, said black solid is a carbon source coating modification phosphoric acid vanadium lithium positive electrode for adopting EDTA.
With said employing EDTA is that carbon source coating modification phosphoric acid vanadium lithium positive electrode prepares test battery test loop performance, and concrete steps are following:
Employing EDTA with after grinding is a carbon source coating modification phosphoric acid vanadium lithium positive electrode: the acetylene black conductive agent: the mass ratio of polyvinylidene fluoride binding agent=80:10:10 mixes; Become slurries with N-methyl pyrrolidone solvent then, apply to be put on scraper and process electrode slice on the aluminium foil.Electrode slice at 80 ℃ of vacuumize 10h, is obtained lithium ion battery after the taking-up compacting and uses positive plate.With said positive plate is positive pole, and the pure metal lithium sheet is a negative pole, and Celgard2400 is a barrier film; (volume ratio of EC and DMC is 1:1 to the EC/DMC of 1mol/L LiPF6; Wherein EC is an ethylene carbonate, and DMC is a dimethyl carbonate) solution is electrolyte, in being full of the glove box of argon gas, is assembled into button 2032 type batteries; Do the constant current charge-discharge loop test at the land test macro then, discharging and recharging cut-ff voltage is 3.0~4.3V.
Fig. 1 is for the employing EDTA of embodiment 1 preparation is X-ray diffraction (XRD) figure of carbon source coating modification phosphoric acid vanadium lithium positive electrode, explain that what obtain is the phosphoric acid vanadium lithium material of monocline, and free from admixture produces mutually;
Fig. 2 is ESEM (SEM) figure of carbon source coating modification phosphoric acid vanadium lithium positive electrode for the employing EDTA of embodiment 1 preparation; Explain that the granular size that said employing EDTA is a carbon source coating modification phosphoric acid vanadium lithium positive electrode is no more than 3 μ; And particle size distribution is even, does not have obvious agglomeration;
Fig. 3 is transmission electron microscope (TEM) figure of carbon source coating modification phosphoric acid vanadium lithium positive electrode for the employing EDTA of embodiment 1 preparation; Middle black part is divided into phosphoric acid vanadium lithium; The amorphous carbon that the transparent part at black particle edge forms for the EDTA pyrolysis, said amorphous carbon evenly is coated on the phosphoric acid vanadium lithium matrix;
When Fig. 4 was 0.1C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the first charge-discharge curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode.The discharge capacity first that said employing EDTA is a carbon source coating modification phosphoric acid vanadium lithium positive electrode is 129mAh/g, near theoretical capacity 133mAh/g.First charge-discharge enclosed pasture efficient is 97%, has excellent reversibility;
When Fig. 5 was 0.1C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the cycle performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode.Said employing EDTA is that carbon source coating modification phosphoric acid vanadium lithium positive electrode circulates under 0.1C after 50 times, and capability retention has excellent cycle performance up to more than 98%;
When Fig. 6 is 2C for charge-discharge magnification; The employing EDTA of embodiment 1 preparation is the cycle performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode; Said employing EDTA is that carbon source coating modification phosphoric acid vanadium lithium positive electrode circulates under 2C after 50 times; Capability retention is 95.1%, circulates that capacity is 108mAh/g after 100 times, and capability retention is 93.1%.Therefore under the high current charge-discharge condition, still has excellent cycle performance;
When Fig. 7 was respectively 0.1C, 1C, 2C and 3C for charge-discharge magnification, the employing EDTA of embodiment 1 preparation was the high rate performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode.Said employing EDTA be carbon source coating modification phosphoric acid vanadium lithium positive electrode under different charge-discharge magnifications, capacity all remains on more than the 110mAh/g, has excellent chemical property.
A kind of employing EDTA of the present invention is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, and said method step is following:
(1) with lithium source 0.016mol LiF, vanadium source 0.005mol V
2O
5, phosphorus source 0.015mol NH
4H
2PO
4Grind in mortar with 0.008mol EDTA, after mixing, drip adding 3ml deionized water, grind and obtain uniform solidliquid mixture;
(2) be lined with in solidliquid mixture is moved in the agitated reactor of polytetrafluoroethylene cover,, obtain presoma at 70 ℃ of reaction 15h;
(3) with presoma in nitrogen, 300 ℃ of following sintering 5h obtain material previously treated behind the natural cooling;
(4) material previously treated is ground, behind 5MPa compacting 10min, obtain the solid sheet that thickness is 0.5 ~ 1cm; In nitrogen; 700 ℃ of following sintering 10h obtain black solid behind the natural cooling, said black solid is a carbon source coating modification phosphoric acid vanadium lithium positive electrode for adopting EDTA.
XRD, SEM and TEM test result that said employing EDTA is a carbon source coating modification phosphoric acid vanadium lithium positive electrode are similar with embodiment 1.Being carbon source coating modification phosphoric acid vanadium lithium positive electrode with said employing EDTA prepares test battery test chemical property by the method for embodiment 1.When Fig. 8 was 0.1C for charge-discharge magnification, the employing EDTA of embodiment 2 preparations was the cycle performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode; Circulate after 30 weeks, the capacity that said employing EDTA is a carbon source coating modification phosphoric acid vanadium lithium positive electrode remains on more than the 110mAh/g, and capability retention has excellent cycle performance up to more than 99%.
Embodiment 3
A kind of employing EDTA of the present invention is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, and said method step is following:
(1) with lithium source 0.0164mol LiOH, vanadium source 0.01mol NH
4VO
3, phosphorus source 0.015mol (NH
4)
2HPO
4Grind in mortar with 0.004mol EDTA, after mixing, drip adding 2.5ml deionized water, grind and obtain uniform solidliquid mixture;
(2) be lined with in solidliquid mixture is moved in the agitated reactor of polytetrafluoroethylene cover,, obtain presoma at 90 ℃ of reaction 8h;
(3) with presoma in nitrogen, 400 ℃ of following sintering 3h obtain material previously treated behind the natural cooling;
(4) material previously treated is ground, behind 10MPa compacting 8min, obtain the solid sheet that thickness is 0.5 ~ 1cm; In nitrogen; 850 ℃ of following sintering 6h obtain black solid behind the natural cooling, said black solid is a carbon source coating modification phosphoric acid vanadium lithium positive electrode for adopting EDTA.
XRD, SEM and TEM test result that said employing EDTA is a carbon source coating modification phosphoric acid vanadium lithium positive electrode are similar with embodiment 1.Being carbon source coating modification phosphoric acid vanadium lithium positive electrode with said employing EDTA prepares test battery test chemical property by the method for embodiment 1.When Fig. 9 was respectively 0.1C, 1C, 2C and 3C for charge-discharge magnification, the employing EDTA of embodiment 3 preparations was the high rate performance curve of carbon source coating modification phosphoric acid vanadium lithium positive electrode.Even under 3C high current charge-discharge condition, said employing EDTA is that carbon source coating modification phosphoric acid vanadium lithium positive electrode capacity still remains on more than the 100mAh/g, has better electrochemical performance.
In sum, more than being merely preferred embodiment of the present invention, is not to be used to limit protection scope of the present invention.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (4)
- One kind to adopt EDTA be the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, it is characterized in that: said method step is following:(1) with after lithium source, vanadium source, phosphorus source and the EDTA mixing, adds the water grinding and obtain solidliquid mixture;Wherein, the consumption of said lithium source, vanadium source, phosphorus source, EDTA and water is Li:V:P:EDTA: water=(3.0~3.3) mol:2mol:3mol: (0.8~1.6) mol: (400 ~ 600) ml;(2) solidliquid mixture is moved in the airtight container,, obtain presoma at 70~90 ℃ of reaction 8~15h;(3) with presoma at 300 ~ 400 ℃ of sintering 3~5h, obtain material previously treated;(4) with material previously treated at 700~850 ℃ of sintering 6~10h, obtaining adopting EDTA is carbon source coating modification phosphoric acid vanadium lithium positive electrode;In step (3), (4), sintering carries out under inert gas shielding.
- 2. a kind of EDTA of employing according to claim 1 is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode, it is characterized in that: in the step (1), said lithium source is lithium hydroxide, lithium carbonate, lithium acetate, lithium nitrate, lithium fluoride or lithium oxalate; Said vanadium source is vanadic oxide or ammonium metavanadate; Said phosphorus source is ammonium dihydrogen phosphate, diammonium hydrogen phosphate or ammonium phosphate.
- 3. a kind of EDTA of employing according to claim 1 is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode; It is characterized in that: in the step (1); After lithium source, vanadium source, phosphorus source and EDTA mixing, add entry and grind, obtain uniform solidliquid mixture.
- 4. a kind of EDTA of employing according to claim 1 is the method for carbon source coating modification phosphoric acid vanadium lithium positive electrode; It is characterized in that: in the step (4), after the material previously treated grinding, at 5 ~ 15MPa compacting, 5 ~ 10min; Obtain the solid sheet that thickness is 0.5 ~ 1cm, carry out sintering then.
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Cited By (8)
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CN103996852A (en) * | 2014-05-28 | 2014-08-20 | 山东精工电子科技有限公司 | Preparation method of novel nano lithium vanadium phosphate positive electrode material |
CN104282891A (en) * | 2014-09-05 | 2015-01-14 | 中南大学 | Method for synthesizing lithium vanadium phosphate/carbon composite material by adopting one-step sol-gel method |
CN104319374A (en) * | 2014-10-27 | 2015-01-28 | 山东精工电子科技有限公司 | Method for preparing magnesium-doped lithium vanadium phosphate cathode material |
CN104752722A (en) * | 2015-03-18 | 2015-07-01 | 北京理工大学 | Doped modified lithium vanadium phosphate anode material as well as preparation method and application thereof |
CN105655582A (en) * | 2016-02-05 | 2016-06-08 | 北京理工大学 | Method for coating and modifying lithium vanadium phosphate positive pole material with novel carbon source |
CN106058195A (en) * | 2016-07-21 | 2016-10-26 | 天津巴莫科技股份有限公司 | Double-coated lithium vanadium phosphate anode material and preparation method thereof |
CN106169568A (en) * | 2016-08-13 | 2016-11-30 | 南阳师范学院 | A kind of preparation method of anode material for lithium-ion batteries carbon cladding phosphoric acid vanadium lithium |
CN112670494A (en) * | 2021-01-20 | 2021-04-16 | 广东工业大学 | Vanadate electrode material and preparation method and application thereof |
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CN103996852A (en) * | 2014-05-28 | 2014-08-20 | 山东精工电子科技有限公司 | Preparation method of novel nano lithium vanadium phosphate positive electrode material |
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CN104752722A (en) * | 2015-03-18 | 2015-07-01 | 北京理工大学 | Doped modified lithium vanadium phosphate anode material as well as preparation method and application thereof |
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CN112670494A (en) * | 2021-01-20 | 2021-04-16 | 广东工业大学 | Vanadate electrode material and preparation method and application thereof |
CN112670494B (en) * | 2021-01-20 | 2023-06-20 | 广东工业大学 | Vanadate electrode material and preparation method and application thereof |
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Application publication date: 20121017 |