CN103872289A - Preparation method of spherical lithium ion battery positive electrode material LiVPO4F - Google Patents
Preparation method of spherical lithium ion battery positive electrode material LiVPO4F Download PDFInfo
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- CN103872289A CN103872289A CN201410120058.XA CN201410120058A CN103872289A CN 103872289 A CN103872289 A CN 103872289A CN 201410120058 A CN201410120058 A CN 201410120058A CN 103872289 A CN103872289 A CN 103872289A
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- lithium
- ion battery
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- livpo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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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 preparation method of a spherical lithium ion battery positive electrode material fluorine lithium vanadium phosphate (LiVPO4F), which belongs to the technical field of a lithium ion battery. The preparation method is characterized in that the lithium ion battery positive electrode material LiVPO4F is prepared by a liquid-phase high-temperature high-pressure method. The preparation method comprises the specific steps of placing a lithium source, a vanadium source and a phosphorous source in a stoichiometric ratio of 1:1:1 into a high-pressure reaction kettle, adding an organic carbon source as a reducing agent, adjusting the pH value to be 3 with deionized water as a solvent, heating the mixture for 15h under the condition that the pressure is 4MPa and the temperature is 300 DEG C to obtain a precursor of the spherical LiVPO4F; grinding and tabletting the spherical LiVPO4F, placing an amorphous precursor into a tubular sintering furnace, sintering at the temperature of 650 DEG C under a non-oxidization atmosphere for 2h, and cooling the precursor to the room temperature to obtain the spherical positive electrode material LiVPO4F. The synthesis method is simple and easy to control, the appearance of the material is unique, and the electrochemical performance is excellent.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, specifically a kind of liquid phase high-temperature and high-pressure technique that adopts is prepared a kind of ball-shaped lithium-ion battery anode material LiVPO
4the method of F.Belong to technical field of lithium ion.
Background technology
LiVPO
4f is a kind of Olivine-type Cathode Material in Li-ion Batteries.LiVPO
4f has inherited polyanion anode material for lithium-ion batteries safety, environmental protection, thermally-stabilised advantage and the LiVPO such as good
4the space 3D network configuration that F is special, for the deintercalation process of lithium ion provides the good passage that shuttles back and forth, therefore has excellent charge-discharge performance and high rate capability.Simultaneously fluorine add the surface erosion to electrode material that can reduce electrolyte, make material there is good cyclical stability.And China's vanadium resource is abundant, raw material wide material sources, with low cost.Therefore LiVPO
4f is a high-voltage lithium ion positive electrode with very large potential value.
LiVPO
4although F has three-dimensional frame structure, its ionic conductivity is improved greatly, its building-up process complexity, pure phase LiVPO
4the more difficult preparation of F and lower electronic conductivity, seriously limited its chemical property in the time of high rate charge-discharge.The present invention has synthesized the spherical LiVPO with nano-grade size by liquid phase HTHP
4f positive electrode, synthesis step is simple, and the spherical LiVPO of gained
4f has larger specific area, has increased the infiltration of electrolyte to active material, and nano-scale has shortened ion transfer path greatly, and material electric conductivity is improved.The ball-shaped lithium-ion battery anode material LiVPO that the present invention is synthetic
4f has good structural stability and excellent chemical property.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing liquid phase high-temperature and high-pressure technique to prepare ball-shaped lithium-ion battery anode material fluorophosphoric acid vanadium lithium, to improve the chemical property of lithium ion battery anode material vanadium lithium phosphate.
Technical scheme of the present invention is as follows:
(1) by lithium source, vanadium source, phosphorus source according to LiVPO
4the stoichiometric proportion of F is mixed, and adds reducing agent in water, controls the concentration of metal ion at 0.002-2mol L
-1between;
(2) above-mentioned solution is regulated to PH to 1-14;
(3) by above-mentioned solution in autoclave, 100-400 DEG C adds thermal response 1-36H;
(4) above-mentioned reactor product is taken out, filtration, a vacuum 30-150 DEG C oven dry obtain LiVPO
4f presoma;
(5) above-mentioned presoma is placed in to pipe type sintering furnace, in lower 300 DEG C~700 DEG C sintering 1-20H of nonoxidizing atmosphere, cool to room temperature obtains spherical fluorophosphoric acid vanadium lithium anode material;
Further, in step (1), described vanadium source is vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl one;
Further, in step (1), described phosphorus source is the one in ammonium dihydrogen phosphate, phosphorus hydrogen two ammoniums, ammonium phosphate, phosphoric acid, pyrophosphoric acid;
Further, in step (1), described reducing agent is the one in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid;
Further, in step (1), described lithium source is the one of lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate or lithium chloride;
Further, in step (1), described fluorine source is the one of sodium fluoride, lithium fluoride, ammonium fluoride, potassium fluoride;
Further, in step (5), described sintering atmosphere is argon gas, nitrogen, hydrogen, helium, airborne one.
Heating-up temperature in described autoclave is 300 DEG C, and be 15H heating time, the pressure P=4Mpa of autoclave, and LiVPO4F sintering temperature is 650 DEG C, sintering time is 2H;
Advantage of the present invention:
The present invention utilizes solution high temperature and high pressure method to prepare ball-shaped lithium-ion battery anode material LiVPO
4f.Simplify traditional two step carbon thermal reductions and prepared LiVPO
4the experimentation of F, preparing material is the spherical LiVPO of nano-scale
4f, the special and less reunion of microscopic appearance of material.Its spherical structure has the abundant infiltration that higher specific area is conducive to electrolyte, and nanometer materials are conducive to the transmission deintercalation of lithium ion, and spherical microscopic appearance is conducive to drawing abillity.
Brief description of the drawings
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for specification, for explaining the present invention, is not construed as limiting the invention together with embodiments of the present invention.In the accompanying drawings:
Fig. 1 is the SEM diffraction pattern of No. 2 sample amorphous state presomas in embodiment 1;
Fig. 2 is the XRD diffraction pattern of fluorophosphoric acid vanadium lithium in No. 2 samples in embodiment 1;
Fig. 3 is the 0.1C first charge-discharge curve of sample in No. 2 samples in example example 1;
Embodiment
Embodiment 1
Take vanadic oxide 0.91g, diammonium hydrogen phosphate 1.15g, lithium fluoride 0.13g, citric acid 1.4g, add 1000mL deionized water, in autoclave, dissolved, regulate PH=3, autoclave heating-up temperature is 300 DEG C, and be 15H heating time, and autoclave internal pressure is 4MPa; Be cooled to room temperature and take out filtration, by filtration product 80 DEG C of oven dry in vacuum drying oven.Oven dry powder is fully ground in agate mortar, be then placed in sintering furnace, under argon gas atmosphere, in 600 DEG C, 650 DEG C, 700 DEG C, 750 DEG C sintering 2h, be then naturally cooled to room temperature and obtain finished product LiVPO
4f.Products obtained therefrom wherein obtains pure phase LiVPO at 600 DEG C, 650 DEG C through XRD analysis
4f, at other temperature, products obtained therefrom all has Li
3v
2(PO
4)
3and V
2o
3dephasign.The microscopic appearance that detects resulting materials by SEM is spherical.Obtained product is assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, its first discharge specific capacity and 50 specific discharge capacities of circulation are in table 1
The experiment condition of table 1 experimental example 1 and experimental result
Embodiment 2
Take vanadic oxide 0.91g, diammonium hydrogen phosphate 1.15g, lithium fluoride 0.13g, citric acid 1.4g, add 1000mL deionized water, in autoclave, dissolved, regulate PH=3, autoclave heating-up temperature is 300 DEG C, and be 15H heating time, and autoclave internal pressure is 4MPa; Be cooled to room temperature and take out filtration, by filtration product 80 DEG C of oven dry in vacuum drying oven.Oven dry powder is fully ground in agate mortar, is then placed in sintering furnace, under argon gas atmosphere in 650 DEG C of sintering 0.5h, 2h, 4h, then 6h is naturally cooled to room temperature and obtains finished product LiVPO
4f.Products obtained therefrom all obtains pure phase LiVPO through XRD analysis
4f.The microscopic appearance that detects obtained material by SEM is spherical, wherein along with the size of the prolongation sphere material of sintering time increases gradually.Obtained product is assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, its first discharge specific capacity and 50 specific discharge capacities of circulation are in table 2.
The experiment condition of table 2 experimental example 2 and experimental result
Embodiment 3
Take vanadic oxide 0.91g, diammonium hydrogen phosphate 1.15g, lithium fluoride 0.13g, citric acid 1.4g, adds 1000mL deionized water, in autoclave by its dissolving, regulate PH=1,6,8,12, autoclave heating-up temperature is 300 DEG C, and be 15H heating time, and autoclave internal pressure is 4MPa; Be cooled to room temperature and take out filtration, by filtration product 80 DEG C of oven dry in vacuum drying oven.Oven dry powder is fully ground in agate mortar, be then placed in sintering furnace, under argon gas atmosphere, be then naturally cooled to room temperature in 650 DEG C of sintering 2h and obtain finished product LiVPO
4f.Products obtained therefrom all obtains pure phase LiVPO through XRD analysis
4f, detects by SEM, and it is spherical only having No. 1 material microscopic appearance that obtains, and other are all without special appearance.。Obtained product is assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, its first discharge specific capacity and 50 specific discharge capacities of circulation are in table 3.
The experiment condition of table 3 experimental example 3 and experimental result
Claims (8)
1. a preparation method for ball-shaped lithium-ion battery anode material fluorophosphoric acid vanadium lithium, is characterized in that comprising the following steps:
(1) by lithium source, vanadium source, phosphorus source according to LiVPO
4the stoichiometric proportion of F is mixed, and the organic carbon source that simultaneously adds 2 times of lithium source molal quantitys in water, is controlled the concentration of metal ion at 0.002-2mol L as reducing agent
-1between;
(2) above-mentioned solution is regulated to PH to 1-14;
(3) by above-mentioned solution in autoclave, 100-400 DEG C adds thermal response 1-36H;
(4) above-mentioned reactor product is taken out, filtration, a vacuum 30-150 DEG C oven dry obtain LiVPO
4f presoma;
(5) above-mentioned presoma is placed in to pipe type sintering furnace, in lower 300 DEG C~700 DEG C sintering 1-15H of nonoxidizing atmosphere, cool to room temperature obtains spherical fluorophosphoric acid vanadium lithium anode material.
2. the preparation method of a kind of ball-shaped lithium-ion battery anode material fluorophosphoric acid vanadium lithium according to claim 1, is characterized in that: by lithium source, Yu Lin source, vanadium source by LiVPO
4the atom ratio of F mixes at 1: 1: 1, and vanadium metal ion concentration is controlled at 0.002-2mol L
-1between.
3. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 1
4the preparation method of F, is characterized in that, the vanadium source described in step (1) is the one in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl.
4. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 1
4the preparation method of F, is characterized in that, the phosphorus source described in step (1) is the one in ammonium dihydrogen phosphate, phosphorus hydrogen two ammoniums, ammonium phosphate, phosphoric acid, pyrophosphoric acid.
5. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 1
4the preparation method of F is characterized in that, the reducing agent described in step (1) is the one in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
6. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 1
4the preparation method of F is characterized in that, the lithium source described in step (1) is the one of lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, lithium hydroxide, lithium acetate or lithium chloride.
7. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 1
4the preparation method of F is characterized in that, the fluorine source described in step (1) is the one of sodium fluoride, lithium fluoride, ammonium fluoride, potassium fluoride.
8. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 1
4the preparation method of F is characterized in that: the nonoxidizing atmosphere of sintering is argon gas, nitrogen, hydrogen, helium, airborne one.
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104124440A (en) * | 2014-07-28 | 2014-10-29 | 中南大学 | Method for preparing porous spherical positive electrode material (lithium vanadium pyrophosphate) for lithium ion battery |
CN104401957A (en) * | 2014-10-13 | 2015-03-11 | 济南大学 | Hydrothermally preparing method of lithium secondary battery anode material cobalt lithium fluorophosphate |
CN106058250A (en) * | 2016-07-22 | 2016-10-26 | 天津巴莫科技股份有限公司 | Lithium-enriched lithium vanadium phosphate fluoride anode material |
RU2619600C2 (en) * | 2015-09-28 | 2017-05-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Electrode material for metal-ion battery, method of its production, electrode and electrode material based battery |
CN111302322A (en) * | 2020-02-25 | 2020-06-19 | 西安交通大学 | High-density spherical lithium vanadium fluorophosphate cathode material and preparation method thereof |
US11831001B2 (en) | 2021-05-13 | 2023-11-28 | Saft America | Pre-lithiation method and pre-lithiated lithium-ion secondary battery |
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CN101456550A (en) * | 2009-01-06 | 2009-06-17 | 桂林工学院 | Method for preparing lithium ionic cell anode material lithium vanadium fluorophosphate by hydro-thermal synthesis reaction |
CN102079518A (en) * | 2009-11-29 | 2011-06-01 | 宁波大学 | Low-temperature liquid-phase preparation method for LiVPo4F as lithium-ion battery cathode material |
CN102364736A (en) * | 2011-11-11 | 2012-02-29 | 中南大学 | Method for preparing cathode material lithium vanadium fluorophosphates of lithium ion battery |
-
2014
- 2014-03-28 CN CN201410120058.XA patent/CN103872289B/en active Active
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101456550A (en) * | 2009-01-06 | 2009-06-17 | 桂林工学院 | Method for preparing lithium ionic cell anode material lithium vanadium fluorophosphate by hydro-thermal synthesis reaction |
CN102079518A (en) * | 2009-11-29 | 2011-06-01 | 宁波大学 | Low-temperature liquid-phase preparation method for LiVPo4F as lithium-ion battery cathode material |
CN102364736A (en) * | 2011-11-11 | 2012-02-29 | 中南大学 | Method for preparing cathode material lithium vanadium fluorophosphates of lithium ion battery |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104124440A (en) * | 2014-07-28 | 2014-10-29 | 中南大学 | Method for preparing porous spherical positive electrode material (lithium vanadium pyrophosphate) for lithium ion battery |
CN104401957A (en) * | 2014-10-13 | 2015-03-11 | 济南大学 | Hydrothermally preparing method of lithium secondary battery anode material cobalt lithium fluorophosphate |
RU2619600C2 (en) * | 2015-09-28 | 2017-05-17 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Московский государственный университет имени М.В. Ломоносова" (МГУ) | Electrode material for metal-ion battery, method of its production, electrode and electrode material based battery |
CN106058250A (en) * | 2016-07-22 | 2016-10-26 | 天津巴莫科技股份有限公司 | Lithium-enriched lithium vanadium phosphate fluoride anode material |
CN111302322A (en) * | 2020-02-25 | 2020-06-19 | 西安交通大学 | High-density spherical lithium vanadium fluorophosphate cathode material and preparation method thereof |
US11831001B2 (en) | 2021-05-13 | 2023-11-28 | Saft America | Pre-lithiation method and pre-lithiated lithium-ion secondary battery |
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