CN103872289B - A kind of ball-shaped lithium-ion battery anode material LiVPO4The preparation method of F - Google Patents
A kind of ball-shaped lithium-ion battery anode material LiVPO4The preparation method of F Download PDFInfo
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- CN103872289B CN103872289B CN201410120058.XA CN201410120058A CN103872289B CN 103872289 B CN103872289 B CN 103872289B CN 201410120058 A CN201410120058 A CN 201410120058A CN 103872289 B CN103872289 B CN 103872289B
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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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- 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
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Abstract
The invention discloses a kind of preparation method of ball-shaped lithium-ion battery anode material fluorophosphoric acid vanadium lithium, belongs to technical field of lithium ion.It is characterized in that：Lithium ion battery anode material vanadium lithium phosphate is prepared using liquid phase high temperature and high pressure method.Specifically include following steps：By stoichiometric proportion for 1: 1: 1 lithium source, vanadium source, phosphorus source, be placed in autoclave, at the same add organic carbon source as reducing agent, solvent is done with deionized water, PH=3 is adjusted, pressure is 4MPa, 300 DEG C of heating 15H, obtain the presoma of spherical fluorophosphoric acid vanadyl lithium.Ground, tabletting, amorphous state presoma is placed in pipe type sintering furnace, in the lower 650 DEG C of sintering 2H of nonoxidizing atmosphere, is cooled to room temperature and is obtained spherical fluorophosphoric acid vanadium lithium anode material.Synthetic method of the present invention is simple, it is easy to control, and resulting materials pattern is special, shows excellent chemical property.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, specifically a kind of to adopt liquid phase High Temperature High Pressure
Technology prepares a kind of ball-shaped lithium-ion battery anode material LiVPO4The method of F.Belong to technical field of lithium ion.
Background technology
LiVPO4F is a kind of Olivine-type Cathode Material in Li-ion Batteries.LiVPO4F is just inheriting polyanion lithium ion battery
Pole material safety, the advantages of environmentally friendly, thermally-stabilised good and LiVPO4F special space 3D network structures, are the deintercalation of lithium ion
Process provides good shuttle passage, therefore with excellent charge-discharge performance and high rate capability.The addition of fluorine can simultaneously
To reduce the surface erosion to electrode material of electrolyte, make material that there is preferable cyclical stability.And China's vanadium resource
Abundant, raw material sources are extensively, with low cost.Therefore LiVPO4F is a high-voltage lithium ion with very big potential value
Positive electrode.
LiVPO4Although F has three-dimensional frame structure so as to which ionic conductivity is greatly improved, but its building-up process is multiple
It is miscellaneous, pure phase LiVPO4The more difficult preparations of F and relatively low electronic conductivity, seriously limit its electrification in high rate charge-discharge
Learn performance.The present invention has synthesized the spherical LiVPO with nano-grade size by liquid phase High Temperature High Pressure4F positive electrodes, synthesis step
It is rapid simple, and the spherical LiVPO of gained4F has larger specific surface area, increased infiltration of the electrolyte to active material, receives
Meter ruler cun substantially reduces ion transmission path, is improved material electric conductivity.The ball-shaped lithium-ion battery of present invention synthesis
Positive electrode LiVPO4F has good structural stability and excellent chemical property.
The content of the invention
It is an object of the invention to provide one kind prepares ball-shaped lithium-ion battery anode material using liquid phase high-temperature and high-pressure technique
The method of material fluorophosphoric acid vanadium lithium, to improve the chemical property of lithium ion battery anode material vanadium lithium phosphate.
Technical scheme is as follows：
(1) by lithium source, vanadium source, phosphorus source according to LiVPO4The stoichiometric proportion mixing of F, and reducing agent is added in water, control
The concentration of metal ion processed is in 0.002-2mol L-1Between；
(2) above-mentioned solution is adjusted into PH to 1-14；
(3) by above-mentioned solution in autoclave, 100-400 DEG C of reacting by heating 1-36H；
(4) above-mentioned reactor product is taken out, filtration, vacuum 30-150 DEG C drying obtain LiVPO4F presomas；
(5) above-mentioned presoma is placed in pipe type sintering furnace, in lower 300 DEG C～700 DEG C sintering 1-20H of nonoxidizing atmosphere,
It is cooled to room temperature and obtains spherical fluorophosphoric acid vanadium lithium anode material；
Further, in step (1), described vanadium source is vanadic anhydride, ammonium metavanadate, ammonium vanadate, Vanadium sesquioxide, grass
Sour vanadyl is a kind of；
Further, in step (1), described phosphorus source be ammonium dihydrogen phosphate, phosphorus hydrogen diammonium, ammonium phosphate, phosphoric acid, in pyrophosphoric acid
One kind；
Further, in step (1), described reducing agent be tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, the third two
One kind in acid, ascorbic acid；
Further, in step (1), described lithium source be lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate,
One kind of Lithium hydrate, lithium acetate or lithium chloride；
Further, in step (1), described Fluorine source is sodium fluoride, lithium fluoride, ammonium fluoride, one kind of potassium fluoride；
Further, in step (5), described sintering atmosphere is argon, nitrogen, hydrogen, helium, the one kind in air.
Heating-up temperature in the autoclave is 300 DEG C, and heat time heating time is 15H, the pressure P=of autoclave
4Mpa, LiVPO4F sintering temperature is 650 DEG C, and sintering time is 2H；
Advantages of the present invention：
The present invention prepares ball-shaped lithium-ion battery anode material LiVPO using solution high temperature and high pressure method4F.Simplify tradition
Two step carbon thermal reductions prepare LiVPO4The experimentation of F, prepares the spherical LiVPO that material is nano-scale4F, material it is micro-
See that pattern is special and less reunion.There is its spherical structure higher specific surface area to be conducive to the abundant infiltration of electrolyte, nanometer
Level material is conducive to the transmission deintercalation of lithium ion, and spherical microscopic appearance is conducive to the processing characteristics of material.
Description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for description, the reality with the present invention
Applying example is used for explaining the present invention together, is not construed as limiting the invention.In the accompanying drawings：
Fig. 1 is the SEM diffraction patterns of No. 2 sample amorphous state presomas in embodiment 1；
Fig. 2 is the XRD diffraction patterns of fluorophosphoric acid vanadium lithium in No. 2 samples in embodiment 1；
Fig. 3 is the 0.1C first charge-discharge curves of sample in No. 2 samples in example example 1；
Specific embodiment
Embodiment 1
Vanadic anhydride 0.91g, diammonium phosphate 1.15g, lithium fluoride 0.13g, citric acid 1.4g are weighed, 1000mL is added
Deionized water, is dissolved in autoclave, adjusts PH=3, and autoclave heating-up temperature is 300 DEG C, and heat time heating time is
15H, autoclave internal pressure are 4MPa；It is cooled to room temperature and takes out filtration, 80 DEG C of bakings in vacuum drying oven by filtration product
It is dry.Will drying powder be fully ground in agate mortar, be subsequently placed in sintering furnace, under an argon atmosphere in 600 DEG C,
650 DEG C, 700 DEG C, 750 DEG C of sintering 2h, are then naturally cooling to room temperature and obtain finished product LiVPO4F.Products obtained therefrom Jing XRD analysis its
In obtain pure phase LiVPO in 600 DEG C, 650 DEG C4F, at a temperature of other, products obtained therefrom has Li3V2(PO4)3And V2O3Dephasign.Pass through
The microscopic appearance of SEM detection resulting materials is spherical.Resulting product is assembled into into experiment button cell and surveys its discharge and recharge
Specific capacity and cycle performance, carry out charge-discharge test, 50 specific discharge capacities of its first discharge specific capacity and circulation under 0.1C
It is shown in Table 1
The experiment condition and experimental result of 1 experimental example 1 of table
Embodiment 2
Vanadic anhydride 0.91g, diammonium phosphate 1.15g, lithium fluoride 0.13g, citric acid 1.4g are weighed, 1000mL is added
Deionized water, is dissolved in autoclave, adjusts PH=3, and autoclave heating-up temperature is 300 DEG C, and heat time heating time is
15H, autoclave internal pressure are 4MPa；It is cooled to room temperature and takes out filtration, 80 DEG C of bakings in vacuum drying oven by filtration product
It is dry.Drying powder is fully ground in agate mortar, is subsequently placed in sintering furnace, burnt in 650 DEG C under an argon atmosphere
Knot 0.5h, then 2h, 4h, 6h are naturally cooling to room temperature and obtain finished product LiVPO4F.Products obtained therefrom Jing XRD analysis all obtain pure phase
LiVPO4F.Detect that the microscopic appearance of resulting material is by SEM spherical, wherein with the spherical material of the prolongation of sintering time
The size of material gradually increases.Resulting product is assembled into into experiment button cell and surveys its charging and discharging capacity and cycle performance,
Charge-discharge test is carried out under 0.1C, 50 specific discharge capacities of its first discharge specific capacity and circulation are shown in Table 2.
The experiment condition and experimental result of 2 experimental example 2 of table
Embodiment 3
Vanadic anhydride 0.91g, diammonium phosphate 1.15g, lithium fluoride 0.13g, citric acid 1.4g are weighed, is added
1000mL deionized waters, are dissolved in autoclave, adjust PH=1,6,8,12, and autoclave heating-up temperature is 300
DEG C, heat time heating time is 15H, and autoclave internal pressure is 4MPa；It is cooled to room temperature and takes out filtration, by filtration product in vacuum
80 DEG C of drying in baking oven.Drying powder is fully ground in agate mortar, is subsequently placed in sintering furnace, in argon gas atmosphere
Under 2h are sintered in 650 DEG C and then be naturally cooling to room temperature and obtain finished product LiVPO4F.Products obtained therefrom Jing XRD analysis all obtain pure phase
LiVPO4F, detects by SEM, material microscopic appearance is spherical obtained by only No. 1, and other are without special appearance..By gained
To product be assembled into experiment button cell survey its charging and discharging capacity and cycle performance, charge-discharge test is carried out under 0.1C,
50 specific discharge capacities of its first discharge specific capacity and circulation are shown in Table 3.
The experiment condition and experimental result of 3 experimental example 3 of table
Claims (8)
1. a kind of preparation method of ball-shaped lithium-ion battery anode material fluorophosphoric acid vanadium lithium, it is characterised in that comprise the following steps：
（1）By lithium source, vanadium source, phosphorus source, Fluorine source according to LiVPO4The stoichiometric proportion mixing of F, while adding 2 times of lithium source molal quantity
Organic carbon source as reducing agent in water, control metal ion concentration in 0.002～2molL-1Between；
（2）Above-mentioned solution is adjusted into pH to 1～14；
（3）By above-mentioned solution in autoclave, 100～400 DEG C of 1～36h of reacting by heating；
（4）Above-mentioned reactor product is taken out, filtration, 30～150 DEG C of drying of vacuum obtain LiVPO4F presomas；
（5）Above-mentioned presoma is placed in pipe type sintering furnace, 300～700 DEG C of 1～15h of sintering, cooling under nonoxidizing atmosphere
To room temperature, spherical fluorophosphoric acid vanadium lithium anode material is obtained.
2. the preparation method of a kind of ball-shaped lithium-ion battery anode material fluorophosphoric acid vanadium lithium according to claim 1, which is special
Levy and be：Lithium source, vanadium source and phosphorus source are pressed into LiVPO4The atom ratio 1 of F:1:1 mixing, the control of metal vanadium ion concentration exist
0.002～2molL-1Between.
3. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 14The preparation method of F, its feature exist
In：Step（1）In, described vanadium source be vanadic anhydride, ammonium metavanadate, ammonium vanadate, Vanadium sesquioxide, in vanadyl oxalate one
Kind.
4. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 14The preparation method of F, its feature exist
In：Step（1）In, described phosphorus source is ammonium dihydrogen phosphate, diammonium phosphate, ammonium phosphate, phosphoric acid, the one kind in pyrophosphoric acid.
5. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 14The preparation method of F, its feature exist
In：Step（1）In, described reducing agent be tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, in ascorbic acid
One kind.
6. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 14The preparation method of F, its feature exist
In：Step（1）In, described lithium source is lithium carbonate, lithium nitrate, lithium fluoride, lithium oxalate, lithium dihydrogen phosphate, Lithium hydrate, acetic acid
One kind of lithium or lithium chloride.
7. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 14The preparation method of F, its feature exist
In：Step（1）Described in Fluorine source be sodium fluoride, lithium fluoride, ammonium fluoride, one kind of potassium fluoride.
8. a kind of ball-shaped lithium-ion battery anode material LiVPO according to claim 14The preparation method of F, its feature exist
In：The nonoxidizing atmosphere of sintering is argon, nitrogen, hydrogen, the one kind in helium.
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| CN104124440B (en) * | 2014-07-28 | 2017-01-25 | 中南大学 | Method for preparing porous spherical positive electrode material (lithium vanadium pyrophosphate) for lithium ion battery |
| CN104401957B (en) * | 2014-10-13 | 2016-08-24 | 济南大学 | A kind of hydrothermal preparing process of positive electrode material of lithium secondary cell fluorophosphoric acid cobalt lithium |
| 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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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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