CN103872324B - A kind of petal-shaped lithium ion battery negative material VPO4preparation method - Google Patents

A kind of petal-shaped lithium ion battery negative material VPO4preparation method Download PDF

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CN103872324B
CN103872324B CN201410120043.3A CN201410120043A CN103872324B CN 103872324 B CN103872324 B CN 103872324B CN 201410120043 A CN201410120043 A CN 201410120043A CN 103872324 B CN103872324 B CN 103872324B
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lithium ion
petal
negative material
vanadium
ion battery
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CN103872324A (en
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郑俊超
张宝
韩亚东
张佳峰
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Central South University
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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
    • 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
    • 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
    • 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
    • H01M2004/027—Negative electrodes
    • 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

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a kind of method that liquid phase method prepares petal-shaped lithium ion battery negative material vanadium phosphate, belong to technical field of lithium ion.It is characterized in that: use liquid phase method to prepare lithium ion battery negative material vanadium phosphate.Specifically include following steps: by more soluble in water than vanadium source, phosphorus source and the reducing agent being 1: 1: 2 for mole metering, regulating PH=7, stirring obtains homogeneous solution, colloidal sol or suspension；Solution homogeneous for gained, colloidal sol or suspension are transferred in polytetrafluoroethyltank tank, load in pyrolytic tank, be heated to 280 DEG C of reaction 30H in an oven and obtain amorphous state vanadium phosphate presoma.Ground, tabletting, is placed in amorphous state presoma in pipe type sintering furnace, in the lower 725 DEG C of sintering 6H of nonoxidizing atmosphere, is cooled to room temperature and obtains vanadium phosphate product.VPO prepared by the present invention4Negative material, microscopic appearance is that material morphology is special by the petal-shaped microsphere of nanometer sheet stacking, shows the chemical property of excellence.

Description

A kind of petal-shaped lithium ion battery negative material VPO4Preparation method
Technical field
The present invention relates to the preparation method of a kind of lithium ion battery negative material, specifically a kind of employing a kind of petal-shaped lithium ion battery negative material VPO of liquid phase method preparation4Method.Belong to technical field of lithium ion.
Background technology
Along with the arrival in electronic information epoch, for meeting the energy demand of growing various mobile devices, development life-span length, specific power are big, low cost, free of contamination high-performance secondary lithium battery have become as the current trend studied.Lithium ion battery negative material is the key components of lithium ion battery, in commercialization at present, main application is graphite cathode, but either native graphite or its theoretical specific capacity of Delanium is all 372mAh/g, along with the exploitation of some height ratio capacity positive electrodes, the graphite with relatively low specific capacity can not meet the demand of positive electrode already as negative pole.Therefore, the negative material of research and development height ratio capacity has the biggest potential value.
In numerous alternative negative materials, VPO4Pass through PO4 3-Deintercalation that polyanion is lithium ion provides stable 3D frame structure, alleviates the problem that in charge and discharge process, material volume irreversible change is excessive, and VPO4Having higher specific capacity (550mAh/g) and China's vanadium resource enriches, raw material sources is extensive, with low cost.Therefore, VPO4It it is a lithium ion battery negative material with the biggest potential value.
At present, as negative pole VPO4Preparation main by the method for collosol and gel, but its synthesis VPO4Microscopic appearance wayward, be unfavorable for Physical Processing performance, and inhomogenous microscopic appearance also have large effect to the chemical property of material.Exploring new synthetic method is to improve VPO4Negative material chemical property and an effective way of Physical Processing performance.The present invention has synthesized the microspheroidal VPO of nanometer sheet stacking by liquid phase method4Negative material, synthesized material electrochemical performance is excellent, and the second particle of microspheroidal is conducive to improving the Physical Processing performance of material.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing liquid phase method to prepare petal-shaped lithium ion battery negative material vanadium phosphate, to improve lithium ion battery negative material vanadium phosphate chemical property and Physical Processing performance.
Technical scheme is as follows:
(1) vanadium source, phosphorus source being mixed with the mol ratio 1: 1 of vanadium ion, phosphate anion, the organic carbon source being simultaneously introduced lithium source molal quantity 2 times controls at 0.001-2mol/L as reactant feed, concentration of metal ions.
(2) above-mentioned solution is placed in 20-100 DEG C of thermostat water bath stirring 4H, forms solution, colloidal sol or suspension；
(3) above-mentioned solution, colloidal sol or suspension are regulated PH to 1-14；
(4) above-mentioned solution, colloidal sol or suspension are moved in polytetrafluoroethyltank tank, are placed in pyrolytic tank in 100-350 DEG C of reacting by heating 1-72H；
(5) being taken out by above-mentioned reactor product, 40-150 DEG C of drying of filtering vacuum obtains amorphous state VPO4Presoma；
(6) by above-mentioned amorphous state presoma VPO4Being placed in pipe type sintering furnace, under nonoxidizing atmosphere, 300-900 DEG C of sintering 0.1-20H, is cooled to room temperature and obtains petal-shaped VPO4；
Further, the vanadium source described in step (1) is vanadic anhydride, ammonium metavanadate, ammonium vanadate, Vanadium sesquioxide, vanadyl oxalate one；
Further, the one during the phosphorus source described in step (1) is ammonium dihydrogen phosphate, phosphorus hydrogen diammonium, ammonium phosphate, phosphoric acid, pyrophosphoric acid；
Further, 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；
Further, in step (6), the nonoxidizing atmosphere of sintering is the one in argon, nitrogen, hydrogen, helium, carbon monoxide；
Advantages of the present invention:
The present invention utilizes solwution method to prepare petal-shaped lithium ion battery negative material VPO4.Preparing negative pole pole material is by lamellar VPO with nano thickness4Stacking forms microspheroidal VPO4Its laminated structure has higher specific surface area and is conducive to the abundant infiltration of electrolyte, being connected of lamella, shorten from sub transmission path, the transmission of lithium ion, the microsphere of nanometer sheet stacking is conducive to be conducive to lithium ion in the embedding of all directions and abjection, material high rate performance is improved significantly, and be conducive to improving the Physical Processing performance of material using microspheroidal as the second particle of material, especially the tap density of material is greatly improved.The microspheroidal petal-like negative pole pole material VPO of the nanometer sheet stacking of present invention synthesis4There is good excellent chemical property.
Accompanying drawing explanation
Accompanying drawing is for providing a further understanding of the present invention, and constitutes a part for description, is used for together with embodiments of the present invention explaining the present invention, is not intended that limitation of the present invention.In the accompanying drawings:
Fig. 1 is the XRD figure of No. 3 samples in embodiment 1；
Fig. 2 is the SEM diffraction pattern of No. 3 sample presomas in embodiment 1；
Fig. 3 is 0.1C, 1C of No. 3 samples discharge curve first in embodiment 1；
Detailed description of the invention
Embodiment 1
Weighing vanadic anhydride 0.91g, diammonium phosphate 1.15g, citric acid 1.4g, be dissolved in the deionized water of 80mL, in 80 DEG C of water-baths, mechanical agitation is to forming homogeneous blue solution, regulates PH=7；Then gone to polytetrafluoroethyltank tank is placed in 280 DEG C of reacting by heating 30h in pyrolytic tank, be cooled to room temperature and take out filtration, by filtration product 80 DEG C of drying in vacuum drying oven.Drying powder is fully ground in agate mortar, is subsequently placed in sintering furnace, under an argon atmosphere in 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C of sintering 6h, be then naturally cooling to room temperature and obtain vanadium phosphate.Products obtained therefrom wherein obtains pure phase VPO at 600 DEG C, 700 DEG C through XRD analysis4, at a temperature of other, products obtained therefrom has VPO4·H2O or V2O5Dephasign.Being detected by SEM, the microscopic appearance of 1,2, No. 3 resulting materials is the microsphere of nanometer sheet stacking.Obtained product being assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, 1C, its first discharge specific capacity is shown in Table 1.
The experiment condition of table 1 experimental example 1 and experimental result
Embodiment 2
Weighing vanadic anhydride 1.82g, diammonium phosphate 2.3g, citric acid 2.8g, be dissolved in the deionized water of 80mL, in 80 DEG C of water-baths, mechanical agitation is to forming homogeneous green solution, regulates PH=7；Then gone to polytetrafluoroethyltank tank is placed in 280 DEG C of reacting by heating 30h in pyrolytic tank, be cooled to room temperature and take out filtration, by filtration product 80 DEG C of drying in vacuum drying oven.Drying powder is fully ground in agate mortar, is subsequently placed in sintering furnace, sinter 2h, 4h, 8h, 10h in 700 DEG C under an argon atmosphere, be then naturally cooling to room temperature and obtain vanadium phosphate.Products obtained therefrom is all pure phase VPO through XRD analysis4, detected by SEM, the microscopic appearance of 1, No. 2 resulting materials be nanometer sheet stacking microsphere, 3, No. 4 resulting materials without special appearance.Obtained product being assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, 1C, its first discharge specific capacity is shown in Table 2.
The experiment condition of table 2 experimental example 2 and experimental result
Embodiment 3
Weighing ammonium metavanadate 1.17g, diammonium phosphate 1.15g, citric acid 1.4g, be dissolved in the deionized water of 80mL, in 80 DEG C of water-baths, mechanical agitation is to forming homogeneous green solution, regulates PH=7；Then gone to polytetrafluoroethyltank tank is placed in 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C of reacting by heating 30h in pyrolytic tank, be cooled to room temperature and take out filtration, by filtration product 80 DEG C of drying in vacuum drying oven.Drying powder is fully ground in agate mortar, is subsequently placed in sintering furnace, sinter 6h in 700 DEG C under an argon atmosphere, be then naturally cooling to room temperature and obtain vanadium phosphate.Products obtained therefrom is through XRD analysis, and only sample 3 obtains pure phase VPO4.Being detected by SEM, the microscopic appearance of 1,2, No. 3 resulting materials is flaky nanometer structure.Obtained product being assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, 1C, its first discharge specific capacity and circulation are shown in Table 3.
The experiment condition of table 3 experimental example 3 and experimental result
Embodiment 4
Weighing vanadic anhydride 0.91g, diammonium phosphate 1.15g, citric acid 1.4g, be dissolved in the deionized water of 80mL, in 80 DEG C of water-baths, mechanical agitation is to forming homogeneous blue solution, regulates PH=7；Then gone to polytetrafluoroethyltank tank is placed in 280 DEG C of reacting by heating 5h, 10h, 20h, 40h in pyrolytic tank, be cooled to room temperature and take out filtration, by filtration product 80 DEG C of drying in vacuum drying oven.Drying powder is fully ground in agate mortar, is subsequently placed in sintering furnace, sinter 6h in 700 DEG C under an argon atmosphere, be then naturally cooling to room temperature and obtain vanadium phosphate.Products obtained therefrom is through XRD analysis, and only sample 2 obtains pure phase VPO4.Being detected by SEM, the microscopic appearance of 1,2, No. 3 resulting materials is nano-sheet.Obtained product being assembled into experiment button cell and surveys its charging and discharging capacity and cycle performance, carry out charge-discharge test under 0.1C, 1C, its first discharge specific capacity and circulation are shown in Table 4
The experiment condition of table 4 experimental example 4 and experimental result

Claims (5)

1. the preparation method of a petal-shaped lithium ion battery negative material vanadium phosphate, it is characterised in that comprise the following steps:
(1) by vanadium source, phosphorus source and organic carbon source with the mol ratio 1:1:2 mixing of phosphate anion and organic carbon source in vanadium ion, phosphorus source in vanadium source, concentration of metal ions controls 0.001～2mol/L；
(2) above-mentioned solution is placed in 20～100 DEG C of thermostat water baths stirring 4h, forms solution, colloidal sol or suspension；
(3) above-mentioned solution, colloidal sol or suspension are regulated pH to 7；
(4) above-mentioned solution, colloidal sol or suspension are moved in polytetrafluoroethyltank tank, are placed in pyrolytic tank in 100～350 DEG C of reacting by heating 1～72h；
(5) above-mentioned reactor product is taken out, filter, vacuum 40～150 DEG C of drying, obtain amorphous state VPO4Presoma；
(6) by above-mentioned amorphous state presoma VPO4Being placed in pipe type sintering furnace, under nonoxidizing atmosphere, 300～900 DEG C of sintering 0.1～20h, are cooled to room temperature and obtain petal-shaped VPO4。
The preparation method of a kind of petal-shaped lithium ion battery negative material vanadium phosphate the most according to claim 1, it is characterized in that: in step (1), described vanadium source is the one in vanadic anhydride, ammonium metavanadate, ammonium vanadate, Vanadium sesquioxide, vanadyl oxalate.
The preparation method of a kind of petal-shaped lithium ion battery negative material vanadium phosphate the most according to claim 1, it is characterised in that: in step (1), described phosphorus source is the one in ammonium dihydrogen phosphate, diammonium phosphate, ammonium phosphate, phosphoric acid, pyrophosphoric acid.
The preparation method of a kind of petal-shaped lithium ion battery negative material vanadium phosphate the most according to claim 1, it is characterized in that: in step (1), described organic carbon source is the one in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
The preparation method of a kind of petal-shaped lithium ion battery negative material vanadium phosphate the most according to claim 1, it is characterised in that: the nonoxidizing atmosphere of sintering is the one in argon, nitrogen, hydrogen, helium, carbon monoxide.
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CN104091953B (en) * 2014-07-30 2016-06-15 中南大学 Lithium ion battery negative material pyrophosphoric acid vanadium and preparation method thereof
CN104600253B (en) * 2014-12-31 2017-04-12 北京鼎能开源电池科技股份有限公司 Preparation method of ammonium oxovanadium phosphate crystals
CN104835960B (en) * 2015-05-08 2017-08-25 中南大学 A kind of preparation method of lithium ion battery negative material fluorophosphoric acid vanadium
EP3677543A1 (en) * 2015-06-26 2020-07-08 A123 Systems LLC Nanoscale pore structure cathode for high power applications and material synthesis methods
CN105185990B (en) * 2015-08-17 2018-01-02 河南理工大学 A kind of preparation method of the water vanadium phosphate of spherical lithium ion secondary battery positive electrode one
CN107230771B (en) * 2017-07-14 2020-08-14 中南大学 Method for coating lithium ion battery cathode material nickel cobalt lithium manganate with vanadium phosphate

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