CN103872324A - Preparation method of petaloid lithium ion battery negative electrode material VPO4 - Google Patents

Preparation method of petaloid lithium ion battery negative electrode material VPO4 Download PDF

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CN103872324A
CN103872324A CN201410120043.3A CN201410120043A CN103872324A CN 103872324 A CN103872324 A CN 103872324A CN 201410120043 A CN201410120043 A CN 201410120043A CN 103872324 A CN103872324 A CN 103872324A
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lithium ion
ion battery
vpo
battery negative
vanadium
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CN103872324B (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

Abstract

The invention discloses a method for preparing a petaloid lithium ion battery negative electrode material vanadium phosphate (VPO4) by a liquid phase method, which belongs to the technical field of a lithium ion battery. The method is characterized by preparing the lithium ion battery negative electrode material VPO4 by the liquid phase method and comprises the specific steps of dissolving a vanadium source, a phosphorus source and a reducing agent in the molar ratio of 1:1:2 into water, adjusting the pH value to be 7, and stirring the mixture to obtain a homogenous solution, sol or turbid liquid; transferring the obtained homogenous solution, sol or turbid liquid into a polytetrafluoroethylene tank, placing the mixture into a pyrolysis tank, heating the mixture in a drying box to 280 DEG C for reacting for 30h to obtain an amorphous vanadium phosphate precursor; and grinding and tabletting the amorphous vanadium phosphate precursor, sintering the amorphous precursor in a tubular sintering furnace at the temperature of 725 DEG C under the non-oxidation atmosphere for 6h, and cooling the precursor to the room temperature to obtain the vanadium phosphate product. The microstructure of the prepared negative electrode material VPO4 is in the shape of petaloid microsphere formed by stacking nano-sheets, the material is unique in shape, and the electrochemical performance is excellent.

Description

A kind of petal-shaped lithium ion battery negative material VPO 4preparation method
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, specifically a kind of a kind of petal-shaped lithium ion battery negative material of Liquid preparation methods VPO that adopts 4method.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, the trend that the development life-span is long, specific power is large, cost is low, free of contamination high-performance secondary lithium battery has become current research.Lithium ion battery negative material is the key components of lithium ion battery, in commercialization at present, main application is graphite cathode, but no matter be that native graphite or its theoretical specific capacity of Delanium are all 372mAh/g, along with the exploitation of some height ratio capacity positive electrodes, the graphite with lower 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 very large potential value.
In numerous alternative negative materials, VPO 4pass through PO 4 3-the deintercalation that polyanion is lithium ion provides stable 3D frame structure, has alleviated the excessive problem of material volume irreversible change in charge and discharge process, and VPO 4there is higher specific capacity (550mAh/g) and China's vanadium resource abundant, raw material wide material sources, with low cost.Therefore, VPO 4it is a lithium ion battery negative material with very large potential value.
At present, as negative pole VPO 4preparation mainly by the method for collosol and gel, but its synthetic VPO 4microscopic appearance wayward, be unfavorable for Physical Processing performance, and inhomogenous microscopic appearance also has larger impact to the chemical property of material.Exploring new synthetic method is to improve VPO 4an effective way of negative material chemical property and Physical Processing performance.The present invention has synthesized the stacking microspheroidal VPO of nanometer sheet by liquid phase method 4negative material, the material electrochemical performance excellence of synthesized, and also the second particle of microspheroidal is conducive to improve the Physical Processing performance of material.
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing Liquid preparation methods 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 of the present invention is as follows:
(1) vanadium source, phosphorus source are mixed with the mol ratio of vanadium ion, phosphate anion at 1: 1, add the organic carbon source of 2 times of lithium source molal quantitys as reactant feed simultaneously, concentration of metal ions is controlled at 0.001-2mol/L.
(2) above-mentioned solution is placed in to 20-100 DEG C of thermostat water bath and stirs 4H, form solution, colloidal sol or suspension-turbid liquid;
(3) above-mentioned solution, colloidal sol or suspension-turbid liquid are regulated to PH to 1-14;
(4) above-mentioned solution, colloidal sol or suspension-turbid liquid are moved in polytetrafluoroethyltank tank, are placed in pyrolytic tank and add thermal response 1-72H in 100-350 DEG C;
(5) above-mentioned reactor product is taken out, filter 40-150 DEG C of oven dry of vacuum and obtain amorphous state VPO 4presoma;
(6) by above-mentioned amorphous state presoma VPO 4be placed in pipe type sintering furnace, 300-900 DEG C of sintering 0.1-20H under nonoxidizing atmosphere, cool to room temperature obtains petal-shaped VPO 4;
Further, the vanadium source described in step (1) is vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl one;
Further, the phosphorus source described in step (1) is the one in ammonium dihydrogen phosphate, phosphorus hydrogen two ammoniums, 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 gas, nitrogen, hydrogen, helium, carbon monoxide;
Advantage of the present invention:
The present invention utilizes solwution method to prepare petal-shaped lithium ion battery negative material VPO 4.Preparing negative pole utmost point material is by the sheet VPO with nano thickness 4the stacking microspheroidal VPO that forms 4its laminated structure has the abundant infiltration that higher specific area is conducive to electrolyte, being connected of lamella, shorten ion transfer path, be conducive to the transmission of lithium ion, the stacking microballoon forming of nanometer sheet is conducive to lithium ion in the embedding of all directions and deviates from, and material high rate performance is improved significantly, and second particle using microspheroidal as material is conducive to improve the Physical Processing performance of material, especially the tap density of material is greatly improved.The petal-like negative pole utmost point of the stacking microspheroidal forming of the nanometer sheet material VPO that the present invention is synthetic 4there is the chemical property of good excellence.
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 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, the 1C discharge curve first of No. 3 samples in embodiment 1;
Embodiment
Embodiment 1
Take vanadic oxide 0.91g, diammonium hydrogen phosphate 1.15g, citric acid 1.4g, is dissolved in the deionized water of 80mL, and in 80 DEG C of water-baths, mechanical agitation, to forming homogeneous blue solution, regulates PH=7; Then gone to and in polytetrafluoroethyltank tank, be placed in 280 DEG C of pyrolytic tanks and add thermal response 30h, be cooled to room temperature and take out and filter, 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 500 DEG C, 600 DEG C, 700 DEG C, 800 DEG C sintering 6h, be then naturally cooled to room temperature and obtain vanadium phosphate.Products obtained therefrom wherein obtains pure phase VPO at 600 DEG C, 700 DEG C through XRD analysis 4, at other temperature, products obtained therefrom has VPO 4h 2o or V 2o 5dephasign.Detect by SEM, the microscopic appearance of 1,2, No. 3 resulting materials is the stacking microballoon of nanometer sheet.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, 1C, its first discharge specific capacity is in table 1.
The experiment condition of table 1 experimental example 1 and experimental result
Figure BSA0000102402100000041
Embodiment 2
Take vanadic oxide 1.82g, diammonium hydrogen phosphate 2.3g, citric acid 2.8g, is dissolved in the deionized water of 80mL, and in 80 DEG C of water-baths, mechanical agitation, to forming homogeneous green solution, regulates PH=7; Then gone to and in polytetrafluoroethyltank tank, be placed in 280 DEG C of pyrolytic tanks and add thermal response 30h, be cooled to room temperature and take out and filter, 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 700 DEG C of sintering 2h, 4h, 8h, 10h, is then naturally cooled to room temperature and obtains vanadium phosphate.Products obtained therefrom is all pure phase VPO through XRD analysis 4, detect by SEM, the microscopic appearance of 1, No. 2 resulting materials is the stacking microballoon of nanometer sheet, 3, No. 4 resulting materials 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, 1C, its first discharge specific capacity is in table 2.
The experiment condition of table 2 experimental example 2 and experimental result
Figure BSA0000102402100000042
Embodiment 3
Take ammonium metavanadate 1.17g, diammonium hydrogen phosphate 1.15g, citric acid 1.4g, is dissolved in the deionized water of 80mL, and in 80 DEG C of water-baths, mechanical agitation, to forming homogeneous green solution, regulates PH=7; Then gone to and in polytetrafluoroethyltank tank, be placed in 150 DEG C of pyrolytic tanks, 200 DEG C, 250 DEG C, 300 DEG C and add thermal response 30h, be cooled to room temperature and take out and filter, 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 700 DEG C of sintering 6h, be then naturally cooled to room temperature and obtain vanadium phosphate.Products obtained therefrom, through XRD analysis, only has sample 3 to obtain pure phase VPO 4.Detect by SEM, the microscopic appearance of 1,2, No. 3 resulting materials is nano-sheet structure.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, 1C, its first discharge specific capacity and circulation are in table 3.
The experiment condition of table 3 experimental example 3 and experimental result
Figure BSA0000102402100000051
Embodiment 4
Take vanadic oxide 0.91g, diammonium hydrogen phosphate 1.15g, citric acid 1.4g, is dissolved in the deionized water of 80mL, and in 80 DEG C of water-baths, mechanical agitation, to forming homogeneous blue solution, regulates PH=7; Then gone to and in polytetrafluoroethyltank tank, be placed in 280 DEG C of pyrolytic tanks and add thermal response 5h, 10h, 20h, 40h, be cooled to room temperature and take out and filter, 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 700 DEG C of sintering 6h, be then naturally cooled to room temperature and obtain vanadium phosphate.Products obtained therefrom, through XRD analysis, only has sample 2 to obtain pure phase VPO 4.Detect by SEM, the microscopic appearance of 1,2, No. 3 resulting materials is nano-sheet.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, 1C, its first discharge specific capacity and circulation are in table 4
The experiment condition of table 4 experimental example 4 and experimental result

Claims (6)

1. a preparation method for petal-shaped lithium ion battery negative material vanadium phosphate, is characterized in that comprising the following steps:
(1) vanadium source, phosphorus source are mixed with the mol ratio of vanadium ion, phosphate anion at 1: 1, add the organic carbon source of 2 times of lithium source molal quantitys as reactant feed simultaneously, concentration of metal ions is controlled at 0.001-2mol/L;
(2) above-mentioned solution is placed in to 20-100 DEG C of thermostat water bath and stirs 4H, form solution, colloidal sol or suspension-turbid liquid;
(3) above-mentioned solution, colloidal sol or suspension-turbid liquid are regulated to PH to 1-14;
(4) above-mentioned solution, colloidal sol or suspension-turbid liquid are moved in polytetrafluoroethyltank tank, are placed in pyrolytic tank and add thermal response 1-72H in 100-350 DEG C;
(5) above-mentioned reactor product is taken out, filter, vacuum 40-150 DEG C of oven dry obtains amorphous state VPO 4presoma;
(6) by above-mentioned amorphous state presoma VPO 4be placed in pipe type sintering furnace, 300-900 DEG C of sintering 0.1-20H under nonoxidizing atmosphere, cool to room temperature obtains petal-shaped VPO 4.
2. a kind of lithium ion battery negative material VPO according to claim 1 4preparation method, it is characterized in that: vanadium source, phosphorus source are mixed by mole proportioning with reducing agent at 1: 1: 2, and vanadium metal ion concentration is controlled at 0.001-2mol L -1between.
3. a kind of lithium ion battery negative material VPO according to claim 1 4preparation method, it is characterized in that: in step (1), described vanadium source is the one in vanadic oxide, ammonium metavanadate, ammonium vanadate, vanadium trioxide, oxalic acid vanadyl.
4. a kind of lithium ion battery negative material VPO according to claim 1 4preparation method, it is characterized in that: in step (1), described phosphorus source is the one in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate, phosphoric acid, pyrophosphoric acid.
5. a kind of lithium ion battery negative material VPO according to claim 1 4preparation method it is characterized in that:, in step (1), described reducing agent is the one in tartaric acid, citric acid, oxalic acid, ethanedioic acid, adipic acid, malonic acid, ascorbic acid.
6. a kind of lithium ion battery negative material VPO according to claim 1 4preparation method it is characterized in that: the one in argon gas that the nonoxidizing atmosphere of sintering is, nitrogen, hydrogen, helium, carbon monoxide.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104091953A (en) * 2014-07-30 2014-10-08 中南大学 Lithium ion battery negative material-vanadium pyrophosphate and preparation method thereof
CN104600253A (en) * 2014-12-31 2015-05-06 北京鼎能开源电池科技股份有限公司 Preparation method of ammonium oxovanadium phosphate crystals
CN104835960A (en) * 2015-05-08 2015-08-12 中南大学 Preparation method for lithium ion battery cathode material VPO4F
CN105185990A (en) * 2015-08-17 2015-12-23 河南理工大学 Preparation method of spherical lithium-ion secondary battery cathode material vanadium phosphate monohydrate
CN107230771A (en) * 2017-07-14 2017-10-03 中南大学 A kind of method of vanadium phosphate coated lithium ion battery anode material nickel cobalt manganic acid lithium
EP3314686A4 (en) * 2015-06-26 2019-08-07 A123 Systems LLC Nanoscale pore structure cathode for high power applications and material synthesis methods
KR20190140900A (en) * 2017-02-01 2019-12-20 유니베르시떼 드 피까르디 줄 베른 Liquid Method for Manufacturing Vanadium Phosphate-Carbon Composites

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JP2004171875A (en) * 2002-11-19 2004-06-17 Sony Corp Negative electrode and battery using it
CN102079517A (en) * 2009-11-29 2011-06-01 宁波大学 Method for preparing fluorizated lithium vanadium phosphate as lithium-ion battery anode material by using spray pyrolysis method
CN102774821A (en) * 2012-07-30 2012-11-14 四川大学 Solid phase-hydrothermal preparation method for lithium vanadium phosphate

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* Cited by examiner, † Cited by third party
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JP2004171875A (en) * 2002-11-19 2004-06-17 Sony Corp Negative electrode and battery using it
CN102079517A (en) * 2009-11-29 2011-06-01 宁波大学 Method for preparing fluorizated lithium vanadium phosphate as lithium-ion battery anode material by using spray pyrolysis method
CN102774821A (en) * 2012-07-30 2012-11-14 四川大学 Solid phase-hydrothermal preparation method for lithium vanadium phosphate

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104091953A (en) * 2014-07-30 2014-10-08 中南大学 Lithium ion battery negative material-vanadium pyrophosphate and preparation method thereof
CN104600253A (en) * 2014-12-31 2015-05-06 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
CN104835960A (en) * 2015-05-08 2015-08-12 中南大学 Preparation method for lithium ion battery cathode material VPO4F
EP3677543A1 (en) * 2015-06-26 2020-07-08 A123 Systems LLC Nanoscale pore structure cathode for high power applications and material synthesis methods
EP3314686A4 (en) * 2015-06-26 2019-08-07 A123 Systems LLC Nanoscale pore structure cathode for high power applications and material synthesis methods
JP2019194150A (en) * 2015-06-26 2019-11-07 エー１２３ システムズ エルエルシーＡ１２３ Ｓｙｓｔｅｍｓ ＬＬＣ Cathode with nanoscale pore structure for high output application and method for material synthesis
US11088389B2 (en) 2015-06-26 2021-08-10 A123 Systems Llc Nanoscale pore structure cathode for high power applications and material synthesis methods
US11916185B2 (en) 2015-06-26 2024-02-27 A123 Systems Llc Nanoscale pore structure cathode for high power applications and material synthesis methods
CN105185990A (en) * 2015-08-17 2015-12-23 河南理工大学 Preparation method of spherical lithium-ion secondary battery cathode material vanadium phosphate monohydrate
KR20190140900A (en) * 2017-02-01 2019-12-20 유니베르시떼 드 피까르디 줄 베른 Liquid Method for Manufacturing Vanadium Phosphate-Carbon Composites
US11569497B2 (en) 2017-02-01 2023-01-31 Centre National De La Recherche Scientifique Liquid process for preparing a vanadium phosphate-carbon composite material
CN107230771A (en) * 2017-07-14 2017-10-03 中南大学 A kind of method of vanadium phosphate coated lithium ion battery anode material nickel cobalt manganic acid lithium
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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