CN105655586A - Low-energy-consumption method for preparing lithium vanadium fluorophosphate as positive electrode material for lithium-ion battery - Google Patents

Low-energy-consumption method for preparing lithium vanadium fluorophosphate as positive electrode material for lithium-ion battery Download PDF

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Publication number
CN105655586A
CN105655586A CN201610174101.XA CN201610174101A CN105655586A CN 105655586 A CN105655586 A CN 105655586A CN 201610174101 A CN201610174101 A CN 201610174101A CN 105655586 A CN105655586 A CN 105655586A
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lithium
vanadium
carbon
phosphate
preparation
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余爱水
苏俊铭
赵嘉悦
张聪聪
李良昱
陈春光
黄桃
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Fudan University
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Fudan 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
    • 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)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention belongs to the technical field of lithium-ion batteries, in particular to a low-energy-consumption method for preparing lithium vanadium fluorophosphate as a positive electrode material for a lithium-ion battery. The method mainly comprises the steps of preparing a compound precursor of vanadium phosphate and carbon by a carbon thermal reduction method, and preparing a compound of lithium vanadium fluorophosphate and carbon by a high-temperature sintering method. The preparation process has the advantages that the energy consumption is low, the cost is low and the time is short, and the side effects in the preparation process are effectively controlled. The precursor prepared by the first-step carbon thermal reduction method has a relatively small particle size of about 100 nm, and carbon obtained by carbon source decomposition is used to coat the surface of the precursor, thereby helping the thorough conduction of the second-step sintering reaction and improving the electronic conductivity of a final product; the lithium vanadium fluorophosphate product prepared by final sintering is in a loose block state, and the cost of post mechanical polishing in the industry is greatly saved.

Description

A kind of low energy consumption preparation method of lithium ion battery anode material vanadium lithium phosphate
Technical field
The invention belongs to technical field of lithium ion, be specifically related to a kind of anode material for lithium-ion batteries LiVPO4The preparation method of FC.
Background technology
Within 2003, J.Barker delivers first section about LiVPO4F is as the paper of anode material for lithium-ion batteries, it was shown that LiVPO4F is a kind of novel anode material for lithium-ion batteries. LiVPO4F inherits polyanion group positive electrode LiMPO4The structural stability that (M=Fe, Co, Mn etc.) are good, it is possible at high temperature stable circulation. Meanwhile, LiVPO4F V in removal lithium embedded behavior3+/V4+Current potential is up to 4.2V, higher than general LiMPO4Positive electrode. And China's vanadium resource enriches, the annual production of barium oxide is high, with low cost, therefore LiVPO4F is an anode material for lithium-ion batteries with huge potential using value.
LiVPO4F is because of the introducing of fluorine element so that the resistance to elevated temperatures of material relatively LiMPO4Promote further. Also make LiMPO simultaneously4The structure of itself is changed into the three-dimensional lithium ion tunnel being connected two one-dimensional polyhedron chains by fluorion and formed by one-dimensional lithium ion tunnel, and this makes LiVPO4F is compared to LiMPO4There is better lithium ion transport speed and ionic conductivity, and then ensure that the high-rate charge-discharge capability of material itself. Also just owing to this structure changes so that LiVPO4The electronic conductivity of F is lower than LiMPO4. Therefore, LiVPO is improved4The electronic conductivity of F positive electrode becomes its essential condition that can be commercial. And in all synthetic schemes reported now, final calcining preparation pure phase LiVPO4The step of F is required for pass into noble gas protect, to prevent the generation of the by-products such as vanadyl phosphate lithium, phosphoric acid vanadium lithium. Therefore, the difficulty in synthesis also limit the application in lithium ion battery of this material.
The present invention is prepared for LiVPO by two-step sintering4FC composite, technique is simple, and the prices of raw materials are cheap, and the material particle size obtained is at 0.2-1 ��m, shorten lithium ion transmission path in positive pole. And LiVPO4F material surface has carbon granule to be combined with each other, and considerably increases the electronic conductivity that material is overall. The LiVPO that the present invention prepares4F thing is mutually single, Stability Analysis of Structures, has good chemical property.
Summary of the invention
What it is an object of the invention to provide a kind of simplicity prepares anode material for lithium-ion batteries LiVPO4The method of F, to reduce LiVPO4The synthesis cost of F material, improves the electronic conductivity of material, improves its chemical property, improve its commercial feasibility.
Technical scheme is as follows:
(1) by the ratio premixing in vanadium source and phosphorus source 1:1 in molar ratio, it is fully ground again after adding the carbon source of vanadium source molal quantity 1-5 times so that it is mix homogeneously;
(2) use powder compressing machine that mixture is pressed into lamellar, be placed in tube furnace, pass to protective gas, at 350-850 DEG C, calcine 3-12h, obtain the complex precursor of vanadium phosphate and carbon, be designated as VPO4C;
(3) by VPO4C is sufficiently mixed with lithium source and fluorine source, then uses powder compressing machine to be pressed into lamellar, is placed in tube furnace or Muffle furnace, and logical or obstructed protective gas is calcined 0.5-5h at 350-850 DEG C, obtained the complex of fluorophosphoric acid vanadium lithium and carbon, be designated as LiVPO4FC��
Vanadium source described in step of the present invention (1) is selected from Vanadium sesquioxide, vanadium dioxide, four oxidation three vanadium, vanadic anhydride, ammonium metavanadate, vanadyl oxalate.
Step of the present invention (1) phosphorus source is selected from ammonium phosphate, diammonium phosphate, ammonium dihydrogen phosphate, lithium phosphate, ammonium polyphosphate.
Step of the present invention (1) described carbon source is selected from Delanium, Colophonium, superP, sucrose, glucose.
The protective gas passed in step of the present invention (2), (3) is the one in nitrogen, argon, hydrogen-argon-mixed, hydrogen, artificial air.
The described lithium source of step of the present invention (3) is selected from lithium phosphate, lithium carbonate, lithium oxalate, lithium fluoride, Lithium hydrate, lithium nitrate.
The described fluorine source of step of the present invention (1) is selected from ammonium fluoride, potassium fluoride, lithium fluoride, sodium fluoride, Fluohydric acid..
Advantages of the present invention:
Tradition two steps annealing method is prepared LiVPO by the present invention4The improvement of F, by making solid state reaction during high temperature sintering more abundant mixture tabletting before calcining. Use the LiVPO that this programme prepares4FC positive electrode particle diameter is 0.2-1 ��m, shortens lithium ion transmission path in positive pole. And the carbon that material surface (2) situ in steps generates is compounded in LiVPO4On F granule, considerably increase the electronic conductivity that material is overall. The LiVPO that the present invention prepares4F thing is mutually single, Stability Analysis of Structures, has good chemical property.
The precursor that the first step carbon thermal reduction of the present invention prepares has less particle size, about 100nm, and carbon source is decomposed the carbon obtained and is coated on precursor surface, is conducive to second step sintering reaction thoroughly to carry out and improves the electronic conductivity of end product. The present invention finally sinters the fluorophosphoric acid vanadium lithium product prepared in loose bulk, is greatly saved the cost of industrial later stage mechanical lapping.
Accompanying drawing explanation
Fig. 1 is the XRD diffraction pattern of each product in embodiment 2.
Fig. 2 is capacity and the efficiency curve of end product discharge and recharge under 0.1C multiplying power in embodiment 2.
Fig. 3 is the TEM image of precursor in embodiment 2.
Fig. 4 is the TEM image of end product in embodiment 2.
Detailed description of the invention
Further describe the present invention hereafter by specific embodiment in conjunction with accompanying drawing, be not intended that limitation of the present invention.
Embodiment 1
(1) weigh vanadic anhydride 1.82g, diammonium phosphate 2.65g, glucose 1.2g, be placed in agate mortar and grind uniform post-drying, use powder compressing machine that mixture is pressed into lamellar;
(2) being placed in corundum crucible by lamellar reactant, be placed in tube furnace, logical argon, as protective gas, at 550 DEG C, 650 DEG C, 750 DEG C, 850 DEG C, obtains the complex precursor VPO of vanadium phosphate and carbon after high temperature sintering 2,4,6,8h at 950 DEG C4C;
(3) weigh the VPO4C2.92g prepared in (2), add Lithium hydrate 0.48g, ammonium fluoride 0.74g, be placed in agate mortar and grind uniform post-drying. Powder compressing machine is used to be compressed to lamellar by grinding the reactant powders obtained;
(4) being placed in corundum crucible by lamellar reactant, be placed in tube furnace, logical argon is as protective gas, at 550 DEG C; 650 DEG C, 750 DEG C, 850 DEG C, high temperature sintering 0.5 at 950 DEG C; it is cooled to room temperature after 2,4h, obtains the complex LiVPO of fluorophosphoric acid vanadium lithium and carbon4FC��
Embodiment 2
(1) weigh ammonium metavanadate 2.34g, ammonium dihydrogen phosphate 2.3g, superP0.48g, be placed in agate mortar and grind uniform post-drying, use powder compressing machine that mixture is pressed into lamellar;
(2) being placed in corundum crucible by lamellar reactant, be placed in tube furnace, logical nitrogen, as protective gas, at 550 DEG C, 650 DEG C, 750 DEG C, 850 DEG C, obtains the complex precursor VPO of vanadium phosphate and carbon after high temperature sintering 2,4,6,8h at 950 DEG C4C;
(3) weigh the VPO4C2.92g prepared in (2), add lithium fluoride 0.52g, be placed in agate mortar and grind uniform post-drying. Powder compressing machine is used to be compressed to lamellar by grinding the reactant powders obtained;
(4) lamellar reactant is placed in corundum crucible, is placed in Muffle furnace, at 550 DEG C, 650 DEG C, 750 DEG C, 850 DEG C, at 950 DEG C after high temperature sintering 0.5,2,4h, take out immediately, be quickly cooled to room temperature, obtain the complex LiVPO of fluorophosphoric acid vanadium lithium and carbon4FC��
Embodiment 3
(1) weigh vanadyl oxalate 4.9g, ammonium phosphate 4.06g, Delanium 0.48g, be placed in agate mortar and grind uniform post-drying, use powder compressing machine that mixture is pressed into lamellar;
(2) being placed in corundum crucible by lamellar reactant, be placed in tube furnace, logical nitrogen, as protective gas, at 550 DEG C, 650 DEG C, 750 DEG C, 850 DEG C, obtains the complex precursor VPO of vanadium phosphate and carbon after high temperature sintering 2,4,6,8h at 950 DEG C4C;
(3) weigh the VPO4C2.92g prepared in (2), add lithium carbonate 0.74g, ammonium fluoride 0.74g, be placed in agate mortar and grind uniform post-drying. Powder compressing machine is used to be compressed to lamellar by grinding the reactant powders obtained;
(4) being placed in corundum crucible by lamellar reactant, be placed in tube furnace, logical argon is as protective gas, at 550 DEG C; 650 DEG C, 750 DEG C, 850 DEG C, high temperature sintering 0.5 at 950 DEG C; it is cooled to room temperature after 2,4h, obtains the complex LiVPO of fluorophosphoric acid vanadium lithium and carbon4FC��
Wherein, the pattern of embodiment 2 product and electrology characteristic are shown in shown in accompanying drawing 1-4. The pattern of all the other embodiment products is similar with embodiment 2 with electrology characteristic.

Claims (7)

1. the low energy consumption preparation method of a lithium ion battery anode material vanadium lithium phosphate, it is characterised in that concretely comprise the following steps:
(1) by the ratio premixing in vanadium source and phosphorus source 1:1 in molar ratio, it is fully ground again after adding the carbon source of vanadium source molal quantity 1-5 times so that it is mix homogeneously;
(2) use powder compressing machine that mixture is pressed into lamellar, be placed in tube furnace, pass to protective gas, at 350-850 DEG C, calcine 3-12h, obtain the complex precursor of vanadium phosphate and carbon, be designated as VPO4C;
(3) by VPO4C is sufficiently mixed with lithium source and fluorine source, then uses powder compressing machine to be pressed into lamellar, is placed in tube furnace or Muffle furnace, and logical or obstructed protective gas is calcined 0.5-5h at 350-850 DEG C, obtained the complex of fluorophosphoric acid vanadium lithium and carbon, be designated as LiVPO4FC��
2. preparation method according to claim 1, it is characterised in that the vanadium source used in step (1) is selected from Vanadium sesquioxide, vanadium dioxide, four oxidation three vanadium, vanadic anhydride, ammonium metavanadate, vanadyl oxalate.
3. preparation method according to claim 1 and 2, it is characterised in that the phosphorus source used in step (1) is selected from ammonium phosphate, diammonium phosphate, ammonium dihydrogen phosphate, lithium phosphate, ammonium polyphosphate.
4. preparation method according to claim 3, it is characterised in that the carbon source used in step (1) is in Delanium, Colophonium, superP, sucrose, glucose.
5. the preparation method according to claim 1,2 or 4, it is characterised in that the protective gas passed in step (2), (3) is the one in nitrogen, argon, hydrogen-argon-mixed, hydrogen, artificial air.
6. preparation method according to claim 5, it is characterised in that the lithium source used in step (3) is selected from lithium phosphate, lithium carbonate, lithium oxalate, lithium fluoride, Lithium hydrate, lithium nitrate.
7. the preparation method according to claim 1,2,4 or 6, it is characterised in that the fluorine source used in step (3) is selected from ammonium fluoride, potassium fluoride, lithium fluoride, sodium fluoride, Fluohydric acid..
CN201610174101.XA 2016-03-24 2016-03-24 Low-energy-consumption method for preparing lithium vanadium fluorophosphate as positive electrode material for lithium-ion battery Pending CN105655586A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108461751A (en) * 2018-03-31 2018-08-28 广东天劲新能源科技股份有限公司 A kind of preparation method of mesoporous vanadium phosphate cathode material
CN108666558A (en) * 2018-07-12 2018-10-16 西安交通大学 A kind of bilayer carbon coating prepares the preparation method of lithium vanadium fluorophosphates lithium ionic cell anode material
CN109755514A (en) * 2018-12-27 2019-05-14 大连博融新材料有限公司 A kind of carbon coating lithium vanadium fluorophosphates lithium ionic cell anode material and preparation method thereof
CN111072002A (en) * 2019-12-20 2020-04-28 大连博融新材料有限公司 Vanadium phosphate, preparation method thereof and application thereof in lithium ion battery anode material
CN111072004A (en) * 2019-12-20 2020-04-28 大连博融新材料有限公司 Sodium-doped lithium vanadium fluorophosphate material, and preparation method and application thereof
CN112864358A (en) * 2019-11-27 2021-05-28 中国科学院大连化学物理研究所 Vanadium-based polyanion compound prepared by one-step method and application thereof
WO2023203383A1 (en) * 2022-04-19 2023-10-26 Lithium Werks Technology Bv Methods for preparation of electroactive lithium mixed metal materials for high energy density batteries

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CN103022481A (en) * 2011-09-21 2013-04-03 富士重工业株式会社 Positive electrode active material production method, positive electrode, and storage device

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108461751A (en) * 2018-03-31 2018-08-28 广东天劲新能源科技股份有限公司 A kind of preparation method of mesoporous vanadium phosphate cathode material
CN108461751B (en) * 2018-03-31 2022-10-11 广东天劲新能源科技股份有限公司 Preparation method of mesoporous lithium vanadium phosphate cathode material
CN108666558A (en) * 2018-07-12 2018-10-16 西安交通大学 A kind of bilayer carbon coating prepares the preparation method of lithium vanadium fluorophosphates lithium ionic cell anode material
CN109755514A (en) * 2018-12-27 2019-05-14 大连博融新材料有限公司 A kind of carbon coating lithium vanadium fluorophosphates lithium ionic cell anode material and preparation method thereof
CN109755514B (en) * 2018-12-27 2021-10-26 大连博融新材料有限公司 Carbon-coated lithium vanadium fluorophosphate lithium-ion battery positive electrode material and preparation method thereof
CN112864358A (en) * 2019-11-27 2021-05-28 中国科学院大连化学物理研究所 Vanadium-based polyanion compound prepared by one-step method and application thereof
CN112864358B (en) * 2019-11-27 2023-11-07 中国科学院大连化学物理研究所 Vanadium-based polyanion compound prepared by one-step method and application thereof
CN111072002A (en) * 2019-12-20 2020-04-28 大连博融新材料有限公司 Vanadium phosphate, preparation method thereof and application thereof in lithium ion battery anode material
CN111072004A (en) * 2019-12-20 2020-04-28 大连博融新材料有限公司 Sodium-doped lithium vanadium fluorophosphate material, and preparation method and application thereof
WO2023203383A1 (en) * 2022-04-19 2023-10-26 Lithium Werks Technology Bv Methods for preparation of electroactive lithium mixed metal materials for high energy density batteries

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