CN107512740A - A kind of lithium ion battery negative material FeVO4The preparation method of nano wire - Google Patents

A kind of lithium ion battery negative material FeVO4The preparation method of nano wire Download PDF

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Publication number
CN107512740A
CN107512740A CN201710756930.3A CN201710756930A CN107512740A CN 107512740 A CN107512740 A CN 107512740A CN 201710756930 A CN201710756930 A CN 201710756930A CN 107512740 A CN107512740 A CN 107512740A
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fevo
nano wire
lithium ion
ion battery
preparation
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CN107512740B (en
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曾晖
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Hefei Gotion High Tech Power Energy Co Ltd
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Hefei Guoxuan High Tech Power Energy Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • 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 present invention discloses a kind of lithium ion battery negative material FeVO4The preparation method of nano wire, it includes step：Surfactant is added in organic solvent, the oil-based system that concentration is 0.05 0.25mol/L is obtained, the 0.05 2mol/L metavanadate aqueous solution and 0.05 2mol/L trivalent Fe saline solutions is prepared respectively, first the metavanadate aqueous solution is added dropwise in oil-based system, stir, in molar ratio V:Fe=1:1, then trivalent Fe saline solutions are added dropwise, the microemulsion system of stable uniform is obtained after stirring, and be placed in 50 160 DEG C of air dry oven, solvent is drawn off after being evaporated, with water and alcohol centrifuge washing product and drying；Presoma is calcined in atmosphere, is calcined 2 20 hours in 300 700 DEG C, obtains lithium ion battery negative material FeVO4Nano wire.The inventive method is simple, mild condition, prepared FeVO4Nano wire pattern uniformly, Stability Analysis of Structures and good conductivity, the discharge capacity of material can be significantly improved, reduce irreversible capacity loss, improve cycle performance and high rate performance.

Description

A kind of lithium ion battery negative material FeVO4The preparation method of nano wire
Technical field
The present invention relates to technical field of lithium ion, specifically a kind of lithium ion battery negative material FeVO4Nano wire Preparation method.
Background technology
Transition metal vanadate has higher theoretical capacity, security and low cost, has in lithium ion battery potential Using.FeVO4As a kind of potential lithium ion battery negative material, due to its excellent electronic conductivity and V hyperoxia Change state, it, which can be provided, compares Ag2V4O11Higher specific discharge capacity and energy density with copper vanadium oxygen (CVO).Meanwhile relative to silver Vanadium oxygen (SVO) and copper vanadium oxygen (CVO), FeVO4Cost of material it is lower.In recent years, FeVO4As lithium ion battery negative material Cause concern.
Common preparation FeVO4The method of nano wire has hydro-thermal method, solid phase method and sol-gal process.Liu et al. is reported With Fe (NO3)3·9H2O and ammonium metavanadate are raw material, in 180 DEG C of hydro-thermal reaction 5h, are prepared for FeVO respectively4·xH2O and FeVO4·xH2Two kinds of materials of O/ graphenes, as a result show both materials under 100mA/g current density, after circulating 100 times Discharge capacity be respectively 455.4 and 1407.8mAh/g (Synthesis and electrochemical performances of FeVO4·xH2O and FeVO4·xH2O/graphene as novel anode materials[J].Materials Letters,2017,187,15–19.).In addition, Liu et al. also reported with Fe (NO3)3·9H2O and ammonium metavanadate are raw material, After 160 DEG C of hydro-thermal reaction 5h, 500 DEG C of calcining 2h, are prepared for FeVO in air atmosphere4Material, and with graphene to FeVO4 Material is modified and is prepared for FeVO4/ grapheme material, both materials are as a result shown under 100mA/g current density, Discharge capacity after circulating 100 times is respectively 405.2 and 1046.5mAh/g (Synthesis and modification of FeVO4as novel anode for lithium-ion batteries[J].Applied Surface Science, 2017,394,183–189)。
The content of the invention
A kind of the defects of it is an object of the invention to overcome prior art to exist, there is provided lithium ion battery negative material FeVO4The preparation method of nano wire.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of lithium ion battery negative material FeVO4The preparation method of nano wire, comprises the following steps：
(1)FeVO4The preparation of nanowire precursor：Surfactant is added in organic solvent, it is 0.05- to obtain concentration 0.25mol/L oil-based system, the 0.05-2mol/L soluble metavanadate aqueous solution and 0.05-2mol/L are prepared respectively Soluble trivalent Fe saline solutions, first the soluble metavanadate aqueous solution is added dropwise in oil-based system, is stirred, by mole Compare V:Fe=1:1, then the trivalent Fe saline solutions of solubility are added dropwise, the Emulsions of stable uniform are obtained after stirring System, and be placed in 50-160 DEG C of air dry oven, solvent is drawn off after being evaporated, and is produced with water and alcohol centrifuge washing Thing and drying, obtain FeVO4Nanowire precursor；
(2)FeVO4The preparation of nano wire：The FeVO that step (1) is prepared4Nanowire precursor is calcined in atmosphere, in 2-20 hours are calcined under the conditions of 300-700 DEG C, obtain lithium ion battery negative material FeVO4Nano wire.
The surfactant is selected from Aerosol OT (NaAOT), lauryl sodium sulfate, cetyl At least one of trimethylammonium bromide (CTAB), octyl phenyl polyvinylether (Triton X-100).
The organic solvent in isooctane, n-hexane, dimethylbenzene, n-butanol, n-amyl alcohol, n-hexyl alcohol at least one Kind.
The soluble metavanadate is selected from least one of ammonium metavanadate, sodium metavanadate, potassium metavanadate.
The soluble trivalent Fe salt is selected from Fe(NO3)39H2O (Fe (NO3)3·9H2O), Iron(III) chloride hexahydrate (FeCl3·6H2O), at least one of ironic citrate, ferric citrate.
Beneficial effects of the present invention：
1st, the present invention prepares lithium ion battery negative material FeVO using evaporative crystallization method4Nano wire, with synthesis in solid state FeVO4Powder is compared, and has more preferable structural stability and electric conductivity, can significantly improve material discharge capacity, reduce can not Inverse capacitance loss, improve cycle performance and high rate performance.
2nd, FeVO prepared by the present invention4Nano wire is compared to FeVO4Powder body material, specific surface area is relatively large, applied to lithium In ion battery, the contact area between material and electrolyte can be increased, so as to improve the specific discharge capacity of the material.
3rd, synthetic method of the present invention is simple, mild condition, morphology controllable.
Brief description of the drawings
Fig. 1 is FeVO prepared by embodiment 14The circulation curve map of nano wire.
Fig. 2 is FeVO prepared by embodiment 14The cyclic curve figure of nano wire.
Embodiment
The present invention is described in further detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
(1)FeVO4The preparation of nanowire precursor
First compound concentration is 0.05mol/L NaAOT isooctane solutions, then prepares 0.05mol/L ammonium metavanadate respectively Aqueous solution 10mL, and 0.05mol/L Fe(NO3)39H2O aqueous solution 10mL, take concentration molten for 0.05mol/LNaAOT isooctane Liquid 20mL is in 120mL beaker, stirring, and the ammonium metavanadate aqueous solution 10mL that concentration is 0.05mol/L is added dropwise into NaAOT In isooctane solution, stir, in molar ratio (V:Fe=1:1) by concentration it is again the 0.05mol/L Fe(NO3)39H2O aqueous solution 10mL is added dropwise in above-mentioned mixed solution, the microemulsion system of stable uniform is obtained after stirring, then it is placed in by beaker In 100 DEG C of air dry oven, solvent will burn its taking-up after being evaporated, and with water and alcohol centrifuge washing product and drying, be made FeVO4The presoma of nano wire.
(2)FeVO4The preparation of nano wire
The presoma that step (1) is prepared is calcined in atmosphere, is calcined 4 hours in 500 DEG C, obtains negative electrode of lithium ion battery Material FeVO4Nano wire.
By FeVO4Nano wire is assembled into CR2016 button cells, through charge-discharge test, in 0.0.1-3.0V voltage ranges Interior, discharge capacity is up to 1456mAh/g to material 0.1C multiplying powers first, and discharge capacity is up to 821mAh/g to 1C first, such as Fig. 1 institutes Show, the specific discharge capacity after 0.1 circulation 50 times is 1085mAh/g, as shown in Figure 2.
Embodiment 2
(1)FeVO4The preparation of nanowire precursor
First compound concentration is 0.25mol/L cetyl trimethylammonium bromide-butanol solution, is then prepared respectively 1mol/L sodium metavanadate aqueous solution 10mL, and 1mol/L ironic citrate aqueous solution 10mL, it is 0.25mol/L 16 to take concentration Alkyl trimethyl ammonium bromide-butanol solution 20mL is in 120mL beaker, stirring, by the sodium metavanadate that concentration is 1mol/L Aqueous solution 10mL is added dropwise in cetyl trimethylammonium bromide-butanol solution, stirring, in molar ratio (V:Fe=1:1) The ironic citrate aqueous solution 10mL that concentration is 1mol/L is added dropwise in above-mentioned mixed solution again, must be stablized after stirring One microemulsion system, then by beaker, it is placed in 160 DEG C of air dry oven, and solvent will burn its taking-up after being evaporated, and is used Water and alcohol centrifuge washing product and drying, FeVO is made4The presoma of nano wire.
(2)FeVO4The preparation of nano wire
The presoma that step (1) is prepared is calcined in atmosphere, is calcined 20 hours in 300 DEG C, is obtained lithium ion battery and bear Pole material FeVO4Nano wire.
Embodiment 3
(1)FeVO4The preparation of nanowire precursor
First compound concentration is 0.1mol/L octyl phenyl polyvinylether-isooctane solution, then prepares 2mol/L respectively Potassium metavanadate aqueous solution 10mL, and 2mol/L Fe(NO3)39H2O aqueous solution 10mL, take the octyl group that concentration is 0.1mol/L Phenyl polyvinylether-isooctane solution 20mL is in 120mL beaker, stirring, and concentration is water-soluble for 2mol/L potassium metavanadate Liquid 10mL is added dropwise in octyl phenyl polyvinylether-isooctane solution, stirring, in molar ratio (V:Fe=1:1) again by concentration It is added dropwise for 2mol/L Fe(NO3)39H2O aqueous solution 10mL in above-mentioned mixed solution, the micro- of stable uniform is obtained after stirring Emulsion system, then by beaker, it is placed in 50 DEG C of air dry oven, and solvent will burn its taking-up after being evaporated, with water and alcohol Centrifuge washing product and drying, FeVO is made4The presoma of nano wire.
(2)FeVO4The preparation of nano wire
The presoma that step (1) is prepared is calcined in atmosphere, is calcined 2 hours in 700 DEG C, obtains negative electrode of lithium ion battery Material FeVO4Nano wire.
The above-mentioned description to embodiment is it will be appreciated that and using this for the ease of those skilled in the art Invention.Person skilled in the art obviously can easily make various modifications to these embodiments, and illustrating herein General Principle be applied in other embodiment without by performing creative labour.Therefore, the invention is not restricted to reality here Apply example, those skilled in the art do not depart from improvement that scope made and modification all should according to the announcement of the present invention Within protection scope of the present invention.

Claims (5)

  1. A kind of 1. lithium ion battery negative material FeVO4The preparation method of nano wire, it is characterised in that comprise the following steps：
    （1）FeVO4The preparation of nanowire precursor：Surfactant is added in organic solvent, it is 0.05- to obtain concentration 0.25mol/L oil-based system, the 0.05-2mol/L soluble metavanadate aqueous solution and 0.05-2mol/L are prepared respectively Soluble trivalent Fe saline solutions, first the soluble metavanadate aqueous solution is added dropwise in oil-based system, is stirred, by mole Compare V:Fe=1:1, then the trivalent Fe saline solutions of solubility are added dropwise, the microemulsion system of stable uniform is obtained after stirring, And be placed in 50-160 DEG C of air dry oven, solvent is drawn off after being evaporated, with water and alcohol centrifuge washing product And dry, obtain FeVO4Nanowire precursor；
    （2）FeVO4The preparation of nano wire：By step（1）The FeVO prepared4Nanowire precursor is calcined in atmosphere, in 300- 2-20 hours are calcined under the conditions of 700 DEG C, obtain lithium ion battery negative material FeVO4Nano wire.
  2. 2. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, it is characterised in that institute State surfactant and be selected from Aerosol OT（NaAOT）, lauryl sodium sulfate, cetyl trimethyl bromination Ammonium（CTAB）, octyl phenyl polyvinylether（Triton X-100）At least one of.
  3. 3. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, it is characterised in that institute State organic solvent and be selected from least one of isooctane, n-hexane, dimethylbenzene, n-butanol, n-amyl alcohol, n-hexyl alcohol.
  4. 4. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, it is characterised in that institute State soluble metavanadate and be selected from least one of ammonium metavanadate, sodium metavanadate, potassium metavanadate.
  5. 5. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, it is characterised in that institute The trivalent Fe salt for stating solubility is selected from Fe(NO3)39H2O（Fe(NO3)3·9H2O）, Iron(III) chloride hexahydrate（FeCl3·6H2O）、 At least one of ironic citrate, ferric citrate.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111048778A (en) * 2019-10-28 2020-04-21 宁波职业技术学院 Doped modified lithium ion battery vanadate anode material and preparation method thereof
CN111689524A (en) * 2020-04-28 2020-09-22 青海民族大学 Lithium ion battery material FeVO4Process for producing microparticles
CN111841606A (en) * 2020-07-23 2020-10-30 中国环境科学研究院 Heterogeneous FeVO4Catalytic material, preparation method and application thereof
CN111900389A (en) * 2020-05-26 2020-11-06 北京理工大学 Fe2VO4Ordered mesoporous carbon composite material and application thereof

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CN103570067A (en) * 2013-11-15 2014-02-12 合肥国轩高科动力能源股份公司 Method for preparing copper vanadium oxide nano structure material by evaporative crystallization method
CN103825025A (en) * 2014-02-27 2014-05-28 三峡大学 Negative electrode material FeVO4 of lithium ion battery and preparation method thereof
CN105958068A (en) * 2016-07-21 2016-09-21 中南大学 Preparation method of nanorod negative electrode material ferric vanadate for lithium-ion battery

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CN101913651A (en) * 2010-07-30 2010-12-15 北京工业大学 Hydrothermal method for preparing triclinic-phase FeVO4 micro particles
CN103022486A (en) * 2012-12-19 2013-04-03 中国科学院宁波材料技术与工程研究所 Preparation method for anode material of lithium ion battery
CN103570067A (en) * 2013-11-15 2014-02-12 合肥国轩高科动力能源股份公司 Method for preparing copper vanadium oxide nano structure material by evaporative crystallization method
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CN105958068A (en) * 2016-07-21 2016-09-21 中南大学 Preparation method of nanorod negative electrode material ferric vanadate for lithium-ion battery

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111048778A (en) * 2019-10-28 2020-04-21 宁波职业技术学院 Doped modified lithium ion battery vanadate anode material and preparation method thereof
CN111689524A (en) * 2020-04-28 2020-09-22 青海民族大学 Lithium ion battery material FeVO4Process for producing microparticles
CN111900389A (en) * 2020-05-26 2020-11-06 北京理工大学 Fe2VO4Ordered mesoporous carbon composite material and application thereof
CN111841606A (en) * 2020-07-23 2020-10-30 中国环境科学研究院 Heterogeneous FeVO4Catalytic material, preparation method and application thereof
CN111841606B (en) * 2020-07-23 2021-03-12 中国环境科学研究院 Heterogeneous FeVO4Catalytic material, preparation method and application thereof

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