CN107512740B - 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 PDFInfo
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- CN107512740B CN107512740B CN201710756930.3A CN201710756930A CN107512740B CN 107512740 B CN107512740 B CN 107512740B CN 201710756930 A CN201710756930 A CN 201710756930A CN 107512740 B CN107512740 B CN 107512740B
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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
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- 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
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- 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
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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
- 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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- 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
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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
- H01M2004/027—Negative electrodes
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- 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 is comprising steps of surfactant is added in organic solvent, obtain the oil-based system that concentration is 0.05-0.25mol/L, the metavanadate aqueous solution of 0.05-2mol/L and the trivalent Fe saline solution of 0.05-2mol/L are prepared respectively, first metavanadate aqueous solution is added dropwise in oil-based system, stirring, V:Fe=1:1 in molar ratio, trivalent Fe saline solution is added dropwise again, the microemulsion system of stable uniform is obtained after mixing evenly, and it places it 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 air, in 300-700 DEG C roasting 2-20 hours, obtain lithium ion battery negative material FeVO4Nano wire.The method of the present invention is simple, mild condition, prepared FeVO4Nano wire pattern uniformly, stable structure and good conductivity, the discharge capacity of material can be significantly improved, reduce irreversible capacity loss, improve cycle performance and high rate performance.
Description
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 technique
Transition metal vanadate theoretical capacity with higher, safety and low cost, have potential in lithium ion battery
Using.FeVO4As a kind of potential lithium ion battery negative material, due to the hyperoxia of its excellent electronic conductivity and V
Change state, it, which can be provided, compares Ag2V4O11With the higher specific discharge capacity of copper vanadium oxygen (CVO) and energy density.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. people reports
With Fe (NO3)3·9H2O and ammonium metavanadate are that raw material in 180 DEG C of hydro-thermal reaction 5h is prepared for FeVO respectively4·xH2O and
FeVO4·xH2Two kinds of materials of O/ graphene, both materials recycle 100 times under the current density of 100mA/g as the result is shown
Discharge capacity afterwards is 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. people also reported with Fe (NO3)3·9H2O and
Ammonium metavanadate is raw material, and 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 FeVO4Material is modified and is prepared for FeVO4/ grapheme material, both materials are in 100mA/ as the result is shown
Under the current density of g, the discharge capacity after circulation 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)。
Summary of the invention
It is an object of the invention to overcome defect of the existing technology, a kind of lithium ion battery negative material is provided
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, comprising the following steps:
(1)FeVO4The preparation of nanowire precursor: surfactant is added in organic solvent, and obtaining concentration is 0.05-
The oil-based system of 0.25mol/L prepares the soluble metavanadate aqueous solution and 0.05-2mol/L of 0.05-2mol/L respectively
Soluble trivalent Fe saline solution, first soluble metavanadate aqueous solution is added dropwise in oil-based system, stirs, by mole
Than V:Fe=1:1, then soluble trivalent Fe saline solution is added dropwise, obtains the Emulsions of stable uniform after mixing evenly
System, and place it 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
Object and drying, obtain FeVO4Nanowire precursor；
(2)FeVO4The preparation of nano wire: the FeVO that step (1) is prepared4Nanowire precursor is calcined in air, in
It is roasted 2-20 hours under the conditions of 300-700 DEG C, obtains 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 solubility metavanadate is selected from least one of ammonium metavanadate, sodium metavanadate, potassium metavanadate.
The trivalent Fe salt of the 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.
Beneficial effects of the present invention:
1, the present invention prepares lithium ion battery negative material FeVO using evaporative crystallization method4Nano wire, with synthesis in solid state
FeVO4Powder is compared, have better structural stability and electric conductivity, can significantly improve material discharge capacity, reduce can not
Inverse capacitance loss improves cycle performance and high rate performance.
2, FeVO prepared by the present invention4Nano wire is compared to FeVO4Powder body material, specific surface area is relatively large, is applied to lithium
In ion battery, the contact area between material and electrolyte can be increased, to improve the specific discharge capacity of the material.
3, synthetic method of the present invention is simple, mild condition, morphology controllable.
Detailed description of the invention
Fig. 1 is FeVO prepared by embodiment 14The circulation curve graph of nano wire.
Fig. 2 is FeVO prepared by embodiment 14The cyclic curve figure of nano wire.
Specific embodiment
Present invention is further described in detail in the following with reference to the drawings and specific embodiments.
Embodiment 1
(1)FeVO4The preparation of nanowire precursor
First compound concentration is 0.05mol/L NaAOT isooctane solution, then prepares the ammonium metavanadate of 0.05mol/L respectively
The Fe(NO3)39H2O aqueous solution 10mL of aqueous solution 10mL and 0.05mol/L, taking concentration is 0.05mol/LNaAOT isooctane
Solution 20mL is in the beaker of 120mL, stirring, and the ammonium metavanadate aqueous solution 10mL that concentration is 0.05mol/L is added dropwise
In NaAOT isooctane solution, stirring, concentration is again that 0.05mol/L Fe(NO3)39H2O is water-soluble by (V:Fe=1:1) in molar ratio
Liquid 10mL is added dropwise in above-mentioned mixed solution, obtains the microemulsion system of stable uniform after mixing evenly, then it is set by beaker
In in 100 DEG C of air dry oven, solvent will burn its taking-up after being evaporated, with water and alcohol centrifuge washing product and drying, system
Obtain FeVO4The presoma of nano wire.
(2)FeVO4The preparation of nano wire
The presoma that step (1) is prepared is calcined in air, is roasted 4 hours in 500 DEG C, obtains negative electrode of lithium ion battery
Material FeVO4Nano wire.
By FeVO4Nano wire is assembled into CR2016 button cell, through charge-discharge test, in 0.0.1-3.0V voltage range
Interior, discharge capacity is up to 1456mAh/g to material 0.1C multiplying power for the first time, and discharge capacity is up to 821mAh/g to 1C for the first time, such as Fig. 1 institute
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 cetyl trimethylammonium bromide-butanol solution of 0.25mol/L, is then prepared respectively
The ironic citrate aqueous solution 10mL of sodium metavanadate the aqueous solution 10mL and 1mol/L of 1mol/L, taking concentration is 0.25mol/L 16
Alkyl trimethyl ammonium bromide-butanol solution 20mL is in the beaker of 120mL, stirring, the sodium metavanadate for being 1mol/L by concentration
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 mixing evenly
One microemulsion system, then by beaker in its air dry oven for being placed in 160 DEG C, solvent will burn its taking-up after being evaporated, and use
FeVO is made in water and alcohol centrifuge washing product and drying4The presoma of nano wire.
(2)FeVO4The preparation of nano wire
The presoma that step (1) is prepared is calcined in air, is roasted 20 hours in 300 DEG C, it is negative to obtain lithium ion battery
Pole material FeVO4Nano wire.
Embodiment 3
(1)FeVO4The preparation of nanowire precursor
First compound concentration is octyl phenyl polyvinylether-isooctane solution of 0.1mol/L, then prepares 2mol/L respectively
Potassium metavanadate aqueous solution 10mL and 2mol/L Fe(NO3)39H2O aqueous solution 10mL, take concentration be 0.1mol/L octyl
Phenyl polyvinylether-isooctane solution 20mL is in the beaker of 120mL, stirring, and concentration is water-soluble for the potassium metavanadate of 2mol/L
Liquid 10mL is added dropwise in octyl phenyl polyvinylether-isooctane solution, and stirring, (V:Fe=1:1) is again by concentration in molar ratio
It is added dropwise in above-mentioned mixed solution for 2mol/L Fe(NO3)39H2O aqueous solution 10mL, obtains the micro- of stable uniform after mixing evenly
Emulsion system, then by beaker in its air dry oven for being placed in 50 DEG C, solvent will burn its taking-up after being evaporated, with water and alcohol
FeVO is made in centrifuge washing product and drying4The presoma of nano wire.
(2)FeVO4The preparation of nano wire
The presoma that step (1) is prepared is calcined in air, is roasted 2 hours in 700 DEG C, obtains negative electrode of lithium ion battery
Material FeVO4Nano wire.
The above-mentioned description to embodiment is for the ease of those skilled in the art it will be appreciated that and using this
Invention.Person skilled in the art obviously easily can make various modifications to these embodiments, and illustrating herein
General Principle be applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to realities here
Example, those skilled in the art's announcement according to the present invention are applied, improvement and modification made without departing from the scope of the present invention all should
Within protection scope of the present invention.
Claims (5)
1. a kind of lithium ion battery negative material FeVO4The preparation method of nano wire, which comprises the following steps:
(1) FeVO4The preparation of nanowire precursor: surfactant is added in organic solvent, and obtaining concentration is 0.05-
The oil-based system of 0.25mol/L prepares the soluble metavanadate aqueous solution and 0.05-2mol/L of 0.05-2mol/L respectively
Soluble trivalent Fe saline solution, first soluble metavanadate aqueous solution is added dropwise in oil-based system, stirs, by mole
Than V:Fe=1:1, then soluble trivalent Fe saline solution is added dropwise, obtains the microemulsion system of stable uniform after mixing evenly,
And place it in 50-160 DEG C of air dry oven, solvent is drawn off after being evaporated, with water and alcohol centrifuge washing product
And it is dry, obtain FeVO4Nanowire precursor；
(2) FeVO4The preparation of nano wire: the FeVO that step (1) is prepared4Nanowire precursor is calcined in air, in 300-
It is roasted 2-20 hours under the conditions of 700 DEG C, obtains lithium ion battery negative material FeVO4Nano wire.
2. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, which is characterized in that institute
It states surfactant and is selected from Aerosol OT (NaAOT), lauryl sodium sulfate, cetyl trimethyl bromination
At least one of ammonium (CTAB), octyl phenyl polyvinylether (Triton X-100).
3. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, which is characterized in that institute
It states organic solvent and is selected from least one of isooctane, n-hexane, dimethylbenzene, n-butanol, n-amyl alcohol, n-hexyl alcohol.
4. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, which is characterized in that institute
It states soluble metavanadate and is selected from least one of ammonium metavanadate, sodium metavanadate, potassium metavanadate.
5. lithium ion battery negative material FeVO according to claim 14The preparation method of nano wire, which is characterized in that institute
It states soluble trivalent Fe salt and 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111048778B (en) * | 2019-10-28 | 2022-06-24 | 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 |
| CN111900389B (en) * | 2020-05-26 | 2022-06-14 | 北京理工大学 | Fe2VO4Ordered mesoporous carbon composite material 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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| CN101913651B (en) * | 2010-07-30 | 2011-12-21 | 北京工业大学 | Hydrothermal method for preparing triclinic-phase FeVO4 micro particles |
| CN103022486B (en) * | 2012-12-19 | 2015-10-07 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of anode material for lithium-ion batteries |
| CN103570067B (en) * | 2013-11-15 | 2015-08-05 | 合肥国轩高科动力能源股份公司 | With the method for evaporative crystallization legal system for copper vanadium oxygen nano structural material |
| CN103825025B (en) * | 2014-02-27 | 2016-01-27 | 三峡大学 | A kind of lithium ion battery negative material FeVO4 and preparation method thereof |
| CN105958068B (en) * | 2016-07-21 | 2017-06-27 | 中南大学 | A kind of preparation method of nano bar-shape lithium ion battery negative material ferric vandate |
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