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 PDFInfo
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- 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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- 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
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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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
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)
- 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. 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. 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. 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. 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)
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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Cited By (5)
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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