CN105836800A - Synthetic method for dimension-controllable vanadium dioxide nano material, and lithium ion battery - Google Patents
Synthetic method for dimension-controllable vanadium dioxide nano material, and lithium ion battery Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
- C01G31/02—Oxides
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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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
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- 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 synthetic method for a dimension-controllable vanadium dioxide nano material, wherein the VO2(B) nano materials in different dimensions can be controllably synthesized through a novel high-temperature mixed hydrothermal method, wherein the VO2(B) nano materials include one-dimensional (1D) VO2(B) nano belts, two-dimensional (2D) VO2(B) nano sheets, and three-dimensional (3D) hierarchical porous carbon-coated VO2(B) (VO2(B)@C) micro-nano structures. The material can be widely used as electrode materials in a lithium ion battery, wherein the three-dimensional (3D) hierarchical porous VO2(B)@C micro-nano structures have excellent electrochemical performances. The technology has very great application prospect.
Description
Technical field
The present invention relates to a kind of by high temperature mixing water full-boiled process controlledly synthesis different dimensions VO2(B) side of nano material
Method, including one-dimensional (1D) VO2(B) nano belt, two dimension (2D) VO2(B) nanometer sheet and three-dimensional (3D) graded porous carbon are coated with
VO2(B) (VO2(B)@C) micro-nano structure, the material prepared may be used for lithium ion battery electrode material, belongs to energy storage
Material Field.
Background technology
Along with the exhaustion day by day of the Fossil fuel with coal, oil, natural gas etc. as representative, and these conventional fossil fuel
Greenhouse effect, the environmental problem such as atmospheric pollution that burning is brought are increasingly sharpened, and set up with cleaning, reproducible new forms of energy as base
The novel energy structure of plinth is then one of the most material technical field in World Economics from now on.At this novel energy
In structure, energy storage is then seized of great proportion, and will play vital effect.In numerous energy storage technologies, lithium from
Sub-battery is excellent owing to having high-energy-density, long circulation life, memory-less effect, low self-discharge, good environment friendly etc.
Point is it is considered to be most potential energy storing technology, and portable with mobile communication and notebook computer as representative
Electronic equipment is widely used.Fast recently as the extensive stored energy application such as pure electric automobile, intelligent grid
Hailing exhibition, it is the selection of ideal electrokinetic cell that lithium ion battery is also recognized.State Council passed through in " energy-conservation in 2012
With new-energy automobile industrial development planning (2012-2020) ", and explicitly point out with pure electric drive for auto industry make the transition main
Strategic decisions.The Ministry of Science and Technology is further combined with " National Program for Medium-to Long-term Scientific and Technological Development (2006-2020) "
With State Council's " instruction about accelerating new-energy automobile popularization and application " the state key research and development plan issued 2016
Spend and first 6 projects just contain " new-energy automobile " pilot special project, and clearly propose the property of power lithium-ion battery
Can index.Therefore, it is not difficult to find out that these new extensive stored energy application also propose new challenge to lithium ion battery, it is desirable to lithium
Ion battery has the most excellent chemical property (including longer cycle life, higher energy and power density).
In order to improve the chemical property of lithium ion battery further, design the most excellent electrode material and then seem outstanding
For key.VO2(B) it is a kind of typical stratiform transition group metallic oxide, there are energy density height, structure easy-regulating, reserves
The series of advantages such as abundant, with low cost, environmental friendliness are it is considered to be the lithium ion battery electrode material of a kind of great potential.
The electrode material of business-like lithium ion battery is mostly micro materials, and the electro-chemical activity of these micro materials is limited, thus
Limiting the lithium storage content of material, the energy density that result in material is relatively low；Meanwhile, lithium ion diffusion in micro materials and
Transmission range is relatively big, is unfavorable for material discharge and recharge under high magnification, result in the power density of limited material.Along with nanotechnology
With development and the progress of nano material, research finds that nano material has unique Wuli-Shili-Renli system approach, and exploitation is received
Metrical scale electrode material is to improve lithium ion battery energy and the effective way of power density.The electrode material of nanorize has one
Series significantly advantage: 1) specific surface area increases, and the avtive spot of electrochemical reaction increases, simultaneously electrolyte and electrode material
Effectively contact area increases, it is provided that more lithium ion deintercalation site, is conducive to increasing the reversible capacity of electrode material；2) material
Material size is reduced to Nano grade, greatly shortens the diffusion length of lithium ion, increases lithium ion mobility ability, is conducive to improving
High rate performance.Therefore, in order to improve VO further2(B) chemical property of base lithium ion battery electrode material, various low-dimensionals
The VO of nanostructured2(B) it is synthesized, and presents more excellent chemical property.
Along with the characteristic to nano material and the continuous progress of the understanding of application in lithium ion battery, gradually find nanometer
Material there is also some stubborn problems as lithium ion battery electrode material, including: 1) nano material has high specific surface
Can, it is susceptible in cyclic process from reuniting, thus causes avtive spot reduction, lithium ion diffusion hindered, cause electrochemistry
Hydraulic performance decline；2) simultaneously, in charge and discharge process, change in volume and the produced stress of nano material can not get effectively discharging,
Cause electrode efflorescence from face, contact inefficacy with collector, have a strong impact on cycle performance;3) tap density of nano material is relatively low,
It is unfavorable for commercial production and relatively costly.In order to overcome these unfavorable factors above-mentioned, give full play to the advantage of nano material, if
The material of meter and three-dimensional (3D) the classifying porous micro-nano structure of preparation has become as the study hotspot of field of lithium ion battery.Micro--to receive
Structure is to be become micron meter by construction unit (such as nano-particle, nano wire, nanotube, the nanometer sheet etc.) ordered fabrication of nanoscale
The secondary structure of degree.This special secondary structure is highly beneficial to the raising of chemical property: 1) they will have concurrently and receive
Rice construction unit and the advantage of micron secondary structure, the most not only remain nano-material surface effect, small-size effect, quantum chi
The advantages such as very little effect, the cooperative effect the most also the secondary structure obtaining micro-meter scale brought and coupling effect, be conducive to
Improve the chemical property of electrode material each side simultaneously；2) graded porous structure has substantial amounts of micro--mesoporous hole, these holes
Can effectively alleviate and discharge electrode material produced change in volume when discharge and recharge, be conducive to improving cycle performance；3)
Graded porous structure has bigger specific surface area, not only adds the avtive spot of electrochemical reaction, and is lithium ion
Transmission provides more efficiently path, therefore can improve specific capacity and the high rate performance of electrode material.The system of micro-nano structure
Preparation Method can be divided into vapor phase method and liquid phase method, and wherein controllability is good, mild condition, product owing to having for hydro-thermal and solvent-thermal method
Purity advantages of higher is it is considered to be prepare the method that classifying porous micro-nano structure is maximally efficient.Although a lot of materials are all in recent years
Various interesting micro-nano structure has been prepared by distinct methods, but about VO2(B) report of micro-nano structure is still
The most extremely limited；Meanwhile, relevant formation mechenism is still unclear, what is more important is difficulty with entering micro-nano structure
Row regulation and control and autotelic design and preparation.Therefore, in order to more on purpose prepare the barium oxide of more horn of plenty micro--receive knot
Structure thus improve the chemical property of lithium ion battery further, propose a kind of controlled to prepare different dimensions VO2(B) nanometer material
The synthetic method of material then seems the most urgent and important.
Summary of the invention
Technical problem
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of different by high temperature mixing water full-boiled process controlledly synthesis
Dimension VO2(B) method of nano material, including 1D VO2(B) nano belt, 2D VO2(B) nanometer sheet and the classifying porous VO of 3D2
(B)@C micro-nano structure, the simultaneously classifying porous VO of 3D2(B)@C micro-nano structure presents extremely excellent chemical property.
Technical scheme
In order to solve above-mentioned technical problem, under the synthetic method of the vanadium dioxide nano material that the dimension of the present invention is controlled includes
Row step:
Step one: weigh vanadium source material and be placed in a reaction chamber of high temperature mixing hydrothermal reaction kettle, and add 5-8ml deionization
Water；
Step 2: weigh reducing agent that concentration is 0.04～0.2 mol/L in another reaction chamber of reactor；
Step 3: put into heat temperature raising in baking oven after being sealed by reactor；
Step 4: when oven temperature is raised to 160-260 ° of C, rotates reactor, makes the reactant in two chambeies in reactor mix
Conjunction carries out hydro-thermal reaction, and continues insulation 1-12 hour；
Step 5: be cooled to room temperature after hydro-thermal reaction terminates, be precipitated thing；
Step 6: by step 5 obtain precipitate deionized water and absolute ethanol washing for several times, the powder body that then will obtain
Put in vacuum drying oven, under 60-80 ° of C, be dried 10h to obtain dispersibility preferable vanadium oxide powder body.
Further, described vanadium source material is vanadic anhydride, ammonium metavanadate, sodium metavanadate or vanadium acetylacetonate
In any one.
Further, in the method for the present invention, can be obtained not by the mol ratio of regulation reducing agent and vanadium source material
VO with dimension2(B) nano material: when the mol ratio of reducing agent and vanadium source material is 0.2:1, can obtain one-dimensional (1D)
VO2(B) nano belt；When the mol ratio of reducing agent and vanadium source material is 0.3:1～0.8～1, two dimension (2D) VO can be obtained2
(B) nanometer sheet；When the mol ratio of reducing agent and vanadium source material is 0.9:1～1:1, three-dimensional (3D) graded porous carbon can be obtained
The VO of cladding2(B) micro-nano structure.
The present invention also provides for a kind of anode material for lithium-ion batteries, and it uses the VO that technique scheme obtains2(B) it is
Lithium ion battery electrode material.
Beneficial effect
Technical scheme has the advantages that
(1) synthetic method described in have employed the hydrothermal high-temperature hybrid technology of novelty, and this hydrothermal high-temperature mixing method has one and is
Row advantage: without mesophase in building-up process, product good crystallinity, pattern is uniform, and material structure is prone to regulation and control, and response speed is fast,
Repeatable high, synthetic method is simple, low energy consumption, pollution-free, without dephasign etc..
(2) synthetic method controlledly synthesis different dimensions VO of the present invention2(B) method of nano material, including 1D
VO2(B) nano belt, 2D VO2(B) nanometer sheet and the classifying porous VO of 3D2(B)@C micro-nano structure.
(3) the classifying porous VO of 3D2(B)@C micro-nano structure presents extremely excellent chemical property, at 100 mA/g
Electric current density under, its in first week specific discharge capacity be 192 mAh/g, after circulating 160 times, capacity is up to 206 mAh/g.
Accompanying drawing explanation
Fig. 1 is that the X of different dimensions VO2 (B) nano-powder synthesized when glucose is different with the mol ratio of V2O5 penetrates
Ray diffraction diagram is composed, wherein, and (a) glucose and mol ratio 0.2:1 of V2O5;(b) glucose and mol ratio 0.4:1 of V2O5;(c)
Glucose and mol ratio 1:1 of V2O5.
Fig. 2 is sweeping of different dimensions VO2 (B) nano-powder synthesized when glucose is different with the mol ratio of V2O5
Retouch Electronic Speculum figure, wherein, (a) glucose and mol ratio 0.2:1 of V2O5;(b) glucose and mol ratio 0.4:1 of V2O5;(c) Portugal
Grape sugar and mol ratio 1:1 of V2O5.
Fig. 3 is following of different dimensions VO2 (B) nano-powder synthesized when glucose is different with the mol ratio of V2O5
Ring performance schematic diagram, wherein, (a) glucose and mol ratio 0.2:1 of V2O5, product is 1D VO2(B) nano belt;(b) Fructus Vitis viniferae
Sugar and mol ratio 0.4:1 of V2O5, product is 2D VO2(B) nanometer sheet;C () glucose and mol ratio 1:1 of V2O5, product is
3D classifying porous VO2 (B)@C micro-nano structure.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme is further described.
Embodiment one:
The present embodiment is high temperature mixing water full-boiled process controlledly synthesis 1D VO2(B) method of nano belt.Specifically comprise the following steps that
1) V2O5 of 0.182g is joined in a chamber of high temperature mixing hydrothermal reaction kettle liner, add 5ml deionized water；
2) glucose solution of 5ml 0.04M is added in another chamber of liner；
3) put into heat temperature raising in baking oven after being sealed by this reactor, when temperature is raised to 200-260 ° of C, reactor is revolved
Turn, make the reactant in two inner chambers of reactor mix, be incubated 4-8h；
Reaction is cooled to room temperature after terminating；
4) finally by obtain precipitate deionized water and absolute ethanol washing for several times after, under 80 ° of C be dried 10 h with
To dispersibility preferable 1D VO2(B) nano belt, its X ray diffracting spectrum is Fig. 1 (a), and scanning electron microscopic picture is Fig. 2 (a)；
5) cycle performance test: carry out being fully ground mixing by active substance, acetylene black, PVDF 7:2:1 in mass ratio, by this slurry
Material is applied on aluminium foil and is coated, and is punched out by the substrate after molding, finally gives the electrode slice of diameter 12 mm.With gold
Genus lithium is negative pole, and Cdgard 2400 is barrier film, is assembled into 2032 type button cells, then carries out electrification in argon glove box
Learn performance test.Its cycle performance such as Fig. 3 (a): 1D VO2(B) first week specific discharge capacity of nano belt is 174 mAh/g, circulation
After 120 times, its specific discharge capacity reduces to 129 mAh/g, and capability retention is 74%.
Embodiment two:
The present embodiment is hydrothermal high-temperature mixing method controlledly synthesis 2D VO2(B) method of nanometer sheet.Specifically comprise the following steps that
1) V2O5 of 0.182g is joined in a chamber of high temperature mixing hydrothermal reaction kettle liner, add 5ml deionized water；
2) glucose solution of 5ml 0.08M is added in another chamber of liner；
3) put into heat temperature raising in baking oven after being sealed by this reactor, when temperature is raised to 200-260 ° of C, reactor is revolved
Turn, make the reactant in two inner chambers of reactor mix, be incubated 4-8h；
Reaction is cooled to room temperature after terminating；
4) finally by obtain precipitate deionized water and absolute ethanol washing for several times after, under 80 ° of C be dried 10 h with
To dispersibility preferable 2D VO2(B) nanometer sheet, its X ray diffracting spectrum is Fig. 1 (b), and scanning electron microscopic picture is Fig. 2 (b)；
5) cycle performance test: method of testing is same as in Example 1.Its cycle performance such as Fig. 3 (b): 2D VO2(B) nanometer strap
First week specific discharge capacity be 170 mAh/g, after circulating 120 times, its specific discharge capacity reduces to 141 mAh/g, and capability retention is
83%。
Embodiment three:
The present embodiment is the method for hydrothermal high-temperature mixing method controlledly synthesis 3D classifying porous VO2 (B)@C micro-nano structure.Concrete step
Rapid as follows:
1) V2O5 of 0.182g is joined in a chamber of high temperature mixing hydrothermal reaction kettle liner, add 5ml deionized water；
2) glucose solution of 5ml 0.2M is added in another chamber of liner；
3) put into heat temperature raising in baking oven after being sealed by this reactor, when temperature is raised to 200-260 ° of C, reactor is revolved
Turn, make the reactant in two inner chambers of reactor mix, be incubated 4-8h；
Reaction is cooled to room temperature after terminating；
4) finally by obtain precipitate with deionized water and absolute ethanol washing for several times after, under 80 ° of C be dried 10 h to obtain
The preferable 3D of dispersibility classifying porous VO2 (B)@C micro-nano structure, its X ray diffracting spectrum is Fig. 1 (c), scanning electron microscopic picture
For Fig. 2 (c)；
5) cycle performance test: method of testing is same as in Example 1.The classifying porous VO2 of its cycle performance such as Fig. 3 (c): 3D
(B) first all specific discharge capacities of@C micro-nano structure are 192 mAh/g, and after circulating 160 times, its specific discharge capacity is up to 206 mAh/
G, capability retention is 107%.Visible, 3D classifying porous VO2 (B)@C micro-nano structure has more excellent than low-dimensional nano structure
Different chemical property.
Embodiment four:
The present embodiment relates to a kind of anode material for lithium-ion batteries, and what it used above-described embodiment one, two or three has different dimensional
The VO of degree2(B) nano material.
Claims (5)
1. the synthetic method of the vanadium dioxide nano material that a dimension is controlled, it is characterised in that processing step is as follows；
Step one: weigh vanadium source material and be placed in a reaction chamber of high temperature mixing hydrothermal reaction kettle, and add 5-8ml deionization
Water；
Step 2: weigh reducing agent that concentration is 0.04～0.2 mol/L in another reaction chamber of reactor；
Step 3: put into heat temperature raising in baking oven after being sealed by reactor；
Step 4: when oven temperature is raised to 160-260 ° of C, rotates reactor, makes the reactant in two chambeies in reactor mix
Conjunction carries out hydro-thermal reaction, and continues insulation 1-12 hour；
Step 5: be cooled to room temperature after hydro-thermal reaction terminates, be precipitated thing；
Step 6: the precipitate deionized water and the absolute ethanol washing that step 5 are obtained obtain powder body 3-5 time, then incite somebody to action
To powder body put in vacuum drying oven, under 60-80 ° of C be dried 10h to obtain dispersibility preferable vanadium oxide powder body.
2. synthetic method as claimed in claim 1, it is characterised in that described vanadium source material is vanadic anhydride, metavanadic acid
Ammonium, sodium metavanadate or vanadium acetylacetonate.
3. synthetic method as claimed in claim 1, it is characterised in that described reducing agent is glucose, sucrose, polyethylene pyrrole
Pyrrolidone or Polyethylene Glycol.
4. synthetic method as claimed in claim 1, it is characterised in that the mol ratio by regulation reducing agent and vanadium source material can
To obtain the VO of different dimensions2(B) nano material, can obtain one when the mol ratio of reducing agent and vanadium source material is 0.2:1
Dimension VO2(B) nano belt, can obtain two dimension VO when the mol ratio of reducing agent and vanadium source material is 0.3:1～0.8～12 (B)
Nanometer sheet, can obtain three-dimensional graded porous carbon cladding when the mol ratio of reducing agent and vanadium source material is 0.9:1～1:1
VO2(B) micro-nano structure.
5. a lithium ion battery, it is characterised in that described anode material for lithium-ion batteries uses as appointed in claim 1-4
The VO that one described method of meaning obtains2(B) it is lithium ion battery electrode material.
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Cited By (6)
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| CN107394219A (en) * | 2017-07-31 | 2017-11-24 | 中南大学 | A kind of VC/ graphene composite materials and preparation method thereof and the application in lithium-air battery |
| CN107779905A (en) * | 2017-09-19 | 2018-03-09 | 同济大学 | A kind of preparation method of vanadium oxide nanobelt |
| CN108531753A (en) * | 2018-05-30 | 2018-09-14 | 武汉理工大学 | A kind of method of the vanadium shale without ammonia-sinking vanadium |
| CN112397707A (en) * | 2020-11-13 | 2021-02-23 | 何叶红 | Porous VO for lithium ion battery2Microspheres and method for preparing same |
| CN114249322A (en) * | 2021-12-27 | 2022-03-29 | 北京理工大学 | Nano flower-shaped VO2（B）/V2CTxPreparation method of composite material and sodium ion battery |
| CN114873641A (en) * | 2022-05-23 | 2022-08-09 | 陕西科技大学 | Square VO2 nanosheet and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107394219A (en) * | 2017-07-31 | 2017-11-24 | 中南大学 | A kind of VC/ graphene composite materials and preparation method thereof and the application in lithium-air battery |
| CN107394219B (en) * | 2017-07-31 | 2020-08-25 | 中南大学 | VC/graphene composite material, preparation method thereof and application thereof in lithium-air battery |
| CN107779905A (en) * | 2017-09-19 | 2018-03-09 | 同济大学 | A kind of preparation method of vanadium oxide nanobelt |
| CN108531753A (en) * | 2018-05-30 | 2018-09-14 | 武汉理工大学 | A kind of method of the vanadium shale without ammonia-sinking vanadium |
| CN112397707A (en) * | 2020-11-13 | 2021-02-23 | 何叶红 | Porous VO for lithium ion battery2Microspheres and method for preparing same |
| CN114249322A (en) * | 2021-12-27 | 2022-03-29 | 北京理工大学 | Nano flower-shaped VO2（B）/V2CTxPreparation method of composite material and sodium ion battery |
| CN114873641A (en) * | 2022-05-23 | 2022-08-09 | 陕西科技大学 | Square VO2 nanosheet and preparation method and application thereof |
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Application publication date: 20160810 |