CN108847483A - A kind of quick magnanimity preparation V2O5The method and application of nanometer sheet - Google Patents
A kind of quick magnanimity preparation V2O5The method and application of nanometer sheet Download PDFInfo
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- CN108847483A CN108847483A CN201810640278.3A CN201810640278A CN108847483A CN 108847483 A CN108847483 A CN 108847483A CN 201810640278 A CN201810640278 A CN 201810640278A CN 108847483 A CN108847483 A CN 108847483A
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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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- 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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- 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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Abstract
The present invention relates to technical field of nano material, particularly disclose a kind of quick magnanimity preparation V2O5The method and application of nanometer sheet.Firstly, vanadium source is dissolved in solution, qs Electrolyte is added, stirs, is uniformly mixed.Then mixed solution is transferred in microwave reactor, 2~60min of microwave reaction, reaction product is washed, is dried to obtain presoma;Finally, calcining presoma under air atmosphere with Muffle furnace, being cooled to room temperature, V is made2O5Nanometer sheet.The product purity is high, good crystallinity, is used as battery active material and catalyst, shows excellent performance.This method raw material is cheap and easy to get, at low cost, and yield is high, is suitble to large-scale production.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of V2O5The preparation method and application of nanometer sheet.
Background technique
Vanadic anhydride (V2O5) as a kind of important layered inorganic material, have reversibly intercalation/deintercalation molecule or from
Son function, be widely used in recent years lithium ion battery (LIBs), sodium-ion battery (NIBs), kalium ion battery (KIBs) with
And in the metal ions battery such as Zinc ion battery (ZIBs), and get more and more people's extensive concerning.For example, V2O5As lithium-ion electric
When the positive electrode of pond, two Li can be embedded in+Ion and have high theoretical specific capacity (294mAh g-1), this is much higher than LiCoO2
(140mAh g-1) and LiFePO4(170mAh g-1) etc. commercial Li-ion batteries positive electrode specific capacity.Therefore research people
Member is using the V for either physically or chemically constructing different morphologies and crystal structure2O5, to obtain more excellent performance of V2O5It receives
Rice material.So far, a variety of V are had reported2O5Nanostructure, such as V2O5Yolk-shell microballoon, V2O5Multi-level flower-like structure, V2O5
Nano wire and mesoporous V2O5Nanometer sheet etc..However, the synthesis nanostructure V reported2O5Method be mainly hydro-thermal method, chemistry
The methods of vapor deposition, liquid phase removing or electrostatic spinning.These synthetic methods there are processes complicated, at high cost, low output and energy
The disadvantages of high is consumed, V has been seriously affected2O5The industrial applications of nano material.Therefore, it finds a kind of easy, efficiently and can magnanimity system
Standby nanostructure V2O5Method it is extremely urgent.
Summary of the invention
It is an object of that present invention to provide a kind of quick magnanimities to prepare V2O5The method and application of nanometer sheet, this method pass through micro-
Wave-calcining two-step method is prepared for V2O5Nanometer sheet realizes V2O5Controllable preparation.
To achieve the above object, the present invention adopts the following technical scheme that:
Vanadium source is configured to solution, configuration method:By or mixtures thereof hydrogen peroxide, inorganic acid, Organic Alcohol with go from
Sub- water is uniformly mixed under stiring, and vanadium source substance is then added;
Into step 1 vanadium source solution, qs Electrolyte is added, stirs evenly, forms mixed solution;
Mixed solution described in step 2 is transferred to microwave reactor, carries out microwave reaction, product is washed, and it is dry, it is made
Presoma;
In air atmosphere, presoma described in low temperature calcination processing step 3, is cooled to room temperature, obtains V2O5Nanometer sheet.
Further, vanadium source described in step 1 includes NH4VO3、Na3VO4·12H2O、V3O7、V2O3、VO2、V6O13、V2O5Deng;
Further, the component of aqueous solution described in step 1 include in hydrogen peroxide or ethylene glycol, glycerine and isopropanol at least
It is a kind of;
Further, vanadium source solution described in step 1, the concentration in vanadium source are 0.01~1mol/L;
Further, electrolyte described in step 2 includes metal salt, acids, bases etc., wherein and metal salt includes NaCl,
CH3COONa, Na2SO4, Na2CO3Equal sodium salts and other metal cation salts (including:Li+, K+, Mg2+, Ca2+, Zn2+, Al3+Deng);
The addition form of metal salt includes solid powder and solution, and metal salt solution is dissolved in water for metal salt solid powder and is formed, concentration
For 0.01~1mol/L;
Further, microwave reaction described in step 3, microwave power are 100~900W, and the reaction time is 2~60min;
Further, the medium that washing microwave reaction product uses described in step 3 is pure water and dehydrated alcohol;Washing process
Solid-liquid separation method has the modes such as suction filtration, filters pressing or centrifugation.
Further, the drying mode of washed product described in step 3 is freeze-drying or normal drying;The freeze-drying
It is in condenser temperature is -60 DEG C~-40 DEG C ranges freezing 2~for 24 hours, under the conditions of 10~30Pa of vacuum degree, dry 6~for 24 hours.It is described
The temperature of normal drying be 40 DEG C~120 DEG C, drying time be 6~for 24 hours.
Further, low temperature calcination process described in step 4, calcination temperature be 300~500 DEG C, calcination time be 0.5~
2h。
Further, V described in step 42O5Nanometer sheet is applied to battery active material and catalyst material, shows excellent
Performance.
Compared with the existing technology, the present invention at least has the advantages that:
The present invention is prepared for V by microwave-calcining two-step method2O5Nanometer sheet is realized by controlling microwave reaction process
V2O5Then the control of structure and morphology realizes V by calcining2O5The raising of crystallinity, and then realize V2O5Controllable preparation.The party
Method has the characteristics that simple process is easily-controllable, raw material is cheap and easy to get, yield is high, at low cost and suitable large-scale production.In addition, the party
The V of method preparation2O5Nanometer sheet has high-purity, uniform chemical composition and good crystallinity, as lithium ion battery battery
Pole material and catalyst material show excellent performance.
Detailed description of the invention
Fig. 1 is the nanometer sheet V that the present invention implements prepared by example 12O5XRD spectrum;
Fig. 2 is the nanometer sheet V that the present invention implements prepared by example 12O5SEM photograph;
Fig. 3 is the nanometer sheet V that the present invention implements prepared by example 22O5XRD spectrum;
Fig. 4 is the nanometer sheet V that the present invention implements prepared by example 22O5SEM photograph;
Fig. 5 is the nanometer sheet V that the present invention implements prepared by example 22O5Chemical property figure.
Specific embodiment
In order to further appreciate that the present invention, with reference to the accompanying drawing and implement example invention is further described in detail,
It is understood that these descriptions are only further explanation the features and advantages of the present invention, rather than right of the present invention is wanted
The limitation asked.A kind of quick magnanimity preparation V2O5The method and application of nanometer sheet, preparation step are as follows:
(1) vanadium source is configured to solution, configuration method:By or mixtures thereof hydrogen peroxide, inorganic acid, Organic Alcohol with go
Ionized water is uniformly mixed under stiring, and vanadium source substance is then added;
(2) into step 1 vanadium source solution, qs Electrolyte is added, stirs evenly, form mixed solution;
(3) mixed solution described in step 2 being transferred to microwave reactor, carries out microwave reaction, product is washed, and it is dry,
Presoma is made.
(4) in air atmosphere, presoma described in low temperature calcination processing step 3, is cooled to room temperature, obtains V2O5Nanometer sheet.
Example 1 is embodied
100mL deionized water and 5mL hydrogen peroxide are added in 500mL glass flask, after mixing evenly, 5mmol quotient is added
Industry V2O5, persistently stir 30min and obtain kermesinus clear solution, then add 1mmol NaCl, stir 30min.By three mouthfuls
Flask is placed in microwave reactor, connects condensing unit, and setting reaction power is 700W, reaction time 20min.Reaction terminates
Afterwards, natural cooling, uses deionized water respectively, and dehydrated alcohol washs resulting product, removes possible impurity.Freeze-drying, i.e.,
Obtain V2O5Nanometer sheet presoma is warming up to 350 DEG C of heat preservation 60min from 30~60min of room temperature, obtains V then in Muffle furnace2O5
Nanometer sheet.As shown in FIG. 1, FIG. 1 is V manufactured in the present embodiment2O5XRD analysis figure, all X-ray powder diffraction peaks
Index is V2O5Powder, and occur without other impurity peaks, therefore the synthesis of embodiment 1 is the V of high-purity2O5Nano material.
Fig. 2 is V manufactured in the present embodiment2O5The SEM photograph of the nano flower of nanometer sheet assembling, from photo it can be seen that smooth sheet is received
Rice piece.
Example 2 is embodied
10mmol ammonium metavanadate is weighed, 100mL deionized water is dissolved in, 500 μ L ethylene glycol is then added, are put into water-bath
In, heating, magnetic agitation obtain faint yellow intimate clear solution to being completely dissolved at 50 DEG C.With concentrated hydrochloric acid adjust pH value of solution=
0.1, persistently stir 15min.Then acquired solution is transferred in 500mL three-necked flask, is placed in microwave reaction instrument, connected cold
Solidifying device, setting reaction power are 700W, reaction time 2min.After reaction, natural cooling uses deionized water respectively,
Dehydrated alcohol washs resulting product, removes possible impurity.Dry 12h just obtains V at 80 DEG C2O5Precursor, then drying
Sample afterwards just obtains reddish yellow V in 350 DEG C of heat treatment 1h2O5Sample.
Example 3 is embodied
100mL deionized water and 5mL hydrogen peroxide are added in 500mL glass flask, after mixing evenly, 5mmol quotient is added
Industry V2O5, persistently stir 30min and obtain kermesinus clear solution, then add 1mmolMgCl2·6H2O stirs 30min.
Three-necked flask is placed in microwave reactor, condensing unit is connected, setting reaction power is 700W, reaction time 20min.Instead
After answering, natural cooling uses deionized water respectively, and dehydrated alcohol washs resulting product, removes possible impurity.Freezing is dry
It is dry to get arrive V2O5Nanometer sheet presoma is warming up to 350 DEG C of heat preservation 60min from 30~60min of room temperature then in Muffle furnace,
Obtain V2O5Nanometer sheet.As shown in figure 3, Fig. 3 is V manufactured in the present embodiment2O5XRD analysis figure, all x-ray powders spread out
Penetrating peak can refer to be designated as V2O5Powder, and occur without other impurity peaks, therefore the synthesis of embodiment 3 is the V of high-purity2O5
Nano material.Fig. 4 is V manufactured in the present embodiment2O5The SEM photograph of nanometer sheet, from photo it can be seen that smooth large stretch of nanometer
Piece.
Example 4 is embodied
100mL deionized water and 5mL hydrogen peroxide are added in 500mL glass flask, after mixing evenly, 5mmol quotient is added
Industry V2O5, persistently stir 30min and obtain kermesinus clear solution, then add 1mmolCoCl2·6H2O stirs 30min.
Three-necked flask is placed in microwave reactor, condensing unit is connected, setting reaction power is 700W, reaction time 20min.Instead
After answering, natural cooling uses deionized water respectively, and dehydrated alcohol washs resulting product, removes possible impurity.Freezing is dry
It is dry to get arrive V2O5Nanometer sheet presoma is warming up to 350 DEG C of heat preservation 60min from 30~60min of room temperature then in Muffle furnace,
Obtain V2O5Nanometer sheet.
Example 5 is embodied
120mL deionized water and 5mL hydrogen peroxide are added in 500mL glass flask, after mixing evenly, 5mmol quotient is added
Industry V2O5, persistently stir 30min and obtain kermesinus clear solution, then add 1mmolNiCl2·6H2O stirs 30min.
Three-necked flask is placed in microwave reactor, condensing unit is connected, setting reaction power is 700W, reaction time 20min.Instead
After answering, natural cooling uses deionized water respectively, and dehydrated alcohol washs resulting product, removes possible impurity.Freezing is dry
It is dry to get arrive V2O5Nanometer sheet presoma is warming up to 350 DEG C of heat preservation 60min from 30~60min of room temperature then in Muffle furnace,
Obtain V2O5Nanometer sheet.
Claims (10)
1. a kind of quick magnanimity prepares sheet V2O5The method and application of nano material, which is characterized in that include the following steps:(1)
Vanadium source is dissolved in aqueous solution, vanadium source solution is configured to, wherein vanadium source solution concentration is 0.01~1mol/L;(2) to step 1
In the solution of vanadium source, qs Electrolyte is added, stirs evenly, forms mixed solution;(3) step 2 mixed solution is transferred to microwave
Reactor carries out microwave reaction, and product is washed, dry, and presoma is made;(4) in air atmosphere, before low temperature calcination processing
Body is driven, is cooled to room temperature, V is made2O5Nanometer sheet.
2. a kind of quick magnanimity according to claim 1 prepares sheet V2O5The method and application of nano material, feature exist
In vanadium source includes NH4VO3、Na3VO4·12H2O、V6O13、V2O3、VO2、V2O5Deng.
3. a kind of quick magnanimity according to claim 1 prepares sheet V2O5The method and application of nano material, feature exist
In comprising at least one of or mixtures thereof hydrogen peroxide, inorganic acid, Organic Alcohol and deionized water in the component of aqueous solution;Electricity
Solving matter includes metal salt, acids, bases etc..
4. a kind of quick magnanimity according to claim 3 prepares sheet V2O5The method and application of nano material, feature exist
In the metal salt is NaCl, CH3COONa, Na2SO4, Na2CO3Equal sodium salts and other metal cation salts (including:Li+, K+,
Mg2+, Ca2+, Zn2+, Al3+) etc.;The addition form of metal salt includes solid powder and solution.
5. a kind of quick magnanimity according to claim 4 prepares sheet V2O5The method and application of nano material, feature exist
In the metal salt solution is the solution that metal salt powder is dissolved in water formation, and concentration is 0.01~1mol/L.
6. a kind of quick magnanimity according to claim 1 prepares sheet V2O5The method and application of nano material, feature exist
In the microwave power of microwave reaction is 100~900W;The microwave reaction time is 2~60min.
7. a kind of quick magnanimity according to claim 1 prepares sheet V2O5The method and application of nano material, feature exist
In washing microwave reaction product washing uses pure water and dehydrated alcohol;Washing process solid-liquid separation method is suction filtration, filters pressing
Or centrifugation etc.;The drying means of washed product has freeze-drying and normal drying.
8. a kind of quick magnanimity according to claim 7 prepares sheet V2O5The method and application of nano material, feature exist
It is in condenser temperature in, the freeze-drying is -60 DEG C~-40 DEG C ranges freezing 2~for 24 hours, under the conditions of 10~30Pa of vacuum degree,
Dry 6~for 24 hours;The temperature of the normal drying be 40 DEG C~120 DEG C, drying time be 6~for 24 hours.
9. a kind of quick magnanimity according to claim 1 prepares sheet V2O5The method and application of nano material, feature exist
In under air atmosphere, the temperature for calcining presoma is 300~500 DEG C, and the time is 0.5~2h.
10. a kind of quick magnanimity according to claim 1 prepares sheet V2O5The method and application of nano material, feature
It is, the sheet V2O5Nanometer sheet is applied to battery active material and catalyst, shows excellent performance.
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Cited By (1)
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CN110803713A (en) * | 2019-09-12 | 2020-02-18 | 中南大学 | Vanadium pentoxide nanobelt and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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