CN101157479A - Low-dimensional V3O7.H2O nano material and preparation method and application thereof - Google Patents
Low-dimensional V3O7.H2O nano material and preparation method and application thereof Download PDFInfo
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- CN101157479A CN101157479A CNA2007100532569A CN200710053256A CN101157479A CN 101157479 A CN101157479 A CN 101157479A CN A2007100532569 A CNA2007100532569 A CN A2007100532569A CN 200710053256 A CN200710053256 A CN 200710053256A CN 101157479 A CN101157479 A CN 101157479A
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Abstract
The invention discloses low-dimensional V3O7*H2O nanometer material, which is prepared with the following procedures: dispersing vanadate or V2O5 powder into organic solvent and deionzied water to obtain suspension; transferring the suspension into an autoclave or a pressure pipe type reactor and allowing for reaction for 2-48 hours at 140-200 DEG C, thereby, the low-dimensional V3O7*H2O can be obtained. The invention has the advantages of cheap and easily-available raw material, simple process, low cost, easy controllability, stable product quality as well as fine technological repeatability, and makes possible large-scale industrial preparation. The low-dimensional V3O7*H2O nanometer material prepared with the invention has anisotropy as well as excellent optical, electrical and magnetic properties and is expected to apply to fields related to catalysis, high-energy batteries, photoelectric conversion, aeronautics and astronautics, etc.
Description
Technical field
The present invention relates to a kind of low-dimensional V
3O
7H
2O nano material and its preparation method and application.The invention belongs to technical field of inorganic, also belong to technical field of function materials.
Background technology
Low-dimension nano material typically refers to zero dimension (elementide, nanoparticle) and one dimension materials such as (nanotube, nano wire, nanometer rod and nano belt).
V
3O
7Because its unique optics, magnetics and electrical properties are applied to the fields such as catalysis, electrochemistry.Existing synthetic V
3O
7Method, be limited to the generation block materials more.
At present limited research both at home and abroad concentrates on: J.O.Thomas (J.Mater Chem.1995,5,1075-1080.) report: at 500 ℃, N
2Calcine NH in the atmosphere
4VO
3, obtain block V
3O
7The main drawback of this method is that product is wayward and impure, and complex process is unfavorable for suitability for industrialized production, and is difficult to obtain low-dimension nano material with this method.
(Mat.Res.Soc.Symp.Proc.2004,788, the 321-326.) report: use the PMMA fiber as template, with NH such as Whittingham
4VO
3After solution mixes, be 3.4 with the vinegar acid for adjusting pH, at 160 ℃ of Water Under thermal response 3d, with the product that obtains at N
2Middle heat treatment obtains V
3O
7Nanofiber.This reaction main drawback is that the reaction times is longer, complex process, and products therefrom is impure.
X.Zhang etc. (Mater.Chem.Phys.2004,87,168-172.) titanate nanotube is done template, V
2O
5NH
2O colloidal sol is done precursor, at 200 ℃ of Water Under thermal response 48h, gets V
3O
7H
2O/ titanate compound particle nanometer rods.The major defect of this method: product is V
3O
7H
2The mixture of O and titanate is difficult to obtain pure V
3O
7H
2The O low-dimension nano material.
Summary of the invention
The object of the present invention is to provide a kind of low-dimensional V
3O
7H
2O nano material and its production and use, this preparation method can adopt raw material cheap and easy to get under lower temperature conditions, in a large number synthetic low-dimensional V
3O
7H
2O nanobelt, nanometer rods and nanosphere.
The technical scheme that the present invention is concrete: a kind of low-dimensional V
3O
7H
2The O nano material is made by laxative remedy: with vanadate or V
2O
5Powder is distributed in organic solvent and the deionized water, obtains suspension; Suspension is transferred in autoclave or the withstand voltage tubular reactor, at 140～200 ℃ of lower reaction 2～48h, namely obtained low-dimensional V
3O
7H
2O rice material.
According to technical scheme of the present invention, described low-dimension nano material is nano belt, nanometer rod or nanometer ball.
According to technical scheme of the present invention, the organic solvent that is adopted is that (alkyl is C to alkyl alcohol
1～C
12), (alkyl is C to alkyl ketone
1～C
4), N, dinethylformamide (DMF), alkylamine (R
3N: alkyl is C
1～C
4), mercaptan (R-SH), cycloalkanol (C
5～C
6) and naphthenone (C
5～C
6) one or more mixed solvent in waiting.
According to technical scheme of the present invention, the temperature of reaction during reduction reaction is 140～200 ℃; Preferred 160～180 ℃; Reaction times is 2～48h.
According to technical scheme of the present invention, the ratio of reaction mass is vanadate or V
2O
5: organic solvent: ratio=0.001 of the amount of substance of deionized water～0.05: 0.03～0.52: 0.56～2.78.
The present invention adopts vanadate or V
2O
5Powder with common are the machine solvent and water is raw material, adopt identical experimental provision, prepare first V
3O
7H
2O nanobelt, nanometer rods and nanosphere.The advantage of the inventive method is:
(1) raw material is simple, and solvent for use is common organic solvent, and is with low cost;
(2) reaction scheme is short;
(3) temperature of reaction is lower;
(4) operating procedure is simple, can realize the heavy industrialization preparation;
Because the low-dimensional V that obtains
3O
7H
2Therefore the special natures such as the O nano material has that purity height, output are big, perfect structure, surface clean and inner zero defect, dislocation-free can obtain to use widely in association areas such as catalysis, high-energy battery, opto-electronic conversion, Aero-Space.
Description of drawings
Fig. 1 is the X-ray powder diffraction figure of embodiment 1 correspondence;
It is ethanol, acetone, N that Fig. 2,3,4,5,6,7 is respectively organic solvent, and the TEM Electronic Speculum of product correspondence detects figure when the mixture of dinethylformamide, methyl alcohol and hexanol, Dodecyl Mercaptan, hexalin;
The following examples are used to illustrate the present invention, but limit the present invention anything but.
Embodiment
Take by weighing 0.90g V
2O
5Powder is distributed in the 10mL ethanol, adds then the 50mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 24h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O sees accompanying drawing 1; The TEM Electronic Speculum detects finds that product is regular banded structure, is about 30 μ m most, wide about 100-200nm, and thickness is no more than 20nm.See accompanying drawing 2.Reaction temperature is controlled at 140～200 ℃, in the reaction time of 2～48h, all can obtain V
3O
7H
2The regular banded structure of O.
Embodiment 2
According to embodiment 1, with V
2O
5Powder replaces with NH
4VO
3, NaVO
3, KVO
3, K
3VO
4Or Na
3VO
4, other conditions remain unchanged.The TEM Electronic Speculum detects finds that product is regular zonal structure, is about 30 μ m most, wide about 100-200nm, and thickness is no more than 20nm.
Embodiment 3
Take by weighing 0.90g V
2O
5Powder is distributed in the 30mL ethanol, adds then the 70mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 24h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O; The TEM Electronic Speculum detects finds that product is regular banded structure, is about 30 μ m most, wide about 100-200nm, and thickness is no more than 20nm.
Take by weighing 0.18g V
2O
5Powder is distributed in the 2mL ethanol, adds then the 40mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 24h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O; The TEM Electronic Speculum detects finds that product is regular banded structure, is about 30 μ m most, wide about 100-200nm, and thickness is no more than 20nm.
Embodiment 5
Take by weighing 0.90g V
2O
5Powder is distributed in the 10mL ethanol, adds then the 60mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 24h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O; The TEM Electronic Speculum detects finds that product is regular banded structure, is about 30 μ m, wide about 100-200nm, and thickness is no more than 20nm.
Embodiment 6
With 1.50g V
2O
5Powder is distributed to respectively in the 2mL acetone, adds then the 50mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 12h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular banded structure, sees accompanying drawing 3.Reaction temperature is controlled at 140～200 ℃, in the reaction time of 2～48h, all can obtain V
3O
7H
2The regular banded structure of O is about 20 μ m most, wide about 100-200nm, and thickness is no more than 20nm.
Embodiment 7
With 0.80g V
2O
5Powder is distributed to respectively 10mLN, in the dinethylformamide, adds then the 50mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 12h.The nature cooling discharge, through the deionized water washing, vacuum drying namely gets the yellow green powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular banded structure, sees accompanying drawing 4.Reaction temperature is controlled at 140～200 ℃, in the reaction time of 2～48h, all can obtain V
3O
7H
2The regular banded structure of O is about 30 μ m most, wide about 100-200nm, and thickness is no more than 20nm.
Embodiment 8
According to embodiment 7, with N, dinethylformamide replaces with alkylamine (R
3N: alkyl is C
1～C
4), other conditions remain unchanged.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular banded structure, is about 30 μ m most, wide about 100-200nm, thickness is no more than 20nm.
Embodiment 9
With 0.50g V
2O
5Powder is distributed to respectively in the mixture of 10mL methyl alcohol and hexanol, adds then the 50mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 2h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular banded structure, sees accompanying drawing 5.Reaction temperature is controlled at 140～200 ℃, in the reaction time of 2～48h, all can obtain V
3O
7H
2The regular banded structure of O is about 30 μ m most, wide about 100-200nm, and thickness is no more than 20nm.
Embodiment 10
With 1.20g V
2O
5Powder is distributed to respectively in the 10mL lauryl mercaptan, adds then the 50mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 48h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular club shaped structure, sees accompanying drawing 6.Reaction temperature is controlled at 140～200 ℃, in the reaction time of 2～48h, all can obtain V
3O
7H
2The regular club shaped structure of O is about 50 μ m, diameter 30-90nm.
Embodiment 11
With 1.60g V
2O
5Powder is distributed to respectively in the 10mL cyclohexanol, adds then the 50mL deionized water, stir into suspension after, be transferred in the autoclave, in closed reactor in 180 ℃ the reaction 12h.Naturally cooling back discharging, through deionized water wash, vacuum-drying promptly gets the yellow-green colour powder.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular chondritic, sees accompanying drawing 7.Temperature of reaction is controlled at 140～200 ℃, in the reaction times of 2～48h, all can obtain regular ball-like structure, and granular size is about 10-20nm.
Embodiment 12
According to embodiment 7, hexalin is replaced with cyclopentanol, pimelinketone or cyclopentanone, other conditions remain unchanged.Product is accredited as V through X-ray powder diffraction
3O
7H
2O, the TEM Electronic Speculum detects finds that product is regular chondritic, granular size is about 10-20nm.
Claims (7)
1. low-dimensional V
3O
7H
2The O nano material is made by laxative remedy: with vanadate or V
2O
5Powder is distributed in organic solvent and the deionized water, obtains suspension; Suspension is transferred in autoclave or the withstand voltage tubular reactor, at 140～200 ℃ of lower reaction 2～48h, namely obtained low-dimensional V
3O
7H
2O rice material.
2. low-dimensional V according to claim 1
3O
7H
2The O nano material is characterized in that: described low-dimension nano material is nanobelt, nanometer rods or nanosphere.
3. claim 1 or 2 described low-dimensional Vs
3O
7H
2O preparations of nanomaterials method is with vanadate or V
2O
5Powder is distributed in organic solvent and the deionized water, obtains suspension; Suspension is transferred in autoclave or the withstand voltage tubular reactor, at 140～200 ℃ of lower reaction 2～48h, namely obtained low-dimensional V
3O
7H
2O rice material.
4. method according to claim 3 is characterized in that: described organic solvent is C
1～C
12Alkyl alcohol, C
3～C
4Alkyl ketone, N, dinethylformamide, C
1～C
4Alkylamine, mercaptan, C
5～C
6Cycloalkanol and C
5～C
6The mixed solvent of one or more in the naphthenone.
5. according to claim 3 or 4 described preparation methods, it is characterized in that: described vanadate is NH
4VO
3, NaVO
3, KVO
3, K
3VO
4Or Na
3VO
4
6. according to claim 3 or 4 described preparation methods, it is characterized in that: vanadate or V
2O
5: organic solvent: the ratio of the amount of substance of deionized water is 0.001～0.05: 0.03～0.52: 0.56～2.78.
7. claim 1 or 2 described low-dimensional Vs
3O
7H
2The application of O nano material in catalysis, high-energy battery, opto-electronic conversion or aerospace field.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100532569A CN101157479A (en) | 2007-09-18 | 2007-09-18 | Low-dimensional V3O7.H2O nano material and preparation method and application thereof |
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|---|---|---|---|
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236533A (en) * | 2013-04-22 | 2013-08-07 | 中南大学 | Potassium vanadate nanobelt material for lithium ion battery and preparation method thereof |
| CN105271407A (en) * | 2015-10-20 | 2016-01-27 | 辽宁石油化工大学 | Vanadium oxide nano array and preparation method thereof |
| CN109650441A (en) * | 2018-12-19 | 2019-04-19 | 广东工业大学 | One kind seven aoxidizes three vanadium Zinc ion battery positive electrodes and preparation method thereof |
| CN116040681A (en) * | 2023-01-31 | 2023-05-02 | 承德天大钒业有限责任公司 | Three-dimensional porous vanadium pentoxide, and preparation method and application thereof |
-
2007
- 2007-09-18 CN CNA2007100532569A patent/CN101157479A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103236533A (en) * | 2013-04-22 | 2013-08-07 | 中南大学 | Potassium vanadate nanobelt material for lithium ion battery and preparation method thereof |
| CN105271407A (en) * | 2015-10-20 | 2016-01-27 | 辽宁石油化工大学 | Vanadium oxide nano array and preparation method thereof |
| CN109650441A (en) * | 2018-12-19 | 2019-04-19 | 广东工业大学 | One kind seven aoxidizes three vanadium Zinc ion battery positive electrodes and preparation method thereof |
| CN116040681A (en) * | 2023-01-31 | 2023-05-02 | 承德天大钒业有限责任公司 | Three-dimensional porous vanadium pentoxide, and preparation method and application thereof |
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Open date: 20080409 |