CN105384192B - Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 - Google Patents
Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 Download PDFInfo
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- CN105384192B CN105384192B CN201510809085.2A CN201510809085A CN105384192B CN 105384192 B CN105384192 B CN 105384192B CN 201510809085 A CN201510809085 A CN 201510809085A CN 105384192 B CN105384192 B CN 105384192B
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- C01G33/00—Compounds of niobium
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- 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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- C01—INORGANIC CHEMISTRY
- 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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/45—Aggregated particles or particles with an intergrown morphology
Abstract
The invention discloses a method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5. The method mainly comprises the following steps: by taking NbCl5, HO2CCO2H.2H2O and NH4F as raw materials, controlling the NH4F concentration and dripping speed, adding the mixed solution into a stainless steel high pressure reactor with a polytetrafluoroethylene liner under the condition that any surfactant and template agent are not added, reacting at the temperature of 160-220 DEG C for 16-20 hours, cooling to room temperature, taking the material out of the reactor, performing suction filtration on the solution, washing for several times so as to remove impurities by using deionized water, drying at the temperature of 60 DEG C for 2 hours, thereby obtaining a white powdery substance; performing high-temperature calcination on the white powdery substance at the temperature of 450-600 DEG C in a muffle furnace for 2 hours, thereby obtaining the flower type three-dimensional Nb2O5. The method disclosed by the invention is simple in operating process, low in time consumption, readily available in raw materials, non-toxic and harmless in solvent and environmentally friendly.
Description
Technical field the invention belongs to field of material technology, particularly to a kind of preparation method of nano material.
Background technology nb2o5As a kind of important oxide material, because having outstanding physics and chemical property, in light
The fields such as electro-catalysis, solaode, biosensor, lithium ion battery and hybrid super capacitor have potentially should
With, the application especially in hybrid super capacitor, cause the extensive concern of researcher in recent years, become and grind both at home and abroad
The focus studied carefully, but nb2o5The relatively low electrical conductivity of itself and its optimal crystal structure shortcoming very rambunctious constrain it in mixing
Application in type ultracapacitor.Research shows that the pattern of coordination electrode material and microstructure can improve it on slight level
Electrical conductivity, and have been reported by controlling obtained from pattern one-dimensional, two-dimentional and three-dimensional (being assembled by one-dimensional nano structure)
The super capacitor anode material co of nanostructured3o4There is preferable chemical property, but also do not have preparation at present by a wiener
Rice rod is self-assembled into the three-dimensional nb of flower pattern2o5The relevant report of nano material.
Content of the invention is it is an object of the invention to provide a kind of method is simple, raw material is easy to get, nontoxic 1-dimention nano
Rod is self-assembled into the three-dimensional nb of flower pattern2o5Preparation method.
The present invention is mainly with nbcl5、ho2cco2h·2h2o、nh4F is raw material, using hydro-thermal reaction method and high-temperature calcination
The method combining prepares the three-dimensional nb that monodimension nano stick is self-assembled into flower pattern2o5Nano material.
The preparation method of the present invention is as follows:
(1) press every 10ml deionized water and add 0.273g nbcl5Ratio, by nbcl under vigorous magnetic stirring5It is dissolved in
In deionized water, produce white flock precipitate, form white opacity liquid.
(2) press nbcl5:ho2cco2h·2h2O mol ratio is the ratio of 1:5, by the ho of 1m2cco2h·2h2O solution is dropwise
Add in the white opacity liquid of step (1) gained until solution is transparent.
(3) press every 10ml deionized water and add 0.1389～0.2894g nh4The ratio of f, by nh4F is dissolved in deionized water
In, the then ratio of 3:2 by volume, by nh4F solution instills in the clear solution of step (2) gained, and completion of dropping is follow-up
Continuous stirring 2h.
(4) solution of step (3) is put into in teflon-lined rustless steel autoclave, 160～
16～20h is reacted at 220 DEG C.
(5) it is cooled to and takes out reactor after room temperature, solution sucking filtration is washed with deionized for several times removing impurity, then
2h is dried at a temperature of 60 DEG C, obtains white powder material.
(6) the white powder material obtaining step (5), in 450～600 DEG C of high-temperature calcination 2h in Muffle furnace, obtains
It is self-assembled into the three-dimensional nb of flower pattern by monodimension nano stick2o5.
The present invention compared with prior art has the advantage that
1st, synthesized the three-dimensional nb2o5 nano material being self-assembled into flower pattern by monodimension nano stick first.
2nd, any surfactant and template need not be added.
3rd, the method operating process is simple, takes few, raw material is easy to get, and nontoxic solvent is harmless, environmental friendliness.
Brief description
Fig. 1 is the three-dimensional nb that the monodimension nano stick that the embodiment of the present invention 1 obtains is self-assembled into flower pattern2o5The xrd of nano material
Figure.
Fig. 2 is the three-dimensional nb that the monodimension nano stick that the embodiment of the present invention 1 obtains is self-assembled into flower pattern2o5The sem of nano material
Figure.
Specific embodiment
Embodiment 1
By 0.546g nbcl under vigorous magnetic stirring5It is dissolved in 20ml deionized water, produce white flock precipitate, shape
Become white opacity liquid.Then by the ho of about 10ml 1m2cco2h·2h2O solution is added dropwise in this white opacity liquid up to solution
Transparent.Again by the 0.3704g weighing nh4F is dissolved in the deionized water of 20ml, then by this nh4F solution instills above-mentioned gained
Clear solution in, after completion of dropping continue stirring 2h.This reactant liquor is proceeded to 80ml stainless with teflon-lined
In steel autoclave, 180 DEG C of reaction 18h, take out reactor after being cooled to room temperature, product sucking filtration are washed with deionized
For several times removing impurity, then 2h is dried at a temperature of 60 DEG C, obtains white powder material.By this white powder material in Muffle
In 500 DEG C of high-temperature calcination 2h in stove, obtain the three-dimensional nb that monodimension nano stick is self-assembled into flower pattern2o5(as shown in Figure 2).Its crystal
Structure is orthorhombic phase structure (as shown in Figure 1).
Embodiment 2
By 0.546g nbcl under vigorous magnetic stirring5It is dissolved in 20ml deionized water, produce white flock precipitate, shape
Become white opacity liquid.Then by about 10ml about 1m ho2cco2h·2h2O solution be added dropwise in this white opacity liquid until
Solution is transparent, then by the 0.2788g weighing nh4F is dissolved in the deionized water of 20ml, then by this nh4F solution instills above-mentioned
In the clear solution of gained, after completion of dropping, continue stirring 2h.This reactant liquor is proceeded to 80ml and carries teflon-lined
In rustless steel autoclave, 160 DEG C of reaction 20h, take out reactor, by product sucking filtration, deionized water after being cooled to room temperature
Washing is for several times removing impurity, then 2h is dried at a temperature of 60 DEG C, obtains white powder material.This white powder material is existed
In 550 DEG C of high-temperature calcination 2h in Muffle furnace, obtain the three-dimensional nb that monodimension nano stick is self-assembled into flower pattern2o5Nano material.Its crystal
Structure is orthorhombic phase structure.
Embodiment 3
By 0.546g nbcl under vigorous magnetic stirring5It is dissolved in 20ml deionized water, produce white flock precipitate, shape
Become white opacity liquid.Then by about 10ml about 1m ho2cco2h·2h2O solution be added dropwise in this white opacity liquid until
Solution is transparent.Again by the 0.463g weighing nh4F is dissolved in the deionized water of 20ml, then by this nh4F solution instills above-mentioned
In the clear solution of gained, after completion of dropping, continue stirring 2h.This reactant liquor is proceeded to 80ml and carries teflon-lined
In rustless steel autoclave, 200 DEG C of reaction 16h, take out reactor, by product sucking filtration, deionized water after being cooled to room temperature
Washing is for several times removing impurity, then 2h is dried at a temperature of 60 DEG C, obtains white powder material.This white powder material is existed
In 450 DEG C of high-temperature calcination 2h in Muffle furnace, obtain the nb that monodimension nano stick is self-assembled into flower pattern2o5Nano material.Its crystal is tied
Structure is orthorhombic phase structure.
Embodiment 4
By 0.546g nbcl under vigorous magnetic stirring5It is dissolved in 20ml deionized water, produce white flock precipitate, shape
Become white opacity liquid.Then by about 10ml about 1m ho2cco2h·2h2O solution be added dropwise in this white opacity liquid until
Solution is transparent.Again by the 0.5556g weighing nh4F is dissolved in the deionized water of 20ml, then by this nh4F solution instills above-mentioned
In the clear solution of gained, after completion of dropping, continue stirring 2h.This reactant liquor is proceeded to 80ml and carries teflon-lined
In rustless steel autoclave, 220 DEG C of reaction 16h, take out reactor, by product sucking filtration, deionized water after being cooled to room temperature
Washing is for several times removing impurity, then 2h is dried at a temperature of 60 DEG C, obtains white powder material.This white powder material is existed
In 600 DEG C of high-temperature calcination 2h in Muffle furnace, obtain the nb that monodimension nano stick is self-assembled into flower pattern2o5Nano material.Its crystal structure
For orthorhombic phase structure.
Claims (1)
1. a kind of monodimension nano stick is self-assembled into the three-dimensional nb of flower pattern2o5Preparation method it is characterised in that: it includes walking as follows
Rapid:
(1) press every 10ml deionized water and add 0.273g nbcl5Ratio, by nbcl under vigorous magnetic stirring5Be dissolved in from
In sub- water, produce white flock precipitate, form white opacity liquid；
(2) press nbcl5: ho2cco2h·2h2The mol ratio of o is the ratio of 1:5, by 1m ho2cco2h·2h2O solution is added dropwise over
Until solution is transparent in the white opacity liquid of step (1) gained；
(3) press every 10ml deionized water and add 0.1389～0.2894g nh4The ratio of f, by nh4F is dissolved in deionized water,
Then the ratio of 3:2 by volume, by nh4F solution instills in the clear solution of step (2) gained, continues to stir after completion of dropping
Mix 2h；
(4) solution of step (3) is put into in teflon-lined rustless steel autoclave, at 160～220 DEG C
Lower reaction 16～20h；
(5) it is cooled to and takes out reactor after room temperature, solution sucking filtration is washed with deionized for several times removing impurity, then 60
2h is dried at a temperature of DEG C, obtains white powder material；
(6) the white powder material obtaining step (5), in 450～600 DEG C of high-temperature calcination 2h in Muffle furnace, obtains by one
Dimension nanometer rods are self-assembled into the three-dimensional nb of flower pattern2o5.
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| CN106115781B (en) * | 2016-06-23 | 2017-09-22 | 南阳师范学院 | A kind of sea urchin shape Nb2O5Electrode material and preparation method thereof |
| CN106206077B (en) * | 2016-06-30 | 2019-03-05 | 江苏大学 | A kind of nanometer of niobium pentaoxide/FTO electrode material preparation method and its usage |
| CN106532028B (en) * | 2016-12-07 | 2019-12-13 | 南阳师范学院 | sea urchin-shaped niobium pentoxide for lithium ion battery cathode material and preparation method thereof |
| CN106745255B (en) * | 2016-12-07 | 2018-10-30 | 南阳师范学院 | Sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchical structure and preparation method thereof |
| CN106517326B (en) * | 2016-12-07 | 2019-02-22 | 南阳师范学院 | A kind of flower-shaped niobium pentaoxide material and preparation method thereof |
| CN106542578B (en) * | 2016-12-07 | 2018-08-28 | 南阳师范学院 | A kind of sea urchin shape niobium pentaoxide electrode material and preparation method thereof |
| CN106809879B (en) * | 2017-02-27 | 2018-07-27 | 湖南工业大学 | A kind of niobium pentoxide nano stick material and its preparation method and application with regular hollow quadratic box-like |
| CN107359328B (en) * | 2017-06-30 | 2019-12-20 | 陕西科技大学 | Preparation method of grape-shaped niobium oxide/carbon composite electrode material for lithium ion battery |
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| CN101700910B (en) * | 2009-11-24 | 2011-09-07 | 北京有色金属研究总院 | Preparation method of spherical nanoscale niobium pentaoxide powder |
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