CN106745255A - Sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy and preparation method thereof - Google Patents
Sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy and preparation method thereof Download PDFInfo
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- CN106745255A CN106745255A CN201611118323.6A CN201611118323A CN106745255A CN 106745255 A CN106745255 A CN 106745255A CN 201611118323 A CN201611118323 A CN 201611118323A CN 106745255 A CN106745255 A CN 106745255A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G33/00—Compounds of niobium
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- C01—INORGANIC CHEMISTRY
- 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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- C—CHEMISTRY; METALLURGY
- 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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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a kind of preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy, comprise the following steps：Niobium oxalate and ammonium acid fluoride are dissolved in deionized water by a certain percentage；Resulting solution is loaded into autoclave heating response；After cooling sea urchin shape Nb is obtained final product through washing, dry, roasting2O5Microballoon.Sea urchin shape Nb prepared by the present invention2O5Microballoon pattern is homogeneous, good dispersion；Sea urchin shape Nb prepared by the present invention2O5Microballoon specific surface area is big, not only has the advantages that nanostructured, and many new physicochemical characteristics produced with micro-nano multi-level structure, has potential application value in fields such as photocatalysis, photosensitive dye battery, capacitor and lithium ion batteries.
Description
Technical field
The invention belongs to inorganic nano material synthesis field, specifically, it is related to a kind of sea with micro-nano hierarchy
Courage shape niobium pentaoxide microballoon and preparation method thereof.
Background technology
Niobium pentaoxide (Nb2O5) it is a kind of n-type semiconductor, energy gap is 3.4eV, is widely used in light and urges
The field such as change, photosensitive dye battery, capacitor and lithium ion battery.Currently, lot of research confirm material performance with
Its size and pattern etc. have close relationship.For example, Sasidharan et al. (M.Sasidharan, et al.Nb2O5hollow
nanospheres as anode material for enhanced performance in lithium ion
The 2161-2164. of batteries.Materrial Research Bulletin 47 (2012)) to synthesize hollow Nano spherical
Nb2O5, preferable chemical property is shown as lithium ion battery negative.In recent years, by the overall micro- of nano unit assembling
The micro-nano grading structure material of meter level not only has the advantages that nano unit but also some distinctive physicochemical characteristics (ratios because of it
Such as cooperative effect and coupling effect), cause paying close attention to for researcher.Lu et al. (H.Lu, K.Xiang, et
al.Urchin-shaped Nb2O5microspheres synthesized by the facile hydrothermal
method and their lithium ion storage performance.Materials Letters,167(2006)
106-108) synthesize sea urchin shape Nb2O5Microballoon, preferable chemical property is shown as lithium ion battery negative material.Specially
The preparation method and its application (application number as photochemical catalyst of a kind of niobium pentaoxide sea urchin shape Nano microsphere of profit：
201510900901.0, the applying date：2015-12-09, publication number：CN105384193A, publication date：2016-03-09) report
A kind of Nb2O5Sea urchin shape Nano microsphere, excellent performance is shown with photocatalyst.
Appearance structure has a significant impact to the performance tool of niobium pentaoxide, also rarely has at present on micro-nano hierarchy
Sea urchin shape niobium pentaoxide microballoon document report.
The content of the invention
In view of this, the present invention is directed to above-mentioned problem, there is provided a kind of oxygen of sea urchin shape five with micro-nano hierarchy
Change two niobium microballoons and preparation method thereof, the sea urchin shape Nb prepared using the method2O5Pattern rule, good dispersion, can extensive use
In fields such as photocatalysis, photosensitive dye battery, lithium ion battery and capacitors.
In order to solve the above-mentioned technical problem, the invention discloses a kind of oxidation of sea urchin shape five two with micro-nano hierarchy
The preparation method of niobium microballoon, does not write temporarily.
Further, comprise the following steps：
Step 1), niobium oxalate and ammonium acid fluoride be added in deionized water by a certain percentage under agitation, stir
0.1-24 hours；
Step 2), by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature
Heating response in drying box；
Step 3), by step 2) gained reaction precipitate washs 3-9 times with ethanol and deionized water, is subsequently placed in very respectively
Dried in empty drying box；
Step 4), by step 3) gained powder is placed in tubular type kiln roasting, obtains final product the sea urchin shape with micro-nano hierarchy
Nb2O5Microballoon.
Further, step 1) concentration of niobium is 0.022-0.028mol/L in the solution for preparing.
Further, step 1) mol ratio of mesoxalic acid niobium and ammonium acid fluoride is 1:0.1-1:0.6.
Further, step 2) in heating-up temperature be 178-185 DEG C, the heat time be 20-30 hours.
Further, step 3) in vacuum drying temperature be 60-120 DEG C.
Further, step 4) in sintering temperature be 600-1000 DEG C, roasting time be 0.5-1.5 hours.
The invention also discloses a kind of sea urchin shape with micro-nano hierarchy prepared by above-mentioned preparation method
Niobium pentaoxide microballoon.
Compared with prior art, the present invention can be obtained including following technique effect：
1) the sea urchin shape Nb of present invention synthesis2O5Microballoon is assembled by nano-filaments and formed, and the diameter of nano-filaments is about
5-20 nanometers, the diameter of microballoon is about 1 micron, and with preferable dispersiveness.
2) the sea urchin shape Nb of present invention synthesis2O5Microballoon specific surface area is big, not only has the advantages that nanostructured, and tool
There are some distinctive physicochemical characteristics (such as cooperative effect etc.).
3) the sea urchin shape Nb of present invention synthesis2O5Microballoon is in photocatalysis, photosensitive dye battery, capacitor and lithium-ion electric
The fields such as pond have potential application value.
4) present invention has process is simple, and reaction controllability is strong, it is easy to large-scale industrial production.
Certainly, implementing any product of the invention must be not necessarily required to while reaching all the above technique effect.
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes a part of the invention, this hair
Bright schematic description and description does not constitute inappropriate limitation of the present invention for explaining the present invention.In the accompanying drawings：
Fig. 1 is that the embodiment of the present invention 1 prepares sea urchin shape Nb2O5The x-ray diffraction pattern of microballoon；
Fig. 2 is that the embodiment of the present invention 1 prepares sea urchin shape Nb2O5ESEM (SEM) photo of microballoon；
Fig. 3 is that the embodiment of the present invention 1 prepares sea urchin shape Nb2O5Transmission electron microscope (TEM) photo of microballoon；
Fig. 4 is ESEM (SEM) photo for the product that comparative example of the present invention 1 is prepared；
Fig. 5 is ESEM (SEM) photo for the product that comparative example of the present invention 2 is prepared.
Specific embodiment
Describe embodiments of the present invention in detail below in conjunction with drawings and Examples, thereby how the present invention is applied
Technological means can fully understand and implement according to this to solve technical problem and reach the implementation process of technology effect.
Embodiment 1
Step 1) it is under agitation in molar ratio 1 by niobium oxalate and ammonium acid fluoride:0.5 is added in deionized water,
Stirring 24 hours, the concentration of niobium is 0.026mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 24 hours at 180 DEG C；
Step 3) by step 2) gained reaction precipitate washed 3-9 times with ethanol and deionized water respectively, is subsequently placed in temperature
Spend in the vacuum drying chamber for 80 DEG C and dry；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 1 hour at 600 DEG C, obtain final product with micro-nano point
The sea urchin shape Nb of level structure2O5Microballoon.
As shown in figure 1, the diffraction maximum of sample and Nb in PDF cards2O5Standard diffraction peak coincide, do not find that other are miscellaneous
Mass peak, illustrates that the sample of synthesis is purer.As shown in Fig. 2 sample has well-regulated sea urchin shape microballoon pattern, and with preferable point
Dissipate property.As shown in figure 3, sea urchin shape Nb2O5It is to be constructed to form by a large amount of nanobelts.
Embodiment 2
Step 1) it is under agitation in molar ratio 1 by niobium oxalate and ammonium acid fluoride:0.1 is added in deionized water,
Stirring 14 hours, the concentration of niobium is 0.022mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 30 hours at 178 DEG C；
Step 3) by step 2) gained reaction precipitate washed 3-9 times with ethanol and deionized water respectively, is subsequently placed in temperature
Spend in the vacuum drying chamber for 110 DEG C and dry；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 1.5 hours at 600 DEG C, obtain final product with micro-nano
The sea urchin shape Nb of hierarchy2O5Microballoon.
Embodiment 3
Step 1) it is under agitation in molar ratio 1 by niobium oxalate and ammonium acid fluoride:0.6 is added in deionized water,
Stirring 10 hours, the concentration of niobium is 0.028mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 20 hours at 180 DEG C；
Step 3) by step 2) gained reaction precipitate washed 3-9 times with ethanol and deionized water respectively, is subsequently placed in temperature
Spend in the vacuum drying chamber for 100 DEG C and dry；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 0.5 hour at 1000 DEG C, obtain final product with micro-nano
The sea urchin shape Nb of hierarchy2O5Microballoon.
Embodiment 4
Step 1) it is under agitation in molar ratio 1 by niobium oxalate and ammonium acid fluoride:0.4 is added in deionized water,
Stirring 3 hours, the concentration of niobium is 0.024mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 24 hours at 185 DEG C；
Step 3) by step 2) gained reaction precipitate washed 3-9 times with ethanol and deionized water respectively, is subsequently placed in temperature
Spend in the vacuum drying chamber for 60 DEG C and dry；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 1.2 hours at 800 DEG C, obtain final product with micro-nano
The sea urchin shape Nb of hierarchy2O5Microballoon.
Embodiment 5
Step 1) it is under agitation in molar ratio 1 by niobium oxalate and ammonium acid fluoride:0.3 is added in deionized water,
Stirring 0.1 hour, the concentration of niobium is 0.027mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 28 hours at 182 DEG C；
Step 3) by step 2) gained reaction precipitate washed 3-9 times with ethanol and deionized water respectively, is subsequently placed in temperature
Spend in the vacuum drying chamber for 120 DEG C and dry；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 1 hour at 900 DEG C, obtain final product with micro-nano point
The sea urchin shape Nb of level structure2O5Microballoon.
Comparative example 1
Step 1) it is under agitation in molar ratio 1 by columbium pentachloride and ammonium acid fluoride:0.5 is added to deionized water
In, stirring 24 hours, the concentration of niobium is 0.026mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 24 hours at 180 DEG C；
Step 3) by step 2) gained reaction precipitate washs 3-9 times with ethanol and deionized water, is subsequently placed in very respectively
Dried in empty drying box；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 1 hour at 600 DEG C, cannot have micro-nano
The sea urchin shape Nb of hierarchy2O5Microballoon.As shown in figure 4, sample shows random pattern.
Comparative example 2
Step 1) it is under agitation in molar ratio 1 by ammonium niobium oxalate and ammonium acid fluoride:0.5 is added to deionized water
In, stirring 24 hours, the concentration of niobium is 0.026mol/L wherein in solution；
Step 2) by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in constant temperature and does
In dry case, heating response 24 hours at 180 DEG C；
Step 3) by step 2) gained reaction precipitate washs 3-9 times with ethanol and deionized water, is subsequently placed in very respectively
Dried in empty drying box；
Step 4) by step 3) gained powder is placed in tube furnace, is calcined 1 hour at 600 DEG C, cannot have micro-nano
The sea urchin shape Nb of hierarchy2O5Microballoon.As shown in figure 5, sample shows uneven bulk morphologies.
Described above has shown and described some preferred embodiments of invention, but as previously described, it should be understood that invention is not
Form disclosed herein is confined to, the exclusion to other embodiment is not to be taken as, and can be used for various other combinations, modification
And environment, and can be carried out by the technology or knowledge of above-mentioned teaching or association area in invention contemplated scope described herein
Change.And the change and change that those skilled in the art are carried out do not depart from the spirit and scope of invention, then all should be in the appended power of invention
In the protection domain that profit is required.
Claims (7)
1. a kind of preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy, it is characterised in that including with
Lower step：
Step 1), niobium oxalate and ammonium acid fluoride be added in deionized water by a certain percentage under agitation, stir 0.1-
24 hours；
Step 2), by step 1) resulting solution is transferred in the stainless steel cauldron of inner liner polytetrafluoroethylene, is placed in freeze-day with constant temperature
Heating response in case；
Step 3), by step 2) gained reaction precipitate washs 3-9 times with ethanol and deionized water respectively, is subsequently placed in vacuum dry
Dried in dry case；
Step 4), by step 3) gained powder is placed in tubular type kiln roasting, obtains final product the sea urchin shape Nb with micro-nano hierarchy2O5
Microballoon.
2. the preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy according to claim 1, its
It is characterised by, step 1) concentration of niobium is 0.022-0.028mol/L in the solution for preparing.
3. the preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy according to claim 1, its
It is characterised by, the step 1) mol ratio of mesoxalic acid niobium and ammonium acid fluoride is 1:0.1-1:0.6.
4. the preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy according to claim 1, its
Be characterised by, the step 2) in heating-up temperature be 178-185 DEG C, the heat time be 20-30 hours.
5. the preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy according to claim 1, its
Be characterised by, the step 3) in vacuum drying temperature be 60-120 DEG C.
6. the preparation method of the sea urchin shape niobium pentaoxide microballoon with micro-nano hierarchy according to claim 1, its
Be characterised by, the step 4) in sintering temperature for 600-1000 DEG C, roasting time is 0.5-1.5 hours.
7. the preparation method in a kind of 1-6 as claim described in any claim prepare with micro-nano hierarchy
Sea urchin shape niobium pentaoxide microballoon.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107739051A (en) * | 2017-11-27 | 2018-02-27 | 江苏大学 | A kind of method of the hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers |
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| CN103253708A (en) * | 2013-05-08 | 2013-08-21 | 北京工业大学 | Solvothermal preparation method of niobium pentoxide nanowire by use of acetic acid |
| CN104528827A (en) * | 2014-12-31 | 2015-04-22 | 湖州师范学院 | Hydrothermal preparation method for nanometer NbO2F powder |
| CN105384193A (en) * | 2015-12-09 | 2016-03-09 | 郑州轻工业学院 | Preparation method of niobium (V) pentoxide urchin-like nano sphere and application of nano sphere as photocatalyst |
| CN105384192A (en) * | 2015-11-20 | 2016-03-09 | 燕山大学 | Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 |
| CN106115781A (en) * | 2016-06-23 | 2016-11-16 | 南阳师范学院 | A kind of Hemicentrotus seu Strongylocentrotus shape Nb2o5electrode material and preparation method thereof |
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2016
- 2016-12-07 CN CN201611118323.6A patent/CN106745255B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103253708A (en) * | 2013-05-08 | 2013-08-21 | 北京工业大学 | Solvothermal preparation method of niobium pentoxide nanowire by use of acetic acid |
| CN104528827A (en) * | 2014-12-31 | 2015-04-22 | 湖州师范学院 | Hydrothermal preparation method for nanometer NbO2F powder |
| CN105384192A (en) * | 2015-11-20 | 2016-03-09 | 燕山大学 | Method for preparing one-dimensional nanorod self-assembled flower type three-dimensional Nb2O5 |
| CN105384193A (en) * | 2015-12-09 | 2016-03-09 | 郑州轻工业学院 | Preparation method of niobium (V) pentoxide urchin-like nano sphere and application of nano sphere as photocatalyst |
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| CN107739051A (en) * | 2017-11-27 | 2018-02-27 | 江苏大学 | A kind of method of the hot controlledly synthesis niobium pentaoxide micron ball of no templating solvent and micro-flowers |
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