CN105236487B - A kind of barium oxide nanosphere and preparation method thereof - Google Patents
A kind of barium oxide nanosphere and preparation method thereof Download PDFInfo
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- CN105236487B CN105236487B CN201510690007.5A CN201510690007A CN105236487B CN 105236487 B CN105236487 B CN 105236487B CN 201510690007 A CN201510690007 A CN 201510690007A CN 105236487 B CN105236487 B CN 105236487B
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- barium oxide
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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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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention provides a kind of barium oxide nanosphere and preparation method thereof, belong to nano material and technical field of nanometer material preparation.Its preparation process uses solvent-thermal process method, and solvent is the mixed solvent of water and alcohol, and vanadium oxonium ion is self-assembly of barium oxide nanometer sphere in the presence of template.A diameter of 50 ~ 5000 nm of barium oxide nanosphere.Synthesis technique of the present invention is easy, and extensively, cost is relatively low for raw material sources, the features such as the morphology controllable of material, with great Development volue and application prospect.
Description
Technical field
The present invention relates to a kind of barium oxide nanosphere, belong to nano material and technical field of nanometer material preparation；This hair
The bright preparation method for having further related to above-mentioned barium oxide nanosphere.
Background technology
Nanosecond science and technology are a cross disciplines that is emerging and developing rapidly, be related to physics, chemistry, material, information, biology,
The every field such as medical science, the energy.The new industrial revolution will be brought by generally believing the development of nanosecond science and technology in the world, and be mankind's warp
Ji social development brings new opportunity, by one of science and technology as 21 century main flow.The research of nano material is to new material
Design and development and people there is important value and application prospect to the structural behaviour understanding of material.
Barium oxide due to its excellent performance so as to electrochemistry, catalysis, sensor, intelligence cladding, optical information storage,
The extensive use in the fields such as photoswitch, photochromic, electrochromism and infrared acquisition.The barium oxide nanometer of different type pattern
Material is reported in succession, such as：Krumeich etc. is reported using three isopropanol oxidation vanadium and prepared by template of fatty amine
The Performance of Vanadium Oxide Nanotubes (J. Am. Chem. Soc., 1999,121,8324-8331) of similar carbon nano tube structure.
Zero dimensional nanometer materials refer to the material that nanoscale is on three dimensions, mainly there is a cluster, nano-particle,
Nano-hollow ball and nanosphere etc..Nanosphere is as a kind of nanostructured, with specific surface area is big, density is small, surface penetration energy
Power is strong, good stability the features such as.Therefore had a wide range of applications in terms of chemistry, biology, material, medicine.Thanh-Dinh
Nguyen is with VO (O2)2(TOA) it is vanadium source predecessor, oleyl amine is surfactant；Using methylamine as solvent, under solvent thermal reaction, system
For a diameter of 4 nm nanoparticle；Be prepared for during using ethanol as solvent the nm of diameter 20 ~ 25 particulate (Langmuir,
2009, 25(9): 5322~5332)。
At present, barium oxide nanosphere still belongs to blank, and there is not been reported.
The content of the invention
The present invention is directed to above-mentioned problems of the prior art there is provided a kind of barium oxide nanosphere, by vanadium oxonium ion
Obtained, the problem of solving in the prior art also in blank by solvent-thermal process method in the presence of template.
Another object of the present invention is to provide a kind of barium oxide nanosphere preparation method.
Technical scheme is as follows：
Barium oxide nanosphere, is formed by vanadium oxonium ion self assembly, a diameter of 50 ~ 5000 nm of barium oxide nanosphere.
The invention provides the preparation method of above-mentioned barium oxide nanosphere is as follows：
Required solvent is prepared according to volume ratio first, described solvent is the mixed solvent of water and alcohol, water and alcohol
Ratio be 1:0.1~10.
Vanadium source is fully reacted with template in mixed solvent afterwards and is hydrolyzed, the consumption of template and the consumption of vanadium
Mol ratio 1：0.1~10；The ratio of vanadium source and mixed solvent is 1mol:50~200 L；
Reacted material is subjected to crystallization again, crystallization temperature is 100 ~ 250 DEG C, and crystallization time is 2 ~ 10 d.
Described alcohol is C1 ~ C6 monohydric alcohol or dihydric alcohol.
Described template is aniline or p-phenylenediamine；Described vanadium source is vanadyl oxalate or vanadyl acetylacetonate.
The preferred molar ratio of the consumption of described template and the consumption of vanadium is 1：1~5.
Described vanadium source and the ratio of mixed solvent are preferably 1 mol:100~150 L.
Described crystallization temperature is preferably 150 ~ 200 DEG C, and crystallization time is preferably 4 ~ 8 d.
Described hydrolytic process is:Template is dissolved in the mixed solvent prepared in proportion, while vanadium source is also molten
Vanadium liquid is slowly added into above-mentioned template solution by solution under agitation in same mixed solvent, play after finishing
Strong stirring is allowed to fully reaction.
In a word, method disclosed by the invention has the advantage that：The template and vanadium source used is relatively common, prepares cost ratio
It is relatively low；The preparation technology flow used is simple, and the pattern of resulting nano material is special, and hierarchical structure understands, and controllable.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that embodiment 1 obtains sample.
Fig. 2 is the scanning electron microscope (SEM) photograph that embodiment 2 obtains sample.
Fig. 3 is the scanning electron microscope (SEM) photograph that embodiment 3 obtains sample.
Fig. 4 is the scanning electron microscope (SEM) photograph that embodiment 4 obtains sample.
Fig. 5 is the scanning electron microscope (SEM) photograph that embodiment 5 obtains sample.
Fig. 6 is the scanning electron microscope (SEM) photograph that embodiment 6 obtains sample.
Embodiment
Embodiment 1
20 mmol vanadyl oxalates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water and alcohol
Volume ratio be, water：Ethanol=1:4；Template is made in the mixed solvent that 20 mmol p-phenylenediamine are added to 50 mL water and alcohol
The volume ratio of solution, its reclaimed water and alcohol is, water：Ethanol=1:4；Above-mentioned vanadium liquid is added under stirring state above-mentioned containing template
In the solution of agent, 1 h is stirred vigorously afterwards and is allowed to abundant reaction, its reacted material is then moved into polytetrafluoroethylsubstrate substrate
Stainless steel cauldron in, the d of crystallization 5 at 180 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol simultaneously
1 d is sufficiently stirred at room temperature refilter after organic matter to remove completely, is dried at 70 DEG C, is obtained barium oxide nanosphere.Its
ESEM is Fig. 1.
Embodiment 2
20 mmol vanadyl oxalates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water and alcohol
Volume ratio be, water：Ethanol=1:0.5；40 mmol p-phenylenediamine are added and obtain containing mould in the mixed solvent of 50 mL water and alcohol
The volume ratio of the solution of plate agent, its reclaimed water and alcohol is, water：Ethanol=1:0.5, above-mentioned vanadium liquid is added under stirring state above-mentioned
In solution containing template, 1 h is stirred vigorously afterwards and is allowed to abundant reaction, polytetrafluoroethylsubstrate substrate is then moved it into not
In rust steel reactor, the d of crystallization 5 at 160 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol and in room
1 d is sufficiently stirred under temperature refilter after organic matter to remove completely, is dried at 70 DEG C, is obtained barium oxide nanosphere.It is scanned
Electronic Speculum is Fig. 2.
Embodiment 3
20 mmol vanadyl oxalates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water and alcohol
Volume ratio be, water：Ethanol=1:0.25,60 mmol aniline are added and obtain containing template in the mixed solvent of 50 mL water and alcohol
The volume ratio of the solution of agent, its reclaimed water and alcohol is, water：Ethanol=1:0.25, above-mentioned vanadium liquid is added to above-mentioned contain under stirring state
Have in the solution of template, 1 h is stirred vigorously afterwards and is allowed to abundant reaction, the stainless of polytetrafluoroethylsubstrate substrate is then moved it into
In steel reactor, the crystallization 3d at 200 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol and in room temperature
Under be sufficiently stirred for 1 d and refiltered after organic matter with being removed completely, dried at 70 DEG C, obtain barium oxide nanosphere.It scans electricity
Mirror is Fig. 3.
Embodiment 4
20 mmol vanadyl acetylacetonates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water
Volume ratio with alcohol is, water：Ethanol=1:1, it will separately be obtained in the mixed solvent of 40 mmol p-phenylenediamine, 50 mL water of addition and alcohol
The volume ratio of template solution, its reclaimed water and alcohol is, water：Ethanol=1:1, vanadium liquid is added to containing template under stirring state
Solution in, 1 h is stirred vigorously afterwards and is allowed to abundant reaction, the stainless steel cauldron of polytetrafluoroethylsubstrate substrate is then moved it into
In, the d of crystallization 6 at 150 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol and fully stirred at room temperature
Mix 1 d refilter after organic matter to remove completely, dried at 70 DEG C, obtain barium oxide nanosphere.Its ESEM is Fig. 4.
Embodiment 5
20 mmol vanadyl acetylacetonates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water
Volume ratio with alcohol is, water：Ethanol=1:1, separately it will obtain template in the mixed solvent of 80 mmol aniline, 50 mL water of addition and alcohol
The volume ratio of agent solution, its reclaimed water and alcohol is, water：Ethanol=1:1, vanadium liquid is added to containing the molten of template under stirring state
In liquid, 1 h is stirred vigorously afterwards and is allowed in abundant reaction, the stainless steel cauldron for then moving it into polytetrafluoroethylsubstrate substrate,
The d of crystallization 3 at 200 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol and 1 is sufficiently stirred at room temperature
D refiltered after organic matter with being removed completely, is dried at 70 DEG C, is obtained barium oxide nanosphere.Its ESEM is Fig. 5.
Embodiment 6
20 mmol vanadyl acetylacetonates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water
Volume ratio with alcohol is, water：Ethanol=1:0.5,20 mmol p-phenylenediamine are added and obtained in the mixed solvent of 50 mL water and alcohol
The volume ratio of template solution, its reclaimed water and alcohol is, water：Ethanol=1:0.5, vanadium liquid is added to containing template under stirring state
In the solution of agent, 1 h is stirred vigorously afterwards and is allowed to abundant reaction, the stainless steel reaction of polytetrafluoroethylsubstrate substrate is then moved it into
In kettle, the d of crystallization 8 at 140 DEG C.Product passes through washing filtering, filter cake is transferred in 50 mL ethanol and abundant at room temperature
Stir 1 d refilter after organic matter to remove completely, dried at 70 DEG C, obtain barium oxide nanosphere.Its ESEM is figure
6。
Embodiment 7
20 mmol vanadyl acetylacetonates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water
Volume ratio with alcohol is, water：Ethylene glycol=1:1,40 mmol aniline are added in the mixed solvent of 50 mL water and alcohol and obtain template
The volume ratio of agent solution, its reclaimed water and alcohol is, water：Ethylene glycol=1:1, vanadium liquid is added to containing template under stirring state
In solution, 1 h is stirred vigorously afterwards and is allowed to abundant reaction, the stainless steel cauldron of polytetrafluoroethylsubstrate substrate is then moved it into
In, the d of crystallization 6 at 160 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol and fully stirred at room temperature
Mix 1 d refilter after organic matter to remove completely, dried at 70 DEG C, obtain barium oxide nanosphere.
Embodiment 8
20 mmol vanadyl oxalates are added in the mixed solvent of 50 mL water and alcohol and obtain vanadium solution, its reclaimed water and alcohol
Volume ratio be, water：Hexanol=1:5,40 mmol p-phenylenediamine are added in the mixed solvent of 50 mL water and alcohol and obtain template
The volume ratio of solution, its reclaimed water and alcohol is, water：Hexanol=1:5, vanadium liquid is added to the solution containing template under stirring state
In, 1 h is stirred vigorously afterwards to be allowed in abundant reaction, the stainless steel cauldron for then moving it into polytetrafluoroethylsubstrate substrate,
Crystallization 4d at 180 DEG C.Product passes through washing filtering, and filter cake is transferred in 50 mL ethanol and 1 d is sufficiently stirred at room temperature
Refiltered after organic matter with being removed completely, dried at 70 DEG C, obtain barium oxide nanosphere.
Embodiment 9
Required solvent is prepared according to volume ratio first, described solvent is water and the mixed solvent of methanol, water with
The ratio of methanol is 1:0.1；
Vanadyl oxalate is fully reacted with aniline in mixed solvent afterwards and is hydrolyzed, the consumption and vanadyl oxalate of aniline
Consumption mol ratio 1：0.1；The ratio of vanadyl oxalate and mixed solvent is 1mol:50 L；
Reacted material is subjected to crystallization again, crystallization temperature is 100 DEG C, and crystallization time is 10 d.
Other step be the same as Examples 1.
Embodiment 10
Required solvent is prepared according to volume ratio first, described solvent is water and the mixed solvent of propyl alcohol, water with
The ratio of propyl alcohol is 1: 10；
By vanadyl acetylacetonate and phenylenediamine, fully reaction is hydrolyzed in mixed solvent afterwards, the consumption of phenylenediamine with
The mol ratio 1 of the consumption of vanadyl acetylacetonate：10；The ratio of vanadyl acetylacetonate and mixed solvent is 1mol: 200 L；
Reacted material is subjected to crystallization again, crystallization temperature is 250 DEG C, and crystallization time is 2d.
Other step be the same as Examples 1.
Embodiment 11
Required solvent is prepared according to volume ratio first, described solvent is water and the mixed solvent of butanol, water with
The ratio of butanol is 1:5；
Vanadyl acetylacetonate is fully reacted with aniline in mixed solvent afterwards and is hydrolyzed, the consumption and acetyl of aniline
The mol ratio of the consumption of acetone vanadyl:1：5；The ratio of vanadyl acetylacetonate and mixed solvent is 1 mol:100 L；
Reacted material is subjected to crystallization again, crystallization temperature is 150 DEG C, and crystallization time is 8d.
Other step be the same as Examples 1.
Embodiment 12
Required solvent is prepared according to volume ratio first, described solvent is water and the mixed solvent of amylalcohol, water with
The ratio of amylalcohol is 1:6；
Vanadyl oxalate is fully reacted with phenylenediamine in mixed solvent afterwards and is hydrolyzed, the consumption and oxalic acid of phenylenediamine
The mol ratio of the consumption of vanadyl:1：1；The ratio of vanadyl oxalate and mixed solvent is 1 mol: 150 L；
Reacted material is subjected to crystallization again, crystallization temperature is 200 DEG C, and crystallization time is 4d.
Other step be the same as Examples 1.
Methanol, propyl alcohol, butanol, amylalcohol, hexylene glycol, butanediol can be replaced ethanol, other step be the same as Examples by the present invention
1, obtain corresponding barium oxide nanosphere.
Above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to the embodiment of the present invention and is retouched
The technical scheme stated.It will be understood by those within the art that, still the present invention can be modified or equivalent,
To reach identical technique effect.As long as satisfaction uses needs, all within the scope of the present invention.
Claims (4)
1. the preparation method of barium oxide nanosphere, barium oxide nanosphere is formed by vanadium oxonium ion self assembly, barium oxide is received
A diameter of 50 ~ 5000 nm of rice ball；
It is characterized in that comprising the following steps：
Required solvent is prepared according to volume ratio first, described solvent is the ratio of water and the mixed solvent of alcohol, water and alcohol
Example is 1:0.1~10；
Vanadium source is fully reacted with template in mixed solvent afterwards and is hydrolyzed, the consumption of template and the consumption in vanadium source
Mol ratio is 1：1~5；The ratio of vanadium source and mixed solvent is 1 mol:50~200 L；
Reacted material is subjected to crystallization again, crystallization temperature is 100 ~ 250 DEG C, and crystallization time is 2 ~ 10 d；Described alcohol is
C1 ~ C6 monohydric alcohol or dihydric alcohol；Described template is aniline or p-phenylenediamine；Described vanadium source is vanadyl oxalate or acetyl
Acetone vanadyl.
2. the preparation method of barium oxide nanosphere according to claim 1, it is characterised in that described vanadium source is with mixing
The ratio of solvent is 1 mol:100~150 L.
3. the preparation method of barium oxide nanosphere according to claim 1, it is characterised in that described crystallization temperature is
150 ~ 200 DEG C, crystallization time is 4 ~ 8 d.
4. the preparation method of barium oxide nanosphere according to claim 1, it is characterised in that described hydrolytic process is:
Template is dissolved in the mixed solvent prepared in proportion, while vanadium source is also dissolved in same mixed solvent, stirred
Vanadium liquid is slowly added into above-mentioned template solution in the case of mixing, is stirred vigorously after finishing and is allowed to fully reaction.
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| CN102616850A (en) * | 2012-04-11 | 2012-08-01 | 黑龙江大学 | Preparation method for monodisperse vanadium pentoxide solid microspheres |
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| CN101830511B (en) * | 2010-05-18 | 2012-10-31 | 中国科学院上海硅酸盐研究所 | Preparation method of rutile phase vanadium dioxide hollow sphere and application |
| US9997778B2 (en) * | 2012-11-05 | 2018-06-12 | University Of Washington Through Its Center For Commercialization | Polycrystalline vanadium oxide nanosheets |
| CN103011290B (en) * | 2012-11-23 | 2014-05-28 | 湖北大学 | Method for preparing vanadium trioxide microsphere powder under induction action of tartaric acid |
| CN103811741B (en) * | 2014-02-26 | 2016-01-06 | 武汉理工大学 | Barium oxide nanowire wrap around the flower-shaped hollow microsphere of chestnut and its preparation method and application |
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