CN100389073C - Preparation method of dendroid barium tungstate nano crystal - Google Patents
Preparation method of dendroid barium tungstate nano crystal Download PDFInfo
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- CN100389073C CN100389073C CNB2006101160198A CN200610116019A CN100389073C CN 100389073 C CN100389073 C CN 100389073C CN B2006101160198 A CNB2006101160198 A CN B2006101160198A CN 200610116019 A CN200610116019 A CN 200610116019A CN 100389073 C CN100389073 C CN 100389073C
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Abstract
The invention discloses a preparing method of branched-shaped barium tungstate nanometer crystal, which comprises the following steps: adopting micro-emulsion as media; allocating barium salt solution and sodium tungstate solution with the same quantity and density and octane, butanol and cetyl trimethyl ammonium bromide (CTAB) into transparent micro-emulsion according to certain rate; blending two emulsions within certain temperature scale rapidly; stirring for 1 min continuously to obtain the product.
Description
Technical field
The present invention relates to a kind of preparation method of dendroid barium tungstate nano crystal, in certain temperature range, adopting the microemulsion of reversed phase micelle is media, can obtain the dendrite of barium wolframate in the extremely short reaction times.Belong to the functional materials preparing technical field.
Background technology
Increasingly mature along with the nanometer technology of preparing, the nano material of exploitation different-shape, size, research size, pattern have become one of main direction of nanotechnology research to effect of material performance.Traditional phosphor is prepared into the nano material with certain pattern, utilizes nano effect, can further promote the performance of luminescent material.The barium wolframate of scheelite-type structure has superior luminescent properties and good colour developing, discoloration effect.Can be used as photoluminescence or laser donor material, have a wide range of applications and market potential exploitation value.At present, the method for preparing the tungstate nano material mainly contains solid phase method and liquid phase method: solid phase method comprises ball milled, solid reaction process, and liquid phase method comprises polymkeric substance companion method and reverse micelle microemulsion method.In the recent two decades, the inorganic nano material of different shape is successfully synthesized in the past, as: nano wire, nanotube, nano belt, nanometer sheet and nanometer tree branches etc.Wherein dendritic nanocrystal because its special 3D shape all has crucial meaning for research crystalline growth mechanism and exploitation property, and is subjected to countries in the world material scholar's attention.Studies show that in polymkeric substance/nano composite material, nanometer strengthens each diversity structure that particle produces high-sequential, obviously improves the mechanical property of materials.Dendrite has and helps other material is permeated in the matrix material, perhaps controllable structure is introduced in the matrix material.
The dendrite that obtains at present mainly comprises metal, semi-conductor, oxide compound, ternary metal salt etc., as silver, lead sulfide, zunsober, ferric oxide, baryta yellow etc.Its preparation method comprises vapor phase process, liquid phase method etc., but mostly exists shortcomings such as complicated process of preparation, long reaction time.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, propose a kind of preparation method of dendroid barium tungstate nano crystal, technology is simple, and is with low cost, can obtain the dendroid nanocrystal that is evenly distributed fast.
For realizing this purpose, it is that media prepares the barium tungstate nanometer crystal that the present invention adopts microemulsion.At first respectively with barium salt aqueous solution equivalent, same concentrations and the sodium wolframate aqueous solution, be mixed with transparent microemulsion with octane, propyl carbinol, cetyl trimethylammonium bromide (CTAB) by a certain percentage, in certain temperature range, after the rapid mixing of two kinds of microemulsions, continue to stir 1 minute, obtain white product, be the nanocrystal of dendroid barium wolframate.
Method of the present invention comprises following concrete steps:
1, the preparation of barium ion microemulsion:
At first in Erlenmeyer flask, add octane, propyl carbinol, cetyl trimethylammonium bromide (CTAB) successively, under magnetic agitation, add the barium salt aqueous solution then.Stirred 30 minutes, and formed the barium ion microemulsion of homogeneous phase transparent.Wherein the concentration of CTAB is 0.15～0.25moll
-1, the mol ratio of propyl carbinol and CTAB is 3.47～4.52, and the mole number of water is 30～40 with the ratio of CTAB mole number in the barium salt aqueous solution, and all the other are octane; Barium salt concentration of aqueous solution 0.1～0.2moll
-1
2, the preparation of tungstate ion microemulsion:
According to step 1, substitute the barium salt aqueous solution with same concentrations, isopyknic sodium wolframate aqueous solution, all the other compositions are identical with barium ion microemulsion composition, obtain the tungstate ion microemulsion.
The said barium salt of the present invention is: bariumchloride, nitrate of baryta.
3, dendroid barium tungstate nano crystal is synthetic:
Barium ion microemulsion and tungstate ion microemulsion with above-mentioned acquisition, in 20～35 ℃ of scopes, mix rapidly, continue to stir 1 minute, obtain the oyster white mixed solution, centrifugation, repeatedly wash with deionized water and dehydrated alcohol, 60 ℃ of vacuum dryings 6 hours can obtain to have the barium tungstate nanometer crystal of dendritic structure.
In the said certain temperature range of the present invention be:.
Method temperature of reaction of the present invention is low, and the reaction times is short, only needs 1 minute, and operation steps is simple, and cost is low, productive rate height, favorable repeatability.It is media that the present invention has adopted microemulsion, makes the dendroid nanocrystal size be evenly distributed, and has avoided the rapid generation of initial reaction stage bulky crystal.The dendrite of preparation is by a trunk, and four rows form perpendicular to the short branch of trunk.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of the embodiment of the invention 1 resulting dendroid barium tungstate crystal.(embodiment 1-2 has identical x-ray diffraction pattern).
Fig. 2 is the field emission scanning electron microscope photo and the transmission electron microscope photo of the embodiment of the invention 1 resulting dendroid barium tungstate crystal.
Fig. 3 is the transmission electron microscope photo of the embodiment of the invention 2 resulting dendroid barium tungstate crystals.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.Following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1
1) in a 50ml Erlenmeyer flask, adds 13.42ml octane, 1.08ml propyl carbinol, 1.2g cetyl trimethylammonium bromide (CTAB) successively, add the 0.2moll of 2ml under the magnetic agitation
-1Barium chloride solution.Stirred 30 minutes, and formed the barium ion microemulsion of homogeneous phase transparent.
2) in a 50ml Erlenmeyer flask, add 13.42ml octane, 1.08ml propyl carbinol, 1.2g cetyl trimethylammonium bromide (CTAB) successively, add the 0.2moll of 2ml under the magnetic agitation
-1The sodium wolframate aqueous solution.Stirred 30 minutes, and formed the tungstate ion microemulsion of homogeneous phase transparent.
3) the above-mentioned two kinds microemulsions that contain bariumchloride and sodium wolframate are respectively mixed rapidly at 25 ℃, continue to stir 1 minute, reaction finishes.Centrifugation is repeatedly washed with deionized water and dehydrated alcohol, and 60 ℃ of vacuum dryings 6 hours can obtain dendroid barium tungstate nano crystal.
The x-ray diffraction pattern of resulting dendroid barium tungstate crystal such as Fig. 1.Prepared as seen from Figure 1 material is the tetragonal structure barium wolframate.Fig. 2 is field emission scanning electron microscope photo and the transmission electron microscope photo that obtains the dendroid barium tungstate crystal.As seen from the figure, long 3～6 μ m of this dendritic structure trunk, branch head 300～500nm.
1) in a 50ml Erlenmeyer flask, adds 13.18ml octane, 1.20ml propyl carbinol, 1.3g cetyl trimethylammonium bromide (CTAB) successively, add the 0.15moll of 2.26ml under the magnetic agitation
-1Barium nitrate aqueous solution.Stirred 30 minutes, and formed the barium ion microemulsion of homogeneous phase transparent.
2) in a 50ml Erlenmeyer flask, add 13.18ml octane, 1.20ml propyl carbinol, 1.3g cetyl trimethylammonium bromide (CTAB) successively, add the 0.15moll of 2.26ml under the magnetic agitation
-1The sodium wolframate aqueous solution.Stirred 30 minutes, and formed the tungstate ion microemulsion of homogeneous phase transparent.
3) the above-mentioned two kinds microemulsions that contain nitrate of baryta and sodium wolframate are respectively mixed rapidly at 30 ℃, continue to stir 1 minute, reaction finishes.Centrifugation is repeatedly washed with deionized water and dehydrated alcohol, and 60 ℃ of vacuum dryings 6 hours can obtain the dendroid barium tungstate crystal.
Fig. 3 is resulting dendroid barium tungstate crystal transmission electron microscope photo.As seen from the figure, the long 3-10 μ of this dendritic structure trunk m, the long 100-300nm of branch.
Claims (2)
1. the preparation method of a dendroid barium tungstate nano crystal is characterized in that comprising the steps:
1) preparation barium ion microemulsion: in Erlenmeyer flask, add octane, propyl carbinol, cetyl trimethylammonium bromide successively, add the barium salt aqueous solution under the magnetic agitation, stirred 30 minutes, form the barium ion microemulsion of homogeneous phase transparent; Wherein the concentration of cetyl trimethylammonium bromide is 0.15～0.25moll
-1, the mol ratio of propyl carbinol and cetyl trimethylammonium bromide is 3.47～4.52, and the mole number of water is 30～40 with the ratio of cetyl trimethylammonium bromide mole number in the barium salt aqueous solution, and all the other are octane; Barium salt concentration of aqueous solution 0.1～0.2moll
-1
2) preparation tungstate ion microemulsion: according to step 1), substitute the barium salt aqueous solution with same concentrations and isopyknic sodium wolframate aqueous solution, all the other compositions are identical with barium ion microemulsion composition, obtain the tungstate ion microemulsion;
3) synthetic dendroid barium tungstate nano crystal: the barium ion microemulsion and the tungstate ion microemulsion of above-mentioned acquisition are mixed rapidly in 20～35 ℃ of scopes, continue to stir 1 minute, reaction finishes; Centrifugation, with deionized water and absolute ethanol washing, 60 ℃ of vacuum dryings 6 hours promptly obtain to have the barium tungstate nanometer crystal of dendritic structure.
2. according to the preparation method of the dendroid barium tungstate nano crystal of claim 1, it is characterized in that described barium salt is bariumchloride or nitrate of baryta.
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| CN101805022B (en) * | 2010-04-28 | 2011-11-16 | 燕山大学 | Method for preparing barium tungstate nanometer double-line arrays by using DNA as templates |
| CN102557140B (en) * | 2012-03-02 | 2013-08-28 | 河北联合大学 | Preparation method of porous fusiform barium tungstate |
| CN104591288B (en) * | 2015-01-19 | 2016-06-08 | 洛阳理工学院 | A kind of preparation method of barium tungstate nanometer line |
| CN109761278B (en) * | 2019-02-15 | 2021-10-19 | 山东师范大学 | Method for synthesizing barium chromate nano material by taking surfactant-free microemulsion as template |
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Non-Patent Citations (4)
| Title |
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| 不同形状的钨酸钡纳米粒子的合成. 周萍等.应用化学，第23卷第4期. 2006 |
| 不同形状的钨酸钡纳米粒子的合成. 周萍等.应用化学，第23卷第4期. 2006 * |
| 混合碱土金属钨酸盐的合成及其溶混性. 杨水金.黄淮学刊，第10卷第2期. 1994 |
| 混合碱土金属钨酸盐的合成及其溶混性. 杨水金.黄淮学刊，第10卷第2期. 1994 * |
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