CN1936116A - Method for preparing derdritical barium molybdate nano crystal - Google Patents
Method for preparing derdritical barium molybdate nano crystal Download PDFInfo
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- CN1936116A CN1936116A CN 200610116020 CN200610116020A CN1936116A CN 1936116 A CN1936116 A CN 1936116A CN 200610116020 CN200610116020 CN 200610116020 CN 200610116020 A CN200610116020 A CN 200610116020A CN 1936116 A CN1936116 A CN 1936116A
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Abstract
The invention relates to a manufacture method for branching barium molybdate nanometer crystal. It adopts micro-emulsion as medium to take manufacturing. The method includes the following steps: mixing equiponderant and same concentration barium salt solution, barium molybdate solution at a certain ratio with normal octane, normal butyl alcohol, and CTAB to make transparent micro-emulsion; rapidly mixing the two emulsions and whisking for 1min at a certain temperature range until reaction finishing, the branching barium molybdate nanometer crystal would be gained. The invention has the advantages of simple operation steps, low cost, rapid reaction speed. And the crystal is four branches structure and has equal size distribution.
Description
Technical field
The present invention relates to a kind of preparation method of derdritical barium molybdate nano crystal, in certain temperature range, adopting the microemulsion of reversed phase micelle is media, can obtain the dendrite of barium molybdate in the extremely short reaction times.Belong to the functional materials preparing technical field.
Background technology
Nano material has features such as unique nanocrystal and high density crystal boundary, produce peculiar mechanism such as surface effects, volume effect, quantum size effect and grain boundary effect thus, make performances such as its mechanics, magnetic, light, electricity, sound, heat and chemically reactive be better than traditional polycrystal and amorphous material.Therefore, nano material and manufacturing technology thereof are subjected to various countries and generally pay attention to, and become the research focus in the present material science.The barium molybdate 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 molybdate 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 derdritical barium molybdate nano crystal,, can obtain the dendroid nanocrystal that is evenly distributed fast by simple and cheaply technology.
For realizing this purpose, it is that media prepares the barium molybdate nano crystal that the present invention adopts microemulsion.At first respectively with barium salt aqueous solution equivalent, same concentrations and sodium molybdate 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 molybdate.
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 0.10～0.26moll
-1, the mol ratio of propyl carbinol and CTAB is 3.38～4.52, and the mole number of water is 30～42 with the ratio of CTAB mole number in the barium salt aqueous solution, and all the other are octane; Described barium salt concentration of aqueous solution 0.1～0.2 5moll
-1
2, the preparation of molybdenum acid ion microemulsion:
According to step 1, substitute the barium salt aqueous solution with same concentrations, isopyknic sodium molybdate aqueous solution, all the other compositions are identical with barium ion microemulsion composition, obtain the molybdenum acid ion microemulsion.
The said barium salt of the present invention is: bariumchloride, nitrate of baryta.
3, derdritical barium molybdate nano crystal is synthetic:
Barium ion microemulsion and molybdenum acid 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 molybdate nano crystal of dendritic structure.
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, and productive rate height, favorable repeatability can be used for producing in enormous quantities.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 four branched structures, and by a trunk, four rows form perpendicular to the short branch of trunk.
Description of drawings
Fig. 1 is the embodiment of the invention 1 a resulting dendroid barium molybdate crystalline x-ray diffraction pattern.(embodiment 1-2 has identical x-ray diffraction pattern).
Fig. 2 is the embodiment of the invention 1 resulting dendroid barium molybdate crystalline field emission scanning electron microscope photo and a transmission electron microscope photo.
Fig. 3 is the embodiment of the invention 2 resulting dendroid barium molybdate crystalline transmission electron microscope photos.
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
-1Sodium molybdate aqueous solution.Stirred 30 minutes, and formed the molybdenum acid ion microemulsion of homogeneous phase transparent.
3) the above-mentioned two kinds microemulsions that contain bariumchloride and Sodium orthomolybdate 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 derdritical barium molybdate nano crystal.
Resulting dendroid barium molybdate crystalline x-ray diffraction pattern such as Fig. 1.Prepared as seen from Figure 1 material is the tetragonal structure barium molybdate.Fig. 2 obtains dendroid barium molybdate crystalline field emission scanning electron microscope photo and transmission electron microscope photo.As seen from the figure, the long 4-10 μ of this dendritic structure trunk m, the long 300-600nm of branch.
Embodiment 2
1) in a 50ml Erlenmeyer flask, adds 12.91ml octane, 1.10ml propyl carbinol, 1.15g cetyl trimethylammonium bromide (CTAB) successively, add the 0.15moll of 1.84ml 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 12.91ml octane, 1.10ml propyl carbinol, 1.15g cetyl trimethylammonium bromide (CTAB) successively, add the 0.15moll of 1.84ml under the magnetic agitation
-1Sodium molybdate aqueous solution.Stirred 30 minutes, and formed the molybdenum acid ion microemulsion of homogeneous phase transparent.
3) the above-mentioned two kinds microemulsions that contain nitrate of baryta and Sodium orthomolybdate 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 dendroid barium molybdate crystal.
Fig. 3 is resulting dendroid barium molybdate crystal transmission electron microscope photo.As seen from the figure, the long 3-8 μ of this dendritic structure trunk m, the long 100-300nm of branch.
Claims (2)
1, a kind of preparation method of derdritical barium molybdate 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 0.10～0.26moll
-1, the mol ratio of propyl carbinol and cetyl trimethylammonium bromide is 3.38～4.52, and the mole number of water is 30～42 with the ratio of cetyl trimethylammonium bromide mole number in the barium salt aqueous solution, and all the other are octane; Described barium salt concentration of aqueous solution 0.1～0.25moll
-1
2) preparation molybdenum acid ion microemulsion: according to step 1), substitute the barium salt aqueous solution with same concentrations, isopyknic sodium molybdate aqueous solution, all the other compositions are identical with barium ion microemulsion composition, obtain the molybdenum acid ion microemulsion;
3) synthetic derdritical barium molybdate nano crystal: the barium ion microemulsion and the molybdenum acid ion microemulsion of above-mentioned acquisition are mixed rapidly in 20～35 ℃ of scopes, continue to stir 1 minute, obtain the oyster white mixed solution, centrifugation, with deionized water and absolute ethanol washing, 60 ℃ of vacuum dryings 6 hours promptly obtain to have the barium molybdate nano crystal of dendritic structure.
2, according to the preparation method of the derdritical barium molybdate nano crystal of claim 1, it is characterized in that described barium salt is bariumchloride or nitrate of baryta.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106915774A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
| CN109231270A (en) * | 2018-12-06 | 2019-01-18 | 洛阳理工学院 | A kind of preparation method of lead molybdate skeleton |
-
2006
- 2006-09-14 CN CN 200610116020 patent/CN1936116A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106915774A (en) * | 2017-05-04 | 2017-07-04 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
| CN106915774B (en) * | 2017-05-04 | 2018-05-22 | 洛阳理工学院 | A kind of preparation method of barium molybdate nano piece self assembly ball |
| CN109231270A (en) * | 2018-12-06 | 2019-01-18 | 洛阳理工学院 | A kind of preparation method of lead molybdate skeleton |
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