CN102583548B - Preparation method of nanometer flower-shaped magnesium tungstate materials assembled by ultrathin nanometer sheets - Google Patents
Preparation method of nanometer flower-shaped magnesium tungstate materials assembled by ultrathin nanometer sheets Download PDFInfo
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- CN102583548B CN102583548B CN201210052231.8A CN201210052231A CN102583548B CN 102583548 B CN102583548 B CN 102583548B CN 201210052231 A CN201210052231 A CN 201210052231A CN 102583548 B CN102583548 B CN 102583548B
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Abstract
The invention relates to a preparation method of nanometer flower-shaped magnesium tungstate materials assembled by ultrathin nanometer sheets. Sodium tungstate and magnesium nitrate are used as reaction raw materials, distilled water is used as a solvent, and a microwave radiation method is adopted for controllably preparing the magnesium tungstate materials. The obtained magnesium tungstate nanometer flower is a hollow structure material orderly assembled by a large number of ultrathin nanometer sheets with smooth surfaces in the specific direction, wherein the thickness of the nanometer sheets is 10 to 20 nanometers, the diameter is 0.3 to 0.6 microns, and the diameter of the combined nanometer flower is 9 to 12 microns. According to the microwave reaction process, the materials can be prompted to be uniformly nucleated, in addition, the advantages of no temperature lag effect, excellent reaction kinetics and the like are realized, and necessary theoretical basis and practical experience are laid for the low-cost scale preparation and the integral performance improvement of magnesium tungstate function materials. The magnesium tungstate nanometer flower has the characteristics of novel structure, regular appearance, high crystallinity and the like, and the application value of the magnesium tungstate nanometer flower in the fields of photoelectricity, medical treatment, catalysis and the like is expected to be obviously improved.
Description
[technical field]: the invention belongs to inorganic micro-nano functional materials preparation field, especially relate to a kind of preparation method of nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling.
[background technology]: metal tungstates is the important inorganic functional material of a class, it has unique and stable crystalline structure, therefore can be widely used in the important technology fields such as photoluminescence, medical environmental protection, high energy physics scintillation material and photochemical catalysis.In recent years, by body phase metal tungstates material micro-nano rice, and then fully promote such material macroscopic view over-all properties and become study hotspot and the emphasis in tungstate material field.
At present, with regard to the preparation of material, the conventional synthetic method of metal tungstates micro Nano material mainly contains the (Q.Zhang such as molten-salt growth method, hydrothermal method, microemulsion method, W.T.Yao, X.Y.Chen, L.W.Zhu, Y.B.Fu, G.B.Zhang, L.S.Sheng, S.H.Yu, Cryst.Growth Des., 2007,7,1423-1431; J.Lin, J.Lin, Y.F.Zhu, Inorg.Chem., 2007,46,8372-8378.).But existing document is less to the preparation report of magnesium wolframate nano material, particularly adopt the efficient controlled preparation of microwave irradiation have novel pattern magnesium wolframate nano material document still less, and the problem in science such as partial synthesis method exists growth structure guidance difficulties, operational condition harshness, complex process, product rate is on the low side, this has restricted systematic study and the widespread use of this type of material to a great extent.The technical problem existing for the controlled preparation of above-mentioned magnesium wolframate micro Nano material aspect, patent of the present invention aims to provide a kind of preparation method of nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling, the hollow magnesium wolframate nano flower material that the ultrathin nanometer sheet that adopts microwave irradiation successfully to synthesize thickness homogeneous assembles.Compared with the conventional preparation method of the synthetic route that patent of the present invention provides and existing tungstate material, have microtexture selectivity strong, without Temperature Hysteresis Effect, reaction kinetics excellence, nucleus nucleation evenly and without advantages such as other additives, this technological line is the preparation of magnesium wolframate micro Nano material low-coat scale and promotes integrated application performance and established necessary theoretical basis and practical experience.
[summary of the invention]: the content of patent of the present invention is to provide a kind of preparation method of nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling, its feature is that microwave irradiation has that microtexture selectivity is strong, material nucleus nucleation is even, reaction process is simple and without advantages such as extra supplementary additives; Prepared hollow structure magnesium wolframate nano flower is to be formed by specific direction ordered fabrication by the ultrathin nanometer sheet of a large amount of thickness homogeneous, have that novel structure, pattern are regular, degree of crystallinity advantages of higher, be expected to significantly promote its using value in fields such as photoelectricity, medical treatment and catalysis.
[technical scheme of the present invention]: patent of the present invention relates to a kind of preparation method of nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling, this synthetic route is taking sodium wolframate and magnesium nitrate as reaction raw materials, taking distilled water as solvent, adopt the controlled preparation hollow structure of microwave irradiation magnesium wolframate nano flower material, comprise the following steps:
The first, at room temperature, by 0.3299 gram of sodium wolframate (NaWO
42H
2o) solid is dissolved in 10 ml distilled waters, preparation sodium tungstate solution;
The second, by 0.2564 gram of magnesium nitrate (Mg (NO
3)
26H
2o) crystal is fully dissolved in 10 ml distilled waters, preparation magnesium nitrate solution;
Three, step 1 solution is transferred in step 2, and violent stirring 5 minutes;
Four, the mixing solutions obtaining in the 3rd step is slowly poured in reaction vessel, and be placed in microwave radiation reactor continuous heating 25～35 minutes;
Five, question response completes, and the suspension liquid obtaining is naturally cooled to centrifugation after room temperature, and use respectively distilled water, washing with alcohol 3～4 times, is at 70 DEG C freeze-day with constant temperature 24 hours, can obtain the nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling.
Described magnesium wolframate nano material shows that through X-ray diffraction analysis the thing of products therefrom is MgWO mutually
4, its hollow Nano flower for being assembled by specific direction by the smooth nanometer sheet of exhibiting high surface, it has good dispersity, compound with regular structure, the equal first-class feature of diameter, and wherein the thickness of nanometer sheet is that 10～20 nanometers, diameter are 0.3～0.6 micron; After combination, micro-flowers diameter is 1～3 micron.
[advantage of the present invention and effect]: patent of the present invention discloses a kind of preparation method of nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling, tool has the following advantages and beneficial effect: 1, without the magnesium wolframate hollow structure nano flower material that adds other structural promoters and can prepare pattern excellence in reaction system, it has, and good dispersity, degree of crystallinity are high, structured size, the equal first-class feature of diameter; 2, microwave reaction process can be impelled material homogeneous nucleation and have without advantages such as Temperature Hysteresis Effect, reaction kinetics excellences; 3, this technological line is that the preparation of magnesium wolframate function nano material low cost scale and lifting over-all properties have been established necessary theoretical basis and practical experience
[brief description of the drawings]:
Fig. 1 is the X-ray diffraction analysis figure of synthetic sample
Fig. 2 is low power scanning electronic microscope (SEM) figure of the nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling
Fig. 3 is the magnification at high multiple SEM figure of the nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling
[embodiment]:
Embodiment: preparation method and the structural characterization of the nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling
At room temperature, first by 0.3299 gram of sodium wolframate (NaWO
42H
2o) solid is dissolved in 10 ml distilled waters and configures sodium tungstate solution, secondly by 0.2564 gram of magnesium nitrate (Mg (NO
3)
26H
2o) crystal is fully dissolved in 10 ml distilled waters, preparation magnesium nitrate solution; Above-mentioned two kinds of solution are mixed and violent stirring was slowly poured in round-bottomed flask after 5 minutes, and be placed in microwave radiation reactor and heat 30 minutes; After question response completes, the suspension liquid obtaining is naturally cooled to room temperature, then centrifugation, and use respectively distilled water and washing with alcohol 4 times, then at 70 DEG C freeze-day with constant temperature 24 hours, can obtain the hollow Nano flower magnesium wolframate material of ultrathin nanometer sheet assembling.Show that through X-ray diffraction analysis the thing of products therefrom is MgWO mutually
4, corresponding standard card number: 45-412 (as Fig. 1).From low power SEM figure (as Fig. 2), as, the hollow structure nano flower that product is favorable dispersity, single micro-flowers diameter is 1～3 micron; Can further analyze knownly by high magnification SEM image (as Fig. 3), nano flower is that ultrathin nanometer sheet that exhibiting high surface is smooth forms by specific direction ordered fabrication, and wherein nanometer sheet thickness is that 10～20 nanometers, diameter are 0.3～0.6 micron.
Claims (1)
1. a preparation method for the nano flower-like magnesium wolframate material of ultrathin nanometer sheet assembling, is characterized in that: at room temperature, and first by 0.3299 gram of sodium wolframate Na
2wO
42H
2o solid is dissolved in 10 ml distilled waters and configures sodium tungstate solution, secondly by 0.2564 gram of magnesium nitrate Mg (NO
3)
26H
2o crystal is fully dissolved in 10 ml distilled waters, preparation magnesium nitrate solution; Above-mentioned two kinds of solution are mixed and violent stirring was slowly poured in round-bottomed flask after 5 minutes, and be placed in microwave radiation reactor and heat 30 minutes; After question response completes, the suspension liquid obtaining is naturally cooled to room temperature, then centrifugation, and use respectively distilled water and washing with alcohol 4 times, then at 70 DEG C freeze-day with constant temperature 24 hours, can obtain the hollow Nano flower magnesium wolframate material of ultrathin nanometer sheet assembling; Show that through X-ray diffraction analysis the thing of products therefrom is MgWO mutually
4, corresponding standard card number: 45-412; From low power SEM figure, the hollow structure nano flower that product is favorable dispersity, single micro-flowers diameter is 1～3 micron; Can further analyze knownly by high magnification SEM image, nano flower is that ultrathin nanometer sheet that exhibiting high surface is smooth forms by specific direction ordered fabrication, and wherein nanometer sheet thickness is that 10～20 nanometers, diameter are 0.3～0.6 micron.
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| CN102583548B true CN102583548B (en) | 2014-08-27 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4419575C1 (en) * | 1994-06-03 | 1995-10-19 | Starck H C Gmbh Co Kg | Metal tungstate for prodn. of lead perovskite electro-ceramics and X=ray improving luminescent materials |
| CN101062786A (en) * | 2007-05-08 | 2007-10-31 | 河北理工大学 | Production method of Ag2WO4 composite antibacterial agent by microwave heating process and application in sanitary ceramic glaze |
| CN102225784A (en) * | 2011-03-29 | 2011-10-26 | 河北联合大学 | Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation |
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2012
- 2012-03-02 CN CN201210052231.8A patent/CN102583548B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4419575C1 (en) * | 1994-06-03 | 1995-10-19 | Starck H C Gmbh Co Kg | Metal tungstate for prodn. of lead perovskite electro-ceramics and X=ray improving luminescent materials |
| CN101062786A (en) * | 2007-05-08 | 2007-10-31 | 河北理工大学 | Production method of Ag2WO4 composite antibacterial agent by microwave heating process and application in sanitary ceramic glaze |
| CN102225784A (en) * | 2011-03-29 | 2011-10-26 | 河北联合大学 | Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation |
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Inventor after: Sun Yan Inventor after: Rong Tao Inventor after: Li Chunsheng Inventor after: Ma Xuegang Inventor after: Song Dawei Inventor after: Shi Jifu Inventor after: Zhang Shaoyan Inventor after: Wang Lina Inventor after: Hu Yiwen Inventor after: Sun Bowei Inventor before: Sun Yan Inventor before: Li Chunsheng Inventor before: Wang Yaozu Inventor before: Ma Xuegang Inventor before: Wang Lina |
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Free format text: CORRECT: INVENTOR; FROM: SUN YAN LI CHUNSHENG WANG YAOZU MA XUEGANG WANG LINA TO: SUN YAN LI CHUNSHENG MA XUEGANG SONG DAWEI SHI JIFU ZHANG SHAOYAN WANG LINA HU YIWEN SUN BOWEI RONG TAO |
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