CN102936031B - Room temperature quick preparation method of nano-zinc oxide mesocrystal - Google Patents
Room temperature quick preparation method of nano-zinc oxide mesocrystal Download PDFInfo
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- CN102936031B CN102936031B CN201210462185.9A CN201210462185A CN102936031B CN 102936031 B CN102936031 B CN 102936031B CN 201210462185 A CN201210462185 A CN 201210462185A CN 102936031 B CN102936031 B CN 102936031B
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Abstract
The invention provides a preparation method of nano-zinc oxide mesocrystal. The method is characterized by mixing and stirring soluble zinc salt solution, alkali solution and ammonium fluoride solution according to a certain ratio to prepare mixed solution, enabling the mixed solution to react under room temperature for a plurality of minutes to obtain white precipitate, filtering and drying the white precipitate to obtain zinc oxide mesocrystal assembled by nanosheet, the thickness of the nanosheet is 19-22nm, and the diameter of the mesocrystal is 0.8-4mum. The preparation method has the advantages of being high in efficiency, low in cost, simple in process and suitable for industrial production. The obtained nano-zinc mesocrystal has large specific surface area, is capable of resolving the problem of agglomeration among particles, is suitable for preparation and application of materials and devices for air sensing, photocatalysis, antibiosis, sound wave and the like, and has wide application prospect.
Description
Technical field
The present invention relates to the preparation method of conductor oxidate nano material, be specifically related to the mesomorphic preparation method of a kind of zinc oxide micron/nano.
Background technology
Zinc oxide (ZnO) is a kind of novel I I-VI family semiconductor material with wide forbidden band, nontoxicity, and raw material is cheap and easy to get, has excellent photoelectricity, piezoelectricity and dielectric characteristics.Nano-ZnO can be widely used as gas sensitive, catalytic material, anti-biotic material and photoelectric material etc., therefore becomes in the world the popular research material in nanometer field nearly ten years; When nano-ZnO is used as air-sensitive, photocatalyst material, require it to there is large as far as possible specific surface area, to increase the contact area of ZnO and medium, thereby improve the sensitivity of gas sensor or strengthen photocatalysis effect.
Mesomorphic is that a kind of special crystalline material exists form, and it is by self-assembly, to form a larger micro-nano crystal by nanocrystal between polycrystalline and monocrystalline, and in macroscopic view, micro-nano crystal is arranged and is monocrystalline form because of the orderly extension of nanocrystal; On microcosmic, between micro-nano crystals nanocrystal, there is apparent interface or space, mesomorphic because its special structure and large specific surface area have an important using value industrial.
In Chinese patent (application number 201110160877.3), we have reported the mesomorphic water-bath preparation method of a kind of spherical zinc oxide of being assembled by nanometer sheet.The method relates to the low temperature water bath processing of 60 ℃ ~ 100 ℃, and the reaction times reach tens of hours, for overcoming above-mentioned preparation method's deficiency, we have invented the lower reaction times of room temperature is only the fast preparation method of several minutes.
Summary of the invention
The object of the present invention is to provide the mesomorphic room-temperature water bath preparation method of a kind of nano-ZnO, the method equipment is simple, productive rate efficiency is high, reproducible, be easy to suitability for industrialized production.
For achieving the above object, in technical scheme of the present invention, adopt room-temperature water bath legal system mesomorphic for nano-ZnO.
The above-mentioned mesomorphic preparation method of a kind of nano-ZnO, concrete steps are:
(1) preparation of mixing solutions: by a certain amount of zinc salt, alkali and NH
4f is dissolved in respectively distilled water, and above-mentioned solution is mixed, stirred, and makes mixed solution;
(2) room temperature reaction: by the mixed solution making lower stirring 1 ~ 10 minute;
(3) cleaning-drying: by the solution filter through room temperature reaction, cleaning and filtering thing, dry at 30 ℃ ~ 60 ℃ temperature.
In above-mentioned preparation method, in step 1, zinc salt is Zn (NO
3)
2, Zn (CH
3cOO)
2, ZnSO
4and ZnCl
2in a kind of; Alkali is a kind of in NaOH and KOH.
In above-mentioned preparation method, in step 1, the mol ratio of zinc salt and alkali is 0.1 ~ 0.375:1, NH
4the mol ratio of F and alkali is 0 ~ 0.5:1, and in mixed solution, the concentration of zinc salt is 0.1 ~ 0.3mol/L.
Compared with the prior art, the invention has the advantages that:
Under room temperature, react, solution, without heating, can reduce energy consumption to greatest extent; Reaction times significantly shortens, and only needs several minutes, is convenient to quick suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the mesomorphic scanning electron microscope diagram of nano-ZnO of embodiment 1 preparation;
Fig. 2 is the mesomorphic X-ray diffractogram of nano-ZnO of embodiment 1 preparation;
Fig. 3 is the mesomorphic scanning electron microscope diagram of nano-ZnO of embodiment 2 preparations;
Fig. 4 is the mesomorphic scanning electron microscope diagram of nano-ZnO of embodiment 3 preparations;
Fig. 5 is the mesomorphic scanning electron microscope diagram of nano-ZnO of embodiment 4 preparations;
Fig. 6 be the nano-ZnO of embodiment 4 preparation mesomorphic with the photocatalytic degradation of other photocatalysts to organic dye methylene blue.
Embodiment
The following examples are to further illustrate of the present invention, rather than limit the scope of the invention.
Embodiment 1:
1:0.375 takes NaOH, Zn (NO in molar ratio
3)
2be dissolved in respectively in distilled water; Above-mentioned solution is mixed, stirred, make mixed solution, Zn (NO in mixed solution
3)
2concentration be 0.1mol/L; The mixed solution making is reacted 10 minutes in stirring at room; By the solution filter through room temperature reaction, cleaning and filtering thing, it is dry at the temperature of 40 ℃ that can to obtain the ZnO being assembled by nanometer sheet mesomorphic, as shown in Figure 1, the thick 19-22 nm of nanometer sheet sheet, mesomorphic diameter 1 ~ 4 μ m, Fig. 2 is the X-ray diffractogram of this sample, and all diffraction peaks all can be characterized by ZnO.
Embodiment 2:
1:0.125:0.25 takes NaOH, ZnSO in molar ratio
4, NH
4f is dissolved in respectively in distilled water; Above-mentioned solution is mixed, stirred, make mixed solution, ZnSO in mixed solution
4concentration be 0.2mol/L; The mixed solution making is reacted 5 minutes in stirring at room; By the solution filter through room temperature reaction, cleaning and filtering thing, dry at the temperature of 50 ℃ can to obtain the ZnO being assembled by nanometer sheet mesomorphic, the thick 19-22 nm of sheet, mesomorphic diameter 0.8 ~ 1.2 μ m(Fig. 3).
Embodiment 3:
1:0.125:0.375 takes KOH, ZnCl in molar ratio
2, NH
4f is dissolved in respectively in distilled water; Above-mentioned solution is mixed, stirred, make mixed solution, ZnCl in mixed solution
2concentration be 0.3mol/L; The mixed solution making is reacted 1 minute in stirring at room; By the solution filter through room temperature reaction, cleaning and filtering thing, dry at the temperature of 40 ℃ can to obtain the ZnO being assembled by nanometer sheet mesomorphic, the thick 19-22 nm of sheet, mesomorphic diameter 0.8 ~ 1.2 μ m(Fig. 4).
Embodiment 4:
1:0.2:0.5 takes a certain amount of NaOH, Zn (CH in molar ratio
3cOO)
2, NH
4f is dissolved in respectively in distilled water; Above-mentioned solution is mixed, stirred, make mixed solution, Zn (CH in mixed solution
3cOO)
2concentration be 0.3mol/L; The mixed solution making is reacted 5 minutes in stirring at room; By the solution filter through room temperature reaction, cleaning and filtering thing, dry at the temperature of 60 ℃ can to obtain the ZnO being assembled by nanometer sheet mesomorphic, the thick 19-22 nm of sheet, mesomorphic diameter 0.8 ~ 1.2 μ m(Fig. 5).
The nano-ZnO of the present invention of usining is mesomorphic as photocatalyst for degrading organic dye methylene blue, and under uviolizing, it is obviously better than ZnO nano particle to the degradation rate of methylene blue, and is better than famous photocatalyst P25 TiO
2(Fig. 6).
Claims (4)
1. the mesomorphic preparation method of nano zine oxide, is characterized in that: by soluble Zn salts solution, alkaline solution and ammonium fluoride solution, mixed by a certain percentage, stirred, make mixed solution; Mixed solution is obtained to white precipitate through room temperature reaction; White precipitate filtration drying is obtained to the zinc oxide of being assembled by nanometer sheet mesomorphic; The mol ratio of described zinc salt and alkali is 0.1 ~ 0.375:1, NH
4the mol ratio of F and alkali is 0 ~ 0.5:1, and in mixed solution, the concentration of zinc salt is 0.1 ~ 0.3mol/L; Described reaction is at room temperature carried out, and the reaction times is 1 ~ 10 minute.
2. the mesomorphic preparation method of a kind of nano zine oxide as claimed in claim 1, is characterized in that: described zinc salt is Zn (NO
3)
2, Zn (CH
3cOO)
2, ZnSO
4and ZnCl
2in a kind of.
3. the mesomorphic preparation method of a kind of nano zine oxide as claimed in claim 1, is characterized in that: described alkali is a kind of in NaOH and KOH.
4. the mesomorphic preparation method of a kind of nano zine oxide as claimed in claim 1, is characterized in that: the thick 19-22nm of described nanometer sheet, mesomorphic diameter 0.8 ~ 4 μ m.
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| CN103586013B (en) * | 2013-11-13 | 2015-04-22 | 河北师范大学 | Method for preparing wheat-ear-shaped nano ZnO photocatalyst |
| CN103771490B (en) * | 2014-01-04 | 2015-08-19 | 东华理工大学 | A kind of simple and easy stirring at room temperature prepares the method for micro-/ nano zinc oxide |
| CN106243786B (en) * | 2016-07-29 | 2018-05-11 | 贵州大学 | A kind of preparation method of the fabric ultraviolet resistant of simple and efficient |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249286A (en) * | 2011-06-16 | 2011-11-23 | 江苏大学 | Method for preparing zinc oxide micron sphere |
| CN102557111A (en) * | 2012-03-01 | 2012-07-11 | 浙江工业大学 | Preparation method of snowflake-shaped ZnO |
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| CN102249286A (en) * | 2011-06-16 | 2011-11-23 | 江苏大学 | Method for preparing zinc oxide micron sphere |
| CN102557111A (en) * | 2012-03-01 | 2012-07-11 | 浙江工业大学 | Preparation method of snowflake-shaped ZnO |
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