CN101214990A - Normal temperature synthesis method for nanometer zinc oxide - Google Patents
Normal temperature synthesis method for nanometer zinc oxide Download PDFInfo
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- CN101214990A CN101214990A CNA2007101736239A CN200710173623A CN101214990A CN 101214990 A CN101214990 A CN 101214990A CN A2007101736239 A CNA2007101736239 A CN A2007101736239A CN 200710173623 A CN200710173623 A CN 200710173623A CN 101214990 A CN101214990 A CN 101214990A
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Abstract
The invention relates to a method for synthesizing nanometer zinc oxide in normal temperature, belonging to the technical field of nanometer material. The invention chooses organic zinc salt and inorganic base or organic base as raw materials, add organic zinc salt into deionized water, after being stirred and dissolved, slowly add inorganic base or organic base, when white precipitate is generated, continue to stir for 1-10 hours, after centrifugal separation, use deionized water and absolute ethyl alcohol to wash precipitate, after being dried in a drying oven, the product is produced. The invention has the advantages of low price of material, simple process, convenient operation, lowed consumption, easy control and the like.
Description
Technical field
The present invention relates to a kind of normal temperature synthesis method of nano zine oxide, belong to field of nanometer material technology.
Background technology
Zinc oxide is countries nowadays high-tech research and one of most important optoelectronic semiconductor material in exploitation field, forward position.Countries in the world, scientist particularly beautiful, Japan and Korea S. three states has dropped into a large amount of research in succession with great enthusiasm.Nano zinc oxide material have its body bulk material incomparable excellent properties, as nontoxic and non-migrating, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc., have a wide range of applications aspect numerous at ceramic, ultraviolet shielded, weaving, rubber, catalyzer and photocatalyst, transmitter and absorbing material, window of tube and electrical condenser, image recording material etc., favored by people, become the focus that scientific and technical personnel pay close attention to.The performance of material depends on grain-size, distribution and the pattern of composition material, thereby the controlled nanometer Zinc oxide powder of synthesis of high purity, particle diameter and pattern is the first step of preparation high-performance nano material.
The preparation method of existing nano zinc oxide material is a lot, can reduce solid phase method, liquid phase method and vapor phase process.Wherein liquid phase method has comprised direct precipitation method, sluggish precipitation, sol-gel method etc.; Vapor phase process comprises chemical decomposition method and spray pyrolysis etc.Preparation method's difference, the size and the pattern that obtain crystal grain have nothing in common with each other.Prepared at present nano zinc oxide material, comprised nanoparticle (D.Qian, J.Z.Jiang from zero dimension to three-dimensional different-shape, P.L.Hansen, Chem.Commun. (2003) 1078), nanometer rod (B.Cheng, E.T.Samulski, Chem.Commun. (2004) 986)), nano belt (J.H.Park, H.J.Choi, Y.J.Choi, S.H.Sohn, et al J.Mater.Chem.14 (2004) 3955) and other complicated patterns.But prior preparation method, the carrying out that all needs (as heating, microwave-assisted, supersound process etc.) promotion reaction under certain conditions, cause the energy consumption in the building-up process to rise, raise the cost, therefore seeking cheaply effectively, the method for controlled oxidation zinc pattern has important practical significance.
Summary of the invention
The object of the present invention is to provide a kind of normal temperature synthesis method of nano zine oxide.
To achieve these goals, the present invention realizes by following steps:
(1) preparation of raw material:
Selecting organic zinc salt and mineral alkali or organic bases for use is raw material.
The preferred zinc acetate of described organic zinc salt;
Described mineral alkali or organic bases are sodium hydroxide or potassium hydroxide or triethylamine, preferred triethylamine.
(2) organic zinc salt is added in the deionized water, after the stirring and dissolving, slowly add mineral alkali or organic bases, generate white precipitate, continue to stir 1～10 hour.
The concentration of organic zinc salt is 0.01～0.08mol/L, adds mineral alkali or organic bases 0.01～0.5mol in every liter of organic zinc salt solution;
(3) after the centrifugation,, in baking oven, dry, make product with deionized water and absolute ethanol washing precipitation.
The pattern of the zinc oxide nano-particle that the present invention is prepared is along with the difference of selected alkali has very big difference.Obtain the zinc-oxide nano polycrystalline of pin bunch shape during for precipitation agent with sodium hydroxide, its particle diameter is at 100～200nm (seeing Fig. 2 A); When being precipitation agent, obtain equally distributed bar-shaped zinc oxide with potassium hydroxide, the about 200nm of diameter, length is 600nm (seeing Fig. 2 B); And when being precipitation agent with the triethylamine, what obtain is a kind of Zinc oxide single crystal of triangular shape, and particle diameter is at 100～150nm (seeing Fig. 2 C and D).When being precipitation agent with the triethylamine, the particle size of zinc oxide is decreased to below the 50nm with the reduction of zinc salt concentration in the reaction soln.The triangular shape oxidized zinc products of this 50nm can form stable dispersion liquid in ethanol.Obvious sedimentation can not take place through the placement more than month in this dispersion liquid yet.
The inventive method is simple, and energy consumption is low, and is easy to operate, and the raw material of selecting for use is easy to get.In addition, the room temperature preparation method also can enlarge the Technological adaptability of nano zine oxide under different application field and application conditions, helps the raising of material property.
Description of drawings
Fig. 1 is preparation technology's schema of the present invention.
Fig. 2 is the SEM photo of the present invention according to the product of embodiment 1, example 2, example 3.That insert among Fig. 2 a and Fig. 2 c is selected area electron diffraction figure.
Embodiment
Embodiment 1
Accurate weighing 0.440g (2mmol) two hydration zinc acetates, stirring and dissolving accurately takes by weighing 0.352g sodium hydroxide (8.5mmol) again under the room temperature in the 50ml deionized water, slowly adds in the above-mentioned solution, continues to stir 2h under the room temperature.Reaction soln carries out centrifugation, and precipitation spends ionized water and absolute ethanol washing respectively, and dry under 60 ℃, obtains white powder.Product is the zinc-oxide nano polycrystalline of pin bunch shape, and diameter is at 100～200nm, and its SEM photo and selected area electron diffraction figure list among Fig. 2 a.
Embodiment 2
Accurate weighing 0.440g (2mmol) two hydration zinc acetates, stirring and dissolving adds 0.476g potassium hydroxide (8.5mmol) under the room temperature in the 50ml deionized water, continues to stir 2h under the room temperature.Reaction soln carries out centrifugation, and precipitation spends ionized water respectively and dehydrated alcohol washs, and is dry down at 60 ℃ then.Fig. 2 b is the TEM photo of product.Photo shows that product is equally distributed bar-shaped zinc-oxide nano crystal grain, and particle diameter is 200nm, and length is 600nm.
Embodiment 3
Accurate weighing 0.440g (2mmol) two hydration zinc acetates, stirring and dissolving adds the 2.5ml triethylamine under the room temperature in the 50ml deionized water, continues to stir 8h under the room temperature.Reaction soln carries out centrifugation, and precipitation spends ionized water respectively and dehydrated alcohol washs, and is dry down at 60 ℃ then.To find out, product is the zinc-oxide nano monocrystalline of triangular shape from Fig. 2 c, d, and size is between 100～150nm.
Claims (5)
1. the normal temperature synthesis method of a nano zine oxide comprises the steps:
(1) selecting organic zinc salt and mineral alkali or organic bases for use is raw material;
(2) organic zinc salt is added in the deionized water, after the stirring and dissolving, slowly add mineral alkali or organic bases, generate white precipitate, continue to stir 1～10 hour;
(3) after the centrifugation,, in baking oven, dry, make product with deionized water and absolute ethanol washing precipitation.
2. by the normal temperature synthesis method of the described a kind of nano zine oxide of claim 1, it is characterized in that described organic zinc salt is a zinc acetate.
3. by the normal temperature synthesis method of the described a kind of nano zine oxide of claim 1, it is characterized in that described mineral alkali or organic bases are sodium hydroxide or potassium hydroxide or triethylamine
4. by the normal temperature synthesis method of the described a kind of nano zine oxide of claim 3, it is characterized in that described mineral alkali or organic bases are triethylamine.
5. by the normal temperature synthesis method of the described a kind of nano zine oxide of claim 1, the concentration that it is characterized in that described organic zinc salt is 0.01～0.08mol/L, adds mineral alkali or organic bases 0.01～0.5mol in every liter of organic zinc salt solution;
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| CN2007101736239A CN101214990B (en) | 2007-12-28 | 2007-12-28 | Normal temperature synthesis method for nanometer zinc oxide |
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| CN2007101736239A CN101214990B (en) | 2007-12-28 | 2007-12-28 | Normal temperature synthesis method for nanometer zinc oxide |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275977A (en) * | 2011-07-19 | 2011-12-14 | 西安交通大学 | Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio |
| CN102608170A (en) * | 2011-10-08 | 2012-07-25 | 北京中科微纳物联网技术股份有限公司 | High-performance gas sensor |
| CN102849780A (en) * | 2012-09-11 | 2013-01-02 | 南京工业大学 | Method for synthesizing ZnO nano-structure by using organic weak base |
| CN103771490A (en) * | 2014-01-04 | 2014-05-07 | 东华理工大学 | Simple method for preparing micrometer/nanometer zinc oxide by stirring at room temperature |
| CN107441778A (en) * | 2017-09-08 | 2017-12-08 | 宣城市聚源精细化工有限公司 | One kind defoams rapid defoamer |
| CN108570850A (en) * | 2018-02-15 | 2018-09-25 | 湖北大学 | A kind of preparation method of the excellent super wetting woven fabric of stabilization patience for water-oil separating |
| CN110903582A (en) * | 2019-11-27 | 2020-03-24 | 桂林理工大学 | Polyvinyl alcohol/starch nano composite material with ultraviolet blocking function and preparation method thereof |
| CN111514937A (en) * | 2020-05-13 | 2020-08-11 | 中国石油大学(华东) | Preparation method of porphyrin-based metal organic framework material sensitized oxide catalyst |
| CN116282127A (en) * | 2023-02-28 | 2023-06-23 | 安徽工程大学 | Balsam pear type nano zinc oxide and preparation method and application thereof |
-
2007
- 2007-12-28 CN CN2007101736239A patent/CN101214990B/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275977A (en) * | 2011-07-19 | 2011-12-14 | 西安交通大学 | Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio |
| CN102275977B (en) * | 2011-07-19 | 2013-01-02 | 西安交通大学 | Preparation method of zinc oxide mesoscopic crystal with adjustable aspect ratio |
| CN102608170A (en) * | 2011-10-08 | 2012-07-25 | 北京中科微纳物联网技术股份有限公司 | High-performance gas sensor |
| CN102849780A (en) * | 2012-09-11 | 2013-01-02 | 南京工业大学 | Method for synthesizing ZnO nano-structure by using organic weak base |
| CN103771490A (en) * | 2014-01-04 | 2014-05-07 | 东华理工大学 | Simple method for preparing micrometer/nanometer zinc oxide by stirring at room temperature |
| 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 |
| CN107441778A (en) * | 2017-09-08 | 2017-12-08 | 宣城市聚源精细化工有限公司 | One kind defoams rapid defoamer |
| CN108570850A (en) * | 2018-02-15 | 2018-09-25 | 湖北大学 | A kind of preparation method of the excellent super wetting woven fabric of stabilization patience for water-oil separating |
| CN108570850B (en) * | 2018-02-15 | 2021-03-02 | 湖北大学 | Preparation method of super-wetting woven fabric with excellent stability and tolerance for oil-water separation |
| CN110903582A (en) * | 2019-11-27 | 2020-03-24 | 桂林理工大学 | Polyvinyl alcohol/starch nano composite material with ultraviolet blocking function and preparation method thereof |
| CN111514937A (en) * | 2020-05-13 | 2020-08-11 | 中国石油大学(华东) | Preparation method of porphyrin-based metal organic framework material sensitized oxide catalyst |
| CN116282127A (en) * | 2023-02-28 | 2023-06-23 | 安徽工程大学 | Balsam pear type nano zinc oxide and preparation method and application thereof |
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| CN101214990B (en) | 2010-10-20 |
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