CN101214990B - Normal temperature synthesis method for nanometer zinc oxide - Google Patents
Normal temperature synthesis method for nanometer zinc oxide Download PDFInfo
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- CN101214990B CN101214990B CN2007101736239A CN200710173623A CN101214990B CN 101214990 B CN101214990 B CN 101214990B CN 2007101736239 A CN2007101736239 A CN 2007101736239A CN 200710173623 A CN200710173623 A CN 200710173623A CN 101214990 B CN101214990 B CN 101214990B
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- Prior art keywords
- zinc oxide
- nano
- normal temperature
- deionized water
- zinc
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 16
- 238000001308 synthesis method Methods 0.000 title claims description 5
- 238000003756 stirring Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 24
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004246 zinc acetate Substances 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims 1
- 238000010189 synthetic method Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 150000003751 zinc Chemical class 0.000 abstract description 8
- 150000007530 organic bases Chemical class 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 150000007529 inorganic bases Chemical class 0.000 abstract 2
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 229960001296 zinc oxide Drugs 0.000 description 12
- 238000001556 precipitation Methods 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 239000003513 alkali Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 description 4
- 239000011707 mineral Substances 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 235000013904 zinc acetate Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000036571 hydration Effects 0.000 description 3
- 238000006703 hydration reaction Methods 0.000 description 3
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 229960000935 dehydrated alcohol Drugs 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000004098 selected area electron diffraction Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 229940024464 emollients and protectives zinc product Drugs 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000001478 photoelectron diffraction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005118 spray pyrolysis Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种纳米氧化锌的常温合成方法，属于属于纳米材料领域。本发明选用有机锌盐和无机碱或有机碱为原料，将有机锌盐加入去离子水中，搅拌溶解后，缓慢加入无机碱或有机碱，生成白色沉淀，继续搅拌1～10小时，离心分离后，用去离子水和无水乙醇洗涤沉淀，在烘箱中烘干，制得产品。本发明原料价便、工艺简单、操作方便、降低能耗，易于控制等特点。The invention relates to a method for synthesizing nano-zinc oxide at normal temperature, belonging to the field of nano-materials. The present invention selects organic zinc salt and inorganic base or organic base as raw materials, adds organic zinc salt into deionized water, after stirring and dissolving, slowly adds inorganic base or organic base to form white precipitate, continues to stir for 1 to 10 hours, and centrifuges , wash the precipitate with deionized water and absolute ethanol, and dry in an oven to obtain the product. The invention has the characteristics of cheap raw materials, simple process, convenient operation, reduced energy 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 (2)
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| CN101214990A CN101214990A (en) | 2008-07-09 |
| CN101214990B true CN101214990B (en) | 2010-10-20 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 nanostructure by using organic weak base |
| 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 |
| 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 |
| CN110903582B (en) * | 2019-11-27 | 2022-12-23 | 深圳市聚亿新材料科技股份有限公司 | Polyvinyl alcohol/starch nano composite material with ultraviolet blocking function and preparation method thereof |
| CN111514937B (en) * | 2020-05-13 | 2023-04-18 | 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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