CN101407333A - Method for synthesizing flower-like nanostructure composed of zinc oxide nano-rod - Google Patents
Method for synthesizing flower-like nanostructure composed of zinc oxide nano-rod Download PDFInfo
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- CN101407333A CN101407333A CNA2007101625522A CN200710162552A CN101407333A CN 101407333 A CN101407333 A CN 101407333A CN A2007101625522 A CNA2007101625522 A CN A2007101625522A CN 200710162552 A CN200710162552 A CN 200710162552A CN 101407333 A CN101407333 A CN 101407333A
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Abstract
The invention discloses a method for synthesizing a flower-shaped nanometer structure consisting of zinc oxide nanometer rods, which belongs to the field of inorganic non-metal materials, and comprises the steps: soluble zinc salt such as zinc acetate is dissolved in water and added with an appropriate amount of paranitrobenzoic acid or ethyl naphthol to be taken as an auxiliary agent, NaOH solution is used for regulating the pH value to be 12-14, and precipitate and the solution are heated in a high-pressure autoclave for the growth of the nanometer zinc oxide. The heating mode can be microwave heating or resistance wire heating, and the outgrown nanometer structure is the flower-shaped nanometer structure consisting of the nanometer rods. The method has the advantages of simple technology and low cost, and uses the paranitrobenzoic acid or ethyl naphthol as the auxiliary agent for controlling the appearance and the size of zinc oxide crystal.
Description
Technical field
The present invention relates to the preparation method of the flower-like nanostructure of zinc oxide nano rod composition, belong to field of inorganic nonmetallic material.
Background technology
ZnO is a kind of novel direct wide bandgap semiconductor materials of II-VI family, have very high conduction, heat conductivility and chemical stability and good uv absorption property, be widely used in aspects such as rubber, pottery, daily-use chemical industry, coating, can be used for making gas sensor, UV-preventing material, transformer and multiple Optical devices.Energy gap is 3.37eV under its room temperature, and corresponding ultraviolet light wavelength is expected to realize visible, Ultraluminescence and Laser emission, and then exploitation short-wave long light-emitting diode and laser apparatus.Since the optical pumping light emission that at room temperature observes microcrystalline film (having nanostructure), ZnO becomes the international focus of shortwave semiconductor laser material rapidly.Nano-ZnO is because its dimensional effect and the significant in a lot of fields and tempting prospect of quantum confined effect.Simultaneously, nano-ZnO shows very strong interfacial effect, makes it than body material and other metal oxide materials higher specific conductivity, the transparency and transmission rate etc. be arranged, thereby occupies critical role in the integrated and world of miniaturization of semiconductor photoelectric device.
Report about one-D nano zinc oxide has had a lot, comprises gas phase synthesis method, as metal-organic chemical vapour deposition method, thermal evaporation, molecular beam epitaxy etc.; Liquid phase method is as the growth method based on solution such as alumina formwork method, electrochemical deposition method, hydrothermal method.Though can synthesize controlled One-Dimensional ZnO nanostructure by precious metal catalyst and two kinds of gas phase transfer methods of high-temperature evaporation, reaction needed is carried out under the high temperature more than 1000 ℃, is difficult to scale operation.By contrast, liquid phase process is then simple and convenient, and is with low cost, has very big advantage, and wherein one of most important method is exactly a hydrothermal method.The method of hydrothermal method synthesizing zinc oxide nanometer rod needs template usually, and template commonly used has hexadecyl trimethyl ammonium bromide (CTAB), quadrol, polyoxyethylene glycol (PEG) etc.
The invention provides novel template, p-nitrobenzoic acid or ethyl naphthol are used for preparing the flower-like structure that zinc oxide nano rod is formed.
Summary of the invention
The invention provides a kind of synthetic method of flower-like structure of zinc oxide nano rod composition, the present invention adopts following technical scheme:
(1) the zinc acetate powder is soluble in water, in addition an amount of p-nitrobenzoic acid or ethyl naphthol template are added to the water, the two mol ratio is between 2.5: 1～10: 1, and they are mixed and stirring;
(2) the pH value with NaOH solution regulator solution is between the 12-14, supersound process 10 minutes;
(3) will precipitate and solution join in the stainless steel cauldron of inner liner polytetrafluoroethylene, in 120-180 ℃ of following constant temperature 12-24h;
(4) cooled and filtered or centrifuge washing obtain powder with absolute ethanol washing at last; Powder is obtained zinc oxide nano-powder in 60 ℃ of dryings.
Compare with existing additive method and technology, the present invention has following advantage:
(1) the present invention has adopted novel p-nitrobenzoic acid or ethyl naphthol template, has obtained the flower-like structure that rod-like nano-zinc oxide is formed;
(2) the flower-like nanometer zinc oxide that obtains of the present invention adopts hydro-thermal genealogy of law wet chemical method, the product size evenly, mean diameter is 80-100nm, does not have reunion substantially.
Description of drawings
Fig. 1: X-ray diffraction (XRD) collection of illustrative plates of preparation method's of the present invention flower-like nanometer zinc oxide;
Fig. 2: the projection electron microscope collection of illustrative plates (TEM) of preparation method's of the present invention flower-like nanometer zinc oxide;
Fig. 3: the scanning electron microscope diagram spectrum (SEM) of preparation method's of the present invention flower-like nanometer zinc oxide;
Can know the XRD collection of illustrative plates of product and zinc oxide standard spectrogram from the X diffracting spectrum of Fig. 1 (JCPDS#36-1451) in full accord, prove that the gained oxide powder is zinc oxide.
Can find out the diameter of resulting zinc oxide nano rod from the image of the projection electron microscope of Fig. 2 At 50-100nm, length is in hundreds of nanometers, and shape becomes the flower-shaped of unusual homogeneous.
Can find out that from the image of the SEM of Fig. 3 the diameter of zinc oxide nano rod exists 50-100nm, length is in hundreds of nanometers, and shape becomes the flower-shaped of unusual homogeneous.
Hence one can see that, by adding an amount of paranitrobenzoic acid or ethyl naphthol as auxiliary reagent, and can Under relatively mild condition, obtain the very flower shape zinc oxide nanostructured of homogeneous of shape.
Embodiment provided by the invention is as follows:
Following Example is to further specify of the present invention, rather than limits the scope of the invention.
Embodiment 1: 2 gram zinc acetates are soluble in water, in addition 0.5 gram ethyl naphthol is added to the water, with the two mixing and stirring.Dropwise drip the NaOH solution 30ml of 2M, supersound process 10 minutes.Precipitation and solution are joined in the stainless steel cauldron of inner liner polytetrafluoroethylene, in 120 ℃ of following constant temperature 12h.Cooled and filtered or centrifuge washing obtain powder with absolute ethanol washing at last; Powder is obtained zinc oxide nano-powder in 60 ℃ of dryings.
Embodiment 2: 2 gram zinc acetates are soluble in water, in addition 0.5 gram ethyl naphthol is added to the water, with the two mixing and stirring.Dropwise drip the NaOH solution 30ml of 2M, supersound process 10 minutes.Precipitation and solution are joined in the microwave reaction kettle of inner liner polytetrafluoroethylene, in 120 ℃ of following constant temperature 0.5h.Cooled and filtered or centrifuge washing obtain powder with absolute ethanol washing at last; Powder is obtained zinc oxide nano-powder in 60 ℃ of dryings.
Embodiment 3: change the ethyl naphthol of embodiment 1 into p-nitrobenzoic acid, all the other processes and consumption are with embodiment 1.
Embodiment 4: change the ethyl naphthol of embodiment 2 into p-nitrobenzoic acid, all the other processes and consumption are with embodiment 2.
Claims (2)
1. the flower-like structure that zinc oxide nano rod is formed is characterized in that utilizing soluble zinc salt and sodium hydroxide to be raw material, adds an amount of p-nitrobenzoic acid or ethyl naphthol as auxiliary reagent, makes precipitation.Through hydro-thermal reaction, can make excellent diameter 50-80nm, length is the flower shape zinc oxide nanostructure of hundreds of nanometers.It may further comprise the steps:
(1) the zinc acetate powder is soluble in water, in addition p-nitrobenzoic acid or ethyl naphthol are added to the water, the two mol ratio is between 2.5: 1～10: 1, and they are mixed and stirring;
(2) the pH value with NaOH solution regulator solution is between the 12-14, supersound process 10 minutes;
(3) will precipitate and solution join in the stainless steel cauldron of inner liner polytetrafluoroethylene, compactedness is 60-80%, in 120-180 ℃ of following constant temperature 12-24h;
(4) cooled and filtered or centrifuge washing obtain powder with absolute ethanol washing at last; Powder is obtained zinc oxide nano-powder in 60 ℃ of dryings.
2. the method for the flower-like structure that Hydrothermal Preparation zinc oxide nano rod according to claim 1 is formed is characterized in that having used in hydrothermal system p-nitrobenzoic acid or ethyl naphthol as auxiliary reagent.
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| CNA2007101625522A CN101407333A (en) | 2007-10-12 | 2007-10-12 | Method for synthesizing flower-like nanostructure composed of zinc oxide nano-rod |
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| CNA2007101625522A CN101407333A (en) | 2007-10-12 | 2007-10-12 | Method for synthesizing flower-like nanostructure composed of zinc oxide nano-rod |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811728A (en) * | 2010-04-27 | 2010-08-25 | 江苏大学 | Microwave method for synthesizing blossom ZnO hierarchical nanostructure |
| CN102260046A (en) * | 2010-05-28 | 2011-11-30 | 中国科学院大连化学物理研究所 | Microwave synthesis method of zinc oxide film with oriented nanorod structure |
| CN102730747A (en) * | 2012-07-16 | 2012-10-17 | 河南师范大学 | Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process |
| CN103288137A (en) * | 2012-02-27 | 2013-09-11 | 新疆教育学院 | Method for preparing molybdenum dioxide nanoparticles by microwave hydrothermal process |
| CN104445366A (en) * | 2014-11-10 | 2015-03-25 | 西北大学 | Method for synthesizing spindlelike ZnO nanomaterial by adopting microwave-assisted extraction process |
| CN104971709A (en) * | 2015-07-03 | 2015-10-14 | 陕西科技大学 | Ce-doped flower-shaped ZnO photocatalyst applicable to treatment of dye wastewater and preparation method thereof |
| CN108344793A (en) * | 2018-02-08 | 2018-07-31 | 亿纳谱（天津）医学检验中心有限公司 | A kind of matrix and preparation method thereof, the mass spectral analysis detection method of metabolic molecule |
| CN112538303A (en) * | 2020-12-10 | 2021-03-23 | 桐乡市创辉科技合伙企业(有限合伙) | Anti-aging zinc oxide modified acrylic resin wear-resistant coating and preparation method thereof |
| CN114196213A (en) * | 2021-12-31 | 2022-03-18 | 湖南柯盛新材料有限公司 | Multifunctional modified silicone rubber and preparation method thereof |
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2007
- 2007-10-12 CN CNA2007101625522A patent/CN101407333A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811728A (en) * | 2010-04-27 | 2010-08-25 | 江苏大学 | Microwave method for synthesizing blossom ZnO hierarchical nanostructure |
| CN101811728B (en) * | 2010-04-27 | 2012-08-15 | 江苏大学 | Microwave method for synthesizing blossom ZnO hierarchical nanostructure |
| CN102260046A (en) * | 2010-05-28 | 2011-11-30 | 中国科学院大连化学物理研究所 | Microwave synthesis method of zinc oxide film with oriented nanorod structure |
| CN103288137A (en) * | 2012-02-27 | 2013-09-11 | 新疆教育学院 | Method for preparing molybdenum dioxide nanoparticles by microwave hydrothermal process |
| CN102730747A (en) * | 2012-07-16 | 2012-10-17 | 河南师范大学 | Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process |
| CN102730747B (en) * | 2012-07-16 | 2014-03-26 | 河南师范大学 | Method for preparing zinc oxide with different microstructures by sol-gel assisted hydrothermal process |
| CN104445366A (en) * | 2014-11-10 | 2015-03-25 | 西北大学 | Method for synthesizing spindlelike ZnO nanomaterial by adopting microwave-assisted extraction process |
| CN104445366B (en) * | 2014-11-10 | 2016-05-04 | 西北大学 | The method of the synthetic spindle flower-like structure ZnO nano material of a kind of microwave abstracting |
| CN104971709A (en) * | 2015-07-03 | 2015-10-14 | 陕西科技大学 | Ce-doped flower-shaped ZnO photocatalyst applicable to treatment of dye wastewater and preparation method thereof |
| CN108344793A (en) * | 2018-02-08 | 2018-07-31 | 亿纳谱（天津）医学检验中心有限公司 | A kind of matrix and preparation method thereof, the mass spectral analysis detection method of metabolic molecule |
| CN108344793B (en) * | 2018-02-08 | 2023-08-25 | 浙江亿纳谱生命科技有限公司 | Matrix, preparation method thereof and mass spectrometry detection method of metabolic molecules |
| CN112538303A (en) * | 2020-12-10 | 2021-03-23 | 桐乡市创辉科技合伙企业(有限合伙) | Anti-aging zinc oxide modified acrylic resin wear-resistant coating and preparation method thereof |
| CN114196213A (en) * | 2021-12-31 | 2022-03-18 | 湖南柯盛新材料有限公司 | Multifunctional modified silicone rubber and preparation method thereof |
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