CN1562762A - Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption - Google Patents
Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption Download PDFInfo
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- CN1562762A CN1562762A CN 200410017850 CN200410017850A CN1562762A CN 1562762 A CN1562762 A CN 1562762A CN 200410017850 CN200410017850 CN 200410017850 CN 200410017850 A CN200410017850 A CN 200410017850A CN 1562762 A CN1562762 A CN 1562762A
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Abstract
At first, mixing zinc salt hexahydrated zinc nitrate and ammonia source hexamethylene tetramine according to mole density ratio 1:1.5 and dissolving them in carbinol solutio, then adding polytene pyrrolidone in certainly ratio, stirring till that solution is clear to produce grow reaction liquid of zinc oxide nanometre crystal, putting said reaction liquid into tetrafluoroethylene reactor, closing and increasing temp. to 95-100 deg.C to do reaction, then natural cooling, centrifuging washing, airing to obtain zinc oxide crystal that particle size is 15 nm.
Description
Technical field
The present invention relates to a kind of single nano-ZnO preparation of disperseing not have reunion and strong uv-absorbing, be specifically related to adopt the chemical solution method preparation to have the zinc oxide nano-crystal of single dispersion, nothing reunion, strong ultraviolet absorption characteristic, belong to the preparing technical field of inorganic nano material.
Background technology
Nano zine oxide is a kind of good semiconductor material, it has performances such as good luminous, opto-electronic conversion, uv-absorbing owing to having bigger energy gap width (similar with gan), be widely used in luminescent material, photoelectric conversion material, rubber, pottery, coating, daily-use chemical industry material, can be used for making gas sensitive, lighting electrode, rubber accelerator, gas sensor, UV-preventing material, transformer and multiple Optical devices.Calendar year 2001, reported on the authoritative impurity Science under the room temperature that nano zine oxide can produce to swash to penetrate phenomenon and cause people's extensive concern, make it become focus in the nano materials research field.Preparation method about nano zinc oxide material reports more in recent years, comprise gas phase synthesis method, for example chemical vapor deposition (CVD), magnetron sputtering method, spray pyrolysis, pulsed laser deposition (PLD), atomic-layer epitaxial growth method and molecular beam epitaxy etc., solution synthetic method comprises sol-gel method, hydrolysis method, hydrothermal method, antiphase emulsifiable method, the precipitator method and electrochemical deposition method.Under comparing, there are shortcomings such as temperature of reaction height, equipment complexity, cost height, efficient be low in the gas phase process.And solution synthetic method is simple and convenient, cost is low, efficient is high.But at present the solution methods that adopts prepares the shortcoming that nano zine oxide exists the inhomogeneous and easy reunion of particle diameter, and these shortcomings have very big influence to performances such as the light of nano zine oxide, electricity, thereby is difficult to satisfy the needs in scientific research and market.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, provide that a kind of particle diameter is even, nothing is reunited, simple to operate, the preparation method of the zinc oxide nano-crystal that temperature of reaction is low, cost is low, production efficiency is high.
For realizing such purpose, in the technical scheme of the present invention, adopt the auxiliary chemical solution method of polyvinylpyrrolidone to prepare the nano zine oxide crystal.Polyvinylpyrrolidone (PVP) is the important source material of day chemical industry.As a kind of novel high polymer tensio-active agent; it have good solvability, biocompatibility, hypotoxicity, film-forming properties and high-molecular surface active, colloid protective capability and with the compound ability of chemical compound lot, thereby become the good protective material of preparation nano material.In the technology of the present invention, at first zinc salt and ammonia source are dissolved in the methanol solution according to certain concentration and ratio respectively, add a certain proportion of PVP again, after the solution clarification, pour in the tetrafluoroethylene reactor, airtight, be warming up to 95-100 ℃, react and can obtain the nano zine oxide crystal in 3-4 hour.The nano zine oxide crystalline of preparation is of a size of the 13-17 nanometer, and particle diameter evenly and is not reunited, and has good ultraviolet absorption characteristic, places 1 year through room temperature, and prepared nano zine oxide is not still reunited.
Preparation method of the present invention comprises following concrete steps:
1. the preparation of reaction soln: zinc salt and ammonia source are dissolved in the methanol solution according to 1: 1.5 volumetric molar concentration ratio respectively, add certain density polyvinylpyrrolidone PVP again, are stirred to the solution clarification, can be prepared into reaction soln.
The said zinc salt of the present invention is a zinc nitrate hexahydrate; The ammonia source is that (HMT is commonly called as six methylene radical four ammonia: urotropine).
The ratio of said each raw material consumption of the present invention is: the ratio of zinc salt, ammonia source, polyvinylpyrrolidone, methanol usage is: 0.0005 mole: 0.00075 mole: 0.5 gram: 100 milliliters.
2. nano zine oxide is synthetic: the growth response solution of the above-mentioned zinc oxide nanocrystalline for preparing is poured in the tetrafluoroethylene reactor, airtight, be warming up to 95-100 ℃, reacted 3-4 hour, reaction naturally cools to normal temperature after finishing, centrifugation can obtain the nano zine oxide crystal through drying naturally after repeatedly washing.
Excellent results of the present invention is:
1. the particle diameter of product nano zine oxide is even, and does not reunite.
2. the product nano zine oxide has good ultraviolet absorption characteristic, compares in not adding the prepared nano zine oxide of PVP, and its uv-absorbing intensity has improved 4 times.
3. PVP is a kind of industrial chemicals commonly used, and the source is abundant, cost is low.
4. because HMT is a kind of ammonia source that is heated and slowly decomposes, can be uniformly and zinc nitrate react, thereby can evenly generate the nano zine oxide crystal.
5. methyl alcohol is the solvent of boiling point of a kind of end, has higher vapour pressure under lower temperature, makes reaction soln viscosity reduce, and provides condition for obtaining the less nanocrystal of particle diameter.
6. because the chemical solution method temperature of reaction that the present invention adopts is low, have only 95～100 ℃, the reaction times is short, the shortest need 3 hours, reaction raw materials is cheap, and solvent methanol is recyclable to be utilized again, reaction system is airtight, can not pollute, thereby the inventive method is simple to operate, cost is low, the efficient height, the nano zine oxide crystal particle diameter of preparation is evenly distributed, do not reunite, and have good ultraviolet absorption characteristic, for the application of nano zinc oxide material is laid a good foundation.
Description of drawings
Fig. 1 is the x-ray diffraction pattern of the embodiment of the invention 1 resulting nano zine oxide powder.
Fig. 2 is the embodiment of the invention 1 a resulting nano zine oxide transmission electron microscope photo.
Among Fig. 2, a large-area transmission Electronic Speculum picture, b is for amplifying the transmission electron microscope picture, and c is the electron diffraction picture.
Fig. 3 be the present invention includes embodiment 1 interior under different PVP concentration the ultraviolet-visible spectrum absorption figure of resulting nano zinc oxide material.
Embodiment
The following examples are to further specify of the present invention, rather than limit the scope of the invention.
Embodiment 1:
1. the preparation of reaction soln: 0.0005mol zinc nitrate, six methylene radical four ammonia of 0.00075mol are dissolved in the 100ml methanol solution, add 0.5 gram PVP again, be stirred to the solution clarification, can be prepared into reaction soln.
2. nano zine oxide is synthetic: the growth response solution of the above-mentioned zinc oxide nanocrystalline for preparing is poured in the tetrafluoroethylene reactor, airtight, be warming up to 100 ℃, reacted 3 hours, reaction naturally cools to normal temperature after finishing, take out the sample centrifugation, can obtain the nano zine oxide crystal through drying naturally after repeatedly washing.
X-ray diffraction spectrogram such as Fig. 1 of resultant zinc-oxide film, prepared as seen from Figure 1 zinc oxide are hexagonal crystal shape (36-1451).The particle diameter of the zincite crystal that calculates according to the Scherrer formula is 15 nanometers.Transmission electron microscope photo such as Fig. 2 a, b, the particle diameter of prepared as seen from the figure zinc oxide are about 15 (between the 13-17) nanometer, and be consistent with XRD.Prepared zincite crystal size distribution evenly, good dispersity, do not reunite.Fig. 2 c is prepared nano zine oxide crystalline electron diffraction photo, and by bright spot among the figure as can be known, prepared nano zine oxide is a monocrystalline.The uv-visible absorption spectroscopy of prepared nano zine oxide such as Fig. 3 curve c.As seen from the figure, prepared nano zine oxide has good absorptivity in the ultraviolet region, and visible region has good perviousness.Fig. 3 curve a, b and d are respectively the uv-visible absorption spectroscopies of the nano zine oxide that obtains in different PVP concentration (0%, 0.25%, 2%), as seen from the figure, in PVP concentration is 0.5% o'clock, and the nano zinc oxide material that is obtained has best uv absorption property.
Embodiment 2:
1. the preparation of reaction soln: 0.0005mol zinc nitrate, six methylene radical four ammonia of 0.00075mol are dissolved in the 100ml methanol solution, add 0.5 gram PVP again, be stirred to the solution clarification, can be prepared into reaction soln.
2. nano zine oxide is synthetic: the growth response solution of the above-mentioned zinc oxide nanocrystalline for preparing is poured in the tetrafluoroethylene reactor, airtight, be warming up to 98 ℃, reacted 3.5 hours, reaction naturally cools to normal temperature after finishing, take out the sample centrifugation, can obtain the nano zine oxide crystal through drying naturally after repeatedly washing.
Embodiment 3:
1. the preparation of reaction soln: 0.0005mol zinc nitrate, six methylene radical four ammonia of 0.00075mol are dissolved in the 100ml methanol solution, add 0.5 gram PVP again, be stirred to the solution clarification, can be prepared into reaction soln.
2. nano zine oxide is synthetic: the growth response solution of the above-mentioned zinc oxide nanocrystalline for preparing is poured in the tetrafluoroethylene reactor, airtight, be warming up to 97 ℃, reacted 4 hours, reaction naturally cools to normal temperature after finishing, take out the sample centrifugation, can obtain the nano zine oxide crystal through drying naturally after repeatedly washing.
Claims (1)
1, a kind of single nano-ZnO preparation of disperseing not have reunion and strong uv-absorbing, it is characterized in that at first being dissolved in zinc nitrate hexahydrate and six methylene radical four ammonia in the methanol solution respectively, add polyvinylpyrrolidone again, be stirred to the growth response solution that the solution clarification is prepared into zinc oxide nanocrystalline, above-mentioned reaction soln is poured in the tetrafluoroethylene reactor, airtight, be warming up to 95-100 ℃, reacted 3-4 hour, reaction naturally cools to normal temperature after finishing, centrifugation, dry after the washing and can obtain the zincite crystal that particle diameter is the 13-17 nanometer, wherein zinc nitrate hexahydrate, six methylene radical four ammonia, polyvinylpyrrolidone, the ratio of methanol usage is: 0.0005 mole: 0.00075 mole: 0.5 gram: 100 milliliters.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410017850 CN1562762A (en) | 2004-04-22 | 2004-04-22 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
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| CN 200410017850 CN1562762A (en) | 2004-04-22 | 2004-04-22 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391848C (en) * | 2006-03-02 | 2008-06-04 | 浙江大学 | Process for preparing zinc oxide nano stick |
| CN101786652A (en) * | 2010-02-26 | 2010-07-28 | 上海理工大学 | Method for preparing zinc oxide nano rod with concave end |
| CN101618850B (en) * | 2009-07-24 | 2011-12-28 | 华南理工大学 | Preparation method of anti-ultraviolet ray zinc zirconium oxide nanocomposite |
| CN102659171A (en) * | 2012-05-15 | 2012-09-12 | 桂林理工大学 | Preparation method of water-soluble zinc oxide nanoparticles |
| CN114105184A (en) * | 2021-12-03 | 2022-03-01 | 江永县潇湘化工有限公司 | Method for preparing small-size zinc oxide by using carbon dioxide |
-
2004
- 2004-04-22 CN CN 200410017850 patent/CN1562762A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100391848C (en) * | 2006-03-02 | 2008-06-04 | 浙江大学 | Process for preparing zinc oxide nano stick |
| CN101618850B (en) * | 2009-07-24 | 2011-12-28 | 华南理工大学 | Preparation method of anti-ultraviolet ray zinc zirconium oxide nanocomposite |
| CN101786652A (en) * | 2010-02-26 | 2010-07-28 | 上海理工大学 | Method for preparing zinc oxide nano rod with concave end |
| CN102659171A (en) * | 2012-05-15 | 2012-09-12 | 桂林理工大学 | Preparation method of water-soluble zinc oxide nanoparticles |
| CN102659171B (en) * | 2012-05-15 | 2014-01-08 | 桂林理工大学 | Preparation method of water-soluble zinc oxide nanoparticles |
| CN114105184A (en) * | 2021-12-03 | 2022-03-01 | 江永县潇湘化工有限公司 | Method for preparing small-size zinc oxide by using carbon dioxide |
| CN114105184B (en) * | 2021-12-03 | 2023-10-24 | 江永县潇湘化工有限公司 | Method for preparing small-size zinc oxide from carbon dioxide |
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