CN102079540A - Preparation method of three-dimensional porous zinc oxide microstructure - Google Patents
Preparation method of three-dimensional porous zinc oxide microstructure Download PDFInfo
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- CN102079540A CN102079540A CN 201110030547 CN201110030547A CN102079540A CN 102079540 A CN102079540 A CN 102079540A CN 201110030547 CN201110030547 CN 201110030547 CN 201110030547 A CN201110030547 A CN 201110030547A CN 102079540 A CN102079540 A CN 102079540A
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Abstract
The invention discloses a preparation method of a three-dimensional porous zinc oxide microstructure, solving the technical problem of high reaction temperature in the process of preparing the three-dimensional porous zinc oxide microstructure by using the existing preparation method. The technical scheme is as follows: respectively preparing zinc acetate solution and urea solution by using high-pure water as a solvent; slowly stirring the zinc acetate solution and dropping in the urea solution, stirring and refluxing the mixture to obtain white precipitate; filtering and washing the white precipitate with deionized water and absolute ethyl alcohol, putting the white precipitate in a vacuum oven for drying; and annealing the dried white precipitate at the air atmosphere to obtain the three-dimensional porous zinc oxide microstructure. Because the three-dimensional porous zinc oxide microstructure is prepared by using a method of combing low temperature soft chemistry and subsequent thermal treatment, the preparation temperature of a precursor is reduced. Compared with the prior art, the preparation temperature is reduced from more than 120 DEG C to 70-90 DEG C.
Description
Technical field
The present invention relates to a kind of preparation method of zinc oxide microstructure, particularly a kind of preparation method of three-dimensional porous zinc oxide microstructure.
Background technology
The three-dimensional porous nano material is except the peculiar property that possesses nano material, and vesicular structure has also been given the application of they novelties.Compare with solid nano material, porous material has bigger specific activity surface-area, and gas can freely spread by vesicular structure, so in the gas sensor field good prospects for application is arranged.
Document " ZnO-based hollow microspheres:biopolymer-assisted assemblies from ZnO nanorods.J.Phys.Chem.B 2006; 110:15847-15852 " discloses a kind of method of utilizing the three-dimensional porous nano zinc oxide material of template for preparing, but follow-up high-temperature heat treatment or chemical etching that this method needs remove template, are not a kind of methods of economy.
Document " Malate-assisted synthesis of ZnO hexagonal architectures with porous characteristics and photoluminescence properties investigation.J.Phys.Chem.C 2007; 111; 1113-1118 " discloses a kind of method for preparing three-dimensional porous Zinc oxide nanoparticle, it utilizes tensio-active agent to prepare the presoma with three-dimensional structure earlier, prepare three-dimensional porous ZnO by the calcining presoma then, but the temperature of reaction during the synthetic presoma of liquid phase all is higher than 120 ℃.
Summary of the invention
Prepare the high deficiency of temperature of reaction in the three-dimensional porous zinc oxide microstructure process in order to overcome prior preparation method, the invention provides a kind of preparation method of three-dimensional porous zinc oxide microstructure, utilize low temperature softening to learn and prepared three-dimensional porous zinc oxide microstructure in conjunction with follow-up heat-treating methods.Adopt soft chemical method, reduced the synthesis temperature of presoma on the one hand, also comparatively economical on the other hand.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of three-dimensional porous zinc oxide microstructure is characterized in may further comprise the steps:
(a) be solvent with the high purity water, dispose the acetic acid zinc solution of 0.1～0.3mol/L and the urea soln of 0.2～0.6mol/L respectively;
(b) acetic acid zinc solution for preparing is splashed in the urea soln, in this process, keep stirring;
(c) mixing solutions that step (b) is prepared obtains white precipitate at 60～90 ℃ of stirring and refluxing 1～3h;
(d) white precipitate with deionized water and dehydrated alcohol are carried out repeatedly filtering and washing, dry in vacuum drying oven then;
(e) dried white precipitate is done anneal in air atmosphere, rise to 300～600 ℃ and be incubated 1～4 hour, obtain 3-dimensional multi-layered porous ZnO microstructure with the heat-up rate of 2～5 ℃/min.
The invention has the beneficial effects as follows: adopt low temperature softening to learn and prepared three-dimensional porous zinc oxide microstructure in conjunction with follow-up heat-treating methods.The preparation temperature and the preparation cost of presoma have been reduced.The preparation temperature of presoma is higher than 120 ℃ and is reduced to 60～90 ℃ by background technology.
Below in conjunction with the drawings and specific embodiments the present invention is elaborated.
Description of drawings
Fig. 1 is the XRD figure spectrum of the three-dimensional porous ZnO microstructure of the inventive method example 1 preparation.
Fig. 2 is the SEM photo of the product that obtains under the different urea contents of the inventive method.
Embodiment
Embodiment 1, is solvent with the high purity water, disposes the acetic acid zinc solution of 0.1mol/L and each 50mL of urea soln of 0.2mol/L respectively; The acetic acid zinc solution for preparing is splashed in the urea soln, in this process, keep stirring; Mixture at 60 ℃ of stirring and refluxing 1.5h, is obtained white precipitate; White precipitate with deionized water and dehydrated alcohol are carried out repeatedly filtering and washing, dry in vacuum drying oven then; Dried white precipitate is done anneal in air atmosphere, rise to 300 ℃ and be incubated 2 hours, obtain 3-dimensional multi-layered porous ZnO microstructure with the heat-up rate of 2 ℃/min.
As can see from Figure 1, presoma has been converted to hexagonal wurtzite zinc oxide fully, does not have appearance and the zinc diffraction peak relevant with the carbonaceous nanoparticle.The size that can estimate the ZnO nano particle that is self-assembled into multilayer porous structure, particularly according to the Shcerer formula is about 20nm.
Embodiment 2, are solvent with the high purity water, dispose the zinc acetate of 0.2mol/L and each 50mL of urea soln of 0.4mol/L respectively; The acetic acid zinc solution for preparing is splashed in the urea soln, in this process, keep stirring; Mixture at 70 ℃ of stirring and refluxing 2h, is obtained white precipitate; White precipitate with deionized water and dehydrated alcohol are carried out repeatedly filtering and washing, dry in vacuum drying oven then; Dried white precipitate is done anneal in air atmosphere, rise to 500 ℃ and be incubated 3 hours, obtain 3-dimensional multi-layered porous ZnO microstructure with the heat-up rate of 3 ℃/min.
Embodiment 3, are solvent with the high purity water, dispose the acetic acid zinc solution of 0.3mol/L and each 50mL of urea soln of 0.8mol/L respectively; The acetic acid zinc solution for preparing is splashed in the urea soln, in this process, keep stirring; Mixture at 80 ℃ of stirring and refluxing 3h, is obtained white precipitate; White precipitate with deionized water and dehydrated alcohol are carried out repeatedly filtering and washing, dry in vacuum drying oven then; Dried white precipitate is done anneal in air atmosphere, rise to 400 ℃ and be incubated 4 hours, obtain 3-dimensional multi-layered porous ZnO microstructure with the heat-up rate of 3 ℃/min.
Embodiment 4, are solvent with the high purity water, dispose the acetic acid zinc solution of 0.3mol/L and each 50mL of urea soln of 0.6mol/L respectively; The acetic acid zinc solution for preparing is splashed in the urea soln, in this process, keep stirring; Mixture at 90 ℃ of stirring and refluxing 1h, is obtained white precipitate; White precipitate with deionized water and dehydrated alcohol are carried out repeatedly filtering and washing, dry in vacuum drying oven then; Dried white precipitate is done anneal in air atmosphere, rise to 600 ℃ and be incubated 1 hour, obtain 3-dimensional multi-layered porous ZnO microstructure with the heat-up rate of 5 ℃/min.
As can be seen from Figure 2, the concentration of urea has a significant impact the pattern of product.When the presoma mol ratio was 1, product was the nanocrystalline of multiwalled three-dimensional structure and prism-shaped.When the presoma mol ratio was 2, product was the multiwalled three-dimensional structure.When precursor concentration is increased to 4, the crystallite of a large amount of dumbbell shapeds appears.And when the presoma mol ratio was 8, wide variation had taken place in the pattern of product, became perlarious nano chain, and these nano chain can be self-assembled into three-dimensional structure along with the increase of urea concentration (the presoma mol ratio is 16).Further observe and find that these nano chain are made up of six sides' nano particle, diameter is that length is more than 200nm about 50nm.
The present invention learns by low temperature softening and has prepared three-dimensional porous zinc oxide microstructure in conjunction with follow-up heat-treating methods.The reduction of production cost and presoma synthesis temperature makes this synthesis technique be expected to be applied to the more preparation of polyoxide porous material.
Claims (1)
1. the preparation method of a three-dimensional porous zinc oxide microstructure is characterized in that comprising the steps:
(a) be solvent with the high purity water, dispose the acetic acid zinc solution of 0.1～0.3mol/L and the urea soln of 0.2～0.6mol/L respectively;
(b) acetic acid zinc solution for preparing is splashed in the urea soln, in this process, keep stirring;
(c) mixing solutions that step (b) is prepared obtains white precipitate at 60～90 ℃ of stirring and refluxing 1～3h;
(d) white precipitate with deionized water and dehydrated alcohol are carried out repeatedly filtering and washing, dry in vacuum drying oven then;
(e) dried white precipitate is done anneal in air atmosphere, rise to 300～600 ℃ and be incubated 1～4 hour, obtain 3-dimensional multi-layered porous ZnO microstructure with the heat-up rate of 2～5 ℃/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318941A (en) * | 2012-09-12 | 2013-09-25 | 上海工程技术大学 | Synthetic method of porous ZnO three-dimensional superstructure assembled by nano-sheets |
| CN103977806A (en) * | 2014-05-16 | 2014-08-13 | 盐城工学院 | Photocatalytic degradation material Co-doped nano ZnO and preparation method thereof |
| CN106186047A (en) * | 2016-08-05 | 2016-12-07 | 武汉理工大学 | A kind of based on secondary nanosphere hierarchical Z nO nano material and preparation method thereof |
| EP3326975A1 (en) * | 2016-11-29 | 2018-05-30 | Consejo Superior De Investigaciones Científicas | Zinc oxide microparticles, preparation method, and use thereof |
| CN115057464A (en) * | 2022-03-25 | 2022-09-16 | 华南理工大学 | Three-dimensional porous ZnO/SnO 2 Composite material, preparation method thereof and application thereof in nickel-zinc battery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004043293A (en) * | 2002-05-20 | 2004-02-12 | Nippon Shokubai Co Ltd | Fibrous fine metal oxide particles |
| CN101177296A (en) * | 2007-10-31 | 2008-05-14 | 山东大学 | Method for preparing sheet porous structural ZnO nano powder |
| CN101786651A (en) * | 2010-01-18 | 2010-07-28 | 安徽师范大学 | Method for preparing flake porous ZnO nano powder |
-
2011
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004043293A (en) * | 2002-05-20 | 2004-02-12 | Nippon Shokubai Co Ltd | Fibrous fine metal oxide particles |
| CN101177296A (en) * | 2007-10-31 | 2008-05-14 | 山东大学 | Method for preparing sheet porous structural ZnO nano powder |
| CN101786651A (en) * | 2010-01-18 | 2010-07-28 | 安徽师范大学 | Method for preparing flake porous ZnO nano powder |
Non-Patent Citations (2)
| Title |
|---|
| 《J Sol-Gel Sci Techn》 20060405 Keita Kakiuchi et al. Fabrication of mesoporous ZnO nanosheets from precursor templates grown in aqueous solutions 63-72 1 第39卷, 2 * |
| 《J. Phys. Chem. C》 20100813 Jin Li et al. Multilayered ZnO Nanosheets with 3D Porous Architectures: Synthesis and Gas Sensing Application 14684-14691 1 第114卷, 第35期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103318941A (en) * | 2012-09-12 | 2013-09-25 | 上海工程技术大学 | Synthetic method of porous ZnO three-dimensional superstructure assembled by nano-sheets |
| CN103977806A (en) * | 2014-05-16 | 2014-08-13 | 盐城工学院 | Photocatalytic degradation material Co-doped nano ZnO and preparation method thereof |
| CN106186047A (en) * | 2016-08-05 | 2016-12-07 | 武汉理工大学 | A kind of based on secondary nanosphere hierarchical Z nO nano material and preparation method thereof |
| CN106186047B (en) * | 2016-08-05 | 2017-12-05 | 武汉理工大学 | One kind is based on secondary nanosphere hierarchical Z nO nano materials and preparation method thereof |
| EP3326975A1 (en) * | 2016-11-29 | 2018-05-30 | Consejo Superior De Investigaciones Científicas | Zinc oxide microparticles, preparation method, and use thereof |
| WO2018099945A1 (en) | 2016-11-29 | 2018-06-07 | Consejo Superior De Investigaciones Científicas | Zinc oxide microparticles, preparation method, and use thereof |
| ES2724825A1 (en) * | 2016-11-29 | 2019-09-16 | Consejo Superior Investigacion | Zinc oxide microparticles, preparation method, and use thereof |
| CN115057464A (en) * | 2022-03-25 | 2022-09-16 | 华南理工大学 | Three-dimensional porous ZnO/SnO 2 Composite material, preparation method thereof and application thereof in nickel-zinc battery |
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Application publication date: 20110601 |