Preparation method of zinc oxide microsphere with nanoflower-shaped microstructure

A microstructure, zinc oxide technology, applied in the direction of zinc oxide/zinc hydroxide, nanotechnology, etc., can solve the problems of difficult engineering scale-up, complicated process, slow preparation, etc., and achieve convenient industrial production, mild reaction environment, and post-treatment. handy effect

Inactive Publication Date: 2012-08-08
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the Chinese patent (CN101249979B) reports a water bath preparation method of prickly spherical zinc oxide. The water bath synthesis method needs ultrasonic activation treatment, the solution needs to be diluted with water, and the water bath temperature must reach the boiling point and need to be stirred. Therefore, the process is relatively complicated and engineering scale-up It is not easy; the literature (Journal of Crystal Growth 282 (2005) 165-172) reports similar ZnO nanostructures, the method adopts the solvothermal method of absolute ethanol as the medium, and the solvent temperature is 190 ° C; Chinese patent (CN102249286A) reports a A method for preparing zinc oxide microspheres in a normal-pressure water bath. The mixed solution needs to be kept in a water bath at 70°C for 10 to 24

Method used

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  • Preparation method of zinc oxide microsphere with nanoflower-shaped microstructure
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  • Preparation method of zinc oxide microsphere with nanoflower-shaped microstructure

Examples

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Example Embodiment

[0022] Example 1

[0023] At room temperature, dissolve 1g of boric acid in 20mL of deionized water, prepare 15mL of zinc acetate aqueous solution with a molar concentration of 0.5mol / L of zinc ion and 10mL of sodium hydroxide solution with a molar concentration of 5mol / L, then stir with a glass rod and slowly add Pour 15 mL of zinc salt aqueous solution into the sodium hydroxide solution, and a clear aqueous solution will be obtained. Then, 20 mL of boric acid solution was quickly poured into the resulting clear solution, and a white precipitate was obtained at rest. Centrifugally clean the precipitate, put it in an oven at 80°C for 4 hours to dry, and then the zinc oxide microspheres constructed from nanosheets can be obtained. The SEM image is as follows figure 1 Shown.

Example Embodiment

[0024] Example 2

[0025] At room temperature, dissolve 5ml of oleic acid in 15ml of absolute ethanol to prepare 15ml of zinc acetate aqueous solution with a molar concentration of zinc ion of 0.5mol / L and 10ml of sodium hydroxide solution with a molar concentration of 5mol / L, and then stir with a glass rod. Slowly pour 15 mL of zinc salt aqueous solution into the sodium hydroxide solution, and a clear aqueous solution will be obtained. Then, 20 mL of the mixed solution of oleic acid and absolute ethanol was quickly poured into the obtained clear liquid, and a white precipitate was obtained at rest. Centrifugally clean the precipitate, put it in an oven at 90°C for 3.5h, and then get the zinc oxide microspheres constructed from nanosheets. The SEM image is as follows figure 2 As shown, the TEM image is as Figure 4 As shown, the XRD graph is as Figure 5 Shown.

Example Embodiment

[0026] Example 3

[0027] At room temperature, dissolve 1g of boric acid in 20mL of deionized water, prepare 15mL of zinc nitrate aqueous solution with a molar concentration of 0.5mol / L of zinc ion and 10mL of sodium hydroxide solution with a molar concentration of 5mol / L, then stir with a glass rod, slowly Pour 15 mL of zinc salt aqueous solution into the sodium hydroxide solution, and a clear aqueous solution will be obtained. Then, 20 mL of boric acid solution was quickly poured into the resulting clear solution, and a white precipitate was obtained at rest. Centrifugally clean the precipitate, put it in an oven at a temperature of 70°C for 5 hours, and then obtain zinc oxide microspheres constructed from nanosheets. The SEM image is as follows image 3 .

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Abstract

The invention relates to a preparation method of a zinc oxide microsphere with a nanoflower-shaped microstructure. The method comprises the following steps of: (1) preparing a solution, to be specific, preparing a soluble zinc salt into an aqueous solution, and preparing a soluble alkali into an aqueous solution; (2) mixing the solutions, to be specific, mixing the soluble zinc salt aqueous solution with the soluble alkali aqueous solution at the room temperature in the volume ratio of 1:10-10:1, slowly pouring an aqueous solution of a soluble zinc salt into the aqueous solution of the soluble alkali, and stirring to obtain a clarifying solution; and (3) preparing a product, to be specific, pouring a weakly-acid solution into the clarifying solution obtained in the step (2), wherein the volume ratio of the weakly-acid solution to the clarifying solution is 1:10-10:1, stirring to obtain a turbid solution containing a large quantity of products, repeatedly washing with deionized water and absolute ethyl alcohol, and drying in a baking oven to obtain a final product. Compared with the prior art, the method has the advantages of capability of rapidly, easily and conveniently preparing a product under the room temperature condition, high yield, low cost, environmental friendliness, wide raw material selection range and contribution to industrial production.

Description

technical field [0001] The invention relates to a method for preparing an oxide semiconductor material, in particular to a method for preparing zinc oxide microspheres with a nano flower-like microstructure. Background technique [0002] As a wide bandgap semiconductor material with a bandgap width of 3.37eV, zinc oxide is non-toxic, and the raw material is cheap and easy to obtain. It has excellent piezoelectric, photoelectric and dielectric properties. Among them, nano-zinc oxide is widely used in the fields of gas sensitivity, photocatalysis, antibacterial and photoelectric materials, but its nano-scale size range brings difficulties to recycling and is not conducive to recycling. Therefore, it is hoped to find a method that can both A zinc oxide product that maintains most of the properties of nanomaterials and is conducive to recycling. [0003] ZnO nanosheets are a readily available nanostructure. In this form, ZnO has a large surface area and very good photochemical ...

Claims

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Application Information

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IPC IPC(8): C01G9/02B82Y40/00
Inventor 郭守武杨彦强吴海霞杨永强
Owner SHANGHAI JIAO TONG UNIV
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