Method for preparing micro structural zinc oxide by hydrothermal method

Abstract

The invention discloses a method for preparing micro structural zinc oxide by a hydrothermal method. Polyvinyl pyrrolidone K-30 is used as a template, zinc acetate dihydrate is used as a zinc source, and H2O2 is used as an oxidant; and a zinc oxide material with four micro structures of sea urchin shape, taper, hexagonal prism self-assembled solid sphere and sugarcoated haw shape is prepared by controlling the reactant concentration, the hydrothermal growth time and the reaction temperature. The method is simple and has the advantages of low cost, mild condition, no environmental pollution and the like. The prepared micro zinc oxide material has high purity, regular crystal structure, good shape controllability and short production period, and has huge application prospect on the aspects of fuel cells, photoelectric conversion materials, chemical sensors and the like.

Description

Technical field

[0001] The invention belongs to the field of semiconductor micron material preparation, and specifically relates to a preparation method of a micron zinc oxide material, in particular to a method for preparing zinc oxide with four special morphologies by adopting an emulsion-assisted hydrothermal method. Background technique

[0002] Zinc oxide is an important wide-bandgap semiconductor material with a wurtzite crystal structure with a bandwidth of 3.37eV. It has excellent chemical properties, thermal stability, optical properties and electrical properties, and can produce near-ultraviolet room temperature at high density Exciton lasers are therefore widely used in gas sensors, piezoelectric materials, catalysts, solar cells, biomedicine and other fields. Research on the preparation, assembly and application of zinc oxide micron and nanostructure units is extremely active. Because zinc oxide nanomaterials have exciton binding energy up to 60meV at room temperatur...

Examples

Embodiment 1

[0025] Taking the preparation of micron sea urchin-like zinc oxide material as an example, the specific preparation method is as follows:

[0026] The mass fraction is 30% H 2 O 2 Add 5g to 71g of distilled water, stir at room temperature for 5 minutes, add polyvinylpyrrolidone K-300.12g, stir at room temperature for 10 minutes, add 0.439g zinc acetate dihydrate, stir at room temperature for 20 minutes, add 4mL of substance with a concentration of 5mol / L NaOH aqueous solution, polyvinylpyrrolidone K-30 and zinc acetate dihydrate, 30% H 2 O 2 The mass ratio of distilled water and NaOH is 1:3.658:41.67:591.7:6.667. Stir at room temperature. After the solution becomes white turbid, continue to stir for 5 minutes. Pour the white turbid solution into a hydrothermal reactor lined with polytetrafluoroethylene In the middle, the hydrothermal reaction vessel was sealed, and the hydrothermal reaction vessel was placed in an oven at a temperature of 180°C for 24 hours, centrifuged, and the p...

Embodiment 2

[0029] In Example 1, the H with a mass fraction of 30% 2 O 2 Add 1g to 56g distilled water, stir at room temperature for 5 minutes, add polyvinylpyrrolidone K-300.12g, stir at room temperature for 10 minutes, add 0.0439g zinc acetate dihydrate, stir at room temperature for 20 minutes, add 2mL of substance with a concentration of 5mol / L NaOH aqueous solution, polyvinylpyrrolidone K-30 and zinc acetate dihydrate, 30% H 2 O 2 The mass ratio of distilled water and NaOH is 1:0.3658:8.333:466.7:3.333, and the other steps are the same as in the corresponding examples to prepare micro-structured zinc oxide. The resulting product was characterized by Quanta 200 environmental scanning electron microscope, the results are shown in figure 2 .

[0030] by figure 2 It can be seen that the obtained product is micron sea urchin-like zinc oxide, and many zinc oxide micron rods grow from the center of the ball. The diameter of the sea urchin ball is 40-80 μm, the length of the rod is 20-40 μm, an...

Embodiment 3

[0032] In Example 1, the H with a mass fraction of 30% 2 O 2 Add 16g to 60g distilled water, stir at room temperature for 5 minutes, add polyvinylpyrrolidone K-300.096g, stir at room temperature for 10 minutes, add 1.054g zinc acetate dihydrate, stir at room temperature for 20 minutes, add 12mL of substance with a concentration of 5mol / L NaOH aqueous solution, polyvinylpyrrolidone K-30 and zinc acetate dihydrate, 30% H 2 O 2 The mass ratio of distilled water and NaOH is 1:10.98:166.7:625:25, and the other steps are the same as in the corresponding examples to prepare micro-structured zinc oxide. The resulting product was characterized by Quanta 200 environmental scanning electron microscope, the results are shown in image 3 .

[0033] by image 3 It can be seen that the resulting product is micron sea urchin-like zinc oxide, and many zinc oxide micron rods grow from the center of the ball. The diameter of the sea urchin ball is 30-60 μm, the length of the rod is 15-30 μm, and the...

Technical field

[0001] The invention belongs to the field of semiconductor micron material preparation, and specifically relates to a preparation method of a micron zinc oxide material, in particular to a method for preparing zinc oxide with four special morphologies by adopting an emulsion-assisted hydrothermal method. Background technique

[0002] Zinc oxide is an important wide-bandgap semiconductor material with a wurtzite crystal structure with a bandwidth of 3.37eV. It has excellent chemical properties, thermal stability, optical properties and electrical properties, and can produce near-ultraviolet room temperature at high density Exciton lasers are therefore widely used in gas sensors, piezoelectric materials, catalysts, solar cells, biomedicine and other fields. Research on the preparation, assembly and application of zinc oxide micron and nanostructure units is extremely active. Because zinc oxide nanomaterials have exciton binding energy up to 60meV at room temperatur...

Examples

Embodiment 1

[0025] Taking the preparation of micron sea urchin-like zinc oxide material as an example, the specific preparation method is as follows:

[0026] The mass fraction is 30% H 2 O 2 Add 5g to 71g of distilled water, stir at room temperature for 5 minutes, add polyvinylpyrrolidone K-300.12g, stir at room temperature for 10 minutes, add 0.439g zinc acetate dihydrate, stir at room temperature for 20 minutes, add 4mL of substance with a concentration of 5mol / L NaOH aqueous solution, polyvinylpyrrolidone K-30 and zinc acetate dihydrate, 30% H 2 O 2 The mass ratio of distilled water and NaOH is 1:3.658:41.67:591.7:6.667. Stir at room temperature. After the solution becomes white turbid, continue to stir for 5 minutes. Pour the white turbid solution into a hydrothermal reactor lined with polytetrafluoroethylene In the middle, the hydrothermal reaction vessel was sealed, and the hydrothermal reaction vessel was placed in an oven at a temperature of 180°C for 24 hours, centrifuged, and the p...

Embodiment 2

[0029] In Example 1, the H with a mass fraction of 30% 2 O 2 Add 1g to 56g distilled water, stir at room temperature for 5 minutes, add polyvinylpyrrolidone K-300.12g, stir at room temperature for 10 minutes, add 0.0439g zinc acetate dihydrate, stir at room temperature for 20 minutes, add 2mL of substance with a concentration of 5mol / L NaOH aqueous solution, polyvinylpyrrolidone K-30 and zinc acetate dihydrate, 30% H 2 O 2 The mass ratio of distilled water and NaOH is 1:0.3658:8.333:466.7:3.333, and the other steps are the same as in the corresponding examples to prepare micro-structured zinc oxide. The resulting product was characterized by Quanta 200 environmental scanning electron microscope, the results are shown in figure 2 .

[0030] by figure 2 It can be seen that the obtained product is micron sea urchin-like zinc oxide, and many zinc oxide micron rods grow from the center of the ball. The diameter of the sea urchin ball is 40-80 μm, the length of the rod is 20-40 μm, an...

Embodiment 3

[0032] In Example 1, the H with a mass fraction of 30% 2 O 2 Add 16g to 60g distilled water, stir at room temperature for 5 minutes, add polyvinylpyrrolidone K-300.096g, stir at room temperature for 10 minutes, add 1.054g zinc acetate dihydrate, stir at room temperature for 20 minutes, add 12mL of substance with a concentration of 5mol / L NaOH aqueous solution, polyvinylpyrrolidone K-30 and zinc acetate dihydrate, 30% H 2 O 2 The mass ratio of distilled water and NaOH is 1:10.98:166.7:625:25, and the other steps are the same as in the corresponding examples to prepare micro-structured zinc oxide. The resulting product was characterized by Quanta 200 environmental scanning electron microscope, the results are shown in image 3 .

[0033] by image 3 It can be seen that the resulting product is micron sea urchin-like zinc oxide, and many zinc oxide micron rods grow from the center of the ball. The diameter of the sea urchin ball is 30-60 μm, the length of the rod is 15-30 μm, and the...

Images