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A kind of preparation method of ultra-thin zinc oxide spherical shell

A technology of zinc oxide and spherical shells, which is applied in the field of optoelectronic nanomaterials preparation, can solve the problems of poor product structure and performance, complex preparation methods of zinc oxide spherical shells, etc., and achieve the advantages of perfect shape, simple and easy operation, and obvious laser luminescence characteristics Effect

Active Publication Date: 2020-03-31
SOUTHEAST UNIV
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Problems solved by technology

[0004] Purpose of the invention: To provide a preparation method for ultra-thin zinc oxide spherical shells in view of the problems of complex preparation methods, poor product structure and performance, and no laser phenomenon in the preparation of zinc oxide spherical shells by the existing template method and hydrothermal method

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  • A kind of preparation method of ultra-thin zinc oxide spherical shell
  • A kind of preparation method of ultra-thin zinc oxide spherical shell
  • A kind of preparation method of ultra-thin zinc oxide spherical shell

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preparation example Construction

[0025] The method for preparing an ultra-thin zinc oxide spherical shell of the present invention mainly includes two steps: firstly, the zinc oxide@zinc microspheres are prepared by laser ablation technology, and then the zinc oxide@zinc microspheres are thermally annealed to obtain micron The ultra-thin zinc oxide spherical shell of high grade is obtained; the method is simple and easy to operate, and the zinc oxide spherical shell with obvious laser light emission characteristics can be obtained by controlling the annealing process.

[0026] Among them, the process of preparing zinc oxide@zinc microspheres by laser ablation is generally carried out by a pulsed laser deposition system. The pulsed laser deposition system includes a pulsed laser, a lens, a metal zinc target, a stage and a substrate, and a gas phase ablation method can be used. , the target is directly ablated by laser in the air. Due to the high-energy ablation of the laser, the metal target will generate metal...

Embodiment 1

[0027] Example 1 Preparation of zinc oxide@zinc microspheres

[0028] Turn on the pulsed laser, adjust the position of the lens, focus the laser beam on the surface of the zinc target; then place the substrate silicon wafer at a distance of 5mm from the target in the lateral direction and 1cm from the laser focus point in the longitudinal direction. Add a few drops of deionized water until the substrate is fully covered; adjust the laser output power to 210mW, and the ablation time to 5min; dry the silicon wafer at 60°C to obtain zinc oxide@zinc microspheres, the structure of which is as follows figure 1 , it can be seen that the zinc oxide@zinc microspheres are hollow core-shell composite microspheres with zinc oxide spherical shells wrapping zinc particles, with a spherical morphology with a smooth surface and a diameter of about 3 μm.

[0029] The laser properties of the as-prepared ZnO@Zn microspheres were tested, and the obtained laser spectra were as follows figure 2 ,...

Embodiment 2

[0030] Example 2 Preparation of zinc oxide spherical shell

[0031] The quartz tube with open ends at both ends was cleaned with alcohol and then dried, and the core-shell structure zinc oxide@zinc composite microspheres prepared in Example 1 were placed in the quartz tube together with the substrate. Place the sample in the special quartz glass tube of the split tube furnace, place it in the center of the tube furnace, close the lid of the tube furnace; turn on the vacuum pump to pump the air pressure in the tube furnace to 100Pa, and introduce nitrogen gas. The flow rate is 80sccm, and the air pressure in the adjustment tube is stabilized at about 100Pa; the controller of the split tube furnace is turned on, and the parameter is set to the heating time of 5h, and annealed at 500 ℃ for 1h, and the obtained zinc oxide spherical shell is as follows image 3 , it can be seen that the shell wall of the spherical shell is thin and the thickness is below 10 nm; however, the surface...

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Abstract

The invention discloses a preparation method of an ultrathin zinc oxide sphere shell. The preparation method of the ultrathin zinc oxide sphere shell comprises the following steps: 1) preparing a zincoxide@zinc microsphere with a core-shell structure by a laser ablation method; 2) putting the prepared zinc oxide@zinc microsphere into a tubular furnace, vacuumizing the tubular furnace until the vacuum degree reaches to below 100 Pa, introducing protective gas and adjusting the gas pressure in the furnace to stabilize the gas pressure to 100 Pa; and 3) after setting the tubular furnace parameter as heating for 5 to 15 hours to reach to 300 to 600 DEG C, annealing for 1 to 3 hours to obtain the ultrathin zinc oxide sphere shell. The method is a template-free method, the template is not needed, the ultrathin zinc oxide sphere shell can be obtained only by controlling the thermal annealing process, and the method is simple and easy to operate; by the method, the ultrathin zinc oxide spherewith undamaged appearance and smooth surface can be prepared, the diameter of the prepared zinc oxide sphere shell is micron-size grade and the thickness of the shell wall of the sphere shell is below 10 nm; furthermore, by the method, the zinc oxide sphere shell with obvious laser light-emitting characteristic can be prepared.

Description

technical field [0001] The invention relates to a method for preparing an ultra-thin zinc oxide spherical shell, in particular to a method for preparing an ultra-thin zinc oxide spherical shell by thermal annealing, and belongs to the field of photoelectric nanomaterial preparation. Background technique [0002] Zinc oxide has a forbidden band width of 3.37 eV and an exciton binding energy of 60 meV at room temperature, so it has good luminescence properties in the ultraviolet region, as well as photocatalytic and sensing properties. Zinc oxide hollow microspheres have the characteristics of controllable shape, size, good monodispersity, high specific surface area and low density, and are widely used in catalysis, medical treatment, optoelectronic devices and other fields. In the existing research, hollow ZnO microspheres are widely used in various fields, such as solar energy, photocatalysis, and gas sensing. In addition, zinc oxide is also a promising material in the fiel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G9/02B82Y40/00
CPCB82Y40/00C01G9/02C01P2004/03C01P2004/34C01P2006/60
Inventor 石增良王潇璇徐春祥
Owner SOUTHEAST UNIV
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