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Preparation method of ultrathin zinc oxide sphere shell

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

Active Publication Date: 2018-06-08
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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  • Preparation method of ultrathin zinc oxide sphere shell
  • Preparation method of ultrathin zinc oxide sphere shell
  • Preparation method of ultrathin zinc oxide sphere shell

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preparation example Construction

[0025] The preparation method of an ultra-thin zinc oxide spherical shell of the present invention mainly includes two steps, first using laser ablation technology to prepare zinc oxide@zinc microspheres, and then performing thermal annealing on zinc oxide@zinc microspheres to obtain micron The method is simple and easy to operate, and by controlling the annealing process, zinc oxide spherical shells with obvious laser luminescence characteristics can also be obtained.

[0026] Among them, the process of preparing zinc oxide@zinc microspheres by laser ablation method is generally carried out by pulsed laser deposition system. The pulsed laser deposition system includes pulsed laser, lens, metal zinc target, stage and substrate, and gas phase ablation method can be used. , directly ablate the target with laser in the air, the metal target will generate metal plasma due to the high energy ablation of the laser, and then agglomerate and oxidize in the liquid environment on the sub...

Embodiment 1

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

[0028] Turn on the pulsed laser, adjust the position of the lens, and focus the laser beam on the surface of the zinc target; then place the substrate silicon wafer at a position 5 mm away from the target in the horizontal direction and 1 cm away from the laser focus point in the vertical direction, and drop on the silicon wafer Add a few drops of deionized water until the substrate is evenly 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 in which zinc oxide spherical shells wrap zinc particles, and have a spherical shape with a smooth surface and a diameter of about 3 μm.

[0029] The laser performance of the prepared zinc oxide@zinc microspheres was tested, and the obt...

Embodiment 2

[0030] Example 2 Preparation of Zinc Oxide Spherical Shell

[0031] The quartz tube with openings 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 cover of the tube furnace; turn on the vacuum pump to pump the air pressure in the tube furnace to 100Pa, and then pass in nitrogen, The flow rate is 80sccm, and the air pressure in the adjustment tube is stabilized at about 100Pa; open the controller of the split tube furnace, set the parameters as heating time 5h, and anneal at 500°C 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 relatively thin, and the thickness is below 10nm; however, the surface of some sp...

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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 nanometer material preparation. Background technique [0002] Zinc oxide has a band gap of 3.37eV and an exciton binding energy of 60meV at room temperature, so it has good luminescent properties in the ultraviolet region, as well as photocatalytic and sensing properties. Zinc oxide hollow microspheres have the characteristics of shape, size controllable, good monodispersity, high specific surface area, and low density, and are widely used in various fields such as catalysis, medical treatment, and optoelectronic devices. In the existing research, ZnO microspheres with hollow structures have been widely used in various fields, such as solar energy, photocatalysis, and gas sensing. In addition, zinc oxide is also a promis...

Claims

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Application Information

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Patent Type & Authority Applications(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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