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Preparation method of shape-controlled micro-nano ZnO under normal pressure and low temperature conditions

A low-temperature, micro-nano technology, applied in zinc oxide/zinc hydroxide and other directions, can solve the problems of poor size control effect, poor morphology uniformity, low crystallinity, etc., and achieve low raw material prices, easy raw materials, and safety. high effect

Inactive Publication Date: 2018-07-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above synthesis requires the use of a large amount of oleylamine or other organic solvents as solvents for the reaction, and most of them require high temperature and high pressure, or more complicated conditions
At the same time, due to the limitations of the preparation process, poor repeatability, low crystallinity, poor shape uniformity, and poor size control have become the main problems in the efficient preparation of ZnO micro-nanostructures with controllable morphology.

Method used

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  • Preparation method of shape-controlled micro-nano ZnO under normal pressure and low temperature conditions
  • Preparation method of shape-controlled micro-nano ZnO under normal pressure and low temperature conditions
  • Preparation method of shape-controlled micro-nano ZnO under normal pressure and low temperature conditions

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Effect test

Embodiment 1

[0024] Add 2mmol of zinc acetate to a mixed solution of 60mL of dimethylformamide and water (volume ratio: 2:1), then add 6mmol of oleylamine, heat and react at 85°C for 30min in an open system at normal pressure, cool, centrifuge, and wash , freeze-dried to obtain micronano ZnO. The SEM image and XRD image of the product are shown in figure 1 and 2 . From the SEM image of the product ( figure 1 ) shows that the morphology of the product is a hexagonal semi-pyramid columnar body, the length is about 260nm, and the diameter of the thickest end is about 200nm. The XRD figure of product ( figure 2 ) results are consistent with the standard XRD spectrum (JCPDS No.36-1451), which proves that the crystal phase of the obtained product is a hexagonal ZnO phase with high crystallinity.

Embodiment 2

[0026] Add 1mmol of zinc nitrate to a mixed solution of 40mL of dimethylformamide and water (volume ratio 1:1), then add 2mmol of oleylamine, heat and react at 80°C for 60min in an open system at normal pressure, cool, centrifuge, and wash , freeze-dried to obtain micronano ZnO. The SEM image of the product is shown in image 3 . It can be seen from the SEM image that the morphology of the product is a hexagonal semi-pyramid columnar body, the length is about 160nm, and the diameter of the thickest end is about 150nm.

Embodiment 3

[0028] Add 1mmol of zinc acetate to a mixed solution of 60mL of dimethylformamide and water (volume ratio: 3:1), then add 4mmol of oleylamine, heat and react at 90°C for 20min in an open system at normal pressure, cool, centrifuge, and wash , freeze-dried to obtain micronano ZnO. The SEM image of the product is shown in Figure 4 . It can be seen from the SEM image that the product is in the shape of a brush-shaped column with a long handle, the total length is about 1-2 μm, the length of the handle is about 480 nm, and the diameter of the brush end is about 650 nm.

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Abstract

The invention relates to a preparation method of shape-controlled micro-nano ZnO under normal pressure and low temperature conditions. The preparation method comprises the following steps: dissolvinga zinc salt in a mixed solution of dimethyl formamide and water to obtain a zinc salt solution, adding oleylamine, reacting under the condition of normal pressure and the temperature of 80 to 90 DEG C, centrifugally separating, washing, and freeze drying, thus obtaining the shape-controlled micro-nano ZnO. The preparation method is simple and easy, the used raw materials are easy to obtain, the cost is low, and the prepared micro-nano ZnO is high in structure and shape controllability; and by using a conventional heating way, the preparation method is performed in a low-temperature normal pressure open system, so that the high temperature and the high pressure which are necessary to use in a hydrothermal method or a solvothermal method can be avoided, the safety is high, and the energy issaved.

Description

technical field [0001] The invention belongs to the field of preparation of zinc oxide, in particular to a method for preparing micronano ZnO with controllable morphology under normal pressure and low temperature conditions. Background technique [0002] ZnO has been widely concerned and applied due to its excellent semiconducting, piezoelectric, pyroelectric and fluorescent properties. Especially in recent years, it has been found that ZnO, as a typical direct bandgap semiconductor compound, has a forbidden band width of 3.37ev at room temperature and an exciton binding energy of 60mev. It can be used in short-wavelength semiconductor lasers, ultraviolet light emitting and detecting devices, and transparent Optoelectronic nanodevices such as semiconductors and electromechanical coupling sensors make ZnO a research hotspot in the field of nanometers. How to effectively control the size and morphology of ZnO has become a hot topic. By selecting an appropriate reaction system...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02
CPCC01G9/02C01P2002/72C01P2004/03C01P2004/40C01P2004/62C01P2006/80
Inventor 邢彦军胡翠翠
Owner DONGHUA UNIV
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