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Monodisperse Cu2O single crystal solid sphere with controllable particle size and preparation method thereof

A monodisperse, solid sphere technology, applied in the direction of copper oxide/copper hydroxide, nanotechnology, etc., can solve problems that have not been reported before, and achieve the effect of expanding the application range and precisely controlling the particle size

Active Publication Date: 2019-06-07
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At room temperature, the precursor copper hydroxide is reduced by ascorbic acid to obtain polyhedral-like single crystal cuprous oxide microspheres (see S.R.Zhang, R.B. Jiang, Y.M.Xie, Q.F.Ruan, B.C.Yang, J.F.Wang, H.Q.Lin, Adv Mater., 2015 , 27, 7432-7439. and Y.K.Bai,; T.F.Yang, Q.Gu, G.heng, R.Zheng, Powder Technol., 2012, 227, 35-42S.), but their surfaces have obvious faces and Leng is not a sphere in the true sense. At present, there is no report on the preparation of a real solid solid single crystal sphere at room temperature and the precise adjustment of particle size.

Method used

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  • Monodisperse Cu2O single crystal solid sphere with controllable particle size and preparation method thereof
  • Monodisperse Cu2O single crystal solid sphere with controllable particle size and preparation method thereof
  • Monodisperse Cu2O single crystal solid sphere with controllable particle size and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add copper source 13.4mM, small molecule ligand 26.8mM sodium citrate dihydrate, polyvinylpyrrolidone (molecular weight Mw=30000) 2.3mM into the mixed solvent of water and polyol (ethylene glycol) (ethylene glycol and water The mass ratio is 3:10), add 20mL of NaOH solution to the mixed solution, and the concentration is 0.5M; at a temperature of 20°C; add 7mL, 0.12M ascorbic acid to the above mixed solution, react for 20min, and add to the mixed solution Add 8mL of ascorbic acid together, react for 1h, centrifuge to separate the precipitate, and dry the product under vacuum at 60°C to obtain uniform single crystal cuprous oxide solid microspheres with a particle size of 170nm, as figure 1 shown. Use 170nm monodispersed cuprous oxide single crystal solid balls as building units to build an amorphous structure, and carry out reflectance spectrum tests and structural color photos as shown in Figure 5 As shown, the reflection peak position is 635nm, and the structure is ...

Embodiment 2

[0029]Copper source 13.4mM, small molecule ligand 16.2mM disodium edetate), polyvinylpyrrolidone (molecular weight Mw=40000) 2.3mM joins in the mixed solvent of water and glycerol (glycerol and water The mass ratio is 2:5), add 20mL of NaOH solution to the mixed solution, the concentration is 0.5M; under the condition of temperature of 60°C; add 7mL, 0.12M glucose dropwise to the above mixed solution under vigorous stirring, and react After 10 minutes, add 8 mL of glucose to the mixed solution, react for 1 hour, centrifuge to separate the precipitate, and dry the product under vacuum at 60°C to obtain monodisperse single-crystal cuprous oxide solid microspheres with a particle size of 200 nm. ,Such as figure 2 shown.

Embodiment 3

[0031] Copper source 13.4mM, small molecule ligand 18.7mM pentasodium diethylenetriaminepentaacetic acid (, polyvinylpyrrolidone (molecular weight Mw=10000) 2.3mM is added in the mixed solvent of water and neopentyl glycol ethylene glycol (new The mass ratio of pentylene glycol to water is 7:10), add 20mL of NaOH solution dropwise to the mixed solution, and the concentration is 0.5M; the temperature is under the condition of 80°C; add 7mL dropwise to the above mixed solution, 0.12M Glucose, after reacting for 10 minutes, add 8 mL of glucose to the mixed solution together, react for 1 hour, centrifuge to separate the precipitate, and dry the product under vacuum at 60°C to obtain a monodisperse single crystal cuprous oxide solid with a particle size of 270nm Microspheres, such as image 3 shown.

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Abstract

The invention discloses a monodisperse Cu2O single crystal solid sphere with a controllable particle size and a preparation method thereof. A micromolecule ligand at least comprises two carboxyl groups, and a high-molecular ligand is polyvinylpyrrolidone. The specific process comprises the following steps: preparing a copper source, the high-molecular ligand, the micromolecule ligand and a mixed solution of water and polyhydric alcohol, then dropwise adding a certain amount of an alkali solution into the solution, adding a reducing agent step by step at 20-80 DEG C, and carrying out centrifuging to obtain the monodisperse Cu2O single crystal solid sphere. According to the monodisperse Cu2O single crystal solid sphere with controllable particle size and the preparation method thereof, operation is simple and cost is low, and the monodisperse Cu2O single crystal solid sphere with a particle size of 40-600 nm can be obtained only by adjusting the amount and variety of the micromolecule ligand. The microsphere provided by the invention can be widely applied to the fields of photonic crystals, electrodes of lithium-sulfur batteries, and catalytic photolysis of water.

Description

technical field [0001] The invention relates to a monodisperse Cu with adjustable particle size 2 O single crystal solid sphere and preparation method thereof, belonging to Cu 2 The technical field of preparation of O single crystal microspheres. Background technique [0002] Cuprous oxide is a P-type semiconductor material with a theoretical refractive index of 2.7, which has been widely used in photolysis of water, catalysts, lithium-sulfur battery electrodes, and photonic crystals. Usually the building blocks of photonic crystals are low refractive index such as PS, SiO 2 etc. will lead to weaker photonic bandgap and pale structural color, in recent years with high refractive index microspheres such as TiO 2 , ZnS, CdS, etc., as the building blocks of photonic crystals, make them have low-angle correlation and high-brightness structural colors and other excellent properties, which have attracted extensive attention of researchers at home and abroad. However, most of t...

Claims

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Application Information

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IPC IPC(8): C01G3/02B82Y40/00
Inventor 武素丽毕佳捷常杰
Owner DALIAN UNIV OF TECH
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