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Preparation method of monodisperse yolk-shell structured CuO microspheres

A monodisperse, microsphere technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems that have not been reported before, and achieve a product that is easy to operate, easy to operate, and has a uniform appearance. Effect

Inactive Publication Date: 2017-03-15
HUAIBEI NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there has been no report on related technologies, and by using a simple, green solvent for solvothermal preparation of CuO microsphere precursors with a monodisperse yolk-shell structure combined with a simple annealing method to obtain monodisperse yolk CuO microspheres with -shell structure have never been reported

Method used

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  • Preparation method of monodisperse yolk-shell structured CuO microspheres
  • Preparation method of monodisperse yolk-shell structured CuO microspheres
  • Preparation method of monodisperse yolk-shell structured CuO microspheres

Examples

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Embodiment 1

[0028] A preparation method of monodisperse yolk-shell structure CuO microspheres, comprising the following steps:

[0029] (1) Accurately weigh 0.242g of copper acetate (Cu(CH 3 COO) 2 ·H 2 0), it is dispersed in the container that ethylene glycol is housed, fully dissolves under the effect of magnetic stirring, forms clear transparent blue solution;

[0030] (2) Transfer the clear and transparent blue solution obtained in step (1) to an autoclave, and heat and react at a constant temperature of 180° C. for 1 h;

[0031] (3) After the reaction is finished, cool to room temperature, remove the supernatant after settling, and obtain a blue solid product after suction filtration;

[0032] (4) drying the blue solid product obtained in step (3) in a vacuum drying oven at 40-60° C. to constant weight to obtain a CuO microsphere precursor with a monodisperse yolk-shell structure for use;

[0033] (5) Using a resistance furnace with a controllable heating rate, heat the product o...

Embodiment 2

[0035] A preparation method of monodisperse yolk-shell structure CuO microspheres, comprising the following steps:

[0036] (1) Accurately weigh 0.242g of copper acetate (Cu(CH 3 COO) 2 ·H 2 (2) and 0.1g, 0.2g, 0.3g or 0.4g polyvinylpyrrolidone (PVP), it is dispersed in the container that ethylene glycol is housed, fully dissolves under the effect of magnetic stirring, forms clear transparent blue solution;

[0037] (2) Transfer the clear and transparent blue solution obtained in step (1) to an autoclave, and heat the reaction at a constant temperature of 140° C. for 1 hour or 3 hours;

[0038] (3) After the reaction is finished, cool to room temperature, remove the supernatant after settling, and obtain a blue solid product after suction filtration;

[0039] (4) drying the blue solid product obtained in step (3) in a vacuum drying oven at 40-60° C. to constant weight to obtain a CuO microsphere precursor with a monodisperse yolk-shell structure for use;

[0040] (5) Using...

Embodiment 3

[0042] A preparation method of monodisperse yolk-shell structure CuO microspheres, comprising the following steps:

[0043] (1) Accurately weigh 0.242g of copper acetate (Cu(CH 3 COO) 2 ·H 2 (2) and 0.1g, 0.2g, 0.3g or 0.4g polyvinylpyrrolidone (PVP), it is dispersed in the container that ethylene glycol is housed, fully dissolves under the effect of magnetic stirring, forms clear transparent blue solution;

[0044] (2) Transfer the clear and transparent blue solution obtained in step (1) to an autoclave, and heat the reaction at a constant temperature of 160° C. for 1 hour or 3 hours;

[0045] (3) After the reaction is finished, cool to room temperature, remove the supernatant after settling, and obtain a blue solid product after suction filtration;

[0046] (4) drying the blue solid product obtained in step (3) in a vacuum drying oven at 40-60° C. to constant weight to obtain a CuO microsphere precursor with a monodisperse yolk-shell structure for use;

[0047] (5) Using a...

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Abstract

The invention discloses a preparation method of monodisperse yolk-shell structured CuO microspheres. The method comprises the following steps: dispersing cupric acetate or cupric acetate and PVP in ethylene glycol, fully dissolving the cupric acetate or cupric acetate and PVP, transferring the above obtained solution into a high-pressure reaction kettle, carrying out a constant-temperature heating reaction, naturally cooling and settling a solution obtained after the reaction ends, removing the obtained supernatant, carrying out suction filtration to obtain a blue solid product, and drying the blue solid product in a vacuum drying box until the weight is constant in order to obtain a yolk-shell structured CuO microsphere precursor with monodisperse characteristic; and carrying out controlled temperature annealing on the obtained precursor in air atmosphere by using a heating rate-controllable electric resistance furnace, and cooling the annealed precursor to room temperature in order to obtain the monodisperse yolk-shell structured CuO microspheres. The method ingeniously using ethylene glycol as an organic solvent and a structure guiding agent realizes controllable design of the structure, and also has the advantages of easily available raw materials, low cost, almost no pollution to environment, realization of easy separation, high purity and good and uniform morphology of the above product, simple preparation process, and easiness in operation, and the product has substantially better photochemical performance than other structures.

Description

technical field [0001] The invention relates to a method for preparing an inorganic functional micro-nano structure material, in particular to a method for preparing CuO microspheres with a monodisperse yolk-shell structure. Background technique [0002] CuO is a p-type narrow-band semiconductor with a band gap of about 1.2 eV. It has potential applications in many fields, such as sensors, high-performance electrochemical capacitors, anode materials for lithium-ion batteries, catalysis and photocatalysts, and solar cells. In recent years, due to the excellent properties of micro / nano CuO materials with different sizes and morphologies, more and more material science researchers have attracted attention. [0003] At present, many research groups have developed many methods to controllably prepare CuO micro / nanomaterials with specific structures and morphologies for these fields, and achieved good results. For example, using surfactants to prepare copper oxide nanoflowers wit...

Claims

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Application Information

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IPC IPC(8): C01G3/02B01J23/72
CPCC01G3/02B01J23/72C01P2004/34C01P2004/03C01P2004/04C01P2002/72C01P2004/61B01J35/397B01J35/39
Inventor 张永兴蒋波赵园园李飞李汗周祥博
Owner HUAIBEI NORMAL UNIVERSITY
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