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Preparation method of micron-scale flower-like combined metal oxide

A composite metal, micron-scale technology, applied in chemical instruments and methods, single crystal growth, polycrystalline material growth and other directions, can solve problems such as reports that have not yet appeared

Active Publication Date: 2012-05-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there have been no reports on the controllable synthesis of spinel composite metal oxide flowers.

Method used

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  • Preparation method of micron-scale flower-like combined metal oxide
  • Preparation method of micron-scale flower-like combined metal oxide
  • Preparation method of micron-scale flower-like combined metal oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0022] According to the technical solution of the present invention, 0.356g of 50% wt. manganese nitrate aqueous solution and 0.146g of cobalt nitrate were added to 42mL of ethylene glycol under magnetic stirring at room temperature, and magnetic stirring was used to form a uniform solution. Add 11.9g of polyvinylpyrrolidone to the homogeneous solution, and stir the solution until it becomes transparent. Add 2.93 g of sodium acetate, and stir for 3 hours. Then put it into a closed container (60 mL) for solvothermal reaction, and react at 200° C. for 2 hours. After cooling to room temperature, washing with deionized water and absolute ethanol, drying in a vacuum oven at 50° C. for 6 hours, the product can be obtained as a micron-sized flower-shaped composite metal basic carbonate. The product is put into a reaction furnace and calcined at 350° C. for 2 hours to prepare a micron-sized flower-shaped composite metal oxide. The morphology of the product is detected by a scanning ...

Embodiment 2

[0024] According to the technical solution of the present invention, 0.356g of 50% wt. manganese nitrate aqueous solution and 0.291g of cobalt nitrate were added to 42mL of ethylene glycol under magnetic stirring at room temperature, and magnetic stirring was used to form a uniform solution. Add 5.9g of polyvinylpyrrolidone to the homogeneous solution, and stir the solution until it becomes transparent. 0 g of sodium acetate was added and stirred for 1 hour. Then put it into a closed container (60 mL) for solvothermal reaction, and react at 120° C. for 24 hours. After cooling to room temperature, washing with deionized water and absolute ethanol, drying in a vacuum oven at 50° C. for 6 hours, the product can be obtained as a micron-sized flower-shaped composite metal basic carbonate. The product is put into a reaction furnace and calcined at 300° C. for 4 hours to prepare a micron-sized flower-shaped composite metal oxide. The appearance of the product is detected by a scann...

Embodiment 3

[0026] According to the technical solution of the present invention, 0.353g of manganese chloride and 0.249g of nickel acetate are respectively added to 32mL of ethylene glycol at room temperature, and magnetically stirred to form a uniform solution. Add 11.9g of polyvinylpyrrolidone to the homogeneous solution, and stir the solution until it becomes transparent. Add 2.93 g of sodium acetate, and stir for 3 hours. Then put it into a closed container (60 mL) for solvothermal reaction, and react at 200° C. for 2 hours. After cooling to room temperature, washing with deionized water and absolute ethanol, drying in a vacuum oven at 50° C. for 6 hours, the product can be obtained as a micron-sized flower-shaped composite metal basic carbonate. The product is put into a reaction furnace and calcined at 400° C. for 5 hours to prepare a micron-sized flower-shaped composite metal oxide. The morphology of the product is detected by a scanning electron microscope: flowers with a diamet...

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Abstract

The invention discloses a preparation method of a micron-scale flower-like composite metal oxide, relating to a solvent thermosynthesis method of a spinel composite oxide micron flower material. The preparation method comprises the following steps of: with a metal salt as a raw material and glycol as a solvent, adding a surfactant and sodium acetate, and carrying out solvent thermal reaction in a closed container under the condition of 120-220 DEG C to form the micron-scale flower-like composite metal subcarbonate; and with the subcarbonate as a precursor, controlling a temperature rise speed and heating to 300-700 DEG C, and annealing to prepare the corresponding composite metal oxide micron-scale flowers. The preparation method disclosed by the invention has the advantages of simple process, low cost, stable product quality, easiness in control and good process repeatability and can be widely applied to the fields, such as lithium ion batteries, catalysis and the like.

Description

technical field [0001] The invention relates to a preparation method of a micron-scale flower-shaped composite metal oxide, in particular to a preparation method of a micron-scale flower-shaped composite metal oxide with a spinel structure. The morphology control of spinel oxides is a frontier topic in international nanomaterials research, especially the morphology control of spinel composite oxides has not yet been realized. Background technique [0002] Among the existing synthesis methods with controllable morphology of spinel oxides, most of them can only control the morphology of single metal oxides. At present, the research on the synthesis of spinel multi-metal oxides at home and abroad mainly focuses on the magnetic iron-containing oxides and bimetallic types. L.S.Zhong et al. reported in "Advanced Materials" 2006, Volume 18, page 2426 that the self-assembled three-dimensional flower-like nanostructure of iron oxide has a good effect in sewage treatment. D.H.Zhang ...

Claims

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Application Information

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IPC IPC(8): C30B29/22C30B29/60
Inventor 杨维慎刘焕英朱雪峰丛铀
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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