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Preparation method of solid or hollow Cu4O3 microballoons

A microsphere and micro-nano technology, which is applied in the field of preparation of Cu4O3 microspheres, can solve the problems of unseen and unstable structure, and achieve the effects of fast reaction, convenient operation and easy large-scale production.

Active Publication Date: 2014-01-15
JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In the prior art, solvothermal reaction is mainly used for the preparation of metastable phase substances, for Cu 4 o 3 This kind of metastable substance whose structure is unstable due to the simultaneous presence of Cu(I) and Cu(II) has not been reported by any solvothermal reaction.

Method used

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  • Preparation method of solid or hollow Cu4O3 microballoons
  • Preparation method of solid or hollow Cu4O3 microballoons
  • Preparation method of solid or hollow Cu4O3 microballoons

Examples

Experimental program
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Effect test

Embodiment 1

[0038] Weigh 0.4g Cu(NO 3 ) 2 ·3H 2 O, dissolved in 30ml of methanol-N,N-dimethylformamide mixed solution, methanol accounted for 10% of the volume of the mixed solvent, placed in a 100ml lined polytetrafluoroethylene reactor at 160 ° C for 15h, the reaction ended Afterwards, the product was filtered, washed five times with water and absolute ethanol, and dried in a vacuum oven at 60°C for 8 hours.

[0039] Cu prepared above 4 o 3 The materials were tested by XRD on the X’Pert PRO MPD multifunctional X-ray diffractometer produced by Panalytical Company (Panalytical) in the Netherlands.

[0040] Cu prepared above 4 o 3 The surface morphology of the materials was observed with a JSM6700 field emission scanning electron microscope produced by Japan Electronics Corporation.

[0041] Cu prepared above 4 o 3 Materials The particle information was observed with a JEM-2100 lanthanum hexaboride transmission electron microscope produced by Japan Electronics Corporation.

[004...

Embodiment 2

[0046] Weigh 1.5g Cu(NO 3 ) 2 ·3H 2 O, be dissolved in the ethanol-N-methylformamide mixed solution of 50ml, the volume ratio that ethanol accounts for mixed solvent is 20%, is placed in the 100ml lining enamel reaction kettle 200 ℃ of reaction 10h, after the reaction finishes, the product is filtered, Wash with water and absolute ethanol 5 times each, and dry in a vacuum oven at 60°C for 8 hours.

[0047] Figure 4 a is the Cu obtained in Example 2 4 o 3 XRD pattern of the material, b is pure Cu 4 o 3 The standard card (JCPDS49-1830), as can be seen from the figure, the prepared product is completely consistent with the standard card. It can be seen that the material synthesized by this method is pure Cu 4 o 3 .

[0048] Figure 5 For the Cu obtained in Example 2 4 o 3 The SEM image of the material, it can be seen from the figure that the synthesized Cu 4 o 3 The particles of the material are spherical, and the particle size is about 500nm-1μm.

[0049] Figur...

Embodiment 3

[0051] Weigh 3g Cu(NO 3 ) 2 ·3H 2 O, dissolved in 75ml of propanol-N, N-methylformamide mixed solution, propanol accounted for 50% of the volume ratio of the mixed solvent, placed in a 100ml lined polytetrafluoroethylene reactor at 250 ° C for 2h, After the reaction, the product was filtered, washed five times with water and absolute ethanol, and dried in a vacuum oven at 60° C. for 8 hours. The prepared product is hollow spherical Cu 4 o 3 Material, the particle size is about 500nm-1μm.

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Abstract

The invention discloses a preparation method of solid or hollow Cu4O3 microballoons by a solvothermal technology. The preparation method comprises the following steps that 1, at least one copper salt is dissolved in a mixed solvent containing an alcohol and at least one amide to form a solution with copper ion concentration of 0.05 to 0.2M; and 2, the prepared solution is transferred into a reactor to undergo a reaction at a temperature of 100 to 250 DEG C for 2 to 20 hours to produce black precipitates and the black precipitates are dried to form Cu4O3 microballoons. The Cu4O3 microballoons prepared by the preparation method are solid or hollow, wherein the solid Cu4O3 microballoons have particle sizes of 2 to 5 micrometers and the hollow Cu4O3 microballoons have particle sizes of 500 nanometers to 2 micrometers. The preparation has a simple technical route, convenient operation processes and a fast reaction rate, does not need any complicated experimental equipment, and is easy for large-scale production.

Description

technical field [0001] The present invention relates to a Cu 4 o 3 Preparation method of microspheres, in particular to a solid or hollow Cu 4 o 3 Preparation method of microspheres. Solid or hollow Cu prepared by the present invention 4 o 3 Microspheres can be used in catalytic reactions, photocatalysis, and electrode materials for lithium-ion batteries. Background technique [0002] Micro-copper oxide and nano-copper oxide materials have good catalytic and electrode activity, and have been one of the focuses of research because of their superior physical and chemical properties. Micro-nano copper oxide and cuprous oxide, as multifunctional fine inorganic materials, have a very wide range of uses in industrial production, such as in catalysis, photolysis, electromagnetic materials and other functional materials. [0003] In addition to copper oxide and cuprous oxide, which have been widely used, copper oxide also has an oxide: Cu 4 o 3 . Cu 4 o 3 It was first di...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G3/02
Inventor 苏发兵赵丽润车红卫王莹利翟世辉
Owner JIANGXI INST OF RARE EARTHS CHINESE ACAD OF SCI
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