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Preparation method of annular self assembled copper sulfide hollow spheres

A self-assembly, copper sulfide technology, applied in copper sulfide and other directions, can solve the problems of long reaction time and environmental pollution in experimental conditions, and achieve the effects of improving reaction rate, large reaction area and low energy consumption

Inactive Publication Date: 2012-06-20
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods usually require special instruments, or require strict experimental conditions and relatively long reaction times, and because there is a large amount of H in the process of synthesizing copper sulfide 2 S gas generation, if the reaction is carried out in an open system, it will inevitably cause some pollution to the environment

Method used

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  • Preparation method of annular self assembled copper sulfide hollow spheres
  • Preparation method of annular self assembled copper sulfide hollow spheres
  • Preparation method of annular self assembled copper sulfide hollow spheres

Examples

Experimental program
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Embodiment 1

[0017] 1) Analytical pure copper nitrate trihydrate Cu(NO 3 ) 2 ·3H 2 O was added to deionized water to make Cu 2+ A transparent solution A with a concentration of 0.04mol / L;

[0018] 2) Add analytically pure polyvinylpyrrolidone K30 (PVP) to solution A, the concentration of PVP is 0.02mol / L, to form a precursor solution, and let it stand for 12 hours to obtain solution B;

[0019] 3) Add analytically pure thiourea (SC(NH 2 ) 2 ), so that the mol ratio of the copper source / sulfur source in the solution is 1: 3, the resulting solution C;

[0020] 4) Pour solution C into a microwave hydrothermal reaction kettle with a filling degree of 50%, then seal the reaction kettle, put it into a microwave hydrothermal reaction instrument with dual temperature and pressure control, select the temperature control mode at 180°C, and react for 10 minutes , naturally cool to room temperature after the reaction;

[0021] 5) Open the hydrothermal reaction kettle, collect the product by cen...

Embodiment 2

[0024] 1) Analytical pure copper sulfate pentahydrate (CuSO 4 ·5H 2 O) added to deionized water to make Cu 2+ A transparent solution A with a concentration of 0.15mol / L;

[0025] 2) Add analytically pure polyvinylpyrrolidone K30 (PVP) to solution A to form a precursor solution, wherein the concentration of PVP is 0.03mol / L, and stand for 12 hours to obtain solution B;

[0026] 3) Add analytically pure sodium thiosulfate (Na 2 S 2 (03), so that the mol ratio of the copper source / sulfur source in the solution is 1: 5, the resulting solution C;

[0027] 4) Pour solution C into a microwave hydrothermal reaction kettle with a filling degree of 60%, then seal the reaction kettle, put it into a microwave hydrothermal reaction instrument with dual temperature and pressure control, select the temperature control mode at 150°C, and react for 60 minutes , naturally cool to room temperature after the reaction;

[0028] 5) Open the hydrothermal reaction kettle, collect the product by...

Embodiment 3

[0030] 1) Analytical pure copper nitrate trihydrate Cu(NO 3 ) 2 ·3H 2 O was added to deionized water to make Cu 2+ A transparent solution A with a concentration of 0.48mol / L;

[0031] 2) Add analytically pure polyvinylpyrrolidone K30 (PVP) to solution A, the concentration of PVP is 0.05mol / L to form a precursor solution, and let it stand for 12 hours to obtain solution B;

[0032] 3) Add analytically pure thiourea (SC(NH 2 ) 2 ), so that the mol ratio of the copper source / sulfur source in the solution is 1: 4, the resulting solution C;

[0033] 4) Pour solution C into a microwave hydrothermal reactor with a filling degree of 50%, then seal the reactor, put it into a microwave hydrothermal reactor with temperature and pressure dual control, select the temperature control mode at 100°C, and react for 120 minutes , naturally cool to room temperature after the reaction;

[0034] 5) Open the hydrothermal reaction kettle, collect the product by centrifugation, wash it with de...

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Abstract

The invention relates to a preparation method of annular self assembled copper sulfide hollow spheres. The method comprises the steps that: soluble copper salt is added into de-ionized water to obtain solution A; polyvinylpyrrolidone K30 is added into the solution A to form precursor solution B; thiourea or sodium thiosulfate is added into solution B to obtain solution C; the solution C is poured into a microwave hydrothermal reaction kettle, then, the reaction kettle is sealed and is put into a temperature and pressure dual-control microwave hydrothermal reaction instrument, a temperature control mode or a pressure control mode is selected for reaction, and the solution is naturally cooled to the room temperature after reaction completion; and the hydrothermal reaction kettle is opened, products are respectively washed by the de-ionized water and absolute ethyl alcohol after centrifugal collection, and final products of annular self assembled copper sulfide hollow spheres are obtained after drying. The method has the advantages that a simple microwave hydrothermal method preparation process is adopted, the reaction period is short, the energy consumption is low, the reaction is completed in one step in liquid phases, and the later-period treatment is not needed.

Description

technical field [0001] The invention belongs to a method for preparing copper sulfide, in particular to a method for preparing ring-shaped self-assembled copper sulfide hollow spheres. Background technique [0002] Transition metal sulfides are of great interest to researchers because of their potential applications in semiconductors, light-emitting devices, and superconductivity. CuS is a very important p-type semiconductor with a band gap of 1.2eV. Due to its excellent conductivity, electrical, and optical properties, it is widely used in thermocouples, optical filters, solar cells, sensors, and catalysis. So far, various morphologies of copper sulfide have been successfully synthesized, such as nanodisk, hollow sphere, flower and tube. However, so far, ring-shaped self-assembled CuS hollow spheres have not been reported. [0003] At present, the methods for preparing copper sulfide mainly include pyrolysis [Yu-Biao Chen, Ling Chen, and Li-Ming Wu. Water-Induced Thermol...

Claims

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Application Information

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IPC IPC(8): C01G3/12
Inventor 黄剑锋齐慧曹丽云张培培吴建鹏
Owner SHAANXI UNIV OF SCI & TECH
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