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Preparation method of spherical copper sulphide (CuS) particles

A technology of copper sulfide and particles, which is applied in the direction of copper sulfide, can solve the problems of high energy consumption, environmental pollution, long reaction time, etc., and achieve the effect of low energy consumption, short reaction cycle and uniform size

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, long reaction time, high energy consumption, 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 spherical copper sulphide (CuS) particles
  • Preparation method of spherical copper sulphide (CuS) particles

Examples

Experimental program
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Embodiment 1

[0016] 1) Analytical pure copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O) join in the mixed solvent of deionized water and ethylene glycol, make Cu 2+ A transparent solution A with a concentration of 0.07mol / L, wherein the volume ratio of ethylene glycol to deionized water is 1:2.5;

[0017] 2) Add analytically pure thiourea (SC(NH 2 ) 2 ), so that Cu in the solution 2+ / SC(NH 2 ) 2 The molar ratio is 1:0.8, the resulting solution B;

[0018] 3) Add analytically pure polyvinylpyrrolidone K30 (PVP) to solution B, so that the concentration of PVP in the solution is 0.004g / mL to form precursor solution C;

[0019] 4) Pour the precursor solution C into a microwave hydrothermal reactor with a filling degree of 60%, then seal the reactor, put it into a microwave hydrothermal reactor with dual temperature and pressure controls, and select the temperature control mode at 240°C. React for 40min, and naturally cool to room temperature after the reaction;

[0020] 5) Open the h...

Embodiment 2

[0023] 1) Analytical pure copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O) join in the mixed solvent of deionized water and ethylene glycol, make Cu 2+ A transparent solution A with a concentration of 0.06mol / L, wherein the volume ratio of ethylene glycol to deionized water is 1:3;

[0024] 2) Add analytically pure thiourea (SC(NH 2 ) 2 ), so that Cu in the solution 2+ / SC(NH 2 ) 2 The molar ratio is 1: 1, the resulting solution B;

[0025] 3) Add analytically pure polyvinylpyrrolidone K30 (PVP) to solution B, so that the concentration of PVP in the solution is 0.008g / mL to form precursor solution C;

[0026] 4) Pour the precursor solution C into a microwave hydrothermal reactor with a filling degree of 70%, then seal the reactor, put it into a microwave hydrothermal reactor with temperature and pressure dual control, select the temperature control mode at 150°C, React for 80 minutes, and cool to room temperature naturally after the reaction;

[0027] 5) Turn on the h...

Embodiment 3

[0029] 1) Analytical pure copper nitrate trihydrate (Cu(NO 3 ) 2 ·3H 2 O) join in the mixed solvent of deionized water and ethylene glycol, make Cu 2+ A transparent solution A with a concentration of 0.12mol / L, wherein the volume ratio of ethylene glycol to deionized water is 1:4;

[0030] 2) Add analytically pure thiourea (SC(NH 2 ) 2 ), so that Cu in the solution 2+ / SC(NH 2 ) 2 The molar ratio of is 1: 2.5, resulting solution B;

[0031] 3) Add analytically pure polyvinylpyrrolidone K30 (PVP) to solution B, so that the concentration of PVP in the solution is 0.012g / mL to form precursor solution C;

[0032] 4) Pour the precursor 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 dual temperature and pressure controls, and select the temperature control mode at 170°C. React for 60 minutes, and naturally cool to room temperature after the reaction;

[0033]5) Turn on ...

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Abstract

The invention relates to a preparation method of spherical (CuS) particles. The preparation method comprises the steps that: copper nitric acid trihydrate is added into a mixed solvent consisting of de-ionized water and ethylene glycol to obtain solution A; thiourea is added into the solution A to obtain solution B; polyvinylpyrrolidone K30 is added into the solution B to form precursor solution C; the precursor 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 spherical CuS particles 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. The prepared CuS particles have regular sphere shapes and uniform size.

Description

technical field [0001] The invention belongs to a method for preparing semiconductor material copper sulfide, in particular to a method for preparing spherical copper sulfide particles. Background technique [0002] In the field of material synthesis, sulfides are widely interested and focused by researchers because of their potential application value 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 recording, solar cells, sensors, and catalysis. So far, copper sulfide with various morphologies has been successfully synthesized, such as nanodisk , Hollow spherical and flower-like and other specific shapes. [0003] At present, the methods for preparing copper sulfide mainly include pyrolysis [Yu-Biao Chen, Ling Chen, and Li-Ming Wu. Water-Induced Thermolytic Formation of H...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/12
Inventor 黄剑锋齐慧曹丽云刘佳吴建鹏
Owner SHAANXI UNIV OF SCI & TECH
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