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Preparation method of copper sulfide thin film with x-shaped-flaky crystal crossing structure

A flake crystal, copper sulfide technology, applied in chemical instruments and methods, single crystal growth, crystal growth and other directions, can solve the problems of environmental pollution, long reaction time of experimental conditions, etc., and achieves easy availability of raw materials, uniform film morphology, The effect of short response times

Active Publication Date: 2014-08-27
吴文婕
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 certain pollution to the environment

Method used

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  • Preparation method of copper sulfide thin film with x-shaped-flaky crystal crossing structure
  • Preparation method of copper sulfide thin film with x-shaped-flaky crystal crossing structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Soak the glass substrate in dilute hydrochloric acid, use ultrasonic vibration for 30 minutes, wash it with distilled water three times, then place the substrate in a mixed solution of concentrated sulfuric acid, hydrogen peroxide and deionized water, let it stand for 24 hours, take it out and wash it with distilled water and dry Washed with water and ethanol, and then washed with N 2 Blow dry and place for later use; wherein the volume ratio of concentrated sulfuric acid, hydrogen peroxide and deionized water is 1:1:1;

[0021] 2) Analytical pure copper nitrate trihydrate Cu(NO 3 ) 2 ·3H 2 O was added to deionized water to make Cu 2+ A transparent solution with a concentration of 0.003mol / L, and then add ethylenediaminetetraacetic acid (EDTA), so that [Cu 2+ ]:[EDTA]=5:1 to obtain solution A;

[0022] 3) Add analytically pure thiourea (SC(NH 2 ) 2 ), making the solution SC(NH 2 ) 2 The concentration is 0.018mol / L to obtain solution B;

[0023] 4) Add ammon...

Embodiment 2

[0029] 1) Soak the glass substrate in dilute hydrochloric acid, use ultrasonic vibration for 45 minutes, wash it with distilled water three times, then place the substrate in a mixed solution of concentrated sulfuric acid, hydrogen peroxide and deionized water, let it stand for 48 hours, take it out and wash it with distilled water and dry Wash with water and ethanol separately, then blow dry with N2, and place it for later use; wherein the volume ratio of concentrated sulfuric acid, hydrogen peroxide and deionized water is 1:1:1;

[0030] 2) Add analytically pure copper acetate to deionized water to make Cu 2+ A transparent solution with a concentration of 0.006mol / L, and then add ethylenediaminetetraacetic acid (EDTA), so that [Cu 2+ ]:[EDTA]=10:1 to obtain solution A;

[0031] 3) Add analytically pure thioacetamide (H 3 CCSNH 2 ), so that the solution H 3 CCSNH 2 The concentration is 0.36mol / L to obtain solution B;

[0032] 4) Add ammonia water (NH 3 ·H 2 O), adjust...

Embodiment 3

[0037] 1) Soak the glass substrate in dilute hydrochloric acid, use ultrasonic vibration for 60 minutes, wash with distilled water three times, then place the substrate in a mixed solution of concentrated sulfuric acid, hydrogen peroxide and deionized water, let it stand for 72 hours, take it out and wash it with distilled water and dry Washed with water and ethanol, and then washed with N 2 Blow dry and place for later use; wherein the volume ratio of concentrated sulfuric acid, hydrogen peroxide and deionized water is 1:1:1;

[0038] 2) Analytical pure copper nitrate trihydrate Cu(NO 3 ) 2 ·3H 2 O was added to deionized water to make Cu 2+ A transparent solution with a concentration of 0.012mol / L, and then add ethylenediaminetetraacetic acid (EDTA), so that [Cu 2+ ]:[EDTA]=8:1, to obtain solution A;

[0039] 3) Add analytically pure thiourea (SC(NH 2 ) 2 ), making the solution SC(NH 2 ) 2 The concentration is 0.06mol / L to obtain solution B;

[0040] 4) Add ammonia ...

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Abstract

The invention relates to a preparation method of a copper sulfide thin film with an x-shaped-flaky crystal crossing structure, which comprises the following steps of: adding analytically-pure soluble copper salt into deionized water and adding ethylene diamine tetraacetic acid to obtain solution A; adding thiourea into the solution A to obtain solution B; adding ammonia water into the solution B to form precursor solution C; and pouring the precursor solution C into a microwave hydrothermal reaction kettle, vertically putting a treated glass substrate into the reaction vessel, putting the sealed glass substrate into a temperature and pressure double-control microwave hydrothermal reaction instrument, selecting a temperature control mode for reaction, taking out the substrate after the end of reaction, transferring NaOH solution into the microwave hydrothermal reaction instrument, taking out the substrate after secondary crystallization and vacuum-drying to obtain a final product, i.e. the copper sulfide thin film with the x-shaped flaky crystal cross structure. The preparation method has the beneficial effects that the preparation method adopts a secondary microwave hydrothermal process and is short in reaction period and low in energy consumption; the prepared thin film has the advantages of uniform shape, compact structure, high crystalline degree and fewer defects; and adopted raw materials are easily obtained and are low in cost.

Description

technical field [0001] The invention belongs to a method for preparing a copper sulfide film, in particular to a method for preparing a copper sulfide film with an X-shaped-flaky crystal cross structure. 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. [0003] At present, the method for preparing sulfide thin films mainly contains the continuous ion layer adsorption reaction method [M. Ali Yildirim, Aytunc Ates, Aykut Astam.Annealing and light effect onstructural, optical and electrical properties of CuS, CuZnS and ZnS thinfilms grown by the SILAR method [J].Physica.E, 2009, 41:1365-1372.], chemic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/36C30B7/10
Inventor 黄剑锋齐慧张培培曹丽云吴建鹏
Owner 吴文婕