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Method for preparing copper sulfide film with microwave hydrothermal assisted sol-gel method

A sol-gel method, microwave hydrothermal technology, applied in copper sulfide and other directions, can solve problems such as environmental pollution, long reaction time of experimental conditions, etc., and achieve the effects of environmental friendliness, low cost, and simple operation

Active Publication Date: 2013-08-14
磊菱半导体设备(江苏)有限公司
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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 certain pollution to the environment

Method used

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  • Method for preparing copper sulfide film with microwave hydrothermal assisted sol-gel method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Soak the glass substrate in dilute hydrochloric acid, use ultrasonic vibration for 30 minutes, wash it with distilled water, then place the substrate in a mixed solution of concentrated sulfuric acid, hydrogen peroxide and deionized water for activation treatment, let it stand for 24 hours, take it out and use Wash with distilled water and absolute ethanol separately, then place in absolute ethanol, and set aside;

[0019] Wherein the volume ratio of concentrated sulfuric acid, hydrogen peroxide and deionized water is 1:1:1;

[0020] 2) Analytical pure copper acetate (Cu(CH 3 COO) 2 ·H 2 O) join in ethanol, make the transparent solution that cupric acetate concentration is 0.006mol / L, and add the triethanolamine (C 2 h 7 NO) as a stabilizer, and then refluxed in a water bath at 60°C for 2 hours to form a uniform transparent sol, and then aged at room temperature for 8 hours to obtain Sol A;

[0021] 3) Blow dry the glass substrate treated in step 1) with nitroge...

Embodiment 2

[0028] 1) Soak the glass substrate in dilute hydrochloric acid, use ultrasonic vibration for 60 minutes, wash it with distilled water, then place the substrate in a mixed solution of concentrated sulfuric acid, hydrogen peroxide and deionized water for activation treatment, let it stand for 48 hours, take it out and use Wash with distilled water and absolute ethanol separately, then place in absolute ethanol, and set aside;

[0029] Wherein the volume ratio of concentrated sulfuric acid, hydrogen peroxide and deionized water is 1:1:1;

[0030] 2) Analytical pure copper acetate (Cu(CH 3 COO) 2 ·H 2 O) join in ethanol, make the transparent solution that cupric acetate concentration is 0.05mol / L, and add the triethanolamine (C 2 h 7 NO) as a stabilizer, and then refluxed in a water bath at 60°C for 3 hours to form a uniform transparent sol, which was then aged at room temperature for 10 hours to obtain Sol A;

[0031] 3) Blow dry the glass substrate treated in step 1) with n...

Embodiment 3

[0037]1) Soak the glass substrate in dilute hydrochloric acid, use ultrasonic vibration for 50 minutes, wash it with distilled water, then place the substrate in a mixed solution of concentrated sulfuric acid, hydrogen peroxide and deionized water for activation treatment, let it stand for 72 hours, take it out and use Wash with distilled water and absolute ethanol separately, then place in absolute ethanol, and set aside;

[0038] Wherein the volume ratio of concentrated sulfuric acid, hydrogen peroxide and deionized water is 1:1:1;

[0039] 2) Analytical pure copper acetate (Cu(CH 3 COO) 2 ·H 2 (0) join in ethanol, make the transparent solution that cupric acetate concentration is 0.003mol / L, and add the triethanolamine (C 2 h 7 NO) as a stabilizer, and then refluxed in a water bath at 60°C for 5 hours to form a uniform transparent sol, which was then aged at room temperature for 24 hours to obtain Sol A;

[0040] 3) Blow dry the glass substrate treated in step 1) with ...

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Abstract

The invention discloses a method for preparing a copper sulfide film with a microwave hydrothermal assisted sol-gel method. The method comprises the following steps of: successively soaking a glass substrate in diluted hydrochloric acid, concentrated sulfuric acid and a mixed solution of hydrogen peroxide and deionized water for activation treatment, adding cupric acetate in ethanol, and then adding triethanolamine to obtain sol A; soaking the activated glass substrate into the sol A, carrying out film coating on the activated glass substrate with an average-rate pulling method, and drying the substrate subjected to film coating; adding thioacetamide or thiourea in the deionized water to obtain a solution D; and transferring the solution D into a microwave hydrothermal reaction kettle, sealing and then putting the reaction kettle in a temperature-pressure double-control microwave hydrothermal reaction instrument and then reacting by selecting a temperature control mode, washing with the deionized water and absolute ethyl alcohol after the reaction is finished, and then drying in vacuum to obtain the copper sulfide film. According to the invention, the copper sulfide film is prepared by using the microwave hydrothermal assisted sol-gel method, thus the advantages of the two methods are sufficiently bonded; and the prepared film is uniform and compact, and is strong in bonding force, high in crystallization degree, low in defect and good in property.

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 by a microwave hydrothermal assisted sol-gel method. Background technique [0002] In recent years, due to the excellent physical and chemical properties of transition metal sulfides, such as their potential application value in semiconductors, light-emitting devices, and superconductivity, they have attracted great interest from researchers. CuS is a very important p-type semiconductor with a band gap of 2.0eV. 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 on structural, optical and electrical properties of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C17/22C01G3/12
Inventor 黄剑锋齐慧张培培曹丽云吴建鹏
Owner 磊菱半导体设备(江苏)有限公司