Chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at low temperature

A nanocrystalline and sheet-like technology, applied in the fields of nanotechnology, nanotechnology, nanostructure manufacturing, etc., can solve the problems of high solvent toxicity, impure products, complicated processes, etc., and achieve convenient operation, uniform appearance and good repeatability. Effect

Inactive Publication Date: 2010-08-04
XUCHANG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The problem to be solved by the present invention is: overcome the current preparation of Cu x S y In the method of x:y=1~2 crystals, there are disadvantages such as dependence on reaction vessel and surfactant, high energy consumption, high toxicity of solvent, impure product, complicated process, etc.

Method used

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  • Chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at low temperature
  • Chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at low temperature
  • Chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at low temperature

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 1. Preparation: Flatten the analytically pure metal copper foil and put it into a beaker filled with dilute hydrochloric acid (concentrated hydrochloric acid and deionized water, volume ratio 1:201 and absolute ethanol solution, and clean it with an ultrasonic cleaner for 3 minutes. Soak in N,N-2 methylformamide for later use; wash the glass bottle (capacity 10ml) with tap water, distilled water, and absolute ethanol in sequence, and dry it for later use;

[0045] 2. Reaction steps: Weigh 0.01g of sulfur powder and put it in the glass bottle (capacity 10ml) prepared in step 1, then fill it with 8ml of N, N-dimethylformamide, keep the temperature in an ice-water bath for 1 hour, and then put the sulfur powder Pour it to the bottom side of the glass bottle, put the metal copper foil treated in step 1 into the glass bottle horizontally, avoid direct contact with sulfur powder, put the glass bottle in an ice-water bath to react in a stable place, and react at 0°C 18 hours; ...

Embodiment 2

[0048] 1, preparatory work: with embodiment 1;

[0049] 2. Reaction steps: Weigh 0.01g of sulfur powder and put it in the glass bottle (volume 10ml) prepared in step 1, then fill it with 8ml of N,N-dimethylformamide, keep the temperature in an ice-water bath for 1 hour, and then put the sulfur Pour the powder to the bottom side of the glass bottle, put the metal copper foil treated in step 1 into the glass bottle horizontally, avoid direct contact with the sulfur powder, put the glass bottle in an ice-water bath and react in a stable place, at 0°C Respond for 24 hours;

[0050] 3, aftertreatment: with embodiment 1, obtain Cu 2 S film samples. The color of the product is gray-black, and the microstructure under the scanning electron microscope is a large-area flaky nanocrystal with a uniform and flat surface. Scanning electron micrographs see diagram 2-1 , XRD pattern see Figure 2-2 .

Embodiment 3

[0052] 1, preparatory work: with embodiment 1;

[0053] 2. Reaction steps: Weigh 0.01g of sulfur powder and put it in the glass bottle (capacity 10ml) prepared in step 1, then fill it with 8ml of N,N-dimethylformamide, place it at 20°C for 1 hour, then put Pour the sulfur powder to the bottom side of the glass bottle, put the metal copper foil treated in step 1 into the glass bottle horizontally, avoid direct contact with the sulfur powder, place the glass bottle in a stable place for reaction, and react at 20°C for 8 hours ;

[0054] 3, aftertreatment: with embodiment 1, obtain Cu 8 S 9 and Cu 2 S two-phase mixed nanocrystalline film sample. The color of the product is blue-black, and the microstructure under the scanning electron microscope is a large-area flaky nanocrystal with a uniform and flat surface. Scanning electron micrographs see Figure 3-1 , XRD pattern see Figure 3-2 .

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Abstract

The invention provides a chemical method for synthesizing flaky CuxSy nanocrystalline optoelectronic film controllably at a low temperature. The method comprises the following steps: firstly adding sulfur powder in a container, secondly adding organic solvent N,N-dimethylformamide or absolute alcohol, wherein the volume of organic solvent is more than a half of the capacity of the container; standing at 0-60 DEG C for 1h to ensure that the sulfur powder dissolved in organic solvent is saturated, horizontally placing substrate material with a new and clean metal copper surface on the bottom of the container to avoid directly contacting with sulfur powder, reacting at 0-60 DEG C for 5-24h, cleaning the product with absolute alcohol, drying at room temperature to in-situ prepare the big area film material composed of flaky CuxSy nanocrystalline on the metal copper surface of the substrate material, wherein x:y=1-2. The method of the invention adopts low temperature, has low energy consumption, is simple, green and environmentally friendly and particularly applicable to large-area industrial production, and does not use any template, add any surfactant and perform complicated post-processing operations such as purification.

Description

Technical field: [0001] The invention belongs to the technical field of material chemistry, and in particular relates to a large-area synthesis of sheet-like Cu at low temperature. x S y A chemical method for x:y=1-2 nanocrystalline photoelectric thin film materials. Background technique: [0002] Copper sulfide (Cu x S y x:y=1~2) is an important binary compound, and this compound is well known because of its many non-uniform combinations and heterogeneous mixing states. Now there are at least 5 kinds of copper sulfides that are stable at room temperature. The sulfur-rich phase is: copper blue (CuS); the copper-rich phase is: orthorhombic blue chalcocite (Cu 1.75 S), blue chalcocite (Cu 1.8 S), chalcocite (Cu 1.95 S) and chalcocite (Cu 2 S). There are now more than 21 kinds of copper sulfides synthesized, including CuS, Cu 1.96 S, Cu 7 S 4 , Cu 9 S 5 , Cu 2 S and so on. At present, this type of thin film material is an important optoelectronic semiconductor ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/12B82B3/00
Inventor 郑直雷岩贾会敏李大鹏陈秋霞黄保军李品将张艳鸽杨风岭
Owner XUCHANG UNIV
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