Method for synthesizing copper diselenide nano-crystals in polyhydric alcohol-based solution

A technology of copper diselenide and nanocrystals, which is applied in the field of nanomaterials, can solve problems such as cumbersome processes, harsh reaction conditions, and complex equipment, and achieve the effects of good repeatability, low cost, and stable phase

Inactive Publication Date: 2013-12-25
TIANJIN UNIV
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  • Claims
  • Application Information

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Problems solved by technology

In summary, the solid-state reaction method to prepare CuSe 2 materials, there are many defects such as cumbersome process, complicated equipment, time-consuming and energy-consuming, harsh reaction conditions, difficult to control chemical components, and low product purity, which largely hinder the development of CuSe 2 commercialization of materials

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  • Method for synthesizing copper diselenide nano-crystals in polyhydric alcohol-based solution
  • Method for synthesizing copper diselenide nano-crystals in polyhydric alcohol-based solution
  • Method for synthesizing copper diselenide nano-crystals in polyhydric alcohol-based solution

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Embodiment Construction

[0020] The raw materials used in the present invention are commercially available analytically pure raw materials, and the present invention will be further described below in conjunction with the examples.

[0021] The present invention prepares CuSe in triethylene glycol system 2 The nanoparticle process is as follows:

[0022] (1) Preparation of precursor solution

[0023] Weigh 0.25mmol copper chloride dihydrate (CuCl 2 2H 2 (2), be dissolved in 10ml triethylene glycol, stir at room temperature for 45min to obtain a stable cation source solution; add in 40ml triethylene glycol in a three-neck round-bottomed flask, add selenium powder, then add 0.1g polyvinylpyrrolidone , referred to as PVP; magnetically stirred for 5 minutes to obtain anion source solution; wherein the Cu / Se molar ratios were 1:2, 1:1.9, 1:1.8, 1:1.7, respectively.

[0024] (2) Synthesis of CuSe by reflux reaction 2

[0025] Put the three-necked bottle in a heat pack, inject nitrogen gas into the thr...

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Abstract

The invention discloses a method for synthesizing copper diselenide nano-crystals in a polyhydric alcohol-based solution. The method comprises the following steps of: (1), dissolving weighed 0.25mmol of copper chloride dihydrate into 10ml of triethylene glycol, to obtain a stable positive ion source solution, in addition, adding 40ml of triethylene glycol into a three-necked flask, adding selenium powder, and adding 0.1g of polyvinyl pyrrolidone, to obtain a negative ion source solution, wherein the mol ratio of Cu / Se is 1:2, 1:1.9, 1:1.8 and 1:1.7 respectively; (2), slowly heating the negative ion solution, rapidly injecting the positive ion source solution when the negative ion solution is heated to 210-270 DEG C, and carrying out backflow reaction, so as to synthesize the CuSe2 nano-crystal solution. By adoption of the method, the components of a product can be controlled accurately, the phase is stable, the repeatability is good, the cost is low, the synthesizing temperature is low, and furthermore, the synthesized copper diselenide nano-crystal solution is safe and low in toxicity.

Description

technical field [0001] The present invention relates to nanomaterials, in particular to a method for the synthesis of CuSe in polyol-based solutions 2 nanocrystal approach. Background technique [0002] CuSe 2 It is a typical Cu-Se compound and usually exists in two forms: pyrite (cubic crystal structure) and marcasite (orthorhombic crystal structure). It exhibits superconductivity when it is lower than 2.4k, and can be used as a target for preparing copper indium selenide / copper indium gallium selenide thin film solar cells by sputtering. According to the phase diagram, CuSe 2 Produced by the peritectic reaction between CuSe and a Se-rich liquid phase of defined composition, the reaction temperature is reported to be 340°C, 343°C, 342°C, 332°C, and the accepted representative temperature is 332°C (see D.J.Chakrabarti, et. al., Bulletin of Alloy Phase Diagrams, 1981, 2, 305-315), the reaction enthalpy is 9.6±4kJ mol -1 , but the reaction proceeds very slowly, while the ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
Inventor 靳正国刘彤李佳
Owner TIANJIN UNIV
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