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

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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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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