阅读说明：本技术 一种光吸收增强的球状CuS亚微米材料及其制备方法 (Light absorption enhanced spherical CuS submicron material and preparation method thereof ) 是由 方俊飞 谢康乐 于 2020-06-04 设计创作，主要内容包括：本发明公开了一种光吸收增强的球状CuS亚微米材料及其制备方法。本发明通过将硫酸铜和硫代硫酸钠加入去离子水后充分搅拌,同时加入聚乙烯吡咯烷酮(PVP)继续搅拌使它们完全溶解,将充分溶解后的混合溶液转移至聚四氟乙烯内衬的反应釜中,置于120～160℃恒温环境中加热反应8~12h,将反应产物洗涤、离心,将所得到的黑褐色沉淀物干燥,得到光吸收增强的球状CuS亚微米材料。本发明方法操作简单,适于工业化生产,所得到的球状CuS亚微米材料结晶度高、比表面积大,对太阳光的吸收性能好,可用于对太阳能的高效吸收和光热转换利用。(The invention discloses a light absorption enhanced spherical CuS submicron material and a preparation method thereof. The method comprises the steps of adding copper sulfate and sodium thiosulfate into deionized water, fully stirring, adding polyvinylpyrrolidone (PVP) and continuously stirring to completely dissolve the copper sulfate and the sodium thiosulfate, transferring the fully dissolved mixed solution into a reaction kettle with a polytetrafluoroethylene lining, heating and reacting for 8-12 hours at the constant temperature of 120-160 ℃, washing and centrifuging reaction products, and drying obtained dark brown precipitates to obtain the spherical CuS submicron material with enhanced light absorption. The method is simple to operate and suitable for industrial production, and the obtained spherical CuS submicron material is high in crystallinity, large in specific surface area and good in sunlight absorption performance, and can be used for efficient absorption and photothermal conversion utilization of solar energy.)

1. A light absorption enhanced spherical CuS submicron material and a preparation method thereof are characterized in that the method comprises the following steps:

respectively weighing copper sulfate and sodium thiosulfate in a beaker, adding deionized water, fully stirring, then adding a certain amount of PVP, and continuously stirring to completely dissolve the PVP and the PVP;

transferring the fully dissolved solution into a reaction kettle with a 100ml polytetrafluoroethylene lining, setting the temperature of a drying oven to be 120-160 ℃ for hydrothermal reaction, and setting the reaction time to be 8-12 h;

(3) and taking out the obtained precipitate, carrying out centrifugal separation, repeatedly washing and centrifuging by using deionized water, and then drying in a constant-temperature drying oven for 4-8 hours to obtain the spherical CuS submicron material.

2. The method for preparing CuS submicron materials with spherical structures according to claim 1, wherein in the step (1), the molar weight ratio of copper sulfate to sodium thiosulfate is 1: 1, the molar volume ratio of copper sulfate to deionized water is 5 mmol: 60 mL.

3. The method for preparing the CuS submicron material with the spherical structure according to claim 1, wherein in the step (1), the mass-to-volume ratio of PVP to deionized water is (0.25-0.75) g: 60 mL.

4. The method for preparing the spherical-structured CuS submicron material according to claim 1, wherein in the step (3), the washing and centrifuging are: washing the reaction product with deionized water, centrifuging, and repeating the washing and centrifuging operations for 3-5 times;

in the step (3), the drying temperature of the precipitate is 60-90 ℃.

5. The spherical CuS submicron material with enhanced light absorption obtained by the preparation method of any one of claims 1 to 4.

Technical Field

The invention belongs to the field of micro-nano functional material science, and particularly relates to a spherical CuS submicron material with enhanced light absorption and a preparation method thereof.

Background

Copper sulfide (CuS) is a p-type semiconductor material with a photonic band gap of about 1.2 to 2.0eV, and thus has good light absorption properties in both visible and near-infrared regions. The nano or micron CuS can show special optical, electrical and thermal properties due to the unique microstructure and size effect, and can be widely applied to the fields of light absorption, photo-thermal conversion, photocatalysis, solar cells and the like, so that the synthesis and performance research of the CuS micro-nano material also becomes one of the focuses of domestic and foreign material scientists.

The hydrothermal synthesis method is a synthesis method in which reactants are subjected to a chemical reaction in a fluid atmosphere such as an aqueous solution or steam under a high-temperature and high-pressure environment provided in a specific closed container (high-pressure reaction vessel); the nano particles prepared by the hydrothermal synthesis method have high purity and good crystal form, the whole preparation process is relatively simple, and the consumption cost is relatively low, so that the CuS nano material prepared by the hydrothermal synthesis method is greatly favored by researchers. Fang et al (J Fang, et al, Solar energy Materials and Solar Cells, 2018, 185: 456-; however, no surfactant is added during the reaction process, and the concentration used is relatively high, which leads to a certain agglomeration phenomenon of the prepared material, which may reduce the absorption capacity of the prepared material to sunlight. Therefore, the preparation method needs to be improved to prepare the spherical CuS micro-nano material with large specific surface area and uniform structure distribution for enhancing the sunlight absorption performance of the spherical CuS micro-nano material. Therefore, the method for preparing the spherical CuS micro-nano material which is more optimized, convenient to operate and low in energy consumption is very significant.

Disclosure of Invention

The invention aims to provide a spherical CuS submicron material with enhanced light absorption and a preparation method thereof.

The purpose of the invention can be realized by the following technical scheme:

a light absorption enhanced spherical CuS submicron material and a preparation method thereof are characterized by comprising the following steps:

(1) respectively weighing copper sulfate and sodium thiosulfate in a beaker, adding deionized water, fully stirring, then adding a certain amount of PVP, and continuously stirring to completely dissolve the PVP and the PVP;

(2) transferring the fully dissolved solution into a 100ml polytetrafluoroethylene reaction kettle, and carrying out hydrothermal reaction at a certain temperature and for a certain time;

(3) and taking out the obtained precipitate, carrying out centrifugal separation, repeatedly washing and centrifuging by using deionized water, and then drying in a constant-temperature drying oven for 4-8 hours to obtain the spherical CuS submicron material.

Preferably, in the step (1), the molar weight ratio of the copper sulfate to the sodium thiosulfate is 1: 1, the molar volume ratio of copper sulfate to deionized water is 5 mmol: 60 mL.

Preferably, in the step (1), the mass-to-volume ratio of the added PVP to the deionized water is (0.25-0.75) g: 60 mL.

Preferably, in the step (2), the reaction temperature is 120-160 ℃, and the reaction time is 8-12 h.

Preferably, in step (3), the washing and centrifuging are: washing the reaction product with deionized water, centrifuging, and repeating the washing and centrifuging operations for 3-5 times.

Preferably, in the step (3), the drying temperature of the precipitate is 60-90 ℃.

Compared with the prior art, the spherical CuS submicron material with large specific surface area and uniform structure distribution is prepared by a simple hydrothermal reaction method, is used for improving the absorption performance of sunlight, provides a simple and feasible method for efficiently absorbing and utilizing solar energy, and has the following advantages:

(1) the preparation process of the spherical CuS material is simple, different amounts of submicron structural materials can be obtained by changing the addition amount of reactants and the size of a reaction container, and the method is suitable for industrial production.

(2) The crystallinity of the prepared CuS submicron material can be higher by controlling the time and the temperature of the hydrothermal reaction, and the material can have a larger specific surface area by changing the addition amount of the surfactant, so that the absorption performance of the material on sunlight is enhanced, and a greater possibility is provided for efficiently absorbing and converting and utilizing solar energy.

Drawings

FIG. 1 is an X-ray diffraction pattern of a CuS submicron material prepared in example 1 of the present invention;

FIG. 2 is a scanning electron microscope picture of a CuS submicron material prepared in example 2 of the present invention;

FIG. 3 is a graph of the sum of N and CuS submicron materials prepared in example 2 of the present invention₂Adsorption-desorption curves;

fig. 4 is a uv-vis-nir absorption spectrum curve of the CuS submicron material prepared in examples 1 and 2 of the present invention.

Detailed Description

The technical solution of the present invention is fully described in further detail by the following specific examples. The following examples are further illustrative of the present invention and do not limit the scope of the present invention.