阅读说明：本技术 一种硫化亚铜粉体的制备方法 (Preparation method of cuprous sulfide powder ) 是由 孙安红 于 2019-12-20 设计创作，主要内容包括：本发明提供一种硫化亚铜粉体的制备方法,包括以下步骤：步骤(1).配制Cu(Ac)<Sub>2</Sub>和Na<Sub>2</Sub>S水或醇溶液,调节Cu(Ac)<Sub>2</Sub>水或醇溶液的pH＝4-5,室温下将Cu(Ac)<Sub>2</Sub>水或醇溶液逐滴滴入Na<Sub>2</Sub>S水或醇溶液中,同时搅拌,滴加完毕后继续搅拌20min：反应结束后过滤沉淀,过滤后经真空干燥、研磨得到硫化铜粉末；步骤(2).将步骤(1)得到的硫化铜粉末在分析纯硅酸钠熔炼保护层和氮气气氛的条件进行熔炼；步骤(3).熔炼结束温度降低至室温后,将步骤(2)得到的硫化亚铜经破碎球磨得到粒度均匀的硫化亚铜粉末；然后以去离子水洗涤所得固体物料以去除其中的水溶性杂质,最后再真空干燥,即得硫化亚铜纳米粉体。本方法原料丰富廉价,成本低廉,制备工艺简单,条件温和,可控性好,生产效率高,易于实现产业化、无污染。(The invention provides a preparation method of cuprous sulfide powder, which comprises the following steps: step (1) preparation of Cu (Ac) 2 And Na 2 S aqueous or alcoholic solution, adjusting Cu (Ac) 2 pH of water or alcohol solution is 4-5, and Cu (Ac) is added at room temperature 2 Dropwise adding Na into water or alcohol solution 2 And S, stirring simultaneously in water or an alcohol solution, and continuing stirring for 20min after the dropwise addition is finished: filtering the precipitate after the reaction is finished, and drying and grinding the precipitate in vacuum after the filtration to obtain copper sulfide powder; step (2), smelting the copper sulfide powder obtained in the step (1) under the conditions of analyzing a pure sodium silicate smelting protective layer and a nitrogen atmosphere; step (3), after the temperature is reduced to room temperature after the smelting is finished, carrying out crushing and ball milling on the cuprous sulfide obtained in the step (2) to obtain cuprous sulfide powder with uniform particle size; and washing the obtained solid material with deionized water to remove water-soluble impurities in the solid material, and finally drying in vacuum to obtain the cuprous sulfide nano powder. The method has the advantages of abundant and cheap raw materials, low cost, simple preparation process, mild conditions, good controllability, high production efficiency, easy realization of industrialization, and no pollution。)

1. A preparation method of cuprous sulfide powder is characterized by comprising the following steps: the method comprises the following steps:

step (1) preparation of Cu (Ac)₂And Na₂S aqueous or alcoholic solution, adjusting Cu (Ac)₂pH of water or alcohol solution is 4-5, and Cu (Ac) is added at room temperature₂Dropwise adding Na into water or alcohol solution₂And S, stirring simultaneously in water or an alcohol solution, and continuing stirring for 20min after the dropwise addition is finished: filtering the precipitate after the reaction is finished, and drying and grinding the precipitate in vacuum after the filtration to obtain copper sulfide powder;

step (2), placing the copper sulfide powder obtained in the step (1) in a corundum crucible to be compacted, and smelting under the conditions of analyzing a pure sodium silicate smelting protective layer and a nitrogen atmosphere;

step (3), after the temperature is reduced to room temperature after the smelting is finished, carrying out crushing and ball milling on the cuprous sulfide obtained in the step (2) to obtain cuprous sulfide powder with uniform particle size; and washing the obtained solid material with deionized water to remove water-soluble impurities in the solid material, and finally drying in vacuum to obtain the cuprous sulfide nano powder.

2. The preparation method of cuprous sulfide powder according to claim 1, wherein the method comprises the following steps: the smelting in the step (2) comprises two stages: in the first stage, the temperature is raised from room temperature to 850 ℃, and the temperature is kept at 850 ℃ for 30 minutes, so that the sodium silicate is completely changed into a melt and covers the surface of the copper sulfide powder, and copper oxide and cuprous oxide are prevented from being generated; in the second stage, the temperature is increased from 850 ℃ to 1100-1300 ℃, and the temperature is kept at 1100-1300 ℃ for 1-1.5 hours.

3. The preparation method of cuprous sulfide powder according to claim 1, wherein the method comprises the following steps: and (3) crushing the cuprous sulfide obtained in the step (2), and then ball-milling in a roller ball mill for 0.5-10 hours by adopting zirconia balls.

4. The preparation method of cuprous sulfide powder according to claim 1, wherein the method comprises the following steps: the vacuum drying in the step (3) is vacuum drying at 80 ℃ and 0.1MPa for 2 hours.

Technical Field

The invention relates to a preparation method of powder, in particular to a preparation method of cuprous sulfide powder.

Background

Cuprous sulfide (Cu)₂S) is used as a novel semiconductor material, and has excellent photoelectric properties, nonlinear optical properties, photocatalytic properties and the like. The photocatalyst is applied to the fields of solar cells, seawater cells, photocatalysis and the like at present, and shows excellent photoelectric properties and photocatalysis effects. Due to the special nonlinear optical property, the material has huge application potential in the fields of laser generators, infrared detectors, optical sensors and the like.

The superfine spherical powder has the advantages of large specific surface area, high surface activity, high chemical reaction speed, good solubility, excellent sintering performance, unique electrical property, magnetic property, optical property and the like, so the superfine spherical powder is widely applied to a plurality of high and new technical fields.

The cuprous sulfide powder is prepared by pyrogenic process, wherein copper powder or copper oxide powder is heated by introducing hydrogen sulfide or adding elemental sulfur to prepare a cuprous sulfide sintered body, and the cuprous sulfide sintered body is subjected to ball milling and screening to obtain the cuprous sulfide powder. However, the obtained cuprous sulfide powder contains unreacted copper powder or copper oxide, so that the cuprous sulfide powder has low purity, and has the defects of no specific morphology, coarse granularity, wide distribution, poor stability and the like.

Disclosure of Invention

The technical problem to be solved by the invention is to provide a preparation method of cuprous sulfide powder, so as to solve the problems in the background technology.

The technical problem solved by the invention is realized by adopting the following technical scheme: a preparation method of cuprous sulfide powder comprises the following steps:

step (1) preparation of Cu (Ac)₂And Na₂S aqueous or alcoholic solution, adjusting Cu (Ac)₂pH of water or alcohol solution is 4-5, and Cu (Ac) is added at room temperature₂Dropwise adding Na into water or alcohol solution₂And S, stirring simultaneously in water or an alcohol solution, and continuing stirring for 20min after the dropwise addition is finished: filtering the precipitate after the reaction is finished, and drying and grinding the precipitate in vacuum after the filtration to obtain copper sulfide powder;

step (2), placing the copper sulfide powder obtained in the step (1) in a corundum crucible to be compacted, and smelting under the conditions of analyzing a pure sodium silicate smelting protective layer and a nitrogen atmosphere;

step (3), after the temperature is reduced to room temperature after the smelting is finished, carrying out crushing and ball milling on the cuprous sulfide obtained in the step (2) to obtain cuprous sulfide powder with uniform particle size; and washing the obtained solid material with deionized water to remove water-soluble impurities in the solid material, and finally drying in vacuum to obtain the cuprous sulfide nano powder.

The smelting in the step (2) comprises two stages: in the first stage, the temperature is raised from room temperature to 850 ℃, and the temperature is kept at 850 ℃ for 30 minutes, so that the sodium silicate is completely changed into a melt and covers the surface of the copper sulfide powder, and copper oxide and cuprous oxide are prevented from being generated; in the second stage, the temperature is increased from 850 ℃ to 1100-1300 ℃, and the temperature is kept at 1100-1300 ℃ for 1-1.5 hours.

And (3) crushing the cuprous sulfide obtained in the step (2), and then ball-milling in a roller ball mill for 0.5-10 hours by adopting zirconia balls.

The vacuum drying in the step (3) is vacuum drying at 80 ℃ and 0.1MPa for 2 hours.

Compared with the prior art, the invention has the beneficial effects that: the method has the advantages of rich and cheap raw materials, low cost, simple preparation process, mild conditions, good controllability, high production efficiency, easy realization of industrialization and no pollution.

Detailed Description

In order to make the technical means, the characteristics, the objectives and the functions of the present invention easy to understand, the present invention will be further described with reference to the following embodiments.