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Preparation method of nano tricopper diselenide

A selenization and nanotechnology, applied in chemical instruments and methods, binary selenium/tellurium compounds, copper compounds, etc., can solve the problems of high cost, product agglomeration, high risk, etc., and achieve low cost, simple operation, and avoidance of the effect of reunion

Inactive Publication Date: 2005-03-30
SHANGHAI JIAOTONG UNIV
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Problems solved by technology

These methods mainly focus on the preparation of nano-copper diselenide by sonochemical method, microwave-assisted heating method, hydrothermal method and solvothermal method. In these methods, ultrasonic radiation, microwave radiation and hydrothermal method, solvothermal method The high temperature and high pressure provide the required negative divalent selenium ions for the generation of nano-copper diselenide. Although the above method is simple in process, it generally has the disadvantages of serious product agglomeration, expensive equipment, high cost, and high risk.

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  • Preparation method of nano tricopper diselenide
  • Preparation method of nano tricopper diselenide
  • Preparation method of nano tricopper diselenide

Examples

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Embodiment 1

[0016] ①In a 50mL quartz Erlenmeyer flask, dissolve 0.2g of copper nitrate in 26mL of deionized water, and add triethanolamine at a molar ratio of 1:1 to obtain a complex of divalent copper ions and triethanolamine—copper triethanolamine complex cation aqueous solution.

[0017] ② Dissolve 0.06 mol of anhydrous sodium sulfite in 100 mL of deionized water, then add 0.02 mol of selenium powder, and reflux for 5 hours to obtain a 0.2 M aqueous sodium selenosulfate solution.

[0018] ③ Measure 4mL of the sodium selenosulfate aqueous solution prepared in step ② and add it to the aqueous solution of triethanolamine and copper complex cations prepared in step ①, pass nitrogen gas for 15 minutes, and then place the Erlenmeyer flask at a distance of 20cm from a 250W high-pressure mercury lamp After irradiating for 4 hours, cooling water was used to keep the reaction system at room temperature. The obtained product was centrifuged, washed three times with deionized water, and dried at ...

Embodiment 2

[0021] ①In a 50mL quartz Erlenmeyer flask, dissolve 0.2g of anhydrous copper sulfate in 26mL of deionized water, and add triethanolamine at a molar ratio of 1:1.2 to obtain a complex of divalent copper ions and triethanolamine——triethanolamine Copper complex cation aqueous solution.

[0022] ② Dissolve 0.05 mol of anhydrous sodium sulfite in 100 mL of deionized water, then add 0.02 mol of selenium powder, and reflux for 5 hours to obtain a 0.2 M aqueous sodium selenosulfate solution.

[0023] ③ Measure 3mL of the sodium selenosulfate aqueous solution prepared in step ② and add it to the aqueous solution of triethanolamine and copper complex cations prepared in step ①, pass nitrogen gas for 20 minutes, and then place the Erlenmeyer flask at a distance of 20cm from a 250W high-pressure mercury lamp After irradiating for 4 hours, cooling water was used to keep the reaction system at room temperature. The obtained product was centrifuged, washed three times with deionized water, ...

Embodiment 3

[0025] ①In a 50mL quartz Erlenmeyer flask, dissolve 0.2g of copper chloride in 26mL of deionized water, and add triethanolamine at a molar ratio of 1:1.5 to obtain a complex of divalent copper ions and triethanolamine——triethanolamine complex Copper complex cation aqueous solution.

[0026] ② Dissolve 0.06 mol of anhydrous sodium sulfite in 100 mL of deionized water, then add 0.02 mol of selenium powder, and reflux for 4 hours to obtain a 0.2 M aqueous sodium selenosulfate solution.

[0027] ③ Measure 4mL of the sodium selenosulfate aqueous solution prepared in step ② and add it to the triethanolamine-copper complex cation aqueous solution prepared in step ①, pass nitrogen gas for 30 minutes, and then place the conical flask at a distance of 20cm from a 250W high-pressure mercury lamp After irradiating for 8 hours, cooling water was used to keep the reaction system at room temperature. The obtained product was centrifuged, washed three times with deionized water, and dried at...

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Abstract

The preparation method of nano tricopper diselenide includes the following steps: preparing coordination compound of cupric ion and triethanolamine-triethanolaminocopper complex cation aqueous solution and aqueous solution of sodium selenosulfate, then mixing said two aqueous solutions in quartz conical flask, introducing nitrogen gas and discharging air completely, using high-voltage mercury vapour lamp to make irradiation, and using cooling water to retain and make the temp. of reaction system be room temp., irradiating for 4-8 hr, then can obtain nano tricopped diselenide with tetragonal structure and average grain size of 40-50 nm.

Description

Technical field: [0001] The invention relates to a preparation method of nanometer copper diselenide, in particular to the preparation of nanometer copper diselenide by photochemical method. Background technique: [0002] Nano-powder has many unique physical and chemical properties due to its size effect, which has attracted people's attention. Nano-copper diselenide has become one of the research hotspots in academia because it can be widely used in solar cells, superionic conductors and other fields. In recent years, there have been many reports on the preparation methods of nano-copper diselenide. These methods mainly focus on the preparation of nano-copper diselenide by sonochemical method, microwave-assisted heating method, hydrothermal method and solvothermal method. In these methods, ultrasonic radiation, microwave radiation and hydrothermal method, solvothermal method The high temperature and high pressure provide the required negative divalent selenium ions for th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B19/04C01G3/00
Inventor 阎玉林钱雪峰朱子康
Owner SHANGHAI JIAOTONG UNIV
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