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Preparation method of spherical silver selenide particles

A silver selenide, spherical technology, applied in binary selenium/tellurium compounds, nanotechnology for materials and surface science, nanotechnology, etc., can solve problems such as high operation requirements, high cost, and difficulty in large-scale production. Achieve the effects of simple process operation, low environmental pollution and low equipment requirements

Active Publication Date: 2015-11-11
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The "preparation method of silver selenide nanomaterials" disclosed in Chinese patent document CN101555000A uses nitrogen atmosphere protection, which increases the difficulty of the process; the "synthesis method of silver selenide nanospheres" disclosed in patent document CN101575088A uses silver nitrate, Selenophene and aniline are raw materials, the raw materials are not easy to obtain, the required reaction temperature is 240 ° C, and the silver selenide nanospheres are seriously agglomerated; "a method for preparing monodisperse semiconductor selenide nanoparticles" disclosed in the patent document CN1772599A needs to add alkali Metal hydroxide and fatty acid, and using hydrazine hydrate as a reducing agent, the toxicity is relatively high, and the operation requirements are high; the "preparation method of monodisperse silver, silver sulfide and silver selenide nanocrystals" disclosed in the patent document CN101274751A first high-temperature heat Decompose silver nitrate, then add selenium powder to react, mainly 6-12nm silver selenide nanoparticles, and need two steps
Visible, existing preparation Ag 2 The technology of Se micro-nano materials often requires inert atmosphere protection, or requires complex and highly toxic precursor solutions, or complex equipment, high cost, and difficulty in large-scale production, and the obtained nanoparticles also have agglomeration, so it is difficult to achieve its industrial application

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  • Preparation method of spherical silver selenide particles

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Experimental program
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Effect test

Embodiment 1

[0026] A kind of preparation method of spherical silver selenide particle of the present invention, comprises the following steps:

[0027] 1) Weigh 0.34g of silver nitrate, 0.08g of selenium powder, 0.5g of polyvinylpyrrolidone, 2mL of concentrated ammonia water and 33mL of ethylene glycol into a stainless steel reaction kettle, ultrasonically disperse for 5 minutes until uniformly dispersed, and obtain a reaction solution.

[0028] 2) Heating the reaction solution obtained in step 1) to 200° C., reacting for 12 hours, cooling to room temperature naturally, and then centrifuging (centrifugal sedimentation speed is 10,000 rpm) to obtain a silver selenide precipitate product.

[0029] 3) Wash the silver selenide precipitate product obtained in step 2) three times with absolute ethanol, then place the cleaned silver selenide precipitate product in a vacuum drying oven, and dry at 50° C. for 8 hours to obtain spherical selenide silver particles.

[0030] The scanning electron mi...

Embodiment 2

[0033] A kind of preparation method of spherical silver selenide particle of the present invention, comprises the following steps:

[0034] 1) Weigh 0.34g of silver nitrate, 0.08g of selenium powder, 1.0g of polyvinylpyrrolidone, 1mL of concentrated ammonia water and 34mL of ethylene glycol into a stainless steel reaction kettle, ultrasonically disperse for 5 minutes until uniformly dispersed, and obtain a reaction solution.

[0035] 2) Heating the reaction solution obtained in step 1) to 180° C., reacting for 10 hours, cooling to room temperature naturally, and then centrifuging (centrifugal sedimentation speed is 10,000 rpm) to obtain a silver selenide precipitate product.

[0036] 3) Wash the silver selenide precipitate product obtained in step 2) with absolute ethanol five times, then place the cleaned silver selenide precipitate product in a vacuum drying oven, and dry at 50° C. for 8 hours to obtain spherical selenium silver particles.

[0037] The spherical silver sele...

Embodiment 3

[0039] A kind of preparation method of spherical silver selenide particle of the present invention, comprises the following steps:

[0040] 1) Weigh 0.34g of silver nitrate, 0.08g of selenium powder, 0.5g of polyvinylpyrrolidone, 0.6mL of concentrated ammonia water and 34.4mL of ethylene glycol into a stainless steel reaction kettle, ultrasonically disperse for 5 minutes until uniformly dispersed, and obtain a reaction solution.

[0041] 2) Heating the reaction liquid obtained in step 1) to 180° C., reacting for 4 hours, cooling to room temperature naturally, and then centrifuging (centrifugal sedimentation speed is 10,000 rpm) to obtain a silver selenide precipitate product.

[0042] 3) Wash the silver selenide obtained in step 2) three times with absolute ethanol, then place the washed silver selenide precipitation product in a vacuum drying oven, and dry at 60° C. for 8 hours to obtain spherical silver selenide particles .

[0043] The spherical silver selenide particles p...

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Abstract

The invention discloses a preparation method of spherical silver selenide particles. The method comprises the steps that selenium powder and a silver-ammonia complex serve as raw materials to react in organic solvent at the temperature ranging from 160 DEG C to 220 DEG C for 4-24 h, and the spherical silver selenide particles are prepared after cleaning and drying are conducted. According to the preparation method of the spherical silver selenide particles, the selenium powder and the silver-ammonia complex serve as the raw materials, ethylene glycol serves as the solvent and a reducing agent, and the toxicity and the pollution to the environment are small in the preparation process; the prepared Ag2Se is good in dispersity, the particle size ranges fromm 50 nm to 500 nm, and the preparation method of the spherical silver selenide particles can be used for industrial production.

Description

technical field [0001] The invention relates to a preparation method of silver selenide, in particular to a preparation method of spherical silver selenide particles. Background technique [0002] Ag 2 Se belongs to the non-magnetic narrow bandgap semiconductor, and is one of the semiconductor materials with great application value. Ag 2 Se has two stable phase structures: low-temperature β-phase and high-temperature α-phase. The phase transition temperature of silver selenide is 133°C, and the low temperature phase is β-Ag 2 Se is a semiconductor material with a narrow band gap, which has relatively high thermoelectric coefficient, low thermal conductivity and high electrical conductivity. It is widely used in the field of optical materials and thermoelectric materials as a photosensitizer; Another low temperature metastable phase t-Ag 2 Se also has potential application value in the fields of optoelectronics and thermoelectricity. High temperature phase α-Ag 2 Se ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/04B82Y30/00
Inventor 田庆华李宇郭学益邓多
Owner CENT SOUTH UNIV