Method for preparing nano-material lead selenide through organic phase method

A technology of nanomaterials and lead selenide, applied in the direction of nanotechnology, nanotechnology, binary selenium/tellurium compounds, etc., can solve the problems of cumbersome operation, long duration and high cost, and achieve simple preparation process and strong practicability , the effect of little pollution

Inactive Publication Date: 2013-06-26
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there are many methods for preparing nanomaterial lead selenide, including hydrothermal method, microwave method, sonochemical method, photochemical method, radiation chemical method, etc. The above methods have strict preparation conditions, cumbersome operation, long duration and high cost. , serious environmental pollution; there is also a simple aqueous phase method, although this method is simple and easy, but it cannot solve the problem of difficult combination of nanomaterials and organic polymers, and cannot obtain satisfactory results in the application of composite materials

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  • Method for preparing nano-material lead selenide through organic phase method
  • Method for preparing nano-material lead selenide through organic phase method
  • Method for preparing nano-material lead selenide through organic phase method

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Embodiment 1

[0022] The specific preparation steps of this embodiment are as follows:

[0023] First weigh 0.005mol of selenium powder in a three-necked bottle, add 0.01mol of sodium borohydride and 30ml of anhydrous tetrahydrofuran, and react in an ice bath under the protection of argon until light yellow to generate the required sodium selenium hydride solution; then weigh 0.005 Put 80ml of anhydrous tetrahydrofuran into the three-necked bottle, pass argon to the solution system to remove dissolved oxygen, stir rapidly under the protection of argon, add the newly prepared sodium selenium hydride solution, heat to 60°C, and reflux for 0.5h After the reaction was stopped, after the solution was naturally cooled to room temperature, it was washed with absolute ethanol, centrifuged, and vacuum-dried to obtain a black powdery PbSe nanocrystalline material, which was spherical in shape and had an average diameter of 10.58nm.

Embodiment 2

[0025] The specific preparation steps of this embodiment are as follows:

[0026] First weigh 0.005mol of selenium powder in a three-necked bottle, add 0.01mol of sodium borohydride and 30ml of anhydrous tetrahydrofuran, and react in an ice bath under the protection of argon until light yellow to generate the required sodium selenium hydride solution; then weigh 0.005 mol of lead acetate in a three-necked flask, add 80ml of anhydrous tetrahydrofuran. Pass argon to the solution system to remove dissolved oxygen, add the newly prepared sodium selenium hydride solution with rapid stirring under the protection of argon, heat to 70 ° C, and stop the reaction after reflux for 0.5 h. After the solution is naturally cooled to room temperature, use After washing with water and ethanol, centrifuging and vacuum drying, a black powdery PbSe nanocrystalline material was obtained, the shape of which was spherical nanoparticles, and the average diameter was 8.84nm.

Embodiment 3

[0028] The specific preparation steps of this embodiment are as follows:

[0029] First weigh 0.005mol of selenium powder in a three-necked bottle, add 0.01mol of sodium borohydride and 30ml of anhydrous tetrahydrofuran, and react in an ice bath under the protection of argon until light yellow to generate the required sodium selenium hydride solution; then weigh 0.005 mol of lead acetate in a three-necked flask, add 80ml of anhydrous tetrahydrofuran. Pass argon to the solution system to remove dissolved oxygen, quickly stir and add the newly prepared sodium selenium hydride solution under the protection of argon, heat to 60 ° C, and stop the reaction after reflux for 1.0 h. After the solution is naturally cooled to room temperature, use After washing with water and ethanol, centrifuging and vacuum drying, a black powdery PbSe nanocrystalline material was obtained, the shape of which was spherical nanoparticles, and the average diameter was 4.36nm.

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Abstract

The invention provides a method for preparing a nano-material lead selenide through an organic phase method. The technical characteristics of the method are that: selenium powder, sodium borohydride and anhydrous tetrahydrofuran are added into a three-necked flask; an ice bath reaction is carried out under the protection of argon gas, such that a selenium precursor solution is obtained; lead acetate and anhydrous tetrahydrofuran are added into another three-necked flask; argon gas is delivered into the solution system; the selenium precursor solution is added under the protection of argon gas; the mixture is heated to 40-80 DEG C, and reflux is carried out for 0-2.0h; the reaction is stopped, and the solution is naturally cooled to room temperature; the solution is washed by using anhydrous ethanol, and is centrifuged and vacuum-dried, such that a black powdery PbSe nano-crystal material is prepared. The method is simple and easy. The synthesized material can be effectively compounded with an organic material. The method and the material have high practicality.

Description

technical field [0001] The invention relates to a method for preparing nano-material lead selenide by using an organic phase method. The method is simple and easy to implement, and can solve the problem of difficult compounding of nano-materials and organic materials. It has strong practicability and can be used in laboratories. The method for fast and effective preparation belongs to the technical field of inorganic nanometer material preparation. Background technique [0002] Since the discovery of nanomaterials, they have become one of the most dynamic materials among new materials. Due to the small size effect, surface effect, quantum size effect and multi-exciton effect, nanomaterials exhibit completely different properties from traditional large crystal materials in many aspects, and have been widely used in many research and application fields. It plays an irreplaceable role in promoting the development of the national economy and the progress of the future society. ...

Claims

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Application Information

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IPC IPC(8): C01B19/04B82Y30/00
Inventor 郑建邦屈俊荣吴广荣王春锋郝娟曹崇德
Owner NORTHWESTERN POLYTECHNICAL UNIV
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