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Preparation method of metal selenide nano-powder

A technology of metal selenide and nanopowder, which is applied in the direction of metal selenide/telluride, binary selenium/tellurium compound, etc., can solve the problems of limited reactivity and insoluble selenium powder, and achieve rich raw material resources and high ratio Excellent surface area and crystallinity

Inactive Publication Date: 2018-08-24
GUILIN UNIV OF ELECTRONIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method is low in cost, especially in the direct solution method, hot injection method, hydrothermal / solvothermal method, when selenium powder is used as the selenium source, the morphology and composition of the metal selenide can be regulated, but the selenium powder is in many solvents. Insoluble, which limits its reactivity and thus limits the preparation of metal selenide nanopowders by wet chemical methods

Method used

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  • Preparation method of metal selenide nano-powder
  • Preparation method of metal selenide nano-powder
  • Preparation method of metal selenide nano-powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 250ml of ethylene glycol into a 500ml three-neck flask, then add SnCl 2 2H 2 O (2.256g) and SeO 2 (2.22g) was added to ethylene glycol, and after stirring for 10 minutes, slowly added 6ml N 2 h 4 ·H 2 O, and then heated to 182 ° C for 24 hours. After stopping the reaction and cooling naturally, pour off the supernatant, wash 3 times with distilled water, each time distilled water is 500ml, then soak 2 hours with dehydrated alcohol (200ml), the black precipitate that obtains after suction filtration with circulating water suction filter is in vacuum Dry in a drying oven at 60°C for 15 hours to obtain SnSe 2 Black powder. SnSe 2 The X-ray diffraction picture of the change with temperature is as follows figure 1 As shown in (a), its transmission electron microscope and scanning electron microscope photos are as follows figure 2 Shown in (a) and (b). It can be seen from the figure that the obtained selenide has high purity, good crystallinity, narrow size dis...

Embodiment 2

[0021] Add 250ml of ethylene glycol into a 500ml three-neck flask, then add SnCl 2 2H 2 O (1.128g) and SeO 2 (0.555g) was added into ethylene glycol, and after stirring for 10 minutes, slowly added 6ml of N 2 h 4 ·H 2 O, and then heated to 160 ° C for 24 hours. After stopping the reaction and cooling naturally, pour off the supernatant, wash 3 times with distilled water, each time distilled water is 500ml, then soak 2 hours with dehydrated alcohol (200ml), the black precipitate that obtains after suction filtration with circulating water suction filter is in vacuum Dry at 60° C. for 15 hours in a drying oven to obtain a black SnSe powder. The X-ray diffraction picture of SnSe black powder changing with temperature is as follows figure 1 Shown in (b).

Embodiment 3

[0023] Add 250ml of ethylene glycol into a 500ml three-neck flask, then add InCl 3 4H 2 O (3.913g) and SeO 2 (2.220g) was added to ethylene glycol, and after stirring for 10 minutes, slowly added 6ml N 2 h 4 ·H 2 O, and then heated to 182 ° C for 48 hours. After stopping the reaction and cooling naturally, pour off the supernatant, wash 3 times with distilled water, each time distilled water is 500ml, then soak 2 hours with dehydrated alcohol (200ml), the black precipitate that obtains after suction filtration with circulating water suction filter is in vacuum Dry in a drying oven at 80°C for 15 hours to obtain In 2 Se 3 Black powder. X-ray diffraction pictures such as image 3 shown. got In 2 Se 3 High purity, good crystallinity, narrow size distribution, high specific surface area and low degree of agglomeration are beneficial to improve the photocatalytic ability of selenides.

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Abstract

The invention discloses a preparation method of metal selenide nano-powder. Hydrazine hydrate is used for carrying out activation treatment on a selenium source; the selenide nano-powder is prepared through a condensation refluxing method; the composition and a nano-shape of the selenide nano-powder can be accurately controlled and obtained selenide has high purity, good crystallization degree andnarrow size distribution and has high specific surface area and low aggregation degree; the photocatalysis capability of the selenide is easy to improve.

Description

Technical field: [0001] The invention relates to the technical field of semiconductor nanomaterials, in particular to a method for preparing metal selenide nanopowder. Background technique: [0002] Selenide nanomaterials are an important class of semiconductor materials. Because of their excellent optical, thermal, electrical, magnetic properties and special structures, they are of high value in many fields and are widely used in hydrogen storage materials and photochemical cells. Electrode materials, gas sensors, lithium-ion batteries, thermoelectric devices, solar cells, phase-change memories and photodetectors have a major impact on people's lives. Common methods for preparing metal selenide nanomaterials mainly include solid-state reaction method, direct solution method, thermal injection method, and hydrothermal / solvothermal method. The above method is low in cost, especially in the direct solution method, hot injection method, hydrothermal / solvothermal method, when s...

Claims

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Application Information

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IPC IPC(8): C01B19/04
CPCC01B19/007C01P2002/72C01P2004/03C01P2004/04
Inventor 苗蕾伍少海刘呈燕王潇漾王秀霞高杰
Owner GUILIN UNIV OF ELECTRONIC TECH