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Preparation method of dendritic lead sulfide material

A lead sulfide and dendritic technology, which is applied in the field of preparation of dendritic lead sulfide materials, can solve the problem of short reaction time of microwave method

Inactive Publication Date: 2013-04-17
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the various methods reported in the literature, the autoclave hydrothermal method has simple equipment, is easy to control and realizes industrial production, and the microwave method has a short reaction time, usually complete reaction in a few minutes or tens of minutes, saving energy; and the surface Active agent assists these methods and is the preferred method of controlling material morphology again, and the surfactant used in the above literature is sodium dodecylbenzenesulfonate anionic surfactant or hexadecyltrimethylammonium bromide cationic surface Active agent or these two mixed surfactants, these two surfactants are petrochemical synthetic products, and have a long chain alkyl structure, have strong flexibility, and have certain defects in controlling the morphology of prepared materials

Method used

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  • Preparation method of dendritic lead sulfide material
  • Preparation method of dendritic lead sulfide material
  • Preparation method of dendritic lead sulfide material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 4mL of 0.4mol / L lead nitrate aqueous solution and thiourea aqueous solution, 1.5mL of 10g / L rosin-based surfactant A ethanol solution into the reaction kettle, add 2.5mL of water, mix well and put the reaction kettle into 160℃ React in an oven for 12 hours, cool to room temperature, wash the black precipitate with deionized water and ethanol three times each, centrifuge to obtain a black precipitate, dry at 80°C for 8 hours to obtain a morphology as follows figure 1 , figure 2 lead sulfide products.

[0026]

[0027] Rosin-based surfactant A Rosin-based surfactant B

Embodiment 2

[0029] Take 4mL of 0.4mol / L lead nitrate aqueous solution and thiourea aqueous solution, 1.8mL of 10g / L rosin-based surfactant B ethanol solution into the reaction kettle, add 2.2mL of water, mix well and put the reaction kettle at 140℃ React in an oven for 36 hours, cool to room temperature, wash the black precipitate with deionized water and ethanol three times each, centrifuge to obtain a black precipitate, dry at 80°C for 8 hours to obtain a morphology as follows image 3 lead sulfide products.

Embodiment 3

[0031] Take 4mL of 0.2mol / L lead nitrate aqueous solution and thiourea aqueous solution, 1.2mL of 10g / L rosin-based surfactant C ethanol solution into the reaction kettle, add 2.8mL water, mix well and put the reaction kettle at 200℃ React in an oven for 12 hours, cool to room temperature, wash the black precipitate with deionized water and ethanol three times each, centrifuge to obtain a black precipitate, dry at 80°C for 8 hours to obtain a morphology as follows Figure 4 lead sulfide products.

[0032]

[0033] Rosin-based Surfactant C

[0034] in, R 1 =(CH 2 ) 3 CH 3 .

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Abstract

The invention provides a method for preparing a lead sulfide material, which comprises the following steps: preparing a reaction mixture of lead nitrate, thiourea, an abietyl surfactant with a molar ratio of 1-2:2-4:0.05-0.15, adding the mixture into a solvent, stirring uniformly to obtain a reaction solution; wherein, the mass ratio of the reaction mixture and the solvent is 1:15-40, and the solvent is one selected from ethanol and deionized water; adding the reaction solution into a sealed high pressure reaction vessel, heating to 160-220 DEG C, performing heat insulation for 12-72 hours, cooling, washing, and drying to obtain the lead sulfide material with a dendritic particle shape.

Description

technical field [0001] The invention relates to a method for preparing a lead sulfide material, in particular to a method for preparing a dendritic lead sulfide material. Background technique [0002] Lead sulfide is an important semiconductor material, which has important application value in near-infrared communication, optoelectronic devices and solar cells. In recent years, it has been found that the shape, size and structure of materials directly affect the properties of materials. Therefore, the preparation of materials with special shape control has become a research hotspot in the field of material preparation. People adopt various methods to prepare lead sulfide materials with multiple shapes, such as people adopting adding surfactant autoclave hydrothermal method to obtain lead sulfide nanospheres (CN101402468A), nanorods (CN101049960A), hollow cubic nanocrystals (CN101402467A ), monodisperse cubic nanocrystals (CN101402467A), hexagonal star nanocrystals (CN101117...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G21/21
Inventor 韩春蕊高强张世锋
Owner BEIJING FORESTRY UNIVERSITY