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Preparation method of cobalt sulfide micro tube with hiberarchy structure

A technology of hierarchical structures and microtubes, which is applied in separation methods, microstructure devices without moving elements, chemical instruments and methods, etc., can solve the problem of microtubes that cannot be synthesized with hierarchical cobalt sulfide, irregular cobalt sulfide morphology, Synthetic method is complicated to operate and other problems, and achieves the effect of excellent electrical and magnetic properties, simple equipment, and cheap and easy-to-obtain raw materials

Inactive Publication Date: 2010-06-23
NORTHEAST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, neither the traditional synthesis method nor the method reported in the literature can synthesize cobalt sulfide microtubes with hierarchical structure, which limits the application of cobalt sulfide.
For example, "Crystal Growth & Design" (Crystal Growth & Design) 2008, Volume 8, page 3745, reported the hydrothermal synthesis of Co 3 S 4 Octahedral nanocrystals; British "Chemical Communications" (Chemical Communications) 2498 pages in 2003 reported the synthesis of CoS nanowires by vapor deposition, which needs to be carried out under argon protection and high temperature conditions of 850 ° C; American "Inorganic Chemistry" (Inorganic Chemistry) 1999, volume 38, page 2621, reported the synthesis of Co by toluene solvothermal method 9 S 8 and CoS 2 Nanocrystals, the raw materials used in this method are very toxic, and the obtained cobalt sulfide has irregular morphology and is easy to agglomerate; Germany "Advanced Functional Materials" (Advanced Functional Materials) 2006, volume 16, page 1389, reported the use of the Kirkendall effect ( Kirkendall effect) to synthesize cobalt sulfide hollow nanocrystals, the synthesis method is complicated to operate, and the raw materials used are expensive
Other methods also include synthesizing cobalt sulfide nanotubes by using the sacrificial template method ("Journal of Colloid and Interface Science", 2007, volume 308, page 271), and using metal organic compounds as precursors to prepare cobalt sulfide films ("Chemistry Vapor Deposition"Chemical Vapor Deposition, 2005, Volume 11, Page 91), but none of them can synthesize microtubes with hierarchical cobalt sulfide

Method used

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  • Preparation method of cobalt sulfide micro tube with hiberarchy structure
  • Preparation method of cobalt sulfide micro tube with hiberarchy structure
  • Preparation method of cobalt sulfide micro tube with hiberarchy structure

Examples

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Embodiment 1

[0016] First, fully mix 4 ml of deionized water with 4 ml of ethylenediamine, weigh 0.0001 mole of cobalt acetate, add it to the above solution under stirring, and continue stirring the mixed solution for 5 minutes; Ammonium bromide CTAB was added to the above solution, slightly heated to dissolve it; then 0.0003 moles of thioacetamide was added to the above mixture, stirred for 15 minutes and then loaded into a stainless steel reactor with a Teflon liner , sealed the reactor, and reacted at 160°C for 24 hours. Then cool to room temperature, open the reactor, filter with Buchner funnel, wash with deionized water and absolute ethanol to obtain a black powder. The product was identified as hexagonal cobalt sulfide (Co 1-x S) (X=0.75) (attached figure 1 ), the black powder was identified as a micron tube by a low-magnification scanning electron microscope, and the average length of the tube was about 15 microns (attached figure 2 ). High-magnification scanning electron micro...

Embodiment 2

[0018] First, fully mix 4 milliliters of deionized water with 4 milliliters of ethylenediamine, weigh 0.0001 moles of cobalt nitrate, add it to the above solution under stirring conditions, and continue to stir the mixed solution for 5 minutes; Ammonium bromide CTAB was added to the above solution, slightly heated to dissolve it; then 0.0003 moles of thioacetamide was added to the above mixture, stirred for 15 minutes and then loaded into a stainless steel reactor with a Teflon liner , sealed the reactor, and reacted at 160°C for 24 hours. Then cool to room temperature, open the reaction kettle, filter with Buchner funnel, and wash with deionized water and absolute ethanol to obtain cobalt sulfide microtubes with the same length as in Example 1.

Embodiment 3

[0020] First, fully mix 4 milliliters of deionized water with 4 milliliters of ethylenediamine, weigh 0.0001 moles of cobalt chloride, add it to the above solution under stirring conditions, and continue to stir the mixed solution for 5 minutes; Add methyl ammonium bromide CTAB to the above solution, heat it slightly to dissolve it; then add 0.0003 moles of thioacetamide to the above mixture, stir for 15 minutes and then put it into a stainless steel with Teflon lining for reaction In the kettle, seal the reaction kettle, and react at 160° C. for 24 hours. Then cool to room temperature, open the reaction kettle, filter with Buchner funnel, and wash with deionized water and absolute ethanol to obtain cobalt sulfide microtubes with the same length as in Example 1.

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Abstract

The invention belongs to an inorganic chemical synthesis method and in particular relates to a preparation method of a cobalt sulfide micro tube with hiberarchy structure; in the invention, water-soluble cobalt salt is used as a metal source, thioacetamide is used as a sulphur source, ethanediamine is used as metal chelating agent, and cetyl trimethylammonium bromide CTAB is used as a template agent, in a closed reactor, hydro-thermal reaction is carried out under a certain temperature condition, so as to synthesize the micron tube-like cobalt sulfide with the hiberarchy structure, the outer diameter of the tube is about 1.5micron, the thickness of the tube wall is about 400nm, the average length is about 15micron, the tube wall is a nanoscale hexagonal sheet, and the length and the thickness of the sheet are 90nm and 22nm respectively; the synthesis method has the advantages of cheap and easy-obtaining raw material, simple equipment, low reaction temperature and good process repeatability and overcomes the problem of environment pollution caused by organic solvent in the previous synthesis method; the obtained product has wide application prospect in the field of biology, catalysis and material science and the like.

Description

technical field [0001] The invention belongs to an inorganic chemical synthesis method, in particular to a preparation method of a cobalt sulfide microtube with a hierarchical structure. Background technique [0002] As an important chalcogen compound, cobalt sulfide has a complex structure and composition and good catalytic, optical, electrical and magnetic properties, and has a wide range of applications in industrial fields such as dearomatization and hydrodesulfurization processes. In addition, It is also widely used in research fields such as solar cell materials. At present, neither the traditional synthesis method nor the method reported in the literature can synthesize cobalt sulfide microtubes with hierarchical structure, which limits the application of cobalt sulfide. For example, "Crystal Growth & Design" (Crystal Growth & Design) 2008, Volume 8, page 3745, reported the hydrothermal synthesis of Co 3 S 4 Octahedral nanocrystals; British "Chemical Communications...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00B81B1/00
Inventor 邢艳刘博
Owner NORTHEAST NORMAL UNIVERSITY
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