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Preparation method of general-purpose multi-metal sulfide nano-material

A multi-metal and nanomaterial technology, applied in the field of nanomaterials, can solve the problems of difficult to control size and valence state, low product phase state purity, harsh preparation conditions, etc., to achieve uniform and controllable morphology and size, and easy control of reaction conditions. , good dispersion effect

Inactive Publication Date: 2012-08-15
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction time of this method is longer, the shape is not easy to control, and the particles are larger
Based on the above-mentioned various preparation methods, there are problems such as relatively harsh preparation conditions, low product phase purity, and difficult control of size and valence state.

Method used

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  • Preparation method of general-purpose multi-metal sulfide nano-material
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  • Preparation method of general-purpose multi-metal sulfide nano-material

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Example 1: Orthorhombic AgInS 2 Synthesis of Nanomaterials. Weigh 0.05mmol of silver diethyldithiocarbamate and 0.05mmol of indium diethyldithiocarbamate as raw materials, and dissolve them into a three-necked flask containing a mixed solvent of dodecanethiol and oleic acid (15g:7g) In the process, vacuumize at room temperature and keep it for 10 minutes, then raise the temperature to 200°C under an inert atmosphere and keep it for 2 hours. Finally, after the solution is naturally cooled to room temperature, add an appropriate amount of absolute ethanol, centrifuge, wash and dry, and the obtained red powder material is dispersed. In polar solvents, with a transmission electron microscope (eg figure 1 shown) and by X-ray diffraction (as figure 2 shown) confirmed that the obtained red powder material is orthorhombic AgInS 2 nanomaterials.

Embodiment 2

[0024] Example 2: Cu 12 Sb 4 S 13 Synthesis of Nanomaterials. Weigh 0.05mmol copper diethyldithiocarbamate and 0.1mmol antimony diethyldithiocarbamate as raw materials, and dissolve them into a three-necked flask filled with a mixed solvent of dodecanethiol and oleylamine (20mmol: 20mmol) In the process, vacuumize at 120°C and keep it for 15 minutes, then raise the temperature to 220°C under an inert atmosphere and keep it for 0.5 hours. Finally, after the solution is naturally cooled to room temperature, add an appropriate amount of absolute ethanol, centrifuge, wash and dry, and the obtained powder material is dispersed in In polar solvents, use a transmission electron microscope (e.g. image 3 shown) and confirmed by X-ray diffraction that the obtained red powder substance is Cu 12 Sb 4 S 13 nanomaterials.

Embodiment 3

[0025] Example 3: Orthorhombic AgBiS 2 Synthesis of Nanomaterials. Weigh 0.1mmol of silver diethyldithiocarbamate and 0.1mmol of bismuth diethyldithiocarbamate as raw materials, and dissolve them in a three-port container containing a mixed solvent of octadecylamine and octadecene (20mmol: 20mmol). Vacuumize the flask at 100°C for 20 minutes, then raise the temperature to 240°C for 1 hour under an inert atmosphere, and finally cool the solution to room temperature naturally, add an appropriate amount of hot absolute ethanol, centrifuge, wash and dry, and the obtained black Powdered substances dispersed in polar solvents were examined by transmission electron microscopy (eg Figure 4 shown) and by X-ray diffraction, it was confirmed that the obtained black powder material was orthorhombic phase AgBiS 2 nanomaterials. Such as Figure 5 As shown, the obtained nanomaterials have good optical properties.

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Abstract

The invention discloses a preparation method of a general-purpose multi-metal sulfide nano-material. The preparation method comprises the following steps of: taking two or more different metal diethyldithiocarbamates, or two or more different metal phenanthroline diethyldithiocarbamates, or the combination of the metal diethyldithiocarbamates and the metal phenanthroline diethyldithiocarbamates as reaction predecessors, performing co-thermal decomposition in a mixed solution of surfactants with different coordination properties, and performing nucleation and growth so as to prepare a high-quality multi-metal sulfide nano-material by one step. The multi-metal sulfide prepared by the preparation method disclosed by the invention has the advantages of pure phase state, adjustable composition, uniform and controllable appearance and size, high yield, low toxicity or no toxicity, better dispersivity in a non-polar organic solvent, easiness in control of reaction conditions, mild preparation conditions, simple operation, good repeatability and capability of realizing large-scale production.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a preparation method of a general multi-component metal sulfide nanometer material. Background technique [0002] Multivariate metal sulfides have excellent optical, electrical, magnetic, and catalytic properties, and are widely used in semiconductors, biomedicine, photoluminescent devices, solar cells, photolysis of water to produce hydrogen, nonlinear optical devices, optical fiber communications, and lubricants , Optical and magnetic recording materials, etc. With the requirement of green and sustainable energy, solar cells and photolysis of water to produce hydrogen are the current energy research hotspots. Some I-III-VI 2 Ternary semiconductor nanomaterials have attractive prospects in the fields of solar cells and optoelectronic applications. With the increasing research and application of multinary metal sulfides, a number of preparation methods ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00C01G30/00C01G29/00C01G19/00B82Y40/00
Inventor 王强斌邓满姣张叶俊沈淑玲
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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