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Preparation method of zinc sulfide nuclear hollow microspheres

A technology of hollow microspheres and zinc sulfide, applied in the field of material chemistry, can solve the problems of less operation steps and long time, and achieve the effect of mild synthesis conditions, simple and easy method, and fewer steps

Inactive Publication Date: 2015-04-22
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the step-by-step operation of the template method, the method has relatively few operating steps, and technically still uses a high-temperature solvothermal reaction (180 o C) It takes a long time (>52h), and the synthesis of core-shell homogeneous ZnS hollow microspheres with a core has not been reported at room temperature and pressure

Method used

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  • Preparation method of zinc sulfide nuclear hollow microspheres
  • Preparation method of zinc sulfide nuclear hollow microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Firstly, 5 mmol of aniline monomer was dissolved in 50 mL of carbon tetrachloride for later use, and then 5 mmol of zinc nitrate, 0.1 mol of sodium hydroxide and 5 mmol of sodium thiosulfate were dissolved in 50 mL of deionized water to obtain solution B, and then 50mL 0.1molL -1 The aqueous solution of sodium persulfate is added to solution B to obtain solution C, and finally solution C is added to the carbon tetrachloride solution of aniline to obtain a two-phase mixed solution with a clear interface (the water phase is on the upper oil phase and the oil phase is on the bottom); The phase mixture was left to stand at room temperature for 20 hours, and a pale yellow precipitate appeared on the two-phase interface; the precipitate was washed alternately with ethanol, tetrahydrofuran and deionized water, and was filtered by centrifuge precipitation or suction filtration equipment after each washing. The filtered product was redispersed in deionized water or ethanol, filt...

Embodiment 2

[0020] Repeat Example 1, but replace zinc nitrate and sodium thiosulfate with zinc chloride and thiourea respectively, to obtain ZnS cored hollow microspheres with a yield of 84.3%.

Embodiment 3

[0022] Repeat Example 1, but replace zinc nitrate and sodium thiosulfate with zinc acetate and thioacetamide respectively, to obtain ZnS cored hollow microspheres with a yield of 91.2%.

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Abstract

The invention discloses a preparation method of zinc sulfide nuclear hollow microspheres. The preparation method is characterized by comprising the following steps: (1) dosing: dissolving a phenylamine monomer in an organic solvent insoluble in water to obtain a solution A for use; sequentially dissolving a zinc-containing compound, strong base and a sulfur-containing compound in deionized water to obtain a solution B; adding the prepared persulfate aqueous solution into the solution B to obtain a solution C; and finally, adding the solution C into the solution A to obtain a insoluble two-phase mixed solution with a clear interface; (2) standing at constant temperature and reacting for 12-24 at room temperature, wherein slight yellow precipitate appears on the two-phase interface; (3) washing; and (4) drying to obtain the ZnS nuclear hollow microspheres. The method is simple and easy to implement, and the morphological control over the synthetic material is stable. The obtained product can be applied to the fields such as secondary battery materials, photovoltaic devices, photocatalysts and gas sensors.

Description

technical field [0001] The invention relates to a preparation method of hollow microspheres with cores, in particular to an interface synthesis method of hollow microspheres with cores of zinc sulfide, belonging to the technical field of material chemistry. Background technique [0002] ZnS is a wide-bandgap II-VI semiconductor compound with excellent optical, electrical, and thermal properties, and is widely used in optical devices, photovoltaic devices, energy storage devices, photocatalysts, and gas sensors. The synthesis of ZnS nanostructures with different shapes has always been a research hotspot, and the synthesis of various ZnS nanospheres, nanorods, and nanotubes has been reported. ZnS hollow microspheres have attracted widespread attention due to their special structure and surface properties. There have been some reports on the synthesis of ZnS hollow microspheres, such as using carbon spheres and silicon spheres as hard templates, or using polyethylene glycol, p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G9/08B82Y30/00
Inventor 汪元元尹桂林何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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