One-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres

A monodisperse, zinc sulfide technology, applied in the direction of zinc sulfide, cadmium sulfide, etc., can solve the problems of many preparation steps, high cost, affecting large-scale applications, etc.

Inactive Publication Date: 2009-09-02
WUHAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the application of templates usually has the disadvantages of h...

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  • One-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres
  • One-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres
  • One-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres

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Experimental program
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Embodiment 1

[0023] Preparation of Monodisperse ZnS Nanohollow Spheres

[0024] Zinc acetate and thiourea were used as reactants. The detailed experimental process is as follows:

[0025] Dissolve 1.6 mmol of zinc acetate in 40 ml of distilled water, then add 40 mmol of thiourea to the solution, and stir at room temperature until the solution is clear, prepare 4 parts of clear solutions according to the method described, and transfer the resulting solutions to polytetrafluoroethylene After sealing in the lined stainless steel reaction kettle, heat the reaction kettle to 140, 170, 180 or 200°C respectively to decompose thiourea and react with zinc acetate for 5 hours, wash the precipitate with distilled water for 3 times, and then put it in a vacuum drying oven Dry at 60±2°C for 6 hours to obtain monodisperse zinc sulfide nano hollow spheres.

[0026] The phase structure of the prepared samples was characterized by XRD. The XRD patterns of ZnS samples prepared at different temperatures a...

Embodiment 2

[0033] In order to test the influence of reaction time on the sample morphology, the reaction temperature was fixed at 140° C., and other reaction conditions such as the amounts of zinc acetate and thiourea were exactly the same as in Example 1 except that the reaction time was different. The results showed that the samples prepared at 1 h were solid spheres with a radius of 100 nm. As the reaction time increased to 5 hours, the morphology of the sample changed to a uniform core-shell structure, the radius increased to 200 nm, and the surface became rough. The morphology of the sample prepared after 10 hours is a hollow sphere with double shells. As the reaction temperature was further increased up to 24 h, a completely hollow structure with larger grain size and thicker shell was finally obtained. From the above results, it can be deduced that the growth mechanism of hollow spheres is the Ostwald aging process, that is, the gradual cavitation process in which small grains gr...

Embodiment 3

[0035] In order to check the influence of the amount of thiourea on the shape of the sample, except that the amount of thiourea takes different values ​​between 20-60mmol, other reaction conditions such as: the amount of zinc acetate (1.6mmol), reaction Temperature (140 ℃), reaction time (5 hours), the amount of water (40 milliliters) etc. are all identical with embodiment 1. The results show that when the amount of thiourea is reduced to 20mmol, the prepared samples are aggregates of nanoparticles, which is due to the reduction of thiourea reduces the amount of complexes it forms with zinc ions, thus zinc ions in the solution Homogeneous nucleation; when the amount of thiourea increased to 60mmol, the prepared samples were nano-solid spheres, because too much thiourea prevented the Ostwald aging process. In experiments, it was found that the optimum amount of thiourea was 30-50 mmol.

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Abstract

The invention relates to a one-step template-free method for preparing a great amount of monodisperse ZnS hollow nanospheres. The method comprises the following steps: the zinc acetate is dissolved in distilled water; thiourea is added to the solution and stirred in the solution at the room temperature until the solution is clear; the obtained solution is transferred to a stainless steel reaction vessel with a polytetrafluoroethylene lining for sealing, then the reaction vessel is heated to the reaction temperature and kept at the reaction temperature for 1 to 48 hours, and the thiourea is decomposed and reacts with the zinc acetate to generate deposition; and after the reaction, the reaction vessel is cooled to the room temperature, then the clear solution on the upper layer is removed, and the obtained deposition is washed with the distilled water and dried in a vacuum drying oven at 30-100 DEG C to obtain the monodisperse ZnS hollow nanospheres. By adopting the method, the monodisperse ZnS hollow nanospheres with radius of 200 nm and with casing layers assembled by nano-particles can be prepared at a large scale. The method is simple and environment-friendly, needs lower temperature and no template and additive agent and takes the water as the solvent. The method can prepare other transition metal oxide hollow nanospheres, such as manganese sulfide, cadmium sulfide, and the like.

Description

technical field [0001] The invention relates to a method for preparing monodisperse zinc sulfide nano hollow spheres, in particular to a one-step template-free method for preparing a large amount of monodisperse zinc sulfide nano hollow spheres. technical background [0002] Hierarchical hollow nanostructures have attracted extensive attention because of their exotic physicochemical properties that are completely different from bulk materials, and have shown promising applications in nanochemical reactors, highly efficient catalysts, drug delivery, low dielectric constant materials, soundproofing materials, and Optical devices and many other fields have a wide range of applications. Traditional methods for preparing hollow spheres generally require removable or expendable templates, including hard templates (such as monodisperse polymer colloids, carbon spheres, silica spheres, reduced metal nanoparticles) or soft templates (such as micelles, high molecules, oil droplets, b...

Claims

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Application Information

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IPC IPC(8): C01G9/08C01G11/02
Inventor 余家国于笑潇程蓓
Owner WUHAN UNIV OF TECH
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