A highly uniform sulfide microsphere with precise and controllable particle size and its preparation method

A sulfide, precise technology, applied in chemical instruments and methods, lead sulfide, zinc sulfide, etc., can solve the problems of narrow particle size range, rough control of product particle size, etc., and achieve the effect of highly uniform particle size

Active Publication Date: 2020-07-14
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But simple conditional control can only roughly control the particle size of the product, and the adjustable particle size range is narrow, usually in the range of 50nm-400nm (see patent CN 1923702 A; CN104213399 A; CN 108321389 A)

Method used

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  • A highly uniform sulfide microsphere with precise and controllable particle size and its preparation method
  • A highly uniform sulfide microsphere with precise and controllable particle size and its preparation method
  • A highly uniform sulfide microsphere with precise and controllable particle size and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Through the multi-step growth method of precisely controlling the particle size, monodisperse ZnS nano-microspheres with a particle size of 235±5nm are prepared, and the three-dimensional photonic crystals are constructed using the microspheres with this particle size. The specific preparation method is:

[0031] 1) Weigh 3.00g of polyvinylpyrrolidone and 100mL of deionized water, fully dissolve the polyvinylpyrrolidone in deionized water; obtain a uniform solution, stir and heat to 75°C; weigh 2.25g of thioacetamide, and add to the reaction system; Measure 0.07mL concentrated nitric acid and add it to the reaction system; weigh 2.97g zinc nitrate hexahydrate, dissolve it in 5mL deionized water in advance, then quickly add it to the reaction system, stir vigorously at 1000rpm for 3min; reduce the stirring speed to 300 -500rpm, stirred and reacted at 75°C for 2h;

[0032] 2) Weigh 2.97g zinc nitrate hexahydrate, pre-dissolve it in 5mL deionized water, then quickly add i...

Embodiment 2

[0039] Through the multi-step growth method of precisely controlling the particle size, monodisperse ZnS nano-microspheres with a particle size of 150±5nm are prepared, and three-dimensional photonic crystals are constructed using the microspheres with this particle size. The specific preparation method is:

[0040] 1) Weigh 3.00g of polyvinylpyrrolidone and 100mL of deionized water, fully dissolve the polyvinylpyrrolidone in deionized water; obtain a uniform solution, stir and heat to 75°C; weigh 2.25g of thioacetamide, and add to the reaction system; Measure 0.07mL concentrated nitric acid and add it to the reaction system; weigh 2.97g zinc nitrate hexahydrate, dissolve it in 5mL deionized water in advance, then quickly add it to the reaction system, stir vigorously at 1000rpm for 3min; reduce the stirring speed to 300 -500rpm, stirred and reacted at 75°C for 2h;

[0041] 2) Weigh 2.97g of zinc nitrate hexahydrate, dissolve it in 5mL of deionized water in advance, then quic...

Embodiment 3

[0045] The monodisperse ZnS nanometer microspheres with a particle size of 1000±5nm are prepared through a multi-step growth method of precisely controlling the particle size. The specific preparation method is:

[0046] 1) Weigh 3.00g of polyvinylpyrrolidone and 100mL of deionized water, fully dissolve the polyvinylpyrrolidone in deionized water; obtain a uniform solution, stir and heat to 75°C; weigh 2.25g of thioacetamide, and add to the reaction system; Measure 0.07mL concentrated nitric acid and add it to the reaction system; weigh 2.97g zinc nitrate hexahydrate, dissolve it in 5mL deionized water in advance, then quickly add it to the reaction system, stir vigorously at 1000rpm for 3min; reduce the stirring speed to 300-500rpm, stirring and reacting at 75°C for 2h;

[0047] 2) Weigh 2.97g zinc nitrate hexahydrate, pre-dissolve it in 5mL deionized water, then quickly add it into a three-neck flask, stir and react in a water bath for 2h; weigh 2.97g zinc nitrate hexahydra...

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Abstract

A highly uniform sulphide microsphere with precisely controllable particle size and a preparation method therefor. The present method is based on the idea of a core-shell-shell structure, and comprises the two processes of primary "core" growth and secondary "layer-layer" growth. In the first growth step, sulphide nanospheres with stable particle size are obtained by means of stable reaction conditions; in the subsequent steps, the particle size of the nanospheres can be precisely controlled by means of controlling the timing and amount of the addition of the metal and sulphur source. According to said synthesis method, by means of a preset target particle size and precisely designing the experiment steps, sulphide nanospheres of the target particle size can be obtained; in addition, the adjustable particle size range of the present method is significantly increased, the adjustable range being 100 nm-1000 nm.

Description

technical field [0001] The invention relates to highly uniform sulfide microspheres with precise and controllable particle diameters and a preparation method thereof, belonging to the field of preparation of photonic crystal materials. Background technique [0002] Semiconductor materials are widely used in solar cells, lasers, photocatalysis and other fields, among which a variety of metal sulfides are the main types of semiconductor materials, such as ZnS, CdS, CuS, PbS, SnS, HgS, MnS, FeS, NiS, CoS, etc. . Further studies have found that semiconductor materials at the micro-nano scale exhibit many unique physical and chemical phenomena, such as quantum effects and nonlinear optical effects. The above phenomena mainly depend on the size, shape and structure of the material. Monodisperse microspheres eliminate the influence of shape on material properties, and the controllable particle size of microspheres can further study the influence of material size on properties. T...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G9/08C01G3/12C01G11/02C01G13/00C01G19/00C01G21/21C01G45/00C01G49/12C01G51/00C01G53/11B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01G3/12C01G9/08C01G11/02C01G13/00C01G19/00C01G21/21C01G45/00C01G49/12C01G51/00C01G53/11
Inventor 武素丽吴越常杰
Owner DALIAN UNIV OF TECH
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