Sulfide highly-uniform microsphere with precisely controllable particle size and preparing method thereof

A sulfide, precise technology, applied in chemical instruments and methods, copper sulfide, lead 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: 2019-06-28
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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  • Sulfide highly-uniform microsphere with precisely controllable particle size and preparing method thereof
  • Sulfide highly-uniform microsphere with precisely controllable particle size and preparing method thereof
  • Sulfide highly-uniform microsphere with precisely controllable particle size and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

[0032] 2) Weigh 2.97g zinc nitrate hexahydrate, dissolve it in 5mL deionized water in advance, then quickly add it to a three-necked flask, stir and react in a wa...

Embodiment 2

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

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

[0041] 2) Weigh 2.97 g of zinc nitrate hexahydrate, dissolve it in 5 mL of deionized water in advance, and then quickly add it to a three-necked fla...

Embodiment 3

[0045] Through a multi-step growth method that precisely regulates the particle size, monodisperse ZnS nanospheres with a particle size of 1000 ± 5 nm are prepared. The specific preparation method is:

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

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

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Abstract

The invention discloses a sulfide highly-uniform microsphere with the precisely controllable particle size and a preparing method thereof. The method includes the primary core growth step and the secondary layer-layer growth step on the basis of the concept of the core-shell-shell structure. In the primary growth step, through stable reaction conditions, the sulfide nanosphere with the stable particle size is obtained; in the subsequent step, the adding moments and amounts of metal salt and a sulfur source are controlled, and then the particle size of the nanospheres can be precisely controlled. According to the synthesis method, the sulfide microsphere with the target particle size can be obtained by precisely designing test steps through the preset target particle size; meanwhile, by means of the method, the controllable particle size range is obviously increased, and the controllable range is 100-1000 nm.

Description

Technical field [0001] The invention relates to a highly uniform sulfide microsphere with precise and controllable particle size and a preparation method thereof, and belongs to the field of photonic crystal material preparation. Background technique [0002] Semiconductor materials are widely used in solar cells, lasers, photocatalysis and other fields. Among them, 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 research found that semiconductor materials of the micro-nano size level exhibit many unique physical and chemical phenomena, such as quantum effects, nonlinear optical effects, etc. The above-mentioned phenomena mainly depend on the size, shape and structure of the material. Monodisperse microspheres eliminate the influence of shape on the properties of materials, and the particle size of the microspheres can be controlled to further study the influence of material size...

Claims

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Application Information

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Patent Type & Authority Applications(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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