Preparation method of nano-crystal doped optical glass

A technology of optical glass and nanocrystal, which is applied in the field of preparation of nanocrystal-doped optical glass, can solve problems such as nanocrystal damage, cracking of silica bulk materials, and interface compatibility problems, and achieve simple process and high product quality. The effect of low cost, easy transportation and storage

Active Publication Date: 2014-09-03
ZHIJING NANOTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this regard, the predecessors have made many attempts, but there is no perfect route to prepare optical glass doped with semiconductor nanocrystals. The main problems are as follows: (1) Due to the interface compatibility problem, it is impossible to High doping concentration while maintaining the transparency of optical glass devices
(2) The recombination process severely damages the nanocrystals, and their fluorescence properties deteriorate
(3) Due to the fact that the silica bulk material prepared by the sol-gel method is prone to cracking, it is impossible to obtain large-area and regular-shaped optical glass devices
(4) There are few types of semiconductor nanocrystals suitable for doping methods, and the scope of application is limited
[0006] In summary, since the current high-quality semiconductor nanocrystalline materials are mainly synthesized by the oil-phase solution method, the obtained oil-soluble nanoparticles have poor compatibility with the alcohol-water system of the sol-gel method, and it is impossible to obtain high-quality optical properties. composite material

Method used

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  • Preparation method of nano-crystal doped optical glass
  • Preparation method of nano-crystal doped optical glass
  • Preparation method of nano-crystal doped optical glass

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preparation example Construction

[0028] The preparation method of seed nanocrystal doped optical glass proposed by the present invention comprises the following steps:

[0029] (1) Mix the oil-soluble semiconductor nanocrystalline material with a high-boiling point organic solvent at a mass concentration of 1-50 mg / mL, and heat it to 120-200° C. under the protection of high-purity nitrogen or argon inert gas to obtain a mixed solution; wherein Described semiconductor nanocrystal material can be precious metal nanocrystals such as Au, Ag, CuInS 2 / ZnS, CuInSe 2 / ZnS, AgInS 2 / ZnS, AgInSe 2 Group I-III-VI nanocrystals such as ZnS, Group III-V nanocrystals such as InP and GaInN, Group II-VI nanocrystals such as ZnS, ZnSe, CdSe, CdSe / CdS, CdSe / ZnS, CdTe / CdS, CdZnTe / CdS crystal, CuS, Cu 1.75 S, Cu 1.8 S, Cu 1.81 S, Cu 1.97 S, Cu 2 S and other metal sulfide nanocrystals, Fe 3 o 4 , Fe 2 o 3 metal oxide nanocrystals or Zn 3 N 2 Any one of them, the high-boiling organic solvent is octadecene, N,N-dimeth...

Embodiment 1

[0040] (1) Mix the oil-soluble semiconductor nanocrystalline material with a high boiling point organic solvent at a mass concentration of 40mg / mL, and heat it to 130°C under the protection of high-purity nitrogen to obtain a mixed solution; wherein the semiconductor nanocrystalline material is Au nanocrystals, the high boiling point organic solvent is N,N-dimethylformamide;

[0041] (2) add surface ligand in above-mentioned mixed solution, the mol ratio of adding is: mixed solution: surface ligand=500:1, after stirring for 10 minutes, obtain reaction product, wherein said surface ligand is 6- Mercaptohexanol;

[0042] (3) the reaction product of step (2) is dissolved in the solvent, and described solvent is methyl alcohol, then adds acetone, obtains precipitation, and precipitation is carried out centrifugation, centrifugation speed is 7000rpm, and centrifugation time is after 3 minutes, Pour off the supernatant and take the lower layer of precipitation, repeat this step two...

Embodiment 2

[0049] (1) Mix the oil-soluble semiconductor nanocrystalline material with a high boiling point organic solvent at a mass concentration of 30mg / mL, and heat it to 130°C under the protection of high-purity nitrogen to obtain a mixed solution; wherein the semiconductor nanocrystalline material is CuInS 2 / ZnS core-shell nanocrystals, the high boiling point organic solvent is octadecene;

[0050] (2) add surface ligand in above-mentioned mixed solution, the mol ratio of adding is: mixed solution: surface ligand=1000:1, after stirring for 20 minutes, obtain reaction product, wherein said surface ligand is 6- Mercaptohexanol;

[0051] (3) The reaction product of step (2) is dissolved in the solvent, and described solvent is ethanol, then adds normal hexane, obtains precipitation, and precipitation is carried out centrifugation, and centrifugation speed is 7000rpm, and centrifugation time is after 3 minutes , pouring off the supernatant and taking the lower layer of precipitation, ...

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Abstract

The invention relates to a preparation method of nano-crystal doped optical glass, belonging to the technical field of optical material preparation. The method comprises the steps of firstly mixing an oil-soluble semiconductor nano-crystal material with an organic solvent with a high boiling point, and adding a surface ligand to obtain a reaction product; dissolving the reaction product into the solvent to obtain an alcohol-soluble nano-crystal material; preparing premixed liquid comprising an alcohol solvent, (3-sulfydryl propyl) trimethoxy silane, tetraethoxysilane, diethoxydimethylsilane and (3-amino propyl) triethoxysilane, mixing the alcohol-soluble nano-crystal material or the oil-soluble nano-crystal material with the premixed liquid, adding additives, forming a sol, sealing, and standing and curing to obtain an optical glass material. The preparation method is simple in technological process, and does not need a high-temperature and high-pressure experimental environment, so that a product is low in cost; the premixed liquid for forming the optical glass can be kept in an uncured state for a long time, so that the optical glass is convenient for transportation and storage.

Description

technical field [0001] The invention relates to a method for preparing nanocrystal-doped optical glass, which belongs to the technical field of optical material preparation. Background technique [0002] Optical glass is the foundation and an important part of the optoelectronic technology industry. Especially after the 1990s, with the continuous integration of optics, electronic information science, and new material science, the application of optical glass as the basic material of optoelectronics in the three major fields of optical transmission, optical storage, and optoelectronic lighting and display has advanced by leaps and bounds. It has become one of the basic conditions for the development of social informatization, especially the development of optoelectronic information technology. [0003] The main function of optical glass is to change the direction of light propagation, or to change the relative spectral distribution of ultraviolet, visible and infrared light....

Claims

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Application Information

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IPC IPC(8): C03C14/00
Inventor钟海政柏泽龙樊世成邹炳锁
OwnerZHIJING NANOTECH CO LTD