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Inorganic lead-cesium halide nanocrystalline composite chalcogenide glass ceramic material and preparation method thereof

A nanocrystalline composite and chalcogenide glass technology, which is applied in glass manufacturing equipment, glass furnace equipment, manufacturing tools, etc., can solve the problems of unobtained chalcogenide glass ceramics, and achieve the effect of improving thermodynamic stability and environmental impact resistance

Active Publication Date: 2019-06-25
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, although there are CsCl, RbI and Cs in chalcogenide glasses 3 LaCl 6 and other halide nanocrystallization studies have been reported, but CsPbX has never been obtained 3 Chalcogenide Glass-ceramics Composite with Perovskite Nanocrystals

Method used

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  • Inorganic lead-cesium halide nanocrystalline composite chalcogenide glass ceramic material and preparation method thereof
  • Inorganic lead-cesium halide nanocrystalline composite chalcogenide glass ceramic material and preparation method thereof
  • Inorganic lead-cesium halide nanocrystalline composite chalcogenide glass ceramic material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: Get X to be Cl, x=0.3, y=0.1, z=0.06, the molar composition of chalcogenide glass-ceramic material is represented by chemical formula: 54GeS 2 30Sb 2 S 3 10Ga 2 S 3 6CsPbCl 3 , according to the molar composition to calculate the raw materials Ge, Ga, Sb, S, CsCl and PbCl 2 Weigh and mix homogeneously in a glove box full of inert gas; then put the homogeneously mixed raw materials into a quartz tube, which is pre-soaked in aqua regia for 2 hours and washed with deionized water before drying, Vacuum again, when the vacuum in the quartz tube is 10 -3 Seal with an oxyacetylene flame at Pa; heat the sealed quartz tube in a swing furnace, first raise the temperature to 340°C at a rate of 2°C / min, keep it warm for 3 hours, and then raise the temperature at a rate of 4°C / min Heat at 750°C for 2 hours; then slowly rise to 920°C at a rate of 1°C / min, swing and melt for 10 hours; then cool down to 850°C at a rate of 3°C / min; stand the quartz ampoule upright for...

Embodiment 2

[0024] Embodiment 2: Take X as Cl, x=0.5, y=0.12, z=0.08, and the molar composition of the chalcogenide glass-ceramic material is expressed as: 30GeS 2 50Sb 2 S 3 12Ga 2 S 3 8CsPbCl 3 , according to the molar composition to calculate the raw materials Ge, Ga, Sb, S, CsCl and PbCl 2 Weigh and mix homogeneously in a glove box full of inert gas; then put the homogeneously mixed raw materials into a quartz tube, which is pre-soaked in aqua regia for 2 hours and washed with deionized water before drying, Vacuum again, when the vacuum in the quartz tube is 10 -3 Seal with an oxyacetylene flame at Pa; put the sealed quartz tube into a swing furnace to heat, first raise the temperature to 340°C at a rate of 2°C / min, keep it warm for 3 hours, and then raise the temperature at a rate of 5°C / min Heat at 750°C for 2 hours; then slowly raise the temperature to 850°C at a rate of 1°C / min, shake and melt for 10 hours; then cool down to 800°C at a rate of 2°C / min; stand the quartz ampou...

Embodiment 3

[0025] Embodiment 3: Taking X as Br, x=0.4, y=0.2, z=0.07, the molar composition of the chalcogenide glass-ceramic material is expressed as: 33GeS 2 40Sb 2 S 3 20Ga 2 S 3 7CsPbBr 3 , according to the molar composition to calculate the raw materials Ge, Ga, Sb, S, CsBr and PbBr 2 Weigh and mix homogeneously in a glove box full of inert gas; then put the homogeneously mixed raw materials into a quartz tube, which is pre-soaked in aqua regia for 2 hours and washed with deionized water before drying, Vacuum again, when the vacuum in the quartz tube is 10 -3 Seal with an oxyacetylene flame at Pa; heat the sealed quartz tube in a swing furnace, first raise the temperature to 340°C at a rate of 2°C / min, keep it warm for 3 hours, and then raise the temperature at a rate of 3°C / min Heat at 750°C for 2 hours; then slowly raise the temperature to 900°C at a rate of 1°C / min, shake and melt for 8 hours; then cool down to 840°C at a rate of 2°C / min; stand the quartz ampoule upright fo...

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Abstract

The molar composition of the inorganic lead-cesium halide nanocrystalline composite chalcogenide glass ceramic material disclosed by the invention is shown as a chemical formula, (1-x-y-z)GeS2.XSb2S3.YGa2S3.ZCsPbX3, wherein x = 0.15-0.75, y = 0.05-0.2, z = 0.05-0.1, and X is Cl, Br or I; and CsPbX3 is compounded in the chalcogenide glass ceramic material in the form of separated nanocrystalline. The material is transparent in a spectral range of 2-10 micrometers and has good thermal and chemical stability and good fracture toughness, so that the material is suitable for rare earth ion doping to research and develop novel mid-infrared light-emitting or laser materials and related quantum dot light-emitting materials. The preparation method of the material comprises the following steps: by taking GeS2-Sb2S3-Ga2S3 as a glass matrix, adding a CsPbX3 component which is nearly saturated; preparing basic chalcogenide glass by a melting quenching method; and performing crystallization heat treatment so that CsPbX3 nanocrystals are controllably separated out. According to the preparation method of the material, proper glass composition can be designed and selected according to functional requirements, so that the size and distribution of precipitated CsPbX3 crystal grains are controlled.

Description

technical field [0001] The invention belongs to the field of functional glass ceramic materials, in particular to an inorganic lead halide cesium nanocrystal composite chalcogenide glass ceramic material and a preparation method thereof, which can be applied to the fields of infrared optics and photonics. Background technique [0002] Inorganic perovskite CsPbX 3 (X=Cl,Br,I) nanocrystals have unique optical versatility, high luminescence quantum efficiency, and easy preparation, which have attracted extensive attention of researchers. However, CsPbX 3 Materials are not stable in oxidative and humid atmospheric environments, which greatly limits their applications in various optoelectronic fields, such as solar cells, lasers, and displays. Therefore, in order to improve the CsPbX 3 To stabilize nanocrystals, an effective method is to compound them with inert matrices such as organic polymers or inorganic glasses. [0003] It is well known that photofunctional nanocrystall...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C10/16C03C4/12C03C4/10C03C6/06C03B5/16C03B25/00C03B32/02
Inventor 林常规王景松赵旭浩刘雪云焦清张培晴
Owner NINGBO UNIV
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