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Preparation method of high-purity and low-loss chalcogenide glass

A chalcogenide glass, low-loss technology, used in glass manufacturing equipment, glass furnace equipment, manufacturing tools, etc., can solve the problem of introducing micron-scale heterogeneous inclusions, and achieve small light scattering, good uniformity, and heterogeneous packaging. body reduction effect

Inactive Publication Date: 2015-06-17
XUZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing high-purity and low-loss chalcogenide glass, which solves the problem that the traditional preparation method is easy to introduce micron-sized heterogeneous inclusions into the glass

Method used

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  • Preparation method of high-purity and low-loss chalcogenide glass
  • Preparation method of high-purity and low-loss chalcogenide glass

Examples

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Effect test

Embodiment 1

[0028] Example 1: The composition of the chalcogenide glass is Ge 12 As 24 Se 64

[0029] Using Ge with a purity of 99.999% and elements As and Se with a purity of 99.9999% as raw materials, according to the above chemical composition ratio, add 100ppm of metal Al with a purity of 99.999% and 1000ppm of ultra-dry GaCl with a purity of 99.999% 3 , weighed in a nitrogen-filled glove box with an oxygen and water content of less than 0.1 ppm and loaded into a pre-cleaned quartz ampoule with a hydroxyl content of less than 1 ppm; vacuumize the quartz ampoule containing the mixture, and when the ampoule Vacuum degree≤10 –3 At Pa, place the ampoule at 120 o Bake in a tube furnace in C for 2 hours, then seal the ampoule with an oxyhydrogen flame; put the sealed quartz ampoule with the glass mixture in a swing furnace, and slowly heat up to 900 o C, after 10 hours of heat preservation, take it out and cool it in the air, and then heat it at 200 o C annealed for 2 hours; open the ...

Embodiment 2

[0030] Example 2: The composition of chalcogenide glass is As 40 S 60

[0031] Using elements As and S with a purity of 99.9999% as raw materials, according to the above chemical composition ratio, add 200ppm of metal Mg with a purity of 99.999% and 1500ppm of ultra-dry GaCl with a purity of 99.999% 3 , weighed in a nitrogen-filled glove box with an oxygen and water content of less than 0.1 ppm and loaded it into a pre-cleaned quartz ampoule with a hydroxyl content lower than 1 ppm; vacuumize the quartz ampoule containing the mixture, and when the vacuum in the ampoule degree≤10 –3 At Pa, place the ampoule at 100 o Bake in a tube furnace in C for 3 hours, then seal the ampoule with an oxyhydrogen flame; put the sealed quartz ampoule with the glass mixture in a swing furnace, and slowly heat up to 850 o C, after 15 hours of heat preservation, take it out and cool it in the air, and then heat it at 190 o C annealed for 3 hours; the annealed ampoule filled with glass was ope...

Embodiment 3

[0032] Example 3: The composition of the chalcogenide glass is Te 20 As 30 Se 50

[0033] Using elements As, Te and Se with a purity of 99.9999% as raw materials, according to the above chemical composition ratio, add 150ppm of metal Zr with a purity of 99.999% and 500ppm of ultra-dry GaCl with a purity of 99.999% 3 In a nitrogen-filled glove box with an oxygen and water content of less than 0.1ppm, weigh the material and put it into a pre-cleaned quartz ampoule with a hydroxyl content of less than 1ppm; vacuumize the quartz ampoule containing the mixture, when the vacuum in the ampoule ≤10 –3 At Pa, place the ampoule at 150 o Bake in a tube furnace in C for 1 hour, and then seal the ampoule with an oxyhydrogen flame; put the sealed quartz ampoule with the glass mixture in a swing furnace, and slowly heat up to 800 o C, after 10 hours of heat preservation, take it out and cool it in the air, and then heat it at 132 o C annealed for 2 hours; the annealed ampoule filled wi...

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Abstract

The invention provides a preparation method of high-purity and low-loss chalcogenide glass, belonging to a preparation method of the chalcogenide glass. The preparation method comprises the following steps of: removing hydrocarbon impurity in the glass by taking ultra-dry gallium chloride as a purifying agent, and distilling and purifying the glass in combination with the conventional deoxidant, aluminum, magnesium or zirconium metal; placing glass mixture into a quartz ampoule to be sealed in by means of vacuum supply, founding the glass mixture in a vacuum ampoule, dynamically distilling the glass, and remelting the mixture after distilling; and effectively removing the hydrocarbon impurity in the glass by taking the ultra-dry gallium chloride as the purifying agent, so that the Mie scattering imperfection is hardly formed in the finally-obtained high-purity chalcogenide glass, and the low-loss homogeneous glass can be obtained. According to the high-purity chalcogenide glass synthesized by the preparation method provided by the invention, the minimum loss under the infrared transmission waveband is less than 0.3dB / m, and the corresponding loss of the absorption peak of the residual impurity is less than 8dB / m, so that the preparation method can be used in the field of an infrared glass optical element and an infrared optical fiber. The ultra-dry gallium chloride purifying agent can be easily obtained, and is lower in price; the carbon, hydrogen and oxygen impurities can be removed from the chalcogenide glass at high efficiency; the prepared chalcogenide glass is better in uniformity and less in light scattering.

Description

technical field [0001] The invention relates to a preparation method of chalcogenide glass, in particular to a preparation method of high-purity and low-loss chalcogenide glass. Background technique [0002] Chalcogenide glass refers to an amorphous material formed by introducing a certain amount of other metal or non-metal elements based on the VIA group elements S, Se, and Te of the periodic table. Due to their higher atomic mass and weaker chemical bond strength, chalcogenide glasses have lower vibrational phonon energies, which give them excellent transmission properties in the infrared range. Among chalcogenide glasses, the typical transmission ranges of sulfide, selenide and telluride glasses are 0.5-10μm, 0.8-14μm, 1.5-20μm, respectively. Infrared optical components and drawn optical fibers made of chalcogenide glass have extremely important application background and potential in the fields of thermal imaging, infrared laser transmission, chemical and biological sen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03B5/16C03C6/00
Inventor 张斌杨志勇任和张鸣杰章健唐定远
Owner XUZHOU NORMAL UNIVERSITY
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