Preparation method and equipment of Ge-Sb-Se systematic infrared glass

A technology of ge-sb-se and infrared glass, which is applied in the field of preparation of Ge-Sb-Se system infrared glass, can solve problems affecting the imaging quality and stability of thermal imaging systems, fluctuations in the composition and performance of chalcogenide glass products, and difficult operation etc. to achieve the effects of reducing the difficulty of volatilization control, improving optical uniformity, and ensuring yield

Active Publication Date: 2013-08-07
CHINA BUILDING MATERIALS ACAD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The structure of the device is complex, the monitoring requirements for reaction temperature and pressure are high, and the operation is difficult
And once the volatilization of selenium is not

Method used

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  • Preparation method and equipment of Ge-Sb-Se systematic infrared glass
  • Preparation method and equipment of Ge-Sb-Se systematic infrared glass
  • Preparation method and equipment of Ge-Sb-Se systematic infrared glass

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Embodiment 1: preparation molecular composition is Ge 15 Sb 5 Se 80 chalcogenide infrared glass

[0034] (1) Preparation of batch materials: In this example, a total of 2000g batch materials were prepared, and 500g batch materials were prepared in four times each time; Ge, Se, Sb and Al with a purity of 5N grade (99.999% purity) were used; according to the atomic ratio Ge 15 Sb 5 Se 80 Carry out calculation and weighing, mix it to make 500g of batch material, then add 50ppm of oxygen scavenger Al based on the total amount of batch material, and put it into a Φ50 quartz ampoule; repeat the weighing of 3 parts of batch material according to the above steps , into three Φ50 quartz ampoules; put the above four quartz ampoules at 300°C, 10 -3 Vacuum baking under Pa condition for 3 hours to further remove impurities adsorbed on the surface of raw materials.

[0035] (2) Melting for the first time: Vacuumize the above-mentioned quartz ampoule containing the batch materi...

Embodiment 2

[0038] Embodiment 2: preparation molecular composition is Ge 35 Sb 10 Se 55 sulfur infrared glass

[0039] (1) Preparation of batch materials: 2000g of batch materials are prepared in this example, using Ge, Se, Sb and Al with a purity of 5N grade (99.999% purity); 35 Sb 10 Se 55 Carry out calculation and weighing, mix it to make a batch, then add 80ppm of oxygen scavenger Al based on the total amount of the batch, and put it into a Φ100 quartz ampoule; put the above quartz ampoule at 320 ° C, 10 -3 Vacuum baking under Pa condition for 8 hours to further remove impurities adsorbed on the surface of raw materials.

[0040] (2) Melting for the first time: Vacuumize the above-mentioned quartz ampoule containing the batch material and oxygen scavenger to 10 -3 Seal after Pa. Put the fused-sealed quartz ampoule in a swing furnace, heat up to 560°C at a rate of 8°C / min, keep at this temperature for 3 hours to fully react Se and Sb, and then heat up to 900°C at a rate of 3°C / m...

Embodiment 3

[0042] Embodiment 3: preparation molecular composition is Ge 25 Sb 25 Se 50 sulfur infrared glass

[0043] (1) (1) Prepare batch materials: 2000g batch materials are prepared in this example, using Ge, Se, Sb and Al with a purity of 5N grade (99.999% purity); 25 Sb 25 Se 50 Carry out calculation and weighing, mix it to make a batch, then add 100ppm of oxygen scavenger Al based on the total amount of the batch, and put it into a Φ100 quartz ampoule; put the above quartz ampoule at 350 ° C, 10 -3 Vacuum baking under Pa conditions for 10 hours to further remove impurities adsorbed on the surface of raw materials.

[0044] (2) Melting for the first time: Vacuumize the above-mentioned quartz ampoule containing the batch material and oxygen scavenger to 10 -3 Seal after Pa. Put the fused-sealed 4 quartz ampoules in a swing furnace, heat up to 580°C at a rate of 10°C / min, keep at this temperature for 5 hours to fully react Se and Sb, and then heat up at a rate of 4°C / min to 8...

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Abstract

The invention discloses a preparation method of Ge-Sb-Se systematic infrared glass and atmosphere protective equipment for the method. The method comprises the following steps of: preparation of batch: mixing Ce, Sb and Se glass raw materials and a deoxidant to form the batch to be pre-treated; first melting: heating the batch to 850-900 DEG C to obtain first glass liquid; then, cooling and quenching the first glass liquid to form glass clinker; second melting: transferring the glass clinker to the atmosphere protective equipment; raising the temperature of a melting room to 650-750 DEG C, and stirring to uniformly and adequately homogenize the glass clinker to form second glass liquid; and cooling, then standing the second glass liquid for a period of time and finally carrying out material moulding. The glass provided by the invention has the advantages that the prepared Ge-Sb-Se systematic infrared glass is stable in composition and performance and uniform in inner quality, so that the imaging quality of Ge-Sb-Se infrared optical system is further improved.

Description

technical field [0001] The invention relates to the technical field of preparation of selenium-based chalcogenide glass, in particular to a preparation method of Ge-Sb-Se system infrared glass with uniform optical, stable composition and large size and equipment used in the method. Background technique [0002] Ge-Sb-Se system infrared glass is a kind of infrared optical material with excellent performance. Its advantages are as follows: it has infrared transmission performance similar to that of single crystal germanium, and the transmission band covers three atmospheric windows; it has good light-thermal stability. characteristics, the temperature coefficient of refractive index is small and adjustable, and the temperature coefficient of refractive index of commercial Ge-Sb-Se system chalcogenide glass is less than 25% of that of single crystal germanium; the resource consumption of germanium is low, and it can be formed by precision molding technology, and the processing c...

Claims

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Application Information

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IPC IPC(8): C03C4/10C03C3/32
CPCC03C3/321
Inventor 刘永华祖成奎赵华王衍行韩滨陈江赵慧峰金扬利
Owner CHINA BUILDING MATERIALS ACAD
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