Preparation device and preparation method of high-purity multispectral chalcohalide glasses

Abstract

The invention discloses a preparation device and preparation method of high-purity multispectral chalcohalide glasses. The preparation device comprises a quartz tube group, a solid-liquid separation and purification device comprising a first electric heating furnace and a solid-liquid separation container and a material leakage tube connected at the lower part of the solid-liquid separation container and used for separating and purifying gallium, a water elimination and purification device comprising a second electric heating furnace and a vacuum pump, and a distillation and purification device comprising a third electric heating furnace and a circulating water cooling mechanism; the preparation device and preparation method of the high-purity multispectral chalcohalide glasses disclosed by the invention have the advantages of being capable of effectively removing oxide impurities on the surface of the gallium taken as a raw material by using the solid-liquid separation and purification device to purify the high-boiling point raw material, namely the gallium and effectively removing free water and crystal water and avoiding introducing new impurities by using the water elimination and purification device and further matching with organic water removers and realizing distillation and purification of halide containing chalcogenide glasses by using the distillation and purification device, and further being capable of effectively preventing deoxidant failures because the decomposition of halides volatilizes halogen elements in the distillation process by the circulating water cooling mechanism to achieve a purification effect.

Description

Technical field [0001] The invention relates to a glass preparation technology, in particular to a preparation device and a preparation method of high-purity multispectral sulfide halogen glass. Background technique [0002] With the popularization and new development of infrared night vision and visible imaging technology, more and more occasions need to combine the high resolution and low cost of visible imaging, as well as the wide spectrum of infrared imaging and special night vision applications. Develop new glass materials that can transmit visible light and infrared windows at the same time. [0003] As we all know, chalcogenide glass is an infrared optical material with a wide infrared transmission range, low cost, and easy precision molding of lenses. It has been widely used in infrared detection, thermal imaging, infrared guidance and other fields. Chalcogenide glass is a glass system that is mainly based on chalcogen elements and introduces a certain amount of other met...

AI Technical Summary

Problems solved by technology

Although multi-spectral chalcohalide glass can transmit in multiple bands and has a wider infrared transmission range than conventional chalcogenide glass, the added halide raw materials have strong hygroscopicity and deliquescence, and it is easy to introduce more free Water and crystal water will increase the absorption of impurities in the 3-5μm band; on the other hand, the halides are easy to decompose and volatilize the halogen element, which will react with the oxygen scavenger to make the oxygen scavenger ineffective, which will increase the difficulty of glass purification. The traditional chalcogenide glass purification technology cannot achieve the purification effect at all; in addition, the glass will easily contain oxygen or Fe, Cr and other trace transition metal impurities from the surface of the glass raw material, which will produce 8-12μm spectral range Infrared absorption band of oxide impurities, resulting in absorption loss and scattering loss, which will reduce the glass transmittance

[0005] At present, although there are component designs or simple preparation techniques for related sulfur halide glass, there are no related reports on the purification device and process technology of sulfur halide glass

In the existing chalcogenide glass purification technology, all of them are aimed at the distillation and purification of conventional chalcogenide glass without halides. This type of chalcogenide glass purification technology cannot be applied to the chalcogenide glass, because Halides are easy to decompose and volatilize simple halogen, which will react with the oxygen scavenger to make the oxygen scavenger ineffective, thus failing to achieve the glass purification effect

Moreover, most of the chalcogenide glass purification technologies in this type of chalcogenide glass purification technology are limited by the temperature resistance of the quartz ampoule itself, and are only purified for low boiling point high vapor pressure glass, such as the invention patent announced by China "a high-purity Preparation device and preparation method of chalcogenide glass" (authorized announcement number CN 101492235B), which adopts a high-temperature melting method for intermeltable low-boiling raw materials to form low-boiling eutectic components, thereby gas Purification and condensation of chalcogenide glass raw materials, the process equipment is complex, easy to introduce non-volatile non-eutectic components (Si, MgSe, etc.), generally for the purification of eutectic high vapor pressure component glass, not applicable Purification of halide glass containing low vapor pressure components gallium and easily decomposed volatile components

At present, there are also purification technologies for high-boiling-point component glasses, such as the "Preparation Device and Preparation Method for Gallium-Containing High-melting-Boiling-Point Chalcogenide Glass" announced by China (authorized announcement number CN 102786222 B), which aims at high-melting boiling point glass. For chalcogenide glass, use a rapid heating furnace to heat the glass raw material pipe and the connecting pipe at the same time, and heat it to 1400°C within 10 seconds, so that the raw materials in the glass raw material pipe are completely distilled into the purification pipe through the connecting pipe to achieve the purpose of purification. This method It has high requirements on equipment, and it is easy to introduce impurities such as carbon and silicon in the quartz glass tube at a high temperature of 1400 ° C, and is not suitable for distillation and purification of glass doped with halides

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