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A preparation device and method for high-purity multi-spectral sulfur halide glass

A technology of sulfur halide glass and preparation equipment, which is applied in the production equipment and field of high-purity multi-spectral sulfur halide glass, which can solve the problems of absorption loss, limited temperature resistance, scattering loss, etc., and achieve strong hygroscopicity and low boiling point Effect

Inactive Publication Date: 2019-06-25
NINGBO UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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  • A preparation device and method for high-purity multi-spectral sulfur halide glass
  • A preparation device and method for high-purity multi-spectral sulfur halide glass
  • A preparation device and method for high-purity multi-spectral sulfur halide glass

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Embodiment 1

[0036] This embodiment proposes a preparation device for high-purity multi-spectral sulfur halide glass, such as figure 1 , figure 2 and image 3 As shown, it includes a quartz tube group, a solid-liquid separation for gallium separation and purification composed of a first electric heating furnace 11, a solid-liquid separation container 12, and a leakage tube 13 connected to the lower right side of the solid-liquid separation container 12. Purification device 1, moisture removal and purification device 2 made up of the second electric heating furnace 21 and vacuum pump 22, distillation purification device 3 made up of the third electric heating furnace 31 and circulating water cooling mechanism 32; the quartz tube group consists of quartz raw material tubes 41, The first quartz connection tube 42, quartz purification tube 43 and the second quartz connection tube 44 are formed, the quartz purification tube 43 is integrally provided with a barbed quartz capillary 45, and the ...

Embodiment 2

[0042] This embodiment proposes a method for preparing high-purity multi-spectral Ge 15 Ga 15 Se 50 (CsI) 20 The preparation method of sulfur halide glass, it comprises the following steps:

[0043] ① Clean and dry the quartz raw material tube 41, the first quartz connecting tube 42, the quartz purification tube 43, the barbed quartz capillary tube 45 and the second quartz connecting tube 44 to complete the dehydroxylation pretreatment.

[0044] Here, the dehydroxylation pretreatment is to remove the impurities in the quartz raw material tube 41, the first quartz connecting tube 42, the quartz purification tube 43, the barbed quartz capillary tube 45 and the second quartz connecting tube 44, and remove the residual moisture after cleaning .

[0045] ②Put solid gallium into the solid-liquid separation container 12; then use the first electric heating furnace 11 to heat the solid-liquid separation container 12, so that the solid-liquid separation container 12 is heated to 45...

Embodiment 3

[0057] This embodiment proposes a method for preparing high-purity multi-spectral Ge 15 Ga 15 Se 50 (CsI) 20 The preparation method of sulfur halide glass, it comprises the following steps:

[0058] ① Clean and dry the quartz raw material tube 41, the first quartz connecting tube 42, the quartz purification tube 43, the barbed quartz capillary tube 45 and the second quartz connecting tube 44 to complete the dehydroxylation pretreatment.

[0059] Here, the dehydroxylation pretreatment is to remove the impurities in the quartz raw material tube 41, the first quartz connecting tube 42, the quartz purification tube 43, the barbed quartz capillary tube 45 and the second quartz connecting tube 44, and remove the residual moisture after cleaning .

[0060] ②Put solid gallium into the solid-liquid separation container 12; then use the first electric heating furnace 11 to heat the solid-liquid separation container 12, so that the solid-liquid separation container 12 is heated to 50...

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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 method for high-purity multi-spectral sulfur halide 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, which requires Develop new glass materials that transmit both visible light and the infrared window of the atmosphere. [0003] As we all know, chalcogenide glass is an infrared optical material with a wide infrared transmission range, low cost, and easy precision molded lenses. It has been widely used in infrared detection, thermal imaging, infrared guidance and other fields. Chalcogenide glass is a glass system mainly composed of chalcogen elements and introducing a certain amount of othe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C3/32
CPCC03C3/323
Inventor 应飞飞李茂忠沈祥王训四子光平郭晨宇戴世勋王侃白玉琢姜杰徐铁峥聂秋华
Owner NINGBO UNIV
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