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A kind of preparation method of high-purity chalcogenide glass

A technology of chalcogenide glass and high-purity sulfur is applied in the field of preparation of high-purity chalcogenide glass, which can solve the problems of affecting the infrared transmission performance of optical fibers, difficult to control the dosage of deoxidizer, affecting the deoxidizing effect of aluminum, etc. Increased light scattering loss, avoidance of defects, and improved infrared transmittance

Active Publication Date: 2017-12-26
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when aluminum is used as the oxygen scavenger, since the reaction product is dense alumina, on the one hand, it affects the subsequent oxygen removal effect of aluminum, and on the other hand, the alumina will react with -OH in the quartz tube wall to form a Corrosion of the wall; there is no corrosion problem of quartz tubes when magnesium is used as an oxygen scavenger. It is a recognized high-efficiency oxygen scavenger, but due to the low melting and boiling point (648°C / 1107°C) of magnesium, it may cause some magnesium to enter after distillation. become impurities in the glass or form crystallites leading to increased scattering
In actual use, the dosage of oxygen scavenger is difficult to control, and the general dosage ranges from 300-1000ppm. Too little dosage will affect the oxygen removal effect, and too much dosage will increase the crystallite scattering, which will affect the infrared transmission performance of the optical fiber.

Method used

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  • A kind of preparation method of high-purity chalcogenide glass
  • A kind of preparation method of high-purity chalcogenide glass

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Embodiment 1

[0021] Embodiment one: with Ge 15 As 25 Se 15 Te 45 Take tellurium-based chalcogenide glass as an example, which is prepared by the preparation method of the present invention, and the specific preparation steps are:

[0022] (1) Pretreatment of quartz ampoules: prepare quartz ampoules with a hydroxyl content lower than 3ppm, such as figure 1 As shown, the quartz ampoule includes a purification glass tube 1, a first connecting tube 2, a capillary tube 3, a distillation tube 4 and a second connecting tube 5 connected in sequence. Pre-dehydroxylation treatment, then wash with deionized water for 6 to 8 times, and then dry;

[0023] (2) Preparation of mixed raw materials for chalcogenide glass: use simple Ge, As, Se and Te with a purity of 99.999% as raw materials, and prepare Ge 15 As 25 Se 15 Te 45 Tellurium-based chalcogenide glass mixed raw material 40g, based on the mass of the prepared tellurium-based chalcogenide glass mixed raw material, simultaneously add 300ppm ...

Embodiment 2

[0028] Embodiment two: with Ge 20 Se 10 Te 70 Take tellurium-based chalcogenide glass as an example, which is prepared by the preparation method of the present invention, and the specific preparation steps are:

[0029] (1) Pretreatment of quartz ampoules: prepare quartz ampoules with a hydroxyl content lower than 3ppm, such as figure 1 As shown, the quartz ampoule includes a purification glass tube 1, a first connecting tube 2, a capillary tube 3, a distillation tube 4 and a second connecting tube 5 connected in sequence. Pre-dehydroxylation treatment, then wash with deionized water for 6 to 8 times, and then dry;

[0030] (2) Preparation of mixed raw materials for chalcogenide glass: use simple Ge, Se and Te with a purity of 99.999% as raw materials, and prepare Ge 20 Se 10 Te 70 Tellurium-based chalcogenide glass mixed raw material 40g, based on the mass of the prepared tellurium-based chalcogenide glass mixed raw material, simultaneously add 250ppm mass percent of hi...

Embodiment 3

[0034] Embodiment three: with Ge 10 As 15 Te 75 Take tellurium-based chalcogenide glass as an example, which is prepared by the preparation method of the present invention, and the specific preparation steps are:

[0035] (1) Pretreatment of quartz ampoules: prepare quartz ampoules with a hydroxyl content lower than 3ppm, such as figure 1 As shown, the quartz ampoule includes a purification glass tube 1, a first connecting tube 2, a capillary tube 3, a distillation tube 4 and a second connecting tube 5 connected in sequence. Pre-dehydroxylation treatment, then wash with deionized water for 6 to 8 times, and then dry;

[0036] (2) Preparation of mixed raw materials for chalcogenide glass: using simple Ge, As and Te with a purity of 99.999% as raw materials, it is prepared as Ge 10 As 15 Te 75 Tellurium-based chalcogenide glass mixed raw material 40g, based on the mass of the prepared tellurium-based chalcogenide glass mixed raw material, simultaneously add 250ppm mass per...

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Abstract

The invention discloses a preparation method for high-purity chalcogenide glass. In the preparation process, 200-300 ppm high purity magnesium and2000-3000 ppm high purity gallium are introduced to be used as deoxidant, the purity of the high purity magnesium and the purity of the high purity gallium are both larger than or equal to 99.999%, and then purification through a closed distillation method and high temperature melting are performed to obtain the uniform high-purity chalcogenide glass. According to the preparation method, plenty of high purity gallium and a small amount of high purity magnesium are used as the deoxidant, so that oxygen impurities in the chalcogenide glass are removed at high efficiency, the purity is increased substantially, scattering of microcrystals in the chalcogenide glass is reduced substantially, the oxygen removal purpose is effectively achieved, scattering caused by corrosion of a quartz tube and a heterogeneous inclosure formed by metal magnesium or aluminum is solved, and finally the high-purity chalcogenide glass with uniform quality is obtained. The high-purity chalcogenide glass is uniform in transmission in an infrared waveband, little in light scattering and free of obvious oxide absorption peaks and can be widely applied to the field of intermediate and far infrared optical fibers.

Description

technical field [0001] The invention relates to the technical field of preparation of optical glass, in particular to a preparation method of high-purity chalcogenide glass. Background technique [0002] Chalcogenide glass refers to an amorphous material formed by introducing elements such as Ge, As, Sb, Sn, Ga, etc., using Group VIA elements of the periodic table, sulfur, selenium, and tellurium as anions. Due to its higher atomic mass and weaker chemical bond energy, chalcogenide glass has lower vibrational phonon energy, which makes it have excellent mid-to-far infrared transmission properties (depending on the composition, its transmission range can range from 0.5- 1um ~ 12-25um), high refractive index (2.0 ~ 3.5), high nonlinear coefficient (100 ~ 1000 times that of quartz materials), among which the infrared transmission window of several telluride glasses is the widest (1.5 ~ 25um or more). Chalcogenide glasses can be used in infrared biochemical sensing technology, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C03C3/32C03C1/00C03C4/10
CPCC03C1/00C03C3/321C03C4/10
Inventor 赵浙明王训四戴世勋聂秋华江岭吴波潘章豪孙礼红刘硕密楠
Owner NINGBO UNIV