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Preparation device of gallium-containing chalcogenide glass having high melting point and high boiling point, and preparation method thereof

A technology of chalcogenide glass and preparation equipment, which is applied in the preparation equipment and field of high melting and boiling point chalcogenide glass, which can solve the problems of pressure cracking, pressure deformation, and low Ga vapor pressure parameter value, and achieve the effect of low impurity content

Inactive Publication Date: 2012-11-21
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chalcogenide glasses with high melting and boiling points generally have metal components, such as the melting point of Ge at 937.4°C, the boiling point at 2830°C, the boiling point of Ga at 2403°C, and the Ga vapor pressure parameter value is low, about 1.2×10 at 1050°C -4 Pa, the glass transition point of quartz glass used to hold glass raw materials in quartz glass tubes (containers) The softening point is 1730 o C, but the upper limit of the temperature that can work effectively for a long time is 1100 oC , if exposed to high temperature (1050-1750 o C), pressure deformation or pressure cracking will occur due to too low viscosity, and the traditional purification process takes at least one day, so these metal components are generally difficult to separate by traditional heating and gasification methods in quartz glass containers , In addition, there is currently no effective preparation device and preparation method for gallium-containing high-melting boiling point chalcogenide glass in the world.

Method used

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  • Preparation device of gallium-containing chalcogenide glass having high melting point and high boiling point, and preparation method thereof
  • Preparation device of gallium-containing chalcogenide glass having high melting point and high boiling point, and preparation method thereof

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Embodiment 1

[0015] Embodiment 1: A preparation device for gallium-containing high melting and boiling point chalcogenide glass, comprising an electric heating furnace 2, a rapid heating furnace 3 and an H-type quartz ampoule, the electric heating furnace 2 has a temperature control device, and the H-type quartz ampoule includes a glass The raw material tube A and the purified glass tube B, the glass raw material tube A and the purified glass tube B are connected through the connecting pipe C, the upper end of the glass raw material tube A is open, the upper end of the glass raw material tube A is connected to a vacuum pump, and the electric heating furnace 2 is used to heat the glass raw material A tube, the rapid heating furnace 3 is used to heat the glass feedstock tube A and connecting tube C at the same time.

[0016] Preparation of high-purity Ge 15 Te 75 Ga 10 Chalcogenide glass, the specific steps are as follows:

[0017] 1) According to the ratio of 15mol%, 75mol%, and 10mol% o...

Embodiment 2

[0024] Preparation of high-purity Ge 23 Se 65 Ga 12 Chalcogenide glass, the specific steps are as follows:

[0025] 1) The raw materials are 20g of germanium, selenium, and gallium in proportions of 23mol%, 65mol%, and 12mol%, respectively. At the same time, 0.005g of magnesium bars are put in according to the mass percentage of 0.025wt%, and TeCl is put into it according to the mass percentage of 0.025wt%. 4 0.005 g, put into pre-dehydroxylated glass feedstock tube A;

[0026] 2) Seal the nozzle of the glass raw material tube A with the vacuum pump to evacuate, and at the same time heat the glass raw material to 110 with the electric heating furnace 2 o C, to remove the glass raw material and water molecules in the H-type quartz ampoule, when the vacuum in the H-type quartz ampoule reaches 2×10 -3 When the Pa is below, use a hydrogen-oxygen flame to seal at position 1 of the glass raw material tube A;

[0027] 3) Use the rapid heating furnace 3 to heat the glass raw...

Embodiment 3

[0030] Preparation of high-purity Ge 15 Ga 10 Te 72 Se 3 Chalcogenide glass, the specific steps are as follows:

[0031] 1) According to the ratio of 15mol%, 10mol%, 72mol% and 3mol% of germanium, gallium, tellurium and selenium as raw materials, 20g of magnesium bar is put into 0.025wt% by mass percentage, and 0.025wt% by mass percentage into TeCl 4 0.005 g, put into pre-dehydroxylated glass feedstock tube A;

[0032] 2) Seal the nozzle of the glass raw material tube A with the vacuum pump and vacuumize it, and heat the glass raw material to 130°C at the same time with the electric heating furnace 2 o C, to remove the glass raw material and water molecules in the H-type quartz ampoule, when the vacuum in the H-type quartz ampoule reaches 2×10 -3 When the Pa is below, use a hydrogen-oxygen flame to seal at position 1 of the glass raw material tube A;

[0033] 3) Use the rapid heating furnace 3 to heat the glass raw material pipe A and the connecting pipe C at the ...

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Abstract

The invention discloses a preparation device of gallium-containing chalcogenide glass having a high melting point and a high boiling point, and a preparation method thereof. The preparation device comprises a resistive heating system, an instant heating furnace, and an H-shaped quartz ampoule, wherein the resistive heating system has a temperature controller; the instant heating furnace can rapidly heat a glass raw material tube and a connection tube; the H-shaped quartz ampoule comprises the glass raw material tube and a purification glass tube; the glass raw material tube is communicated with the purification glass tube through the connection tube; and the upper end opening of the glass raw material tube is connected with a vacuum pump. The preparation device has the following advantage: the heating system can instantly heat the glass raw material tube and the connection tube to 1400DEG C to rapidly gasify a glass raw material in the glass raw material tube, the gasified glass raw material is distilled to the purification glass tube by going through the connection tube, and impurities are residual in the glass raw material tube because of high melting points, so the gallium-containing chalcogenide glass with low impurity contents is obtained.

Description

technical field [0001] The invention relates to a preparation device and a preparation method of a high melting and boiling point chalcogenide glass, in particular to a preparation device and a preparation method of a gallium-containing high melting and boiling point chalcogenide glass. Background technique [0002] Chalcogenide glass is a non-oxide glass with good chemical stability, high refractive index and very wide infrared transmission window. Taking advantage of its excellent far-infrared transmission ability, chalcogenide glass can be applied in the fields of infrared biochemical sensing technology, infrared exploration technology and infrared energy transmission. [0003] However, the infrared transmittance of chalcogenide glass is easily affected by impurities inside the glass. There are oxide absorption bands of various metals or chalcogenide glass elements above the wavelength of 6 μm, especially the chalcogenide glass containing gallium at 15-20 μm There are la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C3/32C03C4/10
Inventor 王训四何钰钜聂秋华张培全徐会娟戴世勋沈祥徐铁峰陈飞飞
Owner NINGBO UNIV
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