Preparation method of chalcogenide glass material

By using a fan blade stirring device that is resistant to high temperature and vacuum resistant during the preparation of sulfur-based glass, the problems of low production efficiency and poor glass stability in the prior art are solved, and a method for efficient preparation of sulfur-based glass is realized. Improves the uniformity and batch stability of the glass.

CN119306373APending Publication Date: 2025-01-14JIANGSU SPECTRAL PHOTONICS NEW MATERIAL CO LTD
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Patent Information

Application Number
CN202411407051.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-10
Publication Date
2025-01-14

AI Technical Summary

Technical Problem

The existing sulfur-based glass preparation methods cannot achieve continuous production, have low production efficiency, a lot of waste of raw materials, and poor stability of glass batches, making it difficult to meet the market's demand for low cost, large batches and high performance.

Method used

The melting and quenching of the quartz ampoule is carried out using a stirring device to melt and quench the molten sulfur-based glass at high temperature by a fan blade-shaped stirring device that is resistant to high temperature, vacuum and density higher than that of the sulfur-based glass, and then annealing and cooling. , improve glass uniformity and preparation efficiency.

Benefits of technology

Improves the uniformity and preparation efficiency of the glass, shortens the sway time during the preparation process, reduces the cost and improves the batch stability.

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Abstract

The invention discloses a chalcogenide glass material preparation method, which comprises: 1) raw material preparation: weighing various raw materials according to a raw material ratio, uniformly mixing, placing the mixed raw materials and a stirring device in a quartz ampoule bottle, and carrying out vacuum pumping packaging; 2) high-temperature melting and quenching: heating the quartz ampoule bottle, and melting the packaged mixed raw materials at high temperature; after heating, quenching the quartz ampoule bottle and the melt packaged in the quartz ampoule bottle by using strong wind or ice water to obtain a semi-finished chalcogenide glass product; and 3) annealing and cooling: putting the quartz ampoule bottle and the semi-finished glass into an annealing furnace for annealing, cooling the quartz ampoule bottle and the semi-finished glass to room temperature after annealing is finished, then opening the quartz ampoule bottle, and taking out the chalcogenide glass and the stirring device. The preparation method has the beneficial effects that the glass uniformity is improved, the swinging time in the preparation process is shortened, and the preparation efficiency is improved.
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Description

Technical Field

[0001] The present invention relates to the technical field of chalcogenide glass materials, in particular to a method for preparing chalcogenide glass materials. Background Art

[0002] Chalcogenide glass refers to glass formed by the elements S, Se, and Te of the VIA group of the periodic table and a certain amount of other elements. The Ge-Sb-Se system chalcogenide glass, which is widely used at present, has the following advantages: 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, and the temperature coefficient of refractive index is small and adjustable; it consumes little germanium resources, can be formed by precision molding technology, and has low processing cost;

[0003] It is widely used in defense technology fields such as individual helmet night vision systems, gun sights, unmanned vehicle monitoring systems and infrared guidance systems. With the development of infrared detector technology and cost control, chalcogenide glass thermal imaging systems also have great application prospects in security, fire protection, temperature measurement, automotive night vision assisted driving, personal vision and smart phones. With the continuous increase in the market demand for chalcogenide glass, higher and higher requirements are put forward for its preparation technology, namely low cost, large volume and high performance.

[0004] At present, the preparation method of chalcogenide glass adopts atmosphere protection melting technology, and obtains chalcogenide glass clinker by ampoule method, and completes the processes of adding materials, glass formation, clarification, homogenization and leaking forming in sequence at different times. However, this method cannot be produced continuously, the production efficiency is still low, and the raw materials are wasted, the cost is increased, and the stability of the obtained glass batches still has certain differences;

[0005] In view of the above situation, it is necessary to improve the existing chalcogenide glass materials so that they can meet the current needs for chalcogenide glass materials. Summary of the invention

[0006] To achieve the above object, the technical solution of the present invention is a method for preparing a chalcogenide glass material, comprising the following steps:

[0007] 1) Raw material preparation: weigh various raw materials according to the raw material ratio and mix them evenly, then place the mixed raw materials and stirring device in a quartz ampoule for vacuum packaging;

[0008] 2) High-temperature melting and quenching: heating the quartz ampoule to melt the encapsulated mixed raw materials at high temperature; after heating, quenching the quartz ampoule and the molten material encapsulated therein with strong wind or ice water to obtain a semi-finished chalcogenide glass;

[0009] 3) Annealing and cooling: The quartz ampoule and the semi-finished glass are placed in an annealing furnace for annealing. After the annealing is completed, the quartz ampoule and the semi-finished glass are cooled to room temperature. Then, the quartz ampoule is opened and the chalcogenide glass and the stirring device are taken out.

[0010] As a further supplement to the technical solution, the stirring device is placed at the bottom of the quartz ampoule.

[0011] As a further supplement to the technical solution, the stirring device is made of high temperature resistant and vacuum resistant materials and does not chemically react with chalcogenide glass and fused quartz.

[0012] As a further supplement to the technical solution, the material density of the stirring device should be greater than the density of the molten chalcogenide glass.

[0013] As a further supplement to the technical solution, the stirring device is in a shape that has greater resistance to the fluid.

[0014] As a further supplement to the technical solution, the stirring device is a fan blade.

[0015] As a further supplement to the technical solution, the size of the stirring device is smaller than the bottleneck of the quartz ampoule.

[0016] The beneficial effects are improving the uniformity of glass, shortening the swing time in the preparation process, and improving the preparation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a schematic diagram of the overall structure of the quartz ampoule bottle of the present invention when it is working;

[0018] Figure 2 It is a schematic structural diagram of the stirring device of the present invention. DETAILED DESCRIPTION

[0019] In order to make the technical solution more clear to those skilled in the art, Figure 1 -2 Detailed description of the technical solution of the present invention:

[0020] A method for preparing a chalcogenide glass material comprises the following steps:

[0021] 1) Raw material preparation: weigh various raw materials according to the raw material ratio and mix them evenly, then place the mixed raw materials and stirring device in a quartz ampoule for vacuum packaging;

[0022] 2) High-temperature melting and quenching: heating the quartz ampoule to melt the encapsulated mixed raw materials at high temperature; after heating, quenching the quartz ampoule and the molten material encapsulated therein with strong wind or ice water to obtain a semi-finished chalcogenide glass;

[0023] 3) Annealing and cooling: The quartz ampoule and the semi-finished glass are placed in an annealing furnace for annealing. After the annealing is completed, the quartz ampoule and the semi-finished glass are cooled to room temperature. Then, the quartz ampoule is opened and the chalcogenide glass and the stirring device are taken out.

[0024] Wherein, the stirring device is placed at the bottom of the quartz ampoule bottle.

[0025] The stirring device is made of high temperature resistant and vacuum resistant materials and does not chemically react with chalcogenide glass and fused quartz.

[0026] Among them, the material density of the stirring device should be greater than the density of the molten chalcogenide glass. For example, the high-density material can be wrapped with quartz material to adjust the overall density so as to meet the above two requirements.

[0027] The stirring device is in a shape that has greater resistance to the fluid.

[0028] Wherein, the stirring device is a fan blade.

[0029] The size of the stirring device is smaller than the bottleneck of the quartz ampoule.

[0030] Its working principle is: during the raw material preparation process, the stirring device is packaged into the ampoule together with the raw materials; when swinging at high temperature, the stirring device will form relative movement with the molten chalcogenide glass liquid due to its greater density than the chalcogenide glass, and at the same time, due to its shape, it has a greater resistance to the fluid, so it can stir the molten chalcogenide glass during its own movement. Then, it is quenched, annealed and cooled simultaneously with the chalcogenide glass; when cutting the chalcogenide glass, this swinging device is at the bottom of the glass rod and can be taken out and reused repeatedly.

[0031] The above technical solutions only reflect the preferred technical solutions of the technical solutions of the present invention. Some changes that may be made to certain parts thereof by technicians in this technical field all reflect the principles of the present invention and fall within the protection scope of the present invention.

Claims

1. A method for preparing a chalcogenide glass material, characterized in that: The following steps are involved: 1) Raw material preparation: weigh various raw materials according to the raw material ratio and mix them evenly, then place the mixed raw materials and stirring device in a quartz ampoule for vacuum packaging; 2) High-temperature melting and quenching: heating the quartz ampoule to melt the encapsulated mixed raw materials at high temperature; after heating, quenching the quartz ampoule and the molten material encapsulated therein with strong wind or ice water to obtain a semi-finished chalcogenide glass; 3) Annealing and cooling: The quartz ampoule and the semi-finished glass are placed in an annealing furnace for annealing. After the annealing is completed, the quartz ampoule and the semi-finished glass are cooled to room temperature. Then, the quartz ampoule is opened and the chalcogenide glass and the stirring device are taken out.

2. The method for preparing a chalcogenide glass material according to claim 1, characterized in that: The stirring device is placed at the bottom of the quartz ampoule.

3. The method for preparing a chalcogenide glass material according to claim 2, characterized in that: The stirring device is made of high temperature resistant and vacuum resistant materials and does not chemically react with chalcogenide glass and fused quartz.

4. The method for preparing a chalcogenide glass material according to claim 3, characterized in that: The material density of the stirring device should be greater than the density of the molten chalcogenide glass.

5. The method for preparing a chalcogenide glass material according to claim 4, characterized in that: The stirring device is in a shape that has greater resistance to the fluid.

6. The method for preparing a chalcogenide glass material according to claim 5, characterized in that: The stirring device is a fan blade.

7. The method for preparing a chalcogenide glass material according to claim 6, characterized in that: The size of the stirring device is smaller than the bottleneck of the quartz ampoule.