Purification method of Ge-Sb-Se chalcogenide glass material
By using temperature control and vacuum extraction technology during the purification of sulfur-based glass, the CS2 and SO2 gas condensed GeSe2/GeSe and Sb2Se3 is generated, which solves the problem of introducing hydrogen and oxygen in reaction with oxygen deoxygen and quartz, and achieves efficient sulfur-based glass Purification improves optical performance.
Patent Information
- Application Number
- CN202411313641.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-20
- Publication Date
- 2024-12-31
AI Technical Summary
In the existing sulfur-based glass purification method, the oxygen deletion agent and the hydrogen deletion agent react with the quartz material under a high temperature environment, introduce hydrogen and oxygen, resulting in infrared absorption and affecting the optical properties of the glass.
Using a purification device including the first, second and third containers, CS2 and SO2 gases are generated through vacuum extraction and temperature control, GeSe2/GeSe and Sb2Se3 are condensed, and the use of oxygen dehydrants and hydrogen dehydrants are avoided, and at high temperatures are Smelting and annealing, replacing traditional methods.
There is no need for traditional oxygen degassers and hydrogen degassers, which improves the purification effect of sulfur-based glass, avoids infrared absorption, and improves optical performance.
Smart Images
Figure CN119219326A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chalcogenide glass material purification, in particular to a method for purifying Ge-Sb-Se chalcogenide glass material. Background Art
[0002] Chalcogenide glass has unique advantages as an infrared lens material. Chalcogenide glass has high processing efficiency and can be precisely molded, which is more than 10 times higher than diamond turning, and the raw material cost is 1 / 3 of that of germanium single crystal. In terms of temperature adaptability, germanium single crystal is relatively "delicate", and the image is unstable when the temperature changes greatly. Chalcogenide glass can face a temperature difference of 110 degrees from -40 degrees Celsius to 70 degrees Celsius without pressure.
[0003] The general method for purifying chalcogenide glass is to add deoxidizer and dehydrogenator to the raw materials and then purify them by distillation. This method can generally achieve good purification effects, but the added deoxidizer and dehydrogenator will react with the ampoule of quartz material under the high temperature environment of melting, and introduce the hydrogen and oxygen in the quartz ampoule into the chalcogenide glass, thereby causing infrared absorption at ~3.9 and 9 microns, affecting the optical properties of the final glass. For this reason, a method for purifying Ge-Sb-Se chalcogenide glass material is designed. Summary of the invention
[0004] The purpose of the present invention is to solve the above problems and to design a method for purifying Ge-Sb-Se chalcogenide glass material.
[0005] To achieve the above object, the technical solution of the present invention is a method for purifying Ge-Sb-Se chalcogenide glass material, comprising the following steps:
[0006] Step 1: Raw material preparation stage;
[0007] Step 2: Purification operation;
[0008] Step 3: Mixture smelting operation;
[0009] Step 4: Annealing operation;
[0010] Step 5: Cooling operation.
[0011] As a further description of the technical solution, in the step 1, raw materials for preparing the chalcogenide glass material are weighed according to the raw material ratio, and the raw materials for preparing the chalcogenide glass material include Ge, Sb, and Se.
[0012] As a further description of the technical solution, in step 2, the purification operation adopts a purification device, and the purification device includes a first container, a second container, and a third container.
[0013] As a further description of the technical solution, the top ends of the first container, the second container and the third container are connected together, and the first container, the second container and the third container are all provided with independent temperature control systems.
[0014] As a further description of this technical solution, the purification operation includes the following steps:
[0015] Step 1: Place Se in zone 1, and Ge and Sb in zone 2;
[0016] Step 2: Vacuum the purification device;
[0017] Step 3: The temperature of the first container is raised to 300-350°C to form Se vapor; the temperature of the second container is raised to 500-700°C to make Se vapor react with impurities (-C, -H and -O) in Ge and Sb to generate CS2, H2S and SO2 volatile gases are discharged during the vacuum process;
[0018] Step 4: The temperature of the third container is controlled at 250-280°C to condense the purified GeSe2 / GeSe and Sb2Se3 in zone 3.
[0019] As a further description of the technical solution, in step three, the third container is sealed with an oxyhydrogen flame, and then the purified GeSe2 / GeSe and Sb2Se3 mixture is melted at 750-900°C.
[0020] As a further description of the technical solution, in step 4, the quartz ampoule and the semi-finished glass are placed in a thermal annealing furnace for annealing.
[0021] As a further description of the technical solution, in step five, after the annealing is completed, the quartz ampoule together with the semi-finished glass is cooled to room temperature, and then the quartz ampoule is opened to take out the chalcogenide glass.
[0022] The beneficial effect is that the method for purifying sulphur-based glass materials of the technical solution is simple to operate and easy to implement. By using the method for purifying sulphur-based glass materials, there is no need to use traditional deoxidizers and dehydrogenators, and no need to introduce new impurities, thereby effectively improving the purification effect of sulphur-based glass materials. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] Figure 1 It is a schematic structural diagram of the purification device of the present invention;
[0024] In the figure, 1 is the first container; 2 is the second container; 3 is the third container. DETAILED DESCRIPTION
[0025] First, the original intention of the design of the present invention is explained. Generally, the purification method of chalcogenide glass is to add deoxidizer and dehydrogenator to the raw material, and then purify it by distillation. This method can generally achieve better purification effect, but the added deoxidizer and dehydrogenator will react with the ampoule of quartz material under the high temperature environment of melting, and introduce hydrogen and oxygen in the quartz ampoule into the chalcogenide glass, thereby bringing about infrared absorption at ~3.9 and 9 microns, affecting the optical properties of the final glass. Therefore, the present invention designs a purification method of Ge-Sb-Se chalcogenide glass material.
[0026] The present invention will be described in detail below in conjunction with the accompanying drawings. Figure 1 As shown, a method for purifying Ge-Sb-Se chalcogenide glass material comprises the following steps:
[0027] Step 1: Raw material preparation stage; in the step 1, raw materials for preparing chalcogenide glass materials are weighed according to the raw material ratio, and the raw materials for preparing include Ge, Sb, and Se.
[0028] Step 2: Purification operation; in step 2, the purification operation adopts a purification device, and the purification device includes a first container 1, a second container 2, and a third container 3.
[0029] The top ends of the first container 1 , the second container 2 , and the third container 3 are connected together, and the first container 1 , the second container 2 , and the third container 3 are all provided with independent temperature control systems.
[0030] The purification operation includes the following steps:
[0031] Step 1: Place Se in zone 1, and Ge and Sb in zone 2;
[0032] Step 2: Vacuum the purification device;
[0033] Step 3: The temperature of the first container 1 is raised to 300-350°C to form Se vapor; the temperature of the second container 2 is raised to 500-700°C to make Se vapor react with impurities (-C, -H and -O) in Ge and Sb to generate CS2, H2S and SO2 volatile gases are discharged during the vacuum process;
[0034] Step 4: The temperature of the third container 3 is controlled at 250-280°C to condense the purified GeSe2 / GeSe and Sb2Se3 in zone 3.
[0035] Step 3: Mixture smelting operation; In the step 3, the third container 3 is sealed with an oxyhydrogen flame, and then the purified GeSe2 / GeSe and Sb2Se3 mixture is smelted at 750-900°C.
[0036] Step 4: Annealing operation; In step 4, the quartz ampoule bottle together with the semi-finished glass is placed in a thermal annealing furnace for annealing.
[0037] Step 5: Cooling operation. In step 5, after the annealing is completed, the quartz ampoule together with the semi-finished glass is cooled to room temperature, and then the quartz ampoule is opened to take out the chalcogenide glass.
[0038] The method for purifying chalcogenide glass materials of the technical solution is simple to operate and easy to implement. By using the method for purifying chalcogenide glass materials, there is no need to use traditional deoxidizers and dehydrogenators, and no need to introduce new impurities, thereby effectively improving the purification effect of chalcogenide glass materials.
[0039] 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 purifying Ge-Sb-Se chalcogenide glass material, characterized in that: The following steps are involved: Step 1: Raw material preparation stage; Step 2: Purification operation; Step 3: Mixture smelting operation; Step 4: Annealing operation; Step 5: Cooling operation.
2. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 1, characterized in that: In the step 1, raw materials for preparing the chalcogenide glass material are weighed according to the raw material ratio, and the raw materials for preparing the chalcogenide glass material include Ge, Sb, and Se.
3. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 1, characterized in that: In the step 2, the purification operation uses a purification device, which includes a first container (1), a second container (2), and a third container (3).
4. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 3, characterized in that: The top ends of the first container (1), the second container (2) and the third container (3) are connected together, and the first container (1), the second container (2) and the third container (3) are all provided with independent temperature control systems.
5. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 3, characterized in that: The purification operation includes the following steps: Step 1: Place Se in zone 1, and Ge and Sb in zone 2; Step 2: Vacuum the purification device; Step 3: The temperature of the first container (1) is raised to 300-350°C to form Se vapor; the temperature of the second container (2) is raised to 500-700°C to allow the Se vapor to react with the impurities (-C, -H and -O) in Ge and Sb to generate CS2, H2S and SO2 volatile gases which are discharged during the vacuuming process; Step 4: The temperature of the third container (3) is controlled at 250-280°C to allow the purified GeSe2 / GeSe and Sb2Se3 to condense in zone 3.
6. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 5, characterized in that: In the step three, the third container (3) is sealed with an oxyhydrogen flame, and then the purified GeSe2 / GeSe and Sb2Se3 mixture is melted at 750-900°C.
7. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 1, characterized in that: In the step 4, the quartz ampoule and the semi-finished glass are placed in a thermal annealing furnace for annealing.
8. The method for purifying Ge-Sb-Se chalcogenide glass material according to claim 1, characterized in that: In the step 5, after the annealing is completed, the quartz ampoule together with the semi-finished glass is cooled to room temperature, and then the quartz ampoule is opened to take out the chalcogenide glass.