A Si-containing chalcogenide glass, its preparation method and application
Patent Information
- Application Number
- CN202410969216.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-19
- Publication Date
- 2026-09-01
- Estimated Expiration
- 2044-07-19
AI Technical Summary
[0018]通过本发明的方法可以使硫系玻璃的硬度最高达到200kg mm-2,其中,硫系玻璃的硬度达到168kgmm-2时,红外窗口透过达到60%。
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Figure CN118771721B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of special glass technology, and in particular to a Si-containing chalcogenide glass, its preparation method, and its application. Background Technology
[0002] Chalcogenide glasses have been used for 70 years, playing an indispensable role in the infrared field. They possess advantages such as ease of processing, high transmittance, and high refractive index, leading to a year-on-year increase in their global market applications. However, the increasing demand for complex environments has limited the application of chalcogenide glasses. Chalcogenide glasses have relatively lower hardness compared to oxide glasses, making their surfaces easily scratched and even shattered. Various methods, such as doping with multiple elements, microcrystallization, and diamond-like carbon (DLC) thin-film coating, are commonly used to improve the hardness of chalcogenide glasses. This invention, by doping the glass with a Cu5Si alloy, utilizes the low eutectic temperature of this alloy to successfully dope high-coordination-number Si elements, increasing the number of covalent bonds within the glass and thus enhancing its hardness. Summary of the Invention
[0003] In view of this, the present invention provides a Si-containing chalcogenide glass, its preparation method, and its application.
[0004] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:
[0005] A Si-containing chalcogenide glass comprises the following components: Cu: 0.5–13 at%; Si: 0.1–3 at%; As: 30–40 at%; Se: 50–60 at%.
[0006] Preferably, the chalcogenide glass is doped with Cu5Si alloy.
[0007] A method for preparing Si-containing chalcogenide glass includes the following steps:
[0008] (1) Weigh the raw materials Cu5Si alloy, As and Se, put the raw materials into a quartz reactor, evacuate and seal the quartz reactor, and remove impurities from the raw materials to obtain the purified product.
[0009] (2) The purified mixture obtained in step (1) is melted, quenched and annealed in sequence to obtain Si-containing chalcogenide glass.
[0010] Preferably, the purification method in step (1) is any one of vacuum distillation, oxygen scavenging, and vacuum distillation combined with oxygen scavenging.
[0011] Preferably, the purification method in step (1) is vacuum distillation combined with an oxygen remover.
[0012] Preferably, the deoxidizer used in the vacuum distillation combined with deoxidizer method is elemental Mg or elemental Al.
[0013] Preferably, the melting temperature in step (2) is 900-950°C and the melting time is 30-35h.
[0014] Preferably, the quenching temperature in step (2) is 400-450℃, and the quenching method is water quenching.
[0015] Preferably, the annealing temperature in step (2) is 170-200°C and the annealing cooling rate is 2-10°C / h.
[0016] Application of Si-containing chalcogenide glass or Si-containing chalcogenide glass prepared by a method thereof in infrared optics.
[0017] The present invention achieves the following technical effects compared to the prior art:
[0018] The method of this invention can achieve a hardness of up to 200 kg / mm² for chalcogenide glasses. -2 Among them, the hardness of chalcogenide glass reaches 168 kg / mm². -2 At that time, the infrared window transmits up to 60%. Attached Figure Description
[0019] Figure 1 Infrared window transmittance curve of the Si-containing chalcogenide glass prepared in Example 1;
[0020] Figure 2 Hardness indentation diagram of the Si-containing chalcogenide glass prepared in Example 1;
[0021] Figure 3 Infrared image of the Si-doped As-Se glass prepared in Comparative Example 1. Detailed Implementation
[0022] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0023] This invention provides a Si-containing chalcogenide glass comprising the following components: Cu: 0.5–13 at%; Si: 0.1–3 at%; As: 30–40 at%; Se: 50–60 at%.
[0024] Si has a high coordination number, high elemental hardness, and a melting point as high as 1410℃, making it impossible to directly prepare Si-containing chalcogenide glasses using traditional melting methods. This invention aims to improve the hardness of chalcogenide glasses by finding Si-containing alloys with lower eutectic temperatures and incorporating them into the glass.
[0025] The melting point of Cu5Si alloy is below 900℃. This invention successfully prepares chalcogenide glass containing Si with high coordination number by melting Cu5Si alloy with elemental As and Se, which increases the number of covalent bonds inside the glass and enhances the hardness of the chalcogenide glass.
[0026] The Si-containing chalcogenide glass provided by this invention increases the hardness of As2Se3 glass by up to 40%, and the chalcogenide glass provided by this invention has higher hardness than existing commercially available As2Se3 infrared chalcogenide glass materials.
[0027] This invention provides a method for preparing Si-containing chalcogenide glass as described above, comprising the following steps:
[0028] (1) Weigh the raw materials, which include Cu5Si alloy, As and Se elements, place the raw materials into a quartz reactor, evacuate and seal the quartz reactor, and remove impurities and purify the raw materials to obtain the purified product.
[0029] (2) The purified mixture obtained in step (1) is melted, quenched and annealed in sequence to obtain Si-containing chalcogenide glass.
[0030] In this invention, the Cu5Si alloy is preferably high-purity Cu5Si powder; the As is preferably high-purity As; the Se is preferably high-purity Se; and the purity of Ge, As, and Se is preferably ≥5N independently.
[0031] This invention uses high-purity materials as raw materials, which can reduce the content of impurities and oxides in the raw materials, thereby further improving the purity of the glass.
[0032] In this invention, the purification is preferably carried out in a quartz reactor, which is preferably an H-type double-tube quartz ampoule. The H-type double-tube quartz ampoule includes a raw material tube, a purification tube, and a connecting tube connecting the raw material tube and the purification tube. One end of the raw material tube has an opening, or both ends of the raw material tube and the purification tube have openings. This device facilitates sealing the opening of the raw material tube during purification, thereby providing a vacuum environment for the mixture and oxygen scavenger placed in the H-type double-tube quartz ampoule, preventing oxidation of the raw material and the introduction of impurities, thus reducing the intrinsic absorption of chalcogenide glass in the infrared region.
[0033] In this invention, the quartz reactor preferably undergoes a dehydroxylation pretreatment; the dehydroxylation pretreatment process preferably includes: sequentially cleaning the quartz reactor with hydrofluoric acid, deionized water, and anhydrous ethanol, and finally placing it in a drying oven for complete drying. By performing a dehydroxylation pretreatment on the quartz reactor, this invention avoids the introduction of impurity oxygen from the quartz reactor into the reaction.
[0034] In this invention, the quartz reactor is preferably preheated and evacuated before purification; the preheating and evacuation are preferably performed simultaneously. In this invention, the preheating temperature is preferably 50–100°C; the vacuum level is preferably ≥5 × 10⁻⁶. -5 Pa, more preferably 5 × 10 Pa -5 ~1×10 -3 Pa; the vacuuming time is preferably ≥3h. This invention, by purifying in a vacuum atmosphere, avoids the influence of oxygen in the air; the above process ensures that the vacuum level of the quartz reactor meets the requirements.
[0035] In this invention, when one end of the raw material tube has an opening, the preferred method for vacuuming is to add the raw material into the raw material tube through the opening on the raw material tube of the quartz reactor, then vacuum the tube, and finally seal the opening on the raw material tube. When both one end of the raw material tube and one end of the purification tube have openings, the preferred method for vacuuming is to add the raw material into the raw material tube through the opening on the raw material tube of the quartz reactor, seal the opening on the raw material tube, then vacuum the tube through the opening on the purification tube, and finally seal the opening on the purification tube. In this invention, the sealing process preferably uses an oxyhydrogen flame or an oxyacetylene flame. By using the above-described sealing method, this invention can reduce the introduction of impurity oxygen into the reaction during the sealing process.
[0036] In this invention, the purification method is preferably any one of vacuum distillation, oxygen scavenging, and vacuum distillation combined with oxygen scavenging, more preferably vacuum distillation combined with oxygen scavenging. This invention can eliminate [-OH] and [HOH] impurities in chalcogenide glasses by purifying the raw materials, thereby reducing the impact of intrinsic absorption loss in chalcogenide glasses on their infrared properties.
[0037] In this invention, the vacuum distillation combined with oxygen scavenging method preferably includes the following steps:
[0038] 1) Mix Cu5Si alloy, As and Se elements to obtain a mixture, then add an oxygen scavenger and mix to obtain the mixture to be purified;
[0039] 2) Add the mixture to be purified obtained in step 1) into a quartz reactor, and then place the quartz reactor into a dual-temperature zone distillation furnace for purification to obtain a purified mixture.
[0040] In this invention, the oxygen scavenger is preferably elemental Mg or elemental Al. The amount of oxygen scavenger used is preferably 0.03–0.1 wt% of the mixture, more preferably 0.05–0.08 wt%. This invention uses the above-mentioned substances as oxygen scavengers. Elemental Mg or elemental Al are both reactive elements with the ability to preferentially combine with oxygen to form bonds, thus eliminating the XO bonds present in chalcogenide glasses that cause a series of harmful absorptions in the near, mid, and far infrared regions. Furthermore, the oxides generated by the oxygen scavenger have low vapor pressures, allowing them to volatilize without remaining in the chalcogenide glass and not affecting its composition. By controlling the amount of oxygen scavenger, the problem of insufficient removal of oxygen impurities in the chalcogenide glass due to insufficient dosage can be avoided, while the problem of glass crystallization and devitrification during glass drawing due to excessive dosage can also be avoided.
[0041] After obtaining the mixture to be purified, the present invention preferably adds the mixture to a quartz reactor, and then places the quartz reactor into a dual-temperature zone distillation furnace for purification to obtain a purified mixture.
[0042] In this invention, the cold end temperature of the dual-temperature zone distillation furnace is preferably 300–500°C, more preferably 350–450°C, and even more preferably 420°C; the hot end temperature of the dual-temperature zone distillation furnace is preferably 900–950°C, more preferably 920–940°C, and even more preferably 930°C. This invention purifies the raw material by distilling it in a dual-temperature zone distillation furnace, utilizing the significant difference in vapor pressure between the elemental components and their oxides at a certain temperature to remove oxygen and other non-volatile impurities, thereby achieving a deoxygenation effect.
[0043] After obtaining the purified mixture, the present invention sequentially melts, quenches and anneals the purified mixture to obtain Si-containing chalcogenide glass.
[0044] In this invention, the melting temperature is preferably 900–950°C, and the melting time is preferably 30–35 hours. By controlling the melting parameters, this invention enables the raw materials to be completely melted and mixed together to form a molten glass state, thereby forming a chalcogenide glass with short-range order and long-range disorder.
[0045] After melting is complete, the present invention preferably allows the molten product to be naturally cooled to the quenching temperature for quenching. The present invention does not impose any particular limitation on the method of natural cooling; it can be determined based on the technical knowledge of those skilled in the art.
[0046] In this invention, the quenching temperature is preferably 400–450°C, and the quenching method is preferably water-cooled quenching. This invention does not have a specific limitation on the quenching time; quenching to room temperature is sufficient. Through quenching treatment, this invention enables the glass structure to exhibit short-range order and long-range disorder, thereby resulting in excellent performance.
[0047] In this invention, the annealing temperature is preferably 170–200°C, and the annealing cooling rate is preferably 2–10°C / h. This invention improves the mechanical strength and thermal stability of chalcogenide glasses by reducing or eliminating the uneven permanent thermal stress formed during quenching through annealing.
[0048] This invention purifies the raw materials to remove excess impurities, and then sequentially melts, quenches, and anneals them. Melting ensures uniform mixing of the components, quenching forms a glass with short-range order and long-range disorder, and annealing further improves the mechanical and physical properties of the glass, thus obtaining high-hardness chalcogenide glass. The preparation method is simple and convenient for large-scale industrial production.
[0049] This invention provides the application of Si-containing chalcogenide glass as described in the above technical solution or Si-containing chalcogenide glass prepared by the above technical solution in infrared optics.
[0050] The present invention does not impose any special limitations on the specific application method, which can be determined based on the technical common sense of those skilled in the art.
[0051] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.
[0052] Example 1
[0053] A Si-containing chalcogenide glass is composed of the following components: Cu: 3.33 at%; Si: 0.67 at%; As: 38.4 at%; Se: 57.6 at%;
[0054] The method for preparing the Si-containing chalcogenide glass comprises the following steps:
[0055] (1) The high-purity Cu5Si powder, high-purity As and high-purity Se are mixed and then purified by vacuum distillation combined with deoxidizing agent method to obtain purified mixture;
[0056] (2) The purified mixture obtained in step (1) is melted, then naturally cooled to the quenching temperature for quenching, and finally heated to the annealing temperature for annealing to obtain Si-containing chalcogenide glass; the melting temperature is 950℃, the melting time is 35h; the quenching temperature is 420℃, the quenching method is water quenching; the annealing temperature is 170℃, and the annealing cooling rate is 10℃ / h;
[0057] The vacuum distillation combined with oxygen scavenging method consists of the following steps:
[0058] 1) Cu5Si powder, high-purity As and high-purity Se are mixed to obtain a mixture, and then an oxygen scavenger is added and mixed to obtain a mixture to be purified; the purity of Cu5Si powder, high-purity As and high-purity Se are all 5N; the oxygen scavenger is elemental Mg, and the amount of the oxygen scavenger is 0.1wt% of the mixture.
[0059] 2) The mixture to be purified obtained in step 1) is added to the raw material tube through the opening on the raw material tube of the H-type double-tube quartz ampoule. Vacuuming and preheating are then performed simultaneously. Finally, the opening on the raw material tube is sealed, and the quartz reactor is placed in a dual-temperature zone distillation furnace for purification. The quartz reactor undergoes a dehydroxylation pretreatment process, which involves sequentially cleaning the quartz reactor with hydrofluoric acid, deionized water, and anhydrous ethanol, followed by complete drying in a drying oven. The preheating temperature is 90°C, and the vacuum degree is 1×10⁻⁶. -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 400℃, and the hot end temperature of the dual-temperature zone distillation furnace is 950℃.
[0060] The properties of the Si-containing chalcogenide glass prepared in Example 1 were tested, and the results are as follows: Figure 1 As shown.
[0061] pass Figure 1 It can be seen that the Si-containing chalcogenide glass prepared by this invention achieves an infrared window transmittance of 60%; the hardness of the Si-containing chalcogenide glass was tested and the result was 168.6 kg mm. -2 .
[0062] Example 2
[0063] A Si-containing chalcogenide glass is composed of the following components: Cu: 5.83 at%; Si: 1.17 at%; As: 37.2 at%; Se: 55.8 at%;
[0064] The method for preparing the Si-containing chalcogenide glass comprises the following steps:
[0065] (1) The high-purity Cu5Si powder, high-purity As and high-purity Se are mixed and then purified by vacuum distillation combined with deoxidizing agent method to obtain purified mixture;
[0066] (2) The purified mixture obtained in step (1) is melted, then naturally cooled to the quenching temperature for quenching, and finally heated to the annealing temperature for annealing to obtain Si-containing chalcogenide glass; the melting temperature is 950℃, the melting time is 30h; the quenching temperature is 430℃, the quenching method is water quenching; the annealing temperature is 175℃, and the annealing cooling rate is 10℃ / h;
[0067] The vacuum distillation combined with oxygen scavenging method consists of the following steps:
[0068] 1) Cu5Si powder, high-purity As and high-purity Se are mixed to obtain a mixture, and then an oxygen scavenger is added and mixed to obtain a mixture to be purified; the purity of Cu5Si powder, high-purity As and high-purity Se are all 5N; the oxygen scavenger is elemental Mg, and the amount of the oxygen scavenger is 0.1wt% of the mixture.
[0069] 2) The mixture to be purified obtained in step 1) is added to the raw material tube through the opening on the raw material tube of the H-type double-tube quartz ampoule. Vacuuming and preheating are then performed simultaneously. Finally, the opening on the raw material tube is sealed, and the quartz reactor is placed in a dual-temperature zone distillation furnace for purification. The quartz reactor undergoes a dehydroxylation pretreatment process, which involves sequentially cleaning the quartz reactor with hydrofluoric acid, deionized water, and anhydrous ethanol, followed by complete drying in a drying oven. The preheating temperature is 90°C, and the vacuum degree is 1×10⁻⁶. -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 400℃, and the hot end temperature of the dual-temperature zone distillation furnace is 950℃.
[0070] The hardness of the Si-containing chalcogenide glass was tested, and the result was 176.8 kg / mm². -2 .
[0071] Example 3
[0072] A Si-containing chalcogenide glass is composed of the following components: Cu: 12.5 at%; Si: 2.5 at%; As: 34 at%; Se: 51 at%;
[0073] The method for preparing the Si-containing chalcogenide glass comprises the following steps:
[0074] (1) The high-purity Cu5Si powder, high-purity As and high-purity Se are mixed and then purified by vacuum distillation combined with deoxidizing agent method to obtain purified mixture;
[0075] (2) The purified mixture obtained in step (1) is melted, then naturally cooled to the quenching temperature for quenching, and finally heated to the annealing temperature for annealing to obtain Si-containing chalcogenide glass; the melting temperature is 950℃ and the melting time is 30h; the quenching temperature is 450℃ and the quenching method is water quenching; the annealing temperature is 180℃ and the annealing cooling rate is 10℃ / h;
[0076] The vacuum distillation combined with oxygen scavenging method consists of the following steps:
[0077] 1) Cu5Si powder, high-purity As and high-purity Se are mixed to obtain a mixture, and then an oxygen scavenger is added and mixed to obtain a mixture to be purified; the purity of Cu5Si powder, high-purity As and high-purity Se are all 5N; the oxygen scavenger is elemental Mg, and the amount of the oxygen scavenger is 0.1wt% of the mixture.
[0078] 2) The mixture to be purified obtained in step 1) is added to the raw material tube through the opening on the raw material tube of the H-type double-tube quartz ampoule. Vacuuming and preheating are then performed simultaneously. Finally, the opening on the raw material tube is sealed, and the quartz reactor is placed in a dual-temperature zone distillation furnace for purification. The quartz reactor undergoes a dehydroxylation pretreatment process, which involves sequentially cleaning the quartz reactor with hydrofluoric acid, deionized water, and anhydrous ethanol, followed by complete drying in a drying oven. The preheating temperature is 90°C, and the vacuum degree is 1×10⁻⁶. -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 400℃, and the hot end temperature of the dual-temperature zone distillation furnace is 950℃.
[0079] The hardness of the Si-containing chalcogenide glass was tested, and the result was 201.2 kg / mm². -2 .
[0080] Comparative Example 1
[0081] A Si-containing chalcogenide glass is composed of the following components: Si: 4 at%; As: 39 at%; Se: 57 at%;
[0082] The method for preparing the Si-containing chalcogenide glass comprises the following steps:
[0083] (1) The high-purity Si, high-purity As and high-purity Se are mixed and then purified by vacuum distillation combined with deoxidizing agent method to obtain purified mixture;
[0084] (2) The purified mixture obtained in step (1) is melted, then naturally cooled to the quenching temperature for quenching, and finally heated to the annealing temperature for annealing to obtain Si-containing chalcogenide glass; the melting temperature is 980℃ and the melting time is 30h; the quenching temperature is 450℃ and the quenching method is water quenching; the annealing temperature is 180℃ and the annealing cooling rate is 5℃ / h.
[0085] The vacuum distillation combined with oxygen scavenging method consists of the following steps:
[0086] 1) Si source, As source and Se source are mixed to obtain a mixture, and then an oxygen scavenger is added and mixed to obtain a mixture to be purified; the purity of the high-purity Si, high-purity As and high-purity Se is 5N; the oxygen scavenger is elemental Mg, and the amount of the oxygen scavenger is 0.1wt% of the mixture;
[0087] 2) The mixture to be purified obtained in step 1) is added to the raw material tube through the opening on the raw material tube of the H-type double-tube quartz ampoule. Vacuuming and preheating are then performed simultaneously. Finally, the opening on the raw material tube is sealed, and the quartz reactor is placed in a dual-temperature zone distillation furnace for purification. The quartz reactor undergoes a dehydroxylation pretreatment process, which involves sequentially cleaning the quartz reactor with hydrofluoric acid, deionized water, and anhydrous ethanol, followed by complete drying in a drying oven. The preheating temperature is 90°C, and the vacuum degree is 1×10⁻⁶. -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 400℃, and the hot end temperature of the dual-temperature zone distillation furnace is 950℃.
[0088] Infrared imaging of the Si-containing chalcogenide glass revealed an internal fog-like appearance, indicating that the Si powder could not be safely melted.
[0089] Comparative Example 2
[0090] A Si-containing chalcogenide glass is composed of the following components: Cu: 17.5 at%; Si: 3.5 at%; As: 31.6 at%; Se: 47.4 at%;
[0091] The method for preparing the Si-containing chalcogenide glass comprises the following steps:
[0092] (1) The high-purity Cu5Si powder, high-purity As and high-purity Se are mixed and then purified by vacuum distillation combined with deoxidizing agent method to obtain purified mixture;
[0093] (2) The purified mixture obtained in step (1) is melted, then naturally cooled to the quenching temperature for quenching, and finally heated to the annealing temperature for annealing to obtain Si-containing chalcogenide glass; the melting temperature is 980℃ and the melting time is 30h; the quenching temperature is 450℃ and the quenching method is water quenching; the annealing temperature is 190℃ and the annealing cooling rate is 5℃ / h.
[0094] The vacuum distillation combined with oxygen scavenging method consists of the following steps:
[0095] 1) Cu5Si powder, high-purity As and high-purity Se are mixed to obtain a mixture, and then an oxygen scavenger is added and mixed to obtain a mixture to be purified; the purity of Cu5Si powder, high-purity As and high-purity Se are all 5N; the oxygen scavenger is elemental Mg, and the amount of the oxygen scavenger is 0.1wt% of the mixture.
[0096] 2) The mixture to be purified obtained in step 1) is added to the raw material tube through the opening on the raw material tube of the H-type double-tube quartz ampoule. Vacuuming and preheating are then performed simultaneously. Finally, the opening on the raw material tube is sealed, and the quartz reactor is placed in a dual-temperature zone distillation furnace for purification. The quartz reactor undergoes a dehydroxylation pretreatment process, which involves sequentially cleaning the quartz reactor with hydrofluoric acid, deionized water, and anhydrous ethanol, followed by complete drying in a drying oven. The preheating temperature is 90°C, and the vacuum degree is 1×10⁻⁶. -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 400℃, and the hot end temperature of the dual-temperature zone distillation furnace is 950℃.
[0097] The Si-containing chalcogenide glass described herein cannot be glassed due to crystallization.
[0098] The comparison between Examples 1-3 and Comparative Examples 1 and 2 shows that when Cu5Si powder is used for doping, the hardness of the glass can be effectively improved, while Si powder cannot be used directly to prepare Si-containing chalcogenide glass through traditional melting.
[0099] The above description is merely a preferred embodiment of the present invention and does not constitute any limitation on the technical scope of the present invention. Therefore, any minor modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention shall still fall within the scope of the technical solution of the present invention.
Claims
1. A method for producing a Si-containing chalcogenide glass, characterized by, The Si-containing chalcogenide glass comprises the following components: Cu: 0.5~13 at%; Si: 0.1~3 at% As: 30~40 at%; Se: 50~60 at%; The chalcogenide glass is doped with alloy; The method for preparing the Si-containing chalcogenide glass includes the following steps: (1) Weigh the raw materials Alloys, As and Se elements are used. The raw materials are placed in a quartz reactor, vacuumed and then sealed. The raw materials are then purified to obtain a purified product. (2) The purified mixture obtained in step (1) is melted, quenched and annealed in sequence to obtain Si-containing chalcogenide glass.
2. The method for preparing Si-containing chalcogenide glass according to claim 1, characterized in that, The purification method in step (1) is any one of vacuum distillation, deoxygenating agent method, and vacuum distillation combined with deoxygenating agent method.
3. The method for preparing Si-containing chalcogenide glass according to claim 2, characterized in that, The purification method in step (1) is vacuum distillation combined with deoxygenating agent method.
4. The method for preparing Si-containing chalcogenide glass according to claim 3, characterized in that, The deoxidizing agent used in the vacuum distillation combined with deoxidizing agent method is elemental Mg or elemental Al.
5. The method for preparing Si-containing chalcogenide glass according to claim 1, characterized in that, The melting temperature in step (2) is 900~950℃ and the melting time is 30~35h.
6. The method for preparing Si-containing chalcogenide glass according to claim 1, characterized in that, The quenching temperature in step (2) is 400~450℃, and the quenching method is water quenching.
7. The method for preparing Si-containing chalcogenide glass according to claim 1, characterized in that, In step (2), the annealing temperature is 170~200℃ and the annealing cooling rate is 2~10℃ / h.
8. The application of the Si-containing chalcogenide glass prepared by the method of claim 1 in infrared optics.
Citation Information
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High-hardness Ge-As-Se chalcogenide glass as well as preparation method and application thereof
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