A P-Se chalcogenide glass with high infrared transmittance and its preparation method

By combining vacuum distillation and deoxidizer purification with controlled melting, quenching and annealing processes, high-transmittance P-Se chalcogenide glass was prepared, which solved the problem of low transmittance of chalcogenide glass and achieved a significant increase in infrared transmittance and improved stability.

CN118771720BActive Publication Date: 2025-09-19NINGBO SUNSHINE HEPU PHOTOELECTRIC TECH CO LTD
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Patent Information

Application Number
CN202411025707.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-07-30
Publication Date
2025-09-19
Estimated Expiration
2044-07-30

AI Technical Summary

Technical Problem

The infrared transmittance of existing chalcogenide glasses is low and cannot meet the needs of certain applications.

Method used

The P and Se source materials are purified by vacuum distillation and deoxidizer, and the proportion of each component is optimized by controlling the melting, quenching and annealing processes, especially adding the P element and controlling its content to prepare high-transmittance P-Se chalcogenide glass.

Benefits of technology

The infrared transmittance of chalcogenide glass has been significantly improved to over 68%, which has enhanced the optical performance and stability of the glass and makes it suitable for infrared optical devices.

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Abstract

The present invention provides a method for preparing a P-Se chalcogenide glass with high infrared transmittance, comprising: S1: selecting a P source material and a Se source material, mixing the two, and then performing vacuum distillation and purification in combination with a deoxidizer to obtain a purified mixture; the vacuum distillation and deoxidizer combination comprising: adding the two mixed materials to a reaction container, preheating the reaction container in advance and evacuating the container simultaneously, wherein the preheating temperature is 50-100°C, and the vacuum degree of the evacuation is 5×10 ‑5 Pa or higher; S2: sequentially melting, quenching, and annealing the purified mixture to obtain a P-Se chalcogenide glass with high infrared transmittance. The present invention also includes this P-Se chalcogenide glass with high infrared transmittance, comprising: P: 35-45 at.%; Se: 55-65 at.%. The chalcogenide glass prepared by the present invention has high transmittance, resolving the problems of the prior art.
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Description

Technical Field

[0001] The present invention relates to the technical field of glass and relates to a P-Se chalcogenide glass having high transmittance in an infrared window and a preparation method thereof. Background Art

[0002] Chalcogenide glass is a new type of inorganic glass with excellent performance. It is an important material in infrared optical materials. Infrared optical chalcogenide glass can be used to make structural lenses. Different types of glass are needed to make lenses in many applications nowadays. As the most important part of the device, the most important glass of the lens is particularly important. Excellent optical glass can greatly improve the performance of the device. For example, night vision goggles can enable people to see clearly at night. This is mainly due to the excellent performance of the lens glass. The lens glass of the night vision goggles can absorb more weak light. When the light passes through the device, it can enable people to see objects at night. Thermal imaging also relies on lens glass to absorb light of different bands, absorbing light from the human body or other light emitting absorption bands to highlight the imaging.

[0003] Chalcogenide glasses are primarily composed of VIA Group chalcogenides doped with other elements, such as Ga (germanium), and other metallic elements. Chalcogenide glasses exhibit excellent optical infrared properties, including high infrared transmittance and a good refractive index. Doping with different elements can enhance the properties of chalcogenide glasses, enabling the production of lenses with varying performance. However, the infrared transmittance of currently available chalcogenide glasses ranges primarily from 45% to 65%, making it relatively unsuitable for future research into the performance of optical infrared materials.

[0004] Therefore, how to improve the transmittance of chalcogenide glass has become a technical problem that needs to be solved urgently in this field. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a method for preparing P-Se chalcogenide glass with high infrared transmittance, so as to solve the problem of low transmittance of chalcogenide glass prepared by conventional preparation methods.

[0006] The present invention provides a method for preparing P-Se chalcogenide glass with high infrared transmittance, comprising the following steps:

[0007] S1: Select a P source material and a Se source material, mix them, and then purify them by vacuum distillation and deoxidizing agent to obtain a purified mixture; the vacuum distillation and deoxidizing agent comprises: adding the mixed materials to a reaction container, preheating the reaction container in advance and evacuating the container at the same time, wherein the preheating temperature is 50-100°C, and the vacuum degree of the evacuation is 5×10 -5 Pa or above;

[0008] S2: The purified mixture obtained in step S1 is melted, quenched, and annealed in sequence to obtain a P-Se chalcogenide glass with high infrared transmittance; the melting temperature is 700-800°C, the quenching temperature is 350-400°C, the annealing temperature is 170-180°C, and the annealing cooling rate is 4-8°C / h.

[0009] The present invention discloses a method for preparing a P-Se chalcogenide glass with high infrared transmittance. By adding elements with larger relative atomic mass and controlling the composition of each component, the transmittance of the chalcogenide glass is improved through the synergistic effect of each component. The method also optimizes the thermal stability and transmittance range of the material by optimizing the amount of each component in the glass, thereby achieving high transmittance of the chalcogenide glass.

[0010] In a possible embodiment, in step S1, the reaction container is a quartz reactor.

[0011] The present invention provides a method for preparing a P-Se chalcogenide glass with high infrared transmittance. The quartz reactor is preferably preheated and evacuated before purification; the preheating and evacuation are preferably performed simultaneously. In the present invention, the preheating temperature is preferably 50 to 100°C; the vacuum degree of the evacuation is preferably ≥5 × 10-5Pa, more preferably 5 × 10-5 to 1 × 10-3Pa; and the evacuation time is preferably ≥3h. The present invention avoids the influence of oxygen in the air by purifying in a vacuum atmosphere; the vacuum degree of the quartz reactor can be made to meet the requirements through the above process, and the present invention does not specifically limit the mixing method, as long as the components can be mixed evenly.

[0012] In a possible embodiment, when the quartz reactor is a quartz reactor with an opening at one end, the vacuuming method is: after mixing the raw materials, add them into the raw material tube through the opening on the raw material tube of the quartz reactor, then vacuumize, and finally seal the opening on the raw material tube; when the quartz reactor is a quartz reactor with openings at both ends, the vacuuming method is: add the raw materials into the raw material tube through the first opening of the quartz reactor, seal the first opening, then vacuumize the second opening, and finally seal the second opening.

[0013] In a possible implementation, the sealing is performed by using an oxyhydrogen flame or an oxyacetylene flame.

[0014] In the above possible implementation manner, by adopting the above method for fusion sealing, the amount of impurity oxygen introduced into the reaction during the sealing process can be reduced.

[0015] As a preferred solution, the purity of the P source material and the Se source material are both above 5N; the vacuum degree is 5×10-5 to 1×10-3 Pa, and the vacuuming time is above 3 hours.

[0016] In the above possible implementation manners, by selecting a high-purity single substance as the raw material, the content of impurities and oxides in the raw material can be reduced, thereby further improving the purity of the glass.

[0017] In a possible implementation manner, in step S2, the melting temperature is 750° C. and the melting time is 27 to 28 hours.

[0018] In the above possible embodiments, by controlling the melting parameters, the raw materials can be completely melted and mixed together to form a glassy liquid, thereby forming a chalcogenide glass with short-range order and long-range disorder. After melting, the present invention quenches the molten product by naturally cooling it to a quenching temperature. The present invention does not specifically limit the method of naturally cooling, and can be determined based on the technical knowledge of those skilled in the art.

[0019] In a possible implementation, in step S2, the quenching temperature is 370-390° C., and the quenching method is air-cooling quenching.

[0020] The present invention has no special limitation on the quenching time, and quenching to room temperature is sufficient. In the above possible implementation manner, the present invention can make the structure of the glass ordered in the short range and disordered in the long range through quenching treatment, thereby having excellent performance.

[0021] In a possible implementation, in step S2, the annealing temperature is 175-178° C., and the annealing cooling rate is 5° C. / h.

[0022] In the above possible implementation manner, by annealing the chalcogenide glass, the uneven permanent thermal stress formed in the chalcogenide glass during the quenching process is reduced or eliminated, thereby improving the mechanical strength and thermal stability of the chalcogenide glass, while also improving the density, transmittance, and thermal expansion coefficient of the chalcogenide glass. By controlling the annealing parameters, the transmittance and stability of the chalcogenide glass are further improved.

[0023] The present invention sequentially melts, quenches and anneals the raw materials, uniformly mixes the components by melting, forms short-range ordered and long-range disordered glass by quenching, and further improves the mechanical and physical properties of the glass by annealing, thereby obtaining high-transmittance glass; the preparation method is simple and convenient for industrial large-scale production.

[0024] Another technical problem to be solved by the present invention is to provide a P-Se chalcogenide glass with high infrared transmittance to solve the problem of low infrared transmittance of the chalcogenide glass in the prior art.

[0025] In order to solve the above problems, the present invention provides a P-Se chalcogenide glass with high infrared transmittance, wherein the P-Se chalcogenide glass with high infrared transmittance is prepared by the preparation method, and the chalcogenide glass comprises: P: 35-45 at.%; Se: 55-65 at.%.

[0026] The high-infrared-transmittance P-Se chalcogenide glass of the present invention has good light transmittance by adding the element P to the glass. By controlling the content of the element P, the light transmittance of the glass can be further improved, thereby giving the glass excellent optical properties. When the components of the chalcogenide glass are controlled to the above-mentioned ratio, the transmittance of the high-transmittance P-Se chalcogenide glass reaches over 68%. The chalcogenide glass provided by the present invention has a higher transmittance than existing infrared chalcogenide glass materials, thus solving the problems existing in the prior art.

[0027] In a possible implementation, the chalcogenide glass includes: P: 40-42 at. %; Se: 58-60 at. %, and the transition temperature of the chalcogenide glass is 175-185° C.

[0028] In the above possible embodiments, by utilizing the light transmission effect of the element P, adding the element P to the chalcogenide glass and controlling its amount to 40-42 at.%, a synergistic effect with the Se element can be achieved, further improving the transmittance of the glass. The chalcogenide glass provided by the present invention has the characteristics of a high transition temperature and good stability, which can provide better stability during use and a long service life. The present invention improves the transmittance of the chalcogenide glass through the synergistic effect of the components by adding elements with larger relative atomic masses and controlling the composition of each component. By optimizing the amount of each component in the glass, the thermal stability and transmittance range of the material are optimized, thus achieving high transmittance of the chalcogenide glass. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 Schematic diagram of the transmittance of the high-transmittance P2Se3 chalcogenide glass infrared window prepared in Example 1.

[0030] Figure 2 Schematic diagram of the refractive index of the high-transmittance P2Se3 chalcogenide glass prepared in Example 1;

[0031] Figure 3 This is the Raman spectrum of the high-transmittance P2Se3 chalcogenide glass prepared in Example 1;

[0032] Figure 4 Schematic diagram of the transmittance of the high-transmittance P2Se chalcogenide glass prepared in Comparative Example 2. DETAILED DESCRIPTION

[0033] First, those skilled in the art should understand that these embodiments are merely used to explain the technical principles of the embodiments of the present application and are not intended to limit the scope of protection of the embodiments of the present application. Those skilled in the art may adjust them as needed to suit specific application scenarios.

[0034] The present invention provides a method for preparing P-Se chalcogenide glass with high infrared transmittance, comprising the following steps:

[0035] S1: Select a P source material and a Se source material, mix them, and then purify them by vacuum distillation and deoxidizing agent to obtain a purified mixture; the vacuum distillation and deoxidizing agent comprises: adding the mixed materials to a reaction container, preheating the reaction container in advance and evacuating the container at the same time, wherein the preheating temperature is 50-100°C, and the vacuum degree of the evacuation is 5×10 -5 Pa or above;

[0036] S2: The purified mixture obtained in step S1 is melted, quenched, and annealed in sequence to obtain a P-Se chalcogenide glass with high infrared transmittance; the melting temperature is 700-800°C, the quenching temperature is 350-400°C, the annealing temperature is 170-180°C, and the annealing cooling rate is 4-8°C / h.

[0037] As a preferred solution, in step S1, the reaction container is a quartz reactor.

[0038] As a preferred solution, when the quartz reactor is a quartz reactor with an opening at one end, the vacuuming method is: after mixing the raw materials, add them into the raw material tube through the opening on the raw material tube of the quartz reactor, then vacuumize, and finally seal the opening on the raw material tube; when the quartz reactor is a quartz reactor with openings at both ends, the vacuuming method is: add the raw materials into the raw material tube through the first opening of the quartz reactor, seal the first opening, then vacuumize the second opening, and finally seal the second opening.

[0039] More specifically, in the present invention, when one end of the raw material tube is provided with an opening, the vacuuming method is preferably: adding the raw material into the raw material tube through the opening on the raw material tube of the quartz reactor, then vacuuming, and finally sealing the opening on the raw material tube; when one end of the raw material tube and one end of the purification tube are both provided with openings, the vacuuming method is preferably: adding the raw material into the raw material tube through the opening on the raw material tube of the quartz reactor, sealing the opening on the raw material tube, then vacuuming through the opening on the purification tube, and finally sealing the opening on the purification tube.

[0040] As a preferred solution, the sealing method is to seal by means of an oxyhydrogen flame or an oxyacetylene flame.

[0041] As a preferred solution, the purity of the P source material and the Se source material are both above 5N; the vacuum degree is 5×10-5 to 1×10-3 Pa, and the vacuuming time is above 3 hours.

[0042] As a preferred solution, in step S2, the melting temperature is 750°C and the melting time is 27 to 28 hours.

[0043] As a preferred solution, in step S2, the quenching temperature is 370-390°C, and the quenching method is air-cooling quenching.

[0044] As a preferred solution, in step S2, the annealing temperature is 175-178°C, and the annealing cooling rate is 5°C / h. In the present invention, the annealing temperature is preferably 170-180°C, more preferably 174-178°C, and further preferably 175-178°C; the annealing cooling rate is preferably 4-8°C / h, more preferably 4-7°C / h, and further preferably 5°C / h.

[0045] The present invention also provides a P-Se chalcogenide glass with high infrared transmittance. The P-Se chalcogenide glass with high infrared transmittance is prepared by the preparation method, and the chalcogenide glass comprises: P: 35-45 at.%; Se: 55-65 at.%.

[0046] As a preferred solution, the chalcogenide glass comprises: P: 40-42 at.%; Se: 58-60 at.%.

[0047] The present invention also includes the use of the infrared-transmittance P-Se chalcogenide glass described in the above technical solution or the infrared-transmittance P-Se chalcogenide glass prepared by the preparation method described in the above technical solution in infrared optics.

[0048] The present invention has no particular limitation on the specific manner of the application, which can be determined based on the technical common sense of those skilled in the art.

[0049] The following provides specific examples and comparative examples that combine actual data, reaction instruments, and equipment to further describe the above technical solutions of the present invention:

[0050] Example 1

[0051] This embodiment provides a P2Se chalcogenide glass with high infrared transmittance, consisting of the following components: Se: 60 at.% and P: 40 at.%;

[0052] The method for preparing the high-transmittance P2Se chalcogenide glass comprises the following steps:

[0053] S1: mixing the high-purity Se and high-purity P and purifying them by vacuum distillation combined with a scavenger method to obtain a purified mixture;

[0054] S2: Melting the purified mixture obtained in step S1, then naturally cooling it to a quenching temperature for quenching, and finally heating it to an annealing temperature for annealing to obtain a high-transmittance P2Se chalcogenide glass; the melting temperature is 760°C, and the melting time is 30 hours; the quenching temperature is 370°C, and the quenching method is air cooling; the annealing temperature is 175°C, and the annealing cooling rate is 5°C / h;

[0055] The vacuum distillation combined with deoxidizer method consists of the following steps:

[0056] A1: A Se source and a P source are mixed to obtain a mixture, and a deoxidizer is added to the mixture to obtain a mixture to be purified; the purity of the high-purity Se and high-purity P is 5N; the deoxidizer is elemental Mg, and the amount of the deoxidizer is 0.1 wt% of the mixture;

[0057] A2: The mixture to be purified obtained in step A1 is added to the raw material tube through the opening on the raw material tube of the H-shaped double-tube quartz ampoule, and then vacuumed and preheated at the same time. 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 is pretreated with dehydroxylation, and the dehydroxylation pretreatment process is to clean the quartz reactor with hydrofluoric acid, deionized water and anhydrous ethanol in sequence, and finally placed in a dry oven for complete drying; the preheating temperature is 90°C; the vacuum degree of the vacuum is 1×10 -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 380°C, and the hot end temperature of the dual-temperature zone distillation furnace is 900°C.

[0058] The performance of the high transmittance P-Se chalcogenide glass prepared in Example 1 was tested, and the results are as follows: Figure 1 and Figure 2 、 Figure 3 shown.

[0059] Depend on Figure 1 It can be seen that the transmittance of the high-transmittance P-Se chalcogenide glass in the infrared window reaches 70%. The transition temperature of the high-transmittance P-Se chalcogenide glass was tested and the result was 180°C, which is suitable for mold stamping. Figure 2 It can be seen that the refractive index of the high-transmittance P-Se chalcogenide glass in the infrared window is 2.258. Figure 3 It can be seen that the high-transmittance P-Se chalcogenide glass shows three peaks in the infrared window Raman spectrum, corresponding to the PP bond, Se-Se bond, and P-Se bond.

[0060] Example 2

[0061] This embodiment provides a P-Se chalcogenide glass with high infrared transmittance, which is composed of the following components: Se: 65 at.% and P: 35 at.%;

[0062] The method for preparing the high-transmittance P-Se chalcogenide glass comprises the following steps:

[0063] S1: High-purity Se and high-purity P are mixed and purified by vacuum distillation combined with a scavenger method to obtain a purified mixture;

[0064] S2: Melting the purified mixture obtained in step S1: and then naturally cooling it to a quenching temperature for quenching, and finally heating it to an annealing temperature for annealing to obtain a high-transmittance P-Se chalcogenide glass; the melting temperature is 750°C, and the melting time is 30 hours; the quenching temperature is 360°C, and the quenching method is air-cooled quenching; the annealing temperature is 173°C, and the annealing cooling rate is 5°C / h.

[0065] The vacuum distillation combined with deoxidizer method consists of the following steps:

[0066] A1: Se source and P source are mixed to obtain a mixture, and a scavenger is added to the mixture to obtain a mixture to be purified; the purity of high-purity Se and high-purity P is 5N; the scavenger is elemental Mg, and the amount of the scavenger is 0.1wt% of the mixture;

[0067] A2: The mixture to be purified obtained in step A1 is added to the raw material tube through the opening on the raw material tube of the H-shaped double-tube quartz ampoule, and then vacuumed and preheated at the same time, and finally the opening on the raw material tube is sealed, and then the quartz reactor is placed in a dual-temperature zone distillation furnace for purification; the quartz reactor is pretreated with dehydroxylation, and the dehydroxylation pretreatment process is to clean the quartz reactor with hydrofluoric acid, deionized water and anhydrous ethanol in sequence, and finally placed in a dry oven for complete drying; the preheating temperature is 90°C; the vacuum degree of the vacuum is 1×10 -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 380°C, and the hot end temperature of the dual-temperature zone distillation furnace is 900°C.

[0068] The performance of the high-transmittance P-Se chalcogenide glass prepared in Example 2 was tested. At 25°C, the high-transmittance P-Se chalcogenide glass had an infrared transmittance of 68%, which is higher than that of common chalcogenide glasses on the market. The transition temperature of the high-transmittance P-Se chalcogenide glass was tested to be 176°C, making it suitable for mold stamping.

[0069] Comparative Example 1:

[0070] This comparative example provides a P-Se chalcogenide glass with high infrared transmittance, which is composed of the following components: Se: 55 at.% and P: 45 at.%;

[0071] The method for preparing the high-transmittance P-Se chalcogenide glass comprises the following steps:

[0072] S1: High-purity Se and high-purity P are mixed and purified by vacuum distillation combined with a scavenger method to obtain a purified mixture;

[0073] S2: Melting the purified mixture obtained in step S1, then naturally cooling it to a quenching temperature for quenching, and finally heating it to an annealing temperature for annealing to obtain a high-transmittance P-Se chalcogenide glass; the melting temperature is 770° C., the melting time is 30 h; the quenching temperature is 380° C., the quenching method is air-cooling quenching; the annealing temperature is 178° C., and the annealing cooling rate is 5° C. / h;

[0074] The vacuum distillation combined with deoxidizer method consists of the following steps:

[0075] A1: Se source and P source are mixed to obtain a mixture, and a scavenger is added to the mixture to obtain a mixture to be purified; the purity of high-purity Se and high-purity P is 5N; the scavenger is elemental Mg, and the amount of the scavenger is 0.1wt% of the mixture;

[0076] A2: The mixture to be purified obtained in step A1 is added to the raw material tube through the opening on the raw material tube of the H-shaped double-tube quartz ampoule, and then vacuumed and preheated at the same time, and finally the opening on the raw material tube is sealed, and then the quartz reactor is placed in a dual-temperature zone distillation furnace for purification; the quartz reactor is pretreated with dehydroxylation, and the dehydroxylation pretreatment process is to clean the quartz reactor with hydrofluoric acid, deionized water and anhydrous ethanol in sequence, and finally placed in a dry oven for complete drying; the preheating temperature is 90°C; the vacuum degree of the vacuum is 1×10 -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 380°C, and the hot end temperature of the dual-temperature zone distillation furnace is 900°C.

[0077] The product prepared in Comparative Example 1 was tested and found to fail to form glass.

[0078] Comparative Example 2:

[0079] This comparative example provides a chalcogenide glass with high infrared transmittance, which is composed of the following components: Se: 33.33 at.% and P: 66.66 at.%;

[0080] The method for preparing the infrared high-permeability sulfide glass comprises the following steps:

[0081] S1: mixing the high-purity Se and high-purity P and purifying them by vacuum distillation combined with a scavenger method to obtain a purified mixture;

[0082] S2: Melting the purified mixture obtained in step S1, then naturally cooling it to a quenching temperature for quenching, and finally heating it to an annealing temperature for annealing to obtain an infrared high-transmittance chalcogenide glass; the melting temperature is 800°C, and the melting time is 30 hours; the quenching temperature is 400°C, and the quenching method is air cooling quenching; the annealing temperature is 180°C, and the annealing cooling rate is 5°C / h;

[0083] The vacuum distillation combined with deoxidizer method consists of the following steps:

[0084] A1: A Se source and a P source are mixed to obtain a mixture, and a deoxidizer is added to the mixture to obtain a mixture to be purified; the purity of the high-purity Se and high-purity P is 5N; the deoxidizer is elemental Mg, and the amount of the deoxidizer is 0.1 wt% of the mixture;

[0085] A2: The mixture to be purified obtained in step A1 is added to the raw material tube through the opening on the raw material tube of the H-shaped double-tube quartz ampoule, and then vacuumed and preheated at the same time, and finally the opening on the raw material tube is sealed, and then the quartz reactor is placed in a dual-temperature zone distillation furnace for purification; the quartz reactor is pretreated with dehydroxylation, and the dehydroxylation pretreatment process is to clean the quartz reactor with hydrofluoric acid, deionized water and anhydrous ethanol in sequence, and finally placed in a dry oven for complete drying; the preheating temperature is 90°C; the vacuum degree of the vacuum is 1×10 -3 Pa, the vacuuming time is 3h; the cold end temperature of the dual-temperature zone distillation furnace is 380°C, and the hot end temperature of the dual-temperature zone distillation furnace is 900°C.

[0086] The performance of the high-transmittance chalcogenide glass prepared in Example 2 was tested. At 25° C., the transmittance of the infrared high-transmittance chalcogenide glass was 45%, which was lower than the transmittance of As2Se3 glass commonly available on the market.

[0087] Figure 4 This is the transmittance of the high-transmittance P2Se chalcogenide glass prepared in Comparative Example 2.

[0088] Depend on Figure 4 It can be seen that the transmittance of the high-transmittance P2Se chalcogenide glass in the infrared window reaches 45%; the transition temperature of the high-transmittance P2Se chalcogenide glass was tested, and the result was 185°C.

[0089] By comparing Examples 1-2 with Comparative Examples 1-2, it can be seen that as the P content in the chalcogenide glass increases, the transmittance of the chalcogenide glass continues to decrease. When the P content is higher than 50%, the prepared chalcogenide glass does not have a high transmittance advantage in the market.

[0090] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

[0091] In the description of the present application, the description with reference to the terms "one embodiment", "some embodiments", "in the present embodiment", "specific example", or "some examples" means that the specific features, mechanisms, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present application. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, mechanisms, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples. In addition, those skilled in the art can combine and combine different embodiments or examples described in this specification and the features of different embodiments or examples, unless they are contradictory.

[0092] The above description is merely a specific embodiment of the present application, but the scope of protection of the present application is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in the present application should be included in the scope of protection of the present application. Therefore, the scope of protection of the present application should be based on the scope of protection of the claims.

Claims

1. A method for preparing P-Se chalcogenide glass with high infrared transmittance, characterized in that: The following steps are involved: S1: Select a P source material and a Se source material, mix them, and then purify them by vacuum distillation and deoxidizing agent to obtain a purified mixture; the vacuum distillation and deoxidizing agent comprises: adding the mixed materials to a reaction container, preheating the reaction container in advance and evacuating the container at the same time, wherein the preheating temperature is 50-100°C, and the vacuum degree of the evacuation is 5×10 -5 Pa or above; S2: melting, quenching, and annealing the purified mixture obtained in step S1 in sequence to obtain a P-Se chalcogenide glass with high infrared transmittance; the melting temperature is 700-800°C, the quenching temperature is 350-400°C, the annealing temperature is 170-180°C, and the annealing cooling rate is 4-8°C / h; The chalcogenide glass comprises: P: 40-42 at. %; Se: 58-60 at. %, and the transition temperature of the chalcogenide glass is 175-185° C.

2. The method for preparing the infrared-high-transmittance P-Se chalcogenide glass according to claim 1, characterized in that: In step S1, the reaction container is a quartz reactor.

3. The method for preparing the infrared-high-transmittance P-Se chalcogenide glass according to claim 2, characterized in that: When the quartz reactor is a quartz reactor with an opening at one end, the vacuuming method is: after mixing the raw materials, add them into the raw material tube through the opening on the raw material tube of the quartz reactor, then vacuumize, and finally seal the opening on the raw material tube; when the quartz reactor is a quartz reactor with openings at both ends, the vacuuming method is: add the raw materials into the raw material tube through the first opening of the quartz reactor, seal the first opening, then vacuumize the second opening, and finally seal the second opening.

4. The method for preparing the infrared-high-transmittance P-Se chalcogenide glass according to claim 3, characterized in that: The sealing method is to seal by using an oxyhydrogen flame or an oxyacetylene flame.

5. The method for preparing the infrared-high-transmittance P-Se chalcogenide glass according to claim 1, characterized in that: The purity of the P source material and the Se source material are both above 5N, and the vacuuming time is above 3 hours.

6. The method for preparing the infrared highly transparent P-Se chalcogenide glass according to claim 1, characterized in that: In step S2, the melting temperature is 750° C. and the melting time is 27 to 28 hours.

7. The method for preparing P-Se chalcogenide glass with high infrared transmittance according to claim 1, characterized in that: In step S2, the quenching temperature is 370-390°C, and the quenching method is air-cooling quenching.

8. The method for preparing P-Se chalcogenide glass with high infrared transmittance according to claim 1, characterized in that: In step S2, the annealing temperature is 175-178°C, and the annealing cooling rate is 5°C / h.

9. A method for preparing P-Se chalcogenide glass with high infrared transmittance, characterized in that: The following steps are involved: S1: High-purity Se and high-purity P are mixed and purified by vacuum distillation combined with a scavenger method to obtain a purified mixture; S2: Melting the purified mixture obtained in step S1, then naturally cooling it to a quenching temperature for quenching, and finally heating it to an annealing temperature for annealing to obtain a high-transmittance P-Se chalcogenide glass; the melting temperature is 750° C., and the melting time is 30 hours; the quenching temperature is 360° C., and the quenching method is air-cooled quenching; the annealing temperature is 173° C., and the annealing cooling rate is 5° C. / h; The vacuum distillation combined with deoxidizer method consists of the following steps: A1: Se source and P source are mixed to obtain a mixture, and a scavenger is added to the mixture to obtain a mixture to be purified; the purity of high-purity Se and high-purity P is 5N; the scavenger is elemental Mg, and the amount of the scavenger is 0.1wt% of the mixture; A2: The mixture to be purified obtained in step A1 is added to the raw material tube through the opening on the raw material tube of the H-shaped double-tube quartz ampoule, and then vacuumed and preheated at the same time. 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 is pretreated with dehydroxylation, and the dehydroxylation pretreatment process is to clean the quartz reactor with hydrofluoric acid, deionized water and anhydrous ethanol in sequence, and finally placed in a dry oven for complete drying; the preheating temperature is 90°C; the vacuum degree of the vacuum is 1×10 -3 Pa, the vacuum time is 3h; the cold end temperature of the dual temperature zone distillation furnace is 380°C, and the hot end temperature of the dual temperature zone distillation furnace is 900°C; The chalcogenide glass includes 65 at. % Se and 35 at. % P, and the transition temperature of the chalcogenide glass is 176° C.

10. A P-Se chalcogenide glass with high infrared transmittance, characterized in that: The infrared highly transparent P-Se chalcogenide glass is prepared by the preparation method according to any one of claims 1 to 8, wherein the chalcogenide glass comprises: P: 40 to 42 at.%; Se: 58 to 60 at.%, and the transition temperature of the chalcogenide glass is 175 to 185°C.