Chalcogenide glass leftover material recycling process

Abstract

The invention relates to a chalcogenide glass leftover material recycling and reusing process, which comprises the following steps: wiping the surface of a blocky leftover material, soaking in acetone, carrying out ultrasonic spray cleaning, draining and drying; the dried blocky leftover materials are loaded into a quartz loading pipe and stopped by a quartz filter element, and the quartz filter pipe is vacuumized and then welded and sealed; the welded and sealed quartz filter tube is vertically arranged in a purification furnace, the blocky leftover materials are heated and melted to form molten glass, the molten glass flows downwards to penetrate through the quartz filter element to be filtered and drops into the quartz collection tube, and when heat preservation is finished, the molten glass is completely collected into the quartz collection tube; taking out the quartz filter tube for quenching and cooling; separating the quartz charging pipe from the quartz collecting pipe; putting the separated quartz collecting tube into a rocking furnace; taking out the quartz collecting tube from the rocking furnace, and quenching and forming; putting the quartz collecting tube into an annealing furnace; and crushing the quartz collecting tube and taking out the glass rod.

Description

Technical Field

[0001] The present disclosure relates to the field of chalcogenide glasses, and more particularly to a process for recycling chalcogenide glass scraps. Background Art

[0002] Chalcogenide glass is a novel matrix material for photonic devices. It is an inorganic glass mainly composed of three elements, sulfur (S), selenium (Se), and tellurium (Te), excluding oxygen and polonium, among the elements in Group VIA of the periodic table, and combined with other elements (such as arsenic, antimony, germanium, etc.). In addition, in order to improve the performance of chalcogenide glass materials, metal ions with large radii, high quality, and high polarizability (such as Bi, Pb, Sn, etc.) are introduced into the chalcogenide glass. Chalcogenide glass materials have currently been widely used in fields such as infrared lenses and thermal imaging lenses.

[0003] As a brittle inorganic non-metallic material, chalcogenide glass materials will generate a large amount of scraps and unqualified processed waste during the process of being processed into various specifications of lenses through a series of steps such as cutting, turning, grinding, and milling. The component composition of chalcogenide glass is relatively complex, and generally contains elements such as As, Se, Sb, and Ge. If not reasonably recycled, the leftover scraps as hazardous waste will also cause waste of rare and precious resources and environmental pollution.

[0004] Currently, relevant patent reports are all based on the characteristics that most compounds of chalcogen elements have high saturated vapor pressures and are easy to sublimate and vaporize. By utilizing the large difference in saturated vapor pressures between chalcogen compounds and impurities and oxides, the above-mentioned defective cut-off materials and processed scraps are subjected to distillation purification and recycling treatment. This method can solve most chalcogenide glass products with high saturated vapor pressures and easy sublimation and vaporization. However, there are many types of chalcogenide glass products, and the saturated vapor pressures of individual components of many chalcogenide glass products are low, and it is difficult to achieve recycling treatment through distillation purification, such as As 30 Se 63 Sb4Sn3 doped chalcogenide glass products. Summary of the Invention

[0005] In view of the problems existing in the background art, one object of the present disclosure is to provide a process for recycling chalcogenide glass scraps, which can recycle components with low saturated vapor pressures that are difficult to recover by distillation.

[0006] Another object of the present disclosure is to provide a process for recycling chalcogenide glass scraps, which can improve the purification efficiency.

[0007] Another object of the present disclosure is to provide a process for recycling chalcogenide glass scraps, which can reduce energy consumption.

[0008] Thus, a process for recycling and reusing chalcogenide glass scraps includes the following steps: S1, wiping the surface of the block scraps clean, then soaking in acetone, ultrasonic spray cleaning, draining and drying; S2, loading the dried block scraps into the quartz loading tube of the quartz filter tube and stopping it with the quartz filter element, evacuating the quartz filter tube, and then welding and sealing the quartz loading tube with a quartz tube cap; S3, vertically loading the welded quartz filter tube into a purification furnace, heating the upper heating zone of the purification furnace corresponding to the quartz loading tube and the quartz filter element and the lower heating zone corresponding to the quartz collecting tube to above the Ts temperature of the chalcogenide glass and keeping them warm, the temperature of the upper heating zone is higher than that of the lower heating zone, and the block scraps are heated and melted. Glass liquid is formed, and the glass liquid flows downward through the quartz filter element to be filtered and drips into the quartz collecting tube. When the insulation is finished, the glass liquid is completely collected in the quartz collecting tube; S4, the quartz filter tube is taken out from the purification furnace and the glass liquid is quenched and cooled; S5, the quartz filter tube is welded and sealed under the quartz filter element to separate the quartz charging tube from the quartz collecting tube; S6, the separated quartz collecting tube is loaded into a rocking furnace for heating and rocking to melt and homogenize the glass liquid, and then cooled; S7, the quartz collecting tube is taken out from the rocking furnace and the glass liquid is quenched and formed into a glass rod; S8, the quartz collecting tube and the glass rod are put into an annealing furnace for annealing; S9, after annealing, the quartz collecting tube is broken and the glass rod is taken out.

[0009] The beneficial effects of the present disclosure are as follows: In the sulfur-based glass scrap recycling and reuse process according to the present disclosure, the glass liquid filtration and purification in step S3 replaces the distillation purification method of the background technology, so that the components with low saturated vapor pressure that are difficult to recover by distillation can be recycled through the glass liquid filtration and purification method, which is beneficial to improving the quality of the glass rods formed by recycling. In addition, the temperature required for the glass liquid filtration in step S3 is lower than the temperature for distillation purification, the energy consumption is low, and the purification efficiency is high. In addition, the glass liquid filtration in step S3 is carried out by gravity, the filtration speed is fast, and the purification efficiency is further improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0010] Figure 1 It is an exploded cross-sectional view of a quartz filter tube used in the chalcogenide glass scrap recycling and reuse process according to the present disclosure.

[0011] Figure 2 yes Figure 1 An enlarged cross-sectional view taken along line AA.

[0012] Figure 3 The diagram shows a state where block-shaped scraps are loaded into a quartz loading tube of a quartz filter tube.

[0013] Figure 4 Shown in Figure 3 The quartz tube cap is loaded into the quartz charging tube.

[0014] Figure 5 It shows that Figure 4 on the basis of

[0015] Figure 6 It shows that Figure 5 the state where the quartz filter tube is placed in the purification furnace on the basis of

[0016] Figure 7 It shows that Figure 6 the state where the blocky scraps form glass liquid and are filtered and collected on the basis of

[0017] The description of the reference numerals is as follows:

[0018] 100 Quartz filter tube 200 Purification furnace

[0019] 11 Quartz loading tube 21 Upper heating zone

[0020] 111 Small equal-diameter section 22 Lower heating zone

[0021] 112 Bulge 23 Furnace body

[0022] 12 Quartz collection tube 300 Blocky scraps

[0023] 13 Quartz filter core 400 Glass liquid

[0024] 14 Quartz tube cap W Welding seal position

[0025] 15 Equal-diameter thin tube Specific embodiments

[0026] It will be understood that the disclosed embodiments are merely examples of the present disclosure, and the present disclosure can be implemented in various forms. Therefore, the specific details disclosed herein should not be construed as limiting, but only as a basis for the claims and as a representative basis for teaching those of ordinary skill in the art to implement the present disclosure in various ways.

[0027] [Recycling process for chalcogenide glass scraps]

[0028] Referring to Figures 1 to 7 , the recycling process for chalcogenide glass scraps according to the present disclosure includes the steps:

[0029] S1. Wipe the surface of the blocky scraps 300 clean, then soak them in acetone, perform ultrasonic spraying cleaning, drain, and dry.

[0030] S2. Load the dried blocky scraps 300 into the quartz loading tube 11 of the quartz filter tube 100 and stop them with the quartz filter core 13. Evacuate the quartz filter tube 100, and then weld-seal the quartz loading tube 11 with the quartz tube cap 14.

[0031] S3. Vertically load the welded quartz filter tube 100 into the purification furnace 200. Heat the upper heating zone 21 of the purification furnace 200 corresponding to the quartz loading tube 11 and the quartz filter core 13 and the lower heating zone 22 corresponding to the quartz collection tube 12 to a temperature above the Ts temperature of the chalcogenide glass and keep it warm. The temperature of the upper heating zone 21 is higher than that of the lower heating zone 22. The massive scraps 300 are heated and melted to form a glass liquid 400. The glass liquid 400 flows downward through the quartz filter core 13, is filtered and drips into the quartz collection tube 12. When the heat preservation ends, the glass liquid 400 is completely collected into the quartz collection tube 12;

[0032] S4. Take out the quartz filter tube 100 from the purification furnace 200 and quench and cool the glass liquid 400;

[0033] S5. Weld and seal the quartz filter tube 100 below the quartz filter core 13 to separate the quartz loading tube 11 from the quartz collection tube 12;

[0034] S6. Load the separated quartz collection tube 12 into a rocking furnace, heat and rock it to melt and homogenize the glass liquid 400, and then cool it down;

[0035] S7. Take out the quartz collection tube 12 from the rocking furnace and quench and shape the glass liquid 400 into a glass rod;

[0036] S8. Put the quartz collection tube 12 together with the glass rod into an annealing furnace for annealing;

[0037] S9. After annealing, break the quartz collection tube 12 and take out the glass rod.

[0038] In the process for recycling chalcogenide glass scraps according to the present disclosure, the liquid filtration and purification of the glass liquid in step S3 replaces the distillation and purification method in the background art, enabling components with a low saturated vapor pressure that are difficult to recover by distillation to be recovered and utilized through the liquid filtration and purification method of the glass liquid, which is beneficial to improving the quality of the glass rod formed by recycling. In addition, the temperature required for the liquid filtration of the glass liquid in step S3 is lower than that of distillation and purification, with low energy consumption and high purification efficiency. In addition, the filtration of the glass liquid in step S3 utilizes gravity, with a fast filtration speed and further improved purification efficiency.

[0039] The process for recycling chalcogenide glass scraps according to the present disclosure is not only suitable for the recycling of chalcogenide glass scraps, but also suitable for the filtration and purification of chalcogenide glass raw materials.

[0040] In step S1, the massive scraps 300 include but are not limited to As 30 Se 63 Sb4Sn3 or Ge 28 Sb 12 Se 60 .

[0041] In step S1, the maximum dimension of the block-shaped scrap 300 is between 20 - 100 mm, or the block-shaped scrap 300 is formed by crushing a larger block-shaped scrap 300 to fit the inner diameter of the quartz loading tube 11 of the quartz filter tube 100.

[0042] Cleaning the surface of step S1 can be, for example: using a scouring pad to clean the foreign matters including cutting coolant, oil stain, and dust on the surface of the block-shaped scrap 300.

[0043] The acetone in step S1 can fully dissolve the organic matter on the block-shaped scrap 300 after cleaning the surface. In one example, the concentration of acetone is 50 - 90%, and it is soaked for 3 - 10 h.

[0044] The ultrasonic spray cleaning, draining, and drying in step S1 ensure the surface cleanliness of the block-shaped scrap 300 for recycling. In one example, in step S1, ultrasonic spray cleaning is performed multiple times, with each ultrasonic cleaning for 10 - 30 min and spray cleaning for 1 - 3 min, and the ultrasonic cleaning and spray cleaning are repeated 2 - 5 times. For example, in step S1, drying is carried out in an oven, the drying temperature is 100 - 150 °C, and the drying time is 5 - 10 h.

[0045] The vacuum pumping in step S2 reduces the content of air remaining in the quartz filter tube 100 after welding and sealing, and avoids affecting the quality of the glass rod in step S9. In one example, in step S2, the quartz filter tube 100 is evacuated to below 5×10 -3 Pa.

[0046] As Figure 1 shown, in one example, the facing ends of the quartz loading tube 11 and the quartz collection tube 12 taper towards each other; the quartz filter core 13 is installed between the equal-diameter thin tubes 15 between the tapered ends of the quartz loading tube 11 and the quartz collection tube 12 facing each other; the welding and sealing in step S5 is performed on the equal-diameter thin tube 15 below the quartz filter core 13.

[0047] As Figure 1 shown, in one example, the inner diameter dimensions of the equal-diameter parts of the quartz loading tube 11 and the quartz collection tube 12 are both 100 mm.

[0048] As Figure 1 shown, in one example, the quartz loading tube 11 tapers to a small equal-diameter section 111 on the side welded to the quartz tube cap 14, which is beneficial to reducing the outer diameter of the quartz tube cap 14 and improving the welding and sealing efficiency.

[0049] As Figure 1As shown, in one example, the quartz loading tube 11 is provided with a plurality of bumps 112 that bulge inwardly and protrude outwardly in the small equal-diameter section 111. The plurality of bumps 112 are used to stop and support the quartz tube cap 14 in the quartz loading tube 11, thereby facilitating the positioning of the quartz tube cap 14 in the quartz loading tube 11 and the evacuation and sealing welding in step S2. The number of the plurality of bumps 112 is, for example, four and they are arranged at equal intervals circumferentially. Before the quartz tube cap 14 is sealed in the quartz loading tube 11, there is a clearance fit, and the clearance is smaller than the degree to which the bumps 112 protrude from the inner wall of the quartz loading tube 11. The clearance is about 1 mm, for example.

[0050] In one example, the aperture diameter of the filter holes of the quartz filter core 13 is 150 - 200 mesh.

[0051] As Figure 1 shown, in one example, the quartz loading tube 11 and the quartz collection tube 12 are an integral single piece.

[0052] The upper heating zone and the lower heating zone 22 in step S3 achieve independent temperature control from each other. In step S3, for example, the upper heating zone and the lower heating zone 22 are heated to 200 - 500 °C above the Ts temperature of the chalcogenide glass, and the upper heating zone is kept 10 - 100 °C higher than the temperature of the lower heating zone 22 and insulated for 2 - 5 h. Further, for example, in step S3, the upper heating zone is heated to 500 - 610 °C, the lower heating zone 22 is heated to 490 - 600 °C, and the upper heating zone is kept 10 °C higher than the temperature of the lower heating zone 22 and insulated for 3 h.

[0053] Referring to Figure 6 and Figure 7 , in one example, the purification furnace 200 includes two semi-cylindrical furnace bodies 23 that are combined in an opening and closing manner, and the upper heating zone 21 and the lower heating zone 22 are arranged inside the furnace bodies 23 that are combined in an opening and closing manner. Thus, it is convenient for the quartz filter tube 100 to be loaded into and unloaded from the purification furnace 200.

[0054] In step S6, for example, the rocking furnace is heated to 800 - 900 °C and insulated for 5 - 10 h to melt and homogenize the glass liquid 400. After the glass liquid 400 is melted and homogenized, it is cooled to 400 - 700 °C. Further, in one example, in step S6, the rocking furnace is heated to 800 - 900 °C and insulated for 6 h to melt and homogenize the glass liquid 400. After the glass liquid 400 is melted and homogenized, it is cooled to 500 - 600 °C. In one example, in step S6, the rocking furnace rocks at a rocking angle of ±60° and a rocking rate of 5 ° / s.

[0055] In step S8, for example, the annealing temperature of the annealing furnace is the Tg temperature of the chalcogenide glass.

[0056] In one example, after step S9 is completed, the impurity grade of the glass rod is grade 1, As 30Se 63 The transmittance of the chalcogenide glass scraps of Sb4Sn3 is on average 64.44 - 64.46% in the 8 - 12μm band; Ge 28 Sb 12 Se 60 The transmittance of the chalcogenide glass scraps of is on average 66.82 - 66.88% in the 8 - 12μm band.

[0057] [Test]

[0058] Example 1

[0059] Refer to Figures 1 to 7 , the recycling process of the chalcogenide glass scraps in Example 1 adopts the following steps:

[0060] S1, wipe the surface of the bulk scraps 300 clean, then soak in acetone, ultrasonic spray cleaning, drain, and dry.

[0061] Among them,

[0062] The composition of the bulk scraps 300 is As 30 Se 63 Sb4Sn3,

[0063] The shape and size of the bulk scraps 300 vary, and the maximum size of the bulk scraps 300 is between 20 - 100mm.

[0064] Wipe the foreign matters on the surface of the bulk scraps 300, including cutting coolant, oil stain, and dust, clean.

[0065] The concentration of acetone is 60%, soak for 5h.

[0066] Ultrasonic spray cleaning is carried out multiple times, each time ultrasonic cleaning for 15min and spray cleaning for 1min, repeat ultrasonic cleaning and spray cleaning 3 times.

[0067] Drying is carried out in an oven, the drying temperature is 110℃, and the drying time is 10h.

[0068] S2, load the dried bulk scraps 300 into the quartz loading tube 11 of the quartz filter tube 100 and stop it with the quartz filter core 13, evacuate the quartz filter tube 100, and then weld - seal the quartz loading tube 11 with the quartz tube cap 14.

[0069] Among them,

[0070] The quartz loading tube 11 and the quartz collection tube 12 are an integral single piece.

[0071] The inner diameter dimensions of the equal - diameter parts of the quartz loading tube 11 and the quartz collection tube 12 are both 100mm.

[0072] The facing ends of the quartz loading tube 11 and the quartz collection tube 12 taper towards each other, and the quartz filter core 13 is installed between the equal-diameter thin tubes 15 between the tapering ends of the quartz loading tube 11 and the quartz collection tube 12 facing each other.

[0073] The quartz loading tube 11 tapers to a small equal-diameter section 111 on the side sealed with the quartz tube cap 14.

[0074] The quartz loading tube 11 is provided with four bulges 112 that are concave on the outside and convex on the inside and bulge inward at the small equal-diameter section 111. The four bulges 112 stop and support the quartz tube cap 14 in the quartz loading tube 11.

[0075] The aperture diameter of the filter holes of the quartz filter core 13 is 200 mesh.

[0076] Before the quartz tube cap 14 is sealed in the quartz loading tube 11, there is a clearance fit, and the clearance is less than the degree to which the bulge 112 protrudes from the inner wall of the quartz loading tube 11. The clearance is 1 mm.

[0077] Vacuum is pumped to 5×10 -3 Pa;

[0078] S3. Vertically install the well-sealed quartz filter tube 100 into the purification furnace 200. Heat the upper heating zone 21 corresponding to the quartz loading tube 11 and the quartz filter core 13 and the lower heating zone 22 corresponding to the quartz collection tube 12 in the purification furnace 200 to above the Ts temperature of the chalcogenide glass and keep it warm. The upper heating zone 21 is at a higher temperature than the lower heating zone 22. The blocky waste material 300 is heated and melted to form the glass liquid 400. The glass liquid 400 flows downward through the quartz filter core 13, is filtered, and drips into the quartz collection tube 12. When the heat preservation ends, the glass liquid 400 is completely collected in the quartz collection tube 12.

[0079] Among them,

[0080] The purification furnace 200 includes two semi-cylindrical furnace bodies 23 combined in an openable and closable manner. The upper heating zone 21 and the lower heating zone 22 are arranged inside the openable and closable combined furnace body 23.

[0081] The upper heating zone is heated to 500 °C, and the lower heating zone 22 is heated to 490 °C. Keep the upper heating zone at a temperature 10 °C higher than the lower heating zone 22 and keep it warm for 3 h.

[0082] S4. Take out the quartz filter tube 100 from the purification furnace 200 and quench and cool the glass liquid 400.

[0083] S5. Seal the equal-diameter thin tube 15 of the quartz filter tube 100 below the quartz filter core 13 to separate the quartz loading tube 11 from the quartz collection tube 12.

[0084] S6, placing the separated quartz collecting tube 12 into a rocking furnace, heating and rocking it, so that the glass liquid 400 is melted and homogenized, and then cooling it.

[0085] in,

[0086] The swing furnace is heated to 800°C and kept warm for 6 hours to melt and homogenize the glass liquid 400. After the glass liquid 400 is melted and homogenized, the temperature is lowered to 500°C.

[0087] The rocking furnace rocked at a rocking angle of ±60° and a rocking rate of 5° / s;

[0088] S7, taking out the quartz collecting tube 12 from the rocking furnace and quenching the glass liquid 400 into a glass rod;

[0089] S8, placing the quartz collecting tube 12 together with the glass rod into an annealing furnace for annealing, wherein the annealing temperature of the annealing furnace is 190° C.;

[0090] S9, after annealing, the quartz collecting tube 12 is broken and the glass rod is taken out.

[0091] Example 2

[0092] Reference Figures 1 to 7 The chalcogenide glass scrap recycling process of Example 2 adopts the following steps:

[0093] S1, clean the surface of the block scrap 300, then soak it in acetone, clean it with ultrasonic spray, drain it and dry it.

[0094] in,

[0095] The composition of the block scrap 300 is Ge 28 Sb 12 Se 60 ,

[0096] The block scraps 300 have different shapes and sizes, and the maximum size of the block scraps 300 is between 20-90 mm.

[0097] Use a scouring pad to clean the foreign matter including cutting coolant, oil, and dust on the surface of the block scrap 300.

[0098] Acetone concentration is 60%, soak for 5 hours,

[0099] Ultrasonic cleaning and spray cleaning were performed multiple times, with each ultrasonic cleaning lasting 15 minutes and spray cleaning lasting 1 minute. Ultrasonic cleaning and spray cleaning were repeated 3 times.

[0100] The drying is carried out in an oven at a temperature of 110°C and a drying time of 10 h;

[0101] S2. Load the dried blocky scraps 300 into the quartz loading tube 11 of the quartz filter tube 100 and stop it with the quartz filter core 13. Evacuate the quartz filter tube 100, and then seal the quartz loading tube 11 with the quartz tube cap 14.

[0102] Among them,

[0103] The quartz loading tube 11 and the quartz collection tube 12 are an integral single piece.

[0104] The inner diameter of the equal-diameter parts of the quartz loading tube 11 and the quartz collection tube 12 is 100 mm.

[0105] The facing ends of the quartz loading tube 11 and the quartz collection tube 12 taper towards each other. The quartz filter core 13 is installed between the equal-diameter thin tubes 15 between the tapered ends of the quartz loading tube 11 and the quartz collection tube 12.

[0106] The quartz loading tube 11 tapers to a small equal-diameter section 111 on the side sealed with the quartz tube cap 14.

[0107] The quartz loading tube 11 is provided with four bulges 112 that are concave on the outside and convex on the inside and bulge towards the inside at the small equal-diameter section 111. The four bulges 112 stop and support the quartz tube cap 14 in the quartz loading tube 11.

[0108] The aperture of the filter holes of the quartz filter core 13 is 200 mesh.

[0109] Before being sealed in the quartz loading tube 11, the quartz tube cap 14 has a clearance fit, and the clearance is less than the degree to which the bulge 112 protrudes from the inner wall of the quartz loading tube 11. The clearance is 1 mm.

[0110] Evacuate to 5×10 -3 Pa;

[0111] S3. Vertically load the sealed quartz filter tube 100 into the purification furnace 200. Heat the upper heating zone 21 corresponding to the quartz loading tube 11 and the quartz filter core 13 and the lower heating zone 22 corresponding to the quartz collection tube 12 in the purification furnace 200 to above the Ts temperature of the chalcogenide glass and keep it warm. The upper heating zone 21 is hotter than the lower heating zone 22. The blocky scraps 300 are heated and melted to form a glass liquid 400. The glass liquid 400 flows downward through the quartz filter core 13, is filtered, and drips into the quartz collection tube 12. When the heat preservation ends, the glass liquid 400 is completely collected in the quartz collection tube 12.

[0112] Among them,

[0113] The purification furnace 200 includes two semi-cylindrical furnace bodies 23 that are combined in an opening and closing manner. The upper heating zone 21 and the lower heating zone 22 are arranged inside the opening and closing combined furnace body 23.

[0114] The upper heating zone is heated to 610 °C, and the lower heating zone 22 is heated to 600 °C. Keep the temperature of the upper heating zone 10 °C higher than that of the lower heating zone 22 and hold for 3 h;

[0115] S4. Take out the quartz filter tube 100 from the purification furnace 200 and quench and cool the glass liquid 400;

[0116] S5. Seal the equal-diameter thin tube 15 of the quartz filter tube 100 below the quartz filter core 13 to separate the quartz charging tube 11 from the quartz collection tube 12;

[0117] S6. Load the separated quartz collection tube 12 into a rocking furnace, heat and rock it to melt and homogenize the glass liquid 400, and then cool it down.

[0118] Among them,

[0119] The rocking furnace is heated to 900 °C and held for 6 h to melt and homogenize the glass liquid 400. After the glass liquid 400 is melted and homogenized, it is cooled to 600 °C.

[0120] The rocking furnace rocks at a rocking angle of ±60° and a rocking rate of 5° / s;

[0121] S7. Take out the quartz collection tube 12 from the rocking furnace and quench and form the glass liquid 400 into a glass rod;

[0122] S8. Put the quartz collection tube 12 together with the glass rod into an annealing furnace for annealing. Among them, the annealing temperature of the annealing furnace is 280 °C;

[0123] S9. After annealing, break the quartz collection tube 12 and take out the glass rod.

[0124] Steps S3 to S5 of Example 1 and Example 2 are carried out for two quartz filter tubes 100 respectively, and steps S6 to S9 are carried out for two quartz collection tubes 12 simultaneously. The corresponding detected rod materials are rod material 1 and rod material 2 in Table 1 and Table 2.

[0125] Table 1 and Table 2 give the test results of the rod materials prepared from high-purity raw materials and the rod materials prepared by the recycling process (i.e., glass rods, which are rod material 1 and rod material 2 in Table 1 and Table 2). Among them, the impurity grades are judged and detected according to the methods specified in GB / T 32561.3-2016.

[0126] Table 1 Test Results of Rod Materials Prepared from High-Purity Raw Materials and Rod Materials Prepared by Recycling Process (for As 30 Se 63 Sb4Sn3)

[0127]

[0128] Table 2 Detection Results of Rods Prepared from High-Purity Raw Materials and Rods Prepared by Recycling Process (for Ge 28 Sb 12 Se 60 )

[0129]

[0130]

[0131] Multiple exemplary embodiments are described with the above detailed description, but this document is not intended to be limited to the explicitly disclosed combinations. Thus, unless otherwise specified, the various features disclosed herein may be combined together to form multiple additional combinations not shown for the sake of brevity.

Claims

1. A process for recycling and reusing chalcogenide glass scraps, characterized in that: Includes steps: S1, clean the surface of the block scrap (300), then soak it in acetone, clean it with ultrasonic spray, drain it and dry it; S2, loading the dried block scraps (300) into the quartz loading tube (11) of the quartz filter tube (100) and stopping it with the quartz filter core (13), evacuating the quartz filter tube (100), and then welding and sealing the quartz loading tube (11) with a quartz tube cap (14); S3, vertically loading the welded quartz filter tube (100) into the purification furnace (200), heating the upper heating zone (21) corresponding to the quartz charging tube (11) and the quartz filter core (13) and the lower heating zone (22) corresponding to the quartz collecting tube (12) of the purification furnace (200) to a temperature above the Ts temperature of the chalcogenide glass and keeping the temperature, the temperature of the upper heating zone (21) is higher than that of the lower heating zone (22), the blocky scraps (300) are heated and melted to form glass liquid (400), the glass liquid (400) flows downward, passes through the quartz filter core (13), is filtered and drips into the quartz collecting tube (12), and when the insulation is finished, the glass liquid (400) is completely collected in the quartz collecting tube (12); S4, taking out the quartz filter tube (100) from the purification furnace (200) and quenching and cooling the glass liquid (400); S5, welding and sealing the quartz filter tube (100) below the quartz filter core (13) to separate the quartz loading tube (11) from the quartz collecting tube (12); S6, placing the separated quartz collecting tube (12) into a rocking furnace, heating and rocking it, so that the glass liquid (400) is melted and homogenized, and then cooling it; S7, taking out the quartz collecting tube (12) from the rocking furnace and quenching the glass liquid (400) into a glass rod; S8, placing the quartz collecting tube (12) together with the glass rod into an annealing furnace for annealing; S9, after annealing, the quartz collecting tube (12) is broken and the glass rod is taken out.

2. The chalcogenide glass scrap recycling process according to claim 1, characterized in that: In step S1, the block scrap (300) includes As 30 Se 63 Sb4Sn3 or Ge 28 Sb 12 Se 60 ; and / or In step S1, the maximum size of the block scrap (300) is between 20-100 mm or the block scrap (300) is crushed from a larger block scrap (300); and / or In step S1, foreign matters including cutting coolant, oil stains, and dust on the surface of the block scrap (300) are wiped clean with a scouring pad; and / or In step S1, the concentration of acetone is 50-90%, and the soaking time is 3-10 hours; and / or In step S1, ultrasonic spray cleaning is performed multiple times, each time ultrasonic cleaning lasts 10-30 minutes and spray cleaning lasts 1-3 minutes, and ultrasonic cleaning and spray cleaning are repeated 2-5 times; and / or In step S1, drying is performed in an oven at a drying temperature of 100-150°C and a drying time of 5-10 hours.

3. The chalcogenide glass scrap recycling process according to claim 1, characterized in that: In step S2, the quartz filter tube (100) is evacuated to 5×10 -3 Pa or less; and / or In step S2, the two ends of the quartz charging tube (11) and the quartz collecting tube (12) facing each other are tapered, the quartz filter element (13) is installed between the equal-diameter capillary tube (15) between the mutually tapered ends of the quartz charging tube (11) and the quartz collecting tube (12), and the sealing welding in step S5 is to seal the equal-diameter capillary tube (15) below the quartz filter element (13); and / or In step S2, the inner diameters of the equal diameter parts of the quartz charging tube (11) and the quartz collecting tube (12) are both 100 mm; and / or In step S2, the pore size of the filter holes of the quartz filter element (13) is 150-200 mesh; and / or In step S2, the quartz charging tube (11) and the quartz collecting tube (12) are integrated into a single piece.

4. The chalcogenide glass scrap recycling process according to claim 1, characterized in that: In step S2, the quartz charging tube (11) is gradually reduced to a small equal diameter section (111) at the side where it is welded and sealed with the quartz tube cap (14).

5. The chalcogenide glass scrap recycling process according to claim 4, characterized in that: In step S2, the quartz charging tube (11) is provided with a plurality of bulges (112) which are concave on the outside and convex on the inside and bulge inwardly at the small equal-diameter section (111), and the plurality of bulges (112) are used to stop and support the quartz tube cap (14) in the quartz charging tube (11).

6. The chalcogenide glass scrap recycling process according to claim 1, characterized in that: In step S3, the upper heating zone and the lower heating zone (22) are heated to 200-500°C above the Ts temperature of the chalcogenide glass, and the temperature of the upper heating zone is kept 10-100°C higher than that of the lower heating zone (22) for 2-5 hours; and / or In step S3, the purification furnace (200) includes two semi-cylindrical furnace bodies (23) in an open-closed combination, and the upper heating zone (21) and the lower heating zone (22) are arranged on the inner side of the open-closed combination furnace body (23).

7. The process for recycling and reusing chalcogenide glass scraps according to claim 6, characterized in that: In step S3, the upper heating zone is heated to 500-610°C, and the lower heating zone (22) is heated to 490-600°C. The temperature of the upper heating zone is kept 10°C higher than that of the lower heating zone (22) for 3 hours.

8. The chalcogenide glass scrap recycling process according to claim 1, characterized in that: In step S6, the rocking furnace is heated to 800-900°C and kept at this temperature for 5-10 hours to melt and homogenize the glass liquid (400). After the glass liquid (400) is melted and homogenized, the temperature is lowered to 400-700°C.

9. The chalcogenide glass scrap recycling process according to claim 8, characterized in that: In step S6, the rocking furnace is heated to 800-900° C. and kept at this temperature for 6 hours to melt and homogenize the glass liquid (400), and after the glass liquid (400) is melted and homogenized, the temperature is lowered to 500-600° C.; and / or In step S6 , the rocking furnace is rocked at a rocking angle of ±60° and a rocking rate of 5° / s.

10. The chalcogenide glass scrap recycling process according to claim 1, characterized in that: In step S8, the annealing temperature of the annealing furnace is the Tg temperature of the chalcogenide glass; and / or After step S9 is completed, the impurity level of the glass rod is level 1, As 30 Se 63 The transmittance of the Sb4Sn3 chalcogenide glass scraps in the 8-12μm band is 64.44-64.46% on average. 28 Sb 12 Se 60 The average transmittance of the chalcogenide glass scraps in the 8-12μm band is 66.82-66.88%.

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