Optical Glass Preparation Device and Preparation Method

Abstract

The present application relates to an optical glass preparation device and a preparation method in the technical field of infrared glass preparation. The optical glass preparation device includes: a heating furnace, which forms a furnace cavity therein; a material container; a swing rotation mechanism, which is arranged in the furnace cavity and is used for fixing the material container and driving the material container to swing and rotate to mix materials; a melt quenching mechanism, which is communicated with the furnace cavity and is used for rapidly cooling the melt formed by melting the materials in the material container. The optical glass preparation device and the preparation method of the present application can obtain chalcogenide glass products with good optical uniformity, stable transmission performance, and large size, and reduce operation risks and improve safety.

Description

Technical Field

[0001] This application relates to the technical field of infrared glass preparation, and particularly to an optical glass preparation device and a preparation method. Background Art

[0002] Chalcogenide glass is an amorphous infrared optical material formed based on the sulfur (S), selenium (Se), and tellurium (Te) in Group VI of the periodic table, and introducing other metal or non-metal elements (such as Ge, As, Sb elements, etc.). Compared with crystal infrared materials such as single crystal and polycrystal, it has the characteristics of good optical uniformity, easy preparation, and achromatism. Especially, it can be used for the forming and processing of large-size and special-shaped infrared devices, and has become one of the key points in the research and application of infrared materials.

[0003] Currently, the preparation of chalcogenide glass mostly uses an encapsulated quartz bottle placed in a tube furnace and undergoes three stages: heating up, high-temperature rocking melting, and cooling down. Then, at 200 - 600 °C, the quartz bottle containing the melt is manually taken out for rapid cooling to obtain a chalcogenide glass blank. Since the quartz bottle needs to be manually taken out for rapid cooling, it is extremely easy to cause the vibration of the quartz bottle, resulting in defects such as streaks, seriously affecting the internal quality of the glass, and it is difficult to ensure the consistency of batches. At the same time, high-temperature operations pose safety hazards. Especially when preparing large-size chalcogenide glass, the weight of the entire quartz bottle increases, the operation difficulty is further increased, and the disadvantages of more internal stripe defects, unstable batches, and high safety risks are further highlighted. Summary of the Invention

[0004] In view of the problems existing in the background art, this application provides an optical glass preparation device and a preparation method, which can obtain chalcogenide glass products with good optical uniformity, stable transmittance performance, and large size, and reduce operation risks and improve safety.

[0005] According to one aspect of the present invention, an optical glass preparation device is provided, including: a heating furnace, which forms a furnace cavity inside; a material container; a rocking and rotating mechanism, installed in the furnace cavity, used to fix the material container and drive the material container to rock and rotate to mix the materials; a melt quenching mechanism, communicated with the furnace cavity, used to rapidly cool the melt formed by melting the materials in the material container.

[0006] By using the optical glass preparation device in this technical solution, encapsulate the materials in the material container, fix the material container on the rocking and rotating mechanism in the furnace cavity, then close the furnace cavity, and cooperate with the rocking and rotating mechanism and the melt quenching mechanism in the heating furnace to sequentially complete five processes: heating up, high-temperature rocking melting, cooling down, rapid melt cooling, and annealing, realizing smooth connection and conversion of each process. Finally, chalcogenide glass products with good optical uniformity, stable transmittance performance, and large size can be obtained, and the operation risk can be reduced and the safety can be improved.

[0007] In addition, the optical glass preparation device according to the present application may further have the following additional technical features:

[0008] In some embodiments of the present invention, the melt quenching mechanism includes a cold and hot box and a gas pipeline passing through the cold and hot box, wherein both ends of the gas pipeline respectively form an air inlet end and an air outlet end, the air outlet end is connected to the furnace cavity, and the air inlet end is connected to an external gas source.

[0009] In some embodiments of the present invention, the air outlet end of the gas pipeline extends into the furnace cavity, and the melt quenching mechanism further includes a distance adjustment structure, which is arranged on the side wall of the heating furnace and is used to adjust the distance between the air outlet end and the material container on the swing and rotation mechanism.

[0010] In some embodiments of the present invention, the gas pipeline includes a gas pipe and a heat exchange pipe connected to the gas pipe, and the heat exchange pipe is located inside the cold and hot box;

[0011] Preferably, the heat exchange pipe is a spiral pipe;

[0012] Preferably, a gas valve is connected to the gas pipe;

[0013] Preferably, a flow rate control valve is connected to the gas pipe between the external gas source and the gas valve;

[0014] Preferably, the outer wall of the gas pipe is wrapped with a heat insulation layer;

[0015] Preferably, a gas nozzle is connected to the air outlet end.

[0016] In some embodiments of the present invention, the cold and hot box includes an inner cavity formed inside the cold and hot box, a cold and hot box heater is arranged on the side wall of the cold and hot box, and the inner cavity is connected to a refrigeration unit;

[0017] Preferably, a temperature sensor is arranged in the inner cavity;

[0018] Preferably, a heat insulation layer is arranged on the side wall of the cold and hot box outside the cold and hot box heater.

[0019] In some embodiments of the present invention, the swing and rotation mechanism includes:

[0020] A container fixing frame, located inside the furnace cavity and used to fix the material container;

[0021] A rotating main shaft, one end of which is connected to the container fixing frame, the other end of which passes out of the heating furnace, and the rotating main shaft is rotationally connected to the heating furnace;

[0022] A driver, connected to the rotating main shaft, is used to drive the rotating main shaft to rotate.

[0023] In some embodiments of the present invention, the container fixing frame includes support side plates, a plurality of limiting rings and two end plates. Among them, the two end plates are arranged oppositely and are respectively connected to both ends of the support side plates. The two end plates are respectively used to limit both ends of the material container, and the plurality of limiting rings are arranged at intervals along the length direction of the support side plates and are used to limit the bottle body of the material container.

[0024] Preferably, heat-resistant buffer pads are provided on the sides of the two end plates and the support side plate facing the material container, and heat-resistant buffer ring pads are provided on the sides of the limiting rings facing the material container.

[0025] Preferably, the swing rotation mechanism further includes a positioner. The positioner is used to monitor the vertical state of the material container and is signal-connected to the driver. When the mouth of the material container is upward and in a vertical state, it feeds back to the driver and controls the driver to shut down.

[0026] According to another aspect of the present invention, an optical glass preparation method uses the above-mentioned optical glass preparation device to prepare optical glass. The optical glass preparation method includes the following steps: encapsulating materials in a material container; the materials in the material container are melted by high-temperature swing in a heating furnace to form a melt; the melt is left standing in the furnace cavity and then cooled; the cooled melt is quickly cooled by a melt quenching mechanism in the furnace cavity to form a blank; the blank is annealed in the furnace cavity.

[0027] In addition, according to the optical glass preparation method of the present application, the following additional technical features may also be included:

[0028] In some embodiments of the present invention, the temperature range of the quenching speed of the melt is 5°C / min to 200°C / min.

[0029] Preferably, the melt quenching mechanism uses a gas medium to quickly cool the melt in the material container.

[0030] Preferably, the flow rate of the gas medium is 5 to 200 L / min, the temperature is -70 to 200°C, and the cooling time of the melt is 1 to 20 min.

[0031] In some embodiments of the present invention, the melt quenching process is completed by setting the temperature and flow rate of the gas medium and the cooling time of the melt in one step or multiple steps.

[0032] Compared with the prior art, the present invention has achieved the following technical effects:

[0033] 1. Integrate the five processes of heating up, high-temperature rocking melting, cooling down, rapid cooling of the melt, and annealing in a set of equipment, avoiding manual operations during the processes, preventing defects such as stripes caused by vibration and shaking, ensuring the consistency of the process, and reducing high-temperature operations to improve safety.

[0034] 2. The device adopts a form in which the heating furnace and the rocking and rotating mechanism are independent of each other, avoiding the obstruction of the heating wire to rotation, and enabling stable 360-degree rotation.

[0035] 3. The container fixing frame stably fixes the material container, preventing the breakage of the material container during the heating-up and rotating process. At the same time, in the vertical state, the glass melt part is fully exposed, enabling the melt to be cooled evenly and sufficiently.

[0036] 4. The control of the temperature of the gas medium is increased. Further, by controlling the three process parameters of the temperature T, flow rate v, and time t of the gas medium, the range of the quenching rate Vc is expanded, enabling the system to have the ability to prepare large-size chalcogenide glass.

[0037] 5. Make full use of the characteristic that the gas medium has a relatively high temperature after quenching is completed. Continue to slowly introduce the gas into the front of the furnace to accelerate convection, making the temperatures at all positions in the furnace cavity reach consistency, accelerating the stabilization of the furnace cavity temperature field, avoiding the cracking problem of the glass blank caused by uneven temperature, and realizing the stable connection between the quenching and annealing processes. Description of the Drawings

[0038] By reading the detailed description of the preferred embodiments below, various other advantages and benefits will become clear to those of ordinary skill in the art. The drawings are only for the purpose of showing the preferred embodiments and are not considered to be a limitation of the present application. Moreover, throughout the drawings, the same reference numerals are used to represent the same components. In the drawings:

[0039] Figure 1 is the overall structural schematic diagram of the optical glass preparation device according to the embodiment of the present application;

[0040] Figure 2 is the side schematic diagram of the optical glass preparation device;

[0041] Figure 3 is the structural schematic diagram of the container fixing frame;

[0042] Figure 4 is the structural schematic diagram of the cold and hot box and part of the gas pipeline;

[0043] Figure 5 is the schematic diagram of the melt quenching process;

[0044] Figure 6 is the Ф100mm Ge prepared in Example 1 28 Sb 12 Se60 Transmittance spectrum

[0045] Figure 7 It is a Ф100mm Ge prepared by a conventional method 28 Sb 12 Se 60 Internal quality map

[0046] Figure 8 It is a Ф100mm Ge prepared in Example 1 28 Sb 12 Se 60 Internal quality map

[0047] Figure 9 It is a Ф150mm Ge prepared in Example 2 10 As 40 Se 50 Physical diagram

[0048] Figure 10 It is a Ф150mm Ge prepared in Example 2 10 As 40 Se 50 Transmittance spectrum

[0049] Figure 11 It is a Ф150mm Ge prepared in Example 2 10 As 40 Se 50 Internal quality map

[0050] The reference numerals in the drawings are defined as follows: 1. Heating furnace; 110. Heating furnace main body; 111. Air outlet; 112. Furnace main body heat-insulating shell layer; 113. Furnace cavity heater; 115. Furnace cavity; 120. Side cover of heating furnace; 121. Main control temperature sensor; 122. Temperature monitoring sensor; 123. Observation window; 124. Side cover heat-insulating shell layer; 2. Rocking and rotating mechanism; 201. Vertical positioning point; 202. Inductor; 203. Rotating main shaft; 204. Main shaft support frame; 205. Motor; 206. Motor fixed base; 207. Gear; 208. Driven gear; 209. Triangular suspension rod; 210. Container fixing frame; 211. Upper limit plate; 212. Support side plate; 213. Heat-resistant buffer pad; 214. Inlaid ring; 215. Lower limit plate; 216. Limit ring; 217. Heat-resistant buffer ring pad; 218. Material container; 3. Base; 301. Fixed support; 302. Movable support plate; 303. Guide rail; 304. Guide wheel; 305. Hydraulic cylinder; 306. Traction ring; 307. Track support; 4. Melt quenching mechanism; 410. Distance adjustment structure; 411. Cylinder; 412. Cylinder fixing frame; 413. Air pipe connecting frame; 421. Gas nozzle; 422. Moving pipe; 423. Metal hose; 424. Gas valve; 425. Air pipe; 426. Heat-insulating layer; 427. Spiral pipe; 428. Flow rate control valve; 429. Main air pipe; 430. Cold and hot box; 431. Temperature sensor; 432. Cold and hot box heater; 433. Stainless steel inner cavity; 434. Heat-insulating partition layer; 435. Refrigeration unit; 436. Cold air circulation pipe; 437. Circulation pipe heat insulation. Detailed implementation manners

[0051] It should be clear that the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments in the present application without creative efforts belong to the scope of protection of the present application.

[0052] When the following description refers to the drawings, unless otherwise indicated, the same numbers in different drawings represent the same or similar elements. The implementation manners described in the following exemplary embodiments do not represent all the implementation manners consistent with the present application. On the contrary, they are only examples of devices and methods consistent with some aspects of the present application as detailed in the appended claims.

[0053] In the description of the present application, it should be understood that terms such as "first" and "second" are only used for descriptive purposes and cannot be construed as indicating or implying relative importance. For those of ordinary skill in the art, the specific meanings of the above terms in the present application can be understood according to specific circumstances. In addition, in the description of the present application, unless otherwise specified, "a plurality of" means two or more. "And / or" describes the association relationship of associated objects and indicates that three relationships can exist. For example, A and / or B can represent three situations: A exists alone, A and B exist simultaneously, and B exists alone. The character " / " generally represents an "or" relationship between the associated objects before and after.

[0054] The optical glass preparation device and preparation method provided by the embodiments of the present application will be described below with reference to the accompanying drawings.

[0055] The embodiments of the present application disclose an optical glass preparation device. As Figure 1 and Figure 2 shown, the optical glass preparation device includes a heating furnace 1, a swing rotation mechanism 2, a material container 218, a base 3, and a melt quenching mechanism 4. Among them, a furnace cavity 115 is formed in the heating furnace 1, the swing rotation mechanism 2 is installed in the furnace cavity 115, the swing rotation mechanism 2 is used to fix the material container 218 and drive the material container 218 to swing and rotate to mix the materials, the melt quenching mechanism 4 is communicated with the furnace cavity 115, and the melt quenching mechanism 4 is used to quickly cool the melt formed by melting the materials in the material container 218. The material container 218 is a quartz bottle.

[0056] By using the optical glass preparation device in the present technical solution, materials are encapsulated in the material container 218, the material container 218 is fixed on the swing rotation mechanism 2 in the furnace cavity 115, then the furnace cavity 115 is closed, the heating furnace 1 and the swing rotation mechanism 2 are started, so that the materials in the material container 218 are melted by high-temperature swing in the heating furnace 1 to form a melt. After that, the melt continues to stand in the furnace cavity 115 and then cools down. Then, the melt quenching mechanism 4 quickly cools the cooled melt in the furnace cavity 115 to form a blank, and finally the annealing treatment of the blank is completed in the furnace cavity 115. The five processes of heating up, high-temperature swing melting, cooling down, melt rapid cooling, and annealing are integrated in a set of equipment, and smooth connection and conversion of each process are realized. Through this device, chalcogenide glass products with good optical uniformity, stable transmission performance, and large size can be obtained, and the operation risk can be reduced and the safety can be improved.

[0057] In some embodiments of the present invention, as Figure 1 and Figure 2As shown in the figure, the heating furnace 1 includes a heating furnace main body 110 and a heating furnace side cover 120; among them, the heating furnace main body 110 includes a furnace main body heat preservation shell layer 112, a furnace cavity 115 is formed inside the furnace main body heat preservation shell layer 112, a furnace cavity heater 113 is fixed on the inner wall of the furnace main body heat preservation shell layer 112, and an air outlet 111 is connected to each of the four corners near the top of the heating furnace main body 110.

[0058] The heating furnace side cover 120 includes a side cover heat preservation shell layer 124, a main control temperature sensor 121, four temperature monitoring sensors 122 and an observation window 123 are arranged on the side cover heat preservation shell layer 124. Among them, the main control temperature sensor 121 extends to the center of the furnace cavity 115, and the four temperature monitoring sensors 122 are respectively used to monitor the temperature of each part in the furnace cavity 115, and the observation window 123 is used to observe the situation inside the furnace cavity 115 during the preparation process of optical glass.

[0059] In some embodiments of the present invention, as Figure 1 and Figure 2 shown, the base 3 includes a fixed bracket 301, a movable support plate 302 and a track bracket 307. Among them, the heating furnace main body 110 is fixed on the fixed bracket 301, the heating furnace side cover 120 is fixed on the movable support plate 302, and the upper surfaces of the fixed bracket 301 and the movable support plate 302 are flush to ensure that the opening of the heating furnace side cover 120 is aligned with the heating furnace main body 110.

[0060] Four rows of guide wheels 304 are fixed at the bottom of the movable support plate 302. The four rows of guide wheels 304 are evenly distributed along the width direction of the heating furnace side cover 120, and each row of guide wheels 304 is arranged at intervals along the direction perpendicular to the heating furnace side cover 120. A guide rail 303 is fixed on the track bracket 307 corresponding to each row of guide wheels 304. Between the movable support plate 302 and the track bracket 307, a hydraulic cylinder 305 is arranged in the direction parallel to the guide rail 303. One end of the hydraulic cylinder 305 is connected to the lower surface of the movable support plate 302, and the other end is connected to the upper surface of the track bracket 307 through a traction ring 306. By applying positive and negative pressure to the hydraulic cylinder 305, the movable support plate 302 is driven to move on the track bracket 307, realizing the opening and closing of the heating furnace side cover 120 and the heating furnace main body 110.

[0061] In some embodiments of the present invention, as Figure 1 and Figure 2As shown in the figure, the swing rotation mechanism 2 includes a container fixing frame 210, a rotating main shaft 203, a driver, and a positioner. Among them, the container fixing frame 210 is located inside the furnace cavity 115 and is used to fix the material container 218; one end of the rotating main shaft 203 is connected to the container fixing frame 210, and the other end passes out to the outside of the heating furnace 1, and the rotating main shaft 203 is rotatably connected to the heating furnace 1; the driver is connected to the rotating main shaft 203 and is used to drive the rotating main shaft 203 to rotate; the positioner is used to monitor the vertical state of the material container 218 and is signal-connected to the driver. When the mouth of the material container 218 is upward and in a vertical state, the positioner can feedback to the driver and control the driver to turn off.

[0062] In some embodiments of the present invention, as Figure 3 shown, the container fixing frame 210 includes support side plates 212, several limiting rings 216, and two end plates. Among them, the two end plates are respectively an upper limit plate 211 and a lower limit plate 212. The upper limit plate 211 and the lower limit plate 212 are arranged oppositely and are respectively connected to both ends of the support side plates 212. The upper limit plate 211 and the lower limit plate 212 are respectively used to limit both ends of the material container 218. There are two limiting rings 216, and the two limiting rings 216 are arranged at intervals along the length direction of the support side plates 212 and are used to limit the body of the material container 218.

[0063] On the opposite side of the upper limit plate 211 and the lower limit plate 212 and on the side of the support side plates 212 facing the material container 218, heat-resistant buffer pads 213 are installed. On the side of the limiting rings 216 facing the material container 218, heat-resistant buffer ring pads 217 are installed; the heat-resistant buffer pads 213 are used for contact buffering between the upper limit plate 211, the support side plates 212, the lower limit plate 215 and the material container 218, and the heat-resistant buffer ring pads 217 are used for contact buffering between the limiting rings 216 and the material container 218 to avoid breakage caused by hard contact during the preparation process.

[0064] In some embodiments of the present invention, as Figure 1 and Figure 2 shown, the driver includes a main shaft support frame 204, a motor 205, a motor fixing base 206, a gear 207, and a driven gear 208. Among them, the motor fixing base 206 is fixed on the outer side wall of the heating furnace main body 110 and is located below the rotating main shaft 203. The main shaft support frame 204 and the motor 205 are fixed on the motor fixing base 206. The main shaft support frame 204 is used for rotatably supporting the end of the rotating main shaft 203. The driven gear 208 is coaxially connected to the rotating main shaft 203, and the gear 207 is coaxially connected to the output shaft of the motor 205 and meshes with the driven gear 208.

[0065] In some embodiments of the present invention, as Figure 2 and Figure 3As shown in the figure, a triangular suspension rod 209 is also fixed inside the furnace chamber 115 on the rotating main shaft 203. Multiple container fixing frames 210 can be fixed on the triangular suspension rod 209 through the inlay ring 214 at the same time. Specifically, in this embodiment, four container fixing frames 210 are fixed on the triangular suspension rod 209 at the same time, so as to realize the preparation of multiple groups of optical glass at one time.

[0066] In some embodiments of the present invention, such as Figure 1 shown in the figure, the positioner includes a vertical positioning point 201 and a sensor 202. The vertical positioning point 201 is on the driven gear 208, and the vertical positioning point 201 is arranged on the outer side wall of the heating furnace main body 110. When the swing rotation mechanism 2 works, the sensor 202 is closed, the motor 205 is turned on, driving the gear 207 to rotate, and making the driven gear 208 rotate together, and then making the rotating main shaft 203, the triangular suspension rod 209, and the container fixing frame 210 swing and rotate together. When the material container 218 needs to be erected vertically, the sensor 202 works, recognizes the vertical positioning point 201, controls the motor 205 to stop, and then makes the gear 207, the driven gear 208, the triangular suspension rod 209, and the rotating main shaft 203 stop, so that the container fixing frame 210 remains perpendicular to the ground.

[0067] In some embodiments of the present invention, such as Figure 1 、 2 and shown in Figure 4, the melt quenching mechanism 4 includes a cold and hot box 430, a distance adjusting structure 410, and a gas pipeline passing through the cold and hot box 430. The two ends of the gas pipeline respectively form an air inlet end and an air outlet end. The air outlet end is connected to the furnace chamber 115 and extends into the furnace chamber 115, and the air inlet end is connected to an external gas source. The distance adjusting structure 410 is arranged on the side wall of the heating furnace 1 and is used to adjust the distance between the air outlet end and the material container 218 on the swing rotation mechanism 2.

[0068] Specifically, the gas pipeline is integrally installed on the heating furnace side cover 120 and the movable support plate 302. The gas pipeline includes a gas spray head 421, a movable pipe 422, a metal hose 423, a gas valve 424, a gas pipe 425, a heat insulation layer 426, a heat exchange pipe, a flow control valve 428, and a main gas pipe 429. Among them, the gas spray head 421, the movable pipe 422, the metal hose 423, the gas valve 424, the gas pipe 425, the heat exchange pipe, and the flow rate control valve 428 are connected in sequence to form a branch pipeline. One group of branch pipelines is arranged corresponding to each container fixing frame 210, and then the four groups of branch pipelines are connected to the main gas pipe 429 in parallel, and the main gas pipe 429 supplies gas to each branch pipeline respectively.

[0069] Moreover, in order to further improve the temperature uniformity in each area of the furnace cavity 115 and ensure that the melt in the material container 218 is uniformly cooled from all directions, a set of cold and hot boxes 430, a distance adjustment structure 410 and a gas pipeline are additionally installed at a position on the heating furnace main body 110 opposite to the heating furnace side cover 120, so as to realize the cooling of the melt in the material container 218 from two opposite directions simultaneously.

[0070] The moving pipe 422 passes through the heating furnace side cover 120 and is slidably connected to the heating furnace side cover 120. The gas nozzle 421 is located in the furnace cavity 115 and faces the corresponding container fixing frame 210. The heat insulation layer 426 is coated on the outer layer of the gas pipe 425 for heat insulation. The heat exchange pipe is a spiral pipe 427. The spiral pipe 427 is placed in the cold and hot box 430. By controlling the temperature of the cold and hot box 430, the gas medium passing through the spiral pipe 427 can have a controllable temperature.

[0071] Specifically, the distance adjustment structure includes a cylinder 411, a cylinder fixing frame 412 and a gas pipe connecting frame 413. Among them, the cylinder fixing frame 412 is fixed on the outer side wall of the heating furnace side cover 120. The cylinder body of the cylinder 411 is fixed on the cylinder fixing frame 412. The piston rod of the cylinder 411 is fixedly connected to the four moving pipes 422 through the gas pipe connecting frame 413. The gas pipe connecting frame 413 enables the four moving pipes 422 to be fixedly connected and move synchronously; during the rotation of the container fixing frame 210, the cylinder 411 is used to retract the gas nozzle 421 ( Figure 2 the solid line indicated position of the gas nozzle 421), to avoid the gas nozzle 421 hitting the container fixing frame 210 and hindering the rotation of the material container 218 for mixing the materials. When it is necessary to quickly cool the melt in the material container 218, the cylinder 411 is used to move the gas nozzle 421 near the material container 218 ( Figure 2 the dotted line indicated position of the gas nozzle 421), to improve the precise control of the cooling efficiency of the melt in the material container 218.

[0072] Specifically, the cold and hot box 430 includes an inner cavity formed in the cold and hot box. The inner cavity is a stainless steel inner cavity 433. A cold and hot box heater 432 and a heat insulation layer 434 are installed on the side wall of the cold and hot box 430. The stainless steel inner cavity 433 is connected to a refrigeration unit 435 through a cold air circulation pipe 436. The cold air circulation pipe 436 is coated with a circulation pipe heat insulation 437. The cold and hot box 430 realizes the temperature control of the gas medium by controlling two modes of refrigeration and heating. A temperature sensor 431 is also installed in the stainless steel inner cavity 433.

[0073] In the refrigeration mode, the refrigeration unit 435 operates, and cold air circulates between the stainless-steel inner cavity 433 and the refrigeration unit 435 through the cold air circulation pipe 436. The control console controls the temperature of the stainless-steel inner cavity 433 through real-time feedback of the temperature sensor 431; in the heating mode, the control console controls the heating of the hot and cold box heater 432 through real-time feedback of the temperature sensor 431.

[0074] Specifically, the spiral tube 427 is placed in the stainless-steel inner cavity 433. After the gas medium passes through the spiral tube 427, heat exchange is carried out between the wall of the spiral tube 427 and the stainless-steel inner cavity 433, and the temperature is raised or lowered to the same temperature as the stainless-steel inner cavity 433. When the flow rates are the same, the quenching rates of gas media at different temperatures for glass melts of the same specification and the same composition are different. The higher the temperature of the gas medium, the slower the quenching rate, and the lower the temperature of the gas medium, the faster the quenching rate.

[0075] This embodiment also proposes an optical glass preparation method. This optical glass preparation method uses the above-mentioned optical glass preparation device to prepare optical glass. This optical glass preparation method includes:

[0076] Encapsulate the materials in the material container

[0077] In an oxygen-free environment, weigh and mix multiple elements of germanium, arsenic, selenium, antimony, and tellurium with a purity of 99.999% in a certain proportion and put them into the material container 218, and then evacuate and encapsulate. The vacuum degree in the material container 218 is less than 1×10 -4 Pa to form a material-containing material container 218.

[0078] Then slide the side cover 120 of the heating furnace on the guide rail 303 through the guide wheel 304, the hydraulic cylinder 305, and the traction ring 306 to separate it from the heating furnace main body 110, open the furnace cavity 115, and fix the material-containing material container 218 on the container fixing frame 210 through the upper limit plate 211, the support side plate 212, the heat-resistant buffer pad 213, the inlay ring 214, the lower limit plate 215, the limit ring 216, and the heat-resistant buffer ring pad 217. The container fixing frame 210 is suspended on the triangular suspension rod 209 through the inlay ring 214, and multiple container fixing frames 210 are suspended on the triangular suspension rod 209; then slide the side cover 120 of the heating furnace on the guide rail 303 through the guide wheel 304, the hydraulic cylinder 305, and the traction ring 306 to close the furnace cavity 115.

[0079] The materials in the material container are melted into a melt by high-temperature rocking in the heating furnace

[0080] Start the melting process. The furnace chamber 115 is heated to 930 - 970 °C by the furnace chamber heater 113 and maintained for 4 - 10 hours. At the same time, the material-containing container 218 rotates 360 degrees at a rotation frequency of 3 - 8 revolutions per minute to promote uniform mixing. Specifically, the inductor 202 is turned off, the motor 205 is turned on, driving the gear 207 to rotate and causing the driven gear 208 to rotate together. As a result, the rotating main shaft 203, the triangular suspension rod 209, and the container fixing frame 210 rotate and swing together, and the material is melted to form a melt.

[0081] The melt is left standing in the furnace chamber and then cooled down.

[0082] After the high-temperature melting is completed, the inductor 202 operates, recognizes the vertical positioning point 201, controls the motor 205 to stop, and thus the gear 207, the driven gear 208, the triangular suspension rod 209, and the rotating main shaft 203 stop, keeping the container fixing frame 210 perpendicular to the ground and leaving it standing for 25 - 35 minutes.

[0083] After that, start the cooling process, control the temperature of the furnace chamber 115 to drop to the range of 300 - 500 °C at a cooling rate of 1 - 5 °C / min, and leave it standing for 8 - 12 minutes.

[0084] During the cooling process, the cold and hot box 430 is turned on to control the stainless-steel inner cavity 433 to a certain temperature, which is defined as the gas medium temperature T, and the range of the gas medium temperature T is -70 - 200 °C.

[0085] The cooled melt is rapidly cooled in the furnace chamber by the melt quenching mechanism to form a preform.

[0086] The rapid cooling of the glass melt is achieved through the melt quenching mechanism 4. Specifically, the cylinder 411 pushes the four gas nozzles 421 and the moving pipe 422 to the vicinity of the material container 218 through the push air pipe connecting frame 413, with a spacing of 5 - 10 cm. The gas valve 424 and the flow rate control valve 428 are opened to control the gas medium to spray out from the gas nozzles 421 through the air pipe 425 at a certain flow rate for a certain time to cool the material container 218, and a non-crystalline glass preform is obtained through rapid cooling. The gas medium entering the furnace chamber 115 is discharged from the air outlet 111. The range of the gas medium flow rate is defined as the flow rate v, and the range of the flow rate v is 5 - 200 L / min. The cooling time t of the material container 218 ranges from 1 - 20 minutes. The melt quenching process can be completed by setting the temperature T, the flow rate v, and the time t in one step or multiple steps.

[0087] During the quenching of chalcogenide glass melt, as the quenching progresses, the melt viscosity increases. To avoid cracking and obtain a complete vitreous body, especially when preparing large-sized chalcogenide glass by quenching, the required quenching rate needs to be specifically reduced, and a large quenching rate control range is required. Controlling the gas medium temperature T can control the convective heat flow per unit volume, expanding its range to control the convective heat flow per unit volume, and then controlling the quenching rate; controlling the flow rate v can control the volume of convective gas per unit time; controlling the time t can control the total heat flow. Therefore, by setting three process parameters of temperature T, flow rate v, and time t, a large quenching rate control range can be obtained to meet the process requirements of gradually decreasing quenching rate. The range of gas medium temperature T is -70~200°C, the range of flow rate v is 5~200 L / min, the range of time t is 1~20 min, and the range of quenching rate Vc temperature is 5°C / min~200°C / min.

[0088] At the same time, by utilizing the gas medium at a relatively high temperature when the quenching is completed, the temperature of the furnace chamber 115 can be fully increased and made consistent, ensuring the temperature field and avoiding the problem of cracking of the glass blank caused by uneven temperature, thus realizing a stable connection between the quenching and annealing processes.

[0089] Specifically, as shown in Figure 5 the schematic diagram of the quenching process, for the melt quenching process of preparing chalcogenide glass, by setting temperature T, flow rate v, and time t, the quenching rate gradually decreases, and at the same time, the temperature of the gas medium entering the furnace chamber 115 increases. When the melt quenching process is completed, during t5~t6, the gas valve 424 and the flow rate control valve 428 are closed, and the cylinder 411 withdraws the four gas nozzles 421 and the moving pipe 422 away from the material container 218 together through the air pipe connecting frame 413 and returns to the initial position; then the gas valve 424 and the flow rate control valve 428 are opened again to control the gas medium to enter the furnace chamber 115 from the gas nozzles 421 through the air pipe 425. At this time, the temperature of the gas medium is the same as that at the end of the melt quenching, and the flow rate is further reduced. After continuously introducing gas for 5~15 min, the gas valve 424 and the flow rate control valve 428 are closed to stop inflating.

[0090] Anneal the blank in the furnace chamber

[0091] The melt in the material container 218 is rapidly cooled to obtain an amorphous glass blank. The furnace chamber 115 is heated to 150~450°C at a rate of 0.5~3°C / min by the furnace chamber 115 heater 113 and the main control temperature sensor 121, held for 15~40 h, and then cooled to 18~27°C, that is, room temperature, at a rate of 0.03~0.15°C / min to complete annealing.

[0092] After the annealing process is completed, the side cover 120 of the heating furnace slides on the guide rail 303 through the guide wheel 304, the hydraulic cylinder 305, and the traction ring 306, separates from the heating furnace main body 110, opens the furnace cavity 115, removes the container fixing frame 210 from the triangular suspension rod 209 one by one, cuts the material container 218, and takes out the glass blank, thus completing the processes of high-temperature rocking melting, cooling, melt quenching, and annealing.

[0093] The method for preparing optical glass using the above optical glass preparation device in the present application will be further described below in conjunction with specific embodiments.

[0094] Example 1:

[0095] Prepare Ф100mm Ge 28 Sb 12 Se 60 : Weigh the chalcogenide glass raw materials according to the precise ratio of germanium, antimony, and selenium elemental substances at 28 mol%, 12 mol%, and 60 mol% respectively, make a mixture and load it into the Ф100mm material container 218, evacuate to 1×10 -4 , and then use a hydrogen-oxygen flame to seal it.

[0096] Load the material container 218 into the furnace cavity 115 according to the steps, heat the heating furnace to 950 °C and keep it for 7 h. While maintaining the temperature, rotate the material container 218 with the container fixing frame 210 for mixing, and the rotation frequency is 5 revolutions / min to promote uniform mixing.

[0097] After the high-temperature melting is completed, keep the material container 218 in a vertical state and let it stand for 30 min; control the temperature of the furnace cavity 115 to drop to 500 °C at a cooling rate of 4 °C / min and let it stand for 10 min.

[0098] Open the cold and hot box 3 to control the temperature of the furnace cavity 115 to 30 ± 5 °C, turn on the melt quenching mechanism 4, and cool it with air at a flow rate of 40 L / min for 3 min to end the quenching process.

[0099] Raise the furnace temperature of the heating furnace 1 to 280 °C at a rate of 1 °C / min, keep it for 20 h, and then cool it to room temperature at a rate of 0.07 °C / min to complete the annealing process.

[0100] After the glass obtained by the above process is precisely annealed, it is processed into a 50×50×10 mm glass sample piece. After the surface is polished, the spectral performance is detected. As Figure 6 shown, Ge 28 Sb 12 Se 60 The test results of the glass sample piece show that the transmittance performance: the average transmittance of the 10 mm sample piece in the range of 2 - 12 μm is 64.59%. The internal quality is observed using a striation meter. Figure 8The Ф100mm Ge prepared in this embodiment 28 Sb 12 Se 60 Internal quality map, for comparison Figure 7 Internal quality map of a glass wafer prepared by a conventional method Figure 8 There are no defects such as stripes inside

[0101] Example 2:

[0102] Prepare Ф150mm Ge 10 As 40 Se 50 : Weigh the chalcogenide glass raw materials according to the precise ratio of 10mol%, 40mol% and 50mol% of germanium, arsenic and selenium respectively to make a mixture, and put it into the material container 218 with a diameter of Ф150mm. Vacuum it to 1×10 -4 and then seal it with a hydrogen-oxygen flame

[0103] Put the material container 218 into the furnace chamber 115 according to the steps. Heat the furnace to 970°C and keep it for 10h. While keeping the temperature, rotate the material container 218 with the container fixing frame 210 at a rotation frequency of 4 cycles / min to promote uniform mixing

[0104] After the high-temperature melting is completed, keep the material container 218 in a vertical state and let it stand for 30min; control the temperature of the furnace chamber 115 to drop to 500°C at a cooling rate of 4°C / min and let it stand for 10min

[0105] Open the cold and hot box 3 to control the temperature of the furnace chamber 115 to 80 - 100°C. Open the melt quenching mechanism 4 and cool it with air at a flow rate of 20L / min for 10min to end the quenching process

[0106] Raise the furnace temperature of the heating furnace 1 to 245°C at a rate of 1°C / min, keep it for 40h, and then cool it to room temperature at a rate of 0.05°C / min to complete the annealing process

[0107] The Ф150mm Ge obtained from the above process 10 As 40 Se 50 Chalcogenide glass in kind, such as Figure 9 shown. Process a 50×50×10mm glass wafer, polish its surface and then conduct spectral performance detection, such as Figure 10 shown, Ge 10 As 40 Se 50 The detection results of the glass wafer show that the transmittance performance: the average transmittance of the 10mm wafer in the range of 2 - 12μm is 65.14%; process a 50×50×10mm wafer, observe the internal quality with a striation meter, see Figure 11, there are no defects such as stripes inside.

[0108] As described above, it is only a preferred specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims

1. An optical glass preparation device, characterized in that, it includes: A heating furnace, in which a furnace cavity is formed; A material container; A swing and rotation mechanism, installed in the furnace cavity, for fixing the material container and driving the material container to swing and rotate to mix the materials; the swing and rotation mechanism includes a container fixing frame, a rotating main shaft and a driver. The container fixing frame is located in the furnace cavity for fixing the material container; one end of the rotating main shaft is connected to the container fixing frame, and the other end passes out of the heating furnace, and the rotating main shaft is rotationally connected to the heating furnace. The driver is connected to the rotating main shaft for driving the rotating main shaft to rotate; the container fixing frame includes supporting side plates, several limiting rings and two end plates. Among them, the two end plates are arranged oppositely and are respectively connected to both ends of the supporting side plates. The two end plates are respectively used to limit both ends of the material container, and several limiting rings are arranged at intervals along the length direction of the supporting side plates and are used to limit the bottle body of the material container; A melt quenching mechanism, communicated with the furnace cavity, for quickly cooling the melt formed by melting the materials in the material container; the melt quenching mechanism includes a cold and hot box, a gas pipeline passing through the cold and hot box and a distance adjusting structure. The two ends of the gas pipeline respectively form an air inlet end and an air outlet end. The air outlet end extends into the furnace cavity, and the air inlet end is connected to an external air source; the distance adjusting structure is installed on the side wall of the heating furnace for adjusting the distance between the air outlet end and the material container on the swing and rotation mechanism; the gas pipeline includes a gas pipe and a spiral pipe connected to the gas pipe. The spiral pipe is located in the cold and hot box; a gas valve is connected to the gas pipe, and a flow rate control valve is connected between the external air source and the gas valve on the gas pipe; the air outlet end is connected with a gas spray head; the cold and hot box includes an inner cavity formed in the cold and hot box. A cold and hot box heater is installed on the side wall of the cold and hot box, and the inner cavity is connected with a refrigeration unit.

2. The optical glass preparation device according to claim 1, characterized in that, The outer wall of the gas pipe is wrapped with a heat insulation layer.

3. The optical glass preparation device according to claim 1, characterized in that, A temperature sensor is installed in the inner cavity.

4. The optical glass preparation device according to claim 1, characterized in that, A heat insulation layer is installed on the side wall of the cold and hot box outside the cold and hot box heater.

5. The optical glass preparation device according to claim 1, characterized in that, Heat-resistant buffer pads are installed on the sides of the two end plates and the supporting side plates facing the material container, and heat-resistant buffer ring pads are installed on the sides of the limiting rings facing the material container.

6. The optical glass preparation device according to claim 1, characterized in that, The swing and rotation mechanism further includes a positioner, which is used to monitor the vertical state of the material container and is signal-connected to the driver. When the mouth of the material container is upward and in a vertical state, it feeds back to the driver and controls the driver to turn off.

7. A method for preparing optical glass, which uses the optical glass preparation device described in any one of claims 1-6 to prepare optical glass, Characterized in that, It includes the following steps: Encapsulate the materials in a material container; The materials in the material container are melted by high-temperature rocking in a heating furnace to form a melt; The melt is allowed to stand in the furnace cavity and then cooled; The cooled melt is rapidly cooled in the furnace cavity by a melt quenching mechanism to form a blank; Anneal the blank in the furnace cavity.

8. The method for preparing optical glass according to claim 7, Characterized in that, The temperature range of the quenching rate of the melt is 5°C / min to 200°C / min.

9. The method for preparing optical glass according to claim 8, Characterized in that, The melt quenching mechanism uses a gas medium to rapidly cool the melt in the material container.

10. The method for preparing optical glass according to claim 9, Characterized in that, The flow rate of the gas medium is 5-200 L / min, the temperature is -70-200°C, and the cooling time of the melt is 1-20 min.

11. The method for preparing optical glass according to claim 8, Characterized in that, The melt quenching process is completed by single-step or multi-step setting of the temperature and flow rate of the gas medium and the cooling time of the melt.

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