A system for producing a large-size quartz glass mother material

Abstract

The application belongs to the technical field of quartz glass preparation, and provides a system for preparing large-size quartz glass parent material. The system for preparing large-size quartz glass parent material comprises a vaporization device and a deposition device. The vaporization device comprises a heating pipe, a spraying assembly and a vaporization cavity. The heating pipe surrounds in the vaporization cavity. The spraying assembly comprises a first nozzle and a plurality of second nozzles. The first nozzle and the plurality of second nozzles are located in the vaporization cavity. The first nozzle extends in a first direction. The plurality of second nozzles are uniformly and interval arranged around the first direction on the side of the first nozzle. The deposition device comprises a deposition cavity, a burner assembly and an annealing assembly. The burner assembly and the annealing assembly are located in the deposition cavity. The burner assembly is communicated with the vaporization cavity. The deposition cavity also accommodates a base rod. The system for preparing large-size quartz glass parent material provided by the application has small size fluctuation of the prepared quartz glass parent material and high yield of the quartz glass parent material.

Description

Technical Field

[0001] This application relates to the field of quartz glass preparation technology, and in particular to a system for preparing large-size quartz glass master materials. Background Technology

[0002] Quartz glass is widely used in inertial navigation, optics and optical communication.

[0003] Quartz glass can be prepared using either Chemical Vapor Deposition (CVD) or Outside Vapor Deposition (OVD). CVD-produced quartz glass substrates often have excessively high hydroxyl content, making them unsuitable for high-power laser equipment. OVD, on the other hand, can produce quartz glass with low hydroxyl content. An OVD system is the equipment used to prepare quartz glass using this method. The OVD system includes an evaporator and a deposition chamber. Liquid organosilicon evaporates in the evaporator and then enters the deposition chamber, where it burns to form silica (SiO2) particles that deposit on the surface of a substrate rod, thus creating the quartz glass substrate. The substrate is then sintered to form quartz glass.

[0004] In related technologies, the dimensional fluctuations of quartz glass masterbatch prepared by external vapor deposition systems are large and the yield of quartz glass masterbatch is low. Summary of the Invention

[0005] This application provides a system for preparing large-size quartz glass master materials, which produces quartz glass master materials with small dimensional fluctuations and high yield.

[0006] This application provides a system for preparing large-size quartz glass masterbatch, including a vaporization device and a deposition device; the vaporization device includes a heating tube, a spray assembly and a vaporization chamber, the heating tube is surrounded in the vaporization chamber and has a circulating heating medium in the heating tube, the spray assembly includes a first nozzle and a plurality of second nozzles, the first nozzle and the plurality of second nozzles are all located in the vaporization chamber, the first nozzle extends in a first direction, and the plurality of second nozzles are evenly spaced around the first nozzle in the first direction;

[0007] The deposition apparatus includes a deposition chamber, a torch assembly, and an annealing assembly. The torch assembly and the annealing assembly are both located in the deposition chamber. The torch assembly is connected to the vaporization chamber. A base rod is also housed in the deposition chamber.

[0008] The first and second nozzles are used to spray liquid organosilicon; the heating tube is used to heat the liquid organosilicon to vaporize it in the vaporization chamber to form vaporized organosilicon; the torch assembly is used to burn the vaporized organosilicon to form silicon dioxide and deposit it on the surface of the base rod to form quartz glass matrix; the annealing assembly is used to anneal the quartz glass matrix.

[0009] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application has a second nozzle extending along a second direction, wherein the second direction is radially centered on the first direction.

[0010] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application includes a first nozzle and a plurality of second nozzles. The plurality of second nozzles are evenly spaced around the periphery of the first nozzle in a first direction. The spraying direction of the first nozzle is consistent with the first direction, and the spraying direction of the second nozzles is radial with the first direction as the center.

[0011] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application includes a second nozzle comprising a third nozzle and a plurality of fourth nozzles. The plurality of fourth nozzles are evenly spaced around the third nozzle in a second direction. The spraying direction of the third nozzle is consistent with the second direction, and the spraying direction of the fourth nozzles is radial with the second direction as the center.

[0012] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application further includes a cleaning pipe connected to a spray assembly.

[0013] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application further includes a heat preservation device, an air outlet on the vaporization chamber, an air inlet on the torch assembly, one end of the heat preservation device being connected to the air outlet, and the other end being connected to the air inlet.

[0014] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application has a chuck in the deposition chamber for holding both ends of a base rod; and two sets of annealing components are respectively arranged close to the two chucks to anneal the arc-shaped portions at both ends of the quartz glass masterbatch.

[0015] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application includes an annealing assembly comprising an annealing base and multiple sets of annealing lamps. The annealing base is coaxially arranged with the base rod, and the cross-section of the annealing base along the radial direction of the base rod is arc-shaped. The multiple sets of annealing lamps are evenly spaced on the inner sidewall of the annealing base.

[0016] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application includes multiple annealing lamps, including a first annealing lamp, a second annealing lamp, and a third annealing lamp, with the first annealing lamp and the third annealing lamp arranged on both sides of the second annealing lamp along an arc-shaped extension direction.

[0017] The deposition process is divided into a pre-deposition stage, a post-deposition stage, and an annealing stage. The second annealing lamp is turned on during the pre-deposition stage; the first, second, and third annealing lamps are all turned on during the post-deposition stage; and the first, second, and third annealing lamps are turned off sequentially at set intervals during the annealing stage.

[0018] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application includes a torch assembly comprising a torch base and a torch located on the torch base, the torch including a plurality of nozzles, an air inlet communicating with the torch, and the torch base being movable relative to the base rod along the axial direction of the base rod within the deposition chamber.

[0019] In one possible implementation, the system for preparing large-size quartz glass masterbatch provided in this application further includes an exhaust device comprising multiple exhaust pipes evenly spaced above the blowtorch.

[0020] In one possible implementation, the system for preparing large-size quartz glass master material provided in this application includes an exhaust device that further includes an anemometer, an exhaust valve, and a controller. The anemometer and the exhaust valve are both installed on the exhaust pipe, and both the anemometer and the exhaust valve are electrically connected to the controller. The controller is equipped with a preset wind speed threshold.

[0021] The anemometer is used to measure the wind speed in the exhaust duct, and the controller is used to compare the wind speed value with a preset wind speed threshold and adjust the opening of the exhaust valve according to the comparison result.

[0022] The system for preparing large-size quartz glass masterbatch provided in this application comprises a vaporization device and a deposition device. The vaporization device includes a heating tube, a spray assembly, and a vaporization chamber. The heating tube surrounds the vaporization chamber and contains a circulating heating medium. The spray assembly includes a first nozzle and multiple second nozzles, all located within the vaporization chamber. The deposition device includes a deposition chamber, a torch assembly, and an annealing assembly. The torch assembly and annealing assembly are located within the deposition chamber and are connected to the vaporization chamber. A base rod is also housed within the deposition chamber. By configuring the first nozzle and multiple second nozzles evenly spaced around it in a first direction, the liquid organosilicon sprayed from the spray assembly can be more evenly distributed within the vaporization chamber. Consequently, the vapor pressure distribution of the liquid organosilicon within the vaporization chamber is more uniform, resulting in a more uniform flow rate into the torch assembly. By surrounding the vaporization chamber with the heating tube and providing a circulating heating medium within it, the temperature distribution within the vaporization chamber is made uniform, further improving the flow rate uniformity of the vaporized organosilicon. As a result, the silica deposited on the surface of the substrate rod after combustion by the torch assembly is more uniform, resulting in smaller dimensional fluctuations in the quartz glass matrix. The annealing assembly performs real-time annealing of the quartz glass matrix during the deposition process, thereby reducing the probability of abnormalities such as cracking, eccentricity, or rod breakage at the ends of the quartz glass matrix, thus improving the yield of the quartz glass matrix. Attached Figure Description

[0023] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0024] Figure 1 This is a schematic diagram of the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application;

[0025] Figure 2 A diagram showing the usage state of the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application;

[0026] Figure 3 A schematic diagram of the vaporization device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application;

[0027] Figure 4 A flow rate comparison diagram of the vaporization device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application and the evaporator in the prior art;

[0028] Figure 5A temperature comparison diagram of the vaporization device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application and the evaporator of the prior art;

[0029] Figure 6 A schematic diagram of the spraying device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application;

[0030] Figure 7 for Figure 6 A bottom view;

[0031] Figure 8 A diagram showing the relative positions of the annealing components and the quartz glass matrix in a system for preparing large-size quartz glass matrix provided in an embodiment of this application.

[0032] Figure 9 For along Figure 8 Side view;

[0033] Figure 10 A schematic diagram of the annealing component in a system for preparing large-size quartz glass masterbatch provided in an embodiment of this application;

[0034] Figure 11 for Figure 10 Side view.

[0035] Explanation of reference numerals in the attached figures:

[0036] 10-base rod;

[0037] 20 - Quartz glass substrate; 21 - Curved section; 22 - Parallel section;

[0038] 100-Vaporization device;

[0039] 110 - Heating tube; 111 - Heating tube inlet; 112 - Heating tube outlet

[0040] 120 - Spray assembly; 120a - Liquid inlet; 120b - Liquid outlet;

[0041] 121 - First nozzle; 1211 - First nozzle; 1212 - Second nozzle;

[0042] 122 - Second nozzle; 1221 - Third nozzle; 1222 - Fourth nozzle;

[0043] 130 - Vaporization chamber; 131 - Gas outlet;

[0044] 140 - Cleaning pipe; 141 - Valve;

[0045] 200 - Deposition apparatus;

[0046] 210 - Deposition chamber; 211 - Chuck;

[0047] 220 - Blowtorch assembly; 221 - Air inlet; 222 - Blowtorch base; 223 - Blowtorch; 2231 - Nozzle;

[0048] 230 - Annealing assembly; 231 - Annealing base; 232 - Annealing lamp assembly; 232a - Annealing lamp; 2321 - First annealing lamp assembly; 2322 - Second annealing lamp assembly; 2323 - Third annealing lamp assembly; 233 - Support base;

[0049] 240 - Exhaust device; 241 - Exhaust duct; 242 - Anemometer; 243 - Exhaust valve; 2431 - Electric air valve; 2432 - Exhaust valve plate; 244 - Controller;

[0050] 300-Oil Bath Mold Temperature Controller;

[0051] 400 - Insulation device;

[0052] D1 - First direction;

[0053] D2 - Second direction;

[0054] X - Length direction;

[0055] Y-width direction;

[0056] Z-Height Direction. Detailed Implementation

[0057] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.

[0058] In the description of this application, it should be noted that, unless otherwise expressly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, an indirect connection through an intermediate medium, or the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this application according to the specific circumstances.

[0059] In the description of this application, it should be understood that the terms "upper", "lower", "front", "back", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this application and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application.

[0060] The terms "first," "second," and "third" (if any) in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a particular order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented, for example, in orders other than those illustrated or described herein.

[0061] Furthermore, the terms “comprising” and “having”, and any variations thereof, are intended to cover non-exclusive inclusion, such as a process, method, system, product, or maintenance tool that includes a series of steps or units, not necessarily limited to those steps or units that are explicitly listed, but may include other steps or units that are not explicitly listed or that are inherent to such process, method, product, or maintenance tool.

[0062] Quartz glass possesses excellent physical and chemical properties, making it suitable for applications in inertial navigation, optics, and optical communications. For example, quartz glass can be used as an imaging system for ultra-large-scale integrated circuit lithography, as well as as a large-aperture, high-performance fused silica lens and window material in laser technology.

[0063] Quartz glass can be prepared using chemical vapor deposition (CVD) or external vapor deposition (EVD). CVD-produced quartz glass has a high hydroxyl content in its matrix, making it unsuitable for high-power laser equipment. EVD, on the other hand, allows for the preparation of quartz glass with low hydroxyl content.

[0064] An external vapor deposition system is an apparatus for preparing quartz glass using the external vapor deposition method. The external vapor deposition system includes an evaporator and a deposition chamber. Liquid organosilicon evaporates in the evaporator and then enters the deposition chamber. Burning in a blowtorch within the deposition chamber forms silica particles that are deposited on the surface of a substrate rod, thus creating a quartz glass matrix. The quartz glass matrix is ​​then sintered to form quartz glass.

[0065] When preparing quartz glass substrates using external vapor deposition systems, silicon tetrachloride (SiCl4) can be used as a raw material. However, the silica produced by silicon tetrachloride has a large particle size and a wide particle size distribution range, resulting in poor deposition uniformity. Therefore, organosilicon can be used as a raw material. Organosilicon has a higher boiling point than silicon tetrachloride. Commonly used organosilicones include hexamethylcyclotrisilazane (D3), octamethylcyclotrisilazane (D4), decamethylcyclotetrasiloxane (D5), and dodecylcyclotetrasiloxane (D6). The molecular weight of D3, D4, D5, and D6 gradually increases, and the boiling point gradually increases with the increase of molecular weight. For example, the boiling point of D3 is 134℃, and that of D4 is 175℃. The higher the boiling point, the more energy is required for the vaporization process, and the higher the temperature, the more demanding the evaporator becomes. Therefore, D5 and D6, which have higher boiling points, are generally not used. D3 has a melting point of 64.5℃ and is a white crystal at room temperature. However, due to its high ring strain, D3 molecules are more prone to ring-opening and side reactions at process temperatures, making it inconvenient to use. Therefore, D4 ​​is usually used as the raw material for preparing quartz glass matrix.

[0066] During the vaporization process of D4, the temperature is relatively high. If the temperature distribution in the evaporator is uneven, the vaporized D4 will liquefy again in cooler areas, resulting in an unstable D4 flow rate. In higher areas, D4 will form a gel, which can clog parts of the pipeline, further reducing the stability of the D4 flow rate. This unstable D4 flow rate leads to uneven thickness of the silica deposited on the substrate surface, resulting in significant dimensional fluctuations in the quartz glass matrix. The gel can also flow into the deposition chamber with the vaporized D4, clogging the blowtorches within the deposition chamber.

[0067] In addition, excessive dimensional fluctuations can cause excessive stress at the ends of the quartz glass matrix, resulting in abnormalities such as cracking, eccentricity, or broken rods at the ends of the quartz glass matrix. As the diameter of the quartz glass matrix increases, the probability of such abnormalities increases, resulting in a lower yield of quartz glass matrix.

[0068] Based on this, this application provides a system for preparing large-size quartz glass master materials. The quartz glass master materials prepared by the system have small dimensional fluctuations and high yield.

[0069] Figure 1 This is a schematic diagram of the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application; Figure 2 A diagram showing the usage state of the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application; Figure 3 This is a schematic diagram of the vaporization device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application.

[0070] See Figures 1 to 3 As shown, the system for preparing large-size quartz glass masterbatch provided in this application includes a vaporization device 100 and a deposition device 200. The vaporization device 100 includes a heating pipe 110, a spray assembly 120, and a vaporization chamber 130. The heating pipe 110 surrounds the vaporization chamber 130 and has a circulating heating medium inside. The spray assembly 120 includes a first nozzle 121 and a plurality of second nozzles 122, both of which are located in the vaporization chamber 130. The first nozzle 121 extends in a first direction D1, and the plurality of second nozzles 122 are evenly spaced around the first nozzle 121 in the first direction D1. The deposition device... The apparatus 200 includes a deposition chamber 210, a blowtorch assembly 220, and an annealing assembly 230. Both the blowtorch assembly 220 and the annealing assembly 230 are located in the deposition chamber 210. The blowtorch assembly 220 is connected to the vaporization chamber 130. The deposition chamber also contains a base rod 10. A first nozzle 121 and a second nozzle 122 are used to spray liquid organosilicon. A heating tube 110 is used to heat the liquid organosilicon so that the liquid organosilicon vaporizes in the vaporization chamber 130 to form vaporized organosilicon. The blowtorch assembly 220 is used to burn the vaporized organosilicon to form silicon dioxide and deposit it on the surface of the base rod 10 to form a quartz glass substrate 20. The annealing assembly 230 is used to anneal the quartz glass substrate 20.

[0071] Specifically, the deposition chamber 210 can be a cuboid, and includes a length direction X, a width direction Y, and a height direction Z. The base rod 10 is disposed in the deposition chamber 210 along the length direction X. The torch assembly 220 is located in the deposition chamber 210, and the torch assembly 220 can be positioned below the base rod 10 along the height direction Z. The annealing assembly 230 can be disposed close to the base rod 10.

[0072] The vaporization device 100 can be positioned below the deposition chamber 210 along the height direction Z. The heating tube 110 surrounds the vaporization chamber 130. Figures 1 to 3 In the illustrated embodiment, the heating tube 110 may surround the inner wall of the vaporization chamber 130 to ensure uniform temperature within the vaporization chamber 130. Both the deposition chamber 210 and the vaporization chamber 130 are schematically shown with dashed lines to illustrate the components within them.

[0073] The heating element 110 contains a circulating heating medium, which can be thermally conductive silicone oil. For details, please refer to [link to relevant documentation]. Figure 3As shown, the heating tube 110 includes a heating tube inlet 111 and a heating tube outlet 112. The oil bath mold temperature controller 300 is connected to the inlet 111 and the outlet 112. After the oil bath mold temperature controller 300 heats the thermally conductive silicone oil, it enters the heating tube 110 through the heating tube inlet 111, heats the vaporization chamber 130, and then flows out through the heating tube outlet 112, entering the oil bath mold temperature controller 300 for further heating. This allows the temperature inside the vaporization chamber 130 to remain stable.

[0074] The spray assembly 120 has a liquid inlet 120a and a liquid outlet 120b, with a first nozzle 121 and a second nozzle 122 located on the side of the liquid outlet 120b. The liquid outlet 120b of the spray assembly 120 extends into the vaporization chamber 130, so that both the first nozzle 121 and the second nozzle 122 are located in the vaporization chamber 130. When the heating tube 110 is arranged around the nozzle, a portion of the heating tube 110 can be positioned close to the first nozzle 121 and the second nozzle 122.

[0075] The first nozzle 121 can be the main nozzle, and the first nozzle 121 extends along the first direction D1, wherein the first direction D1 is used to describe the spraying direction of the nozzle in the vaporization device 100, and the first direction D1 is not necessarily related to the length direction X, width direction Y, and height direction Z of the deposition chamber 210. Figure 1 and Figure 2 In the illustrated embodiment, the first direction D1 is the same as the height direction Z. In other embodiments, the first direction D1 may be the same as the length direction X or the width direction Y, or the first direction D1 may be different from the length direction X, the width direction Y, and the height direction Z. The second nozzles 122 are evenly spaced around the first nozzle 121 around the first nozzle 121. Thus, a circular spray assembly 120 is formed on the liquid outlet end 120b of the spray assembly 120, with the first nozzle 121 as the circle and the distance between the second nozzles 122 and the first nozzle 121 as the radius.

[0076] Liquid organosilicon enters from the inlet end 120a of the spray assembly 120 and is sprayed into the vaporization chamber 130 through the first nozzle 121 and the second nozzle 122 at the outlet end 120b. After being heated by the heating tube 110, it vaporizes in the vaporization chamber 130 to form gaseous organosilicon. The gaseous organosilicon enters the torch assembly 220 and burns in the torch assembly 220 to form silicon dioxide. The silicon dioxide is deposited on the surface of the base rod 10 to form the quartz glass substrate 20. The annealing assembly 230 performs real-time annealing on the quartz glass substrate 20 during the deposition process.

[0077] By setting a first nozzle 121 and multiple second nozzles 122 evenly spaced around the first nozzle 121 in the first direction D1, the liquid organosilicon sprayed from the spray assembly 120 can be more evenly distributed in the vaporization chamber 130. Therefore, the vapor pressure distribution of the liquid organosilicon in the vaporization chamber 130 is more uniform, resulting in a more uniform flow rate into the torch assembly 220. By surrounding the vaporization chamber 130 with a heating tube 110 and providing a circulating heating medium within the heating tube 110, the temperature distribution in the vaporization chamber 130 is made uniform. This avoids localized low temperatures in the vaporization chamber 130, which could cause the organosilicon to liquefy again and lead to unstable flow of gaseous organosilicon. It also avoids localized high temperatures that could cause organosilicon to gel and block the outlet of the vaporization chamber 130. The uniform temperature distribution in the vaporization chamber 130 further improves the flow uniformity of the vaporized organosilicon. As a result, the silica deposited on the surface of the base rod 10 after combustion by the torch assembly 220 is more uniform, resulting in smaller dimensional fluctuations in the quartz glass substrate 20. For example, the diameter fluctuation of the quartz glass substrate 20 is less than 2.4 mm; and the diameter fluctuation of the quartz glass substrate 20 after sintering is less than 3.1 mm.

[0078] Figure 4 A flow rate comparison diagram of the vaporization device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application and the evaporator in the prior art.

[0079] See Figure 4 As shown, in Figure 4 The graph below shows the vaporization device 100 provided in this embodiment of the application, where the flow rate of vaporized organosilicon is within the range of ±0.05 g / min. Figure 4 The graph above shows the evaporator in the related technology, where the flow rate of vaporized organosilicon is distributed within the range of ±0.5 g / min. After being vaporized by the vaporization device 100 provided in this application embodiment, the flow rate of gaseous organosilicon has a smaller fluctuation range and a more stable flow rate.

[0080] Figure 5 A temperature comparison diagram of the vaporization device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application and the evaporator of the prior art.

[0081] See Figure 5 As shown, in Figure 5 The graph below shows the vaporization device 100 provided in this embodiment of the application. The temperature distribution in the vaporization chamber 130 is within the range of 0.2℃. Figure 5 The graph above shows an evaporator in the related technology, where the temperature distribution is within the range of 2°C. In this embodiment, the temperature in the vaporization device 100 is more stable.

[0082] The system for preparing large-size quartz glass masterbatch provided in this application embodiment includes a vaporization device 100 and a deposition device 200. The vaporization device 100 includes a heating tube 110, a spray assembly 120, and a vaporization chamber 130. The heating tube 110 surrounds the vaporization chamber 130 and has a circulating heating medium inside. The spray assembly 120 includes a first nozzle 121 and a plurality of second nozzles 122, all of which are located in the vaporization chamber 130. The deposition device 200 includes a deposition chamber 210, a torch assembly 220, and an annealing assembly 230. The torch assembly 220 and the annealing assembly 230 are both located in the deposition chamber 210. The torch assembly 220 is connected to the vaporization chamber 130. A base rod 10 is also accommodated in the deposition chamber. By setting a first nozzle 121 and multiple second nozzles 122 evenly spaced around the first nozzle 121 in the first direction D1, the liquid organosilicon sprayed from the spray assembly 120 can be more evenly distributed in the vaporization chamber 130. Therefore, the vapor pressure distribution of the liquid organosilicon in the vaporization chamber 130 is more uniform, resulting in a more uniform flow rate into the torch assembly 220. By surrounding the vaporization chamber 130 with a heating tube 110 and providing a circulating heating medium within the heating tube 110, the temperature distribution in the vaporization chamber 130 is made uniform, further improving the flow rate uniformity of the vaporized organosilicon. Consequently, the silica deposited on the surface of the base rod 10 after combustion in the torch assembly 220 is also more uniform, resulting in smaller dimensional fluctuations in the quartz glass matrix. The annealing component 230 performs real-time annealing on the quartz glass substrate 20 during the deposition process. This reduces the probability of abnormalities such as cracking, eccentricity, or broken rods at the ends of the quartz glass substrate, thereby improving the yield of the quartz glass substrate 20.

[0083] Please continue reading Figure 3 As shown, the second nozzle 122 extends along the second direction D2, wherein the second direction D2 is radial with the first direction D1 as the center.

[0084] The second direction D2 has a first angle with the first direction D1. It should be noted that the second nozzle 122 is arranged around the first nozzle 121 along the first direction D1. Therefore, the second direction D2 is multiple directions, and each second direction D2 has a first angle with the first direction D1, so that the second direction D2 is radial with the first direction D1 as the center. Thus, the first nozzle 121 can spray liquid organosilicon along the first direction D1, and multiple second nozzles 122 can spray liquid organosilicon along the second direction D2, so that the liquid organosilicon is more evenly distributed in the vaporization chamber 130 and has more sufficient contact with the surrounding heating tube 110, thereby facilitating the heating of the liquid organosilicon.

[0085] Figure 6A schematic diagram of the spraying device in the system for preparing large-size quartz glass masterbatch provided in the embodiments of this application; Figure 7 for Figure 6 A bottom view.

[0086] See Figure 6 and Figure 7 As shown, the first nozzle 121 includes a first nozzle 1211 and a plurality of second nozzles 1212. The plurality of second nozzles 1212 are evenly spaced around the first nozzle 1211 in a first direction D1. The spraying direction of the first nozzle 1211 is consistent with the first direction D1, and the spraying direction of the second nozzles 1212 is radial with the first direction D1 as the center.

[0087] The diameter of the first nozzle 1211 can be larger than the diameter of the second nozzle 1212. The first nozzle 1211 sprays liquid organosilicon along the first direction D1, and the second nozzle 1212 sprays liquid organosilicon around the periphery of the first nozzle 1211, so that the spraying direction of the second nozzle 1212 is radial with the first direction D1 as the center. By setting the first nozzle 1211 and multiple second nozzles 1212 in the first nozzle 121, and making the spraying direction of the first nozzle 1211 consistent with the first direction D1, and the spraying direction of the second nozzles 1212 radial with the first direction D1 as the center, the uniformity of the liquid organosilicon in the vaporization chamber 130 can be further increased.

[0088] Please continue reading Figure 6 and Figure 7 As shown, the second nozzle 122 includes a third nozzle 1221 and a plurality of fourth nozzles 1222. The plurality of fourth nozzles 1222 are evenly spaced around the third nozzle 1221 around the second direction D2. The spraying direction of the third nozzle 1221 is consistent with the second direction D2, and the spraying direction of the fourth nozzles 1222 is radial with the second direction D2 as the center.

[0089] The diameter of the third nozzle 1221 can be larger than the diameter of the fourth nozzle 1222. The third nozzle 1221 sprays liquid organosilicon along the second direction D2, and the fourth nozzle 1222 sprays liquid organosilicon around the third nozzle 1221, so that the spraying direction of the fourth nozzle 1222 is radial with the second direction D2 as the center. By setting the third nozzle 1221 and multiple fourth nozzles 1222 in the second nozzle 122, and making the spraying direction of the third nozzle 1221 consistent with the second direction D2, and the spraying direction of the fourth nozzles 1222 radial with the second direction D2 as the center, the uniformity of the liquid organosilicon in the vaporization chamber 130 can be further increased.

[0090] Please continue reading Figures 1 to 3 As shown, the vaporization device 100 also includes a cleaning pipe 140, which is connected to the spray assembly 120.

[0091] The cleaning pipe 140 is connected to the spray assembly 120. A valve 141 is installed on the cleaning pipe 140. When the spray assembly 120 sprays liquid silicone, the valve 141 is closed. After the spray assembly 120 finishes spraying, the valve 141 is opened, and cleaning fluid is injected from the cleaning pipe 140 to clean the spray assembly 120 and prevent a small amount of gel from clogging the spray assembly 120.

[0092] The cleaning agent can be a silicone cleaner or a hydrocarbon solvent (such as xylene or dichloromethane). Cleaning can also be performed under heated conditions for better results. The cleaning time can be controlled from approximately 30 minutes to 1 hour. After cleaning, the vaporization device 100 can be purged with nitrogen gas at a flow rate of 50 L / min to further remove any residual gel.

[0093] Please continue reading Figure 1 and Figure 2 As shown, the system for preparing large-size quartz glass masterbatch also includes a heat preservation device 400, a vaporization chamber 130 having an air outlet 131, a blowtorch assembly 220 including an air inlet 221, one end of the heat preservation device 400 being connected to the air outlet 131, and the other end being connected to the air inlet 221.

[0094] The heat preservation device 400 can keep the gaseous organosilicon warm as it enters the torch assembly 220 from the vaporization chamber 130, thus preventing the gaseous organosilicon from liquefying due to a drop in temperature.

[0095] The specific structure of the annealing assembly 230 will be described below.

[0096] Figure 8 This is a diagram showing the relative positions of the annealing component and the quartz glass substrate in a system for preparing large-size quartz glass substrates provided in an embodiment of this application.

[0097] Please continue reading Figure 1 , Figure 2 and Figure 8 As shown, a chuck 211 is provided in the deposition chamber 210, which is used to hold the two ends of the base rod 10; there are two sets of annealing components 230, which are respectively set close to the two chucks 211 to anneal the arc-shaped portions 21 at both ends of the quartz glass base material 20.

[0098] In preparing the quartz glass matrix 20, tail shanks are first joined at both ends of the base rod 10. The two tail shanks are then clamped in chucks 211. Silica is then deposited on the base rod 10. During deposition, parallel portions 22 and arc-shaped portions 21 at both ends of the parallel portions 22 are formed on the base rod 10. Anomalies such as cracking, eccentricity, or breakage can occur at the position of the arc-shaped portions 21 near the parallel portions 22. Therefore, two sets of annealing assemblies 230 can be provided, positioned close to the two chucks 211, allowing annealing to be performed on the position of the arc-shaped portions 21 near the parallel portions 22.

[0099] Figure 9 For along Figure 8 Side view; Figure 10 A schematic diagram of the annealing component in a system for preparing large-size quartz glass masterbatch provided in an embodiment of this application; Figure 11 for Figure 10 Side view.

[0100] See Figures 8 to 11 As shown, the annealing assembly 230 includes an annealing base 231 and multiple sets of annealing lamps 232. The annealing base 231 is coaxially arranged with the base rod 10. The cross section of the annealing base 231 along the radial direction of the base rod 10 is arc-shaped. The multiple sets of annealing lamps 232 are evenly spaced on the inner sidewall of the annealing base 231.

[0101] The annealing assembly 230 can be mounted on the support 233. The annealing base 231 is coaxially arranged with the base rod 10, and the radial section of the annealing base 231 along the base rod 10 is arc-shaped, which allows the annealing assembly 230 to be closer to the quartz glass mother material 20, resulting in a better annealing effect.

[0102] Each annealing lamp group 232 includes multiple annealing lamps 232a, which can also be blowtorches. The annealing lamp 232a has an oxygen outlet pipe located in the inner layer and a hydrogen outlet pipe located in the outer layer.

[0103] Multiple sets of annealing lamps 232 are evenly spaced on the inner wall of the annealing base 231, which makes the heating of the base rod 10 by the annealing lamps 232 more uniform and further optimizes the annealing effect.

[0104] Please continue reading Figure 10 and Figure 11As shown, the multiple annealing lamp groups 232 include a first annealing lamp group 2321, a second annealing lamp group 2322, and a third annealing lamp group 2323. The first annealing lamp group 2321 and the third annealing lamp group 2323 are arranged on both sides of the second annealing lamp group 2322 along the arc-shaped extension direction. The deposition process is divided into a pre-deposition stage, a post-deposition stage, and an annealing stage. The second annealing lamp group 2322 is in the open state during the pre-deposition stage. The first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 are all in the open state during the post-deposition stage. The first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 are turned off sequentially at set intervals during the annealing stage.

[0105] The deposition chamber 210 has an airflow that flows along the height direction. The second annealing lamp group 2322 is located in the middle of the first annealing lamp group 2321 and the third annealing lamp group 2323 along the arc-shaped extension direction. Therefore, the second annealing lamp group 2322 is minimally affected by the airflow. In the pre-deposition stage (for example, when the weight of silicon dioxide deposition is less than 30 kg, a weight gauge is provided on the chuck 211 to measure the weight added to the base rod 10), the weight and thickness of silicon dioxide deposited on the base rod 10 are relatively small. At this time, only turning on the second annealing lamp group 2322 is sufficient to meet the annealing requirements.

[0106] In the post-deposition stage (e.g., when the weight of silica deposition is greater than 30 kg until the torch assembly 220 is turned off at the end of deposition), the first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 need to be turned on simultaneously to meet the annealing requirements.

[0107] During the annealing stage (e.g., from the end of deposition when the torch assembly 220 is turned off until the quartz glass substrate 20 has settled in the deposition chamber 210), suddenly turning off all annealing torches 232 will cause a sudden drop in temperature around the curved section 21. This sudden temperature change will generate significant stress in the quartz glass substrate 20, which can lead to cracking, misalignment, or breakage. Therefore, the first annealing torch assembly 2321, the second annealing torch assembly 2322, and the third annealing torch assembly 2323 need to be turned off sequentially at set intervals to meet the annealing requirements.

[0108] Table 1 shows a comparison of anomalies caused by opening different annealing lamps during the pre-deposition stage.

[0109]

[0110] Specifically, control program 1 indicates that only the first annealing lamp group 2321 is turned on; control program 2 indicates that only the second annealing lamp group 2322 is turned on; control program 3 indicates that only the third annealing lamp is turned on; control program 4 indicates that both the first annealing lamp group 2321 and the second annealing lamp group 2322 are turned on simultaneously; control program 5 indicates that both the first annealing lamp group 2321 and the third annealing lamp are turned on simultaneously; control program 6 indicates that both the second annealing lamp group 2322 and the third annealing lamp group 2323 are turned on simultaneously; and control program 7 indicates that the first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 are turned on simultaneously.

[0111] It can be seen that the cumulative anomaly rate of control procedure two in the pre-deposition stage is 0.19%, which is the lowest anomaly rate.

[0112] Table 2 shows a comparison of anomalies caused by opening different annealing lamps during the post-deposition stage.

[0113]

[0114] Specifically, control program 1 indicates that only the first annealing lamp group 2321 is turned on; control program 2 indicates that only the second annealing lamp group 2322 is turned on; control program 3 indicates that only the third annealing lamp is turned on; control program 4 indicates that both the first annealing lamp group 2321 and the second annealing lamp group 2322 are turned on simultaneously; control program 5 indicates that both the first annealing lamp group 2321 and the third annealing lamp are turned on simultaneously; control program 6 indicates that both the second annealing lamp group 2322 and the third annealing lamp group 2323 are turned on simultaneously; and control program 7 indicates that the first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 are turned on simultaneously.

[0115] It can be seen that the cumulative anomaly rate of control procedure seven in the post-deposition stage is 0.56%, which is the lowest anomaly rate.

[0116] Table 3 is a comparison table of anomalies caused by opening different annealing lamps during the annealing stage.

[0117]

[0118] Specifically, control program one indicates that the first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 should be turned off immediately upon the start of the settling period; control program two indicates that the first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 should be turned off after a five-minute settling period; control program three indicates that the first annealing lamp group 2321, the second annealing lamp group 2322, and the third annealing lamp group 2323 should be turned off after a ten-minute settling period; and control program four indicates that the first annealing lamp group 2321 and the second annealing lamp group 2322 should be turned off after a twenty-minute settling period. Lamp group 2322 and third annealing lamp group 2323; Control program five indicates that after a 10-minute rest period, two of the three annealing lamp groups 232 will be turned off, and after a 20-minute rest period, the remaining annealing lamp will be turned off; Control program six indicates that after a 10-minute rest period, one of the three annealing lamp groups 232 will be turned off, and after a 20-minute rest period, the remaining two annealing lamps will be turned off; Control program seven indicates that after a 10-minute rest period, one of the three annealing lamp groups 232 will be turned off, after a 15-minute rest period, another annealing lamp will be turned off, and after a 20-minute rest period, the remaining annealing lamp will be turned off.

[0119] It can be seen that the cumulative anomaly rate of control procedures six and seven during the annealing stage is 0.56%, which is the lowest.

[0120] By setting up three sets of annealing lamps 232 and controlling the opening and closing of the three sets of annealing lamps 232 in the manner described above, the yield of quartz glass mother material 20 can be effectively improved, especially the yield of large-diameter quartz glass mother material 20 (e.g., quartz glass mother material 20 with a diameter greater than 450mm). It should be noted that after sintering, the diameter of quartz glass mother material 20 with a diameter of 450mm is approximately 300mm.

[0121] Please continue reading Figure 1 and Figure 2 As shown, the blowtorch assembly 220 includes a blowtorch base 222 and a blowtorch 223 located on the blowtorch base. The blowtorch 223 includes a plurality of nozzles 2231. The air inlet 221 communicates with the blowtorch 223. The blowtorch base 222 can move relative to the base rod 10 along the axial direction of the base rod 10 within the deposition chamber 210.

[0122] The torch base 222 can move relative to the base rod 10 to move multiple torches 223 located on the torch base 222. In this embodiment, the torch base 222 can move at a variable speed; during the deposition process, the moving speed of the torch base 222 can gradually change from 260 mm / min to 150 mm / min. During the deposition process, the chuck 211 can also rotate relative to the torches 223 to drive the base rod 10 to rotate. The chuck 211 can also rotate at a variable speed, with its rotational speed gradually changing from 13.0 rpm to 7.5 rpm. The ratio of the moving speed of the torch base 222 to the rotational speed of the chuck 211 can be maintained at 20:1. Furthermore, as the diameter of the quartz glass substrate 20 increases, the torch base 222 can also move relative to the base rod 10 along the height direction Z.

[0123] Multiple blowtorches 223 are evenly spaced on the blowtorch base 222. For example, the number of blowtorches 223 can be set to 10 to 20, and the spacing between the blowtorches 223 can be 50mm-300mm. Gaseous organosilicon enters the blowtorch base 222 from the air inlet 221 and is distributed from the blowtorch base 222 to each blowtorch 223.

[0124] The blowtorch 223 typically adopts an annular nozzle structure, with gaseous organosilicon nozzle, inert gas nozzle and fuel gas nozzle respectively arranged from the inside to the outside. After these gases are ejected from the blowtorch, they mix and burn to generate silica particles, which are then deposited onto the base rod 10 through thermophoresis.

[0125] The following explanation will be based on the example of preparing a quartz glass substrate 20 with a diameter of approximately 450 mm.

[0126] The selected base rod 10 has a diameter of, for example, 50 mm and a length of 2000 mm. Including the tail shank, the total length can be 3000 mm. The target deposition weight of silica is 400 kg. After deposition, the diameter of the quartz glass substrate 20 is approximately 450.12 mm, and the density is approximately 1.226 g / cm³. 3 The parallel portion 22 of the quartz glass substrate 20 has a length of 2000 mm. The quartz glass substrate 20 has a uniform density distribution from the inner to the outer layer, which facilitates subsequent removal of hydroxyl groups; the hydroxyl content can be less than or equal to 10 ppm. The reaction formula for the combustion of gaseous organosilicon is as follows:

[0127] (CH3)8O4Si4+2H2+17O2→4SiO2+8CO2+14H2O

[0128] It should be noted that after the quartz glass parent material 20 is dehydroxylated and sintered, the diameter of the quartz glass produced is about 382 mm, the length of the parallel part 22 is 1600 mm, the weight of the parallel part 22 is 403 kg, and the measured hydroxyl content is about 7.8 to 8.1 ppm.

[0129] Please continue reading Figure 1 and Figure 2 As shown, the deposition device 200 also includes an exhaust device 240, which includes a plurality of exhaust pipes 241, which are evenly spaced above the blowtorch 223.

[0130] An air inlet channel is provided below the sedimentation chamber 210, and multiple exhaust pipes 241 are located above the sedimentation chamber 210. The air is diverted from the air inlet channel into the sedimentation chamber 210 and discharged from the multiple exhaust pipes 241.

[0131] Please continue reading Figure 1 and Figure 2 As shown, the exhaust device 240 also includes an anemometer 242, an exhaust valve 243, and a controller 244. The anemometer 242 and the exhaust valve 243 are both installed on the exhaust pipe 241, and both the anemometer 242 and the exhaust valve 243 are electrically connected to the controller 244. The controller 244 is set with a preset wind speed threshold. The anemometer 242 is used to measure the wind speed value in the exhaust pipe 241, and the controller 244 is used to compare the wind speed value with the preset wind speed threshold, and adjust the opening of the exhaust valve 243 according to the comparison result.

[0132] The controller 244 can be a programmable logic controller (Power Line Communication, or PLC). The exhaust valve 243 includes an electric exhaust valve 2431 and an exhaust valve plate 2432 connected to the electric exhaust valve 2431. The electric exhaust valve 2431 is electrically connected to the controller 244.

[0133] After the anemometer 242 measures the wind speed value in the exhaust duct 241, it transmits the wind speed value to the controller 244. The controller 244 has a preset wind speed threshold, which can be a range of values. The controller 244 compares the wind speed value with the preset wind speed threshold. When the wind speed value is less than the lower limit of the preset wind speed threshold, the controller 244 controls the opening of the exhaust valve 2432 through the electric damper 2431 to increase the wind speed value in the exhaust duct 241 to within the preset wind speed threshold range. When the wind speed value is greater than the upper limit of the preset wind speed threshold, the controller 244 controls the opening of the exhaust valve 2432 through the electric damper 2431 to decrease the opening of the exhaust valve 2432 to decrease the wind speed value in the exhaust duct 241 to within the preset wind speed threshold range.

[0134] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit them. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of this application.

Claims

1. A system for preparing large-size quartz glass masterbatch, characterized in that, It includes a vaporization device and a deposition device; the vaporization device includes a heating pipe, a spray assembly and a vaporization chamber, the heating pipe is surrounded in the vaporization chamber and has a circulating heating medium inside the heating pipe, the spray assembly includes a first nozzle and a plurality of second nozzles, the first nozzle and the plurality of second nozzles are all located in the vaporization chamber, the first nozzle extends in a first direction, and the plurality of second nozzles are evenly spaced around the first nozzle in the first direction; The deposition apparatus includes a deposition chamber, a blowtorch assembly, and an annealing assembly. The blowtorch assembly and the annealing assembly are both located in the deposition chamber. The blowtorch assembly is connected to the vaporization chamber. A base rod is also housed in the deposition chamber. The first nozzle and the second nozzle are used to spray liquid organosilicon; the heating tube is used to heat the liquid organosilicon to vaporize it in the vaporization chamber to form vaporized organosilicon; the blowtorch assembly is used to burn the vaporized organosilicon to form silicon dioxide and deposit it on the surface of the base rod to form a quartz glass matrix; the annealing assembly is used to anneal the quartz glass matrix. The annealing assembly includes an annealing base and multiple sets of annealing lamps. The annealing base is coaxially arranged with the base rod. The cross-section of the annealing base along the radial direction of the base rod is arc-shaped. The multiple sets of annealing lamps are evenly spaced on the inner sidewall of the annealing base.

2. The system for preparing large-size quartz glass masterbatch according to claim 1, characterized in that, The second nozzle extends along a second direction, wherein the second direction is radial about the first direction.

3. The system for preparing large-size quartz glass masterbatch according to claim 2, characterized in that, The first nozzle includes a first nozzle and a plurality of second nozzles. The plurality of second nozzles are evenly spaced around the first nozzle in the periphery of the first nozzle. The spraying direction of the first nozzle is consistent with the first direction, and the spraying direction of the second nozzles is radial with the first direction as the center.

4. The system for preparing large-size quartz glass masterbatch according to claim 3, characterized in that, The second nozzle includes a third nozzle and a plurality of fourth nozzles. The plurality of fourth nozzles are evenly spaced around the third nozzle around the second direction. The spraying direction of the third nozzle is consistent with the second direction, and the spraying direction of the fourth nozzles is radial with the second direction as the center.

5. The system for preparing large-size quartz glass masterbatch according to claim 4, characterized in that, The vaporization device also includes a cleaning pipe, which is connected to the spray assembly.

6. The system for preparing large-size quartz glass masterbatch according to claim 5, characterized in that, It also includes a heat preservation device, the vaporization chamber has an air outlet, the torch assembly includes an air inlet, one end of the heat preservation device is connected to the air outlet, and the other end is connected to the air inlet.

7. The system for preparing large-size quartz glass masterbatch according to any one of claims 1 to 6, characterized in that, The deposition chamber is provided with a chuck for holding the two ends of the base rod; there are two sets of annealing components, which are respectively located close to the two chucks to anneal the arc-shaped portions at both ends of the quartz glass matrix.

8. The system for preparing large-size quartz glass masterbatch according to claim 7, characterized in that, The multiple sets of annealing lamps include a first annealing lamp, a second annealing lamp, and a third annealing lamp, wherein the first annealing lamp and the third annealing lamp are arranged on both sides of the second annealing lamp along the arc-shaped extension direction; The deposition process is divided into a pre-deposition stage, a post-deposition stage, and an annealing stage. The second annealing lamp is turned on during the pre-deposition stage. The first, second, and third annealing lamps are all turned on during the post-deposition stage. During the annealing stage, the first, second, and third annealing lamps are turned off sequentially at set intervals.

9. The system for preparing large-size quartz glass masterbatch according to claim 6, characterized in that, The torch assembly includes a torch base and a torch located on the torch base. The torch includes multiple nozzles. The air inlet communicates with the torch. The torch base is movable relative to the base rod along the axial direction of the base rod within the deposition chamber.

10. The system for preparing large-size quartz glass masterbatch according to any one of claims 1 to 6, characterized in that, The deposition apparatus also includes an exhaust system, which comprises multiple exhaust pipes evenly spaced above the blowtorch.

11. The system for preparing large-size quartz glass masterbatch according to claim 10, characterized in that, The ventilation device also includes an anemometer, an exhaust valve, and a controller. The anemometer and the exhaust valve are both installed on the exhaust pipe, and both the anemometer and the exhaust valve are electrically connected to the controller. The controller is equipped with a preset wind speed threshold. The anemometer is used to measure the wind speed in the exhaust duct, and the controller is used to compare the wind speed with the preset wind speed threshold and adjust the opening of the exhaust valve according to the comparison result.

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