Quartz powder body preparation system and method

Abstract

The application provides a quartz powder body preparation system and a preparation method. The quartz powder body preparation system comprises a focused burner and a deposition assembly; the focused burner is used for spraying reaction raw materials, the focused burner comprises a raw material nozzle in the center, and a plurality of groups of combustion nozzles are arranged layer by layer from the inside to the outside around the raw material nozzle, and the focal lengths of the plurality of groups of combustion nozzles are different. The deposition assembly is used for depositing the reaction raw materials sprayed by the focused burner to form a quartz powder body, and the deposition assembly comprises a target rod with a deposition end, and the cross-sectional outer diameter of the middle part of the deposition end is larger than that of the two ends of the deposition end. After sintering, the large-size quartz glass has excellent performance of high uniformity and low stress, and the quartz powder body preparation method uses the quartz powder body preparation system to prepare a quartz powder body.

Description

TECHNICAL FIELD

[0001] The application relates to the field of material chemical industry, and particularly relates to a quartz powder body preparation system and a preparation method. BACKGROUND

[0002] High-purity synthetic quartz glass is widely used in high-end fields such as semiconductors, aerospace, high-energy lasers and precision optics due to its extremely low metal impurity content, high transmittance, low residual stress, excellent optical uniformity and strong corrosion resistance. High-purity synthetic quartz glass is mainly prepared by a chemical process in which a silicon source is hydrolyzed in a high-temperature flame. The mainstream synthesis process is divided into one-step and two-step methods according to the synthesis process. CVD is a one-step preparation process, which directly prepares quartz glass pellets by hydrolyzing silicon sources such as silicon tetrachloride and organosilane in a hydrogen-oxygen flame at high temperature. This method can prepare large-size high-purity quartz glass, but the hydroxyl content in the quartz prepared by this method is high (about 1000 ppm). Another one-step preparation process is PCVD, which uses a high-temperature plasma flame to drive the silicon source (usually SiCl4) to directly react with oxygen to form silicon dioxide. This method avoids the formation of hydroxyl in quartz glass and can limit the hydroxyl content to below 1 ppm, but chlorine impurities are easily introduced into the quartz glass during the preparation process.

[0003] The two-step method hydrolyzes silicon sources such as silicon tetrachloride and organosilane in a hydrogen-oxygen flame at high temperature to obtain a silicon dioxide powder body, and then sintering at high temperature to glassify the quartz powder body to prepare a high-purity synthetic quartz glass material. The two-step synthesis process mainly includes VAD and OVD. The OVD method deposits quartz particles on the periphery of a cylindrical target rod to form a ring-shaped powder body. Due to technical problems, it is difficult to prepare large-size quartz glass. Some patents propose to use the OVD method to prepare a large-diameter quartz glass ring, but the OVD method has a deposition core rod in the center, which cannot prepare large-size quartz pellets. The VAD method deposits the initial end at the bottom of the cylindrical target, and the powder body extends out of the target rod to form a column as the deposition proceeds. After the quartz powder body is prepared by the VAD method, the composition and structure of the powder body can be further optimized by purification and other technologies, so that high-purity quartz glass with higher performance can be obtained. For example, heating the powder body in a chlorine atmosphere at an intermediate temperature can effectively remove residual metal elements and hydroxyl groups in the structure. From the perspective of the process, theoretically, the VAD method is the best route for preparing large-size high-purity quartz glass with high uniformity, low stress, low hydroxyl and other high-performance characteristics.

[0004] However, the current VAD method is limited by the structure of the torch and the deposition parameters, and the quartz glass rod prepared by the method usually has a diameter of less than 200 mm. At the same time, since the deposition target rod of the current VAD method is usually in the form of a cylindrical rod, the area of the target rod available for deposition at the initial deposition stage is small, which results in low efficiency and low rate at the early stage of deposition. At the same time, the quartz obtained at the initial deposition position is affected by unstable deposition parameters and the risk of contamination caused by contact with the target rod, and the performance of the product is affected. Therefore, the initial deposition position and the non-parallel part in contact with the target rod are usually cut off during the preparation process. Ultimately, it is difficult to prepare large-size high-performance quartz glass by the VAD method, and the efficiency of the deposition process is low. At the same time, due to the numerous influencing factors in the deposition process, it is difficult to monitor the deposition parameters and process in real time, which leads to room for improvement in the uniformity and stress of the material. How to solve the above problems is a problem that needs to be considered by those skilled in the art. SUMMARY

[0005] To solve the above problems, the quartz powder body preparation system and preparation method provided by the embodiments of the present application can use silicon tetrachloride, organosilane and other silicon sources as raw materials to prepare large-size quartz powder bodies with high deposition powder uniformity, and use the above powder bodies to sinter high-performance large-size quartz glass with high uniformity and low stress.

[0006] The embodiments of the present application provide a quartz powder body preparation system, which comprises a focusing torch and a deposition assembly. The focusing torch is used to spray reaction raw materials, and the focusing torch comprises a raw material nozzle located at the center and a plurality of groups of combustion nozzles arranged layer by layer from the inside to the outside around the raw material nozzle, and the focal lengths of the plurality of groups of combustion nozzles are different. The deposition assembly is used to deposit the reaction raw materials sprayed by the focusing torch to form a quartz powder body, and the deposition assembly comprises a target rod having a deposition end portion, the cross-sectional outer diameter of the middle part of the deposition end portion is larger than the cross-sectional outer diameter of the two ends of the deposition end portion, the deposition end portion comprises an end body and a concave-convex structure arranged on the surface of the end body, the concave-convex structure comprises a plurality of convex portions and a plurality of concave portions, and the plurality of convex portions and the plurality of concave portions are arranged in sequence and alternately.

[0007] It can be understood that the quartz powder body preparation system of the present application uses a focusing torch with a plurality of groups of combustion nozzles, optimizes the structure and deposition flow of the focusing torch, and makes the focal lengths of the plurality of groups of combustion nozzles arranged layer by layer from the inside to the outside around the raw material nozzle different, so as to realize the preparation of large-size, high-performance and high-purity quartz glass, wherein the rod diameter of the obtained quartz powder body can be greater than or equal to 350 mm. At the same time, the quartz powder body preparation system of the present application also uses a target rod with smaller ends and a larger middle part, which compensates for the low efficiency stage at the initial deposition stage through the shape of the target rod, solves the problems of low rate and low efficiency at the initial stage of powder body deposition, and greatly shortens the time of the rod body forming stage.

[0008] In an embodiment, each group of the combustion nozzles comprises two sub-nozzles arranged in layers from inside to outside, one of the two sub-nozzles is used to spray combustible gas, and the other is used to spray combustion-supporting gas.

[0009] In an embodiment, the focal lengths of the groups of the combustion nozzles arranged in layers from inside to outside around the raw material nozzle gradually increase.

[0010] In an embodiment, the focusing torch comprises three groups of combustion nozzles, i.e., a first combustion nozzle, a second combustion nozzle, and a third combustion nozzle, the first combustion nozzle is arranged around the raw material nozzle, the second combustion nozzle is arranged around the first combustion nozzle, the third combustion nozzle is arranged around the second combustion nozzle, the focal length of the third combustion nozzle is greater than that of the second combustion nozzle, and the focal length of the second combustion nozzle is greater than that of the first combustion nozzle.

[0011] In an embodiment, the first combustion nozzle comprises a first sub-nozzle arranged around the raw material nozzle and a second sub-nozzle arranged around the first sub-nozzle; the second combustion nozzle comprises a third sub-nozzle arranged around the second sub-nozzle and a fourth sub-nozzle arranged around the third sub-nozzle; the third combustion nozzle comprises a fifth sub-nozzle arranged around the fourth sub-nozzle and a sixth sub-nozzle arranged around the fifth sub-nozzle; the first sub-nozzle, the third sub-nozzle, and the fifth sub-nozzle are used to spray combustion-supporting gas, and the second sub-nozzle, the fourth sub-nozzle, and the sixth sub-nozzle are used to spray combustible gas.

[0012] In an embodiment, the combustion-supporting gas comprises oxygen, and the combustible gas comprises hydrogen.

[0013] It can be understood that the shape of the target rod and the concave-convex design of the surface increase the weighing capacity of the target rod, and the weight of the prepared quartz powder body can be greater than or equal to 200 kg.

[0014] In an embodiment, the cross-sectional outer diameter of the middle part of the end body is greater than that of the two ends of the end body.

[0015] In an embodiment, the shape of the end body is one of an oval shape, a water drop shape, and a circular-triangle bipyramid shape.

[0016] In an embodiment, the deposition assembly further comprises a lifting platform and a tension sensor component, the target rod is connected to the lifting platform, the tension sensor component is arranged between the lifting platform and the target rod, and is used to sense the downward tension applied by the target rod to the lifting platform; the quartz powder body preparation system further comprises a laser rod diameter measuring instrument, and the laser rod diameter measuring instrument is used to measure the outer diameter of the quartz powder body deposited on the target rod.

[0017] In an embodiment, the quartz powder body is sintered at high temperature to obtain a quartz ingot, and the quartz glass rod obtained after sintering has a diameter greater than or equal to 250 mm, and has high optical uniformity and low stress.

[0018] The embodiment of the present application also provides a quartz powder body preparation method, which uses the quartz powder body preparation system according to any one of the preceding embodiments to prepare a quartz powder body.

[0019] It can be understood that the quartz powder body preparation method of the present application uses the quartz powder body preparation system in the preceding embodiments, and based on the quartz powder body preparation system, the quartz powder body preparation method of the present application can obtain a high-performance large-size quartz powder body with high deposition powder uniformity, wherein the diameter of the quartz powder body is greater than or equal to 350 mm, and the weight of the quartz powder body is greater than or equal to 200 kg; at the same time, the low efficiency in the initial stage of deposition is compensated by the shape of the target rod, the problem of low rate and low efficiency in the initial stage of powder body deposition is solved, the time of rod body forming stage is greatly shortened, and the production efficiency is improved. The diameter of the quartz glass rod obtained after sintering is greater than or equal to 250 mm, and has high optical uniformity and low stress. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 A structural schematic diagram of a deposition device of the quartz powder body preparation system provided by the embodiment of the present application is shown.

[0021] Figure 2 A planar structural schematic diagram of a focusing burner of the quartz powder body preparation system provided by the embodiment of the present application is shown.

[0022] Figure 3 A sectional focal length structural schematic diagram of the focusing burner of the quartz powder body preparation system provided by the embodiment of the present application is shown.

[0023] Figure 4 A schematic diagram of various embodiments of a target rod of the quartz powder body preparation system provided by the embodiment of the present application is shown.

[0024] Figure 5 A schematic diagram of a concave-convex structure of the target rod of the quartz powder body preparation system provided by the embodiment of the present application is shown.

[0025] Main element symbol explanation: 10, quartz powder body preparation system; 11, focused torch; 110, combustion nozzle; 1101, first combustion nozzle; 1102, second combustion nozzle; 1103, third combustion nozzle; 111, raw material nozzle; 112, first sub-nozzle; 113, second sub-nozzle; 114, third sub-nozzle; 115, fourth sub-nozzle; 116, fifth sub-nozzle; 117, sixth sub-nozzle; 12, deposition assembly; 121, target rod; 1211, deposition end; 1212, tail handle section; 1213, end body; 1214, concave-convex structure; 1215, convex part; 1216, concave part; 122, lifting platform; 123, tension sensor component; 124, deposition cavity; 13, laser rod diameter measuring instrument; 130, light sensing unit; 14, data processing assembly; 141, data recording and visualization screen; 142, tension sensing transmission line; 143, rod diameter sensing transmission line.

[0026] The following detailed description will further describe the present application in conjunction with the above-mentioned drawings. DETAILED DESCRIPTION

[0027] The following description will refer to the accompanying drawings to more fully describe the present application. The drawings show exemplary embodiments of the present application. However, the present application can be embodied in many different forms and should not be construed as limited to the exemplary embodiments set forth herein. These exemplary embodiments are provided so that this application will be thorough and complete, and will fully convey the scope of the application to those skilled in the art. Like reference numerals refer to like elements throughout.

[0028] The terminology used herein is for the purpose of describing particular example embodiments only and is not intended to be limiting of the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. Furthermore, to the extent that the terms "including", "includes", "having", "has", "a", "an", "one" or "said one" are used in this specification and / or claims, they are intended to be inclusive (meaning that there can be additional items) and / or they are intended to be quantitatively-satisfied by at least the recited item (meaning that any additional included items do not negate the use of "comprising", "including", "having", "a", "an", "one", or "said one").

[0029] Unless otherwise defined, all terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. It will be further understood that terms, such as those defined in commonly used dictionaries, should be interpreted as having a meaning that is consistent with their meaning in the context of the relevant art and the present disclosure and will not be interpreted in an idealized or overly formal sense unless expressly so defined herein.

[0030] Generally, the VAD rule is that the initial end is deposited at the bottom of the cylindrical target, and as the deposition progresses, the powder body extends out of the target rod to form a column. After preparing the quartz powder body by VAD method, the composition and structure of the powder body can be further optimized by purification and other technologies, so as to obtain high-performance high-purity quartz glass. There are relevant literature patents reporting that by heating the powder body at a medium temperature with chlorine, the residual metal elements and hydroxyl groups in the structure can be effectively removed. From the process point of view, theoretically, VAD method is the best route for preparing large-size high-purity quartz glass with high uniformity, low stress, low hydroxyl and other high-performance characteristics. However, at present, VAD method is limited by the structure of the torch and the deposition parameters, and the quartz glass rod prepared has a diameter usually below 200 mm. At the same time, due to the fact that the deposition target rod of the current VAD method is in a cylindrical rod structure, the area available for deposition at the initial deposition stage is small, which results in insufficient efficiency and low rate at the early stage of deposition. At the same time, the quartz obtained at the initial deposition position is affected by unstable deposition parameters and the risk of contamination caused by contact with the target rod, and the performance of the product is affected. Therefore, the non-parallel part of the target rod contacted at the initial deposition stage is often cut off during the preparation process. Ultimately, it is difficult to prepare large-size high-performance quartz glass by VAD method, and the efficiency of the deposition process is low. At the same time, due to the numerous influencing factors of the deposition process, it is difficult to monitor the parameters and process of the deposition in real time, which leads to room for improvement in the uniformity, stress and other key performance of the material.

[0031] For example, the invention patent JP33073993 designs a focusing torch with double focus and proposes a method for preparing large-diameter, high-uniformity and low-stress quartz glass using the torch. In the method, the torch is divided into two parts, i.e. reaction gas and combustion gas. The reaction gas structure is designed as a five-tube structure, and the combustion gas is distributed in the space between the outermost layer of the reaction gas and the sixth tube. The gas distribution from the middle to the outermost sixth tube is as follows: (1) first: SiCl4+O2; (2) second: O2; (3) third: H2; (4) fourth: O2; (5) fifth: H2; (6) fine tube between the fifth and sixth: O2; (7) sixth: H2. The gas tube distribution position is on the circumference of concentric circles to obtain a temperature distribution with central symmetry and slow change. At the same time, the flow rate of the combustible gas and the combustion-supporting gas is adjusted to be in the range of 5-50 m / s, and the flow rate ratio of the adjacent gases is controlled to be in the range of 1-0.4. Finally, a quartz glass rod with a diameter of 200 mm and a refractive index uniform distribution (≤0.5×10 -6) and quartz glass with circularly symmetric distribution. But the method designed focusing structure burner raw material layer aperture is small, the first heavy pipeline can pass into the raw material amount is not enough (only can use 20g / L of SiCl4), hindered the rod body further thickening, ultimately affected the quartz glass aperture further increase. In addition to the above-mentioned burner outer layer of oxygen through a group of distribution in the concentric circle on the thin tube, considering the oxygen from each independent thin tube flow from the thin tube center to the edge will show the flow rate distribution trend, although the patent by increasing the number of thin tube for the relief gas flow rate distribution problem, but the flow rate distribution of the layer of oxygen is still difficult to uniform, the uniform distribution of temperature in the deposition process and the refractive index distribution of the material. The invention patent CN108358437A proposes a method for improving the weight of the target rod by roughening the surface of the top hemisphere-shaped cylindrical target rod, wherein the target rod used is a cylindrical structure, and the lower end is a hemispherical shape with equal diameter / larger diameter. The surface of the target rod is roughened, and the roughness Rz is greater than 35μm, and at the same time, there is a concave-convex surface with a spacing of 1mm and a depth of 0.5mm-1.5mm below the roughened surface. Using this type of target rod, quartz glass with a weight of 160Kg can be prepared. The target rod used in this method is cylindrical, and in the initial stage of deposition, the efficiency of deposition is low due to the small contact area of the target rod with the deposition flame, and the powder body forming is slow. The invention patent CN201720650395.9 proposes a device for measuring the bulk density of the powder body prepared by VAD method, wherein the device installs a weight measurement component on the equipment lifting platform and installs a volume measurement component outside the deposition cavity. In the end state of deposition, the weight of the powder body is obtained by the pressure sensor; the outer diameter profile data of the bulk body is recorded by scanning to obtain the volume of the powder body, and the density of the powder body is directly read by the calculation software, which is used to solve the problem of rod dropping caused by density difference and heavy rod body in the sintering process of the powder body. However, for high-purity synthetic quartz, the change of weight and rod diameter with deposition time during the powder deposition process has important influence on the stress and uniformity of the material. The method collects relevant data after the deposition is completed, and the weight and rod diameter of the material are not monitored in real time during the deposition process.

[0032] Correspondingly, the application provides a quartz powder body preparation system and a preparation method. The quartz powder body preparation system comprises a focused burner and a deposition assembly; the focused burner is used for spraying reaction raw materials, and the focused burner comprises a raw material nozzle located at the center and a plurality of groups of combustion nozzles arranged layer by layer around the raw material nozzle from the inside to the outside, and the focal lengths of the plurality of groups of combustion nozzles are different. The deposition assembly is used for depositing the reaction raw materials sprayed by the focused burner to form a quartz powder body, and the deposition assembly comprises a target rod with a deposition end, and the cross-sectional outer diameter of the middle part of the deposition end is larger than that of the two ends of the deposition end. The quartz powder body preparation method uses the quartz powder body preparation system to prepare a quartz powder body.

[0033] Further, the application provides a quartz powder body preparation system, which comprises a focused burner and a deposition assembly. The focused burner is used for spraying reaction raw materials, and the focused burner comprises a raw material nozzle located at the center and a plurality of groups of combustion nozzles arranged layer by layer around the raw material nozzle from the inside to the outside, and the focal lengths of the plurality of groups of combustion nozzles are different. The deposition assembly is used for depositing the reaction raw materials sprayed by the focused burner to form a quartz powder body, and the deposition assembly comprises a target rod with a deposition end, and the cross-sectional outer diameter of the middle part of the deposition end is larger than that of the two ends of the deposition end. The corresponding quartz powder body preparation method can obtain a high-performance large-size quartz powder body with high deposition powder uniformity and low stress characteristics, wherein the rod diameter of the quartz powder body can be greater than or equal to 350 mm, and the rod weight can be greater than or equal to 200 kg. At the same time, by compensating for the low efficiency stage at the beginning of the deposition through the shape of the target rod, the problem of low rate and low efficiency at the beginning of the powder body deposition is solved, which greatly shortens the time of the rod body forming stage and improves the production efficiency. After sintering, the quartz glass rod diameter can be greater than or equal to 250 mm, and the quartz glass rod has the characteristics of high optical uniformity and low stress.

[0034] The specific embodiments of the application will be further described in detail below with reference to the accompanying drawings.

[0035] As shown in Figures 1 to 4 The application provides a quartz powder body preparation system 10, which comprises a focused burner 11, a deposition assembly 12, a laser rod diameter measuring instrument 13, and a data processing assembly 14. The focused burner 11 is used for spraying reaction raw materials, the deposition assembly 12 is used for depositing the reaction raw materials sprayed by the focused burner 11 to form a quartz powder body, the laser rod diameter measuring instrument 13 is used for measuring the outer diameter of the quartz powder body deposited on the target rod 121 of the deposition assembly 12, and the data processing assembly 14 is electrically connected with at least one of the focused burner 11, the deposition assembly 12, and the laser rod diameter measuring instrument 13, and is used for receiving, processing, and returning electrical signals to control at least one of the focused burner 11, the deposition assembly 12, and the laser rod diameter measuring instrument 13.

[0036] In one embodiment, the focusing torch 11 includes a raw material nozzle 111 located at the center, and multiple sets of combustion nozzles 110 arranged layer by layer around the raw material nozzle 111 from the inside out, the multiple sets of combustion nozzles 110 having different focal lengths. The deposition assembly 12 includes a target rod 121 having a deposition end 1211, the outer diameter of the cross-section at the middle of the deposition end 1211 being larger than the outer diameter of the cross-section at both ends of the deposition end 1211.

[0037] Understandably, the quartz powder preparation system 10 of this application uses a focusing torch 11 with multiple sets of combustion nozzles 110. The structure and deposition flow rate of the focusing torch 11 are optimized, so that the focal lengths of the multiple sets of combustion nozzles 110 arranged layer by layer around the raw material nozzles 111 from the inside out are different, achieving the preparation of large-size, high-performance quartz powder. The diameter of the obtained quartz powder rod can be greater than or equal to 350 mm, and the weight of the quartz powder rod can be greater than or equal to 200 kg. Simultaneously, the quartz powder preparation system 10 of this application also uses a target rod 121 that is smaller at both ends and larger in the middle. The shape of the target rod 121 compensates for the low efficiency in the initial stage of deposition, solving the problem of low deposition rate and low efficiency in the initial stage of powder deposition, and greatly shortening the time of the rod forming stage.

[0038] The term "high performance" at least refers to the high uniformity of the deposited powder and the high optical uniformity and low stress of the quartz glass after sintering. Further, "high uniformity of deposited powder" specifically refers to a particle size distribution (span) of ≤0.6, and "high optical uniformity" specifically refers to an optical uniformity of ≤0.5×10⁻⁶ for the quartz glass. -6 The term "low stress" specifically refers to residual stress in quartz glass ≤ 1 nm / cm.

[0039] The quartz powder preparation system 10 provided in this application embodiment has the advantages of fast quartz powder deposition rate and uniform deposition. The quartz powder preparation system 10 can prepare quartz powder with large size. It is understood that the large-size quartz glass prepared by the quartz powder preparation system 10 provided in this application embodiment can also have extremely high performance.

[0040] Further integration Figure 1 As shown, in one embodiment, the deposition assembly 12 further includes a lifting platform 122, a tension sensor component 123, and a deposition chamber 124. The deposition chamber 124 has a cavity for accommodating the target rod 121 and providing sufficient space for quartz growth on the target rod 121. The lifting platform 122 is suspended above the chamber and is used to connect the target rod 121. A pressure sensor is connected to the lifting platform 122 and the target rod 121 to sense the downward tension exerted by the target rod 121 on the lifting platform 122.

[0041] In the embodiment, the target rod 121 is connected with the lifting platform 122, and the tension sensor component 123 is arranged between the lifting platform 122 and the target rod 121. It can be understood that, as the deposited quartz on the target rod 121 gradually increases, the weight of the quartz rod formed on the target rod 121 gradually increases, and the pulling force applied to the target rod 121 also gradually increases. The weight of the quartz powder body can be monitored in real time by monitoring the pulling force on the target rod 121 in real time.

[0042] In an embodiment, the laser rod diameter measuring instrument 13 can be arranged inside the deposition cavity 124, which can include two or more spaced apart light sensing units 130. The light sensing units 130 cooperate to obtain the rod diameter of the quartz powder body and realize real-time monitoring of the rod diameter of the quartz powder body.

[0043] In the embodiment, the inner wall of the deposition cavity 124 can be provided with a plurality of movable sliding rails, and a plurality of light sensing units 130 can be arranged on the movable sliding rails. The light sensing units 130 can move back and forth along the main growth direction of the quartz powder body (usually the vertical direction or the gravity direction) and obtain the rod diameter of the quartz powder body at different positions in the direction, so as to realize real-time monitoring of the rod diameter of each region of the quartz powder body and further improve the detection accuracy of the rod diameter of the quartz powder body.

[0044] In an embodiment, the data processing assembly 14 includes a data recording and visualization screen 141, a tension sensing transmission line 142, and a rod diameter sensing transmission line 143. The tension sensing transmission line 142 is used to connect the tension sensor component 123, and the rod diameter sensing transmission line 143 is used to connect the light sensing unit 130. The data recording and visualization screen 141 is usually arranged outside the deposition cavity 124, and the data recording and visualization screen 141 is connected with the tension sensing transmission line 142 and the rod diameter sensing transmission line 143, respectively. The data recording and visualization screen 141 is integrated with a display screen and a data processing circuit, which can receive, record, sense, analyze, and present the data transmitted by the tension sensing transmission line 142 and the rod diameter sensing transmission line 143, and can transmit the processed data back to the tension sensor component 123 and the laser rod diameter measuring instrument 13 and control the working state.

[0045] In the embodiment, the rod weight measurement mainly relies on the tension sensor component 123 arranged on the material lifting rod. The material works at a predetermined rotation and lifting speed, and is zeroed at the software end. At this time, the device is in a standby state, and then the focused torch 11 is ignited. The formed silicon dioxide powder gradually deposits, and its weight also gradually increases. The net weight of the quartz powder body changes with time, which is measured by the tension sensor in real time. The time interval for the tension sensor to collect data is 1 second to 30 minutes, and preferably 1 minute to 10 minutes.

[0046] Specifically, the time interval for the tension sensor to collect data can be 1 minute, 2 minutes, 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, 20 minutes, 21 minutes, 22 minutes, 23 minutes, 24 minutes, 25 minutes, 26 minutes, 27 minutes, 28 minutes, 29 minutes, or 30 minutes.

[0047] In the present embodiment, the standby state of the laser rod diameter measuring instrument 13 is located at the top of the deposition cavity 124, and scans from the top to the bottom of the quartz powder body and then reversely scans back to the top standby position, records the rod diameter distribution of the quartz powder body and forms a 3D scanning map of the material. The scanning interval of the diameter measuring instrument is 3 to 30 minutes, preferably 5 to 10 minutes. Through the above method, the change of the powder form with time during the deposition process can be followed in real time. Through the visualization function of the software, the change of the average density of the material at different stages and the longitudinal local density distribution can be calculated. Combined with the flow information during deposition, the deposition rate and deposition efficiency of the material at different stages can be obtained synchronously. The density of the quartz powder body during the deposition process is 0.3 to 1.5 g / cm 3 , preferably 0.5 to 0.6 g / cm 3 .

[0048] Specifically, the scanning interval of the diameter measuring instrument can be 3 minutes, 4 minutes, 5 minutes, 6 minutes, 7 minutes, 8 minutes, 9 minutes, 10 minutes, 11 minutes, 12 minutes, 13 minutes, 14 minutes, 15 minutes, 16 minutes, 17 minutes, 18 minutes, 19 minutes, 20 minutes, 21 minutes, 22 minutes, 23 minutes, 24 minutes, 25 minutes, 26 minutes, 27 minutes, 28 minutes, 29 minutes, or 30 minutes.

[0049] Specifically, the density of the quartz powder body during the deposition process can specifically include 0.3 g / cm³, 0.4 g / cm³, 0.5 g / cm³, 0.6 g / cm³, 0.7 g / cm³, 0.8 g / cm³, 0.9 g / cm³, 1.0 g / cm³, 1.1 g / cm³, 1.2 g / cm³, 1.3 g / cm³, 1.4 g / cm³, or 1.5 g / cm³.

[0050] It can be understood that the lifting platform 122, the tension sensor component 123, and the deposition cavity 124 of the present embodiment can help realize the parameter monitoring of the quartz powder body, and specifically can measure the rod diameter and rod weight of the quartz powder body, and also help realize the means for large-size quartz powder body.

[0051] In an embodiment, the focus torch 11 is arranged below the target rod 121 along the vertical direction or the direction of gravity and sprays upward.

[0052] Further combined Figure 2 and Figure 3 As shown, in an embodiment, each group of combustion nozzles 110 includes two sub-nozzles arranged in layers from inside to outside, one of which is used to spray combustible gas, and the other is used to spray combustion-supporting gas.

[0053] In an embodiment, the focal lengths of the groups of combustion nozzles 110 arranged from inside to outside around the raw material nozzle 111 gradually increase.

[0054] In the present embodiment, the focus torch 11 includes three groups of combustion nozzles 110, namely the first combustion nozzle 1101, the second combustion nozzle 1102, and the third combustion nozzle 1103. The first combustion nozzle 1101 is arranged around the raw material nozzle 111, the second combustion nozzle 1102 is arranged around the first combustion nozzle 1101, and the third combustion nozzle 1103 is arranged around the second combustion nozzle 1102. The focal length of the third combustion nozzle 1103 is greater than that of the second combustion nozzle 1102, and the focal length of the second combustion nozzle 1102 is greater than that of the first combustion nozzle 1101.

[0055] In an embodiment, the first combustion nozzle 1101 includes a first sub-nozzle 112 arranged around the raw material nozzle 111 and a second sub-nozzle 113 arranged around the first sub-nozzle 112; the second combustion nozzle 1102 includes a third sub-nozzle 114 arranged around the second sub-nozzle 113 and a fourth sub-nozzle 115 arranged around the third sub-nozzle 114; the third combustion nozzle 1103 includes a fifth sub-nozzle 116 arranged around the fourth sub-nozzle 115 and a sixth sub-nozzle 117 arranged around the fifth sub-nozzle 116; the first sub-nozzle 112, the third sub-nozzle 114, and the fifth sub-nozzle 116 are used to spray combustion-supporting gas, and the second sub-nozzle 113, the fourth sub-nozzle 115, and the sixth sub-nozzle 117 are used to spray combustible gas; the combustion-supporting gas includes oxygen, and the combustible gas includes hydrogen.

[0056] In the present embodiment, the focus torch 11 is composed of seven coaxial quartz rings, from the center to the outermost layer, they are the first to the seventh. The first is the raw material and carrier gas layer, the second is the combustion-supporting gas O2 (inner layer oxygen), the third is the combustible gas H2 (inner layer hydrogen), the fourth is the combustion-supporting gas O2 (middle layer oxygen), the fifth is the combustible gas H2 (middle layer hydrogen), the sixth is the combustion-supporting gas O2 (outer layer oxygen), and the seventh is the combustible gas H2 (outer layer hydrogen).

[0057] In the embodiment, the first heavy quartz pipe (raw material nozzle 111) has an inner diameter of 5 to 15 mm, preferably 7 to 12 mm at the outlet; the gap between the layers of quartz pipes is 1 to 4 mm, preferably 2 to 3 mm; and the wall thickness of the quartz pipe is 1 to 3 mm, preferably 1 to 2 mm.

[0058] Specifically, the first heavy quartz pipe (raw material nozzle 111) has an inner diameter of 5 mm, 6 mm, 7 mm, 8 mm, 9 mm, 10 mm, 11 mm, 12 mm, 13 mm, 14 mm, or 15 mm at the outlet. The gap between the layers of quartz pipes is 1 mm, 2 mm, 3 mm, or 4 mm. The wall thickness of the quartz pipe is 1 mm, 2 mm, or 3 mm.

[0059] In the embodiment, the first heavy quartz pipe (raw material nozzle 111) to the third heavy quartz pipe (second sub-nozzle 113) have the same focal length f1, to ensure that the reaction raw materials and the two groups of gases in the inner layer are in a stable reaction state to form silicon dioxide powder particles.

[0060] In the embodiment, the fourth heavy quartz pipe (third sub-nozzle 114) and the fifth heavy quartz pipe (fourth sub-nozzle 115) have the same focal length f2, and the sixth heavy quartz pipe (fifth sub-nozzle 116) and the seventh heavy quartz pipe (sixth sub-nozzle 117) have the same focal length f3; the three groups of focal lengths gradually increase, i.e., f3>f2>f1. It can be understood that this design causes the hydrogen-oxygen combustion gas in the middle layer and the outer layer to gradually expand layer by layer, which is beneficial to obtain a larger and more uniform flame.

[0061] In the embodiment, the focal length of the torch is 80 to 300 mm, preferably 120 to 200 mm.

[0062] Specifically, the focal length of the torch is 80 mm, 90 mm, 100 mm, 110 mm, 120 mm, 130 mm, 140 mm, 150 mm, 160 mm, 170 mm, 180 mm, 190 mm, 200 mm, 210 mm, 220 mm, 230 mm, 240 mm, 250 mm, 260 mm, 270 mm, 280 mm, 290 mm, or 300 mm.

[0063] In another aspect, the distance from the focal point of the first heavy quartz pipe (raw material nozzle 111) to the focal point of the third heavy quartz pipe (second sub-nozzle 113) to the focal point of the fourth heavy quartz pipe (third sub-nozzle 114) and the fifth heavy quartz pipe (fourth sub-nozzle 115) is d1, and the distance from the focal point of the fourth heavy quartz pipe (third sub-nozzle 114) and the fifth heavy quartz pipe (fourth sub-nozzle 115) to the focal point of the sixth heavy quartz pipe (fifth sub-nozzle 116) and the seventh heavy quartz pipe (sixth sub-nozzle 117) is d2, which can also be adjusted according to the actual flame requirements, for example, d1 = d2.

[0064] It can be understood that the reaction raw material is sprayed out by the deposition burner, and the reaction raw material can generate silicon dioxide powder particles in a high temperature environment through a chemical reaction, and is deposited on the target rod 121 through thermal migration. The deposition burner has a more stable and efficient reaction environment for the reaction raw material through the above design, so that the particle size distribution of the reaction obtained silicon dioxide is more uniform, and the combustion is more sufficient, and has a more stable flame shape and flame temperature, and the diameter of the powder body obtained by deposition reaches more than 350 mm.

[0065] It can be understood that the focusing burner 11 provided by the embodiment of the present application has more excellent performance than the traditional burner, especially in improving the length and covering capacity of the flame, making the sprayed flame larger, so as to prepare large size (large diameter) quartz powder body, thereby obtaining large size quartz ingot.

[0066] Further combining Figure 4 As shown, the target rod 121 is composed of a deposition end portion 1211 and a tail handle section 1212, the deposition end portion 1211 includes an end body 1213 and a concave-convex structure 1214 arranged on the surface of the end body 1213, the deposition end portion 1211 is arranged at the end of the tail handle, and the other end of the tail handle is connected to a tension sensor component 123 or a lifting platform 122.

[0067] In an embodiment, the cross-sectional outer diameter of the middle part of the end body 1213 is larger than the cross-sectional outer diameter of the two ends of the end body 1213.

[0068] It can be understood that the flame of the focusing burner 11 is aligned with the maximum curvature of the deposition end portion 1211, such as the upper end fillet in the rounded cylindrical shape, so that the flame and the deposited powder body in the initial stage of deposition can be distributed on the top and bottom of the deposition end portion 1211, thereby enabling the powder body to completely cover the deposition end portion 1211.

[0069] In the embodiment, the shape of the end body 1213 is one of an oval shape, a water drop shape, a rounded triangular double cone shape, and a rounded cone shape. Specifically, as shown in FIG. 6, the end body 1213 is a rounded triangular double cone shape. Figure 4As shown in (a) of FIG. 12, the side view of the end body 1213 is generally elliptical, and the upper and lower ends of the end body 1213 along the direction of gravity have relatively large curvature, and the middle part is generally cylindrical. As shown in (b) of FIG. 12, Figure 4 As shown in (b) of FIG. 12, the side view of the end body 1213 is generally drop-shaped, and the tail end of the drop-shaped end body 1213 corresponds to the handle, the upper and lower ends of the end body 1213 along the direction of gravity have relatively large curvature than the middle part, and the curvature of the upper end and the lower end can be different. As shown in (c) of FIG. 12, Figure 4 As shown in (c) of FIG. 12, the side view of the end body 1213 is generally a circular triangle bipyramid, and the upper and lower ends of the end body 1213 along the direction of gravity have relatively large curvature than the middle part, and the lower end is relatively sharp and the upper end is relatively round. As shown in (d) of FIG. 12, Figure 4 As shown in (d) of FIG. 12, the side view of the end body 1213 is generally a circular cone, and the upper and lower ends of the end body 1213 along the direction of gravity have relatively large curvature than the middle part, and the lower end is relatively sharp and the upper end is relatively flat.

[0070] In this embodiment, the handle end is cylindrical, and the diameter is 20 to 80 mm, and the length is 20 to 80 mm; preferably, the diameter is 30 to 60 mm, and the length is 30 to 50 mm. The deposition end 1211 is a shape with a large deposition surface area, and the maximum diameter is 50 to 200 mm, and the preferred maximum diameter is 80 to 140 mm, and a larger surface area can accelerate the speed of powder body forming.

[0071] Specifically, the maximum diameter of the deposition end 1211 can be 50 mm, 60 mm, 70 mm, 80 mm, 90 mm, 100 mm, 110 mm, 120 mm, 130 mm, 140 mm, 150 mm, 160 mm, 170 mm, 180 mm, 190 mm, 200 mm.

[0072] It can be understood that the flame of the focusing torch 11 is aligned with the maximum curvature of the deposition end 1211, such as the upper corner of the circular cylindrical shape, so that the flame and the deposited powder body in the initial stage of deposition can be distributed on the top and bottom of the deposition end 1211, so that the powder body can completely cover the deposition end 1211.

[0073] Further in combination with Figure 5 As shown in (a) of FIG. 12, the side view of the end body 1213 is generally elliptical, and the upper and lower ends of the end body 1213 along the direction of gravity have relatively large curvature, and the middle part is generally cylindrical. As shown in (b) of FIG. 12,

[0074] In the embodiment, the surface of the deposition end 1211 has a concave-convex square tooth mark perpendicular to the axial direction, wherein the cross section of the convex part 1215 is substantially square, and the cross section of the concave part 1216 between the convex parts 1215 is also substantially square. The depth of the tooth mark corresponding to the concave part 1216 is 0.5-5 mm, and the pitch of the tooth mark corresponding to the concave part 1216 is 1-10 mm; preferably, the depth of the tooth mark is 1-3 mm, and the pitch is 1-3 mm.

[0075] Specifically, the depth of the tooth mark corresponding to the concave part 1216 can be 0.5 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm, or 5 mm. The pitch of the tooth mark corresponding to the concave part 1216 can be 0.5 mm, 1 mm, 1.5 mm, 2 mm, 2.5 mm, 3 mm, 3.5 mm, 4 mm, 4.5 mm, 5 mm, 5.5 mm, 6 mm, 6.5 mm, 7 mm, 7.5 mm, 8 mm, 8.5 mm, 9 mm, 9.5 mm, or 10 mm.

[0076] Meanwhile, the surface of the deposition end 1211 is polished, and the surface roughness Rz is greater than 20 μm, and preferably greater than 50 μm. The presence of the surface tooth mark and the surface roughening treatment can provide stronger adhesion and improve the load capacity of the target rod 121. Based on the target rod 121, the powder body can enter the parallel part for stable deposition in 2-6 hours.

[0077] It can be understood that the shape of the target rod 121 provided in the embodiments of the application can compensate for the deposition efficiency in the initial stage, can provide a larger cross-sectional area to promote the rapid forming of the quartz powder body, and the final shape of the quartz mass is not related to the shape of the target rod, so it will not have a negative impact on the preparation of the quartz mass. At the same time, the concave-convex structure 1214 on the surface of the target rod 121 can increase the friction and improve the load capacity of the target rod 121, so as to prepare a large-size (large-diameter) quartz powder body, thereby obtaining a large-size quartz mass.

[0078] The embodiments of the application also provide a quartz powder body preparation method for preparing a quartz powder body using the quartz powder body preparation system 10 of any one of the preceding embodiments.

[0079] It can be understood that the quartz powder body preparation method of the application uses the quartz powder body preparation system 10 of the preceding embodiments, and based on the quartz powder body preparation system 10, the rod diameter of the quartz powder body obtained by the quartz powder body preparation method of the application can be greater than or equal to 350 mm, and the rod weight can be greater than or equal to 200 kg.

[0080] Meanwhile, the low efficiency in the initial stage of powder deposition is compensated by the shape of the target rod 121, solving the problem of low rate and efficiency in the initial stage of powder deposition, greatly shortening the time of rod forming stage and improving the production efficiency.

[0081] It can be understood that the quartz powder body is finally obtained by high temperature sintering, and the high temperature sintering process can be selected from known and feasible process steps, which can be understood by those skilled in the art, and will not be described here. The quartz glass rod obtained after sintering can be greater than or equal to 250mm, and has the characteristics of high optical uniformity and low stress.

[0082] Example 1: Select an elliptical deposition target rod with a tail diameter of 30mm, a length of 40mm, a tail and a maximum diameter of 100mm; the surface of the target rod is a square groove with a depth of 1mm and a pitch of 1mm; the surface roughness Rz=35μm. SiCl4 is used as raw material with a flow rate of 45g / min, and helium is used as carrier gas. The torch parameters are shown in Table 1. After 4h of deposition, the parallel part is entered, and the quartz powder body rod diameter is 355mm, the sintered quartz mass diameter is 250mm, and the rod weight is 191kg. The optical uniformity and stress birefringence detection results of the mother rod are 0.8×10 -6 and 1.0nm / cm, respectively.

[0083] Table 1

[0084]

[0085] Example 2: Select a water drop type deposition target rod with a tail diameter of 40mm, a length of 40mm, a tail and a maximum diameter of 100mm; the surface of the target rod is a square groove with a depth of 2mm and a pitch of 2mm; the surface roughness Rz=50μm. D4 is used as raw material with a flow rate of 45g / min, and oxygen is used as carrier gas. The torch parameters are shown in Table 2. After 3.5h of deposition, the parallel part is entered, and the quartz powder body rod diameter is 358mm, the sintered quartz mass diameter is 256mm, and the rod weight is 200kg. The optical uniformity and stress birefringence detection results of the mother rod are 0.6×10 -6 and 0.9nm / cm, respectively.

[0086] Table 2

[0087]

[0088] Example 3: The deposition target rod with a tail diameter of 60 mm, a tail length of 50 mm, a tail diameter and a maximum diameter of 110 mm and a round triangle double-cone shape was selected. The surface of the target rod was square groove with a depth of 2 mm and a pitch of 2 mm. The surface roughness Rz was 60 μm. SiCl4 was used as the raw material with a flow rate of 40 g / min. Argon was used as the carrier gas. The torch parameters are shown in Table 3. After 2 h of deposition, the parallel part was entered. The final quartz powder body rod diameter was 371 mm. The sintered quartz mass diameter was 272 mm. The rod weight was 227 kg. The optical uniformity and stress birefringence detection results of the mother rod were 0.5 x 10 -6 and 0.6 nm / cm, respectively.

[0089] Table 3

[0090]

[0091] Example 4: The deposition target rod with a tail diameter of 60 mm, a tail length of 50 mm, a tail diameter and a maximum diameter of 110 mm and a round triangle double-cone shape was selected. The surface of the target rod was square groove with a depth of 3 mm and a pitch of 3 mm. The surface roughness Rz was 75 μm. D8 was used as the raw material with a flow rate of 60 g / min. Argon was used as the carrier gas. The torch parameters are shown in Table 4. After 2 h of deposition, the parallel part was entered. The final powder body rod diameter was 388 mm. The sintered quartz mass diameter was 286 mm. The rod weight was 251 kg. The optical uniformity and stress birefringence detection results of the mother rod were 0.5 x 10 -6 and 0.6 nm / cm, respectively.

[0092] Table 4

[0093]

[0094] Example 5: The deposition target rod with a tail diameter of 40 mm, a tail length of 40 mm, a tail diameter and a maximum diameter of 80 mm and a round cone shape was selected. The surface of the target rod was square groove with a depth of 2 mm and a pitch of 2 mm. The surface roughness Rz was 60 μm. SiCl4 was used as the raw material with a flow rate of 50 g / min. Helium was used as the carrier gas. The torch parameters are shown in Table 5. After 2 h of deposition, the parallel part was entered. The final powder body rod diameter was 358 mm. The sintered quartz mass diameter was 253 mm. The rod weight was 196 kg. The optical uniformity and stress birefringence detection results of the mother rod were 0.7 x 10 -6 and 0.8 nm / cm, respectively.

[0095] Table 5

[0096]

[0097] In the foregoing, specific embodiments of the application have been described with reference to the accompanying drawings. It will, however, be evident that various modifications and changes can be made thereto without departing from the broader spirit and scope of the application as set forth in the appended claims. The specification and drawings are, accordingly, to be regarded in an illustrative rather than a restrictive sense.

Claims

1. A system for producing a quartz powder body, characterized by The application relates to a quartz powder body preparation system and a quartz powder body preparation method. The quartz powder body preparation system comprises a focusing burner for spraying reaction raw materials, wherein the focusing burner comprises a raw material spraying port in the center and a plurality of groups of combustion spraying ports arranged layer by layer from the inside to the outside around the raw material spraying port, the focal lengths of the plurality of groups of combustion spraying ports are different, each group of combustion spraying ports comprises two sub-spraying ports arranged layer by layer from the inside to the outside, one of the two sub-spraying ports is used for spraying combustible gas, and the other is used for spraying combustion-supporting gas; and a deposition assembly for depositing the reaction raw materials sprayed by the focusing burner to form a quartz powder body, wherein the deposition assembly comprises a target rod with a deposition end, the middle part of the deposition end has a larger cross-sectional outer diameter than the two ends of the deposition end, the deposition end comprises an end body and a concave-convex structure arranged on the surface of the end body, the concave-convex structure comprises a plurality of convex parts and a plurality of concave parts, and the plurality of convex parts and the plurality of concave parts are arranged alternately and staggered. The flame of the focusing burner is aligned with the position with the maximum curvature of the deposition end. The focal lengths of the plurality of groups of combustion spraying ports arranged layer by layer from the inside to the outside around the raw material spraying port gradually increase.

2. The quartz powder body preparation system of claim 1, wherein, The focusing burner comprises three groups of combustion spraying ports, namely a first combustion spraying port, a second combustion spraying port and a third combustion spraying port, the first combustion spraying port is arranged around the raw material spraying port, the second combustion spraying port is arranged around the first combustion spraying port, the third combustion spraying port is arranged around the second combustion spraying port, the focal length of the third combustion spraying port is greater than that of the second combustion spraying port, and the focal length of the second combustion spraying port is greater than that of the first combustion spraying port.

3. The quartz powder body preparation system of claim 1, wherein, The first combustion spraying port comprises a first sub-spraying port around the raw material spraying port and a second sub-spraying port around the first sub-spraying port; the second combustion spraying port comprises a third sub-spraying port around the second sub-spraying port and a fourth sub-spraying port around the third sub-spraying port; the third combustion spraying port comprises a fifth sub-spraying port around the fourth sub-spraying port and a sixth sub-spraying port around the fifth sub-spraying port; the first sub-spraying port, the third sub-spraying port and the fifth sub-spraying port are used for spraying combustion-supporting gas, and the second sub-spraying port, the fourth sub-spraying port and the sixth sub-spraying port are used for spraying combustible gas.

4. The quartz powder body preparation system of claim 3, wherein The combustion-supporting gas comprises oxygen, and the combustible gas comprises hydrogen.

5. The quartz powder body preparation system of claim 4, wherein, The middle part of the end body has a larger cross-sectional outer diameter than the two ends of the end body.

6. The quartz powder body preparation system of claim 5, wherein, The shape of the end body is one of an oval shape, a water drop shape and a circular-triangle double-cone shape.

7. The quartz powder body preparation system of claim 6, wherein, The deposition assembly further comprises a lifting platform and a tension sensor component, the target rod is connected with the lifting platform, the tension sensor component is arranged between the lifting platform and the target rod and is used for sensing the downward tension applied by the target rod to the lifting platform; and the quartz powder body preparation system further comprises a laser rod diameter measuring instrument used for measuring the outer diameter of the quartz mass deposited on the target rod.

8. The quartz powder body preparation system of claim 1, wherein, The quartz powder body preparation method is prepared by using the quartz powder body preparation system according to any one of claims 1 to 8.

9. A method for producing a quartz powder body, characterized by ​

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