WO2021184713A1 - Sintering device and sintering method for optical fiber preform soot body - Google Patents

Sintering device and sintering method for optical fiber preform soot body Download PDF

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Publication number
WO2021184713A1
WO2021184713A1 PCT/CN2020/115863 CN2020115863W WO2021184713A1 WO 2021184713 A1 WO2021184713 A1 WO 2021184713A1 CN 2020115863 W CN2020115863 W CN 2020115863W WO 2021184713 A1 WO2021184713 A1 WO 2021184713A1
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sintering
furnace core
core tube
pressure
optical fiber
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PCT/CN2020/115863
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French (fr)
Chinese (zh)
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崔东明
孔明
伍淑坚
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烽火通信科技股份有限公司
武汉烽火锐拓科技有限公司
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Publication of WO2021184713A1 publication Critical patent/WO2021184713A1/en

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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/014Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01446Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C03B37/0146Furnaces therefor, e.g. muffle tubes, furnace linings
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

Definitions

  • the application relates to the field of optical fiber preform preparation, and in particular to a sintering device and method for the loose body of an optical fiber preform.
  • Patent CN1174820A introduces a method for degassing the sintered optical fiber preform in a high-temperature furnace using the principle of gas thermal diffusion, but this method requires additional special degassing equipment, and the degassing time is long, thereby increasing The equipment investment has reduced the production cost and efficiency of the optical fiber preform.
  • negative pressure sintering is a sintering method with higher sintering efficiency. Due to the good sealing of the equipment, the vitrification process is carried out under negative pressure, so that there is basically no gas residue in the sintered densified glass body. No additional degassing process is required, and in addition, the amount of He used can be effectively reduced.
  • the design of conventional sintering equipment cannot meet the requirements of high temperature and negative pressure conditions, and the existing negative pressure sintering adopts a long temperature zone, which means that the entire loose body mother rod is placed in a heating furnace and integrated sintered under negative pressure conditions. The actual forming process It is difficult to control and is only suitable for the sintering of core rods and mother rods with smaller dimensions.
  • Patent CN101838114A describes a method for optical fiber deuterium treatment. This method optimizes the deuterium treatment time, but only from the perspective of optical fiber processing, and does not solve this problem from the source of optical fiber preform manufacturing.
  • the embodiments of the application provide a sintering device and method for loose bodies of optical fiber preforms, which integrate dehydroxylation, vitrification sintering and deuteration, which can effectively eliminate the residual gas in the optical fiber preforms and reduce the amount of He in sintering.
  • the optical fiber preform eliminates structural defects at the source of manufacturing, thereby reducing the optical fiber's hydrogen sensitivity.
  • a sintering device for the loose body of an optical fiber preform which includes:
  • Furnace core tube which is assembled in the sintering box
  • a heating assembly which is assembled in the sintering box and located outside the furnace core tube, and the heating assembly forms a heating zone in a partial space of the furnace core tube;
  • a lead rod, the bottom end of the lead rod extends into the furnace core tube and is used to connect the loose body of the preform
  • a rod-feeding mechanism which is connected with the lead rod, and the rod-delivery mechanism is used to drive the lead rod to move in a vertical direction, so that the loose body of the preform is heated in the heating zone;
  • the first tube group which penetrates the walls of the sintering box and the furnace core tube and communicates with the inner cavity of the furnace core tube, and includes a first air inlet tube and a first exhaust tube;
  • the second tube group penetrates the wall surface of the sintering box body and communicates with the inner cavity of the sintering box, and includes a second air inlet pipe and a second exhaust pipe.
  • the sintering device further includes a negative pressure mechanism connected to the second exhaust pipe and the first exhaust pipe.
  • the sintering device further includes:
  • a pressure measuring mechanism which is used to measure the pressure in the furnace core tube and the pressure in the sintering box;
  • a control system which is used to control the rod feeding mechanism to drive the movement of the lead rod, control the opening and closing of the heating assembly, control the pressure measurement mechanism to measure pressure, control the opening and closing of the negative pressure mechanism, and control the on and off of the first tube group and the second tube group .
  • an opening and closing valve is provided on the second air inlet pipe, the opening and closing valve is used to connect a second gas source, and the second gas source is used to provide Ar;
  • the first air inlet pipe is provided with a multi-way valve, the multi-way valve is used to connect to a first gas source, and the first gas source is used to provide Cl 2 , O 2 , He, D 2 and/or Ar;
  • the control system is connected to the opening and closing valve and the multi-way valve, and is used to control the opening and closing valve to control Ar to enter the second intake pipe, and to control the multi-way valve to control the access to the first intake pipe.
  • Type of gas
  • the pressure measurement mechanism includes:
  • the first pressure sensor and the second pressure sensor are separately arranged on the first air inlet pipe and the second air inlet pipe. State the pressure in the furnace core tube and the sintering box;
  • a third pressure sensor and a fourth pressure sensor are separately arranged on the first exhaust pipe and the second exhaust pipe, the third pressure sensor and the fourth pressure sensor are respectively used to measure the furnace core tube and the sintering box The pressure in the furnace core tube and the sintering box during vacuuming.
  • a method for sintering a loose body of an optical fiber preform which includes the following steps:
  • the furnace core tube is pumped to the preset first negative pressure through the first exhaust pipe, and the sintering box is pumped to the preset first negative pressure through the second exhaust pipe.
  • the heating assembly is heated to a preset dehydroxylation temperature, Cl 2 , O 2 and He are introduced into the furnace core tube through the first air inlet pipe, and into the sintering box body through the second air inlet pipe Enter Ar, and make the pressure difference between the inside and outside of the furnace core tube within the preset second pressure range;
  • Heating the heating assembly to a preset vitrification and sintering temperature, and moving the loose body of the preform under the second negative pressure until the sintering of the loose body of the entire preform is completed;
  • it further includes the following steps:
  • the lead rod is driven so that the top or bottom end of the loose body of the preform is located in the heating zone.
  • the flow rates of Cl 2 , O 2 and He are 0.5 to 1.5 L/min, 0.6 to 1.2 L/min, and 15 to 25 L/min.
  • the first pressure range, the second pressure range, the third pressure range, and the fourth pressure range are all -1 to 1 mbar.
  • the sintering device provided in this application has two sealing systems, one of which is a sealing system composed of a furnace core tube, which can be used for dehydroxylation, negative pressure removal of residual gas, negative pressure vitrification sintering and negative pressure deuteration treatment; second It is a sealing system composed of a sintering box, which is synchronized with the furnace core tube by gas or pumped into a negative pressure to balance the pressure difference between the inside and outside of the furnace core tube to protect the furnace core tube.
  • the furnace core tube is first pumped to a negative pressure after the dehydroxylation is completed. Under negative pressure, the loose body of the preform can be removed more completely The residual Cl 2 and O 2 in the carbon dioxide can reduce defects such as bubbles.
  • the vitrification sintering is performed under negative pressure without the use of He.
  • the amount of He is greatly reduced, which effectively reduces the cost of manufacturing the polished rod.
  • the optical fiber preform is deuterated under negative pressure during the cooling time in the furnace core tube, and high temperature conditions are used to accelerate the diffusion of deuterium molecules, so that the structural defects formed in the optical rod are combined with deuterium in advance, thereby reducing its hydrogen Sensitivity and difficulty of subsequent optical fiber deuteration without affecting the overall optical rod manufacturing efficiency.
  • Fig. 1 is a schematic diagram of a sintering device for a loose body of an optical fiber preform provided by an embodiment of the application.
  • A heating zone; 1. sintering box; 2. furnace core tube; 20, second insulation layer; 21, furnace core tube cover plate; 3. heating assembly; 30, first insulation layer; 31, heating body; 32. Muffle tube; 4. Lead rod; 5. Preform loose body; 6. Rod feeding mechanism; 60. Frame body; 61. Slide arm; 7. First intake pipe; 8. First exhaust pipe; 9. 10. Second intake pipe; 10. Second exhaust pipe; 11. Negative pressure mechanism; 12. Dynamic sealing mechanism; 13. Quartz adapter; 14. Pressure measuring mechanism; 140. First pressure sensor; 141. Second pressure Sensor; 142, the third pressure sensor; 143, the fourth pressure sensor.
  • the embodiment of the application provides a sintering device for the loose body of an optical fiber preform, which integrates dehydroxylation, vitrification, sintering and deuteration. It can effectively eliminate the residual gas in the optical fiber preform and reduce the amount of He in sintering. Eliminate structural defects at the source of the preform manufacturing, thereby reducing the fiber's hydrogen sensitivity.
  • the optical fiber preform loose body sintering device includes a sintering box body 1, a furnace core tube 2, a heating assembly 3, a lead rod 4, a rod feeding mechanism 6, a first tube group, and a second tube.
  • the cover plate 21 constitutes a sealed furnace core tube 2.
  • the heating assembly 3 is assembled in the sintering box 1 and located outside the furnace core tube 2.
  • the heating assembly 3 forms a heating zone A in a part of the furnace core tube 2; the bottom end of the lead rod 4 extends into the furnace core tube 2 and is used to connect the prefabricated
  • the rod loose body 5 and the lead rod 4 are sealed at the position where the sintering box body 1 and the furnace core tube 2 penetrate, so as to avoid the sintering box body 1 and the furnace core tube 2 from communicating.
  • the rod feeding mechanism 6 is connected with the lead rod 4, and the rod feeding mechanism 6 is used to drive the lead rod 4 to move in the vertical direction, so that the preform loose body 5 is heated in the heating zone A;
  • the first tube group penetrates the walls of the sintering box 1 and the furnace core tube 2 and communicates with the inner cavity of the furnace core tube 2, which includes a first air inlet pipe 7 and a first exhaust pipe 8, a first air inlet pipe 7 and a first exhaust pipe 8 Seal at the junction with the wall surface of the sintering box 1 and the furnace core tube 2;
  • the second tube group penetrates the wall of the sintering box 1 and communicates with the inner cavity of the sintering box 1, which includes a second air inlet pipe 9 and a second
  • the exhaust pipe 10, the second intake pipe 9 and the second exhaust pipe 10 are sealed at the joint with the wall surface of the sintering box 1.
  • the first air inlet pipe 7 and the second air inlet pipe 9 are used to connect corresponding air sources.
  • the sintering device provided in this application has two sealing systems, one of which is a sealing system composed of a furnace core tube, which can be used for dehydroxylation, negative pressure removal of residual gas, negative pressure vitrification sintering and negative pressure deuteration treatment; second It is a sealing system composed of a sintering box, which is synchronized with the furnace core tube by gas or pumped into a negative pressure to balance the pressure difference between the inside and outside of the furnace core tube to protect the furnace core tube.
  • the furnace core tube is first pumped to a negative pressure after the dehydroxylation is completed. Under negative pressure, the loose body of the preform can be removed more completely The residual Cl 2 and O 2 in the carbon dioxide can reduce defects such as bubbles.
  • the vitrification sintering is performed under negative pressure without the use of He.
  • the amount of He is greatly reduced, which effectively reduces the cost of manufacturing the polished rod.
  • the optical fiber preform is deuterated under negative pressure during the cooling time in the furnace core tube, and high temperature conditions are used to accelerate the diffusion of deuterium molecules, so that the structural defects formed in the optical rod are combined with deuterium in advance, thereby reducing its hydrogen Sensitivity and difficulty of subsequent optical fiber deuteration without affecting the overall optical rod manufacturing efficiency.
  • the length of the heating zone A is less than the length of the preform loose body 5, so that during the heating process, the preform loose body 5 needs to be in the rod feeding mechanism 6 It moves in the vertical direction under the drive of, to complete the heating of the entire preform loose body 5.
  • the length of the heating zone in this application is less than the length of the preform loose body.
  • the heating assembly 3 is configured such that when the preform loose body 5 is connected to the lead 4, the bottom or top end of the preform loose body 5 is located in the heating zone A, so that the preform can be moved The loose body 5 facilitates sintering from one end to the other.
  • the rod feeding mechanism 6 includes a frame body 60 and a sliding arm 61.
  • the sliding arm 61 is movably arranged on the frame body 60 in the vertical direction, and the lead rod 4 is connected to the frame body 60.
  • the rod feeding mechanism 6 is simple in structure and low in cost, and can realize the lifting and lowering of the loose body 5 of the preform.
  • the lead 4 is rotatably arranged on the sliding arm 61, Thereby, the loose body 5 of the preform can be driven to rotate around its own axis.
  • the heating assembly 3 includes a first insulation layer 30, a heating body 31, and a muffle tube 32 all in a ring shape, and the first insulation layer 30, the heating body 31 and the horse
  • the flange tubes 32 are sequentially arranged at intervals from the sintering box body 1 toward the furnace core tube 2.
  • the heating body adopts a graphite heating body.
  • the use of a muffle tube can make the temperature field of the heating zone more stable and uniform, and at the same time isolate and protect the graphite heating body.
  • the graphite heating body directly heats the muffle tube at high temperature. The volatilized carbon on the graphite heating body avoids damage to the furnace core tube due to the existence of the muffle furnace.
  • the sintering device further includes a negative pressure mechanism 11, which is connected to the second exhaust pipe 10 and the first exhaust pipe 8, and is realized by a negative pressure mechanism 11. Vacuuming the furnace core tube and the sintering box body saves the number of equipment, and the negative pressure mechanism 11 can adopt a vacuum pump.
  • the first intake pipe 7 penetrates one of the upper and lower portions of the furnace core tube 2
  • the first exhaust pipe 8 penetrates the furnace core tube The other of the upper part and the lower part of 2; and in order to facilitate the connection through a negative pressure mechanism 11, the second exhaust pipe 10 is arranged close to the first exhaust pipe 8;
  • a second insulation layer 20 is provided on the outer wall of the furnace core tube 2 located outside the heating assembly.
  • the lead rod 4 and the furnace core tube 2 are connected with a dynamic sealing mechanism 12.
  • the dynamic sealing mechanism 12 seals the lead rod 4 and the furnace core tube 2 by means of packing or oil seal.
  • the bottom end of the lead rod 4 is provided with Quartz adapter 13 to which the loose body 5 of the preform is connected.
  • the second air inlet pipe 9 is provided with an opening and closing valve, which is connected to the second air source, and the second air source is used to provide Ar;
  • the first air inlet pipe 7 is provided with a multi-pass Valve, multi-way valve is used to connect the first gas source, the first gas source is used to provide Cl 2 , O 2 , He, D 2 and/or Ar, where D 2 and Ar are usually mixed gas, the control system and the start The closing valve and the multi-way valve are connected.
  • the opening and closing valve is controlled by the control system to control Ar to enter the second air inlet pipe 9, thereby venting or shutting off the sintering box 1, and the multi-way valve is controlled by the control system to control the entry into the first air inlet pipe.
  • the sintering device further includes a pressure measuring mechanism 14 and a control system.
  • the pressure measuring mechanism 14 can be used to measure the pressure in the furnace core tube 2 and the pressure in the sintering box 1.
  • the first intake pipe 7 is provided with a multi-way valve, and the second intake pipe 9, the first exhaust pipe 8 and the second exhaust pipe 10 are provided with opening and closing valves;
  • the measuring mechanism 14, the heating assembly 3, the rod feeding mechanism 6, and the negative pressure mechanism 11 are connected.
  • the control system is used to control the rod feeding mechanism 6 to drive the guide rod 4 to move to make the preform loose body 5 move up and down, and to control the heating assembly 3 to open and close.
  • the second negative pressure or the third negative pressure the pressure measuring mechanism 14 is controlled to perform pressure measurement to ensure that the pressure in the furnace core tube is at the first negative pressure, the second negative pressure or the third negative pressure, and the pressure difference between the inside and outside of the furnace core tube is at a preset
  • the first pressure range, the second pressure range, the third pressure range, or the fourth pressure range is controlled to perform pressure measurement to ensure that the pressure in the furnace core tube is at the first negative pressure, the second negative pressure or the third negative pressure, and the pressure difference between the inside and outside of the furnace core tube is at a preset The first pressure range, the second pressure range, the third pressure range, or the fourth pressure range.
  • the first air inlet pipe 7 penetrates one of the upper and lower portions of the furnace core tube 2, and the first exhaust pipe 8 penetrates the other of the upper and lower portions of the furnace core tube 2.
  • the second intake pipe 9 is located close to the first intake pipe 7, and the second exhaust pipe 10 is located close to the first exhaust pipe 8;
  • the pressure measuring mechanism 14 includes: separately located in the first intake pipe 7 and the second intake pipe 9
  • the first pressure sensor 140 and the second pressure sensor 141, the first pressure sensor 140 and the second pressure sensor 141 are respectively used to measure the furnace core tube 2 and the sintering box 1 when the furnace core tube 2 and the sintering box 1 Pressure; and, a third pressure sensor 142 and a fourth pressure sensor 143 separately provided on the first exhaust pipe 8 and the second exhaust pipe 10, the third pressure sensor 142 and the fourth pressure sensor 143 are used to measure the furnace core tube 2 and the pressure in the furnace core tube 2 and the sintering box 1 when the sintering box 1 is vacuumed.
  • the advantage of using the above four pressure sensors for the layout is that the furnace core tube 2 is usually very long, and there are some differences in the pressure at the upper and lower ends of the furnace core tube 2 during ventilation or vacuuming. Therefore, the first pressure sensor 140 and the second pressure sensor 140 are used for air intake. The second pressure sensor 141 performs measurement, and the third pressure sensor 142 and the fourth pressure sensor 143 are used to measure when vacuuming, to ensure that the measured pressure is more accurate.
  • a method for sintering the loose body of an optical fiber preform includes the following steps:
  • the heating assembly 3 is heated to the preset dehydroxylation temperature, Cl 2 , O 2 and He are introduced into the furnace core tube 2 through the first air inlet pipe 7, and into the sintering box 1 through the second air inlet pipe 9 Ar, the pressure difference between the inside and outside of the furnace core tube 2 is within the preset second pressure range; in this step, the heating element 3 has a heating rate of 25-50°C/min, and a dehydroxylation temperature of 1100-1250°C.
  • the heating assembly 3 is heated to the preset vitrification and sintering temperature, and under the second negative pressure, the preform loose body 5 is moved until the sintering of the entire preform loose body 5 is completed; in this step, the vitrification and sintering temperature is 1500-1600°C, the heating speed of the heating assembly 3 is 25-50°C/min, and the moving speed of the preform loose body 5 is 3-8mm/min.
  • step S5 the second negative pressure has been pumped, and in step S6, when the temperature is raised, on the one hand, since the second negative pressure is close to vacuum and there is less gas, the temperature rise pressure changes little, step S6
  • the pressure in S6 is basically under the second negative pressure.
  • the internal pressure of S6 deviates from the second negative pressure due to the increase in temperature, it can be adjusted by the negative pressure mechanism so that the pressure is at the second negative pressure. Down.
  • the following step is further included: driving the lead 4 so that the top or bottom end of the loose body 5 of the preform is located in the heating zone A.
  • the flow rates of Cl 2 , O 2 and He are 0.5 to 1.5 L/min, 0.6 to 1.2 L/min, and 15 to 25 L/min.
  • the first pressure range, the second pressure range, the third pressure range, and the fourth pressure range are all -1 to 1 mbar.
  • the vacuum pump is turned on to pump the inside and outside of the furnace core tube 2 to 20 mbar to discharge the air in the tube, and the heating body 31 is heated to 1200 °C at a heating rate of 25 °C/min, and the furnace core tube 2 is passed through Into 1slm Cl 2 , 0.8slm O 2 and 15slm He, turn on the rod feeding mechanism 6 to make the preform loose body 5 move downwards at a speed of 15mm/min for dehydroxylation.
  • the heating body 31 is heated to 1550 °C at a heating rate of 25 °C/min, and the rod feeding mechanism 6 is turned on to make the preform loose body 5 under a negative pressure environment.
  • the speed of 4mm/min is gradually sintered from bottom to top to be transparent.
  • the heating body 31 enters the cooling stage, the vacuum pump is turned off, and the volume D 2 is introduced into the furnace core tube 2
  • the D 2 /Ar mixture with a concentration of 1.5% and Ar is introduced into the sintering box 1, when the pressure in the furnace core tube 2 reaches 0.6 bar, the ventilation is stopped and the deuteration is maintained for 3 hours, and then the vacuum pump is turned on to reduce the D 2 in the furnace core tube 2
  • the /Ar mixed gas and Ar in the sintering box 1 are removed, and then a large flow of Ar is passed into the quartz furnace core tube.
  • the rising rod feeding mechanism lifts the sintered optical fiber preform out of the furnace core tube. There are no obvious bubbles in the sintered transparent optical fiber preform.
  • the typical attenuation of the drawn optical fiber at 1383nm is 0.275db/km. Deuterium treatment at 1.5% D 2 volume concentration can effectively reduce its hydrogen sensitivity. .
  • it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, It can also be an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, and it can be the internal communication between two components.
  • a fixed connection a detachable connection, or an integral connection
  • it can be a mechanical connection, It can also be an electrical connection
  • it can be directly connected, or indirectly connected through an intermediate medium, and it can be the internal communication between two components.

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Abstract

The present application relates to a sintering device and a sintering method for an optical fiber preform soot body. The sintering device comprises a sintering box, a furnace core tube, a heating assembly, a lead rod, a preform feeding mechanism, a first pipe group, and a second pipe group. The furnace core tube and the heating assembly are arranged in the sintering box, the heating assembly forming a heating zone. The lead rod extends into the furnace core tube and is used to connect a preform soot body. The preform feeding mechanism is connected to the lead rod to drive the lead rod to move so that the preform soot body is heated in the heating zone. The first pipe group runs through the walls of the sintering box and the furnace core tube and communicates with an inner cavity of the furnace core tube, and comprises a first intake pipe and a first exhaust pipe. The second pipe group runs through the wall of the sintering box and communicates with an internal cavity of the sintering box, and comprises a second intake pipe and a second exhaust pipe. The present application integrates dehydroxylation, vitrification sintering, and deuteration, and can effectively eliminate a residual gas inside an optical fiber preform, reduce the amount of He used, and eliminate structural defects from the source of optical fiber preform manufacturing, thereby reducing the hydrogen sensitivity of an optical fiber.

Description

一种光纤预制棒疏松体的烧结装置及烧结方法Sintering device and method for loose body of optical fiber preform 技术领域Technical field
本申请涉及光纤预制棒制备领域,特别涉及一种光纤预制棒疏松体的烧结装置及烧结方法。The application relates to the field of optical fiber preform preparation, and in particular to a sintering device and method for the loose body of an optical fiber preform.
背景技术Background technique
外部气相沉积法(OVD)和轴向气相沉积法(VAD)由于较高的性价比成为业内主流的制棒技术,其先通过SiCl 4等原料的高温水解反应和热泳原理制得大尺寸光纤预制棒疏松体,然后再经过脱水-烧结工艺得到低水峰、致密无缺陷的透明玻璃体。 External vapor deposition (OVD) and axial vapor deposition (VAD) have become the mainstream rod making technology in the industry due to their high cost performance. First , large-size optical fiber preforms are prepared through the high-temperature hydrolysis reaction of SiCl 4 and other raw materials and the principle of thermophoresis. Rod loose body, and then through dehydration-sintering process to obtain low water peak, dense and defect-free transparent glass body.
由于光纤预制棒疏松体在沉积过程中不可避免的会包含游离态水和硅羟基(Si-OH),因此,在玻璃化烧结前需要通入氧化性气体如Cl 2和O 2进行高温脱羟处理,然后再通入大流量He将疏松体孔隙中的Cl 2和O 2等置换出来,但此法很难彻底的将Cl 2和O 2等清除干净,以致于少量气体可能会残留在烧结玻璃化的光棒内形成气泡缺陷。 Since the loose body of the optical fiber preform will inevitably contain free water and silanol (Si-OH) during the deposition process, it is necessary to pass oxidizing gas such as Cl 2 and O 2 for high temperature dehydroxylation treatment before vitrification and sintering , And then pass in a large flow of He to replace Cl 2 and O 2 in the pores of the loose body, but this method is difficult to completely remove Cl 2 and O 2 so that a small amount of gas may remain in the sintered glass Bubble defects are formed in the transformed light rod.
此外,上述常规的脱水-烧结工艺中需要使用大量He,而He价格高昂,使得制棒成本居高不下,同时,部分He在烧结致密化过程中会残存在玻璃体内。专利CN1174820A介绍了一种将烧结完成的光纤预制棒置于高温炉中利用气体的热扩散原理进行脱气的方法,但此法需要额外配备专门的脱气设备,而且脱气时间长,从而增加设备投入,降低了光纤预制棒生产成本和效率。In addition, the above-mentioned conventional dehydration-sintering process needs to use a large amount of He, and the high price of He makes the cost of rod making high. At the same time, part of He will remain in the glass body during the sintering and densification process. Patent CN1174820A introduces a method for degassing the sintered optical fiber preform in a high-temperature furnace using the principle of gas thermal diffusion, but this method requires additional special degassing equipment, and the degassing time is long, thereby increasing The equipment investment has reduced the production cost and efficiency of the optical fiber preform.
相对于常规的烧结工艺,负压烧结是一种具有更高烧结效率的烧结方法,其由于设备密封性好,玻璃化过程在负压中进行,使得烧结致密化的玻璃体中基本无气体残留,无需额外脱气工序,另外,还能够有效减少He的使用量。但常规烧结装置的设计无法满足高温负压条件的要求,而现有的负压烧结采用长温区也即将整个疏松体母棒置于加热炉中在负压条件下一体化烧结,实际成型过程难以控制,且仅适 用于尺寸较小的芯棒母棒烧结。Compared with the conventional sintering process, negative pressure sintering is a sintering method with higher sintering efficiency. Due to the good sealing of the equipment, the vitrification process is carried out under negative pressure, so that there is basically no gas residue in the sintered densified glass body. No additional degassing process is required, and in addition, the amount of He used can be effectively reduced. However, the design of conventional sintering equipment cannot meet the requirements of high temperature and negative pressure conditions, and the existing negative pressure sintering adopts a long temperature zone, which means that the entire loose body mother rod is placed in a heating furnace and integrated sintered under negative pressure conditions. The actual forming process It is difficult to control and is only suitable for the sintering of core rods and mother rods with smaller dimensions.
另外,部分光纤预制棒在制造过程中存在大量结构缺陷,从而导致生产的光纤需要氘化很长的时间才能达到降低氢敏感性的目的,增加了光纤生产周期。专利CN101838114A描述了一种光纤氘气处理方法,此方法优化了氘气处理时间,但仅是从光纤处理角度考虑,未从光纤预制棒制造源头上解决此问题。In addition, some optical fiber preforms have a large number of structural defects during the manufacturing process, which leads to the deuteration of the produced optical fiber for a long time to achieve the purpose of reducing the hydrogen sensitivity, which increases the optical fiber production cycle. Patent CN101838114A describes a method for optical fiber deuterium treatment. This method optimizes the deuterium treatment time, but only from the perspective of optical fiber processing, and does not solve this problem from the source of optical fiber preform manufacturing.
发明内容Summary of the invention
本申请实施例提供一种光纤预制棒疏松体的烧结装置及烧结方法,集脱羟、玻璃化烧结和氘化于一体,能够有效消除光纤预制棒内部气体残留,减少烧结中的He用量,从光纤预制棒制造源头上消除结构缺陷,从而降低光纤氢敏感性。The embodiments of the application provide a sintering device and method for loose bodies of optical fiber preforms, which integrate dehydroxylation, vitrification sintering and deuteration, which can effectively eliminate the residual gas in the optical fiber preforms and reduce the amount of He in sintering. The optical fiber preform eliminates structural defects at the source of manufacturing, thereby reducing the optical fiber's hydrogen sensitivity.
第一方面,提供了一种光纤预制棒疏松体的烧结装置,其包括:In the first aspect, a sintering device for the loose body of an optical fiber preform is provided, which includes:
烧结箱体;Sintered box;
炉心管,其组设于所述烧结箱体内;Furnace core tube, which is assembled in the sintering box;
加热组件,其组设于所述烧结箱体内,并位于所述炉心管外侧,所述加热组件在所述炉心管部分空间内形成加热区;A heating assembly, which is assembled in the sintering box and located outside the furnace core tube, and the heating assembly forms a heating zone in a partial space of the furnace core tube;
引杆,所述引杆底端伸至所述炉心管内并用于连接预制棒疏松体;A lead rod, the bottom end of the lead rod extends into the furnace core tube and is used to connect the loose body of the preform;
送棒机构,其与所述引杆相连,所述送棒机构用于驱动引杆沿竖直方向移动,以使预制棒疏松体在加热区内加热;A rod-feeding mechanism, which is connected with the lead rod, and the rod-delivery mechanism is used to drive the lead rod to move in a vertical direction, so that the loose body of the preform is heated in the heating zone;
第一管组,其贯穿所述烧结箱体和炉心管的壁面并与炉心管内腔连通,其包括第一进气管和第一排气管;The first tube group, which penetrates the walls of the sintering box and the furnace core tube and communicates with the inner cavity of the furnace core tube, and includes a first air inlet tube and a first exhaust tube;
第二管组,其贯穿所述烧结箱体的壁面并与烧结箱体内腔连通,其包括第二进气管和第二排气管。The second tube group penetrates the wall surface of the sintering box body and communicates with the inner cavity of the sintering box, and includes a second air inlet pipe and a second exhaust pipe.
在一些实施例中,所述烧结装置还包括负压机构,所述负压机构与所述第二排气管和第一排气管相连。In some embodiments, the sintering device further includes a negative pressure mechanism connected to the second exhaust pipe and the first exhaust pipe.
在一些实施例中,所述烧结装置还包括:In some embodiments, the sintering device further includes:
压力测量机构,其用于测量所述炉心管内的压力和烧结箱体内的 压力;A pressure measuring mechanism, which is used to measure the pressure in the furnace core tube and the pressure in the sintering box;
控制系统,其用于控制所述送棒机构驱动引杆移动、控制加热组件启闭、控制压力测量机构测量压力、控制负压机构启闭、控制第一管组和第二管组的通断。A control system, which is used to control the rod feeding mechanism to drive the movement of the lead rod, control the opening and closing of the heating assembly, control the pressure measurement mechanism to measure pressure, control the opening and closing of the negative pressure mechanism, and control the on and off of the first tube group and the second tube group .
在一些实施例中,所述第二进气管上设有启闭阀,所述启闭阀用于连接第二气源,所述第二气源用于提供Ar;In some embodiments, an opening and closing valve is provided on the second air inlet pipe, the opening and closing valve is used to connect a second gas source, and the second gas source is used to provide Ar;
所述第一进气管上设有多通阀,所述多通阀用于连接第一气源,所述第一气源用于提供Cl 2、O 2、He、D 2和/或Ar; The first air inlet pipe is provided with a multi-way valve, the multi-way valve is used to connect to a first gas source, and the first gas source is used to provide Cl 2 , O 2 , He, D 2 and/or Ar;
所述控制系统与所述启闭阀和所述多通阀相连,并用于通过控制启闭阀以控制Ar进入第二进气管,以及通过控制所述多通阀以控制进入第一进气管的气体种类。The control system is connected to the opening and closing valve and the multi-way valve, and is used to control the opening and closing valve to control Ar to enter the second intake pipe, and to control the multi-way valve to control the access to the first intake pipe. Type of gas.
在一些实施例中,所述压力测量机构包括:In some embodiments, the pressure measurement mechanism includes:
分设于第一进气管和第二进气管上的第一压力传感器和第二压力传感器,所述第一压力传感器和第二压力传感器分别用于测量所述炉心管以及烧结箱体进气时所述炉心管和烧结箱体内的压力;The first pressure sensor and the second pressure sensor are separately arranged on the first air inlet pipe and the second air inlet pipe. State the pressure in the furnace core tube and the sintering box;
以及,分设于第一排气管和第二排气管上的第三压力传感器和第四压力传感器,所述第三压力传感器和第四压力传感器分别用于测量所述炉心管以及烧结箱体抽真空时所述炉心管和烧结箱体内的压力。And, a third pressure sensor and a fourth pressure sensor are separately arranged on the first exhaust pipe and the second exhaust pipe, the third pressure sensor and the fourth pressure sensor are respectively used to measure the furnace core tube and the sintering box The pressure in the furnace core tube and the sintering box during vacuuming.
第二方面,提供了一种光纤预制棒疏松体的烧结方法,包括如下步骤:In a second aspect, a method for sintering a loose body of an optical fiber preform is provided, which includes the following steps:
提供如上任一所述的烧结装置,并将预制棒疏松体连接于所述引杆上;Provide a sintering device as described in any one of the above, and connect the loose body of the preform to the lead rod;
通过负压机构,经所述第一排气管将炉心管抽至预设的第一负压,经所述第二排气管将所述烧结箱体抽至炉心管内外压差位于预设的第一压力范围内;Through the negative pressure mechanism, the furnace core tube is pumped to the preset first negative pressure through the first exhaust pipe, and the sintering box is pumped to the preset first negative pressure through the second exhaust pipe. Within the first pressure range;
将所述加热组件升温至预设的脱羟温度,通过所述第一进气管向所述炉心管内通入Cl 2、O 2和He,通过所述第二进气管向所述烧结箱体内通入Ar,并使所述炉心管内外压差位于预设的第二压力范围内; The heating assembly is heated to a preset dehydroxylation temperature, Cl 2 , O 2 and He are introduced into the furnace core tube through the first air inlet pipe, and into the sintering box body through the second air inlet pipe Enter Ar, and make the pressure difference between the inside and outside of the furnace core tube within the preset second pressure range;
移动预制棒疏松体,使所述预制棒疏松体逐步经过所述加热区,并完成整个预制棒疏松体的脱羟;Move the preform loose body so that the preform loose body gradually passes through the heating zone, and complete the dehydroxylation of the entire preform loose body;
将所述炉心管抽至预设的第二负压,同时将烧结箱体抽至炉心管内外压差位于预设的第三压力范围内,脱除预制棒疏松体内残余气体;Pumping the furnace core tube to a preset second negative pressure, and at the same time pumping the sintering box body until the pressure difference between the inside and outside of the furnace core tube is within the preset third pressure range, to remove the residual gas in the preform rod;
将所述加热组件升温至预设的玻璃化烧结温度,在所述第二负压下,移动预制棒疏松体,直至完成整个预制棒疏松体的烧结;Heating the heating assembly to a preset vitrification and sintering temperature, and moving the loose body of the preform under the second negative pressure until the sintering of the loose body of the entire preform is completed;
降温至预设温度,向所述炉心管内通入D 2和Ar,直至达到第三负压,同时向所述烧结箱体内通入Ar,直至所述炉心管内外压力差位于预设的第四压力范围内,进行氘化处理,得到光纤预制棒。 Cool down to a preset temperature, pass D 2 and Ar into the furnace core tube until the third negative pressure is reached, and pass Ar into the sintering box at the same time, until the pressure difference between the inside and outside of the furnace core tube is at the preset fourth Deuterium treatment is performed within the pressure range to obtain an optical fiber preform.
在一些实施例中,还包括如下步骤:In some embodiments, it further includes the following steps:
排走所述炉心管内的D 2和Ar,以及烧结箱体内的Ar; Drain the D 2 and Ar in the furnace core tube and the Ar in the sintering box;
向所述炉心管及烧结箱体内通入Ar,直至压力达到大气压时,取出光纤预制棒。Pour Ar into the furnace core tube and the sintering box until the pressure reaches atmospheric pressure, then take out the optical fiber preform.
在一些实施例中,在升温至预设的脱羟温度之前,还包括如下步骤:In some embodiments, before raising the temperature to the preset dehydroxylation temperature, the following steps are further included:
驱动引杆以使所述预制棒疏松体顶端或底端位于加热区内。The lead rod is driven so that the top or bottom end of the loose body of the preform is located in the heating zone.
在一些实施例中,所述Cl 2、O 2和He的流量依次为0.5~1.5L/min、0.6~1.2L/min和15~25L/min。 In some embodiments, the flow rates of Cl 2 , O 2 and He are 0.5 to 1.5 L/min, 0.6 to 1.2 L/min, and 15 to 25 L/min.
在一些实施例中,第一压力范围、第二压力范围、第三压力范围和第四压力范围均为-1~1mbar。In some embodiments, the first pressure range, the second pressure range, the third pressure range, and the fourth pressure range are all -1 to 1 mbar.
本申请提供的技术方案带来的有益效果包括:The beneficial effects brought about by the technical solution provided by this application include:
本申请提供的烧结装置具有两个密封系统,其一为炉心管构成的密封系统,可以用来进行脱羟、负压脱除残余气体、负压玻璃化烧结以及负压氘化处理;其二为烧结箱体构成的密封系统,与炉心管同步通气体或着抽成负压,用来平衡炉心管内外压力差,以保护炉心管。The sintering device provided in this application has two sealing systems, one of which is a sealing system composed of a furnace core tube, which can be used for dehydroxylation, negative pressure removal of residual gas, negative pressure vitrification sintering and negative pressure deuteration treatment; second It is a sealing system composed of a sintering box, which is synchronized with the furnace core tube by gas or pumped into a negative pressure to balance the pressure difference between the inside and outside of the furnace core tube to protect the furnace core tube.
相比于通过大流量He进行置换,本申请提供的烧结装置在使用时,当脱羟完成后先将炉心管抽至负压,在负压条件下,能够更彻底的脱除预制棒疏松体中残留的Cl 2和O 2,减少气泡等缺陷。 Compared with the replacement by a large flow of He, when the sintering device provided in this application is used, the furnace core tube is first pumped to a negative pressure after the dehydroxylation is completed. Under negative pressure, the loose body of the preform can be removed more completely The residual Cl 2 and O 2 in the carbon dioxide can reduce defects such as bubbles.
利用本申请,玻璃化烧结是在负压中进行,不需要使用He,相比传统烧结方法,He用量大为减少,有效降低了光棒制造成本,同时玻璃体中不会残留He,无需再额外进行高温脱气处理。With this application, the vitrification sintering is performed under negative pressure without the use of He. Compared with the traditional sintering method, the amount of He is greatly reduced, which effectively reduces the cost of manufacturing the polished rod. At the same time, there is no residual He in the glass body and no additional need Carry out high temperature degassing treatment.
利用本申请,光纤预制棒在炉心管中冷却时间进行负压条件下的氘化处理,利用高温条件加快氘气分子的扩散,使光棒中形成的结构缺陷预先与氘结合,从而降低其氢敏感性和后续光纤氘化难度,同时不影响整体光棒制造效率。Using this application, the optical fiber preform is deuterated under negative pressure during the cooling time in the furnace core tube, and high temperature conditions are used to accelerate the diffusion of deuterium molecules, so that the structural defects formed in the optical rod are combined with deuterium in advance, thereby reducing its hydrogen Sensitivity and difficulty of subsequent optical fiber deuteration without affecting the overall optical rod manufacturing efficiency.
利用本申请进行负压条件下的预制棒制造,可以避免Cl 2和O 2等气体的泄露,减少了加热组件被氧化的几率。 Using this application to manufacture preforms under negative pressure conditions can avoid the leakage of gases such as Cl 2 and O 2 and reduce the probability of heating components being oxidized.
附图说明Description of the drawings
为了更清楚地说明本申请实施例中的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本申请的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to more clearly describe the technical solutions in the embodiments of the present application, the following will briefly introduce the drawings that need to be used in the description of the embodiments. Obviously, the drawings in the following description are only some embodiments of the present application. For those of ordinary skill in the art, other drawings can be obtained based on these drawings without creative work.
图1为本申请实施例提供的光纤预制棒疏松体的烧结装置示意图。Fig. 1 is a schematic diagram of a sintering device for a loose body of an optical fiber preform provided by an embodiment of the application.
图中:A、加热区;1、烧结箱体;2、炉心管;20、第二保温层;21、炉心管盖板;3、加热组件;30、第一保温层;31、加热体;32、马弗管;4、引杆;5、预制棒疏松体;6、送棒机构;60、架体;61、滑臂;7、第一进气管;8、第一排气管;9、第二进气管;10、第二排气管;11、负压机构;12、动密封机构;13、石英转接头;14、压力测量机构;140、第一压力传感器;141、第二压力传感器;142、第三压力传感器;143、第四压力传感器。In the figure: A, heating zone; 1. sintering box; 2. furnace core tube; 20, second insulation layer; 21, furnace core tube cover plate; 3. heating assembly; 30, first insulation layer; 31, heating body; 32. Muffle tube; 4. Lead rod; 5. Preform loose body; 6. Rod feeding mechanism; 60. Frame body; 61. Slide arm; 7. First intake pipe; 8. First exhaust pipe; 9. 10. Second intake pipe; 10. Second exhaust pipe; 11. Negative pressure mechanism; 12. Dynamic sealing mechanism; 13. Quartz adapter; 14. Pressure measuring mechanism; 140. First pressure sensor; 141. Second pressure Sensor; 142, the third pressure sensor; 143, the fourth pressure sensor.
具体实施方式Detailed ways
为使本申请实施例的目的、技术方案和优点更加清楚,下面将结合本申请实施例中的附图,对本申请实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本申请的一部分实施例,而不 是全部的实施例。基于本申请中的实施例,本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例,都属于本申请保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions in the embodiments of the present application will be described clearly and completely in conjunction with the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments These are a part of the embodiments of the present application, but not all of the embodiments. Based on the embodiments in this application, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the protection scope of this application.
本申请实施例提供了一种光纤预制棒疏松体的烧结装置,其集脱羟、玻璃化烧结和氘化于一体,能够有效消除光纤预制棒内部气体残留,减少烧结中的He用量,从光纤预制棒制造源头上消除结构缺陷,从而降低光纤氢敏感性。The embodiment of the application provides a sintering device for the loose body of an optical fiber preform, which integrates dehydroxylation, vitrification, sintering and deuteration. It can effectively eliminate the residual gas in the optical fiber preform and reduce the amount of He in sintering. Eliminate structural defects at the source of the preform manufacturing, thereby reducing the fiber's hydrogen sensitivity.
参见图1所示,本申请实施例提供的光纤预制棒疏松体的烧结装置,包括烧结箱体1、炉心管2、加热组件3、引杆4、送棒机构6、第一管组和第二管组;其中,烧结箱体1采用密封的箱结构;炉心管2组设于烧结箱体1内,炉心管2包括管本体与顶部的炉心管盖板21,管本体与顶部的炉心管盖板21构成密封的炉心管2。加热组件3组设于烧结箱体1内,并位于炉心管2外侧,加热组件3在炉心管2的部分空间内形成加热区A;引杆4底端伸至炉心管2内并用于连接预制棒疏松体5,引杆4与烧结箱体1以及炉心管2相贯穿的位置处密封住,以避免烧结箱体1以及炉心管2相通。Referring to Figure 1, the optical fiber preform loose body sintering device provided by the embodiment of the present application includes a sintering box body 1, a furnace core tube 2, a heating assembly 3, a lead rod 4, a rod feeding mechanism 6, a first tube group, and a second tube. Two tube groups; among them, the sintering box body 1 adopts a sealed box structure; the furnace core tube 2 is set in the sintering box body 1, the furnace core tube 2 includes the tube body and the furnace core tube cover 21 on the top, the tube body and the furnace core tube on the top The cover plate 21 constitutes a sealed furnace core tube 2. The heating assembly 3 is assembled in the sintering box 1 and located outside the furnace core tube 2. The heating assembly 3 forms a heating zone A in a part of the furnace core tube 2; the bottom end of the lead rod 4 extends into the furnace core tube 2 and is used to connect the prefabricated The rod loose body 5 and the lead rod 4 are sealed at the position where the sintering box body 1 and the furnace core tube 2 penetrate, so as to avoid the sintering box body 1 and the furnace core tube 2 from communicating.
送棒机构6与引杆4相连,送棒机构6用于驱动引杆4沿竖直方向移动,以使预制棒疏松体5在加热区A内加热;The rod feeding mechanism 6 is connected with the lead rod 4, and the rod feeding mechanism 6 is used to drive the lead rod 4 to move in the vertical direction, so that the preform loose body 5 is heated in the heating zone A;
第一管组贯穿烧结箱体1和炉心管2的壁面并与炉心管2内腔连通,其包括第一进气管7和第一排气管8,第一进气管7和第一排气管8在与烧结箱体1和炉心管2的壁面的连接处进行密封;第二管组贯穿烧结箱体1的壁面并与烧结箱体1内腔连通,其包括第二进气管9和第二排气管10,第二进气管9和第二排气管10在与烧结箱体1的壁面相连接处进行密封。第一进气管7与第二进气管9用于连接相应的气源。The first tube group penetrates the walls of the sintering box 1 and the furnace core tube 2 and communicates with the inner cavity of the furnace core tube 2, which includes a first air inlet pipe 7 and a first exhaust pipe 8, a first air inlet pipe 7 and a first exhaust pipe 8 Seal at the junction with the wall surface of the sintering box 1 and the furnace core tube 2; the second tube group penetrates the wall of the sintering box 1 and communicates with the inner cavity of the sintering box 1, which includes a second air inlet pipe 9 and a second The exhaust pipe 10, the second intake pipe 9 and the second exhaust pipe 10 are sealed at the joint with the wall surface of the sintering box 1. The first air inlet pipe 7 and the second air inlet pipe 9 are used to connect corresponding air sources.
本申请提供的烧结装置具有两个密封系统,其一为炉心管构成的密封系统,可以用来进行脱羟、负压脱除残余气体、负压玻璃化烧结以及负压氘化处理;其二为烧结箱体构成的密封系统,与炉心管同步 通气体或着抽成负压,用来平衡炉心管内外压力差,以保护炉心管。The sintering device provided in this application has two sealing systems, one of which is a sealing system composed of a furnace core tube, which can be used for dehydroxylation, negative pressure removal of residual gas, negative pressure vitrification sintering and negative pressure deuteration treatment; second It is a sealing system composed of a sintering box, which is synchronized with the furnace core tube by gas or pumped into a negative pressure to balance the pressure difference between the inside and outside of the furnace core tube to protect the furnace core tube.
相比于通过大流量He进行置换,本申请提供的烧结装置在使用时,当脱羟完成后先将炉心管抽至负压,在负压条件下,能够更彻底的脱除预制棒疏松体中残留的Cl 2和O 2,减少气泡等缺陷。 Compared with the replacement by a large flow of He, when the sintering device provided in this application is used, the furnace core tube is first pumped to a negative pressure after the dehydroxylation is completed. Under negative pressure, the loose body of the preform can be removed more completely The residual Cl 2 and O 2 in the carbon dioxide can reduce defects such as bubbles.
利用本申请,玻璃化烧结是在负压中进行,不需要使用He,相比传统烧结方法,He用量大为减少,有效降低了光棒制造成本,同时玻璃体中不会残留He,无需再额外进行高温脱气处理。With this application, the vitrification sintering is performed under negative pressure without the use of He. Compared with the traditional sintering method, the amount of He is greatly reduced, which effectively reduces the cost of manufacturing the polished rod. At the same time, there is no residual He in the glass body and no additional need Carry out high temperature degassing treatment.
利用本申请,光纤预制棒在炉心管中冷却时间进行负压条件下的氘化处理,利用高温条件加快氘气分子的扩散,使光棒中形成的结构缺陷预先与氘结合,从而降低其氢敏感性和后续光纤氘化难度,同时不影响整体光棒制造效率。Using this application, the optical fiber preform is deuterated under negative pressure during the cooling time in the furnace core tube, and high temperature conditions are used to accelerate the diffusion of deuterium molecules, so that the structural defects formed in the optical rod are combined with deuterium in advance, thereby reducing its hydrogen Sensitivity and difficulty of subsequent optical fiber deuteration without affecting the overall optical rod manufacturing efficiency.
利用本申请进行负压条件下的预制棒制造,可以避免Cl 2和O 2等气体的泄露,减少了加热组件被氧化的几率。 Using this application to manufacture preforms under negative pressure conditions can avoid the leakage of gases such as Cl 2 and O 2 and reduce the probability of heating components being oxidized.
在一些优选的实施例中,参见图1所示,沿竖直方向,加热区A的长度小于预制棒疏松体5的长度,这样在加热过程中,预制棒疏松体5需要在送棒机构6的驱动下在竖直方向上移动,以完成整个预制棒疏松体5的加热,本申请加热区的长度小于预制棒疏松体的长度,相对于采用长温区的烧结方式,本申请通过上下移动预制棒疏松体以完成整个棒的处理,成型过程容易控制,温场更为均匀,能够提高疏松体烧结质量。In some preferred embodiments, as shown in FIG. 1, along the vertical direction, the length of the heating zone A is less than the length of the preform loose body 5, so that during the heating process, the preform loose body 5 needs to be in the rod feeding mechanism 6 It moves in the vertical direction under the drive of, to complete the heating of the entire preform loose body 5. The length of the heating zone in this application is less than the length of the preform loose body. Compared with the sintering method using a long temperature zone, this application moves up and down The loose body of the preform can complete the treatment of the whole rod, the forming process is easy to control, the temperature field is more uniform, and the sintering quality of the loose body can be improved.
在一些优选的实施例中,加热组件3被配置为:当预制棒疏松体5连接于引杆4上时,预制棒疏松体5的底端或顶端位于加热区A,这样可以通过移动预制棒疏松体5以便于从一端到另一端进行烧结。In some preferred embodiments, the heating assembly 3 is configured such that when the preform loose body 5 is connected to the lead 4, the bottom or top end of the preform loose body 5 is located in the heating zone A, so that the preform can be moved The loose body 5 facilitates sintering from one end to the other.
在一些优选的实施例中,参见图1所示,送棒机构6包括架体60和滑臂61,滑臂61沿竖直方向可移动地组设于架体60上,引杆4连接于滑臂61上,送棒机构6结构简单,造价便宜,能够实现对预制棒疏松体5的提升和下降,当然了,在一些优选实施例中,引杆4转动地设于滑臂61上,从而可以驱动预制棒疏松体5绕自身轴线旋转。In some preferred embodiments, as shown in FIG. 1, the rod feeding mechanism 6 includes a frame body 60 and a sliding arm 61. The sliding arm 61 is movably arranged on the frame body 60 in the vertical direction, and the lead rod 4 is connected to the frame body 60. On the sliding arm 61, the rod feeding mechanism 6 is simple in structure and low in cost, and can realize the lifting and lowering of the loose body 5 of the preform. Of course, in some preferred embodiments, the lead 4 is rotatably arranged on the sliding arm 61, Thereby, the loose body 5 of the preform can be driven to rotate around its own axis.
在一些优选的实施例中,参见图1所示,加热组件3包括均呈环状的第一保温层30、加热体31和马弗管32,且第一保温层30、加热体31和马弗管32自烧结箱体1朝炉心管2方向依次间隔布置。本实施例中加热体采用石墨加热体,使用马弗管能够使加热区温场更稳定、均匀,同时对石墨加热体隔离对其进行保护,此外,石墨加热体直接对马弗管高温加热,石墨加热体上的挥发的碳因马弗炉的存在而避免对炉心管造成损坏。In some preferred embodiments, as shown in FIG. 1, the heating assembly 3 includes a first insulation layer 30, a heating body 31, and a muffle tube 32 all in a ring shape, and the first insulation layer 30, the heating body 31 and the horse The flange tubes 32 are sequentially arranged at intervals from the sintering box body 1 toward the furnace core tube 2. In this embodiment, the heating body adopts a graphite heating body. The use of a muffle tube can make the temperature field of the heating zone more stable and uniform, and at the same time isolate and protect the graphite heating body. In addition, the graphite heating body directly heats the muffle tube at high temperature. The volatilized carbon on the graphite heating body avoids damage to the furnace core tube due to the existence of the muffle furnace.
在一些优选的实施例中,参见图1所示,烧结装置还包括负压机构11,负压机构11与第二排气管10和第一排气管8相连,通过一个负压机构11实现对炉心管及烧结箱体的抽真空,节省设备数量,负压机构11可以采用真空泵。In some preferred embodiments, as shown in FIG. 1, the sintering device further includes a negative pressure mechanism 11, which is connected to the second exhaust pipe 10 and the first exhaust pipe 8, and is realized by a negative pressure mechanism 11. Vacuuming the furnace core tube and the sintering box body saves the number of equipment, and the negative pressure mechanism 11 can adopt a vacuum pump.
在实际布置时,为了更好地进行排气与进气,参见图1所示,第一进气管7贯穿于炉心管2的上部和下部中的一个,第一排气管8贯穿于炉心管2的上部和下部中的另一个;而为了便于通过一个负压机构11连接,第二排气管10靠近第一排气管8设置;In the actual arrangement, in order to better perform exhaust and intake, as shown in Figure 1, the first intake pipe 7 penetrates one of the upper and lower portions of the furnace core tube 2, and the first exhaust pipe 8 penetrates the furnace core tube The other of the upper part and the lower part of 2; and in order to facilitate the connection through a negative pressure mechanism 11, the second exhaust pipe 10 is arranged close to the first exhaust pipe 8;
在一些优选的实施例中,参见图1所示,炉心管2位于加热组件外侧的外壁上设有第二保温层20。引杆4与炉心管2相连接处设有动密封机构12,动密封机构12通过填料密封或油封的方式对引杆4和炉心管2之间进行密封,引杆4底端设有用于与预制棒疏松体5连接的石英转接头13。In some preferred embodiments, as shown in FIG. 1, a second insulation layer 20 is provided on the outer wall of the furnace core tube 2 located outside the heating assembly. The lead rod 4 and the furnace core tube 2 are connected with a dynamic sealing mechanism 12. The dynamic sealing mechanism 12 seals the lead rod 4 and the furnace core tube 2 by means of packing or oil seal. The bottom end of the lead rod 4 is provided with Quartz adapter 13 to which the loose body 5 of the preform is connected.
在一些优选的实施例中,第二进气管9上设有启闭阀,启闭阀同于连接第二气源,第二气源用于提供Ar;第一进气管7上设有多通阀,多通阀用于连接第一气源,第一气源用于提供Cl 2、O 2、He、D 2和/或Ar,其中D 2和Ar通常是作为混合气体,控制系统与启闭阀以及多通阀相连,通过控制系统控制启闭阀以控制Ar进入第二进气管9,从而对烧结箱体1进行通气或断气,通过控制系统控制多通阀以控制进入第一进气管7的气体种类,比如使Cl 2、O 2、He同时进入炉心管2,或者D 2和Ar进入炉心管2,或者使Ar进入炉心管2,从而实现炉心管2 的通气与断气。 In some preferred embodiments, the second air inlet pipe 9 is provided with an opening and closing valve, which is connected to the second air source, and the second air source is used to provide Ar; the first air inlet pipe 7 is provided with a multi-pass Valve, multi-way valve is used to connect the first gas source, the first gas source is used to provide Cl 2 , O 2 , He, D 2 and/or Ar, where D 2 and Ar are usually mixed gas, the control system and the start The closing valve and the multi-way valve are connected. The opening and closing valve is controlled by the control system to control Ar to enter the second air inlet pipe 9, thereby venting or shutting off the sintering box 1, and the multi-way valve is controlled by the control system to control the entry into the first air inlet pipe. The gas types of 7, for example, allow Cl 2 , O 2 , and He to enter the furnace core tube 2 at the same time, or D 2 and Ar enter the furnace core tube 2, or allow Ar to enter the furnace core tube 2, so as to realize the ventilation and cut-off of the furnace core tube 2.
参见图1所示,在一些优选的实施例中,该烧结装置还包括压力测量机构14以及控制系统,压力测量机构14可以用来测量炉心管2内的压力以及烧结箱体1内的压力,第一进气管7上设多通阀,第二进气管9、第一排气管8和第二排气管10上设启闭阀;而控制系统与多通阀以及各启闭阀、压力测量机构14、加热组件3、送棒机构6、负压机构11相连,控制系统用来控制送棒机构6驱动引杆4移动以使预制棒疏松体5上下移动,控制加热组件3启闭以进行加热或停止加热,控制各启闭阀以及多通阀以启闭第一管组和第二管组,控制负压机构11的开启与关闭,以使炉心管内压力处于第一负压、第二负压或第三负压,控制压力测量机构14进行压力测量,以确保炉心管内压力处于第一负压、第二负压或第三负压,以及确保炉心管内外压力差位于预设的第一压力范围、第二压力范围、第三压力范围或第四压力范围。As shown in Fig. 1, in some preferred embodiments, the sintering device further includes a pressure measuring mechanism 14 and a control system. The pressure measuring mechanism 14 can be used to measure the pressure in the furnace core tube 2 and the pressure in the sintering box 1. The first intake pipe 7 is provided with a multi-way valve, and the second intake pipe 9, the first exhaust pipe 8 and the second exhaust pipe 10 are provided with opening and closing valves; The measuring mechanism 14, the heating assembly 3, the rod feeding mechanism 6, and the negative pressure mechanism 11 are connected. The control system is used to control the rod feeding mechanism 6 to drive the guide rod 4 to move to make the preform loose body 5 move up and down, and to control the heating assembly 3 to open and close. Perform heating or stop heating, control the opening and closing valves and multi-way valves to open and close the first tube group and the second tube group, and control the opening and closing of the negative pressure mechanism 11 so that the pressure in the furnace core tube is at the first negative pressure and the first negative pressure. The second negative pressure or the third negative pressure, the pressure measuring mechanism 14 is controlled to perform pressure measurement to ensure that the pressure in the furnace core tube is at the first negative pressure, the second negative pressure or the third negative pressure, and the pressure difference between the inside and outside of the furnace core tube is at a preset The first pressure range, the second pressure range, the third pressure range, or the fourth pressure range.
参见图1所示,在一些优选的实施例中,第一进气管7贯穿于炉心管2的上部和下部中的一个,第一排气管8贯穿于炉心管2的上部和下部中的另一个;而第二进气管9靠近第一进气管7设置,第二排气管10靠近第一排气管8设置;压力测量机构14包括:分设于第一进气管7和第二进气管9上的第一压力传感器140和第二压力传感器141,第一压力传感器140和第二压力传感器141分别用于测量炉心管2以及烧结箱体1进气时炉心管2和烧结箱体1内的压力;以及,分设于第一排气管8和第二排气管10上的第三压力传感器142和第四压力传感器143,第三压力传感器142和第四压力传感器143分别用于测量炉心管2以及烧结箱体1抽真空时炉心管2和烧结箱体1内的压力。Referring to Figure 1, in some preferred embodiments, the first air inlet pipe 7 penetrates one of the upper and lower portions of the furnace core tube 2, and the first exhaust pipe 8 penetrates the other of the upper and lower portions of the furnace core tube 2. One; and the second intake pipe 9 is located close to the first intake pipe 7, and the second exhaust pipe 10 is located close to the first exhaust pipe 8; the pressure measuring mechanism 14 includes: separately located in the first intake pipe 7 and the second intake pipe 9 The first pressure sensor 140 and the second pressure sensor 141, the first pressure sensor 140 and the second pressure sensor 141 are respectively used to measure the furnace core tube 2 and the sintering box 1 when the furnace core tube 2 and the sintering box 1 Pressure; and, a third pressure sensor 142 and a fourth pressure sensor 143 separately provided on the first exhaust pipe 8 and the second exhaust pipe 10, the third pressure sensor 142 and the fourth pressure sensor 143 are used to measure the furnace core tube 2 and the pressure in the furnace core tube 2 and the sintering box 1 when the sintering box 1 is vacuumed.
上述使用四个压力传感器进行布局的好处是,通常炉心管2很长,在通气或者抽真空时,炉心管2上下两端的压力存在一些差别,故在进气时用第一压力传感器140和第二压力传感器141进行测量,而抽真空时用第三压力传感器142和第四压力传感器143测量,确保测量的压力更加准确。The advantage of using the above four pressure sensors for the layout is that the furnace core tube 2 is usually very long, and there are some differences in the pressure at the upper and lower ends of the furnace core tube 2 during ventilation or vacuuming. Therefore, the first pressure sensor 140 and the second pressure sensor 140 are used for air intake. The second pressure sensor 141 performs measurement, and the third pressure sensor 142 and the fourth pressure sensor 143 are used to measure when vacuuming, to ensure that the measured pressure is more accurate.
结合图1所示,在一些优选的实施例中,还提供了一种光纤预制棒疏松体的烧结方法,包括如下步骤:As shown in Figure 1, in some preferred embodiments, a method for sintering the loose body of an optical fiber preform is also provided, which includes the following steps:
S1:提供上述任一的烧结装置,并将预制棒疏松体5连接于引杆4上;S1: Provide any one of the above-mentioned sintering devices, and connect the loose body 5 of the preform to the lead 4;
S2:通过负压机构11,经第一排气管8将炉心管2抽至预设的第一负压,经第二排气管10将烧结箱体1抽至炉心管2内外压差位于预设的第一压力范围内;本步骤中,第一负压为10~100mbar;S2: Through the negative pressure mechanism 11, the furnace core tube 2 is pumped to the preset first negative pressure through the first exhaust pipe 8, and the sintering box 1 is pumped to the furnace core tube 2 through the second exhaust pipe 10 until the pressure difference between the inside and the outside of the furnace core tube 2 is located Within the preset first pressure range; in this step, the first negative pressure is 10-100 mbar;
S3:将加热组件3升温至预设的脱羟温度,通过第一进气管7向炉心管2内通入Cl 2、O 2和He,通过第二进气管9向烧结箱体1内通入Ar,炉心管2内外压差位于预设的第二压力范围内;本步骤中,加热组件3升温速度为25~50℃/min,脱羟温度为1100~1250℃。 S3: The heating assembly 3 is heated to the preset dehydroxylation temperature, Cl 2 , O 2 and He are introduced into the furnace core tube 2 through the first air inlet pipe 7, and into the sintering box 1 through the second air inlet pipe 9 Ar, the pressure difference between the inside and outside of the furnace core tube 2 is within the preset second pressure range; in this step, the heating element 3 has a heating rate of 25-50°C/min, and a dehydroxylation temperature of 1100-1250°C.
S4:移动预制棒疏松体5,直至在加热区A内完成整个预制棒疏松体5的脱羟;本步骤中,预制棒疏松体5的移动速度为10~30mm/min。S4: Move the preform loose body 5 until the dehydroxylation of the entire preform loose body 5 is completed in the heating zone A; in this step, the moving speed of the preform loose body 5 is 10-30 mm/min.
S5:将炉心管2抽至预设的第二负压,同时将烧结箱体1抽至炉心管2内外压差位于预设的第三压力范围内,保持15~30min脱除预制棒疏松体5内残余气体;本步骤中,第二负压为5~10mbar;S5: Pump the furnace core tube 2 to the preset second negative pressure, and at the same time pump the sintering box 1 until the pressure difference between the inside and outside of the furnace core tube 2 is within the preset third pressure range, and keep it for 15-30 minutes to remove the loose body of the preform 5 Residual gas; in this step, the second negative pressure is 5-10mbar;
S6:将加热组件3升温至预设的玻璃化烧结温度,在第二负压下,移动预制棒疏松体5,直至完成整个预制棒疏松体5的烧结;本步骤中,玻璃化烧结温度为1500~1600℃,加热组件3的升温速度为25~50℃/min,预制棒疏松体5的移动速度为3~8mm/min。S6: The heating assembly 3 is heated to the preset vitrification and sintering temperature, and under the second negative pressure, the preform loose body 5 is moved until the sintering of the entire preform loose body 5 is completed; in this step, the vitrification and sintering temperature is 1500-1600°C, the heating speed of the heating assembly 3 is 25-50°C/min, and the moving speed of the preform loose body 5 is 3-8mm/min.
需要说明的是,在步骤S5中,已经抽至第二负压,在步骤S6中,当升温时,一方面,由于第二负压已接近真空,气体少,故升温压力变化小,步骤S6中的压力基本上第二负压下,另一方面,若S6中因升温导致其内压力偏离第二负压较大,则可以通过负压机构进行调节,以使其压力在第二负压下。It should be noted that in step S5, the second negative pressure has been pumped, and in step S6, when the temperature is raised, on the one hand, since the second negative pressure is close to vacuum and there is less gas, the temperature rise pressure changes little, step S6 The pressure in S6 is basically under the second negative pressure. On the other hand, if the internal pressure of S6 deviates from the second negative pressure due to the increase in temperature, it can be adjusted by the negative pressure mechanism so that the pressure is at the second negative pressure. Down.
S7:降温至预设温度,通过第一进气管7向炉心管2内通入D 2和Ar,其中D 2体积浓度为1%~3%,直至达到第三负压,通过第二进气 管9同时向烧结箱体1内通入Ar,直至炉心管2内外压力差位于预设的第四压力范围内,进行氘化处理,1~3h后结束,得到光纤预制棒。本步骤中,预设温度为800-1000℃,第三负压为0.5-0.8bar, S7: Cool down to a preset temperature, pass D 2 and Ar into the furnace core tube 2 through the first air inlet pipe 7, where the volume concentration of D 2 is 1% to 3%, until the third negative pressure is reached, and pass through the second air inlet pipe 9 Simultaneously pour Ar into the sintering box 1 until the pressure difference between the inside and outside of the furnace core tube 2 is within the preset fourth pressure range, and perform the deuteration treatment, which ends after 1 to 3 hours, and the optical fiber preform is obtained. In this step, the preset temperature is 800-1000°C, the third negative pressure is 0.5-0.8 bar,
S8:排走炉心管2内的D 2和Ar,以及烧结箱体1内的Ar;向炉心管2及烧结箱体1内通入Ar,直至炉心管2及烧结箱体1内压力达到大气压时,取出光纤预制棒。 S8: Drain the D 2 and Ar in the furnace core tube 2 and the Ar in the sintering box 1; pour Ar into the furnace core tube 2 and the sintering box 1 until the pressure in the furnace core tube 2 and the sintering box 1 reaches atmospheric pressure When, take out the optical fiber preform.
在一些优选的实施例中,在升温至预设的脱羟温度之前,还包括如下步骤:驱动引杆4以使预制棒疏松体5顶端或底端位于加热区A内。In some preferred embodiments, before the temperature is raised to the preset dehydroxylation temperature, the following step is further included: driving the lead 4 so that the top or bottom end of the loose body 5 of the preform is located in the heating zone A.
在一些优选的实施例中,Cl 2、O 2和He的流量依次为0.5~1.5L/min、0.6~1.2L/min和15~25L/min。 In some preferred embodiments, the flow rates of Cl 2 , O 2 and He are 0.5 to 1.5 L/min, 0.6 to 1.2 L/min, and 15 to 25 L/min.
在一些优选的实施例中,第一压力范围、第二压力范围、第三压力范围和第四压力范围均为-1~1mbar。In some preferred embodiments, the first pressure range, the second pressure range, the third pressure range, and the fourth pressure range are all -1 to 1 mbar.
具体实施例:Specific embodiment:
将OVD外包层沉积工艺制得的密度为0.3-0.5g/cm 3的大尺寸预制棒疏松体5置入炉心管2内,下降使预制棒疏松体5底端定位到加热区中间,以此作为脱羟和玻璃化烧结的起始位置,开启真空泵将炉心管2内外抽至20mbar以排出管内空气,以25℃/min的升温速度将加热体31升温至1200℃,向炉心管2内通入1slm Cl 2、0.8slm O 2和15slm He,开启送棒机构6使预制棒疏松体5以15mm/min速度向下运动进行脱羟,待预制棒疏松体5顶端到达加热区后,停止通入气体并将预制棒疏松体5提升到起始位置,开启真空泵将炉心管2和烧结箱体1内的压力同步的抽至10mbar,保持30min以使预制棒疏松体5中残留的Cl 2、O 2和He从多孔结构中完全逸出并脱除,然后以25℃/min的升温速度将加热体31升温至1550℃,开启送棒机构6使预制棒疏松体5在负压环境下以4mm/min速度从下到上逐渐烧结至透明,待预制棒疏松体5顶端到达热区后,玻璃化烧结结束,加热体31进入降温阶段,关闭真空泵,向炉心管2内通入D 2体积浓度为1.5%的D 2/Ar混合气以 及向烧结箱体1内通入Ar,当炉心管2内压力达到0.6bar时停止通气并保持氘化3h,然后开启真空泵将炉心管2内D 2/Ar混合气以及烧结箱体1内Ar排除,再向石英炉心管内通入大流量Ar,待压力达到1bar时,上升送棒机构将烧结成型的光纤预制棒从炉心管内提出。烧结成型的透明光纤预制棒内目视无明显气泡,拉制的光纤1383nm衰减典型值为0.275db/km,在1.5%D 2体积浓度下氘化处理1-3h即可有效降低其氢敏感性。 Place the large-size preform loose body 5 with a density of 0.3-0.5 g/cm 3 produced by the OVD outer coating deposition process into the furnace core tube 2 and lower it so that the bottom end of the preform loose body 5 is positioned in the middle of the heating zone. As the starting position for dehydroxylation and vitrification and sintering, the vacuum pump is turned on to pump the inside and outside of the furnace core tube 2 to 20 mbar to discharge the air in the tube, and the heating body 31 is heated to 1200 °C at a heating rate of 25 °C/min, and the furnace core tube 2 is passed through Into 1slm Cl 2 , 0.8slm O 2 and 15slm He, turn on the rod feeding mechanism 6 to make the preform loose body 5 move downwards at a speed of 15mm/min for dehydroxylation. After the top of the preform loose body 5 reaches the heating zone, stop the flow Into the gas and lift the preform loose body 5 to the starting position, turn on the vacuum pump to simultaneously pump the pressure in the furnace core tube 2 and the sintering box 1 to 10mbar, and keep it for 30 minutes to make the remaining Cl 2 , O 2 and He are completely escaped and removed from the porous structure, and then the heating body 31 is heated to 1550 ℃ at a heating rate of 25 ℃/min, and the rod feeding mechanism 6 is turned on to make the preform loose body 5 under a negative pressure environment. The speed of 4mm/min is gradually sintered from bottom to top to be transparent. After the top of the preform loose body 5 reaches the hot zone, the vitrification and sintering is finished, the heating body 31 enters the cooling stage, the vacuum pump is turned off, and the volume D 2 is introduced into the furnace core tube 2 The D 2 /Ar mixture with a concentration of 1.5% and Ar is introduced into the sintering box 1, when the pressure in the furnace core tube 2 reaches 0.6 bar, the ventilation is stopped and the deuteration is maintained for 3 hours, and then the vacuum pump is turned on to reduce the D 2 in the furnace core tube 2 The /Ar mixed gas and Ar in the sintering box 1 are removed, and then a large flow of Ar is passed into the quartz furnace core tube. When the pressure reaches 1 bar, the rising rod feeding mechanism lifts the sintered optical fiber preform out of the furnace core tube. There are no obvious bubbles in the sintered transparent optical fiber preform. The typical attenuation of the drawn optical fiber at 1383nm is 0.275db/km. Deuterium treatment at 1.5% D 2 volume concentration can effectively reduce its hydrogen sensitivity. .
在本申请的描述中,需要说明的是,术语“上”、“下”等指示的方位或位置关系为基于附图所示的方位或位置关系,仅是为了便于描述本申请和简化描述,而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作,因此不能理解为对本申请的限制。除非另有明确的规定和限定,术语“安装”、“相连”、“连接”应做广义理解,例如,可以是固定连接,也可以是可拆卸连接,或一体地连接;可以是机械连接,也可以是电连接;可以是直接相连,也可以通过中间媒介间接相连,可以是两个元件内部的连通。对于本领域的普通技术人员而言,可以根据具体情况理解上述术语在本申请中的具体含义。In the description of this application, it should be noted that the orientation or positional relationship indicated by the terms "upper", "lower", etc. is based on the orientation or positional relationship shown in the drawings, and is only for the convenience of describing the application and simplifying the description. It does not indicate or imply that the pointed device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present application. Unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection, It can also be an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, and it can be the internal communication between two components. For those of ordinary skill in the art, the specific meanings of the above-mentioned terms in this application can be understood according to specific circumstances.
需要说明的是,在本申请中,诸如“第一”和“第二”等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来,而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且,术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含,从而使得包括一系列要素的过程、方法、物品或者设备不仅包括那些要素,而且还包括没有明确列出的其他要素,或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下,由语句“包括一个……”限定的要素,并不排除在包括所述要素的过程、方法、物品或者设备中还存在另外的相同要素。It should be noted that in this application, relational terms such as "first" and "second" are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply There is any such actual relationship or sequence between these entities or operations. Moreover, the terms "include", "include" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements not only includes those elements, but also includes those that are not explicitly listed Other elements of, or also include elements inherent to this process, method, article or equipment. If there are no more restrictions, the element defined by the sentence "including a..." does not exclude the existence of other identical elements in the process, method, article, or equipment that includes the element.
以上所述仅是本申请的具体实施方式,使本领域技术人员能够理解或实现本申请。对这些实施例的多种修改对本领域的技术人员来说将是显而易见的,本文中所定义的一般原理可以在不脱离本申请的精 神或范围的情况下,在其它实施例中实现。因此,本申请将不会被限制于本文所示的这些实施例,而是要符合与本文所申请的原理和新颖特点相一致的最宽的范围。The above are only specific implementations of the application, so that those skilled in the art can understand or implement the application. Various modifications to these embodiments will be obvious to those skilled in the art, and the general principles defined herein can be implemented in other embodiments without departing from the spirit or scope of the application. Therefore, this application will not be limited to the embodiments shown in this document, but should conform to the widest scope consistent with the principles and novel features applied in this document.

Claims (10)

  1. 一种光纤预制棒疏松体的烧结装置,其特征在于,其包括:A sintering device for a loose body of an optical fiber preform, which is characterized in that it comprises:
    烧结箱体(1);Sintering box (1);
    炉心管(2),其组设于所述烧结箱体(1)内;Furnace core tube (2), which is assembled in the sintering box (1);
    加热组件(3),其组设于所述烧结箱体(1)内,并位于所述炉心管(2)外侧,所述加热组件(3)在所述炉心管(2)部分空间内形成加热区(A);The heating component (3) is assembled in the sintering box (1) and located outside the furnace core tube (2), and the heating component (3) is formed in a partial space of the furnace core tube (2) Heating zone (A);
    引杆(4),所述引杆(4)底端伸至所述炉心管(2)内并用于连接预制棒疏松体(5);A lead rod (4), the bottom end of the lead rod (4) extends into the furnace core tube (2) and is used to connect the preform loose body (5);
    送棒机构(6),其与所述引杆(4)相连,所述送棒机构(6)用于驱动引杆(4)沿竖直方向移动,以使预制棒疏松体(5)在加热区(A)内加热;The rod feeding mechanism (6) is connected with the lead rod (4), and the rod feeding mechanism (6) is used to drive the lead rod (4) to move in the vertical direction so that the preform loose body (5) is in the Heating in the heating zone (A);
    第一管组,其贯穿所述烧结箱体(1)和炉心管(2)的壁面并与炉心管(2)内腔连通,其包括第一进气管(7)和第一排气管(8);The first tube group, which penetrates the walls of the sintering box (1) and the furnace core tube (2) and communicates with the inner cavity of the furnace core tube (2), and includes a first air inlet tube (7) and a first exhaust tube ( 8);
    第二管组,其贯穿所述烧结箱体(1)的壁面并与烧结箱体(1)内腔连通,其包括第二进气管(9)和第二排气管(10)。The second tube group penetrates the wall surface of the sintering box (1) and communicates with the inner cavity of the sintering box (1), and includes a second air inlet pipe (9) and a second exhaust pipe (10).
  2. 如权利要求1所述的光纤预制棒疏松体的烧结装置,其特征在于:所述烧结装置还包括负压机构(11),所述负压机构(11)与所述第二排气管(10)和第一排气管(8)相连。The sintering device for the loose body of the optical fiber preform according to claim 1, wherein the sintering device further comprises a negative pressure mechanism (11), the negative pressure mechanism (11) and the second exhaust pipe ( 10) Connect with the first exhaust pipe (8).
  3. 如权利要求2所述的光纤预制棒疏松体的烧结装置,其特征在于,所述烧结装置还包括:The sintering device for the loose body of the optical fiber preform according to claim 2, wherein the sintering device further comprises:
    压力测量机构(14),其用于测量所述炉心管(2)内的压力和烧结箱体(1)内的压力;A pressure measuring mechanism (14), which is used to measure the pressure in the furnace core tube (2) and the pressure in the sintering box (1);
    控制系统,其用于控制所述送棒机构(6)驱动引杆(4)移动、控制加热组件(3)启闭、控制压力测量机构(14)测量压力、控制负压机构(11)启闭、控制第一管组和第二管组的通断。A control system, which is used to control the rod feeding mechanism (6) to drive the lead rod (4) to move, to control the opening and closing of the heating assembly (3), to control the pressure measuring mechanism (14) to measure pressure, and to control the negative pressure mechanism (11) to start Close, control the on and off of the first tube group and the second tube group.
  4. 如权利要求3所述的光纤预制棒疏松体的烧结装置,其特征在于:The sintering device for the loose body of the optical fiber preform according to claim 3, wherein:
    所述第二进气管(9)上设有启闭阀,所述启闭阀用于连接第二气源,所述第二气源用于提供Ar;The second air inlet pipe (9) is provided with an opening and closing valve, the opening and closing valve is used to connect a second air source, and the second air source is used to provide Ar;
    所述第一进气管(7)上设有多通阀,所述多通阀用于连接第一气源,所述第一气源用于提供Cl 2、O 2、He、D 2和/或Ar; The first air inlet pipe (7) is provided with a multi-way valve, the multi-way valve is used to connect a first air source, and the first air source is used to provide Cl 2 , O 2 , He, D 2 and/ Or Ar;
    所述控制系统与所述启闭阀和所述多通阀相连,并用于通过控制启闭阀以控制Ar进入第二进气管(9),以及通过控制所述多通阀以控制进入第一进气管(7)的气体种类。The control system is connected to the opening and closing valve and the multi-way valve, and is used to control the opening and closing valve to control Ar to enter the second intake pipe (9), and to control the multi-way valve to control the access to the first intake pipe (9). The gas type of the intake pipe (7).
  5. 如权利要求3所述的光纤预制棒疏松体的烧结装置,其特征在于,所述压力测量机构(14)包括:The sintering device for the loose body of the optical fiber preform according to claim 3, wherein the pressure measuring mechanism (14) comprises:
    分设于第一进气管(7)和第二进气管(9)上的第一压力传感器(140)和第二压力传感器(141),所述第一压力传感器(140)和第二压力传感器(141)分别用于测量所述炉心管(2)以及烧结箱体(1)进气时所述炉心管(2)和烧结箱体(1)内的压力;The first pressure sensor (140) and the second pressure sensor (141) are separately arranged on the first intake pipe (7) and the second intake pipe (9). The first pressure sensor (140) and the second pressure sensor ( 141) respectively used to measure the pressure in the furnace core tube (2) and the sintering box body (1) when the furnace core tube (2) and the sintering box body (1) are fed;
    以及,分设于第一排气管(8)和第二排气管(10)上的第三压力传感器(142)和第四压力传感器(143),所述第三压力传感器(142)和第四压力传感器(143)分别用于测量所述炉心管(2)以及烧结箱体(1)抽真空时所述炉心管(2)和烧结箱体(1)内的压力。And, a third pressure sensor (142) and a fourth pressure sensor (143) separately provided on the first exhaust pipe (8) and the second exhaust pipe (10), the third pressure sensor (142) and the second Four pressure sensors (143) are respectively used to measure the pressure in the furnace core tube (2) and the sintering box (1) when the furnace core tube (2) and the sintering box (1) are evacuated.
  6. 一种光纤预制棒疏松体的烧结方法,其特征在于,包括如下步骤:A method for sintering a loose body of an optical fiber preform, which is characterized in that it comprises the following steps:
    提供如权利要求1至5任一所述的烧结装置,并将预制棒疏松体(5)连接于所述引杆(4)上;Provide a sintering device according to any one of claims 1 to 5, and connect the preform loose body (5) to the lead rod (4);
    通过负压机构(11),经所述第一排气管(8)将炉心管(2)抽至预设的第一负压,经所述第二排气管(10)将所述烧结箱体(1)抽至炉心管(2)内外压差位于预设的第一压力范围内;Through the negative pressure mechanism (11), the furnace core tube (2) is pumped to a preset first negative pressure through the first exhaust pipe (8), and the sintered tube is sintered through the second exhaust pipe (10). The box body (1) is pumped to the furnace core tube (2) where the pressure difference between inside and outside is within the preset first pressure range;
    将所述加热组件(3)升温至预设的脱羟温度,通过所述第一进气管(7)向所述炉心管(2)内通入Cl 2、O 2和He,通过所述第二进气管(9)向所述烧结箱体(1)内通入Ar,并使所述炉心管(2)内外压差位于预设的第二压力范围内; The heating assembly (3) is heated to a preset dehydroxylation temperature, and Cl 2 , O 2 and He are introduced into the furnace core tube (2) through the first air inlet pipe (7), and pass through the first gas inlet pipe (7). Two air inlet pipes (9) pass Ar into the sintering box (1), and make the pressure difference between the inside and outside of the furnace core pipe (2) be within a preset second pressure range;
    移动预制棒疏松体(5),使所述预制棒疏松体(5)逐步经过所述加热区(A),并完成整个预制棒疏松体(5)的脱羟;Move the preform loose body (5) so that the preform loose body (5) gradually passes through the heating zone (A), and completes the dehydroxylation of the entire preform loose body (5);
    将所述炉心管(2)抽至预设的第二负压,同时将烧结箱体(1)抽至炉心管(2)内外压差位于预设的第三压力范围内,脱除预制棒疏松体(5)内残余气体;The furnace core tube (2) is pumped to the preset second negative pressure, while the sintering box (1) is pumped to the furnace core tube (2) where the pressure difference between the inside and outside of the furnace core tube (2) is within the preset third pressure range, and the preform is removed Residual gas in the loose body (5);
    将所述加热组件(3)升温至预设的玻璃化烧结温度,在所述第二负压下,移动预制棒疏松体(5),直至完成整个预制棒疏松体(5)的烧结;The heating assembly (3) is heated to a preset vitrification and sintering temperature, and the preform loose body (5) is moved under the second negative pressure until the sintering of the entire preform loose body (5) is completed;
    降温至预设温度,向所述炉心管(2)内通入D 2和Ar,直至达到第三负压,同时向所述烧结箱体(1)内通入Ar,直至所述炉心管(2)内外压力差位于预设的第四压力范围内,进行氘化处理,得到光纤预制棒。 Cool down to a preset temperature, pass D 2 and Ar into the furnace core tube (2) until the third negative pressure is reached, and at the same time pass Ar into the sintering box (1) until the furnace core tube ( 2) The internal and external pressure difference is within the preset fourth pressure range, and the deuteration process is performed to obtain the optical fiber preform.
  7. 如权利要求6所述的光纤预制棒疏松体的烧结方法,其特征在于,还包括如下步骤:The method for sintering the loose body of the optical fiber preform according to claim 6, further comprising the following steps:
    排走所述炉心管(2)内的D 2和Ar,以及烧结箱体(1)内的Ar; Drain the D 2 and Ar in the furnace core tube (2) and the Ar in the sintering box (1);
    向所述炉心管(2)及烧结箱体(1)内通入Ar,直至压力达到大气压时,取出光纤预制棒。Ar is introduced into the furnace core tube (2) and the sintering box (1) until the pressure reaches the atmospheric pressure, and then the optical fiber preform is taken out.
  8. 如权利要求6所述的光纤预制棒疏松体的烧结方法,其特征在于,在升温至预设的脱羟温度之前,还包括如下步骤:7. The method for sintering the loose body of the optical fiber preform according to claim 6, characterized in that, before raising the temperature to the preset dehydroxylation temperature, the method further comprises the following steps:
    驱动引杆(4)以使所述预制棒疏松体(5)顶端或底端位于加热区(A)内。The leading rod (4) is driven to make the top or bottom end of the preform loose body (5) located in the heating zone (A).
  9. 如权利要求6所述的光纤预制棒疏松体的烧结方法,其特征在于:所述Cl 2、O 2和He的流量依次为0.5~1.5L/min、0.6~1.2L/min和15~25L/min。 The method for sintering the loose body of an optical fiber preform according to claim 6, wherein the flow rates of Cl 2 , O 2 and He are 0.5 to 1.5 L/min, 0.6 to 1.2 L/min, and 15 to 25 L, respectively. /min.
  10. 如权利要求6所述的光纤预制棒疏松体的烧结方法,其特征在于:第一压力范围、第二压力范围、第三压力范围和第四压力范围均为-1~1mbar。The method for sintering the loose body of the optical fiber preform according to claim 6, wherein the first pressure range, the second pressure range, the third pressure range and the fourth pressure range are all -1 to 1 mbar.
PCT/CN2020/115863 2020-03-17 2020-09-17 Sintering device and sintering method for optical fiber preform soot body WO2021184713A1 (en)

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