WO2021184713A1 - 一种光纤预制棒疏松体的烧结装置及烧结方法 - Google Patents

一种光纤预制棒疏松体的烧结装置及烧结方法 Download PDF

Info

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
Authority
WO
WIPO (PCT)
Prior art keywords
sintering
furnace core
core tube
pressure
optical fiber
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2020/115863
Other languages
English (en)
French (fr)
Inventor
崔东明
孔明
伍淑坚
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Fiberhome Ruituo Technologies Co Ltd
Fiberhome Telecommunication Technologies Co Ltd
Original Assignee
Wuhan Fiberhome Ruituo Technologies Co Ltd
Fiberhome Telecommunication Technologies Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuhan Fiberhome Ruituo Technologies Co Ltd, Fiberhome Telecommunication Technologies Co Ltd filed Critical Wuhan Fiberhome Ruituo Technologies Co Ltd
Publication of WO2021184713A1 publication Critical patent/WO2021184713A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture 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]
    • C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C03B37/0146—Furnaces therefor, e.g. muffle tubes, furnace linings
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving 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.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Thermal Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)

Abstract

本申请涉及光纤预制棒疏松体的烧结装置及烧结方法，其包括烧结箱体、炉心管、加热组件、引杆、送棒机构、第一管组、第二管组；炉心管、加热组件组设于烧结箱体内，加热组件形成加热区；引杆伸至炉心管内并用于连接预制棒疏松体；送棒机构与引杆相连，用于驱动引杆移动，以使预制棒疏松体在加热区内加热；第一管组贯穿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；第二管组贯穿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。本申请集脱羟、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。

Description

一种光纤预制棒疏松体的烧结装置及烧结方法 技术领域
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。
背景技术
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。
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。
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。
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。
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。
发明内容
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。
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：
烧结箱体；
炉心管，其组设于所述烧结箱体内；
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；
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；
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；
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；
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。
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。
在一些实施例中，所述烧结装置还包括：
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；
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。
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；
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；
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。
在一些实施例中，所述压力测量机构包括：
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；
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。
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：
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；
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；
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；
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；
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；
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；
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。
在一些实施例中，还包括如下步骤：
排走所述炉心管内的D 2和Ar，以及烧结箱体内的Ar；
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。
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：
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。
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。
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。
本申请提供的技术方案带来的有益效果包括：
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。
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。
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。
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。
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。
附图说明
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。
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。
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。
具体实施方式
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。
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。
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。
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；
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。
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。
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。
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。
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。
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。
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。
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。
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。
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。
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。
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；
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。
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。
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。
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。
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。
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：
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；
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；
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℃。
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。
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；
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。
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。
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，
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。
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。
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。
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。
具体实施例：
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。
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。
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。
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。

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：
    烧结箱体(1)；
    炉心管(2)，其组设于所述烧结箱体(1)内；
    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)；
    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)；
    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；
    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)；
    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)。
  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。
  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：
    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；
    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。
  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：
    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；
    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；
    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。
  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：
    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；
    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。
  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：
    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；
    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；
    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；
    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；
    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；
    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；
    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。
  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：
    排走所述炉心管(2)内的D 2和Ar，以及烧结箱体(1)内的Ar；
    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。
  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：
    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。
  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。
  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。
PCT/CN2020/115863 2020-03-17 2020-09-17 一种光纤预制棒疏松体的烧结装置及烧结方法 Ceased WO2021184713A1 (zh)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN202010188691.8A CN111423106A (zh) 2020-03-17 2020-03-17 一种光纤预制棒疏松体的烧结装置及烧结方法
CN202010188691.8 2020-03-17

Publications (1)

Publication Number Publication Date
WO2021184713A1 true WO2021184713A1 (zh) 2021-09-23

Family

ID=71548293

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2020/115863 Ceased WO2021184713A1 (zh) 2020-03-17 2020-09-17 一种光纤预制棒疏松体的烧结装置及烧结方法

Country Status (2)

Country Link
CN (1) CN111423106A (zh)
WO (1) WO2021184713A1 (zh)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113908771A (zh) * 2021-10-15 2022-01-11 中国科学技术大学 一种基于连续分子束源的低压闪热解流动管反应装置
CN115536264A (zh) * 2022-09-27 2022-12-30 浙江富通光纤技术有限公司 一种光纤预制棒烧结工艺自动化供气装置及其控制方法
CN115947537A (zh) * 2022-12-24 2023-04-11 藤仓烽火光电材料科技有限公司 一种石英芯棒的表面处理装置及表面处理方法
CN117486483A (zh) * 2023-10-31 2024-02-02 中国建筑材料科学研究总院有限公司 一种低缺陷的光纤面板及其制备方法和应用

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111423106A (zh) * 2020-03-17 2020-07-17 烽火通信科技股份有限公司 一种光纤预制棒疏松体的烧结装置及烧结方法
CN112624600B (zh) * 2021-01-12 2023-06-23 江苏法尔胜光子有限公司 一种光纤预制棒制备用烧结炉抽风罩及抽风压力在线调节方法
CN113105111A (zh) * 2021-05-28 2021-07-13 通鼎互联信息股份有限公司 一种低氦预制棒外包烧结装置及其方法
CN113248132B (zh) * 2021-07-08 2021-09-21 藤仓烽火光电材料科技有限公司 一种用于生产光纤预制棒的加热炉系统及其加热方法
CN118598501B (zh) * 2024-08-08 2024-11-15 江苏亨通光导新材料有限公司 一种低水峰光纤预制棒无氦烧结装置及其使用方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781087A (zh) * 2010-02-09 2010-07-21 中天科技精密材料有限公司 一种疏松体光纤预制棒一体化烧结脱气的设备及其方法
CN105669019A (zh) * 2016-04-19 2016-06-15 江苏亨通光导新材料有限公司 光纤预制棒的制造装置及其制造方法
CN107540209A (zh) * 2017-10-25 2018-01-05 江苏亨通光导新材料有限公司 一种光纤预制棒母棒的烧结装置及对应的烧结方法
CN109502962A (zh) * 2018-12-28 2019-03-22 通鼎互联信息股份有限公司 一种光纤预制棒的烧结装置及烧结方法
CN111423106A (zh) * 2020-03-17 2020-07-17 烽火通信科技股份有限公司 一种光纤预制棒疏松体的烧结装置及烧结方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101781087A (zh) * 2010-02-09 2010-07-21 中天科技精密材料有限公司 一种疏松体光纤预制棒一体化烧结脱气的设备及其方法
CN105669019A (zh) * 2016-04-19 2016-06-15 江苏亨通光导新材料有限公司 光纤预制棒的制造装置及其制造方法
CN107540209A (zh) * 2017-10-25 2018-01-05 江苏亨通光导新材料有限公司 一种光纤预制棒母棒的烧结装置及对应的烧结方法
CN109502962A (zh) * 2018-12-28 2019-03-22 通鼎互联信息股份有限公司 一种光纤预制棒的烧结装置及烧结方法
CN111423106A (zh) * 2020-03-17 2020-07-17 烽火通信科技股份有限公司 一种光纤预制棒疏松体的烧结装置及烧结方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113908771A (zh) * 2021-10-15 2022-01-11 中国科学技术大学 一种基于连续分子束源的低压闪热解流动管反应装置
CN113908771B (zh) * 2021-10-15 2022-07-15 中国科学技术大学 一种基于连续分子束源的低压闪热解流动管反应装置
CN115536264A (zh) * 2022-09-27 2022-12-30 浙江富通光纤技术有限公司 一种光纤预制棒烧结工艺自动化供气装置及其控制方法
CN115536264B (zh) * 2022-09-27 2023-12-08 浙江富通光纤技术有限公司 一种光纤预制棒烧结工艺自动化供气装置及其控制方法
CN115947537A (zh) * 2022-12-24 2023-04-11 藤仓烽火光电材料科技有限公司 一种石英芯棒的表面处理装置及表面处理方法
CN117486483A (zh) * 2023-10-31 2024-02-02 中国建筑材料科学研究总院有限公司 一种低缺陷的光纤面板及其制备方法和应用

Also Published As

Publication number Publication date
CN111423106A (zh) 2020-07-17

Similar Documents

Publication Publication Date Title
WO2021184713A1 (zh) 一种光纤预制棒疏松体的烧结装置及烧结方法
CN101781087B (zh) 一种疏松体光纤预制棒一体化烧结脱气的设备及其方法
JP4159247B2 (ja) 光ファイバの予成形体の製造方法及びその装置
CN105669019B (zh) 光纤预制棒的制造装置及其制造方法
CN112876044B (zh) 高纯度低羟基高均匀性石英玻璃的化学沉积方法及装置
US11554978B2 (en) Method for reducing processing time for optical fiber preforms
CN207512075U (zh) 分段式光纤预制棒烧结炉装置
CN104788014B (zh) 一种光纤预制棒制备及光纤拉丝的方法
WO2018036142A1 (zh) 一种光纤预制棒套管烧结装置及其烧结方法
CN105753311A (zh) 一种光纤预制棒的脱气装置及方法
CN113105111A (zh) 一种低氦预制棒外包烧结装置及其方法
CN113860722B (zh) 光纤预制棒制造设备及方法
US20200031706A1 (en) Method and apparatus for drying and consolidating a preform for optical fibres
CN205616787U (zh) 光纤预制棒的制造装置
CN221397697U (zh) 一种粉棒加热玻璃化装置
CN118812155A (zh) 一种光纤预制棒烧结设备及方法
CN113277716B (zh) 一种生产高品质合成石英玻璃的设备
CN211999485U (zh) 双层真空脱羟退火装置
CN119019088B (zh) 一种光纤预制棒的烧结装置和烧结方法
CN214937032U (zh) 一种低氦预制棒外包烧结装置
CN207418597U (zh) 一种光纤预制棒母棒的烧结装置
CN223047420U (zh) 一种低水峰光纤预制棒无氦烧结装置
CN211946808U (zh) Vad疏松体脱水烧结装置
CN121717552A (zh) 一种大尺寸光纤预制棒包层脱水烧结装置及方法
CN212199012U (zh) 一种vad烧结炉芯管的气封装置

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 20925262

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 20925262

Country of ref document: EP

Kind code of ref document: A1