WO2018036142A1 - Sintering device with casing tube for optical fibre preform rod and sintering method therefor - Google Patents

Sintering device with casing tube for optical fibre preform rod and sintering method therefor Download PDF

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Publication number
WO2018036142A1
WO2018036142A1 PCT/CN2017/077199 CN2017077199W WO2018036142A1 WO 2018036142 A1 WO2018036142 A1 WO 2018036142A1 CN 2017077199 W CN2017077199 W CN 2017077199W WO 2018036142 A1 WO2018036142 A1 WO 2018036142A1
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Prior art keywords
sleeve
optical fiber
fiber preform
sintering
fixing device
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PCT/CN2017/077199
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French (fr)
Chinese (zh)
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冯程
肖华
杜森
劳雪刚
马康库
柏文俊
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江苏亨通光导新材料有限公司
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Priority to RU2018107936A priority Critical patent/RU2018107936A/en
Publication of WO2018036142A1 publication Critical patent/WO2018036142A1/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
    • C03B37/01205Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01225Means for changing or stabilising the shape, e.g. diameter, of tubes or rods in general, e.g. collapsing
    • C03B37/01248Means for changing or stabilising the shape, e.g. diameter, of tubes or rods in general, e.g. collapsing by collapsing without drawing
    • 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]
    • 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]
    • C03B37/018Manufacture 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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • C03B37/01853Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • 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
    • 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]
    • C03B37/018Manufacture 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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
    • 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 present invention relates to the field of optical fiber preform manufacturing, and in particular to an optical fiber preform sleeve sintering device and a sintering method thereof.
  • the large-scale optical fiber preform production process in the field is mainly deposited by VAD and OVD processes to form a loose body.
  • VAD, OVD process that is, the preform is made by vapor deposition.
  • the SiO 2 granules are produced in the combustion chamber by introducing the raw materials into a flame, and are deposited on a preset target rod or a middle rod to form a loose body.
  • the loose body is formed by the VAD and OVD processes, it is placed in a sintering furnace and sintered under high temperature to form a vitrified preform.
  • the finished preform is drawn to obtain a finished fiber or melt-shrinked using a quartz sleeve of the same grade as the fiber material to produce a larger-sized optical fiber preform.
  • the sintering process must prevent moisture and other impurities such as various metallic impurities from entering the preform.
  • moisture and other impurities such as various metallic impurities
  • the attenuation of the optical fiber made by the preform in a large wavelength range will greatly increase, resulting in product failure.
  • the loose body In order to prevent the moisture contained in the loose body from adversely affecting the quality of the product, the loose body must be dehydrated before the loose body is vitrified to form a transparent preform.
  • a common method of dehydration is to remove the hydroxyl and moisture in the loose body by physical and chemical action by heating the loose body to a high temperature of 1100 ° C to 1300 ° C in an inert gas atmosphere containing Cl 2 or other chlorine-based desiccant. .
  • the loose body After the loose body is dehydrated, it is placed in an inert gas atmosphere such as He or Ar, and heated to 1450 ° C or higher. Under these conditions, the loose body vitrified to form a transparent quartz preform.
  • an inert gas atmosphere such as He or Ar
  • the loose process in the process of dewatering and sintering of loose bodies, the loose process must be placed in a closed environment to provide a corresponding atmosphere for dehydration and complete transparency, while avoiding Foreign matter enters it.
  • the sealing environment is generally provided by installing a furnace tube in a heating furnace, and the loose body is placed in the furnace core tube, and various process gases are introduced under high temperature conditions for dehydration and sintering.
  • Chinese patent CN101426742B "Method for manufacturing optical fiber preform" invents a loose body sintering method.
  • the loose body is suspended in a furnace tube having a heating zone.
  • the loose body is passed through the heating zone from bottom to top, and a chlorine-based gas and an inert gas are introduced for dehydration.
  • a chlorine-based gas and an inert gas are introduced for dehydration.
  • the loose body is moved to the lower side of the heating zone, the heating zone is heated to the sintering temperature, and an inert gas is introduced, and then the loose body passes through the heating zone from bottom to top to completely transparently vitrify.
  • This method is similar to other conventional methods in that a furnace tube made of quartz material is used. Its originality is mainly to improve the uniformity of product quality, to avoid the impurities in the furnace core tube from entering the interior of the preform during the dehydration and sintering process, and to take the loose body from the bottom to the top through the heating zone during the dehydration and sintering process.
  • a dehydration atmosphere is provided by 10% chlorine gas and 90% helium gas, 100% helium gas provides a sintering atmosphere, and an optical fiber made of an optical fiber preform manufactured at a suitable dehydration temperature and a sintering temperature has good attenuation. Level.
  • Chinese Patent CN102992611B "Method for Producing Glass Base Material” invents a manufacturing method for providing a closed environment by a furnace tube made of carbon material.
  • the optical fiber produced by this method shows good attenuation performance.
  • the above method is to increase the necessity of dehydration and sintering conditions by adding a high-purity material furnace tube to the sintering furnace.
  • the residual stress of the quartz material furnace tube during the heat treatment process is prone to cracking during the processing, transportation, storage and use, resulting in scrapping.
  • the furnace tube is devitrified, and if the temperature is restored to a low temperature, cracking will occur.
  • the carbon material furnace tube itself is easily contaminated by external conditions. If it is in contact with the atmosphere, the furnace tube itself Will be oxidized. Higher requirements are placed on the airtightness of the equipment. In addition, when the loose body is placed from the atmospheric environment into the furnace tube, oxygen is inevitably entered into it, and long-term use will inevitably lead to aging of the furnace tube and affect product performance.
  • the invention aims to provide an optical fiber preform sleeve sintering device and a sintering method thereof, which can effectively reduce equipment complexity, reduce equipment space occupation, reduce production cost, and facilitate large-scale mass production.
  • the technical solution of the present invention is:
  • the upper fixing device and the lower fixing device are driven by a rotating mechanism, and the two are synchronously rotatable.
  • the furnace consists of one or more heating elements disposed on the casing The outside.
  • the sleeve is a quartz sleeve.
  • the step S3 specifically includes:
  • Heating the furnace to 1100 ° C ⁇ 1300 ° C, and moving back and forth 1 or more times in the vertical direction;
  • the desiccant and the process gas are introduced into the casing by the air inlet mechanism; the passage of the exhaust system and the exhaust mechanism is opened through the valve switch, and the pressure in the casing is maintained at an appropriate level to provide a dehydration atmosphere environment.
  • the process gas is one or more of chlorine gas, helium gas and nitrogen gas.
  • the sleeve is a quartz sleeve.
  • the present invention at least includes the following beneficial effects:
  • the optical fiber preform sleeve sintering device and the sintering method thereof of the invention use the casing vacuum method to sinter the optical fiber preform loose body, thereby avoiding the use of expensive and easy to damage furnace core tube, which can be manufactured Large size loose body.
  • the vacuum environment is beneficial to improve the quality of the preform, speed up the sintering and increase the production efficiency.
  • the furnace-free tube sintering method is adopted to reduce the production cost, reduce the complexity of the equipment, reduce the space occupation of the equipment, and is advantageous for mass production.
  • FIG. 1 is a schematic structural view of an optical fiber preform sleeve sintering device according to the present invention
  • FIG. 2 is a schematic view showing the process of sintering and shrinking the upper portion of the optical fiber preform sleeve sintering device according to the present invention.
  • Figure 3 is a temperature distribution diagram of the center of the heating furnace
  • Figure 4 is a temperature distribution diagram of the center of the furnace in the melting stage.
  • an optical fiber preform sleeve sintering device includes a sleeve 3, an upper fixing device 1, a lower fixing device 6, and a heating furnace 5, wherein the sleeve 3 Installed in the heating furnace 5 in a vertical manner by the upper fixing device 1 and the lower fixing device 6, an optical fiber preform loose body 4 is disposed in the sleeve 3 and realized with the upper fixing device 1
  • the upper fixing device 1 is provided with an exhausting mechanism 2
  • the exhausting mechanism 2 is connected to the exhaust system and the vacuum pump through a valve switch
  • the lower fixing device 6 is provided with an air intake mechanism 7.
  • the upper fixing device 1 and the lower fixing device 6 are driven by a rotating mechanism, Can rotate synchronously.
  • the optical fiber preform loose body 4 is connected to the upper fixing device 1 via a connecting mechanism 8.
  • the furnace 5 consists of one or more heating elements which are arranged outside the sleeve 3.
  • the sleeve 3 is a quartz sleeve 3.
  • the sintering device uses the casing 3 vacuuming method to sinter the optical fiber preform loose body 4, thereby avoiding the use of expensive and easily damaged furnace core tubes, and can prepare large-sized loose bodies.
  • the vacuum environment is beneficial to improve the quality of the preform, speed up the sintering and increase the production efficiency.
  • the sintering method of the optical fiber preform sleeve sintering device according to Embodiment 1 includes the following steps:
  • the sleeve 3 is vertically installed in the heating furnace 5 through the upper fixing device 1 and the lower fixing device 6;
  • the step S3 specifically includes:
  • the desiccant and the process gas are introduced into the casing 3 by the air inlet mechanism 7; the passage of the exhaust system and the exhaust mechanism 2 is opened through the valve switch, and the pressure in the casing 3 is maintained within a range of 10 to 40 Pa to provide dehydration. Atmosphere.
  • the method of moving the heating furnace 5 greatly reduces the size of the equipment, reduces the amount of gas, and reduces the production cost.
  • the sleeve 3 When sintering, the sleeve 3 is melted to form a part of the product, and the preform size is increased, which is advantageous for improving production efficiency.
  • the furnaceless tube sintering method is adopted to reduce the production cost, and a large-sized loose body can be prepared. Reducing the complexity of the equipment and reducing the space occupied by the equipment is conducive to large-scale mass production. Sintering the loose body under vacuuming conditions is advantageous for eliminating bubbles, speeding up the sintering speed, and improving the sintering efficiency.

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

Abstract

A sintering device with a casing tube for an optical fibre preform rod, comprising a casing tube, an upper fixing means, a lower fixing means and a heating furnace, wherein the casing tube is installed vertically in a heating furnace by means of the upper fixing means and the lower fixing means, and a loose body of the optical fibre preform is arranged in the casing tube and connected to the upper fixing means; and an exhaust mechanism is arranged on the upper fixing means, the exhaust mechanism being connected to an exhaust system and a vacuum pump through a valve switch, and a gas inlet mechanism is arranged on the lower fixing means. A sintering method comprises sintering a loose body of the optical fibre preform using a casing tube evacuation method, with the use of furnace core tubes that are expensive and easy to be damaged being avoided, and can prepare a large-size loose body.

Description

一种光纤预制棒套管烧结装置及其烧结方法Optical fiber preform sleeve sintering device and sintering method thereof 技术领域Technical field
本发明涉及光纤预制棒制造领域,具体地是涉及一种光纤预制棒套管烧结装置及其烧结方法。The present invention relates to the field of optical fiber preform manufacturing, and in particular to an optical fiber preform sleeve sintering device and a sintering method thereof.
背景技术Background technique
本领域中大尺寸光纤预制棒生产工艺主要通过VAD,OVD工艺沉积形成松散体。所谓的VAD、OVD工艺,即是利用气相沉积的方法制成预制棒。通过将原料导入火焰中,在燃烧室内生产SiO2颗粒体,并沉积到预置的目标靶棒或者中棒上制成松散体。通过VAD、OVD工艺制成松散体以后,再将其置于烧结炉中,高温条件下烧结形成玻璃化预制棒。将制成的预制棒拉制成得到成品光纤或使用与光纤材料同等级别的石英套管对其进行熔缩外包制造更大尺寸的光纤预制棒。The large-scale optical fiber preform production process in the field is mainly deposited by VAD and OVD processes to form a loose body. The so-called VAD, OVD process, that is, the preform is made by vapor deposition. The SiO 2 granules are produced in the combustion chamber by introducing the raw materials into a flame, and are deposited on a preset target rod or a middle rod to form a loose body. After the loose body is formed by the VAD and OVD processes, it is placed in a sintering furnace and sintered under high temperature to form a vitrified preform. The finished preform is drawn to obtain a finished fiber or melt-shrinked using a quartz sleeve of the same grade as the fiber material to produce a larger-sized optical fiber preform.
对于通过VAD、OVD或者VAD和OVD混合工艺制成的松散体,其烧结过程必须防止水分以及其他杂质诸如各种金属杂质进入预制棒中。一般情况下,若1ppb以上的水分或金属杂质在烧结过程中进入到光纤预制棒中,该预制棒所制成的光纤在很大的波长范围内衰减将大大增加从而导致产品不合格。为了防止松散体中含有的水分对产品质量造成不良影响,在松散体玻璃化形成透明预制棒之前,必须对松散体进行脱水。常见的脱水方法是在包含Cl2或其他氯基干燥剂的惰性气体环境中将松散体加热至1100℃~1300℃的高温条件下,通过物理以及化学作用,将松散体中的羟基以及水分去除。For loose bodies made by VAD, OVD or VAD and OVD mixing processes, the sintering process must prevent moisture and other impurities such as various metallic impurities from entering the preform. In general, if more than 1 ppb of moisture or metal impurities enter the optical fiber preform during the sintering process, the attenuation of the optical fiber made by the preform in a large wavelength range will greatly increase, resulting in product failure. In order to prevent the moisture contained in the loose body from adversely affecting the quality of the product, the loose body must be dehydrated before the loose body is vitrified to form a transparent preform. A common method of dehydration is to remove the hydroxyl and moisture in the loose body by physical and chemical action by heating the loose body to a high temperature of 1100 ° C to 1300 ° C in an inert gas atmosphere containing Cl 2 or other chlorine-based desiccant. .
松散体脱水完毕后,置于He、Ar等惰性气体环境中,同时加热至1450℃以上。在此条件下松散体玻璃化形成透明的石英预制棒。After the loose body is dehydrated, it is placed in an inert gas atmosphere such as He or Ar, and heated to 1450 ° C or higher. Under these conditions, the loose body vitrified to form a transparent quartz preform.
显而易见,常见工艺在松散体的脱水以及烧结过程中,必须将松散体置于一个密闭环境下,为其脱水和完全透明化提供相应的气氛环境,同时避免 外界杂质进入其中。一般通过在加热炉中安装炉芯管来提供密封环境,将松散体置于炉芯管中,在高温条件下通入各种工艺气体,进行脱水和烧结。Obviously, in the process of dewatering and sintering of loose bodies, the loose process must be placed in a closed environment to provide a corresponding atmosphere for dehydration and complete transparency, while avoiding Foreign matter enters it. The sealing environment is generally provided by installing a furnace tube in a heating furnace, and the loose body is placed in the furnace core tube, and various process gases are introduced under high temperature conditions for dehydration and sintering.
中国专利CN101426742B《光纤母材制造方法》发明了一种松散体烧结方法。将松散体悬挂在具备加热区域的炉芯管中。使松散体自下而上穿过加热区,同时通入氯基气体以及惰性气体进行脱水。脱水结束后将松散体移动至加热区下方,将加热区加热至烧结温度,并通入惰性气体,再将松散体自下而上通过加热区,使其完全透明玻璃化。Chinese patent CN101426742B "Method for manufacturing optical fiber preform" invents a loose body sintering method. The loose body is suspended in a furnace tube having a heating zone. The loose body is passed through the heating zone from bottom to top, and a chlorine-based gas and an inert gas are introduced for dehydration. After the dehydration is finished, the loose body is moved to the lower side of the heating zone, the heating zone is heated to the sintering temperature, and an inert gas is introduced, and then the loose body passes through the heating zone from bottom to top to completely transparently vitrify.
该方法与其他传统方法类似,使用石英材料制成的炉芯管。其独创性主要在于为了提高产品质量均匀性,避免炉芯管中的杂质在脱水烧结过程中进入预制棒内部而在脱水、烧结过程中采取了将松散体自下而上通过加热区。根据该方法,由10%的氯气及90%的氦气提供脱水气氛,100%氦气提供烧结气氛,并在合适的脱水温度以及烧结温度下制造的光纤预制棒制成的光纤具有良好的衰减水平。This method is similar to other conventional methods in that a furnace tube made of quartz material is used. Its originality is mainly to improve the uniformity of product quality, to avoid the impurities in the furnace core tube from entering the interior of the preform during the dehydration and sintering process, and to take the loose body from the bottom to the top through the heating zone during the dehydration and sintering process. According to this method, a dehydration atmosphere is provided by 10% chlorine gas and 90% helium gas, 100% helium gas provides a sintering atmosphere, and an optical fiber made of an optical fiber preform manufactured at a suitable dehydration temperature and a sintering temperature has good attenuation. Level.
中国专利CN102992611B《玻璃母材的制造方法》发明了以一种以碳材质制成的炉芯管提供密闭环境的制造方法。通过该方法制成的光纤显示出了良好的衰减性能。Chinese Patent CN102992611B "Method for Producing Glass Base Material" invents a manufacturing method for providing a closed environment by a furnace tube made of carbon material. The optical fiber produced by this method shows good attenuation performance.
诸如上述方法,均是通过在烧结炉中增加一个高纯度材质炉芯管来满足必要的脱水、烧结条件。For example, the above method is to increase the necessity of dehydration and sintering conditions by adding a high-purity material furnace tube to the sintering furnace.
高纯度的材料等级要求导致了昂贵的材料成本。尺寸越大的炉芯管加工难度越大,加工设备更为复杂,大大增加了制造成本。High purity material grade requirements result in expensive material costs. The larger the size of the furnace tube, the more difficult it is to process, and the processing equipment is more complicated, which greatly increases the manufacturing cost.
制造石英材质炉芯管在热处理过程残留应力,在加工过程、运输过程、保管以及使用过程中容易发生破裂从而导致报废。另外,由于石英本身特有的材质特点决定了炉芯管一旦升温至1100℃以上,炉芯管出现析晶现象,如果将温度恢复至低温将发生破裂。The residual stress of the quartz material furnace tube during the heat treatment process is prone to cracking during the processing, transportation, storage and use, resulting in scrapping. In addition, due to the unique material characteristics of the quartz itself, once the furnace tube is heated to above 1100 °C, the furnace tube is devitrified, and if the temperature is restored to a low temperature, cracking will occur.
碳材质炉芯管本身容易受到外界条件污染。若与大气接触,炉芯管本身 将被氧化。对设备的气密性提出了较高要求。另外,将松散体从大气环境中放置到炉芯管中时,不可避免的会导致氧气进入其中,长时间使用必将导致炉芯管老化而影响产品性能。The carbon material furnace tube itself is easily contaminated by external conditions. If it is in contact with the atmosphere, the furnace tube itself Will be oxidized. Higher requirements are placed on the airtightness of the equipment. In addition, when the loose body is placed from the atmospheric environment into the furnace tube, oxygen is inevitably entered into it, and long-term use will inevitably lead to aging of the furnace tube and affect product performance.
另一个至关重要的不足之处在于,由于石英、碳等材质的石英管本身材料的局限性导致了传统的工艺方法一般将炉芯管,加热区固定而采用将松散体穿过加热区完成烧结。由此造成了炉芯管的长度一般大于两倍的松散体长度。显而易见,这不仅大大增加了设备的复杂程度、设备占用空间大小,而且为了达到优选的脱水,完全透明化气氛条件,大大增加了各类工艺气体,特别是价格非常昂贵的、属于不可再生资源的氦气使用量,从而大大增加了光纤预制棒的制造成本。Another crucial shortcoming is that due to the limitations of the material of the quartz tube, such as quartz and carbon, the traditional process generally fixes the furnace tube and the heating zone and uses the loose body to complete the heating zone. sintering. As a result, the length of the furnace tube is generally greater than twice the length of the loose body. Obviously, this not only greatly increases the complexity of the equipment, the size of the equipment, but also achieves the perfect dehydration, completely transparent atmosphere conditions, greatly increasing the various process gases, especially the very expensive, non-renewable resources. The amount of helium used, which greatly increases the manufacturing cost of the optical fiber preform.
因此,本发明的发明人亟需构思一种新技术以改善其问题。Therefore, the inventors of the present invention need to conceive a new technique to improve the problem.
发明内容Summary of the invention
本发明旨在提供一种光纤预制棒套管烧结装置及其烧结方法,其可以有效降低设备复杂程度,降低设备空间占用程度,降低生产成本,有利于大规模批量生产。The invention aims to provide an optical fiber preform sleeve sintering device and a sintering method thereof, which can effectively reduce equipment complexity, reduce equipment space occupation, reduce production cost, and facilitate large-scale mass production.
为解决上述技术问题,本发明的技术方案是:In order to solve the above technical problem, the technical solution of the present invention is:
一种光纤预制棒套管烧结装置,包括套管、上固定装置、下固定装置、加热炉,其中所述套管通过所述上固定装置和所述下固定装置以垂直方式安装在所述加热炉中,一光纤预制棒松散体设置在所述套管内并与所述上固定装置实现连接;所述上固定装置上设有一排气机构,所述排气机构通过阀门开关与排气系统和真空泵相连,所述下固定装置上设有一进气机构。An optical fiber preform sleeve sintering device comprising a sleeve, an upper fixing device, a lower fixing device, and a heating furnace, wherein the sleeve is vertically mounted on the heating by the upper fixing device and the lower fixing device In the furnace, an optical fiber preform loose body is disposed in the sleeve and connected to the upper fixing device; the upper fixing device is provided with an exhaust mechanism, and the exhaust mechanism passes through the valve switch and the exhaust system and A vacuum pump is connected, and the lower fixing device is provided with an air inlet mechanism.
优选地,所述上固定装置和所述下固定装置与由旋转机构驱动,二者可同步旋转。Preferably, the upper fixing device and the lower fixing device are driven by a rotating mechanism, and the two are synchronously rotatable.
优选地,所述光纤预制棒松散体通过一连接机构与所述上固定装置连接。Preferably, the optical fiber preform loose body is connected to the upper fixing device through a connecting mechanism.
优选地,所述加热炉由一个或者多个加热元件组成,其设置在所述套管 的外侧。Preferably, the furnace consists of one or more heating elements disposed on the casing The outside.
优选地,所述套管为石英套管。Preferably, the sleeve is a quartz sleeve.
基于上述所述的光纤预制棒套管烧结装置的烧结方法,包括如下步骤:The sintering method of the optical fiber preform sleeve sintering device according to the above, comprising the following steps:
S1:将套管通过上固定装置和下固定装置以垂直方式安装在加热炉中;S1: installing the sleeve in the heating furnace through the upper fixing device and the lower fixing device in a vertical manner;
S2:将光纤预制棒松散体设置在套管内并与上固定装置实现连接;S2: disposing the optical fiber preform loose body in the sleeve and connecting with the upper fixing device;
S3:通过加热炉的升温和移动去除光纤预制棒松散体中由生产过程引入的羟基;S3: removing the hydroxyl group introduced by the production process in the bulk of the optical fiber preform by the temperature rise and movement of the heating furnace;
S4:将加热炉移动至光纤预制棒松散体的底部,升温至1450℃以上,并形成温度梯度分布;S4: moving the heating furnace to the bottom of the optical fiber preform loose body, heating up to above 1450 ° C, and forming a temperature gradient distribution;
S5:在一定的烧结温度条件下,光纤预制棒松散体下端部分完成玻璃化;S5: under a certain sintering temperature condition, the lower end portion of the loose portion of the optical fiber preform is vitrified;
S6:通过阀门开关将排气机构与真空泵联通,在套管内部形成负压;同时调整加热炉的温度分布,使套管下端熔融收缩,与玻璃化的光纤预制棒松散体融合;S6: connecting the exhaust mechanism with the vacuum pump through the valve switch to form a negative pressure inside the sleeve; adjusting the temperature distribution of the heating furnace to melt and shrink the lower end of the sleeve, and merging with the vitrified optical fiber preform;
S7:底部融合完成后,加热炉以一定的移动速度向上移动,将光纤预制棒松散体分区玻璃化。S7: After the bottom fusion is completed, the heating furnace moves upward at a certain moving speed, and the optical fiber preform loose partition is vitrified.
优选地,所述步骤S3具体包括:Preferably, the step S3 specifically includes:
将加热炉升温至1100℃~1300℃,并沿垂直方向来回移动1次或1次以上;Heating the furnace to 1100 ° C ~ 1300 ° C, and moving back and forth 1 or more times in the vertical direction;
同时由进气机构向套管内通入干燥剂和工艺气体;通过阀门开关打开排气系统与排气机构的通道,将套管内压力保持在合适的水平,提供脱水气氛环境。At the same time, the desiccant and the process gas are introduced into the casing by the air inlet mechanism; the passage of the exhaust system and the exhaust mechanism is opened through the valve switch, and the pressure in the casing is maintained at an appropriate level to provide a dehydration atmosphere environment.
优选地,所述工艺气体为给氯气、氦气、氮气中的一种或者多种。Preferably, the process gas is one or more of chlorine gas, helium gas and nitrogen gas.
优选地,所述套管为石英套管。Preferably, the sleeve is a quartz sleeve.
采用上述技术方案,本发明至少包括如下有益效果:With the above technical solutions, the present invention at least includes the following beneficial effects:
本发明所述的光纤预制棒套管烧结装置及其烧结方法,采用套管抽真空方法烧结光纤预制棒松散体,避免使用价格昂贵且易于损坏的炉芯管,可制 备大尺寸松散体。同时真空环境有利于改善预制棒质量,加快烧结速度,提高生产效率。同时采用无炉芯管烧结方法,降低生产成本,降低设备复杂程度,降低设备空间占用程度,有利于大规模批量生产。The optical fiber preform sleeve sintering device and the sintering method thereof of the invention use the casing vacuum method to sinter the optical fiber preform loose body, thereby avoiding the use of expensive and easy to damage furnace core tube, which can be manufactured Large size loose body. At the same time, the vacuum environment is beneficial to improve the quality of the preform, speed up the sintering and increase the production efficiency. At the same time, the furnace-free tube sintering method is adopted to reduce the production cost, reduce the complexity of the equipment, reduce the space occupation of the equipment, and is advantageous for mass production.
附图说明DRAWINGS
图1为本发明所述的光纤预制棒套管烧结装置的结构示意图;1 is a schematic structural view of an optical fiber preform sleeve sintering device according to the present invention;
图2为本发明所述的光纤预制棒套管烧结装置在底部融合后向上分区烧结熔缩过程的示意图。2 is a schematic view showing the process of sintering and shrinking the upper portion of the optical fiber preform sleeve sintering device according to the present invention.
图3为加热炉中心温度分布图;Figure 3 is a temperature distribution diagram of the center of the heating furnace;
图4为熔缩阶段加热炉中心温度分布图。Figure 4 is a temperature distribution diagram of the center of the furnace in the melting stage.
其中:1.上固定装置,2.排气机构,3.套管,4.光纤预制棒松散体,5.加热炉,6.下固定装置,7.进气机构,8.连接机构。Among them: 1. upper fixing device, 2. exhausting mechanism, 3. casing, 4. optical fiber preform loose body, 5. heating furnace, 6. lower fixing device, 7. air intake mechanism, 8. connecting mechanism.
具体实施方式detailed description
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions in the embodiments of the present invention are clearly and completely described in the following with reference to the accompanying drawings in the embodiments of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative efforts are within the scope of the present invention.
实施例1Example 1
如图1至图2所示,为符合本实施例的一种光纤预制棒套管烧结装置,包括套管3、上固定装置1、下固定装置6、加热炉5,其中所述套管3通过所述上固定装置1和所述下固定装置6以垂直方式安装在所述加热炉5中,一光纤预制棒松散体4设置在所述套管3内并与所述上固定装置1实现连接;所述上固定装置1上设有一排气机构2,所述排气机构2通过阀门开关与排气系统和真空泵相连,所述下固定装置6上设有一进气机构7。As shown in FIG. 1 to FIG. 2, an optical fiber preform sleeve sintering device according to the embodiment includes a sleeve 3, an upper fixing device 1, a lower fixing device 6, and a heating furnace 5, wherein the sleeve 3 Installed in the heating furnace 5 in a vertical manner by the upper fixing device 1 and the lower fixing device 6, an optical fiber preform loose body 4 is disposed in the sleeve 3 and realized with the upper fixing device 1 The upper fixing device 1 is provided with an exhausting mechanism 2, and the exhausting mechanism 2 is connected to the exhaust system and the vacuum pump through a valve switch, and the lower fixing device 6 is provided with an air intake mechanism 7.
优选地,所述上固定装置1和所述下固定装置6与由旋转机构驱动,二 者可同步旋转。Preferably, the upper fixing device 1 and the lower fixing device 6 are driven by a rotating mechanism, Can rotate synchronously.
优选地,所述光纤预制棒松散体4通过一连接机构8与所述上固定装置1连接。Preferably, the optical fiber preform loose body 4 is connected to the upper fixing device 1 via a connecting mechanism 8.
优选地,所述加热炉5由一个或者多个加热元件组成,其设置在所述套管3的外侧。Preferably, the furnace 5 consists of one or more heating elements which are arranged outside the sleeve 3.
优选地,所述套管3为石英套管3。Preferably, the sleeve 3 is a quartz sleeve 3.
该烧结装置采用套管3抽真空方法烧结光纤预制棒松散体4,避免使用价格昂贵且易于损坏的炉芯管,可制备大尺寸松散体。同时真空环境有利于改善预制棒质量,加快烧结速度,提高生产效率。The sintering device uses the casing 3 vacuuming method to sinter the optical fiber preform loose body 4, thereby avoiding the use of expensive and easily damaged furnace core tubes, and can prepare large-sized loose bodies. At the same time, the vacuum environment is beneficial to improve the quality of the preform, speed up the sintering and increase the production efficiency.
实施例2Example 2
基于实施例1所述的光纤预制棒套管烧结装置的烧结方法,包括如下步骤:The sintering method of the optical fiber preform sleeve sintering device according to Embodiment 1 includes the following steps:
S1:将套管3通过上固定装置1和下固定装置6以垂直方式安装在加热炉5中;S1: the sleeve 3 is vertically installed in the heating furnace 5 through the upper fixing device 1 and the lower fixing device 6;
S2:将光纤预制棒松散体4设置在套管3内并与上固定装置1实现连接;S2: disposing the optical fiber preform loose body 4 in the sleeve 3 and connecting with the upper fixing device 1;
S3:通过加热炉5的升温和移动去除光纤预制棒松散体4中由生产过程引入的羟基;S3: removing the hydroxyl group introduced by the production process in the optical fiber preform loose body 4 by the temperature rise and movement of the heating furnace 5;
S4:将加热炉5移动至光纤预制棒松散体4的底部,升温至1450℃以上,并形成温度梯度分布,温度分布如图3所示;S4: moving the heating furnace 5 to the bottom of the optical fiber preform loose body 4, raising the temperature to above 1450 ° C, and forming a temperature gradient distribution, the temperature distribution is shown in FIG. 3;
S5:在1450℃至1550℃的烧结温度条件下,光纤预制棒松散体4下端部分完成玻璃化;S5: at a sintering temperature of 1450 ° C to 1550 ° C, the lower end portion of the optical fiber preform loose body 4 is vitrified;
S6:通过阀门开关将排气机构2与真空泵联通,在套管3内部形成负压;同时调整加热炉5的温度分布,使套管3下端熔融收缩,与玻璃化的光纤预制棒松散体4融合,温度分布如图4所示;S6: connecting the exhaust mechanism 2 and the vacuum pump through the valve switch to form a negative pressure inside the sleeve 3; adjusting the temperature distribution of the heating furnace 5 to melt and contract the lower end of the sleeve 3, and the vitrified optical fiber preform loose body 4 Fusion, temperature distribution is shown in Figure 4;
S7:底部融合完成后,加热炉5以3mm/min至8mm/min速度向上移动, 将光纤预制棒松散体4分区玻璃化。底部融合后向上分区烧结熔缩过程如图2所示。S7: After the bottom fusion is completed, the heating furnace 5 moves upward at a speed of 3 mm/min to 8 mm/min. The optical fiber preform loose body 4 is vitrified. After the bottom is fused, the upper part of the sintering and melting process is shown in Fig. 2.
优选地,所述步骤S3具体包括:Preferably, the step S3 specifically includes:
将加热炉5升温至1100℃~1300℃,并沿垂直方向来回移动1次或1次以上;Heating the furnace 5 to 1100 ° C ~ 1300 ° C, and moving back and forth 1 or more times in the vertical direction;
同时由进气机构7向套管3内通入干燥剂和工艺气体;通过阀门开关打开排气系统与排气机构2的通道,将套管3内压力保持10至40pa的范围内,提供脱水气氛环境。At the same time, the desiccant and the process gas are introduced into the casing 3 by the air inlet mechanism 7; the passage of the exhaust system and the exhaust mechanism 2 is opened through the valve switch, and the pressure in the casing 3 is maintained within a range of 10 to 40 Pa to provide dehydration. Atmosphere.
优选地,所述工艺气体为给氯气、氦气、氮气中的一种或者多种。Preferably, the process gas is one or more of chlorine gas, helium gas and nitrogen gas.
优选地,所述套管3为石英套管3。Preferably, the sleeve 3 is a quartz sleeve 3.
本发明的改进之处在于:The improvement of the present invention is that:
①采用套管3烧结,无石英炉芯管。大大简化设备复杂程度。以及避免由炉芯管本身污染,老化带来的产品质量风险。1 Sintered with casing 3, without quartz furnace core tube. Significantly simplifies equipment complexity. And avoid the product quality risk caused by the pollution of the furnace tube itself and aging.
②采用加热炉5移动的方式,大大缩小设备尺寸,减小气体用量,降低生产成本。2 The method of moving the heating furnace 5 greatly reduces the size of the equipment, reduces the amount of gas, and reduces the production cost.
③烧结时对套管3内抽真空,有利于排除气泡,提高生产效率。3 When vacuuming the inside of the casing 3 during sintering, it is advantageous to eliminate air bubbles and improve production efficiency.
④烧结时,将套管3熔缩形成产品的一部分,增大预制棒尺寸,有利于提高生产效率。4 When sintering, the sleeve 3 is melted to form a part of the product, and the preform size is increased, which is advantageous for improving production efficiency.
采用无炉芯管烧结方法,降低生产成本,可制备大尺寸松散体。降低设备复杂程度,降低设备空间占用程度,有利于大规模批量生产。在抽真空的条件下对松散体进行烧结,有利于排除气泡,加快烧结速度,提高烧结效率。对所公开的实施例的上述说明,使本领域专业技术人员能够实现或使用本发明。对这些实施例的多种修改对本领域的专业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发明的精神或范围的情况下,在其 它实施例中实现。因此,本发明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公开的原理和新颖特点相一致的最宽的范围。 The furnaceless tube sintering method is adopted to reduce the production cost, and a large-sized loose body can be prepared. Reducing the complexity of the equipment and reducing the space occupied by the equipment is conducive to large-scale mass production. Sintering the loose body under vacuuming conditions is advantageous for eliminating bubbles, speeding up the sintering speed, and improving the sintering efficiency. The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. It will be apparent to those skilled in the art that various modifications of the embodiments may be made without departing from the spirit or scope of the invention. It is implemented in its embodiment. Therefore, the present invention is not to be limited to the embodiments shown herein, but the scope of the invention is to be accorded

Claims (9)

  1. 一种光纤预制棒套管烧结装置,其特征在于:包括套管、上固定装置、下固定装置、加热炉,其中所述套管通过所述上固定装置和所述下固定装置以垂直方式安装在所述加热炉中,一光纤预制棒松散体设置在所述套管内并与所述上固定装置实现连接;所述上固定装置上设有一排气机构,所述排气机构通过阀门开关与排气系统和真空泵相连,所述下固定装置上设有一进气机构。An optical fiber preform sleeve sintering device, comprising: a sleeve, an upper fixing device, a lower fixing device, and a heating furnace, wherein the sleeve is vertically installed by the upper fixing device and the lower fixing device In the heating furnace, an optical fiber preform loose body is disposed in the sleeve and connected to the upper fixing device; the upper fixing device is provided with an exhaust mechanism, and the exhaust mechanism passes through a valve switch The exhaust system is connected to a vacuum pump, and the lower fixing device is provided with an air intake mechanism.
  2. 如权利要求1所述的光纤预制棒套管烧结装置,其特征在于:所述上固定装置和所述下固定装置与由旋转机构驱动,二者可同步旋转。The optical fiber preform sleeve sintering apparatus according to claim 1, wherein said upper fixing means and said lower fixing means are driven by a rotating mechanism, and both of them are synchronously rotatable.
  3. 如权利要求1或2所述的光纤预制棒套管烧结装置,其特征在于:所述光纤预制棒松散体通过一连接机构与所述上固定装置连接。The optical fiber preform sleeve sintering apparatus according to claim 1 or 2, wherein said optical fiber preform loose body is connected to said upper fixing means via a connecting mechanism.
  4. 如权利要求1-3任一所述的光纤预制棒套管烧结装置,其特征在于:所述加热炉由一个或者多个加热元件组成,其设置在所述套管的外侧。The optical fiber preform sleeve sintering apparatus according to any one of claims 1 to 3, wherein the heating furnace is composed of one or more heating elements disposed outside the sleeve.
  5. 如权利要求1-4任一所述的光纤预制棒套管烧结装置,其特征在于:所述套管为石英套管。The optical fiber preform sleeve sintering apparatus according to any one of claims 1 to 4, wherein the sleeve is a quartz sleeve.
  6. 一种基于权利要求1-5任一所述的光纤预制棒套管烧结装置的烧结方法,其特征在于,包括如下步骤:A sintering method for an optical fiber preform sleeve sintering apparatus according to any one of claims 1 to 5, characterized in that it comprises the following steps:
    S1:将套管通过上固定装置和下固定装置以垂直方式安装在加热炉中;S1: installing the sleeve in the heating furnace through the upper fixing device and the lower fixing device in a vertical manner;
    S2:将光纤预制棒松散体设置在套管内并与上固定装置实现连接;S2: disposing the optical fiber preform loose body in the sleeve and connecting with the upper fixing device;
    S3:通过加热炉的升温和移动去除光纤预制棒松散体中由生产过程引入的羟基;S3: removing the hydroxyl group introduced by the production process in the bulk of the optical fiber preform by the temperature rise and movement of the heating furnace;
    S4:将加热炉移动至光纤预制棒松散体的底部,升温至1450℃以上,并形成温度梯度分布;S4: moving the heating furnace to the bottom of the optical fiber preform loose body, heating up to above 1450 ° C, and forming a temperature gradient distribution;
    S5:在一定的烧结温度条件下,光纤预制棒松散体下端部分完成玻璃化;S5: under a certain sintering temperature condition, the lower end portion of the loose portion of the optical fiber preform is vitrified;
    S6:通过阀门开关将排气机构与真空泵联通,在套管内部形成负压;同时调整加热炉的温度分布,使套管下端熔融收缩,与玻璃化的光纤预制棒松 散体融合;S6: the exhaust mechanism is connected with the vacuum pump through a valve switch to form a negative pressure inside the sleeve; at the same time, the temperature distribution of the heating furnace is adjusted, so that the lower end of the sleeve is melted and shrunk, and the vitrified optical fiber preform is loosened. Loose body fusion;
    S7:底部融合完成后,加热炉以一定的移动速度向上移动,将光纤预制棒松散体分区玻璃化。S7: After the bottom fusion is completed, the heating furnace moves upward at a certain moving speed, and the optical fiber preform loose partition is vitrified.
  7. 如权利要求6所述的光纤预制棒套管烧结方法,其特征在于,所述步骤S3具体包括:The method for sintering an optical fiber preform sleeve according to claim 6, wherein the step S3 specifically comprises:
    将加热炉升温至1100℃~1300℃,并沿垂直方向来回移动1次或1次以上;Heating the furnace to 1100 ° C ~ 1300 ° C, and moving back and forth 1 or more times in the vertical direction;
    同时由进气机构向套管内通入干燥剂和工艺气体;通过阀门开关打开排气系统与排气机构的通道,将套管内压力保持在合适的水平,提供脱水气氛环境。At the same time, the desiccant and the process gas are introduced into the casing by the air inlet mechanism; the passage of the exhaust system and the exhaust mechanism is opened through the valve switch, and the pressure in the casing is maintained at an appropriate level to provide a dehydration atmosphere environment.
  8. 如权利要求7所述的光纤预制棒套管烧结方法,其特征在于:所述工艺气体为给氯气、氦气、氮气中的一种或者多种。The method for sintering an optical fiber preform sleeve according to claim 7, wherein the process gas is one or more of chlorine gas, helium gas and nitrogen gas.
  9. 如权利要求6-8任一所述的光纤预制棒套管烧结方法,其特征在于:所述套管为石英套管。 The method for sintering an optical fiber preform sleeve according to any one of claims 6 to 8, wherein the sleeve is a quartz sleeve.
PCT/CN2017/077199 2016-08-26 2017-03-19 Sintering device with casing tube for optical fibre preform rod and sintering method therefor WO2018036142A1 (en)

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