WO2020181791A1 - Large-size low-attenuation optical fiber preform and preparation method therefor - Google Patents

Large-size low-attenuation optical fiber preform and preparation method therefor Download PDF

Info

Publication number
WO2020181791A1
WO2020181791A1 PCT/CN2019/114407 CN2019114407W WO2020181791A1 WO 2020181791 A1 WO2020181791 A1 WO 2020181791A1 CN 2019114407 W CN2019114407 W CN 2019114407W WO 2020181791 A1 WO2020181791 A1 WO 2020181791A1
Authority
WO
WIPO (PCT)
Prior art keywords
optical fiber
layer
fiber preform
core layer
sintering furnace
Prior art date
Application number
PCT/CN2019/114407
Other languages
French (fr)
Chinese (zh)
Inventor
莫思铭
李凡
眭立洪
张国栋
周莉
李想
Original Assignee
江苏永鼎股份有限公司
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 江苏永鼎股份有限公司 filed Critical 江苏永鼎股份有限公司
Publication of WO2020181791A1 publication Critical patent/WO2020181791A1/en

Links

Classifications

    • 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]
    • C03B37/01446Thermal 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
    • 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

Definitions

  • the present application belongs to the technical field of optical fiber preform manufacturing, and in particular relates to a large-size low attenuation optical fiber preform and a preparation method thereof.
  • Optical fiber preform is the upstream product of optical fiber, which determines the performance and type of optical fiber. At the same time, optical fiber preform is also the most profitable part of the entire product chain of optical fiber and cable. For a long time, the manufacturing technology of optical fiber preform has been monopolized by foreign companies. Preforms rely heavily on imports, which hinders the development of my country's optical communication network.
  • Optical fiber attenuation is an important indicator of optical fiber transmission, which has a decisive impact on the transmission distance of optical fiber communication.
  • the level of optical fiber attenuation directly affects the transmission distance or the distance between relay stations. Therefore, reducing optical fiber attenuation has great practical significance for optical fiber communication.
  • the large-size optical fiber preform can be drawn for thousands of kilometers, which greatly improves the production efficiency and becomes an effective method to reduce the cost of optical fiber.
  • major optical fiber manufacturers are conducting research on the manufacturing technology of large-size and low-attenuation optical fiber preforms in order to gain greater initiative in the fierce market competition.
  • the technology for manufacturing optical fiber preforms is to first manufacture the preform core rod, and then manufacture the cladding outside the core rod.
  • MCVD chemical vapor deposition
  • PCVD microwave plasma chemistry Vapor phase deposition
  • OTD external vapor deposition
  • VAD axial vapor deposition
  • the outer coating manufacturing technology mainly includes OVD method, sleeve method, plasma spraying method; because the above methods are used in the production of optical fiber preforms
  • the existing manufacturing of optical fiber preforms is a combination of the above two or more methods in order to obtain large-size and low-attenuation optical fiber preforms
  • the technical problem to be solved by the present invention is to solve the technical problem that the hydroxyl content in the large-sized optical fiber preform is difficult to be effectively controlled in the prior art, thereby providing a large-sized low-attenuation optical fiber preform and a preparation method thereof.
  • a method for preparing a large-size and low-attenuation optical fiber preform includes the following steps:
  • the inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the quartz tube as the depressed layer using the MCVD process to obtain a deposition tube, and the deposition tube is fused at high temperature to have an inner core layer, an outer core layer, an inner cladding layer and Preformed rod mandrel of the sunken layer;
  • VAD process to deposit the first cladding loose body on the preform core rod, and pass the first sintering treatment to prepare the primary optical fiber preform;
  • the inner core layer, the outer core layer, the inner cladding layer, the recessed layer, and the first outer cladding layer use silica as the base material and adding dopants, the second outer cladding layer is pure silica, the inner core layer and the outer core layer
  • the relative refractive index of the inner cladding layer, the depressed layer and the first outer cladding layer are ⁇ n 1 , ⁇ n 2 , ⁇ n 3 , ⁇ n 4 , ⁇ n 5 , and the relative refractive index is: ⁇ n 1 > ⁇ n 2 >0> ⁇ n 3 > ⁇ n 5 > ⁇ n 4 .
  • the first sintering treatment or the second sintering treatment method is: the primary optical fiber preform or the optical fiber preform to be sintered is rotated in the sintering furnace, and the heating coil outside the sintering furnace is moved up and down to the inside of the sintering furnace. Gas heating is used to complete sintering.
  • the moving speed of the heating coil is preferably 5-10 mm/min, and the rotation speed is preferably 3-6 rpm.
  • the first sintering treatment includes three steps of dehydroxylation treatment, fluorine doping treatment and vitrification treatment. Firstly, inert gas and chlorine gas are introduced into the sintering furnace, so that the temperature in the sintering furnace is 25-35 mm/min.
  • the heating rate reaches 900 ⁇ 1100°C, and the temperature is kept for 1-2h to complete the dehydroxylation treatment; secondly, fluorine-containing gas and inert gas are introduced into the sintering furnace to make the temperature in the sintering furnace reach 1100 ⁇ 1300 at a heating rate of 15 ⁇ 25mm/min °C, keep for 2-3h, complete the fluorine doping treatment; finally, only inert gas is introduced into the sintering furnace, so that the temperature in the sintering furnace reaches 1400 ⁇ 1600°C at a heating rate of 8 ⁇ 15mm/min, and the heat preservation is 3-4h to complete the glass ⁇ .
  • the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment. Firstly, inert gas and chlorine gas are introduced into the sintering furnace, so that the temperature in the sintering furnace reaches 1000 at a heating rate of 40-60 mm/min. ⁇ 1200°C, keep for 2-4 hours to complete the dehydroxylation treatment; then turn off the chlorine gas and pass only inert gas into the sintering furnace to make the temperature in the sintering furnace reach 1300 ⁇ 1500°C at a heating rate of 10 ⁇ 20mm/min, keep 4 -6h, complete the vitrification process.
  • inert gas and chlorine gas are introduced into the sintering furnace, so that the temperature in the sintering furnace reaches 1000 at a heating rate of 40-60 mm/min. ⁇ 1200°C, keep for 2-4 hours to complete the dehydroxylation treatment; then turn off the chlorine gas and pass only inert gas into the sintering furnace to make the temperature in the sintering furnace reach 1300 ⁇ 1500
  • the inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index ⁇ n 1 of the inner core layer is 0.35% to 0.45%, and the relative refractive index of the outer core layer The refractive index ⁇ n 2 is 0.15% to 0.3%, and the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 1.5-2.
  • the inner cladding layer is a silica glass layer doped with a mixture of Sb 2 O 3 -F, the relative refractive index ⁇ n 3 of the inner cladding layer is -0.2% to -0.05%, and the diameter c of the inner cladding layer and the inner core The ratio c/a of the layer diameter a is 3-4.
  • the depressed layer is an F-doped silica glass layer
  • the relative refractive index ⁇ n 4 of the depressed layer is -0.6% to -0.45%
  • the ratio of the diameter d of the depressed layer to the diameter a of the inner core layer is d/ a is 5-6.5.
  • the first outer cladding layer is an F-doped silica glass layer
  • the relative refractive index ⁇ n 4 of the first outer cladding layer is -0.35% to -0.25%
  • the diameter e of the first outer cladding layer and the inner core layer The ratio e/a of the diameter a is 10-11.5, and the ratio f/a of the diameter f of the optical fiber preform to the diameter a of the inner core layer is 15-17.
  • the present invention also provides an optical fiber preform manufactured by the above method.
  • the present invention also provides an optical fiber, which is formed by directly drawing the above-mentioned optical fiber preform, or formed by drawing after drawing.
  • the present invention uses the MCVD process to prepare the preformed rod core rod including the inner core layer, the outer core layer, the inner cladding layer and the depressed layer, and then deposits the first outer cladding layer loose body through the VAD process, and prepares the primary optical fiber through the first sintering process
  • the loose body of the second outer cladding layer is finally deposited through the OVD process, and the optical fiber preform is obtained through the second sintering process, in which:
  • Each layer of the optical fiber preform has an appropriate relative refractive index difference, and further defines the dopant and radius of each layer of the optical fiber preform, which can increase the effective area and reduce the attenuation coefficient of the optical fiber;
  • the primary optical fiber preform or optical fiber preform to be sintered rotate in the sintering furnace, and use the coil to move up and down to heat the gas inside the sintering furnace, so that the primary optical fiber preform or optical fiber preform to be sintered does not need to move up and down.
  • the risk of rod dropping is reduced, and the temperature accuracy and temperature field uniformity in the sintering furnace of the optical fiber preform can be effectively improved.
  • the first and second cladding layers have a reasonable structure, which effectively reduces The loss of the optical fiber preform is calculated.
  • the diameter of the optical fiber preform prepared by the present invention can reach 215mm
  • the drawing length of a single preform can reach 2930km
  • the attenuation of the prepared optical fiber at 1310nm wavelength is as low as 0.298dB/km
  • the attenuation coefficient at 1383nm wavelength is as low as 0.265dB/km
  • the attenuation coefficient at the wavelength of 1550nm is as low as 0.165dB/km
  • the cut-off wavelength of the fiber is 1265nm ⁇ 1273nm.
  • This embodiment provides a method for preparing a large-size and low-attenuation optical fiber preform, which includes the following steps:
  • the inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the F-doped quartz tube as the depressed layer using the MCVD process to obtain a deposited tube, and the deposited tube is fused at 2300°C to have an inner core layer, an outer core layer, Preformed rod core rods of inner cladding and sinking layer;
  • the first cladding loose body is deposited on the preform core rod by the VAD process, and the primary optical fiber preform is prepared after the first sintering treatment; the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification
  • the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification
  • He gas and chlorine gas are introduced into the sintering furnace, so that the primary optical fiber preform to be sintered rotates at a speed of 3rpm in the sintering furnace, and the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace.
  • the moving speed of the heating coil is 10mm/min, and the temperature in the sintering furnace reaches 900°C at a heating rate of 25mm/min, and the temperature is kept for 2h to complete the dehydration treatment;
  • SiF 4 gas and He gas are introduced into the sintering furnace to maintain
  • the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil make the temperature in the sintering furnace reach 1100°C at a heating rate of 15mm/min, hold for 3 hours, and complete the fluorine doping treatment;
  • only He gas is introduced into the sintering furnace to maintain
  • the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil make the temperature in the sintering furnace reach 1400 °C at a heating rate of 8 mm/min, and keep it for 4 hours to complete the vitrification process;
  • the second cladding loose body is deposited on the primary optical fiber preform by the OVD process, and the optical fiber preform is prepared by the second sintering treatment;
  • the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment, First, pass He gas and chlorine gas into the sintering furnace, so that the optical fiber preform to be sintered rotates at a rotation speed of 3 rpm in the sintering furnace.
  • the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace, and the heating coil moves The speed is 10mm/min, and the temperature in the sintering furnace reaches 1000°C at a heating rate of 40mm/min, and the temperature is kept for 4 hours to complete the dehydroxylation treatment; then the chlorine gas is turned off, and only inert gas is introduced into the sintering furnace to make the temperature in the sintering furnace Reach 1300°C at a heating rate of 10mm/min, keep it for 6 hours, and complete the vitrification process;
  • the inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index ⁇ n 1 of the inner core layer is 0.35%, and the relative refractive index ⁇ n 2 of the outer core layer is 0.15 %, the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 1.5;
  • the inner cladding layer is a silica glass layer doped with Sb 2 O 3 -F mixture, and the relative refractive index of the inner cladding layer ⁇ n 3 is -0.2%, the ratio c/a of the inner cladding diameter c to the inner core layer diameter a is 3;
  • the relative refractive index ⁇ n 4 of the sinking layer is -0.6%, and the sinking layer diameter d is
  • the ratio d/a of the core layer diameter a is 5;
  • the first cladding layer is an F-doped silica glass layer, the relative refractive index ⁇ n 4
  • the diameter of the optical fiber preform reaches 205mm, and the prepared optical fiber preform is drawn into the fiber online.
  • the length of a single rod can reach 2880km.
  • the attenuation of the fiber at 1310nm is 0.301dB/km, and the attenuation at 1383nm It is 0.265dB/km, the attenuation at 1550nm is 0.165dB/km, and the cut-off wavelength is 1273nm.
  • This embodiment provides a method for preparing a large-size and low-attenuation optical fiber preform, which includes the following steps:
  • the inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the F-doped quartz tube as the depressed layer by the MCVD process to obtain a deposition tube, and the deposition tube is fused at 2400°C to have an inner core layer, an outer core layer, Preformed rod core rods of inner cladding and sinking layer;
  • the first cladding loose body is deposited on the preform core rod by the VAD process, and the primary optical fiber preform is prepared after the first sintering treatment; the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification
  • the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification
  • He gas and chlorine gas are introduced into the sintering furnace, so that the primary optical fiber preform to be sintered rotates at a rotation speed of 6 rpm in the sintering furnace.
  • the up and down movement of the heating coil outside the sintering furnace can affect the gas inside the sintering furnace.
  • Heating the moving speed of the heating coil is 5mm/min, and the temperature in the sintering furnace reaches 1100°C at a heating rate of 35mm/min, and the temperature is kept for 1h to complete the dehydration treatment; secondly, CF 4 gas and He gas are passed into the sintering furnace. Maintain the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil to make the temperature in the sintering furnace reach 1300°C at a heating rate of 25mm/min, hold for 2 hours, and complete the fluorine doping treatment; finally, only He gas is introduced into the sintering furnace.
  • the second cladding loose body is deposited on the primary optical fiber preform by the OVD process, and the optical fiber preform is prepared by the second sintering treatment;
  • the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment, First, pass He gas and chlorine gas into the sintering furnace, so that the optical fiber preform to be sintered rotates at a speed of 6 rpm in the sintering furnace.
  • the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace, and the moving speed of the heating coil
  • the temperature in the sintering furnace is set to 5mm/min, and the temperature in the sintering furnace is increased to 1200°C at a heating rate of 60mm/min, and the temperature is kept for 2 hours to complete the dehydroxylation treatment.
  • the heating rate of 20mm/min reaches 1500°C, and the heat preservation is 4h to complete the vitrification treatment;
  • the inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index ⁇ n 1 of the inner core layer is 0.45%, and the relative refractive index ⁇ n 2 of the outer core layer is 0.3 %, the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 2; the inner cladding layer is a silica glass layer doped with Sb 2 O 3 -F mixture, and the relative refractive index of the inner cladding layer ⁇ n 3 is -0.05%, the ratio c/a of the inner cladding diameter c to the inner core layer diameter a is 4; the relative refractive index ⁇ n 4 of the depressed layer is -0.45%, and the depressed layer diameter d is The ratio d/a of the core layer diameter a is 6.5; the first outer cladding layer is an F-doped silica glass layer, and the relative refractive index ⁇ n 4 of the first outer cla
  • the diameter of the optical fiber preform reaches 215mm.
  • the prepared optical fiber preform is drawn on-line to draw the fiber.
  • the length of a single rod can reach 2930km.
  • the fiber attenuation at 1310nm is 0.302dB/km and the attenuation at 1383nm. It is 0.271dB/km, the attenuation at 1550nm is 0.171dB/km, and the cut-off wavelength is 1265nm.
  • This embodiment provides a method for preparing a large-size and low-attenuation optical fiber preform, which includes the following steps:
  • the inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the F-doped quartz tube as the depressed layer using the MCVD process to obtain a deposited tube, and the deposited tube is fused at 2500°C to have an inner core layer, an outer core layer, Preformed rod core rods of inner cladding and sinking layer;
  • the first cladding loose body is deposited on the preform core rod by the VAD process, and the primary optical fiber preform is prepared after the first sintering treatment; the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification
  • the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification
  • He gas and chlorine gas are introduced into the sintering furnace to make the primary optical fiber preform to be sintered rotate at a speed of 5 rpm in the sintering furnace, and the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace.
  • the moving speed of the heating coil is 8mm/min, and the temperature in the sintering furnace is reached to 1000°C at a heating rate of 30mm/min, and the temperature is kept for 1.5h to complete the dehydration treatment; secondly, SF 6 gas and He gas are introduced into the sintering furnace.
  • the second cladding loose body is deposited on the primary optical fiber preform by the OVD process, and the optical fiber preform is prepared by the second sintering treatment;
  • the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment, First, pass He gas and chlorine gas into the sintering furnace, so that the optical fiber preform to be sintered rotates at a speed of 5 rpm in the sintering furnace.
  • the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace, and the moving speed of the heating coil
  • the temperature in the sintering furnace is 8mm/min, and the temperature in the sintering furnace reaches 1100°C at a heating rate of 50mm/min, and the temperature is kept for 3 hours to complete the dehydroxylation treatment;
  • the heating rate of 15mm/min reaches 1400°C, and the temperature is kept for 6 hours to complete the vitrification process;
  • the inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index ⁇ n 1 of the inner core layer is 0.4%, and the relative refractive index ⁇ n 2 of the outer core layer is 0.2 %, the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 1.7;
  • the inner cladding layer is a silica glass layer doped with Sb 2 O 3 -F mixture, and the relative refractive index of the inner cladding layer ⁇ n 3 is -0.1%, the ratio c/a of the inner cladding diameter c to the inner core layer diameter a is 3.5;
  • the relative refractive index ⁇ n 4 of the sinking layer is -0.5%, and the sinking layer diameter d is
  • the ratio d/a of the core layer diameter a is 6;
  • the first cladding layer is an F-doped silica glass layer, the relative refractive index ⁇ n
  • the diameter of the optical fiber preform reaches 210mm.
  • the prepared optical fiber preform is drawn online to draw a low-loss optical fiber.
  • the length of a single rod can reach 2915km.
  • the attenuation of the fiber at 1310nm is 0.298dB/km.
  • the attenuation is 0.272dB/km, the attenuation at 1550nm is 0.168dB/km, and the cut-off wavelength is 1268nm.

Abstract

Disclosed are a large-size low-attenuation optical fiber preform and a preparation method therefor. The method comprises: preparing a preform core rod comprising an inner core layer, an outer core layer, an inner cladding layer, and a depressed layer by using an MCVD process, then depositing a first outer cladding loose body by means of a VAD process and preparing a primary optical fiber preform by means of primary sintering treatment, and finally depositing a second outer cladding loose body by means of an OVD process and obtaining an optical fiber preform by means of secondary sintering treatment. The diameter of the prepared optical fiber preform may be up to 215 mm, the fiber pulling length of a single preform may be up to 2930 km, the attenuation coefficient of an optical fiber at a wavelength of 1310 nm is as low as 0.298 dB/km, the attenuation coefficient of the optical fiber at a wavelength of 1383 nm is as low as 0.265 dB/km, the attenuation coefficient of the optical fiber at a wavelength of 1550 nm is as low as 0.165 dB/km, and the cutoff wavelength of the optical fiber is from 1265 nm to 1273 nm.

Description

一种大规格低衰减的光纤预制棒及其制备方法Large-size and low-attenuation optical fiber preform and preparation method thereof
本申请要求2019年3月11日向中国国家知识产权局递交的申请号为201910181908.X的发明专利申请的优先权,该优先权文本内容明确通过援引加入并入本申请中。This application claims the priority of the invention patent application with the application number 201910181908.X filed with the State Intellectual Property Office of China on March 11, 2019. The content of the priority text is expressly incorporated into this application by reference.
技术领域Technical field
本申请属于光纤预制棒制造技术领域,尤其是涉及一种大规格低衰减的光纤预制棒及其制备方法。The present application belongs to the technical field of optical fiber preform manufacturing, and in particular relates to a large-size low attenuation optical fiber preform and a preparation method thereof.
背景技术Background technique
光纤预制棒是光纤的上游产品,决定着光纤的性能与种类,同时,光纤预制棒也是光纤光缆整条产品链利润最大的部分,长期以来光纤预制棒制造技术被国外公司所垄断,导致我国光纤预制棒严重依赖进口,阻碍了我国光通信网络的发展。Optical fiber preform is the upstream product of optical fiber, which determines the performance and type of optical fiber. At the same time, optical fiber preform is also the most profitable part of the entire product chain of optical fiber and cable. For a long time, the manufacturing technology of optical fiber preform has been monopolized by foreign companies. Preforms rely heavily on imports, which hinders the development of my country's optical communication network.
光纤衰减是光纤传输的重要指标,对光纤通信的传输距离有决定性的影响,光纤衰减的高低直接影响传输距离或中继站间隔距离的远近,因此,降低光纤衰减对光纤通信有着重大的现实意义。同时,大尺寸光纤预制棒拉丝可达上千公里,大大提高了生产效率,成为目前能降低光纤成本的有效方法。目前,各大光纤制造商纷纷进行研究大规格低衰减光纤预制棒的制造技术,以期在激烈的市场竞争中获得更大的主动权。Optical fiber attenuation is an important indicator of optical fiber transmission, which has a decisive impact on the transmission distance of optical fiber communication. The level of optical fiber attenuation directly affects the transmission distance or the distance between relay stations. Therefore, reducing optical fiber attenuation has great practical significance for optical fiber communication. At the same time, the large-size optical fiber preform can be drawn for thousands of kilometers, which greatly improves the production efficiency and becomes an effective method to reduce the cost of optical fiber. At present, major optical fiber manufacturers are conducting research on the manufacturing technology of large-size and low-attenuation optical fiber preforms in order to gain greater initiative in the fierce market competition.
通常,制造光纤预制棒的技术为先制造预制棒芯棒,然后在芯棒外制造包层,芯棒制造技术主要有以下四种:改进的化学汽相沉积法(MCVD)、微波等离子体化学汽相沉积(PCVD)、外部气相沉积法 (OVD)和轴向气相沉积法(VAD),外包层制造技术主要包括OVD法,套管法,等离子体喷涂法;由于上述方法在光纤预制棒生产上各有利弊,现有制造光纤预制棒均为上述两种以上方法的组合,以期得到大规格低衰减的光纤预制棒,但是目前大规格光纤预制棒所制备的的光纤衰减难以得到有效控制。Generally, the technology for manufacturing optical fiber preforms is to first manufacture the preform core rod, and then manufacture the cladding outside the core rod. There are four main core rod manufacturing technologies: improved chemical vapor deposition (MCVD), microwave plasma chemistry Vapor phase deposition (PCVD), external vapor deposition (OVD) and axial vapor deposition (VAD), the outer coating manufacturing technology mainly includes OVD method, sleeve method, plasma spraying method; because the above methods are used in the production of optical fiber preforms Each of the above has advantages and disadvantages. The existing manufacturing of optical fiber preforms is a combination of the above two or more methods in order to obtain large-size and low-attenuation optical fiber preforms. However, the current optical fiber attenuation prepared by large-size optical fiber preforms is difficult to effectively control.
发明内容Summary of the invention
本发明要解决的技术问题是:为解决现有技术中大规格光纤预制棒中的羟基含量难以得到有效控制的技术问题,从而提供一种大规格低衰减光纤预制棒及其制备方法。The technical problem to be solved by the present invention is to solve the technical problem that the hydroxyl content in the large-sized optical fiber preform is difficult to be effectively controlled in the prior art, thereby providing a large-sized low-attenuation optical fiber preform and a preparation method thereof.
本发明解决其技术问题所采用的技术方案是:The technical solutions adopted by the present invention to solve its technical problems are:
一种大规格低衰减光纤预制棒的制备方法,包括如下步骤:A method for preparing a large-size and low-attenuation optical fiber preform includes the following steps:
利用MCVD工艺在作为下陷层的石英管内壁依次沉积内包层、外芯层和内芯层,获得沉积管,并将沉积管在高温下熔缩成具有内芯层、外芯层、内包层和下陷层的预制棒芯棒;The inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the quartz tube as the depressed layer using the MCVD process to obtain a deposition tube, and the deposition tube is fused at high temperature to have an inner core layer, an outer core layer, an inner cladding layer and Preformed rod mandrel of the sunken layer;
利用VAD工艺在预制棒芯棒上沉积第一外包层疏松体,并经过第一次烧结处理,制备出初级光纤预制棒;Use the VAD process to deposit the first cladding loose body on the preform core rod, and pass the first sintering treatment to prepare the primary optical fiber preform;
利用OVD工艺在初级光纤预制棒上沉积第二外包层疏松体,并经过第二次烧结处理,制备出光纤预制棒;Use the OVD process to deposit the loose body of the second outer cladding layer on the primary optical fiber preform, and pass the second sintering treatment to prepare the optical fiber preform;
所述内芯层、外芯层、内包层、下陷层、第一外包层以二氧化硅作为基底材料并加入掺杂剂,第二外包层为纯二氧化硅,内芯层、外芯层、内包层、下陷层、第一外包层的相对折射率依次为Δn 1、Δn 2、Δn 3、Δn 4、Δn 5,相对折射率大小为:Δn 1>Δn 2>0> Δn 3>Δn 5>Δn 4The inner core layer, the outer core layer, the inner cladding layer, the recessed layer, and the first outer cladding layer use silica as the base material and adding dopants, the second outer cladding layer is pure silica, the inner core layer and the outer core layer The relative refractive index of the inner cladding layer, the depressed layer and the first outer cladding layer are Δn 1 , Δn 2 , Δn 3 , Δn 4 , Δn 5 , and the relative refractive index is: Δn 1 >Δn 2 >0> Δn 3 >Δn 5 >Δn 4 .
优选地,所述第一次烧结处理或第二次烧结处理方法为:使待烧结的初级光纤预制棒或光纤预制棒在烧结炉内自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,完成烧结,加热线圈的移动速度优选为5-10mm/min,自转速度优选为3-6rpm。Preferably, the first sintering treatment or the second sintering treatment method is: the primary optical fiber preform or the optical fiber preform to be sintered is rotated in the sintering furnace, and the heating coil outside the sintering furnace is moved up and down to the inside of the sintering furnace. Gas heating is used to complete sintering. The moving speed of the heating coil is preferably 5-10 mm/min, and the rotation speed is preferably 3-6 rpm.
优选地,所述第一次烧结处理包括脱羟处理、掺氟处理和玻璃化处理三个步骤,首先向烧结炉内通入惰性气体和氯气,使烧结炉内温度以25~35mm/min的升温速率达到900~1100℃,保温1-2h,完成脱羟处理;其次向烧结炉内通入含氟气体和惰性气体,使烧结炉内温度以15~25mm/min的升温速率达到1100~1300℃,保温2-3h,完成掺氟处理;最后向烧结炉内只通入惰性气体,使烧结炉内温度以8~15mm/min的升温速率达到1400~1600℃,保温3-4h,完成玻璃化处理。Preferably, the first sintering treatment includes three steps of dehydroxylation treatment, fluorine doping treatment and vitrification treatment. Firstly, inert gas and chlorine gas are introduced into the sintering furnace, so that the temperature in the sintering furnace is 25-35 mm/min. The heating rate reaches 900~1100℃, and the temperature is kept for 1-2h to complete the dehydroxylation treatment; secondly, fluorine-containing gas and inert gas are introduced into the sintering furnace to make the temperature in the sintering furnace reach 1100~1300 at a heating rate of 15~25mm/min ℃, keep for 2-3h, complete the fluorine doping treatment; finally, only inert gas is introduced into the sintering furnace, so that the temperature in the sintering furnace reaches 1400~1600℃ at a heating rate of 8~15mm/min, and the heat preservation is 3-4h to complete the glass化处理.
优选地,所述第二次烧结处理包括脱羟处理和玻璃化处理两个步骤,首先向烧结炉内通入惰性气体和氯气,使烧结炉内温度以40~60mm/min的升温速率达到1000~1200℃,保温2-4h,完成脱羟处理;再关闭氯气,向烧结炉内只通入惰性气体,使烧结炉内温度以10~20mm/min的升温速率达到1300~1500℃,保温4-6h,完成玻璃化处理。Preferably, the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment. Firstly, inert gas and chlorine gas are introduced into the sintering furnace, so that the temperature in the sintering furnace reaches 1000 at a heating rate of 40-60 mm/min. ~1200℃, keep for 2-4 hours to complete the dehydroxylation treatment; then turn off the chlorine gas and pass only inert gas into the sintering furnace to make the temperature in the sintering furnace reach 1300~1500℃ at a heating rate of 10~20mm/min, keep 4 -6h, complete the vitrification process.
优选地,所述内芯层和外芯层为掺入P 2O 5-F混合物的二氧化硅玻璃层,内芯层的相对折射率Δn 1为0.35%~0.45%,外芯层的相对折射率Δn 2为0.15%~0.3%,所述外芯层直径b与内芯层直径a的比值b/a为 1.5-2。 Preferably, the inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index Δn 1 of the inner core layer is 0.35% to 0.45%, and the relative refractive index of the outer core layer The refractive index Δn 2 is 0.15% to 0.3%, and the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 1.5-2.
优选地,所述内包层为掺入Sb 2O 3-F混合物的二氧化硅玻璃层,内包层的相对折射率Δn 3为-0.2%~-0.05%,所述内包层直径c与内芯层直径a的比值c/a为3-4。 Preferably, the inner cladding layer is a silica glass layer doped with a mixture of Sb 2 O 3 -F, the relative refractive index Δn 3 of the inner cladding layer is -0.2% to -0.05%, and the diameter c of the inner cladding layer and the inner core The ratio c/a of the layer diameter a is 3-4.
优选地,所述下陷层为掺F的二氧化硅玻璃层,下陷层的相对折射率Δn 4为-0.6%~-0.45%,所述下陷层直径d与内芯层直径a的比值d/a为5-6.5。 Preferably, the depressed layer is an F-doped silica glass layer, the relative refractive index Δn 4 of the depressed layer is -0.6% to -0.45%, and the ratio of the diameter d of the depressed layer to the diameter a of the inner core layer is d/ a is 5-6.5.
优选地,所述第一外包层为掺F的二氧化硅玻璃层,第一外包层的相对折射率Δn 4为-0.35%~-0.25%,所述第一外包层直径e与内芯层直径a的比值e/a为10-11.5,所述光纤预制棒的直径f与内芯层直径a的比值f/a为15-17。 Preferably, the first outer cladding layer is an F-doped silica glass layer, the relative refractive index Δn 4 of the first outer cladding layer is -0.35% to -0.25%, and the diameter e of the first outer cladding layer and the inner core layer The ratio e/a of the diameter a is 10-11.5, and the ratio f/a of the diameter f of the optical fiber preform to the diameter a of the inner core layer is 15-17.
本发明还提供一种由上述方法制造的光纤预制棒。The present invention also provides an optical fiber preform manufactured by the above method.
本发明还提供一种光纤,所述光纤由上述的光纤预制棒直接拉丝而成,或经拉伸后再拉丝而成。The present invention also provides an optical fiber, which is formed by directly drawing the above-mentioned optical fiber preform, or formed by drawing after drawing.
本发明的有益效果是:The beneficial effects of the present invention are:
本发明利用MCVD工艺制备包括内芯层、外芯层、内包层和下陷层的预制棒芯棒,再通过VAD工艺沉积第一外包层疏松体,并经过第一次烧结处理得到制备出初级光纤预制棒,最后通过OVD工艺沉积第二外包层疏松体,并经过第二次烧结处理得到光纤预制棒,其中:The present invention uses the MCVD process to prepare the preformed rod core rod including the inner core layer, the outer core layer, the inner cladding layer and the depressed layer, and then deposits the first outer cladding layer loose body through the VAD process, and prepares the primary optical fiber through the first sintering process For the preform, the loose body of the second outer cladding layer is finally deposited through the OVD process, and the optical fiber preform is obtained through the second sintering process, in which:
光纤预制棒每一层具有合适的相对折射率差,并进一步限定了光纤预制棒每一层的掺杂剂和半径,可以增加有效面积,降低光纤的衰减系数;Each layer of the optical fiber preform has an appropriate relative refractive index difference, and further defines the dopant and radius of each layer of the optical fiber preform, which can increase the effective area and reduce the attenuation coefficient of the optical fiber;
使待烧结的初级光纤预制棒或光纤预制棒在烧结炉内自转,采用线圈上下移动的方式对对烧结炉内部气体加热,可以使待烧结的初级光纤预制棒或光纤预制棒不需要上下移动,减少了掉棒风险,并可以有效改善光纤预制棒烧结炉内的温度准确性和温场均匀性,通过进一步限定烧结处理工艺,使第一外包层和第二外包层具有合理的结构,有效降低了光纤预制棒的损耗。Make the primary optical fiber preform or optical fiber preform to be sintered rotate in the sintering furnace, and use the coil to move up and down to heat the gas inside the sintering furnace, so that the primary optical fiber preform or optical fiber preform to be sintered does not need to move up and down. The risk of rod dropping is reduced, and the temperature accuracy and temperature field uniformity in the sintering furnace of the optical fiber preform can be effectively improved. By further limiting the sintering process, the first and second cladding layers have a reasonable structure, which effectively reduces The loss of the optical fiber preform is calculated.
最终,本发明制备的光纤预制棒的直径可达215mm,单根预制棒拉纤长度可达到2930km,制备的光纤在1310nm波长处的衰减低至0.298dB/km,在1383nm波长处的衰减系数低至0.265dB/km,在1550nm波长处的衰减系数低至0.165dB/km,光纤的截止波长为1265nm~1273nm。Finally, the diameter of the optical fiber preform prepared by the present invention can reach 215mm, the drawing length of a single preform can reach 2930km, the attenuation of the prepared optical fiber at 1310nm wavelength is as low as 0.298dB/km, and the attenuation coefficient at 1383nm wavelength is as low as 0.265dB/km, the attenuation coefficient at the wavelength of 1550nm is as low as 0.165dB/km, and the cut-off wavelength of the fiber is 1265nm~1273nm.
具体实施方式detailed description
需要说明的是,在不冲突的情况下,本申请中的实施例及实施例中的特征可以相互组合。It should be noted that the embodiments in this application and the features in the embodiments can be combined with each other if there is no conflict.
实施例1Example 1
本实施例提供一种大规格低衰减光纤预制棒的制备方法,包括如下步骤:This embodiment provides a method for preparing a large-size and low-attenuation optical fiber preform, which includes the following steps:
利用MCVD工艺在作为下陷层的掺F石英管内壁依次沉积内包层、外芯层和内芯层,获得沉积管,并将沉积管在2300℃下熔缩成具有内芯层、外芯层、内包层和下陷层的预制棒芯棒;The inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the F-doped quartz tube as the depressed layer using the MCVD process to obtain a deposited tube, and the deposited tube is fused at 2300°C to have an inner core layer, an outer core layer, Preformed rod core rods of inner cladding and sinking layer;
利用VAD工艺在预制棒芯棒上沉积第一外包层疏松体,并经过第一次烧结处理,制备出初级光纤预制棒;所述第一次烧结处理包括 脱羟处理、掺氟处理和玻璃化处理三个步骤,首先向烧结炉内通入He气和氯气,使待烧结的初级光纤预制棒在烧结炉内以3rpm的速度自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,加热线圈的移动速度为10mm/min,并使烧结炉内温度以25mm/min的升温速率达到900℃,保温2h,完成脱水处理;其次向烧结炉内通入SiF 4气体和He气,维持初级光纤预制棒的自转速度和加热线圈的上下移动,使烧结炉内温度以15mm/min的升温速率达到1100℃,保温3h,完成掺氟处理;最后向烧结炉内只通入He气,维持初级光纤预制棒的自转速度和加热线圈的上下移动,使烧结炉内温度以8mm/min的升温速率达到1400℃,保温4h,完成玻璃化处理; The first cladding loose body is deposited on the preform core rod by the VAD process, and the primary optical fiber preform is prepared after the first sintering treatment; the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification There are three processing steps. Firstly, He gas and chlorine gas are introduced into the sintering furnace, so that the primary optical fiber preform to be sintered rotates at a speed of 3rpm in the sintering furnace, and the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace. , The moving speed of the heating coil is 10mm/min, and the temperature in the sintering furnace reaches 900℃ at a heating rate of 25mm/min, and the temperature is kept for 2h to complete the dehydration treatment; secondly, SiF 4 gas and He gas are introduced into the sintering furnace to maintain The rotation speed of the primary optical fiber preform and the up and down movement of the heating coil make the temperature in the sintering furnace reach 1100°C at a heating rate of 15mm/min, hold for 3 hours, and complete the fluorine doping treatment; finally, only He gas is introduced into the sintering furnace to maintain The rotation speed of the primary optical fiber preform and the up and down movement of the heating coil make the temperature in the sintering furnace reach 1400 ℃ at a heating rate of 8 mm/min, and keep it for 4 hours to complete the vitrification process;
利用OVD工艺在初级光纤预制棒上沉积第二外包层疏松体,并经过第二次烧结处理,制备出光纤预制棒;所述第二次烧结处理包括脱羟处理和玻璃化处理两个步骤,首先向烧结炉内通入He气和氯气,使待烧结的光纤预制棒在烧结炉内以3rpm的自转速度自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,加热线圈的移动速度为10mm/min,并使烧结炉内温度以40mm/min的升温速率达到1000℃,保温4h,完成脱羟处理;再关闭氯气,向烧结炉内只通入惰性气体,使烧结炉内温度以10mm/min的升温速率达到1300℃,保温6h,完成玻璃化处理;The second cladding loose body is deposited on the primary optical fiber preform by the OVD process, and the optical fiber preform is prepared by the second sintering treatment; the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment, First, pass He gas and chlorine gas into the sintering furnace, so that the optical fiber preform to be sintered rotates at a rotation speed of 3 rpm in the sintering furnace. The gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace, and the heating coil moves The speed is 10mm/min, and the temperature in the sintering furnace reaches 1000℃ at a heating rate of 40mm/min, and the temperature is kept for 4 hours to complete the dehydroxylation treatment; then the chlorine gas is turned off, and only inert gas is introduced into the sintering furnace to make the temperature in the sintering furnace Reach 1300℃ at a heating rate of 10mm/min, keep it for 6 hours, and complete the vitrification process;
所述内芯层和外芯层为掺入P 2O 5-F混合物的二氧化硅玻璃层,内芯层的相对折射率Δn 1为0.35%,外芯层的相对折射率Δn 2为0.15%,所述外芯层直径b与内芯层直径a的比值b/a为1.5;所述内包层为 掺入Sb 2O 3-F混合物的二氧化硅玻璃层,内包层的相对折射率Δn 3为-0.2%,所述内包层直径c与内芯层直径a的比值c/a为3;所述下陷层的相对折射率Δn 4为-0.6%,所述下陷层直径d与内芯层直径a的比值d/a为5;所述第一外包层为掺F的二氧化硅玻璃层,第一外包层的相对折射率Δn 4为-0.35%,第一外包层直径e与内芯层直径a的比值e/a为10,光纤预制棒的直径f与内芯层直径a的比值f/a为15。 The inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index Δn 1 of the inner core layer is 0.35%, and the relative refractive index Δn 2 of the outer core layer is 0.15 %, the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 1.5; the inner cladding layer is a silica glass layer doped with Sb 2 O 3 -F mixture, and the relative refractive index of the inner cladding layer Δn 3 is -0.2%, the ratio c/a of the inner cladding diameter c to the inner core layer diameter a is 3; the relative refractive index Δn 4 of the sinking layer is -0.6%, and the sinking layer diameter d is The ratio d/a of the core layer diameter a is 5; the first cladding layer is an F-doped silica glass layer, the relative refractive index Δn 4 of the first cladding layer is -0.35%, and the first cladding layer diameter e is equal to The ratio e/a of the inner core diameter a is 10, and the ratio f/a of the diameter f of the optical fiber preform to the inner core diameter a is 15.
经测试,光纤预制棒的直径达到205mm,将制备的光纤预制棒在线拉制光纤,单根棒拉纤长度可达到2880km,拉丝后光纤在1310nm的衰耗为0.301dB/km,在1383nm的衰耗为0.265dB/km,在1550nm的衰耗为0.165dB/km,截止波长为1273nm。After testing, the diameter of the optical fiber preform reaches 205mm, and the prepared optical fiber preform is drawn into the fiber online. The length of a single rod can reach 2880km. After the drawing, the attenuation of the fiber at 1310nm is 0.301dB/km, and the attenuation at 1383nm It is 0.265dB/km, the attenuation at 1550nm is 0.165dB/km, and the cut-off wavelength is 1273nm.
实施例2Example 2
本实施例提供一种大规格低衰减光纤预制棒的制备方法,包括如下步骤:This embodiment provides a method for preparing a large-size and low-attenuation optical fiber preform, which includes the following steps:
利用MCVD工艺在作为下陷层的掺F石英管内壁依次沉积内包层、外芯层和内芯层,获得沉积管,并将沉积管在2400℃下熔缩成具有内芯层、外芯层、内包层和下陷层的预制棒芯棒;The inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the F-doped quartz tube as the depressed layer by the MCVD process to obtain a deposition tube, and the deposition tube is fused at 2400°C to have an inner core layer, an outer core layer, Preformed rod core rods of inner cladding and sinking layer;
利用VAD工艺在预制棒芯棒上沉积第一外包层疏松体,并经过第一次烧结处理,制备出初级光纤预制棒;所述第一次烧结处理包括脱羟处理、掺氟处理和玻璃化处理三个步骤,首先向烧结炉内通入He气和氯气,使待烧结的初级光纤预制棒在烧结炉内以6rpm的自转速度自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,加热线圈的移动速度为5mm/min,并使烧结炉内温度以35mm/min 的升温速率达到1100℃,保温1h,完成脱水处理;其次向烧结炉内通入CF 4气体和He气,维持初级光纤预制棒的自转速度和加热线圈的上下移动,使烧结炉内温度以25mm/min的升温速率达到1300℃,保温2h,完成掺氟处理;最后向烧结炉内只通入He气,维持初级光纤预制棒的自转速度和加热线圈的上下移动,使烧结炉内温度以15mm/min的升温速率达到1600℃,保温3h,完成玻璃化处理; The first cladding loose body is deposited on the preform core rod by the VAD process, and the primary optical fiber preform is prepared after the first sintering treatment; the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification There are three processing steps. Firstly, He gas and chlorine gas are introduced into the sintering furnace, so that the primary optical fiber preform to be sintered rotates at a rotation speed of 6 rpm in the sintering furnace. The up and down movement of the heating coil outside the sintering furnace can affect the gas inside the sintering furnace. Heating, the moving speed of the heating coil is 5mm/min, and the temperature in the sintering furnace reaches 1100℃ at a heating rate of 35mm/min, and the temperature is kept for 1h to complete the dehydration treatment; secondly, CF 4 gas and He gas are passed into the sintering furnace. Maintain the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil to make the temperature in the sintering furnace reach 1300°C at a heating rate of 25mm/min, hold for 2 hours, and complete the fluorine doping treatment; finally, only He gas is introduced into the sintering furnace. Maintain the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil, so that the temperature in the sintering furnace reaches 1600°C at a heating rate of 15 mm/min, and the temperature is kept for 3 hours to complete the vitrification process;
利用OVD工艺在初级光纤预制棒上沉积第二外包层疏松体,并经过第二次烧结处理,制备出光纤预制棒;所述第二次烧结处理包括脱羟处理和玻璃化处理两个步骤,首先向烧结炉内通入He气和氯气,使待烧结的光纤预制棒在烧结炉内以6rpm的速度自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,加热线圈的移动速度为5mm/min,并使烧结炉内温度以60mm/min的升温速率达到1200℃,保温2h,完成脱羟处理;再关闭氯气,向烧结炉内只通入He气,使烧结炉内温度以20mm/min的升温速率达到1500℃,保温4h,完成玻璃化处理;The second cladding loose body is deposited on the primary optical fiber preform by the OVD process, and the optical fiber preform is prepared by the second sintering treatment; the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment, First, pass He gas and chlorine gas into the sintering furnace, so that the optical fiber preform to be sintered rotates at a speed of 6 rpm in the sintering furnace. The gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace, and the moving speed of the heating coil The temperature in the sintering furnace is set to 5mm/min, and the temperature in the sintering furnace is increased to 1200℃ at a heating rate of 60mm/min, and the temperature is kept for 2 hours to complete the dehydroxylation treatment. The heating rate of 20mm/min reaches 1500℃, and the heat preservation is 4h to complete the vitrification treatment;
所述内芯层和外芯层为掺入P 2O 5-F混合物的二氧化硅玻璃层,内芯层的相对折射率Δn 1为0.45%,外芯层的相对折射率Δn 2为0.3%,所述外芯层直径b与内芯层直径a的比值b/a为2;所述内包层为掺入Sb 2O 3-F混合物的二氧化硅玻璃层,内包层的相对折射率Δn 3为-0.05%,所述内包层直径c与内芯层直径a的比值c/a为4;所述下陷层的相对折射率Δn 4为-0.45%,所述下陷层直径d与内芯层直径a的比值d/a为6.5;所述第一外包层为掺F的二氧化硅玻璃层,第一外包层的相 对折射率Δn 4为-0.25%,所述第一外包层直径e与内芯层直径a的比值e/a为11.5,光纤预制棒的直径f与内芯层直径a的比值f/a为17。 The inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index Δn 1 of the inner core layer is 0.45%, and the relative refractive index Δn 2 of the outer core layer is 0.3 %, the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 2; the inner cladding layer is a silica glass layer doped with Sb 2 O 3 -F mixture, and the relative refractive index of the inner cladding layer Δn 3 is -0.05%, the ratio c/a of the inner cladding diameter c to the inner core layer diameter a is 4; the relative refractive index Δn 4 of the depressed layer is -0.45%, and the depressed layer diameter d is The ratio d/a of the core layer diameter a is 6.5; the first outer cladding layer is an F-doped silica glass layer, and the relative refractive index Δn 4 of the first outer cladding layer is -0.25%. The ratio e/a of e to the inner core diameter a is 11.5, and the ratio f/a of the fiber preform diameter f to the inner core diameter a is 17.
经测试,光纤预制棒的直径达到215mm,将制备的光纤预制棒在线拉制光纤,单根棒拉纤长度可达到2930km,拉丝后光纤在1310nm的衰耗为0.302dB/km,在1383nm的衰耗为0.271dB/km,在1550nm的衰耗为0.171dB/km,截止波长为1265nm。After testing, the diameter of the optical fiber preform reaches 215mm. The prepared optical fiber preform is drawn on-line to draw the fiber. The length of a single rod can reach 2930km. After drawing, the fiber attenuation at 1310nm is 0.302dB/km and the attenuation at 1383nm. It is 0.271dB/km, the attenuation at 1550nm is 0.171dB/km, and the cut-off wavelength is 1265nm.
实施例3Example 3
本实施例提供一种大规格低衰减光纤预制棒的制备方法,包括如下步骤:This embodiment provides a method for preparing a large-size and low-attenuation optical fiber preform, which includes the following steps:
利用MCVD工艺在作为下陷层的掺F石英管内壁依次沉积内包层、外芯层和内芯层,获得沉积管,并将沉积管在2500℃下熔缩成具有内芯层、外芯层、内包层和下陷层的预制棒芯棒;The inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the F-doped quartz tube as the depressed layer using the MCVD process to obtain a deposited tube, and the deposited tube is fused at 2500°C to have an inner core layer, an outer core layer, Preformed rod core rods of inner cladding and sinking layer;
利用VAD工艺在预制棒芯棒上沉积第一外包层疏松体,并经过第一次烧结处理,制备出初级光纤预制棒;所述第一次烧结处理包括脱羟处理、掺氟处理和玻璃化处理三个步骤,首先向烧结炉内通入He气和氯气,使待烧结的初级光纤预制棒在烧结炉内以5rpm的速度自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,加热线圈的移动速度为8mm/min,并使烧结炉内温度以30mm/min的升温速率达到1000℃,保温1.5h,完成脱水处理;其次向烧结炉内通入SF 6气体和He气,维持初级光纤预制棒的自转速度和加热线圈的上下移动,使烧结炉内温度以20mm/min的升温速率达到1200℃,保温2.5h,完成掺氟处理;最后向烧结炉内只通入He气,维持初级 光纤预制棒的自转速度和加热线圈的上下移动,使烧结炉内温度以12mm/min的升温速率达到1500℃,保温3.5h,完成玻璃化处理; The first cladding loose body is deposited on the preform core rod by the VAD process, and the primary optical fiber preform is prepared after the first sintering treatment; the first sintering treatment includes dehydroxylation treatment, fluorine doping treatment and vitrification There are three processing steps. Firstly, He gas and chlorine gas are introduced into the sintering furnace to make the primary optical fiber preform to be sintered rotate at a speed of 5 rpm in the sintering furnace, and the gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace. , The moving speed of the heating coil is 8mm/min, and the temperature in the sintering furnace is reached to 1000℃ at a heating rate of 30mm/min, and the temperature is kept for 1.5h to complete the dehydration treatment; secondly, SF 6 gas and He gas are introduced into the sintering furnace. Maintain the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil, make the temperature in the sintering furnace reach 1200℃ at a heating rate of 20mm/min, hold for 2.5 hours, and complete the fluorine doping treatment; finally, only He gas is introduced into the sintering furnace , Maintain the rotation speed of the primary optical fiber preform and the up and down movement of the heating coil, so that the temperature in the sintering furnace reaches 1500°C at a heating rate of 12 mm/min, and keep it for 3.5 hours to complete the vitrification process;
利用OVD工艺在初级光纤预制棒上沉积第二外包层疏松体,并经过第二次烧结处理,制备出光纤预制棒;所述第二次烧结处理包括脱羟处理和玻璃化处理两个步骤,首先向烧结炉内通入He气和氯气,使待烧结的光纤预制棒在烧结炉内以5rpm的速度自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,加热线圈的移动速度为8mm/min,并使烧结炉内温度以50mm/min的升温速率达到1100℃,保温3h,完成脱羟处理;再关闭氯气,向烧结炉内只通入He气,使烧结炉内温度以15mm/min的升温速率达到1400℃,保温6h,完成玻璃化处理;The second cladding loose body is deposited on the primary optical fiber preform by the OVD process, and the optical fiber preform is prepared by the second sintering treatment; the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment, First, pass He gas and chlorine gas into the sintering furnace, so that the optical fiber preform to be sintered rotates at a speed of 5 rpm in the sintering furnace. The gas inside the sintering furnace is heated by the up and down movement of the heating coil outside the sintering furnace, and the moving speed of the heating coil The temperature in the sintering furnace is 8mm/min, and the temperature in the sintering furnace reaches 1100°C at a heating rate of 50mm/min, and the temperature is kept for 3 hours to complete the dehydroxylation treatment; The heating rate of 15mm/min reaches 1400℃, and the temperature is kept for 6 hours to complete the vitrification process;
所述内芯层和外芯层为掺入P 2O 5-F混合物的二氧化硅玻璃层,内芯层的相对折射率Δn 1为0.4%,外芯层的相对折射率Δn 2为0.2%,所述外芯层直径b与内芯层直径a的比值b/a为1.7;所述内包层为掺入Sb 2O 3-F混合物的二氧化硅玻璃层,内包层的相对折射率Δn 3为-0.1%,所述内包层直径c与内芯层直径a的比值c/a为3.5;所述下陷层的相对折射率Δn 4为-0.5%,所述下陷层直径d与内芯层直径a的比值d/a为6;所述第一外包层为掺F的二氧化硅玻璃层,第一外包层的相对折射率Δn 4为-0.3%,所述第一外包层直径e与内芯层直径a的比值e/a为11,所述光纤预制棒的直径f与内芯层直径a的比值f/a为16。 The inner core layer and the outer core layer are silica glass layers doped with P 2 O 5 -F mixture, the relative refractive index Δn 1 of the inner core layer is 0.4%, and the relative refractive index Δn 2 of the outer core layer is 0.2 %, the ratio b/a of the outer core layer diameter b to the inner core layer diameter a is 1.7; the inner cladding layer is a silica glass layer doped with Sb 2 O 3 -F mixture, and the relative refractive index of the inner cladding layer Δn 3 is -0.1%, the ratio c/a of the inner cladding diameter c to the inner core layer diameter a is 3.5; the relative refractive index Δn 4 of the sinking layer is -0.5%, and the sinking layer diameter d is The ratio d/a of the core layer diameter a is 6; the first cladding layer is an F-doped silica glass layer, the relative refractive index Δn 4 of the first cladding layer is -0.3%, and the diameter of the first cladding layer is The ratio e/a of e to the inner core diameter a is 11, and the ratio f/a of the diameter f of the optical fiber preform to the inner core diameter a is 16.
经测试,光纤预制棒的直径达到210mm,将制备的光纤预制棒在线拉制低损耗光纤,单根棒拉纤长度可达到2915km,拉丝后光纤 在1310nm的衰耗为0.298dB/km,在1383nm的衰耗为0.272dB/km,在1550nm的衰耗为0.168dB/km,截止波长为1268nm。After testing, the diameter of the optical fiber preform reaches 210mm. The prepared optical fiber preform is drawn online to draw a low-loss optical fiber. The length of a single rod can reach 2915km. After the drawing, the attenuation of the fiber at 1310nm is 0.298dB/km. The attenuation is 0.272dB/km, the attenuation at 1550nm is 0.168dB/km, and the cut-off wavelength is 1268nm.
以上述依据本申请的理想实施例为启示,通过上述的说明内容,相关工作人员完全可以在不偏离本项申请技术思想的范围内,进行多样的变更以及修改。本项申请的技术性范围并不局限于说明书上的内容,必须要根据权利要求范围来确定其技术性范围。Taking the above-mentioned ideal embodiment based on this application as enlightenment, through the above description content, relevant staff can make various changes and modifications without departing from the technical idea of this application. The technical scope of this application is not limited to the content in the specification, and its technical scope must be determined according to the scope of the claims.

Claims (10)

  1. 一种大规格低衰减光纤预制棒的制备方法,其特征在于,包括如下步骤:A method for preparing a large-size low-attenuation optical fiber preform is characterized in that it comprises the following steps:
    利用MCVD工艺在作为下陷层的石英管内壁依次沉积内包层、外芯层和内芯层,获得沉积管,并将沉积管在高温下熔缩成具有内芯层、外芯层、内包层和下陷层的预制棒芯棒;The inner cladding layer, the outer core layer and the inner core layer are sequentially deposited on the inner wall of the quartz tube as the depressed layer using the MCVD process to obtain a deposition tube, and the deposition tube is fused at high temperature to have an inner core layer, an outer core layer, an inner cladding layer and Preformed rod mandrel of the sunken layer;
    利用VAD工艺在预制棒芯棒上沉积第一外包层疏松体,并经过第一次烧结处理,制备出初级光纤预制棒;Use the VAD process to deposit the first cladding loose body on the preform core rod, and pass the first sintering treatment to prepare the primary optical fiber preform;
    利用OVD工艺在初级光纤预制棒上沉积第二外包层疏松体,并经过第二次烧结处理,制备出光纤预制棒;Use the OVD process to deposit the loose body of the second outer cladding layer on the primary optical fiber preform, and pass the second sintering treatment to prepare the optical fiber preform;
    所述内芯层、外芯层、内包层、下陷层、第一外包层以二氧化硅作为基底材料并加入掺杂剂,第二外包层为纯二氧化硅,内芯层、外芯层、内包层、下陷层、第一外包层的相对折射率依次为Δn 1、Δn 2、Δn 3、Δn 4、Δn 5,相对折射率大小为:Δn 1>Δn 2>0>Δn 3>Δn 5>Δn 4The inner core layer, the outer core layer, the inner cladding layer, the recessed layer, and the first outer cladding layer use silica as the base material and adding dopants, the second outer cladding layer is pure silica, the inner core layer and the outer core layer The relative refractive index of the inner cladding layer, the depressed layer, and the first outer cladding layer are Δn 1 , Δn 2 , Δn 3 , Δn 4 , Δn 5 , and the relative refractive index is: Δn 1 >Δn 2 >0>Δn 3 >Δn 5 >Δn 4 .
  2. 根据权利要求1所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述第一次烧结处理或第二次烧结处理方法为:使待烧结的初级光纤预制棒或光纤预制棒在烧结炉内自转,通过烧结炉外加热线圈的上下移动对烧结炉内部气体加热,完成烧结,加热线圈的移动速度优选为5-10mm/min,自转速度优选为3-6rpm。The method for preparing a large-format low-attenuation optical fiber preform according to claim 1, wherein the first sintering treatment or the second sintering treatment method is: making the primary optical fiber preform to be sintered or the optical fiber preform Rotate in the sintering furnace, and heat the gas inside the sintering furnace by moving up and down the heating coil outside the sintering furnace to complete sintering. The moving speed of the heating coil is preferably 5-10 mm/min, and the rotation speed is preferably 3-6 rpm.
  3. 根据权利要求1或2所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述第一次烧结处理包括脱羟处理、掺氟处理和玻璃化处理三个步骤,首先向烧结炉内通入惰性气体和氯气, 使烧结炉内温度以25~35mm/min的升温速率达到900~1100℃,保温1-2h,完成脱羟处理;其次向烧结炉内通入含氟气体和惰性气体,使烧结炉内温度以15~25mm/min的升温速率达到1100~1300℃,保温2-3h,完成掺氟处理;最后向烧结炉内只通入惰性气体,使烧结炉内温度以8~15mm/min的升温速率达到1400~1600℃,保温3-4h,完成玻璃化处理。The method for preparing a large-format low-attenuation optical fiber preform according to claim 1 or 2, wherein the first sintering treatment includes three steps of dehydroxylation treatment, fluorine doping treatment and vitrification treatment. Inert gas and chlorine gas are introduced into the furnace to make the temperature in the sintering furnace reach 900-1100°C at a heating rate of 25-35mm/min, and hold for 1-2h to complete the dehydroxylation treatment; secondly, fluorine-containing gas and gas are introduced into the sintering furnace Inert gas, make the temperature in the sintering furnace reach 1100-1300℃ at a heating rate of 15-25mm/min, keep the temperature for 2-3h, and complete the fluorine doping treatment; finally, only inert gas is introduced into the sintering furnace to make the temperature in the sintering furnace below The heating rate of 8~15mm/min reaches 1400~1600℃, and the temperature is kept for 3-4h to complete the vitrification process.
  4. 根据权利要求1-3任一项所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述第二次烧结处理包括脱羟处理和玻璃化处理两个步骤,首先向烧结炉内通入惰性气体和氯气,使烧结炉内温度以40~60mm/min的升温速率达到1000~1200℃,保温2-4h,完成脱羟处理;再关闭氯气,向烧结炉内只通入惰性气体,使烧结炉内温度以10~20mm/min的升温速率达到1300~1500℃,保温4-6h,完成玻璃化处理。The method for preparing a large-format low-attenuation optical fiber preform according to any one of claims 1 to 3, wherein the second sintering treatment includes two steps of dehydroxylation treatment and vitrification treatment. Inert gas and chlorine gas are introduced to make the temperature in the sintering furnace reach 1000-1200°C at a heating rate of 40-60 mm/min, and hold for 2-4 hours to complete the dehydroxylation treatment; then turn off the chlorine gas and pass only inert gas into the sintering furnace Use gas to make the temperature in the sintering furnace reach 1300-1500°C at a heating rate of 10-20mm/min, keep it for 4-6h, and complete the vitrification process.
  5. 根据权利要求1-4任一项所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述内芯层和外芯层为掺入P 2O 5-F混合物的二氧化硅玻璃层,内芯层的相对折射率Δn 1为0.35%~0.45%,外芯层的相对折射率Δn 2为0.15%~0.3%,所述外芯层直径b与内芯层直径a的比值b/a为1.5-2。 The method for preparing a large-size low-attenuation optical fiber preform according to any one of claims 1 to 4, wherein the inner core layer and the outer core layer are silica doped with P 2 O 5 -F mixture Glass layer, the relative refractive index Δn 1 of the inner core layer is 0.35% to 0.45%, the relative refractive index Δn 2 of the outer core layer is 0.15% to 0.3%, and the ratio of the diameter b of the outer core layer to the diameter a of the inner core layer b/a is 1.5-2.
  6. 根据权利要求1-5任一项所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述内包层为掺入Sb 2O 3-F混合物的二氧化硅玻璃层,内包层的相对折射率Δn 3为-0.2%~-0.05%,所述内包层直径c与内芯层直径a的比值c/a为3-4。 The method for preparing a large-format low-attenuation optical fiber preform according to any one of claims 1-5, wherein the inner cladding is a silica glass layer doped with Sb 2 O 3 -F mixture, and the inner cladding The relative refractive index Δn 3 is -0.2% to -0.05%, and the ratio c/a of the inner cladding diameter c to the inner core diameter a is 3-4.
  7. 根据权利要求1-6任一项所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述下陷层为掺F的二氧化硅玻璃层,下陷层的相对折射率Δn 4为-0.6%~-0.45%,所述下陷层直径d与内芯层直径a的比值d/a为5-6.5。 The method for preparing a large-format low-attenuation optical fiber preform according to any one of claims 1-6, wherein the depressed layer is an F-doped silica glass layer, and the relative refractive index Δn 4 of the depressed layer is -0.6% to -0.45%, the ratio d/a of the diameter d of the sinking layer to the diameter a of the inner core layer is 5-6.5.
  8. 根据权利要求1-7任一项所述的大规格低衰减光纤预制棒的制备方法,其特征在于,所述第一外包层为掺F的二氧化硅玻璃层,第一外包层的相对折射率Δn 4为-0.35%~-0.25%,所述第一外包层直径e与内芯层直径a的比值e/a为10-11.5,所述光纤预制棒的直径f与内芯层直径a的比值f/a为15-17。 The method for preparing a large-format low-attenuation optical fiber preform according to any one of claims 1-7, wherein the first cladding layer is an F-doped silica glass layer, and the relative refractive index of the first cladding layer is The ratio Δn 4 is -0.35% to -0.25%, the ratio e/a of the diameter e of the first outer cladding layer to the diameter a of the inner core layer is 10-11.5, and the diameter f of the optical fiber preform and the inner core layer diameter a The ratio f/a is 15-17.
  9. 一种由权利要求1-8任一项所述的方法制造的光纤预制棒。An optical fiber preform manufactured by the method of any one of claims 1-8.
  10. 一种光纤,其特征在于,所述光纤由权利要求1-8任一项所述的光纤预制棒直接拉丝而成,或经拉伸后再拉丝而成。An optical fiber, characterized in that the optical fiber is formed by directly drawing the optical fiber preform according to any one of claims 1-8, or formed by drawing after drawing.
PCT/CN2019/114407 2019-03-11 2019-10-30 Large-size low-attenuation optical fiber preform and preparation method therefor WO2020181791A1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910181908.XA CN109970335B (en) 2019-03-11 2019-03-11 Large-size low-attenuation optical fiber preform and preparation method thereof
CN201910181908.X 2019-03-11

Publications (1)

Publication Number Publication Date
WO2020181791A1 true WO2020181791A1 (en) 2020-09-17

Family

ID=67078407

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2019/114407 WO2020181791A1 (en) 2019-03-11 2019-10-30 Large-size low-attenuation optical fiber preform and preparation method therefor

Country Status (2)

Country Link
CN (1) CN109970335B (en)
WO (1) WO2020181791A1 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109970335B (en) * 2019-03-11 2020-11-17 江苏永鼎股份有限公司 Large-size low-attenuation optical fiber preform and preparation method thereof
CN111253059A (en) * 2020-03-10 2020-06-09 杭州金星通光纤科技有限公司 Dehydration sintering device and method for optical fiber preform
CN111646689A (en) * 2020-06-28 2020-09-11 浙江富通光纤技术有限公司 Preparation method of pure silica core optical fiber preform

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1483007A (en) * 2000-12-22 2004-03-17 康宁股份有限公司 Treating soot preforms with a reducing agent
CN101891380A (en) * 2010-07-13 2010-11-24 长飞光纤光缆有限公司 Large-size optical fiber preform and manufacturing method of optical fiber thereof
US20120033924A1 (en) * 2005-06-29 2012-02-09 Lance Gibson Low loss optical fiber designs and methods for their manufacture
CN105217951A (en) * 2015-09-21 2016-01-06 长飞光纤光缆股份有限公司 A kind of stretched vertically method and apparatus of preform
CN109970335A (en) * 2019-03-11 2019-07-05 江苏永鼎股份有限公司 A kind of preform and preparation method thereof of the low decaying of big specification

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102944910B (en) * 2012-10-30 2015-07-22 长飞光纤光缆股份有限公司 Single-mode fiber with larger effective area
US9110220B2 (en) * 2013-07-16 2015-08-18 Corning Incorporated High bandwidth MMF and method of making
CN103941334A (en) * 2014-04-21 2014-07-23 长飞光纤光缆股份有限公司 Low-attenuation single mode fiber
CN104698534B (en) * 2015-03-31 2017-11-17 长飞光纤光缆股份有限公司 A kind of low decay less fundamental mode optical fibre
CN107678087A (en) * 2017-11-07 2018-02-09 长飞光纤光缆股份有限公司 A kind of low attenuation large effective area single-mode fiber
CN108469648B (en) * 2018-05-14 2020-05-05 烽火通信科技股份有限公司 Ultralow-loss large-effective-area single-mode fiber and manufacturing method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1483007A (en) * 2000-12-22 2004-03-17 康宁股份有限公司 Treating soot preforms with a reducing agent
US20120033924A1 (en) * 2005-06-29 2012-02-09 Lance Gibson Low loss optical fiber designs and methods for their manufacture
CN101891380A (en) * 2010-07-13 2010-11-24 长飞光纤光缆有限公司 Large-size optical fiber preform and manufacturing method of optical fiber thereof
CN105217951A (en) * 2015-09-21 2016-01-06 长飞光纤光缆股份有限公司 A kind of stretched vertically method and apparatus of preform
CN109970335A (en) * 2019-03-11 2019-07-05 江苏永鼎股份有限公司 A kind of preform and preparation method thereof of the low decaying of big specification

Also Published As

Publication number Publication date
CN109970335A (en) 2019-07-05
CN109970335B (en) 2020-11-17

Similar Documents

Publication Publication Date Title
AU2012203014B2 (en) Single mode optical fiber
WO2020181791A1 (en) Large-size low-attenuation optical fiber preform and preparation method therefor
CN102249533B (en) Method for manufacturing large-size low-water-peak prefabricated rod
EP1942081B1 (en) Extended baking process for quartz glass deposition tubes.
CN102757179B (en) Method for preparing large-size optical fiber preform
CN109665713B (en) Low water peak large-size optical fiber preform and manufacturing method thereof
WO2019085693A1 (en) Preparation of ultra-low loss optical fiber preform and optical fiber by means of axial vapor deposition
JP5590617B2 (en) Manufacturing method of optical fiber preform having low refractive index portion at a position separated from core
JP2011526879A5 (en) Method for forming a bending-resistant optical fiber
CN109553295B (en) Large-size low-loss optical fiber preform and manufacturing method thereof
WO2020177355A1 (en) Single-mode optical fiber having ultra-low loss and large effective area and preparation method therefor
CN108585470B (en) Device and method for preparing high germanium-doped core rod by VAD (vapor axial deposition)
CN113213752B (en) Method for preparing ultralow-loss optical fiber preform and optical fiber by external gas phase deposition method
WO2020119439A1 (en) Single-mode optical fiber having low loss and large effective area and preparation method therefor
CN104909557A (en) MCVD (modified chemical vapor deposition) device for preparing rare earth doped optical fiber performs
CN104291676A (en) Method for producing large-size bending insensitive multi-mode optical fiber preforms
WO2020155707A1 (en) Optical fiber preform rod of large size and low loss and preparation method therefor
CN111646689A (en) Preparation method of pure silica core optical fiber preform
CN103760634B (en) Single mode fiber
CN109942182B (en) Optical fiber preform manufacturing method based on sleeve method
WO2020181787A1 (en) Optical fiber with high core-cladding concentricity and preparation method therefor
CN111847867B (en) Optical fiber preform and preparation method thereof
CN101066834B (en) Process of preparing fiber preformrod
WO2020177352A1 (en) Optical fiber preform based on continuous fused quartz bushing, and manufacturing method therefor
CN109399910B (en) Large-core-diameter optical fiber preform and preparation method of optical fiber

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: 19918956

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: 19918956

Country of ref document: EP

Kind code of ref document: A1