WO2020181788A1 - Method for manufacturing optical fiber preform based on sleeve method - Google Patents

Method for manufacturing optical fiber preform based on sleeve method Download PDF

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Publication number
WO2020181788A1
WO2020181788A1 PCT/CN2019/114352 CN2019114352W WO2020181788A1 WO 2020181788 A1 WO2020181788 A1 WO 2020181788A1 CN 2019114352 W CN2019114352 W CN 2019114352W WO 2020181788 A1 WO2020181788 A1 WO 2020181788A1
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WIPO (PCT)
Prior art keywords
optical fiber
rod
core rod
diameter
mother
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PCT/CN2019/114352
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French (fr)
Chinese (zh)
Inventor
莫思铭
李凡
眭立洪
张国栋
周莉
李想
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江苏永鼎光纤科技有限公司
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Publication of WO2020181788A1 publication Critical patent/WO2020181788A1/en

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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
    • 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
    • C03B37/02Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
    • C03B37/025Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms

Definitions

  • the invention relates to a method for manufacturing an optical fiber preform based on a sleeve method, and belongs to the field of optical fiber preform manufacturing.
  • MCVD chemical vapor deposition
  • PCVD microwave plasma chemical vapor deposition
  • OLED external vapor deposition
  • VAD axial vapor deposition
  • MCVD and PCVD In-tube deposition methods
  • VAD and OVD directly manufactures mandrels with large outer diameters, and the cost is high, which cannot reflect the advantages of using the casing method to manufacture large-size preforms.
  • the tube method is to insert a core rod into a quartz tube to form an optical fiber preform. It is a better method for manufacturing large-size optical fiber preforms.
  • strict control of the core rod and the tube is required.
  • the fiber preform based on the tube method requires the bow and the uniformity of the diameter of the fiber core rod, and the current fiber preform prepared based on the tube method It is difficult to ensure the uniformity of bow and diameter of the core rod of the rod, resulting in large loss of the optical fiber preform prepared by the sleeve method.
  • the technical problem to be solved by the present invention is to provide a method for manufacturing an optical fiber preform based on the sleeve method to solve the technical problem that the core rod bow and diameter uniformity of the optical fiber preform prepared based on the sleeve method is difficult to ensure.
  • a method for manufacturing an optical fiber preform based on the sleeve method the steps are as follows:
  • the optical fiber core rod mother rod being a core layer and an inner cladding layer from the inside to the outside;
  • the fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1 mm/m;
  • the stretching method is: the two ends of the fiber core rod mother rod are respectively connected to the drawing rod and Pull down the lead rod, and make the mother rod of the optical fiber core rod vertically pass through the drawing furnace, make the upper drawing lead rod and the lower drawing lead rod synchronously rotate at the same speed, and turn on the drawing furnace to set the mother rod of the optical fiber core rod. Heat from bottom to top and make the upper drawing rod move upward.
  • the upward moving speed of the upper drawing rod depends on the required diameter of the mandrel after drawing, the speed at which the drawing furnace moves upward, and the fiber core of the drawn section
  • the diameter of the rod mother rod is calculated in advance before stretching;
  • the OVD process is used to deposit the depressed layer loose body on the outside of the stretched optical fiber core rod, and then perform sintering treatment to obtain a synthetic core rod;
  • the synthetic mandrel After the surface of the synthetic mandrel is corroded, cleaned and dried, it is inserted into the quartz sleeve to form an optical fiber preform.
  • V 1 k ⁇ V 2 ⁇ V 3 (D 1 2 -D 2 2 )/D 1 2 is satisfied during the heating and drawing process of the mother rod of the optical fiber core rod, where V 1 is the upper drawing rod Real-time moving speed, V 2 is the rotation speed of the fiber core rod mother rod, V 3 is the preset moving speed of the drawing furnace upwards, D 1 is the diameter of the fiber core rod mother rod of the stretched section, D 2 is the drawing after the required diameter of the mandrel, k is 0.1-0.15, V 2 of 6-9mm / min, V 3 of 30-40mm / min.
  • the temperature at which the drawing furnace heats the mother rod of the optical fiber core rod is controlled at 1800-2300°C, and the heating area is filled with inert gas during heating.
  • the sintering treatment method is as follows: pass inert gas and chlorine gas into the sintering furnace, first raise the sintering furnace to 1000-1200°C at a heating rate of 50-60°C/min, keep it for 2-3h, and then heat it for 20 The temperature rise rate of -30°C/min is increased to 1300-1500°C, and the temperature is kept for 5-6h.
  • the sintered synthetic mandrel is heat-treated, and the heat treatment method is as follows: the synthetic mandrel, which has been kept at 1300-1500°C for 5-6h, is cooled to a temperature of ⁇ 100°C with a coolant within 2 minutes, and then cooled The latter synthetic mandrel is heated to 600-800°C for 2 to 3 hours.
  • the steps of using the VAD process to prepare the optical fiber core rod mother rod are: firstly deposit the powder core rod by the axial vapor deposition method, and then perform the dehydroxylation treatment, fluorine doping treatment and vitrification treatment on the powder core rod in the sintering furnace :
  • dehydroxylation treatment pass Cl 2 gas and inert gas into the sintering furnace, and the dehydroxylation temperature is 800-1000°C;
  • fluorine doping treatment pass fluorine-containing gas and inert gas into the sintering furnace, and the sintering furnace temperature It is 1000 ⁇ 1300°C; during vitrification, only inert gas is introduced into the sintering furnace, and the glass transition temperature is 1400 ⁇ 1600°C.
  • the core layer is a silica glass layer doped with P 2 O 5 , the relative refractive index ⁇ n 1 of the core layer is 0.35% to 0.5%, and the inner cladding layer and the depression layer are fluorine-doped silica
  • the relative refractive index ⁇ n 2 of the inner cladding layer is -0.05% to -0.01%, and the relative refractive index ⁇ n 3 of the depressed layer is -0.25% to -0.1%.
  • the ratio b/a of the diameter b of the fiber core rod to the core diameter a after stretching is 3.0 to 5.0
  • the ratio c/a of the diameter c of the composite core rod to the core diameter a is 7 to 9
  • the optical fiber is prefabricated
  • the ratio d/c of the effective diameter d of the rod to the diameter c of the composite core rod is 2.5 to 3.5.
  • 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 drawing directly from the above-mentioned optical fiber preform, or formed by drawing after drawing.
  • the present invention uses the VAD process to prepare an optical fiber core rod mother rod including a core layer and an inner cladding layer, and then heats and stretches the optical fiber core rod mother rod to make the bow of the optical fiber core rod less than 1 mm/m after drawing, and then passes through OVD
  • the process prepares the sink layer, and finally inserts the synthetic core rod into the quartz sleeve to form an optical fiber preform, where:
  • the fiber core rod mother rod is stretched vertically upwards.
  • the diameter of each position of the mother rod is scanned in advance to calculate the upper stretching guide during the stretching process.
  • the upward moving speed of the rod controls the coaxiality of the mandrel after stretching and ensures the bow and diameter uniformity of the mandrel after stretching; further, after the powder mandrel is prepared by the VAD method, a reasonable
  • the dehydroxylation, fluorine doping and vitrification process can not only effectively remove the hydroxyl groups, but also optimize the viscosity matching of the core and cladding, reduce the Rayleigh scattering of the drawn fiber, and achieve the purpose of low loss;
  • the dopant, refractive index and diameter of the core layer, inner cladding layer and sink layer are reasonably limited, which can ensure the fiber length of the optical fiber preform and reduce the attenuation coefficient of the optical fiber.
  • the quartz sleeve is used as the optical fiber preform.
  • the outer cladding material can effectively reduce the manufacturing cost of optical fiber preform;
  • the diameter of the optical fiber preform prepared by the present invention can reach 221mm
  • the drawing length of a single preform can reach 2995km
  • the fiber attenuation at 1310nm wavelength is ⁇ 0.305dB/km
  • the attenuation coefficient at 1383nm wavelength is ⁇ 0.275dB/km
  • the attenuation coefficient at 1550nm wavelength is ⁇ 0.165dB/km.
  • This embodiment provides a method for manufacturing an optical fiber preform based on the sleeve method, and the steps are as follows:
  • the optical fiber core rod mother rod is prepared by the VAD process.
  • the optical fiber core rod mother rod has a core layer and an inner cladding layer from the inside to the outside.
  • the core layer is a silica glass layer doped with P 2 O 5 , and the core layer is
  • the relative refractive index ⁇ n 1 is 0.35%
  • the inner cladding layer is a fluorine-doped silica glass layer
  • the relative refractive index ⁇ n 2 of the inner cladding layer is -0.05%;
  • the specific steps for preparing the optical fiber core rod mother rod are: first use the shaft
  • the powder core rod is deposited by the vapor deposition method, and then the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, Cl 2 gas and helium gas are passed into the sintering furnace,
  • the dehydroxylation temperature is 800°C; during fluorine doping treatment, fluorine
  • the fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1mm/m, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a after stretching is 3.0;
  • the stretching method is as follows: connect the two ends of the optical fiber core rod mother rod to the upper and lower drawing lead rods respectively, and make the optical fiber core rod mother rod vertically pass through the drawing furnace, so that the upper drawing lead rod and The lower drawing rod rotates synchronously at the same speed, the drawing furnace is turned on to heat the fiber core rod mother rod from bottom to top, and the upper drawing rod is moved upward, and the upward moving speed of the upper drawing rod is according to After stretching, the required diameter of the core rod, the upward moving speed of the stretching furnace, and the diameter of the fiber core rod mother rod of the stretched section are calculated in advance before stretching.
  • V 1 k ⁇ V 2 ⁇ V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, and V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset upward moving speed of the stretching furnace, D 1 is the diameter of the fiber core rod mother rod of the stretched section, and D 2 is the required diameter of the core rod after stretching, the k is 0.1, the V 2 is 9 mm/min, the V 3 is 30 mm/min, the temperature at which the drawing furnace heats the optical fiber core rod mother rod is controlled at 1800°C, and helium is filled in the heating area during heating;
  • the depressed layer loose body is deposited on the outside of the stretched fiber core rod by the OVD process, and then sintering and heat treatment are sequentially performed to obtain a synthetic core rod.
  • the depressed layer is a fluorine-doped silica glass layer, and the relative refraction of the depressed layer
  • the ratio ⁇ n 3 is -0.25%, and the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 7
  • the sintering method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first
  • the heating rate of 50°C/min is increased to 1000°C and the temperature is kept for 3 hours, and then the temperature rise rate of 20°C/min is raised to 1300°C and the temperature is kept for 6 hours
  • the heat treatment method is: the synthetic mandrel is heated at 1300°C for 6 hours Use cooling liquid to cool to a temperature of ⁇ 100°C within 2 minutes, and
  • the surface of the synthetic mandrel is etched with a mixture of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm. Then the corroded synthetic mandrel is cleaned and dried, and then the synthetic mandrel is inserted into the quartz sleeve.
  • the tube is assembled into an optical fiber preform, and the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 2.5.
  • the diameter of the optical fiber preform reaches 203mm, and the prepared optical fiber preform is drawn on-line.
  • the length of a single rod can reach 2865km.
  • the fiber attenuation at 1310nm is 0.302dB/km, and the attenuation at 1383nm It is 0.271dB/km, and the attenuation at 1550nm is 0.163dB/km.
  • This embodiment provides a method for manufacturing an optical fiber preform based on the sleeve method, and the steps are as follows:
  • the optical fiber core rod mother rod is prepared by the VAD process.
  • the optical fiber core rod mother rod has a core layer and an inner cladding layer from the inside to the outside.
  • the core layer is a silica glass layer doped with P 2 O 5 , and the core layer is
  • the relative refractive index ⁇ n 1 is 0.5%
  • the inner cladding layer is a fluorine-doped silica glass layer
  • the relative refractive index ⁇ n 2 of the inner cladding layer is -0.01%
  • the specific steps for preparing the optical fiber core rod mother rod are:
  • the powder core rod is deposited by the vapor deposition method, and then the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, Cl 2 gas and helium gas are passed into the sintering furnace,
  • the dehydroxylation temperature is 1000°C; during fluorine doping treatment, fluorine-containing gas and heli
  • the fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1 mm/m, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a after stretching is 5.0;
  • the stretching method is as follows: connect the two ends of the optical fiber core rod mother rod to the upper and lower drawing lead rods respectively, and make the optical fiber core rod mother rod vertically pass through the drawing furnace, so that the upper drawing lead rod and The lower drawing rod rotates synchronously at the same speed, the drawing furnace is turned on to heat the fiber core rod mother rod from bottom to top, and the upper drawing rod is moved upward, and the upward moving speed of the upper drawing rod is according to After stretching, the required diameter of the core rod, the upward moving speed of the stretching furnace, and the diameter of the fiber core rod mother rod of the stretched section are calculated in advance before stretching.
  • V 1 k ⁇ V 2 ⁇ V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, and V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset upward moving speed of the stretching furnace, D 1 is the diameter of the fiber core rod mother rod of the stretched section, and D 2 is the required diameter of the core rod after stretching, the k is 0.15, the V 2 is 6 mm/min, and the V 3 is 40 mm/min.
  • the temperature of the fiber core rod mother rod heated by the drawing furnace is controlled at 2300°C, and helium is filled in the heating area during heating;
  • the depressed layer loose body is deposited on the outside of the stretched fiber core rod by the OVD process, and then sintering and heat treatment are sequentially performed to obtain a synthetic core rod.
  • the depressed layer is a fluorine-doped silica glass layer, and the relative refraction of the depressed layer
  • the rate ⁇ n 3 is -0.1%, and the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 9
  • the sintering method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first
  • the temperature rise rate of 60°C/min is increased to 1200°C and the temperature is kept for 2 hours, and then the temperature rise rate is 30°C/min to 1500°C and the temperature is kept for 5 hours
  • the heat treatment method is: the synthetic core rod after being kept at 1500°C for 5 hours Use cooling liquid to cool to a temperature of ⁇ 100°C within 2 minutes, and then heat the
  • the surface of the synthetic mandrel is etched with a mixture of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm. Then the corroded synthetic mandrel is cleaned and dried, and then the synthetic mandrel is inserted into the quartz sleeve In the tube, the optical fiber preform is assembled, and the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 3.5.
  • the diameter of the optical fiber preform reaches 221mm.
  • the prepared optical fiber preform is drawn into the optical fiber online.
  • the length of a single rod can reach 2995km.
  • the fiber attenuation at 1310nm is 0.305dB/km, and the attenuation at 1383nm. It is 0.275dB/km, and the attenuation at 1550nm is 0.165dB/km.
  • This embodiment provides a method for manufacturing an optical fiber preform based on the sleeve method, and the steps are as follows:
  • the optical fiber core rod mother rod is prepared by the VAD process.
  • the optical fiber core rod mother rod has a core layer and an inner cladding layer from the inside to the outside.
  • the core layer is a silica glass layer doped with P 2 O 5 , and the core layer is
  • the relative refractive index ⁇ n 1 is 0.4%
  • the inner cladding layer is a fluorine-doped silica glass layer
  • the relative refractive index ⁇ n 2 of the inner cladding layer is -0.08%;
  • the specific steps for preparing the optical fiber core rod mother rod are:
  • the powder core rod is deposited by the vapor deposition method, and then the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, Cl 2 gas and helium gas are passed into the sintering furnace,
  • the dehydroxylation temperature is 900°C; during fluorine doping treatment, fluorine-containing gas and
  • the fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1mm/m, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a after stretching is 4.0;
  • the stretching method is as follows: connect the two ends of the optical fiber core rod mother rod to the upper and lower drawing lead rods respectively, and make the optical fiber core rod mother rod vertically pass through the drawing furnace, so that the upper drawing lead rod and The lower drawing rod rotates synchronously at the same speed, the drawing furnace is turned on to heat the fiber core rod mother rod from bottom to top, and the upper drawing rod is moved upward, and the upward moving speed of the upper drawing rod is according to After stretching, the required diameter of the core rod, the upward moving speed of the stretching furnace, and the diameter of the fiber core rod mother rod of the stretched section are calculated in advance before stretching.
  • V 1 k ⁇ V 2 ⁇ V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, and V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset moving speed of the stretching furnace upward, D 1 is the diameter of the fiber core rod mother rod of the stretched section, D 2 is the required diameter of the core rod after stretching, the k is 0.12, the V 2 is 8 mm/min, the V 3 is 35 mm/min, the temperature at which the drawing furnace heats the optical fiber core rod mother rod is controlled at 2000° C., and helium is filled in the heating area during heating;
  • the depressed layer loose body is deposited on the outside of the stretched fiber core rod by the OVD process, and then sintering and heat treatment are sequentially performed to obtain a synthetic core rod.
  • the depressed layer is a fluorine-doped silica glass layer, and the relative refraction of the depressed layer
  • the ratio ⁇ n 3 is -0.2%, and the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 8
  • the sintering method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first
  • the temperature rise rate of 55°C/min is increased to 1100°C and the temperature is kept for 2h, and then the temperature rise rate is 25°C/min to 1400°C and the temperature is kept for 5.5h
  • the heat treatment method is: the synthesis after being kept at 1400°C for 5.5h
  • the core rod is cooled to a temperature of ⁇ 100°C with the
  • the surface of the synthetic mandrel is etched with a mixture of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm. Then the corroded synthetic mandrel is cleaned and dried, and then the synthetic mandrel is inserted into the quartz sleeve.
  • the tube is assembled into an optical fiber preform, and the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 3.
  • the diameter of the optical fiber preform reaches 215mm, and the prepared optical fiber preform is drawn on-line.
  • the length of a single rod can reach 2905km.
  • the fiber attenuation at 1310nm is 0.303dB/km, and the attenuation at 1383nm It is 0.273dB/km, and the attenuation at 1550nm is 0.160dB/km.

Abstract

Disclosed is a method for manufacturing an optical fiber preform based on a sleeve method, the method comprising the following steps: preparing an optical fiber mother core rod comprising a core layer and an inner cladding layer by using a VAD process, then heating and stretching the optical fiber mother core rod such that the curve degree of the stretched optical fiber core rod is less than 1 mm/m, then preparing a depressed layer by means of an OVD process, and finally, inserting the combined core rod into a quartz sleeve to form an optical fiber preform. The diameter of the prepared optical fiber preform may be up to 221 mm, the fiber pulling length of a single preform may be up to 2995 km, the attenuation coefficient of an optical fiber at a wavelength of 1310 nm is less than or equal to 0.305 dB/km, the attenuation coefficient of the optical fiber at a wavelength of 1383 nm is less than or equal to 0.275 dB/km, and the attenuation coefficient of the optical fiber at a wavelength of 1550 nm is less than or equal to 0.165 dB/km.

Description

一种基于套管法的光纤预制棒制造方法Method for manufacturing optical fiber preform based on sleeve method 技术领域Technical field
本发明涉及一种基于套管法的光纤预制棒制造方法,属于光纤预制棒制造领域。The invention relates to a method for manufacturing an optical fiber preform based on a sleeve method, and belongs to the field of optical fiber preform manufacturing.
背景技术Background technique
目前,生产光纤预制棒的方法主要有以下四种:改进的化学汽相沉积法(MCVD)、微波等离子体化学汽相沉积法(PCVD)、外部气相沉积法(OVD)和轴向气相沉积法(VAD),但仅通过上述方法制造大外径的光纤预制棒存在以下问题:管内沉积法(MCVD和PCVD)受衬管尺寸的限制,无法直接制造大外径的光纤预制棒,而管外沉积法(VAD和OVD)法直接制造大外径的芯棒,成本较高,无法体现采用套管法制造大尺寸预制棒的优势。At present, there are four main methods for producing optical fiber preforms: improved chemical vapor deposition (MCVD), microwave plasma chemical vapor deposition (PCVD), external vapor deposition (OVD) and axial vapor deposition (VAD), but only using the above method to manufacture large outer diameter optical fiber preforms has the following problems: In-tube deposition methods (MCVD and PCVD) are limited by the size of the liner tube, and it is impossible to directly manufacture large outer diameter optical fiber preforms. The deposition method (VAD and OVD) method directly manufactures mandrels with large outer diameters, and the cost is high, which cannot reflect the advantages of using the casing method to manufacture large-size preforms.
套管法是将芯棒插入石英套管中组成光纤预制棒,它是制造大尺寸光纤预制棒的较好方法,但是采用套管法制备光纤预制棒时要求严格控制芯棒和套管间的间隙,以保证光纤具有好的芯包同心度和光学性能,因此,基于套管法的光纤预制棒要求保证光纤芯棒的弓曲度和直径均匀性,而目前基于套管法制备的光纤预制棒的芯棒弓曲度和直径均匀性难以保证,导致以套管法制备的光纤预制棒的损耗较大。The tube method is to insert a core rod into a quartz tube to form an optical fiber preform. It is a better method for manufacturing large-size optical fiber preforms. However, when the tube method is used to prepare an optical fiber preform, strict control of the core rod and the tube is required. To ensure that the fiber has good core-wrap concentricity and optical performance, the fiber preform based on the tube method requires the bow and the uniformity of the diameter of the fiber core rod, and the current fiber preform prepared based on the tube method It is difficult to ensure the uniformity of bow and diameter of the core rod of the rod, resulting in large loss of the optical fiber preform prepared by the sleeve method.
发明内容Summary of the invention
本发明要解决的技术问题是:为解决基于套管法制备的光纤预制棒的芯棒弓曲度和直径均匀性难以保证的技术问题,提供一种基于套管法的光纤预制棒制造方法。The technical problem to be solved by the present invention is to provide a method for manufacturing an optical fiber preform based on the sleeve method to solve the technical problem that the core rod bow and diameter uniformity of the optical fiber preform prepared based on the sleeve method is difficult to ensure.
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:
一种基于套管法的光纤预制棒制造方法,步骤如下:A method for manufacturing an optical fiber preform based on the sleeve method, the steps are as follows:
利用VAD工艺制备光纤芯棒母棒,所述光纤芯棒母棒由内到外依次是芯层和内包层;Utilizing the VAD process to prepare the optical fiber core rod mother rod, the optical fiber core rod mother rod being a core layer and an inner cladding layer from the inside to the outside;
对光纤芯棒母棒进行加热拉伸,使拉伸后光纤芯棒的弓曲度小于1mm/m;所述拉伸方法为:将光纤芯棒母棒两端分别对接上拉伸引棒和下拉伸引棒,并使光纤芯棒母棒竖直穿过拉伸炉,使上拉伸引棒和下拉伸引棒以相同的转速同步旋转,开启拉伸炉对光纤芯棒母棒从下到上进行加热,并使上拉伸引棒向上移动,上拉伸引棒向上移动速度根据拉伸后芯棒所需要的直径、拉伸炉向上移动的速度以及被拉伸段光纤芯棒母棒的直径在拉伸前提前计算得到;The fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1 mm/m; the stretching method is: the two ends of the fiber core rod mother rod are respectively connected to the drawing rod and Pull down the lead rod, and make the mother rod of the optical fiber core rod vertically pass through the drawing furnace, make the upper drawing lead rod and the lower drawing lead rod synchronously rotate at the same speed, and turn on the drawing furnace to set the mother rod of the optical fiber core rod. Heat from bottom to top and make the upper drawing rod move upward. The upward moving speed of the upper drawing rod depends on the required diameter of the mandrel after drawing, the speed at which the drawing furnace moves upward, and the fiber core of the drawn section The diameter of the rod mother rod is calculated in advance before stretching;
利用OVD工艺在拉伸后光纤芯棒的外部沉积下陷层疏松体,然后进行烧结处理,得到合成芯棒;The OVD process is used to deposit the depressed layer loose body on the outside of the stretched optical fiber core rod, and then perform sintering treatment to obtain a synthetic core rod;
将合成芯棒表面经腐蚀、清洗、干燥后,插入石英套管中,组合成光纤预制棒。After the surface of the synthetic mandrel is corroded, cleaned and dried, it is inserted into the quartz sleeve to form an optical fiber preform.
优选地,在光纤芯棒母棒加热拉伸过程中满足V 1=k×V 2×V 3(D 1 2-D 2 2)/D 1 2,其中,V 1为上拉伸引棒的实时移动速度,V 2为光纤芯棒母棒自转的转速,V 3为预设的拉伸炉向上移动的速度,D 1为被拉伸段光纤芯棒母棒的直径,D 2为拉伸后芯棒所需要的直径,k为0.1-0.15,V 2为6-9mm/min,V 3为30-40mm/min。 Preferably, V 1 =k×V 2 ×V 3 (D 1 2 -D 2 2 )/D 1 2 is satisfied during the heating and drawing process of the mother rod of the optical fiber core rod, where V 1 is the upper drawing rod Real-time moving speed, V 2 is the rotation speed of the fiber core rod mother rod, V 3 is the preset moving speed of the drawing furnace upwards, D 1 is the diameter of the fiber core rod mother rod of the stretched section, D 2 is the drawing after the required diameter of the mandrel, k is 0.1-0.15, V 2 of 6-9mm / min, V 3 of 30-40mm / min.
优选地,拉伸炉对光纤芯棒母棒加热的温度控制在1800-2300℃,加热时在加热区 域充入惰性气体。Preferably, the temperature at which the drawing furnace heats the mother rod of the optical fiber core rod is controlled at 1800-2300°C, and the heating area is filled with inert gas during heating.
优选地,所述烧结处理方法为:往烧结炉内通入惰性气体和氯气,首先使烧结炉以50-60℃/min的升温速率升到1000~1200℃,保温2-3h,然后以20-30℃/min的升温速率升到1300-1500℃,保温5-6h。Preferably, the sintering treatment method is as follows: pass inert gas and chlorine gas into the sintering furnace, first raise the sintering furnace to 1000-1200°C at a heating rate of 50-60°C/min, keep it for 2-3h, and then heat it for 20 The temperature rise rate of -30℃/min is increased to 1300-1500℃, and the temperature is kept for 5-6h.
优选地,对烧结处理后的合成芯棒进行热处理,热处理方法为:将在1300-1500℃下保温5-6h后的合成芯棒用冷却液在2min内冷却到温度<100℃,然后将冷却后的合成芯棒升温至600~800℃下保温2~3h。Preferably, the sintered synthetic mandrel is heat-treated, and the heat treatment method is as follows: the synthetic mandrel, which has been kept at 1300-1500°C for 5-6h, is cooled to a temperature of <100°C with a coolant within 2 minutes, and then cooled The latter synthetic mandrel is heated to 600-800°C for 2 to 3 hours.
优选地,利用VAD工艺制备光纤芯棒母棒的步骤为:首先用轴向气相沉积法沉积粉末芯棒,然后在烧结炉中对粉末芯棒进行脱羟处理、氟掺杂处理和玻璃化处理:脱羟处理时,往烧结炉内通入Cl 2气和惰性气体,脱羟温度为800~1000℃;氟掺杂处理时,往烧结炉内通入含氟气体和惰性气体,烧结炉温度为1000~1300℃;玻璃化处理时,往烧结炉内只通入惰性气体,玻璃化温度为1400~1600℃。 Preferably, the steps of using the VAD process to prepare the optical fiber core rod mother rod are: firstly deposit the powder core rod by the axial vapor deposition method, and then perform the dehydroxylation treatment, fluorine doping treatment and vitrification treatment on the powder core rod in the sintering furnace : During dehydroxylation treatment, pass Cl 2 gas and inert gas into the sintering furnace, and the dehydroxylation temperature is 800-1000℃; during fluorine doping treatment, pass fluorine-containing gas and inert gas into the sintering furnace, and the sintering furnace temperature It is 1000~1300℃; during vitrification, only inert gas is introduced into the sintering furnace, and the glass transition temperature is 1400~1600℃.
优选地,所述芯层为掺入P 2O 5的二氧化硅玻璃层,芯层的相对折射率Δn 1为0.35%~0.5%,所述内包层和下陷层为掺氟的二氧化硅玻璃层,内包层的相对折射率Δn 2为-0.05%~-0.01%,下陷层的相对折射率Δn 3为-0.25%~-0.1%。 Preferably, the core layer is a silica glass layer doped with P 2 O 5 , the relative refractive index Δn 1 of the core layer is 0.35% to 0.5%, and the inner cladding layer and the depression layer are fluorine-doped silica For the glass layer, the relative refractive index Δn 2 of the inner cladding layer is -0.05% to -0.01%, and the relative refractive index Δn 3 of the depressed layer is -0.25% to -0.1%.
优选地,拉伸后光纤芯棒的直径b与芯层直径a的比值b/a为3.0~5.0,合成芯棒的直径c与芯层直径a的比值c/a为7~9,光纤预制棒的有效直径d与合成芯棒直径c的比值d/c为2.5~3.5。Preferably, the ratio b/a of the diameter b of the fiber core rod to the core diameter a after stretching is 3.0 to 5.0, and the ratio c/a of the diameter c of the composite core rod to the core diameter a is 7 to 9, and the optical fiber is prefabricated The ratio d/c of the effective diameter d of the rod to the diameter c of the composite core rod is 2.5 to 3.5.
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 drawing directly from 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VAD工艺制备包括芯层和内包层的光纤芯棒母棒,然后对光纤芯棒母棒进行加热拉伸,使拉伸后光纤芯棒的弓曲度小于1mm/m,再通过OVD工艺制备下陷层,最后将合成芯棒插入石英套管中,组合成光纤预制棒,其中:The present invention uses the VAD process to prepare an optical fiber core rod mother rod including a core layer and an inner cladding layer, and then heats and stretches the optical fiber core rod mother rod to make the bow of the optical fiber core rod less than 1 mm/m after drawing, and then passes through OVD The process prepares the sink layer, and finally inserts the synthetic core rod into the quartz sleeve to form an optical fiber preform, where:
(1)VAD工艺步骤后对光纤芯棒母棒的拉伸采用竖直向上拉伸的方式,同时在拉伸前通过对母棒各个位置的直径扫描提前计算出拉伸过程中上拉伸引棒沿向上的移动速度,使拉伸后芯棒的同轴度得到了控制,保证了拉伸后芯棒的弓曲度和直径均匀性;进一步,利用VAD法制备粉末芯棒后,通过合理的脱羟、氟掺杂和玻璃化工艺,不仅能够有效脱除羟基,还能优化芯包层的粘度匹配,降低拉制光纤的瑞利散射,达到低损耗的目的;(1) After the VAD process step, the fiber core rod mother rod is stretched vertically upwards. At the same time, the diameter of each position of the mother rod is scanned in advance to calculate the upper stretching guide during the stretching process. The upward moving speed of the rod controls the coaxiality of the mandrel after stretching and ensures the bow and diameter uniformity of the mandrel after stretching; further, after the powder mandrel is prepared by the VAD method, a reasonable The dehydroxylation, fluorine doping and vitrification process can not only effectively remove the hydroxyl groups, but also optimize the viscosity matching of the core and cladding, reduce the Rayleigh scattering of the drawn fiber, and achieve the purpose of low loss;
(2)OVD工艺步骤后合理的烧结工艺,加上对烧结处理后的合成芯棒进行的热处理处理,不仅有效脱除了羟基,还使得下陷层具有合理结构,能够有效阻挡石英套管中的金属杂质和羟基扩散至芯层,有效降低了拉制光纤的损耗,且通过OVD工艺制备的合成芯棒直径均匀,最终可以精确控制合成芯棒的直径,缩小石英套管与合成芯棒之间的间隙,降低光纤芯/包同心度误差;(2) The reasonable sintering process after the OVD process steps, plus the heat treatment of the sintered synthetic core rod, not only effectively removes the hydroxyl group, but also makes the sunken layer have a reasonable structure, which can effectively block the metal in the quartz sleeve Impurities and hydroxyls diffuse into the core layer, which effectively reduces the loss of the drawn fiber, and the diameter of the synthetic mandrel prepared by the OVD process is uniform, and finally the diameter of the synthetic mandrel can be accurately controlled, and the gap between the quartz sleeve and the synthetic mandrel can be reduced. Gap to reduce the concentricity error of the fiber core/package;
(3)对芯层、内包层、下陷层的掺杂剂、折射率和直径等进行了合理限定,可以保证光纤预制棒的拉纤长度,降低光纤的衰减系数,以石英套管作为光纤预制棒的外包层材料,可以有效降低光纤预制棒的制造成本;(3) The dopant, refractive index and diameter of the core layer, inner cladding layer and sink layer are reasonably limited, which can ensure the fiber length of the optical fiber preform and reduce the attenuation coefficient of the optical fiber. The quartz sleeve is used as the optical fiber preform. The outer cladding material can effectively reduce the manufacturing cost of optical fiber preform;
最终,本发明制备的光纤预制棒的直径可达221mm,单根预制棒拉纤长度可达到 2995km,光纤在1310nm波长处的衰减≤0.305dB/km,在1383nm波长处的衰减系数≤0.275dB/km,在1550nm波长处的衰减系数≤0.165dB/km。Finally, the diameter of the optical fiber preform prepared by the present invention can reach 221mm, the drawing length of a single preform can reach 2995km, the fiber attenuation at 1310nm wavelength is ≤0.305dB/km, and the attenuation coefficient at 1383nm wavelength is ≤0.275dB/km , The attenuation coefficient at 1550nm wavelength is ≤0.165dB/km.
具体实施方式detailed description
现在对本发明作进一步详细的说明。The present invention will now be described in further detail.
实施例1Example 1
本实施例提供一种基于套管法的光纤预制棒制造方法,步骤如下:This embodiment provides a method for manufacturing an optical fiber preform based on the sleeve method, and the steps are as follows:
利用VAD工艺制备光纤芯棒母棒,所述光纤芯棒母棒由内到外依次是芯层和内包层,所述芯层为掺入P 2O 5的二氧化硅玻璃层,芯层的相对折射率Δn 1为0.35%,所述内包层为掺氟的二氧化硅玻璃层,内包层的相对折射率Δn 2为-0.05%;制备光纤芯棒母棒的具体步骤为:首先用轴向气相沉积法沉积粉末芯棒,然后在烧结炉中对粉末芯棒进行脱羟处理、氟掺杂处理和玻璃化处理:脱羟处理时,往烧结炉内通入Cl 2气和氦气,脱羟温度为800℃;氟掺杂处理时,往烧结炉内通入含氟气体和氦气,烧结炉温度为1000℃;玻璃化处理时,往烧结炉内只通入氦气,玻璃化温度为1400℃; The optical fiber core rod mother rod is prepared by the VAD process. The optical fiber core rod mother rod has a core layer and an inner cladding layer from the inside to the outside. The core layer is a silica glass layer doped with P 2 O 5 , and the core layer is The relative refractive index Δn 1 is 0.35%, the inner cladding layer is a fluorine-doped silica glass layer, and the relative refractive index Δn 2 of the inner cladding layer is -0.05%; the specific steps for preparing the optical fiber core rod mother rod are: first use the shaft The powder core rod is deposited by the vapor deposition method, and then the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, Cl 2 gas and helium gas are passed into the sintering furnace, The dehydroxylation temperature is 800℃; during fluorine doping treatment, fluorine-containing gas and helium gas are introduced into the sintering furnace, and the temperature of the sintering furnace is 1000℃; during vitrification, only helium gas is introduced into the sintering furnace for vitrification The temperature is 1400℃;
对光纤芯棒母棒进行加热拉伸,使拉伸后光纤芯棒的弓曲度小于1mm/m,拉伸后光纤芯棒的直径b与芯层直径a的比值b/a为3.0;所述拉伸方法为:将光纤芯棒母棒两端分别对接上拉伸引棒和下拉伸引棒,并使光纤芯棒母棒竖直穿过拉伸炉,使上拉伸引棒和下拉伸引棒以相同的转速同步旋转,开启拉伸炉对光纤芯棒母棒从下到上进行加热,并使上拉伸引棒向上移动,所述上拉伸引棒向上移动速度根据拉伸后芯棒所需要的直径、拉伸炉向上移动的速度以及被拉伸段光纤芯棒母棒的直径在拉伸前提前计算得到,在光纤芯棒母棒加热拉伸过程中满足V 1=k×V 2×V 3(D 1 2-D 2 2)/D 1 2,其中,V 1为上拉伸引棒的实时移动速度,V 2为光纤芯棒母棒自转的转速,V 3为预设的拉伸炉向上移动的速度,D 1为被拉伸段光纤芯棒母棒的直径,D 2为拉伸后芯棒所需要的直径,所述k为0.1,所述V 2为9mm/min,所述V 3为30mm/min,拉伸炉对光纤芯棒母棒加热的温度控制在1800℃,加热时在加热区域充入氦气; The fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1mm/m, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a after stretching is 3.0; The stretching method is as follows: connect the two ends of the optical fiber core rod mother rod to the upper and lower drawing lead rods respectively, and make the optical fiber core rod mother rod vertically pass through the drawing furnace, so that the upper drawing lead rod and The lower drawing rod rotates synchronously at the same speed, the drawing furnace is turned on to heat the fiber core rod mother rod from bottom to top, and the upper drawing rod is moved upward, and the upward moving speed of the upper drawing rod is according to After stretching, the required diameter of the core rod, the upward moving speed of the stretching furnace, and the diameter of the fiber core rod mother rod of the stretched section are calculated in advance before stretching. During the heating and stretching process of the optical fiber core rod mother rod, V 1 = k×V 2 ×V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, and V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset upward moving speed of the stretching furnace, D 1 is the diameter of the fiber core rod mother rod of the stretched section, and D 2 is the required diameter of the core rod after stretching, the k is 0.1, the V 2 is 9 mm/min, the V 3 is 30 mm/min, the temperature at which the drawing furnace heats the optical fiber core rod mother rod is controlled at 1800°C, and helium is filled in the heating area during heating;
利用OVD工艺在拉伸后光纤芯棒的外部沉积下陷层疏松体,然后依次进行烧结处理和热处理,得到合成芯棒,所述下陷层为掺氟的二氧化硅玻璃层,下陷层的相对折射率Δn 3为-0.25%,合成芯棒的直径c与芯层直径a的比值c/a为7;所述烧结处理方法为:往烧结炉内通入惰性气体和氯气,首先使烧结炉以50℃/min的升温速率升到1000℃,保温3h,然后以20℃/min的升温速率升到1300℃,保温6h;所述热处理方法为:将在1300℃下保温6h后的合成芯棒用冷却液在2min内冷却到温度<100℃,然后将冷却后的合成芯棒升温至600℃下保温3h; The depressed layer loose body is deposited on the outside of the stretched fiber core rod by the OVD process, and then sintering and heat treatment are sequentially performed to obtain a synthetic core rod. The depressed layer is a fluorine-doped silica glass layer, and the relative refraction of the depressed layer The ratio Δn 3 is -0.25%, and the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 7; the sintering method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first The heating rate of 50°C/min is increased to 1000°C and the temperature is kept for 3 hours, and then the temperature rise rate of 20°C/min is raised to 1300°C and the temperature is kept for 6 hours; the heat treatment method is: the synthetic mandrel is heated at 1300°C for 6 hours Use cooling liquid to cool to a temperature of <100°C within 2 minutes, and then heat the cooled synthetic mandrel to 600°C for 3 hours;
将合成芯棒表面用摩尔比为1:1的氢氟酸、硝酸的混合酸腐蚀,腐蚀深度不小于0.6mm,然后将腐蚀后的合成芯棒清洗、干燥后,将合成芯棒插入石英套管中,组合成光纤预制棒,光纤预制棒的有效直径d与合成芯棒直径c的比值d/c为2.5。The surface of the synthetic mandrel is etched with a mixture of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm. Then the corroded synthetic mandrel is cleaned and dried, and then the synthetic mandrel is inserted into the quartz sleeve The tube is assembled into an optical fiber preform, and the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 2.5.
经测试,光纤预制棒的直径达到203mm,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2865km,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0.163dB/km。After testing, the diameter of the optical fiber preform reaches 203mm, and the prepared optical fiber preform is drawn on-line. The length of a single rod can reach 2865km. After drawing, the fiber attenuation at 1310nm is 0.302dB/km, and the attenuation at 1383nm It is 0.271dB/km, and the attenuation at 1550nm is 0.163dB/km.
实施例2Example 2
本实施例提供一种基于套管法的光纤预制棒制造方法,步骤如下:This embodiment provides a method for manufacturing an optical fiber preform based on the sleeve method, and the steps are as follows:
利用VAD工艺制备光纤芯棒母棒,所述光纤芯棒母棒由内到外依次是芯层和内包层,所述芯层为掺入P 2O 5的二氧化硅玻璃层,芯层的相对折射率Δn 1为0.5%,所述内包层为掺氟的二氧化硅玻璃层,内包层的相对折射率Δn 2为-0.01%;制备光纤芯棒母棒的具体步骤为:首先用轴向气相沉积法沉积粉末芯棒,然后在烧结炉中对粉末芯棒进行脱羟处理、氟掺杂处理和玻璃化处理:脱羟处理时,往烧结炉内通入Cl 2气和氦气,脱羟温度为1000℃;氟掺杂处理时,往烧结炉内通入含氟气体和氦气,烧结炉温度为1300℃;玻璃化处理时,往烧结炉内只通入氦气,玻璃化温度为1600℃; The optical fiber core rod mother rod is prepared by the VAD process. The optical fiber core rod mother rod has a core layer and an inner cladding layer from the inside to the outside. The core layer is a silica glass layer doped with P 2 O 5 , and the core layer is The relative refractive index Δn 1 is 0.5%, the inner cladding layer is a fluorine-doped silica glass layer, and the relative refractive index Δn 2 of the inner cladding layer is -0.01%; the specific steps for preparing the optical fiber core rod mother rod are: The powder core rod is deposited by the vapor deposition method, and then the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, Cl 2 gas and helium gas are passed into the sintering furnace, The dehydroxylation temperature is 1000°C; during fluorine doping treatment, fluorine-containing gas and helium gas are passed into the sintering furnace, and the temperature of the sintering furnace is 1300°C; during vitrification, only helium gas is passed into the sintering furnace to vitrify The temperature is 1600℃;
对光纤芯棒母棒进行加热拉伸,使拉伸后光纤芯棒的弓曲度小于1mm/m,拉伸后光纤芯棒的直径b与芯层直径a的比值b/a为5.0;所述拉伸方法为:将光纤芯棒母棒两端分别对接上拉伸引棒和下拉伸引棒,并使光纤芯棒母棒竖直穿过拉伸炉,使上拉伸引棒和下拉伸引棒以相同的转速同步旋转,开启拉伸炉对光纤芯棒母棒从下到上进行加热,并使上拉伸引棒向上移动,所述上拉伸引棒向上移动速度根据拉伸后芯棒所需要的直径、拉伸炉向上移动的速度以及被拉伸段光纤芯棒母棒的直径在拉伸前提前计算得到,在光纤芯棒母棒加热拉伸过程中满足V 1=k×V 2×V 3(D 1 2-D 2 2)/D 1 2,其中,V 1为上拉伸引棒的实时移动速度,V 2为光纤芯棒母棒自转的转速,V 3为预设的拉伸炉向上移动的速度,D 1为被拉伸段光纤芯棒母棒的直径,D 2为拉伸后芯棒所需要的直径,所述k为0.15,所述V 2为6mm/min,所述V 3为40mm/min,拉伸炉对光纤芯棒母棒加热的温度控制在2300℃,加热时在加热区域充入氦气; The fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1 mm/m, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a after stretching is 5.0; The stretching method is as follows: connect the two ends of the optical fiber core rod mother rod to the upper and lower drawing lead rods respectively, and make the optical fiber core rod mother rod vertically pass through the drawing furnace, so that the upper drawing lead rod and The lower drawing rod rotates synchronously at the same speed, the drawing furnace is turned on to heat the fiber core rod mother rod from bottom to top, and the upper drawing rod is moved upward, and the upward moving speed of the upper drawing rod is according to After stretching, the required diameter of the core rod, the upward moving speed of the stretching furnace, and the diameter of the fiber core rod mother rod of the stretched section are calculated in advance before stretching. During the heating and stretching process of the optical fiber core rod mother rod, V 1 = k×V 2 ×V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, and V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset upward moving speed of the stretching furnace, D 1 is the diameter of the fiber core rod mother rod of the stretched section, and D 2 is the required diameter of the core rod after stretching, the k is 0.15, the V 2 is 6 mm/min, and the V 3 is 40 mm/min. The temperature of the fiber core rod mother rod heated by the drawing furnace is controlled at 2300°C, and helium is filled in the heating area during heating;
利用OVD工艺在拉伸后光纤芯棒的外部沉积下陷层疏松体,然后依次进行烧结处理和热处理,得到合成芯棒,所述下陷层为掺氟的二氧化硅玻璃层,下陷层的相对折射率Δn 3为-0.1%,合成芯棒的直径c与芯层直径a的比值c/a为9;所述烧结处理方法为:往烧结炉内通入惰性气体和氯气,首先使烧结炉以60℃/min的升温速率升到1200℃,保温2h,然后以30℃/min的升温速率升到1500℃,保温5h;所述热处理方法为:将在1500℃下保温5h后的合成芯棒用冷却液在2min内冷却到温度<100℃,然后将冷却后的合成芯棒升温至800℃下保温2h; The depressed layer loose body is deposited on the outside of the stretched fiber core rod by the OVD process, and then sintering and heat treatment are sequentially performed to obtain a synthetic core rod. The depressed layer is a fluorine-doped silica glass layer, and the relative refraction of the depressed layer The rate Δn 3 is -0.1%, and the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 9; the sintering method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first The temperature rise rate of 60°C/min is increased to 1200°C and the temperature is kept for 2 hours, and then the temperature rise rate is 30°C/min to 1500°C and the temperature is kept for 5 hours; the heat treatment method is: the synthetic core rod after being kept at 1500°C for 5 hours Use cooling liquid to cool to a temperature of <100°C within 2 minutes, and then heat the cooled synthetic mandrel to 800°C for 2 hours;
将合成芯棒表面用摩尔比为1:1的氢氟酸、硝酸的混合酸腐蚀,腐蚀深度不小于0.6mm,然后将腐蚀后的合成芯棒清洗、干燥后,将合成芯棒插入石英套管中,组合成光纤预制棒,光纤预制棒的有效直径d与合成芯棒直径c的比值d/c为3.5。The surface of the synthetic mandrel is etched with a mixture of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm. Then the corroded synthetic mandrel is cleaned and dried, and then the synthetic mandrel is inserted into the quartz sleeve In the tube, the optical fiber preform is assembled, and the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 3.5.
经测试,光纤预制棒的直径达到221mm,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2995km,拉丝后光纤在1310nm的衰耗为0.305dB/km,在1383nm的衰耗为0.275dB/km,在1550nm的衰耗为0.165dB/km。After testing, the diameter of the optical fiber preform reaches 221mm. The prepared optical fiber preform is drawn into the optical fiber online. The length of a single rod can reach 2995km. After the drawing, the fiber attenuation at 1310nm is 0.305dB/km, and the attenuation at 1383nm. It is 0.275dB/km, and the attenuation at 1550nm is 0.165dB/km.
实施例3Example 3
本实施例提供一种基于套管法的光纤预制棒制造方法,步骤如下:This embodiment provides a method for manufacturing an optical fiber preform based on the sleeve method, and the steps are as follows:
利用VAD工艺制备光纤芯棒母棒,所述光纤芯棒母棒由内到外依次是芯层和内包层,所述芯层为掺入P 2O 5的二氧化硅玻璃层,芯层的相对折射率Δn 1为0.4%,所述内包层为掺氟的二氧化硅玻璃层,内包层的相对折射率Δn 2为-0.08%;制备光纤芯棒母棒的具体步骤为:首先用轴向气相沉积法沉积粉末芯棒,然后在烧结炉中对粉末芯棒进行脱羟处理、氟掺杂处理和玻璃化处理:脱羟处理时,往烧结炉内通入Cl 2气和氦气,脱羟温度为900℃;氟掺杂处理时,往烧结炉内通入含氟气体和氦气,烧结炉温度为1100℃;玻璃化处理时,往烧结炉内只通入氦气,玻璃化温度为1500℃; The optical fiber core rod mother rod is prepared by the VAD process. The optical fiber core rod mother rod has a core layer and an inner cladding layer from the inside to the outside. The core layer is a silica glass layer doped with P 2 O 5 , and the core layer is The relative refractive index Δn 1 is 0.4%, the inner cladding layer is a fluorine-doped silica glass layer, and the relative refractive index Δn 2 of the inner cladding layer is -0.08%; the specific steps for preparing the optical fiber core rod mother rod are: The powder core rod is deposited by the vapor deposition method, and then the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, Cl 2 gas and helium gas are passed into the sintering furnace, The dehydroxylation temperature is 900°C; during fluorine doping treatment, fluorine-containing gas and helium gas are passed into the sintering furnace, and the temperature of the sintering furnace is 1100°C; during vitrification, only helium gas is passed into the sintering furnace to vitrify The temperature is 1500℃;
对光纤芯棒母棒进行加热拉伸,使拉伸后光纤芯棒的弓曲度小于1mm/m,拉伸后光纤芯棒的直径b与芯层直径a的比值b/a为4.0;所述拉伸方法为:将光纤芯棒母棒两端分别对接上拉伸引棒和下拉伸引棒,并使光纤芯棒母棒竖直穿过拉伸炉,使上拉伸引棒和下拉伸引棒以相同的转速同步旋转,开启拉伸炉对光纤芯棒母棒从下到上进行加热,并使上拉伸引棒向上移动,所述上拉伸引棒向上移动速度根据拉伸后芯棒所需要的直径、拉伸炉向上移动的速度以及被拉伸段光纤芯棒母棒的直径在拉伸前提前计算得到,在光纤芯棒母棒加热拉伸过程中满足V 1=k×V 2×V 3(D 1 2-D 2 2)/D 1 2,其中,V 1为上拉伸引棒的实时移动速度,V 2为光纤芯棒母棒自转的转速,V 3为预设的拉伸炉向上移动的速度,D 1为被拉伸段光纤芯棒母棒的直径,D 2为拉伸后芯棒所需要的直径,所述k为0.12,所述V 2为8mm/min,所述V 3为35mm/min,拉伸炉对光纤芯棒母棒加热的温度控制在2000℃,加热时在加热区域充入氦气; The fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1mm/m, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a after stretching is 4.0; The stretching method is as follows: connect the two ends of the optical fiber core rod mother rod to the upper and lower drawing lead rods respectively, and make the optical fiber core rod mother rod vertically pass through the drawing furnace, so that the upper drawing lead rod and The lower drawing rod rotates synchronously at the same speed, the drawing furnace is turned on to heat the fiber core rod mother rod from bottom to top, and the upper drawing rod is moved upward, and the upward moving speed of the upper drawing rod is according to After stretching, the required diameter of the core rod, the upward moving speed of the stretching furnace, and the diameter of the fiber core rod mother rod of the stretched section are calculated in advance before stretching. During the heating and stretching process of the optical fiber core rod mother rod, V 1 = k×V 2 ×V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, and V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset moving speed of the stretching furnace upward, D 1 is the diameter of the fiber core rod mother rod of the stretched section, D 2 is the required diameter of the core rod after stretching, the k is 0.12, the V 2 is 8 mm/min, the V 3 is 35 mm/min, the temperature at which the drawing furnace heats the optical fiber core rod mother rod is controlled at 2000° C., and helium is filled in the heating area during heating;
利用OVD工艺在拉伸后光纤芯棒的外部沉积下陷层疏松体,然后依次进行烧结处理和热处理,得到合成芯棒,所述下陷层为掺氟的二氧化硅玻璃层,下陷层的相对折射率Δn 3为-0.2%,合成芯棒的直径c与芯层直径a的比值c/a为8;所述烧结处理方法为:往烧结炉内通入惰性气体和氯气,首先使烧结炉以55℃/min的升温速率升到1100℃,保温2h,然后以25℃/min的升温速率升到1400℃,保温5.5h;所述热处理方法为:将在1400℃下保温5.5h后的合成芯棒用冷却液在2min内冷却到温度<100℃,然后将冷却后的合成芯棒升温至700℃下保温2.5h; The depressed layer loose body is deposited on the outside of the stretched fiber core rod by the OVD process, and then sintering and heat treatment are sequentially performed to obtain a synthetic core rod. The depressed layer is a fluorine-doped silica glass layer, and the relative refraction of the depressed layer The ratio Δn 3 is -0.2%, and the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 8; the sintering method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first The temperature rise rate of 55°C/min is increased to 1100°C and the temperature is kept for 2h, and then the temperature rise rate is 25°C/min to 1400°C and the temperature is kept for 5.5h; the heat treatment method is: the synthesis after being kept at 1400°C for 5.5h The core rod is cooled to a temperature of <100°C with the cooling liquid within 2 minutes, and then the cooled synthetic core rod is heated to 700°C for 2.5 hours;
将合成芯棒表面用摩尔比为1:1的氢氟酸、硝酸的混合酸腐蚀,腐蚀深度不小于0.6mm,然后将腐蚀后的合成芯棒清洗、干燥后,将合成芯棒插入石英套管中,组合成光纤预制棒,光纤预制棒的有效直径d与合成芯棒直径c的比值d/c为3。The surface of the synthetic mandrel is etched with a mixture of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm. Then the corroded synthetic mandrel is cleaned and dried, and then the synthetic mandrel is inserted into the quartz sleeve The tube is assembled into an optical fiber preform, and the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 3.
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2905km,拉丝后光纤在1310nm的衰耗为0.303dB/km,在1383nm的衰耗为0.273dB/km,在1550nm的衰耗为0.160dB/km。After testing, the diameter of the optical fiber preform reaches 215mm, and the prepared optical fiber preform is drawn on-line. The length of a single rod can reach 2905km. After drawing, the fiber attenuation at 1310nm is 0.303dB/km, and the attenuation at 1383nm It is 0.273dB/km, and the attenuation at 1550nm is 0.160dB/km.
以上述依据本发明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发明技术思想的范围内,进行多样的变更以及修改。本项发明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 according to the present invention as enlightenment, through the above-mentioned description content, relevant workers can make various changes and modifications without departing from the scope of the technical idea of the present invention. The technical scope of the present invention is not limited to the content of the description, and its technical scope must be determined according to the scope of the claims.

Claims (10)

  1. 一种基于套管法的光纤预制棒制造方法,其特征在于,步骤如下:利用VAD工艺制备光纤芯棒母棒,所述光纤芯棒母棒由内到外依次是芯层和内包层;A method for manufacturing an optical fiber preform based on a ferrule method is characterized in that the steps are as follows: the optical fiber core rod mother rod is prepared by a VAD process, and the optical fiber core rod mother rod is a core layer and an inner cladding layer from the inside to the outside;
    对光纤芯棒母棒进行加热拉伸,使拉伸后光纤芯棒的弓曲度小于1mm/m;所述拉伸方法为:将光纤芯棒母棒两端分别对接上拉伸引棒和下拉伸引棒,并使光纤芯棒母棒竖直穿过拉伸炉,使上拉伸引棒和下拉伸引棒以相同的转速同步旋转,开启拉伸炉对光纤芯棒母棒从下到上进行加热,并使上拉伸引棒向上移动,上拉伸引棒向上移动速度根据拉伸后芯棒所需要的直径、拉伸炉向上移动的速度以及被拉伸段光纤芯棒母棒的直径在拉伸前提前计算得到;The fiber core rod mother rod is heated and stretched so that the bow of the fiber core rod after stretching is less than 1 mm/m; the stretching method is: the two ends of the fiber core rod mother rod are respectively connected to the drawing rod and Pull down the lead rod, and make the mother rod of the optical fiber core rod vertically pass through the drawing furnace, make the upper drawing lead rod and the lower drawing lead rod synchronously rotate at the same speed, and turn on the drawing furnace to set the mother rod of the optical fiber core rod. Heat from bottom to top and make the upper drawing rod move upward. The upward moving speed of the upper drawing rod depends on the required diameter of the mandrel after drawing, the speed at which the drawing furnace moves upward, and the fiber core of the drawn section The diameter of the rod mother rod is calculated in advance before stretching;
    利用OVD工艺在拉伸后光纤芯棒的外部沉积下陷层疏松体,然后进行烧结处理,得到合成芯棒;The OVD process is used to deposit the depressed layer loose body on the outside of the stretched optical fiber core rod, and then perform sintering treatment to obtain a synthetic core rod;
    将合成芯棒表面经腐蚀、清洗、干燥后,插入石英套管中,组合成光纤预制棒。After the surface of the synthetic mandrel is corroded, cleaned and dried, it is inserted into the quartz sleeve to form an optical fiber preform.
  2. 根据权利要求1所述的基于套管法的光纤预制棒制造方法,其特征在于,在光纤芯棒母棒加热拉伸过程中满足V 1=k×V 2×V 3(D 1 2-D 2 2)/D 1 2,其中,V 1为上拉伸引棒的实时移动速度,V 2为光纤芯棒母棒自转的转速,V 3为预设的拉伸炉向上移动的速度,D 1为被拉伸段光纤芯棒母棒的直径,D 2为拉伸后芯棒所需要的直径,k为0.1-0.15,V 2为6-9mm/min,V 3为30-40mm/min。 The method for manufacturing an optical fiber preform based on the ferrule method according to claim 1, characterized in that, during the heating and drawing process of the mother rod of the optical fiber core rod, it satisfies V 1 =k×V 2 ×V 3 (D 1 2 -D 2 2 )/D 1 2 , where V 1 is the real-time moving speed of the upper drawing rod, V 2 is the rotation speed of the optical fiber core rod mother rod, V 3 is the preset moving speed of the drawing furnace up, D 1 is the diameter of the fiber core rod mother rod of the stretched section, D 2 is the required diameter of the core rod after stretching, k is 0.1-0.15, V 2 is 6-9mm/min, V 3 is 30-40mm/min .
  3. 根据权利要求1或2所述的基于套管法的光纤预制棒制造方法,其特征在于,拉伸炉对光纤芯棒母棒加热的温度控制在1800-2300℃,加热时在加热区域充入惰性气体。The method for manufacturing an optical fiber preform based on the ferrule method according to claim 1 or 2, wherein the temperature at which the drawing furnace heats the optical fiber core rod mother rod is controlled at 1800-2300°C, and the heating area is filled during heating. Inert gas.
  4. 根据权利要求1-3任一项所述的基于套管法的光纤预制棒制造方法,其特征在于,所述烧结处理方法为:往烧结炉内通入惰性气体和氯气,首先使烧结炉以50-60℃/min的升温速率升到1000~1200℃,保温2-3h,然后以20-30℃/min的升温速率升到1300-1500℃,保温5-6h。The method for manufacturing an optical fiber preform based on the ferrule method according to any one of claims 1-3, wherein the sintering treatment method is: inert gas and chlorine gas are introduced into the sintering furnace, and the sintering furnace is first The temperature rise rate of 50-60°C/min is increased to 1000-1200°C and the temperature is kept for 2-3 hours, and then the temperature rise rate is 20-30°C/min to 1300-1500°C and the temperature is kept for 5-6 hours.
  5. 根据权利要求1-4任一项所述的基于套管法的光纤预制棒制造方法,其特征在于,对烧结处理后的合成芯棒进行热处理,热处理方法为:将在1300-1500℃下保温5-6h后的合成芯棒用冷却液在2min内冷却到温度<100℃,然后将冷却后的合成芯棒升温至600~800℃下保温2~3h。The method for manufacturing an optical fiber preform based on the sleeve method according to any one of claims 1 to 4, wherein the sintered synthetic core rod is heat treated, and the heat treatment method is: heat preservation at 1300-1500°C The synthetic core rod after 5-6h is cooled to a temperature of <100°C within 2 minutes with a cooling liquid, and then the cooled synthetic core rod is heated to 600-800°C for 2 to 3 hours.
  6. 根据权利要求1-5任一项所述的基于套管法的光纤预制棒制造方法,其特征在于,利用VAD工艺制备光纤芯棒母棒的步骤为:首先用轴向气相沉积法沉积粉末芯棒,然后在烧结炉中对粉末芯棒进行脱羟处理、氟掺杂处理和玻璃化处理:脱羟处理时,往烧结炉内通入Cl 2气和惰性气体,脱羟温度为800~1000℃;氟掺杂处理时,往烧结炉内通入含氟气体和惰性气体,烧结炉温度为1000~1300℃;玻璃化处理时,往烧结炉内只通入惰性气体,玻璃化温度为1400~1600℃。 The method for manufacturing an optical fiber preform based on the sleeve method according to any one of claims 1 to 5, wherein the step of preparing the optical fiber core rod mother rod by the VAD process is: firstly depositing the powder core by the axial vapor deposition method Then, the powder core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment in the sintering furnace: during the dehydroxylation treatment, pass Cl 2 gas and inert gas into the sintering furnace, and the dehydroxylation temperature is 800~1000 ℃; during fluorine doping treatment, fluorine-containing gas and inert gas are introduced into the sintering furnace, the temperature of the sintering furnace is 1000~1300℃; during vitrification, only inert gas is introduced into the sintering furnace, and the glass transition temperature is 1400 ~1600℃.
  7. 根据权利要求1-6任一项所述的基于套管法的光纤预制棒制造方法,其特征在于,所述芯层为掺入P 2O 5的二氧化硅玻璃层,芯层的相对折射率Δn 1为0.35%~0.5%,所述内包层和下陷层为掺氟的二氧化硅玻璃层,内包层的相对折射率Δn 2为-0.05%~-0.01%,下陷层的相对折射率Δn 3为-0.25%~-0.1%。 The method for manufacturing an optical fiber preform based on the sleeve method according to any one of claims 1-6, wherein the core layer is a silica glass layer doped with P 2 O 5 , and the relative refraction of the core layer is The rate Δn 1 is 0.35% to 0.5%, the inner cladding layer and the sink layer are fluorine-doped silica glass layers, the relative refractive index of the inner cladding layer Δn 2 is -0.05% to -0.01%, and the relative refractive index of the sink layer Δn 3 is -0.25% to -0.1%.
  8. 根据权利要求1-7任一项所述的基于套管法的光纤预制棒制造方法,其特征在于,拉伸后光纤芯棒的直径b与芯层直径a的比值b/a为3.0~5.0,合成芯棒的直径c与芯层直径a的比值c/a为7~9,光纤预制棒的有效直径d与合成芯棒直径c的比值d/c为2.5~3.5。The method for manufacturing an optical fiber preform based on the ferrule method according to any one of claims 1-7, wherein the ratio b/a of the diameter b of the optical fiber core rod to the core diameter a after stretching is 3.0-5.0 , The ratio c/a of the diameter c of the composite core rod to the diameter a of the core layer is 7-9, and the ratio d/c of the effective diameter d of the optical fiber preform to the diameter c of the composite core rod is 2.5-3.5.
  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9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 claim 9, or drawing after drawing.
PCT/CN2019/114352 2019-03-11 2019-10-30 Method for manufacturing optical fiber preform based on sleeve method WO2020181788A1 (en)

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