WO2020177352A1 - Préforme de fibre optique basé sur un manchon de quartz fondu continu, et procédé de fabrication associé - Google Patents

Préforme de fibre optique basé sur un manchon de quartz fondu continu, et procédé de fabrication associé Download PDF

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Publication number
WO2020177352A1
WO2020177352A1 PCT/CN2019/114350 CN2019114350W WO2020177352A1 WO 2020177352 A1 WO2020177352 A1 WO 2020177352A1 CN 2019114350 W CN2019114350 W CN 2019114350W WO 2020177352 A1 WO2020177352 A1 WO 2020177352A1
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Prior art keywords
optical fiber
core rod
fiber preform
synthetic
fused silica
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PCT/CN2019/114350
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English (en)
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 WO2020177352A1 publication Critical patent/WO2020177352A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/018—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] 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

Definitions

  • the invention relates to an optical fiber preform based on a continuous fused silica sleeve and a manufacturing method thereof, belonging to the field of optical fiber preform manufacturing.
  • the process of producing optical fiber preforms mainly adopts a two-step method, that is, first manufacturing the preform core rod, and then manufacturing the cladding outside the core rod.
  • core rod manufacturing technologies improved chemical vapor deposition (MCVD), microwave plasma chemical vapor deposition (PCVD), external vapor deposition (OVD) and axial vapor deposition (VAD), outsourcing Layer manufacturing technology mainly includes OVD method, sleeve method, and plasma spraying method.
  • the sleeve method is to insert a core rod into a quartz sleeve to form an optical fiber preform, which is currently a better method for manufacturing large-size optical fiber preforms.
  • Quartz sleeves are made of natural crystalline quartz or synthetic silane by high temperature melting. Quartz sleeves are classified according to process method, use and appearance, including continuous fused quartz sleeves, fused transparent quartz sleeves, and gas refining transparent quartz sleeves , Synthetic quartz sleeves, opaque quartz sleeves, optical quartz sleeves, quartz sleeves for semiconductors, quartz sleeves for electric light sources, etc., among which continuous fused quartz sleeves are prepared by continuous melting method, and the continuous melting method is simple.
  • One-time input of quartz sand to draw the tube directly has a great cost advantage.
  • the metal impurity content of the continuous fused silica tube is high, and the hydroxyl content is difficult to control. Using it as the outer covering of the optical fiber preform will increase the loss of the optical fiber and make it It is difficult to apply to the production of optical fiber preforms.
  • the technical problem to be solved by the present invention is: in order to solve the technical problem that using continuous fused silica tube as the outer layer of the optical fiber preform will increase the loss of optical fiber, an optical fiber preform based on continuous fused silica tube and a manufacturing method thereof are provided .
  • a manufacturing method of optical fiber preform based on continuous fused silica sleeve the steps are as follows:
  • the OVD process is used to deposit the loose body of the outer covering containing the Sb 2 O 3 -F mixture on the outside of the optical fiber core rod, and then the sintering process is carried out in the sintering furnace to obtain the composite core rod;
  • the sintering treatment method is: passing into the sintering furnace Enter inert gas and chlorine gas, first raise the sintering furnace to 600-800°C at a heating rate of 50-60°C/min, keep it for 1-2h, and then raise it to 1000-1200°C at a heating rate of 30-40°C/min. Keep the temperature for 2-4 hours, and finally increase the temperature to 1300-1500°C at a rate of 10-20°C/min, and keep it for 5-7 hours;
  • the synthetic core rod and the continuous fused silica sleeve are combined into an optical fiber preform.
  • the sintered synthetic mandrel is heat-treated.
  • the heat treatment method is: cooling the synthetic mandrel held at 1300-1500°C for 5-7h to a temperature of ⁇ 100°C within 2 minutes, and then heat the cooled synthetic mandrel The mandrel is heated to 700-1000°C for 2 to 3 hours, and finally the synthetic mandrel is cooled to 300-500°C for 3 to 5 hours.
  • the steps of using the VAD process to prepare the optical fiber core rod are: first deposit the powder core rod by the axial vapor deposition method; then perform the dehydroxylation treatment, fluorine doping treatment and vitrification treatment on the powder core rod in the sintering furnace: During the hydroxyl treatment, pass Cl 2 gas and inert gas into the sintering furnace, and the dehydroxylation temperature is 800 ⁇ 1000°C; during the fluorine doping treatment, pass fluorine-containing gas and inert gas into the sintering furnace, and the temperature of the sintering furnace is 1000 ⁇ 1300°C; During the vitrification process, only inert gas is introduced into the sintering furnace, and the glass transition temperature is 1400 ⁇ 1600°C.
  • the RIC process steps are: corroding the surface of the synthetic mandrel with a mixed acid of hydrofluoric acid and nitric acid with a molar ratio of 1:0.5-1.5, the corrosion depth is not less than 0.6mm, and then cleaning the corroded synthetic mandrel After drying, insert the synthetic mandrel into the continuous fused silica sleeve to form an optical fiber preform.
  • the core layer is a silica glass layer doped with P 2 O 5 or B 2 O 3 , and the relative refractive index ⁇ n 1 of the core layer is 0.3% to 0.4%; the inner cladding layer is doped with GeO 2
  • the relative refractive index ⁇ n 2 of the inner cladding layer is -0.05% to -0.01%, and the ratio b/a of the fiber core rod diameter b to the core layer diameter a is 3 to 5.
  • the relative refractive index ⁇ n 3 of the outer cladding layer is -0.25% to -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 7-9.
  • the synthetic mandrel is fixed in the center of the continuous fused silica sleeve in the RIC process, and the gap between the synthetic mandrel and the continuous fused silica sleeve is controlled to be less than 3 mm, and the effective diameter d of the optical fiber preform is equal to the diameter of the synthetic mandrel.
  • the ratio d/c of c is 2 ⁇ 3.
  • the metal impurity content in the continuous fused quartz sleeve is less than 20 ppm, and the hydroxyl content is less than 6 ppm.
  • the present invention also provides an optical fiber preform manufactured by the above method.
  • the present invention also provides a single-mode optical fiber, which is formed by directly drawing the above-mentioned optical fiber preform, or formed by drawing after drawing.
  • OVD process Use external vapor deposition and sintering process to prepare the required thickness of quartz glass.
  • VAD process Use axial vapor deposition and sintering process to prepare quartz glass of required thickness.
  • RIC process The synthetic mandrel and sleeve are processed, including tapering, extension, corrosion, cleaning, and drying, and then the synthetic mandrel is inserted into the sleeve to form a large-size optical fiber preform.
  • Continuous fused quartz casing a casing made of natural quartz sand using continuous melting process.
  • the relative refractive index ⁇ n 1 of the core layer is defined by the following equation:
  • n 1 is the absolute refractive index of the core layer
  • n c is the absolute refractive index of pure silica glass.
  • the relative refractive index of the inner cladding ⁇ n 2 is defined by the following equation:
  • n 2 is the absolute refractive index of the inner cladding
  • n c is the absolute refractive index of pure silica glass.
  • the relative refractive index ⁇ n 3 of the outer cladding is defined by the following equation:
  • n 3 is the absolute refractive index of the cladding
  • n c is the absolute refractive index of pure silica glass.
  • the effective diameter of the optical fiber preform is the outer diameter of the solid preform, and for the RIC preform,
  • the CSA is the cross-sectional area
  • Core/clad concentricity error the distance between the center of the core layer of the fiber and the center of the fiber.
  • the present invention uses the VAD process to prepare an optical fiber core rod including a core layer and an inner cladding layer, and then prepares an outer cladding layer containing Sb 2 O 3 -F through the OVD process, and finally prepares a large-size and low-loss optical fiber preform through the RIC process, wherein: After the sintering process, the reasonable outer cover layer deposited by the OVD process is further subjected to a heat treatment process, so that the barrier layer has a reasonable material composition and structure, which can effectively prevent the metal impurities and hydroxyl groups in the fused quartz sleeve from diffusing to the core layer, effectively reducing The loss of the drawn fiber is reduced, and the diameter of the synthetic mandrel prepared by the OVD process is uniform, which can accurately control the gap between the sleeve and the synthetic mandrel in the RIC process and reduce the concentricity error of the fiber core/cladding; the powder mandrel is prepared by the VAD method, Then through reasonable dehydroxy
  • the diameter of the optical fiber preform prepared by the present invention can reach 211mm
  • the drawing length of a single preform can reach 2920km
  • the attenuation of the prepared optical fiber at 1310nm wavelength is as low as 0.271dB/km
  • the attenuation coefficient at 1383nm wavelength is as low as 0.245dB/km
  • the attenuation coefficient at 1550nm wavelength is as low as 0.145dB/km
  • the optical fiber prepared from the optical fiber preform has a mode field diameter of 8.1 ⁇ 9.2 ⁇ m at 1310nm wavelength
  • the cut-off wavelength of the optical fiber is 1251nm ⁇ 1271nm .
  • the powder core rod is prepared by the axial vapor deposition method (VAD 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, pass Cl into the sintering furnace 2 gas and He gas, Cl 2 gas flow rate is 1000mL/min, He gas flow rate is 20L/min, and dehydroxylation temperature is 800°C; during fluorine doping treatment, SiF 4 gas and He gas, SiF 4 gas and The flow ratio of He gas is 4:1, in which the He gas flow rate is 30L/min, and the sintering furnace temperature is 1000°C; during vitrification, only He gas is introduced into the sintering furnace, and the He gas flow rate is 40L/min, vitrification The temperature is 1400°C;
  • the fiber core rod has a core-cladding ratio b/a of 3
  • the core layer is a silica glass layer doped with P 2 O 5 , and the relative refractive index difference ⁇ n 1 of the core layer is 0.3%
  • the layer is a silica glass layer doped with GeO 2 -F mixture, and the relative refractive index ⁇ n 2 of the inner cladding layer is -0.05%.
  • the OVD process is used to deposit the outer covering containing the Sb 2 O 3 -F mixture on the outside of the optical fiber core rod, and then perform sintering treatment to obtain a synthetic core rod;
  • the sintering treatment method is: inert gas and chlorine gas are passed into the sintering furnace, Cl 2
  • the gas flow rate is 800mL/min and the He gas flow rate is 40L/min.
  • the sintering furnace is raised to 600°C at a heating rate of 50°C/min, kept for 2 hours, and then raised to 1000°C at a heating rate of 30°C/min. Keep the temperature for 4 hours, and finally increase it to 1300°C at a heating rate of 10°C/min, and keep it for 7 hours;
  • the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 7 and the relative refractive index ⁇ n 3 of the outer cladding layer is -0.25%;
  • the RIC process to combine the synthetic core rod and the continuous fused silica sleeve into an optical fiber preform, specifically: the surface of the synthetic core rod is corroded with a mixed acid of hydrofluoric acid and nitric acid with a molar ratio of 1:0.5, and the corrosion depth is not less than 0.6mm, then clean and dry the corroded synthetic mandrel, insert the synthetic mandrel into the continuous fused quartz sleeve, and fix the synthetic mandrel in the center of the continuous fused quartz sleeve to control the synthetic mandrel and continuous fused quartz sleeve The gap between them is less than 3mm, and the fiber preform is combined into an optical fiber preform.
  • the diameter of the optical fiber preform reaches 201mm.
  • the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 2, and the prepared optical fiber preform is drawn online
  • the length of a single rod can reach 2850km.
  • the metal impurity content of the fused silica sleeve is shown in Table 1, and the performance parameters of the optical fiber are shown in Table 2.
  • the powder core rod is prepared by the axial vapor deposition method (VAD 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, pass Cl into the sintering furnace 2 gas and He gas, Cl 2 gas flow rate is 1000mL/min, He gas flow rate is 20L/min, and dehydroxylation temperature is 1000°C; during fluorine doping treatment, SiF 4 gas and He gas, SiF 4 gas and The flow ratio of He gas is 3:1, among which the He gas flow is 30L/min, and the sintering furnace temperature is 1300°C; during vitrification, only He gas is introduced into the sintering furnace, and the He gas flow is 40L/min, vitrification The temperature is 1600°C;
  • the fiber core rod has a core-wrap ratio b/a of 5
  • the core layer is a silica glass layer doped with B 2 O 3 , and the relative refractive index difference ⁇ n 1 of the core layer is 0.4%
  • the layer is a silica glass layer doped with GeO 2 -F mixture, and the relative refractive index ⁇ n 2 of the inner cladding layer is -0.01%.
  • the OVD process is used to deposit the outer covering containing the Sb 2 O 3 -F mixture on the outside of the optical fiber core rod, and then perform sintering treatment to obtain a synthetic core rod;
  • the sintering treatment method is: inert gas and chlorine gas are passed into the sintering furnace, Cl 2
  • the gas flow rate is 800mL/min and the He gas flow rate is 40L/min.
  • the sintering furnace is raised to 800°C at a heating rate of 60°C/min, kept for 1 hour, and then raised to 1200°C at a heating rate of 40°C/min. Insulate for 2h, and finally rise to 1500°C at a heating rate of 20°C/min for 5h;
  • the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 9 and the relative refractive index ⁇ n 3 of the outer cladding layer is -0.1%;
  • the RIC process to combine the synthetic mandrel and the continuous fused silica sleeve into an optical fiber preform, specifically: the surface of the synthetic mandrel is corroded with a mixed acid of hydrofluoric acid and nitric acid with a molar ratio of 1:1.5, and the corrosion depth is not less than 0.6mm, then clean and dry the corroded synthetic mandrel, insert the synthetic mandrel into the continuous fused quartz sleeve, and fix the synthetic mandrel in the center of the continuous fused quartz sleeve to control the synthetic mandrel and continuous fused quartz sleeve The gap between them is less than 3mm, and the fiber preform is combined into an optical fiber preform.
  • the diameter of the optical fiber preform reaches 211mm.
  • the ratio d/c of the effective diameter d of the optical fiber preform to the composite core rod diameter c is 3, and the prepared optical fiber preform is drawn online
  • the length of a single rod can reach 2920km; among them, the metal impurity content of the fused silica sleeve is shown in Table 3, and the performance parameters of the optical fiber are shown in Table 4.
  • the powder core rod is prepared by the axial vapor deposition method (VAD 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, pass Cl into the sintering furnace 2 gas and He gas, Cl 2 gas flow rate is 1000mL/min, He gas flow rate is 20L/min, and dehydroxylation temperature is 900°C; during fluorine doping treatment, SiF 4 gas and He gas, SiF 4 gas and The flow ratio of He gas is 4:1, in which the He gas flow rate is 30L/min, and the sintering furnace temperature is 1200°C; during vitrification, only He gas is introduced into the sintering furnace, and the He gas flow rate is 40L/min. The temperature is 1500°C;
  • the core-packing ratio b/a of the fiber core rod is 4.5
  • the core layer is a silica glass layer doped with B 2 O 3
  • the relative refractive index difference ⁇ n 1 of the core layer is 0.35%
  • the layer is a silica glass layer doped with GeO 2 -F mixture, and the relative refractive index ⁇ n 2 of the inner cladding layer is -0.03%.
  • the OVD process is used to deposit the outer covering containing the Sb 2 O 3 -F mixture on the outside of the optical fiber core rod, and then perform sintering treatment to obtain a synthetic core rod;
  • the sintering treatment method is: inert gas and chlorine gas are passed into the sintering furnace, Cl 2
  • the gas flow rate is 800mL/min
  • the He gas flow rate is 40L/min.
  • the sintering furnace is raised to 700°C at a heating rate of 55°C/min, kept for 1.5h, and then raised to 1100°C at a heating rate of 35°C/min ,Hold for 3h, finally raise to 1400°C at a heating rate of 15°C/min, keep for 6h;
  • the ratio c/a of the diameter c of the synthetic core rod to the diameter a of the core layer is 8, and the relative refractive index ⁇ n 3 of the outer cladding layer is -0.15%;
  • the RIC process to combine the synthetic mandrel and the continuous fused silica sleeve into an optical fiber preform.
  • the surface of the synthetic mandrel is corroded with a mixed acid of hydrofluoric acid and nitric acid at a molar ratio of 1:1, and the corrosion depth is not less than 0.6mm, then clean and dry the corroded synthetic mandrel, insert the synthetic mandrel into the continuous fused quartz sleeve, and fix the synthetic mandrel in the center of the continuous fused quartz sleeve to control the synthetic mandrel and continuous fused quartz sleeve The gap between them is less than 3mm, and the optical fiber preform is combined into an optical fiber preform.
  • the diameter of the optical fiber preform reaches 205mm, 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 prepared optical fiber preform is drawn online For low-loss optical fiber, the length of a single rod can reach 2895km; among them, the metal impurity content of the fused silica sleeve is shown in Table 5, and the performance parameters of the optical fiber are shown in Table 6.
  • Example 4 The only difference between Example 4 and Example 3 is that the sintered synthetic mandrel is heat-treated.
  • the heat treatment method is: the synthetic mandrel that has been kept at 1400°C for 6 hours is cooled to a temperature of ⁇ 100°C within 2 minutes, and then The cooled synthetic mandrel was heated to 700°C for 3 hours, and finally the synthetic mandrel was cooled to 300°C and held for 5 hours. Finally, the diameter of the obtained optical fiber preform reached 208mm.
  • the prepared optical fiber preform was drawn into low-loss optical fiber online. The length of the rod can reach 2905km.
  • the performance parameters of the optical fiber are shown in Table 7.
  • Example 5 The difference between Example 5 and Example 3 is that the sintered synthetic mandrel is heat-treated.
  • the heat treatment method is: the synthetic mandrel that has been kept at 1400°C for 6 hours is cooled to a temperature of ⁇ 100°C within 2 minutes, and then The cooled synthetic mandrel was heated to 1000°C for 2h, and finally the synthetic mandrel was cooled to 500°C and held for 3h. Finally, the diameter of the obtained optical fiber preform reached 210mm.
  • the prepared optical fiber preform was drawn into low-loss optical fiber online. The length of the rod can reach 2913km, and the performance parameters of the optical fiber are shown in Table 8.

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Abstract

L'invention concerne une préforme de fibre optique basée sur un manchon de quartz fondu continu, et un procédé de fabrication associé. Le procédé de fabrication comprend : la préparation d'une broche de fibre optique avec une couche centrale et une couche de gainage intérieure de l'intérieur vers l'extérieur à l'aide d'un procédé VAD ; le dépôt d'un corps lâche de couche barrière contenant un mélange Sb2O3-F sur la partie externe de la broche de fibre optique à l'aide d'un procédé OVD, puis la réalisation d'un traitement de frittage pour obtenir une broche synthétique ; et la combinaison de la broche synthétique et d'un manchon de quartz fondu continu à l'aide d'un procédé RIC pour obtenir la préforme de fibre optique. Le diamètre de la préforme peut atteindre 211 mm, la longueur d'étirage d'une seule préforme peut atteindre 2920 km, l'atténuation d'une fibre optique étirée à 1310 nm est aussi faible que 0,271 dB/km, le coefficient d'atténuation à 1383 nm est aussi faible que 0,245 dB/km, le coefficient d'atténuation à 1550 nm est aussi faible que 0,145 dB/km, le diamètre de champ de mode à 1310 nm est de 8,1 µm à 9,2 µm, et la longueur d'onde de coupure de câble optique est de 1251 nm à 1271 nm.
PCT/CN2019/114350 2019-03-01 2019-10-30 Préforme de fibre optique basé sur un manchon de quartz fondu continu, et procédé de fabrication associé WO2020177352A1 (fr)

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CN201910156569.XA CN110028235B (zh) 2019-03-01 2019-03-01 一种基于连熔石英套管的光纤预制棒及其制造方法

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CN110028235B (zh) * 2019-03-01 2020-09-08 江苏永鼎股份有限公司 一种基于连熔石英套管的光纤预制棒及其制造方法

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