WO2020155707A1 - 一种大尺寸低损耗的光纤预制棒及其制备方法 - Google Patents

一种大尺寸低损耗的光纤预制棒及其制备方法 Download PDF

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WO2020155707A1
WO2020155707A1 PCT/CN2019/114440 CN2019114440W WO2020155707A1 WO 2020155707 A1 WO2020155707 A1 WO 2020155707A1 CN 2019114440 W CN2019114440 W CN 2019114440W WO 2020155707 A1 WO2020155707 A1 WO 2020155707A1
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Prior art keywords
optical fiber
core rod
fiber preform
synthetic
low
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PCT/CN2019/114440
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English (en)
French (fr)
Inventor
莫思铭
李想
杨红蕾
李凡
邵珠峰
周莉
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江苏永鼎股份有限公司
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Publication of WO2020155707A1 publication Critical patent/WO2020155707A1/zh

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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]
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
    • C03B37/01453—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering for doping the preform with flourine

Definitions

  • the invention relates to a large-size and low-loss optical fiber preform and a preparation method thereof, and belongs to the technical field of optical fiber preform preparation.
  • the VAD process (Vapor Axial Deposition Method) is often used for the production of large-scale optical fiber preform core rods.
  • Large-size optical fiber preforms are prepared on the basis of the core rods prepared by the VAD process.
  • the casing method is usually used to manufacture the outer coating outside the core rod.
  • the hydroxyl content and metal impurity content of the current quartz sleeve are relatively high.
  • the hydroxyl and metal impurities entering the core layer of the mandrel will increase the fiber loss.
  • the core layer and the cladding layer close to the core layer have a low hydroxyl content in a certain thickness to reduce hydrogen loss, but also require that the core rod can effectively block the hydroxyl groups of the quartz sleeve. And metal impurities enter the core layer to ultimately reduce fiber loss and greatly improve the transmission quality of the fiber.
  • the technical problem to be solved by the present invention is: in order to solve the technical problem of large loss of large-size optical fiber preform obtained by preparing the core rod by the VAD process and manufacturing the outer coating outside the core rod by the sleeve method in the prior art, a large-scale optical fiber preform is provided. Optical fiber preform with low loss in size and preparation method thereof.
  • a method for preparing a large-size and low-loss optical fiber preform the steps are as follows:
  • the fiber core rod is prepared by the VAD process, and the surface temperature of the outer cladding loose body is reached to 1000-1100 °C by deposition torch, so that the density of the outer cladding loose body is greater than 0.85g/cm 3 , and then the core rod is dehydroxylated in the sintering furnace Treatment, fluorine doping treatment and vitrification treatment to obtain an optical fiber core rod; the core layer of the optical fiber core rod is the core layer and the inner cladding layer from the inside to the outside, and the ratio b/a of the diameter b of the optical fiber core rod to the core layer diameter a is 3.0 ⁇ 5.0;
  • inert gas and chlorine gas are introduced into the sintering furnace to raise the sintering furnace to 900-1050°C at a heating rate of 9-12°C/min for 4 to 5 hours; when fluorine-doped treatment, sintering Fluorine-containing gas and inert gas are introduced into the furnace, so that the sintering furnace is
  • Insert one or more sections of the optical fiber core rod into a small pure silica tube first use a fluorine-containing gas to chemically etch the outer surface of the core rod and the inner surface of the small tube, and then melt them together to obtain a synthetic core rod.
  • the ratio c/a of the diameter c to the core layer diameter a is 7.0 ⁇ 9.0;
  • the surface of the synthetic mandrel is etched with an acid solution, and then the corroded synthetic mandrel is cleaned and dried, and the synthetic mandrel is inserted into a large pure quartz sleeve to form a large-size and low-loss optical fiber preform.
  • the synthetic core rod in the sintering furnace rotates at a speed of 3-8 rpm; during vitrification, the synthetic core rod in the sintering furnace rotates at a speed of 9-15 rpm.
  • the chlorine gas flow rate for the dehydroxylation treatment is 900-1100 mL/min, and the inert gas flow rate is 20-40 L/min;
  • the fluorine-containing gas is SF 6 , SiF 4 , CF 4 , C 2 F 6 , C 3 F 8 , C 2 F 2 Cl 2 , SOF 2 or a combination of two or more of them, the ratio of the flow rate of the fluorine-containing gas to the inert gas flow through the fluorine doping treatment is 3:1 ⁇ 5:1, of which the inert The gas flow rate is 20-40L/min; the inert gas flow rate for vitrification is 30-50L/min.
  • the core layer is a silica glass layer doped with B 2 O 3 , and the relative refractive index ⁇ n i of the core layer is 0.35% to 0.45%.
  • the acid solution is a mixed acid of hydrofluoric acid and hydrochloric acid, the molar ratio of hydrogen fluoride to hydrogen chloride is 1:0.5 to 1.5, and the corrosion depth of the synthetic core rod is not less than 0.6 mm.
  • the synthetic mandrel is fixed in the center of the pure quartz large sleeve, and the gap between the synthetic mandrel and the continuous fused silica sleeve is controlled to be less than 3 mm.
  • the present invention also provides a large-size and low-loss optical fiber preform manufactured by the above method.
  • the present invention also provides a low-loss single-mode optical fiber, which is formed by directly drawing the above-mentioned large-size and low-loss optical fiber preform, or drawing after drawing.
  • the present invention uses the VAD process to prepare the optical fiber core rod. After the loose body of the outer coating layer is compacted, the core rod is subjected to dehydroxylation treatment, fluorine doping treatment and vitrification treatment.
  • the reasonable process not only effectively removes the hydroxyl group of the core rod, but also makes the inner cladding layer It has a reasonable structure, which can effectively prevent the metal impurities and hydroxyl in the quartz sleeve from diffusing to the core layer.
  • the fluorine doping treatment can also concentrate the optical power on the core layer, effectively reducing the loss of the drawn fiber, and then insert the fiber core rod
  • the pure silica small sleeve is fused together to obtain a synthetic core rod, and then the synthetic core rod is inserted into the pure silica large sleeve to form a large-size and low-loss optical fiber preform; the optical fiber preform prepared by the present invention
  • the diameter of a single preform can reach 212mm, the length of a single preform can reach 2950km, the attenuation of the fiber at 1310nm wavelength is ⁇ 0.307dB/km, the attenuation coefficient at 1383nm wavelength is ⁇ 0.272dB/km, and the attenuation coefficient at 1550nm wavelength is ⁇ 0.184dB/km.
  • This embodiment provides a method for preparing a large-size and low-loss optical fiber preform, and the steps are as follows:
  • the fiber core rod is prepared by the VAD process, and the surface temperature of the outer cladding loose body is reached 1050 °C by deposition torch, so that the density of the outer cladding loose body is greater than 0.85 g/cm 3 , and then the core rod is dehydroxylated in the sintering furnace. Fluorine doping treatment and vitrification treatment to obtain an optical fiber core rod; the core layer of the optical fiber core rod is the core layer and the inner cladding layer from the inside to the outside.
  • the ratio b/a of the diameter b of the fiber core rod to the core layer diameter a is 4.0, and the core layer
  • the ratio of SF 6 gas and helium gas flow is 4:1, of which the helium flow rate is 30L/min, and the synthetic mandrel rotates at a speed of 5rpm. Raise the sintering furnace to 1200°C at a heating rate of 6°C/min for 1.5h; during vitrification, only helium is introduced into the sintering furnace, the flow of helium is 40L/min, and the synthetic mandrel rotates at a speed of 12rpm , And then increase the sintering furnace to 1550°C at a heating rate of 10°C/min, and keep it for 5.5h;
  • Insert one or more sections of the optical fiber core rod into a small pure silica tube first use a fluorine-containing gas to chemically etch the outer surface of the core rod and the inner surface of the small tube, and then melt them together to obtain a synthetic core rod.
  • the ratio c/a of the diameter c of the core layer a is 8.0;
  • the surface of the synthetic mandrel is corroded with a mixed acid of hydrofluoric acid and hydrochloric acid (the molar ratio of hydrogen fluoride to hydrogen chloride is 1:1), the corrosion depth is not less than 0.6mm, and then the corroded synthetic mandrel is washed and dried, and the synthetic mandrel Insert the center of the pure silica large sleeve, control the gap between the synthetic core rod and the continuous fused silica sleeve to be less than 3mm, and combine it into a large-size and low-loss optical fiber preform.
  • the diameter of the optical fiber preform reaches 208mm, which will make the large size and low
  • the lossy optical fiber preform draws low-loss optical fiber online.
  • the length of a single rod can reach 2800km.
  • the fiber attenuation at 1310nm wavelength is 0.305dB/km, and the attenuation coefficient at 1383nm wavelength is 0.271dB/km, at 1550nm wavelength.
  • the attenuation coefficient is 0.181dB/km.
  • This embodiment provides a method for preparing a large-size and low-loss optical fiber preform, and the steps are as follows:
  • the fiber core rod is prepared by the VAD process, and the surface temperature of the outer cladding loose body is reached to 1000 °C by deposition torch, so that the density of the outer cladding loose body is greater than 0.85 g/cm 3 , and then the core rod is dehydroxylated in the sintering furnace. Fluorine doping treatment and vitrification treatment to obtain an optical fiber core rod; the core layer of the optical fiber core rod is the core layer and the inner cladding layer from the inside to the outside.
  • the ratio b/a of the diameter b of the fiber core rod to the core layer diameter a is 3.0, and the core layer
  • helium and chlorine are introduced into the sintering furnace, the flow of chlorine is 900mL/min, the flow of helium is 40L/min, and the synthetic mandrel rotates at a speed of 3rpm to make the sintering furnace at 9°C/min
  • the heating rate was increased to 900°C, and the temperature was kept for 5 hours; during the fluorine doping treatment, SiF 4 gas and helium gas were introduced into the sintering furnace.
  • the ratio of SiF 4 gas to helium gas flow rate was 3:1, of which the helium gas flow rate was 20L/min.
  • the synthetic mandrel rotates at a speed of 3 rpm, so that the sintering furnace rises to 1100 °C at a heating rate of 5 °C/min, and the temperature is kept for 2 hours; during vitrification, only helium gas is introduced into the sintering furnace, and the helium flow rate is 30L/min.
  • the synthetic mandrel rotates at a speed of 9 rpm, and then the sintering furnace is raised to 1450 °C at a heating rate of 8 °C/min, and the temperature is kept for 6 hours;
  • Insert one or more sections of the optical fiber core rod into a small pure silica tube first use a fluorine-containing gas to chemically etch the outer surface of the core rod and the inner surface of the small tube, and then melt them together to obtain a synthetic core rod.
  • the ratio c/a of the diameter c of the core layer a is 7.0;
  • the surface of the synthetic core rod is corroded with a mixed acid of hydrofluoric acid and hydrochloric acid (the molar ratio of hydrogen fluoride to hydrogen chloride is 1:0.5), the corrosion depth is not less than 0.6mm, and then the corroded synthetic core rod is cleaned and dried, and the synthetic core rod Insert the center of the pure silica large sleeve, control the gap between the synthetic core rod and the continuous fused silica sleeve to be less than 3mm, and combine it into a large-size and low-loss optical fiber preform.
  • a mixed acid of hydrofluoric acid and hydrochloric acid the molar ratio of hydrogen fluoride to hydrogen chloride is 1:0.5
  • the diameter of the optical fiber preform reaches 201mm, which will make the large size and low
  • the lossy optical fiber preform draws low-loss optical fiber online
  • the length of a single rod can reach 2710km
  • the attenuation of the optical fiber at 1310nm wavelength is 0.302dB/km
  • the attenuation coefficient at 1383nm wavelength is 0.272dB/km
  • the attenuation coefficient is 0.184dB/km.
  • This embodiment provides a method for preparing a large-size and low-loss optical fiber preform, and the steps are as follows:
  • the fiber core rod is prepared by the VAD process, and the surface temperature of the loose body of the outer cladding layer is reached to 1100 °C by deposition torch, so that the density of the loose body of the outer cladding layer is greater than 0.85g/cm 3 , and then the core rod is dehydroxylated in the sintering furnace. Fluorine doping treatment and vitrification treatment to obtain an optical fiber core rod; the core layer of the optical fiber core rod is the core layer and the inner cladding layer from the inside to the outside.
  • the ratio b/a of the fiber core rod diameter b to the core layer diameter a is 5.0, and the core layer
  • helium and chlorine are introduced into the sintering furnace, the flow of chlorine is 1100mL/min, the flow of helium is 20L/min, the synthetic mandrel rotates at a speed of 8rpm, and the sintering furnace is set at 12°C/min.
  • the heating rate is increased to 1050°C, and the temperature is kept for 4 hours; during the fluorine doping treatment, CF 4 gas and helium gas are introduced into the sintering furnace, and the ratio of CF 4 gas to helium flow rate is 5:1, of which the helium flow rate is 40L/min.
  • the synthetic mandrel rotates at a speed of 8 rpm, so that the sintering furnace rises to 1250 °C at a heating rate of 8 °C/min, and the temperature is kept for 1 hour; during vitrification, only helium gas is passed into the sintering furnace, and the helium flow rate is 50 L/min.
  • the synthetic mandrel rotates at a speed of 15 rpm, and then the sintering furnace is raised to 1650 °C at a heating rate of 12 °C/min, and the temperature is kept for 5 hours;
  • Insert one or more sections of the optical fiber core rod into a small pure silica tube first use a fluorine-containing gas to chemically etch the outer surface of the core rod and the inner surface of the small tube, and then melt them together to obtain a synthetic core rod.
  • the ratio c/a of the diameter c of the core layer a is 9.0;
  • the surface of the synthetic core rod is corroded with a mixed acid of hydrofluoric acid and hydrochloric acid (the molar ratio of hydrogen fluoride to hydrogen chloride is 1:1.5), the corrosion depth is not less than 0.6mm, and then the corroded synthetic core rod is cleaned and dried, and the synthetic core rod Insert the center of the pure silica large sleeve, control the gap between the synthetic core rod and the continuous fused silica sleeve to be less than 3mm, and combine it into a large-size and low-loss optical fiber preform.
  • the diameter of the optical fiber preform reaches 212mm, which will make the large size and low
  • the lossy optical fiber preform draws low-loss optical fiber online.
  • the length of a single rod can reach 2950km.
  • the attenuation of the optical fiber at 1310nm wavelength is 0.307dB/km
  • the attenuation coefficient at 1383nm wavelength is 0.268dB/km
  • the attenuation coefficient is 0.179dB/km.

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Abstract

一种大尺寸低损耗的光纤预制棒及其制备方法，利用VAD工艺制备光纤芯棒，使外包层疏松体致密后，对芯棒进行脱羟处理、掺氟处理和玻璃化处理，之后将光纤芯棒插入纯石英小套管内并将其熔缩到一起，得到合成芯棒，再将合成芯棒插入纯石英大套管中，组合成大尺寸低损耗的光纤预制棒。通过该方法制备得到的光纤预制棒的直径可达212mm，单根预制棒拉纤长度可达到2950km，光纤在1310nm波长处的衰减≤0.307dB/km，在1383nm波长处的衰减系数≤0.272dB/km，在1550nm波长处的衰减系数≤0.184dB/km。

Description

一种大尺寸低损耗的光纤预制棒及其制备方法
本申请要求2019年1月29日向中国国家知识产权局递交的申请号为201910085729.6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。
技术领域
本发明涉及一种大尺寸低损耗的光纤预制棒及其制备方法，属于光纤预制棒制备技术领域。
背景技术
VAD工艺(气相轴向沉积法)常用于大规模光纤预制棒芯棒的生产，在VAD工艺制备的芯棒基础上制备大尺寸的光纤预制棒，通常采用套管法在芯棒外制造外包层，但是目前的石英套管的羟基含量和金属杂质含量均较高，以其作为生产光纤预制棒的外包层时，羟基和金属杂质进入芯棒芯层会增大光纤损耗。因此，要制备大尺寸低损耗的光纤预制棒，不仅要求芯层与靠近芯层一定厚度内的包层内羟基含量很低，以减少氢损，还要求芯棒能够有效阻挡石英套管的羟基和金属杂质进入芯层，以最终减少光纤损耗，大大提高光纤的传输质量。
发明内容
本发明要解决的技术问题是：为解决现有技术中以VAD工艺制备芯棒，以套管法在芯棒外制造外包层得到的大尺寸光纤预制棒损耗大的技术问题，提供一种大尺寸低损耗的光纤预制棒及其制备方法。
一种大尺寸低损耗的光纤预制棒的制备方法，步骤如下：
利用VAD工艺制备光纤芯棒，通过沉积喷灯将外包层疏松体的表面温度达到1000～1100℃，使外包层疏松体的密度大于0.85g/cm 3，然后在烧结炉中对芯棒进行脱羟处理、掺氟处理和玻璃化处理，得到光纤芯棒；所述光纤芯棒内到外依次是芯层和内包层，光纤芯棒的直径b与芯层直径a的比值b/a为3.0～5.0；其中，脱羟处理时，烧结炉内通入惰性气体和氯气，使烧结炉以9～12℃/min的升温速率升到900～1050℃，保温4～5h；掺氟处理时，烧结炉内通入含氟气体和惰性气体，使烧结炉以5～8℃/min的升温速率升到1100～1250℃，保温1～2h；玻璃化处理时，烧结炉内只通入惰性气体，然后使烧结炉以8～12℃/min的升温速率升到1450～1650℃，保温5～6h；
将一段或多段光纤芯棒插入纯石英小套管内，先用含氟气体将芯棒外表面和小套管内表面进行化学刻蚀，然后将其熔缩到一起，得到合成芯棒，合成芯棒的直径c与芯层直径a的比值c/a为7.0～9.0；
将合成芯棒表面用酸性溶液腐蚀，然后将腐蚀后的合成芯棒清洗干燥，将合成芯棒插入纯石英大套管中，组合成大尺寸低损耗的光纤预制棒。
优选地，脱羟处理和掺氟处理时，烧结炉内的合成芯棒以3～8rpm的速度自转；玻璃化处理时，烧结炉内的合成芯棒以9～15rpm的速度自转。
优选地，所述脱羟处理的氯气流量为900～1100mL/min，惰性气体流量为20～40L/min；所述的含氟气体为SF 6、SiF 4、CF 4、C 2F 6、C 3F 8、C 2F 2Cl 2、SOF 2中的一种或两种以上的组合，掺氟处理通入的 含氟气体与惰性气体流量的比值为3:1～5:1，其中惰性气体流量为20～40L/min；玻璃化处理的惰性气体流量为30～50L/min。
优选地，所述芯层为掺入B 2O 3的二氧化硅玻璃层，芯层的相对折射率Δn i为0.35％～0.45％。
优选地，所述内包层的相对折射率为Δn 1＝-0.20％～-0.45％。
优选地，所述酸性溶液为为氢氟酸与盐酸的混合酸，氟化氢与氯化氢的摩尔比为1:0.5～1.5，对合成芯棒的腐蚀深度不小于0.6mm。
优选地，将合成芯棒固定在纯石英大套管中心，控制合成芯棒和连熔石英套管之间的间隙小于3mm。
本发明还提供一种由上述方法制造的大尺寸低损耗的光纤预制棒。
本发明还提供一种低损耗单模光纤，所述光纤由上述的大尺寸低损耗的光纤预制棒直接拉丝而成，或经拉伸后再拉丝而成。
本发明的有益效果是：
本发明利用VAD工艺制备光纤芯棒，使外包层疏松体致密后，对芯棒进行脱羟处理、掺氟处理和玻璃化处理，合理的工艺不仅有效脱除了芯棒的羟基，还使得内包层具有合理的结构，能够有效阻挡石英套管中的金属杂质和羟基扩散至芯层，掺氟处理还能够使光功率集中在芯层，有效降低了拉制光纤的损耗，之后将光纤芯棒插入纯石英小套管内并将其熔缩到一起，得到合成芯棒，再将合成芯棒插入纯石英大套管中，组合成大尺寸低损耗的光纤预制棒；本发明制备得到的光纤预制棒的直径可达212mm，单根预制棒拉纤长度可达到2950km， 光纤在1310nm波长处的衰减≤0.307dB/km，在1383nm波长处的衰减系数≤0.272dB/km，在1550nm波长处的衰减系数≤0.184dB/km。
具体实施方式
现在对本发明作进一步详细的说明。
实施例1
本实施例提供一种大尺寸低损耗的光纤预制棒的制备方法，步骤如下：
利用VAD工艺制备光纤芯棒，通过沉积喷灯将外包层疏松体的表面温度达到1050℃，使外包层疏松体的密度大于0.85g/cm 3，然后在烧结炉中对芯棒进行脱羟处理、掺氟处理和玻璃化处理，得到光纤芯棒；所述光纤芯棒内到外依次是芯层和内包层，光纤芯棒的直径b与芯层直径a的比值b/a为4.0，芯层为掺入B 2O 3的二氧化硅玻璃层，芯层的相对折射率Δn i为0.40％，内包层的相对折射率为Δn 1＝-0.30％；其中，脱羟处理时，烧结炉内通入氦气和氯气，氯气流量为1000mL/min，氦气流量为30L/min，合成芯棒以5rpm的速度自转，使烧结炉以10℃/min的升温速率升到1000℃，保温4.5h；掺氟处理时，烧结炉内通入SF 6气体和氦气，SF 6气体与氦气流量的比值为4:1，其中氦气流量为30L/min，合成芯棒以5rpm的速度自转，使烧结炉以6℃/min的升温速率升到1200℃，保温1.5h；玻璃化处理时，烧结炉内只通入氦气，氦气流量为40L/min，合成芯棒以12rpm的速度自转，然后使烧结炉以10℃/min的升温速率升到1550℃，保温5.5h；
将一段或多段光纤芯棒插入纯石英小套管内，先用含氟气体将芯 棒外表面和小套管内表面进行化学刻蚀，然后将其熔缩到一起，得到合成芯棒，合成芯棒的直径c与芯层直径a的比值c/a为8.0；
将合成芯棒表面用氢氟酸与盐酸的混合酸(氟化氢与氯化氢的摩尔比为1:1)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，将合成芯棒插入纯石英大套管中心，控制合成芯棒和连熔石英套管之间的间隙小于3mm，组合成大尺寸低损耗的光纤预制棒，光纤预制棒的直径达到208mm，将制备的大尺寸低损耗光纤预制棒在线拉制低损耗光纤，单根棒拉纤长度可达到2800km，光纤在1310nm波长处的衰减为0.305dB/km，在1383nm波长处的衰减系数为0.271dB/km，在1550nm波长处的衰减系数为0.181dB/km。
实施例2
本实施例提供一种大尺寸低损耗的光纤预制棒的制备方法，步骤如下：
利用VAD工艺制备光纤芯棒，通过沉积喷灯将外包层疏松体的表面温度达到1000℃，使外包层疏松体的密度大于0.85g/cm 3，然后在烧结炉中对芯棒进行脱羟处理、掺氟处理和玻璃化处理，得到光纤芯棒；所述光纤芯棒内到外依次是芯层和内包层，光纤芯棒的直径b与芯层直径a的比值b/a为3.0，芯层为掺入B 2O 3的二氧化硅玻璃层，芯层的相对折射率Δn i为0.35％，内包层的相对折射率为Δn 1＝-0.20％；
其中，脱羟处理时，烧结炉内通入氦气和氯气，氯气流量为900mL/min，氦气流量为40L/min，合成芯棒以3rpm的速度自转，使烧结炉以9℃/min的升温速率升到900℃，保温5h；掺氟处理时，烧 结炉内通入SiF 4气体和氦气，SiF 4气体与氦气流量的比值为3:1，其中氦气流量为20L/min，合成芯棒以3rpm的速度自转，使烧结炉以5℃/min的升温速率升到1100℃，保温2h；玻璃化处理时，烧结炉内只通入氦气，氦气流量为30L/min，合成芯棒以9rpm的速度自转，然后使烧结炉以8℃/min的升温速率升到1450℃，保温6h；
将一段或多段光纤芯棒插入纯石英小套管内，先用含氟气体将芯棒外表面和小套管内表面进行化学刻蚀，然后将其熔缩到一起，得到合成芯棒，合成芯棒的直径c与芯层直径a的比值c/a为7.0；
将合成芯棒表面用氢氟酸与盐酸的混合酸(氟化氢与氯化氢的摩尔比为1:0.5)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，将合成芯棒插入纯石英大套管中心，控制合成芯棒和连熔石英套管之间的间隙小于3mm，组合成大尺寸低损耗的光纤预制棒，光纤预制棒的直径达到201mm，将制备的大尺寸低损耗光纤预制棒在线拉制低损耗光纤，单根棒拉纤长度可达到2710km，光纤在1310nm波长处的衰减为0.302dB/km，在1383nm波长处的衰减系数为0.272dB/km，在1550nm波长处的衰减系数为0.184dB/km。
实施例3
本实施例提供一种大尺寸低损耗的光纤预制棒的制备方法，步骤如下：
利用VAD工艺制备光纤芯棒，通过沉积喷灯将外包层疏松体的表面温度达到1100℃，使外包层疏松体的密度大于0.85g/cm 3，然后在烧结炉中对芯棒进行脱羟处理、掺氟处理和玻璃化处理，得到光纤 芯棒；所述光纤芯棒内到外依次是芯层和内包层，光纤芯棒的直径b与芯层直径a的比值b/a为5.0，芯层为掺入B 2O 3的二氧化硅玻璃层，芯层的相对折射率Δn i为0.45％，内包层的相对折射率为Δn 1＝-0.45％；
其中，脱羟处理时，烧结炉内通入氦气和氯气，氯气流量为1100mL/min，氦气流量为20L/min，合成芯棒以8rpm的速度自转，使烧结炉以12℃/min的升温速率升到1050℃，保温4h；掺氟处理时，烧结炉内通入CF 4气体和氦气，CF 4气体与氦气流量的比值为5:1，其中氦气流量为40L/min，合成芯棒以8rpm的速度自转，使烧结炉以8℃/min的升温速率升到1250℃，保温1h；玻璃化处理时，烧结炉内只通入氦气，氦气流量为50L/min，合成芯棒以15rpm的速度自转，然后使烧结炉以12℃/min的升温速率升到1650℃，保温5h；
将一段或多段光纤芯棒插入纯石英小套管内，先用含氟气体将芯棒外表面和小套管内表面进行化学刻蚀，然后将其熔缩到一起，得到合成芯棒，合成芯棒的直径c与芯层直径a的比值c/a为9.0；
将合成芯棒表面用氢氟酸与盐酸的混合酸(氟化氢与氯化氢的摩尔比为1:1.5)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，将合成芯棒插入纯石英大套管中心，控制合成芯棒和连熔石英套管之间的间隙小于3mm，组合成大尺寸低损耗的光纤预制棒，光纤预制棒的直径达到212mm，将制备的大尺寸低损耗光纤预制棒在线拉制低损耗光纤，单根棒拉纤长度可达到2950km，光纤在1310nm波长处的衰减为0.307dB/km，在1383nm波长处的衰减系数为0.268dB/km，在1550nm波长处的衰减系数为0.179dB/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。

Claims (9)

  1. 一种大尺寸低损耗的光纤预制棒的制备方法，其特征在于，步骤如下：
    利用VAD工艺制备光纤芯棒，通过沉积喷灯将外包层疏松体的表面温度达到1000～1100℃，使外包层疏松体的密度大于0.85g/cm 3，然后在烧结炉中对芯棒进行脱羟处理、掺氟处理和玻璃化处理，得到光纤芯棒；所述光纤芯棒内到外依次是芯层和内包层，光纤芯棒的直径b与芯层直径a的比值b/a为3.0～5.0；其中，脱羟处理时，烧结炉内通入惰性气体和氯气，使烧结炉以9～12℃/min的升温速率升到900～1050℃，保温4～5h；掺氟处理时，烧结炉内通入含氟气体和惰性气体，使烧结炉以5～8℃/min的升温速率升到1100～1250℃，保温1～2h；玻璃化处理时，烧结炉内只通入惰性气体，然后使烧结炉以8～12℃/min的升温速率升到1450～1650℃，保温5～6h；
    将一段或多段光纤芯棒插入纯石英小套管内，先用含氟气体将芯棒外表面和小套管内表面进行化学刻蚀，然后将其熔缩到一起，得到合成芯棒，合成芯棒的直径c与芯层直径a的比值c/a为7.0～9.0；
    将合成芯棒表面用酸性溶液腐蚀，然后将腐蚀后的合成芯棒清洗干燥，将合成芯棒插入纯石英大套管中，组合成大尺寸低损耗的光纤预制棒。
  2. 根据权利要求1所述的大尺寸低损耗的光纤预制棒的制备方法，其特征在于，脱羟处理和掺氟处理时，烧结炉内的合成芯棒以3～8rpm的速度自转；玻璃化处理时，烧结炉内的合成芯棒以9～15rpm的速度自转。
  3. 根据权利要求1或2所述的大尺寸低损耗的光纤预制棒的制备方法，其特征在于，所述脱羟处理的氯气流量为900～1100mL/min，惰性气体流量为20～40L/min；所述的含氟气体为SF 6、SiF 4、CF 4、C 2F 6、C 3F 8、C 2F 2Cl 2、SOF 2中的一种或两种以上的组合，掺氟处理通入的含氟气体与惰性气体流量的比值为3:1～5:1，其中惰性气体流量为20～40L/min；玻璃化处理的惰性气体流量为30～50L/min。
  4. 根据权利要求1-3任一项所述的大尺寸低损耗的光纤预制棒的制备方法，其特征在于，所述芯层为掺入B 2O 3的二氧化硅玻璃层，芯层的相对折射率Δn i为0.35％～0.45％。
  5. 根据权利要求1-4任一项所述的大尺寸低损耗的光纤预制棒的制备方法，其特征在于，所述内包层的相对折射率为Δn 1＝-0.20％～-0.45％。
  6. 根据权利要求1-3任一项所述的大尺寸低损耗的光纤预制棒的制备方法，其特征在于，所述酸性溶液为氢氟酸与盐酸的混合酸，氟化氢与氯化氢的摩尔比为1:0.5～1.5，对合成芯棒的腐蚀深度不小于0.6mm。
  7. 根据权利要求1-6任一项所述的大尺寸低损耗的光纤预制棒的制备方法，其特征在于，将合成芯棒固定在纯石英大套管中心，控制合成芯棒和连熔石英套管之间的间隙小于3mm。
  8. 一种由权利要求1-7任一项所述的方法制造的大尺寸低损耗的光纤预制棒。
  9. 一种低损耗单模光纤，其特征在于，所述光纤由权利要求8所述的大尺寸低损耗的光纤预制棒直接拉丝而成，或经拉伸后再拉丝而成。
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CN113716856B (zh) * 2020-05-25 2022-12-23 中天科技精密材料有限公司 光纤预制棒的制造设备、方法及光纤预制棒
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