CN114634313B - Temperature matching optical fiber and preparation method thereof - Google Patents

Temperature matching optical fiber and preparation method thereof Download PDF

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Publication number
CN114634313B
CN114634313B CN202011463395.0A CN202011463395A CN114634313B CN 114634313 B CN114634313 B CN 114634313B CN 202011463395 A CN202011463395 A CN 202011463395A CN 114634313 B CN114634313 B CN 114634313B
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percent
glass
optical fiber
temperature
cladding
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CN114634313A (en
Inventor
徐天聪
袁辉平
王咏丽
隋宁菠
魏国盛
李进科
刘珊
郭永解
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Beijing Yiqing Research Institute Co ltd
Beijing Glass Research Institute Co ltd
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Beijing Yiqing Research Institute Co ltd
Beijing Glass Research Institute Co ltd
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C13/00Fibre or filament compositions
    • C03C13/04Fibre optics, e.g. core and clad fibre compositions
    • C03C13/045Silica-containing oxide glass compositions
    • C03C13/046Multicomponent glass compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/02Other methods of shaping glass by casting molten glass, e.g. injection moulding
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/01205Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • C03B37/01211Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
    • 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
    • C03B37/027Fibres composed of different sorts of glass, e.g. glass optical fibres
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C25/00Surface treatment of fibres or filaments made from glass, minerals or slags
    • C03C25/10Coating
    • C03C25/24Coatings containing organic materials
    • C03C25/26Macromolecular compounds or prepolymers
    • C03C25/28Macromolecular compounds or prepolymers obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • C03C25/285Acrylic resins
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02Optical fibres with cladding with or without a coating
    • GPHYSICS
    • G02OPTICS
    • G02BOPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02Optical fibres with cladding with or without a coating
    • G02B6/02395Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture

Abstract

The invention discloses a temperature matching optical fiber and a preparation method thereof, and is characterized in that the optical fiber section structure sequentially comprises a fiber core (1), a cladding (2), an inner coating (3) and an outer coating (4) from the center to the outside. The fiber core and the cladding material are multicomponent glass, and the inner coating and the outer coating material are acrylic resin materials. Wherein the fiber core glass component comprises 68-78% of SiO 2 3.9-5.9% of B 2 O 3 14.5-24.5% GeO 2 1-3% of P 2 O 5 0.1 to 0.3% of Al 2 O 3 0.2 to 0.4% of CaO, 0.2 to 0.4% of MgO, 0.1 to 0.2% of Na 2 O; the cladding glass component comprises 69-79% of SiO 2 19-23% of B 2 O 3 1.9-2.3% of GeO 2 1-3% of P 2 O 5 0.1 to 0.3% of Al 2 O 3 0.1 to 0.3% of CaO, 0.1 to 0.3% of MgO, 0.1 to 0.2% of Na 2 O. The preparation method of the optical fiber comprises the steps of melting fiber core glass and cladding glass, processing a preform rod and drawing the optical fiber. The optical fiber provided by the invention can be used for realizing low-loss fusion welding of the multicomponent glass optical fiber and the quartz optical fiber, and has good mechanical strength and bending resistance, and high practical value.

Description

Temperature matching optical fiber and preparation method thereof
Technical Field
The invention relates to a temperature matching optical fiber and a preparation method thereof, belonging to the field of special optical fibers. The optical fiber is used for transition between the multicomponent optical fiber and the quartz optical fiber, so that low-loss fusion bonding of the multicomponent optical fiber and the quartz optical fiber is realized.
Background
The generation and amplification of 2.1 μm wavelength ultrashort pulse laser adopts Ho 3+ Doped gain fiber, ho 3+ A kind of electronic device 5 I 75 I 8 The transition can generate laser with the wavelength of 2.05-2.15 mu m. To achieve high repetition rate output of 2.1 μm wavelength mode-locked laser pulses, a gain fiber with a high absorption coefficient is required. High gain Ho 3+ Doped optical fibers are mainly based on multicomponent glass mechanisms, such as oxide glasses, fluoride glasses, chalcogenide glasses, etc. Currently, the use of multicomponent glass fibers faces a major problem: low loss fusion bonding with passive devices is difficult to achieve. The traditional passive optical fiber devices such as fiber gratings, couplers and the like still use mature quartz optical fibers, the softening temperature of the quartz optical fibers is extremely high, and the thermal expansion coefficient of the quartz optical fibers is extremely low, so that the fusion bonding of the multicomponent glass optical fibers and the quartz optical fibers is extremely difficult. Therefore, a temperature-matched fiber is needed to achieve low-loss fusion of multicomponent glass fiber and quartz fiber.
Disclosure of Invention
The invention discloses a temperature matching optical fiber and a preparation method thereof. The preparation method of the optical fiber comprises the steps of melting fiber core glass and cladding glass, processing a preform rod and drawing the optical fiber.
The technical scheme adopted by the invention is as follows:
1. the composition of the cladding glass is designed so that the glass has a softening temperature, a coefficient of expansion, and a refractive index that are all between those of the silica optical fiber and the multicomponent glass, while the glass has good fiber forming properties and has small absorption at wavelengths of 2.1 μm and 1.0 μm. In combination with the above-mentioned factors,
the cladding glass comprises 69-79% of SiO 2 19-23% of B 2 O 3 1.9-2.3% of GeO 2 1-3% of P 2 O 5 0.1 to 0.3% of Al 2 O 3 0.1 to 0.3% of CaO, 0.1 to 0.3% of MgO, 0.1 to 0.2% of Na 2 O. The corresponding formula is 69-79% of SiO 2 19-23% of B 2 O 3 1.9-2.3% of GeO 2 1-3% of P 2 O 5 0.1 to 0.3% of Al (OH) 3 0.1 to 0.3% of CaO, 0.1 to 0.3% of MgO, 0.1 to 0.2% of Na 2 CO 3
2. The components of the fiber core glass are designed, the softening temperature, the expansion coefficient and the refractive index of the glass are required to be all between those of the quartz optical fiber and the multicomponent glass, the fiber forming performance of the glass is good, the absorption at wavelengths of 2.1 mu m and 1.0 mu m is small, and the refractive index of the fiber core is slightly higher than that of the cladding glass so as to meet the design requirement of numerical aperture. By considering the above factors comprehensively, the fiber core glass comprises 68-78% of SiO 2 3.9-5.9% of B 2 O 3 14.5-24.5% GeO 2 1-3% of P 2 O 5 0.1 to 0.3% of Al 2 O 3 0.2 to 0.4% of CaO, 0.2 to 0.4% of MgO, 0.1 to 0.2% of Na 2 O. Corresponding formula of 68-78% SiO 2 3.9-5.9% of B 2 O 3 14.5-24.5% GeO 2 1-3% of P 2 O 5 0.1 to 0.3% of Al (OH) 3 0.2 to 0.4% of CaO, 0.2 to 0.4% of MgO, 0.1 to 0.2% of Na 2 CO 3
3. For fiber core and cladding sizing, matching with silica fibers and multicomponent fibers is contemplated. The fiber core diameter of the optical fiber is 10+/-2 mu m, and the cladding diameter is 125+/-10 mu m.
4. For the design of the material and structure of the optical fiber coating layer, the easy stripping property of the coating is considered, and the mechanical strength and the bending resistance of the optical fiber can be ensured. The optical fiber coating adopts an acrylic resin material, the structure is a double-layer coating structure, the diameter of the inner coating is 185+/-20 mu m, and the diameter of the outer coating is 245+/-10 mu m.
Compared with the prior art, the invention has the beneficial effects that:
1. unlike MCVD process to prepare fiber component singly, the present invention prepares cladding glass and fiber core glass separately with glass melting process, and has diversified glass components and flexible design.
2. The invention fully considers the easy stripping property of the coating, ensures the mechanical strength and the bending resistance of the optical fiber by the coating design, and has high practical value.
Drawings
FIG. 1 is a schematic cross-sectional view of a temperature matched fiber.
FIG. 2 shows the positions of the temperature-matched fiber and the silica fiber after fusion-splicing.
In the figure, a fiber core-1, a cladding-2, an inner coating-3, an outer coating-4, a quartz fiber-5, a temperature matching fiber-6 and a multicomponent fiber-7
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The cross section of the temperature matching optical fiber is shown in fig. 1, and the structure sequentially comprises a fiber core, a cladding, an inner coating and an outer coating from the center to the outside.
The specific manufacturing process of the temperature matching optical fiber comprises the following steps:
1. the fiber core and cladding glass are prepared respectively by adopting a glass melting method, and the preparation process comprises the steps of batching, feeding, melting, casting and annealing.
2. And manufacturing a rod-tube method preform, respectively processing the fiber core glass into rod shapes, processing the cladding glass into sleeve shapes, and combining the fiber core glass and the cladding glass into the optical fiber preform.
3. And drawing the preform rod, wherein a double-layer coating process is adopted in the drawing process.
The invention is further illustrated by the following examples.
Embodiment one:
1. glass melting was performed using the five formulations in table 1.
Table 1 five sets of glass formulations in the examples
2. The feeding temperature is 1480-1500 ℃ during melting, the melting temperature of the raw materials is 1500-1600 ℃, stirring is carried out for 1 st time 1.5 hours after the raw materials are completely added, then stirring is carried out for 3 times every 1 hour, heat preservation and clarification are carried out for 1 hour after stirring for 3 times, and then the furnace temperature is reduced to 1450 ℃ within 20 minutes.
3. And (3) placing the cast iron mold for pouring into a muffle furnace, raising the temperature of the muffle furnace to 500 ℃, preserving heat, opening a furnace door of the muffle furnace when the temperature of the molybdenum rod furnace is reduced to 1450 ℃, taking out the preheated mold, placing the mold on a stainless steel platform, discharging the glass material, and pouring the glass material into the mold.
4. Naturally cooling the poured molten glass in a mould, when the molten glass is judged to be cooled to be non-flowing, putting the glass and the mould into an annealing furnace together, and closing the electric self-cooling after the heat preservation time is 3 hours at the annealing temperature of 670+/-20 ℃.
5. The five glasses were tested for expansion coefficient, softening point and refractive index and the results are shown in table 2.
Table 2 five sets of glass performance tests
6. Processing the No. 2 glass as fiber core glass into a cylinder with the diameter of 1.37+/-0.01 mm; processing 4# glass as cladding glass into a sleeve with phi (18+/-0.1) mm and inner diameter phi of 1.39+/-0.01 mm; and placing the fiber core glass into cladding glass to form the rod-tube method preform.
7. And drawing the preform rod at 1400+/-10 ℃ and 20+/-5 m/min.
8. The fiber forming performance of the optical fiber is good, the screening tension can reach 0.5%, the minimum bending radius is less than or equal to 20cm, the fiber loss @2.1 mu m is 0.55dB/m, the optical fiber can be welded with a quartz optical fiber and a multi-component optical fiber through a test, and the optical fiber has practical value and temperature matching optical fibers, the quartz optical fiber and a plurality of groups.

Claims (8)

1. A temperature matching optical fiber is characterized in that the optical fiber structure comprises a fiber core, a cladding, an inner coating and an outer coating from the center to the outside in sequence; the fiber core and the cladding are multicomponent glass, and the fiber core comprises 68-78% of SiO by mass percent 2 3.9 to 5.9 percent of B 2 O 3 14.5 to 24.5 percent of GeO 2 1 to 3 percent of P 2 O 5 0.1 to 0.3 percent of Al 2 O 3 0.2 to 0.4 percent of CaO, 0.2 to 0.4 percent of MgO and 0.1 to 0.2 percent of Na 2 O; the cladding component comprises 69-79% of SiO by mass percent 2 19 to 23 percent of B 2 O 3 1.9 to 2.3 percent of GeO 2 1 to 3 percent of P 2 O 5 0.1 to 0.3 percent of Al 2 O 3 0.1 to 0.3 percent of CaO, 0.1 to 0.3 percent of MgO and 0.1 to 0.2 percent of Na 2 O; the inner coating and the outer coating are both acrylic resin materials.
2. A temperature-matched fiber according to claim 1, wherein the core diameter is 10±2 μm, the cladding diameter is 125±10 μm, the inner coating diameter is 185±20 μm, and the outer coating diameter is 245±10 μm.
3. A temperature-matched optical fiber according to claim 1, wherein the core glass has a softening temperature of 900 to 1300 ℃ and an expansion coefficient of (5 to 20) ×10 -7 and/K, the refractive index is 1.465+ -0.010.
4. The temperature-matched optical fiber according to claim 1, wherein the cladding glass has a softening temperature of 900 to 1300 ℃ and an expansion coefficient of (5 to 20). Times.10 -7 The refractive index is 1.457+ -0.010.
5. The preparation method of the temperature matching optical fiber is characterized by comprising the following steps:
1) Preparing fiber core glass and cladding glass respectively, wherein the preparation process comprises the steps of proportioning, charging, melting, pouring and annealing; the formula of the fiber core glass comprises 68-78% of SiO by mass percent 2 3.9 to 5.9 percent of B 2 O 3 14.5 to 24.5 percent of GeO 2 1 to 3 percent of P 2 O 5 0.1 to 0.3 percent of Al (OH) 3 0.2 to 0.4 percent of CaO, 0.2 to 0.4 percent of MgO and 0.1 to 0.2 percent of Na 2 CO 3 The method comprises the steps of carrying out a first treatment on the surface of the The formula of the cladding glass comprises 69-79% of SiO by mass percent 2 19 to 23 percent of B 2 O 3 1.9 to 2.3 percent of GeO 2 1 to 3 percent of P 2 O 5 0.1 to 0.3 percent of Al (OH) 3 0.1 to 0.3 percent of CaO, 0.1 to 0.3 percent of MgO and 0.1 to 0.2 percent of Na 2 CO 3;
2) Processing the fiber core glass into rod type, processing the cladding glass into sleeve type, and combining the fiber core glass and the cladding glass into an optical fiber preform;
3) And drawing the preform rod, wherein a double-layer coating process is adopted in the drawing process.
6. The method of manufacturing a temperature-matched optical fiber according to claim 5, wherein the feeding temperature is 1300-1500 ℃ and the melting temperature is 1400-1600 ℃ when the core glass and the cladding glass are melted.
7. The method of manufacturing a temperature-matched fiber according to claim 5, wherein the annealing temperature of the core glass and the cladding glass is 500-800 ℃.
8. The method of manufacturing a temperature-matched fiber according to claim 5, wherein the drawing temperature is 1200 to 1600 ℃.
CN202011463395.0A 2020-12-15 2020-12-15 Temperature matching optical fiber and preparation method thereof Active CN114634313B (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4264131A (en) * 1978-05-16 1981-04-28 Tokyo Shibaura Denki Kabushiki Kaisha Optical fiber of high durability prepared from multicomponent glass
US4289516A (en) * 1979-10-04 1981-09-15 Eotec Corporation Low loss optical fibers
JPS56160341A (en) * 1980-05-16 1981-12-10 Nippon Telegr & Teleph Corp <Ntt> Optical fiber
US4339173A (en) * 1975-09-08 1982-07-13 Corning Glass Works Optical waveguide containing P2 O5 and GeO2
US4666247A (en) * 1985-02-08 1987-05-19 American Telephone And Telegraph Company, At&T Bell Laboratories Multiconstituent optical fiber
CN108046610A (en) * 2017-11-29 2018-05-18 中国科学院西安光学精密机械研究所 A kind of low softening temperature welding optic fibre and preparation method thereof
CN109399946A (en) * 2018-11-20 2019-03-01 广州宏晟光电科技股份有限公司 Mechanical formation processes are melted in a kind of fibre cladding glass and its tank furnace

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4339173A (en) * 1975-09-08 1982-07-13 Corning Glass Works Optical waveguide containing P2 O5 and GeO2
US4264131A (en) * 1978-05-16 1981-04-28 Tokyo Shibaura Denki Kabushiki Kaisha Optical fiber of high durability prepared from multicomponent glass
US4289516A (en) * 1979-10-04 1981-09-15 Eotec Corporation Low loss optical fibers
JPS56160341A (en) * 1980-05-16 1981-12-10 Nippon Telegr & Teleph Corp <Ntt> Optical fiber
US4666247A (en) * 1985-02-08 1987-05-19 American Telephone And Telegraph Company, At&T Bell Laboratories Multiconstituent optical fiber
CN108046610A (en) * 2017-11-29 2018-05-18 中国科学院西安光学精密机械研究所 A kind of low softening temperature welding optic fibre and preparation method thereof
CN109399946A (en) * 2018-11-20 2019-03-01 广州宏晟光电科技股份有限公司 Mechanical formation processes are melted in a kind of fibre cladding glass and its tank furnace

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