WO2022050257A1 - 光ファイバ及び光ファイバの製造方法 - Google Patents

光ファイバ及び光ファイバの製造方法 Download PDF

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Publication number
WO2022050257A1
WO2022050257A1 PCT/JP2021/031878 JP2021031878W WO2022050257A1 WO 2022050257 A1 WO2022050257 A1 WO 2022050257A1 JP 2021031878 W JP2021031878 W JP 2021031878W WO 2022050257 A1 WO2022050257 A1 WO 2022050257A1
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Prior art keywords
resin layer
acrylate
resin composition
meth
optical fiber
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PCT/JP2021/031878
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English (en)
French (fr)
Japanese (ja)
Inventor
卓弘 野村
一之 相馬
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Sumitomo Electric Industries Ltd
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Sumitomo Electric Industries Ltd
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Priority to JP2022546331A priority Critical patent/JP7771962B2/ja
Priority to US17/789,287 priority patent/US12111494B2/en
Priority to CN202180006832.2A priority patent/CN114761853B/zh
Publication of WO2022050257A1 publication Critical patent/WO2022050257A1/ja
Anticipated expiration legal-status Critical
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    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
    • G02B6/122—Basic optical elements, e.g. light-guiding paths
    • G02B6/1221—Basic optical elements, e.g. light-guiding paths made from organic materials
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02—Optical fibres with cladding with or without a coating
    • G02B6/02395—Glass optical fibre with a protective coating, e.g. two layer polymer coating deposited directly on a silica cladding surface during fibre manufacture
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/46—Polymerisation initiated by wave energy or particle radiation
    • C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
    • C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
    • C08F20/02—Monocarboxylic acids having less than ten carbon atoms, Derivatives thereof
    • C08F20/10—Esters
    • C08F20/26—Esters containing oxygen in addition to the carboxy oxygen
    • C08F20/30—Esters containing oxygen in addition to the carboxy oxygen containing aromatic rings in the alcohol moiety

Definitions

  • the present disclosure relates to an optical fiber and a method for manufacturing an optical fiber.
  • This application claims priority based on Japanese Application No. 2020-148903 filed on September 4, 2020, and incorporates all the contents described in the Japanese application.
  • the optical fiber is provided with a coating resin layer for protecting the glass fiber which is an optical transmitter.
  • the coating resin layer is composed of, for example, two layers, a primary resin layer in contact with the glass fiber and a secondary resin layer formed on the outer layer of the primary resin layer.
  • Patent Document 1 discloses that the removability of the coated resin layer is adjusted by paying attention to the adhesion angle of the mineral oil with respect to the primary resin layer and the elastic modulus of the secondary resin layer.
  • the optical fiber according to one aspect of the present disclosure includes a glass fiber including a core and a clad, and a coated resin layer that is in contact with the glass fiber and coats the glass fiber, and the coated resin layer is in contact with the glass fiber and the glass.
  • a first resin composition having a primary resin layer covering a fiber and a secondary resin layer covering a primary resin layer, wherein the primary resin layer contains a photopolymerizable compound and a phosphine oxide-based photopolymerization initiator.
  • the secondary resin layer contains the cured product of the second resin composition containing the photopolymerizable compound and the phosphine oxide-based photopolymerization initiator, and the unreacted phosphin oxide-based material in the coated resin layer.
  • the amount of the photopolymerization initiator is 0.5% by mass or less.
  • FIG. 1 is a schematic cross-sectional view showing an example of an optical fiber according to the present embodiment.
  • the optical fiber according to one aspect of the present disclosure includes a glass fiber including a core and a clad, and a coated resin layer that is in contact with the glass fiber and coats the glass fiber.
  • the coated resin layer has a primary resin layer that is in contact with the glass fiber and coats the glass fiber, and a secondary resin layer that coats the primary resin layer.
  • the primary resin layer contains a cured product of the first resin composition containing a photopolymerizable compound and a phosphine oxide-based photopolymerization initiator
  • the secondary resin layer contains a photopolymerizable compound and a phosphine oxide-based photopolymerization initiator. It contains a cured product of the second resin composition containing the agent.
  • the amount of the unreacted phosphine oxide-based photopolymerization initiator in the coating resin layer is 0.5% by mass or less.
  • the unreacted photopolymerization initiator contained in the coating resin layer is cleaved and the coating resin layer is cured, and the glass fiber to the coating resin layer is cured. May be difficult to remove.
  • the phosphine oxide-based photopolymerization initiator has high reactivity, it is important to reduce the unreacted amount of the phosphine oxide-based photopolymerization initiator in the coated resin layer.
  • the optical fiber according to the present embodiment can reduce the change over time in the coating removeability.
  • the second resin composition may further contain an acetophenone-based photopolymerization initiator from the viewpoint of improving the surface curability.
  • the first resin composition and the second resin composition may not contain a photopolymerization initiator other than the phosphine oxide-based photopolymerization initiator from the viewpoint of reducing the cost of the resin composition.
  • At least one of the first resin composition or the second resin composition contains nonylphenol polyethylene glycol acrylate as a photopolymerizable compound and is not yet in the coating resin layer.
  • the amount of nonylphenol polyethylene glycol acrylate in the reaction may be less than 1.0% by mass.
  • a first resin composition and a second resin composition are applied to a glass fiber having a temperature of 80 ° C. or lower in this order so as to be far from the glass fiber. It includes a step and a curing step of curing the resin composition by irradiating the resin composition with ultraviolet rays after the coating step.
  • the ultraviolet light emitted by the ultraviolet light emitting diode may be irradiated. This makes it possible to further reduce the unreacted ratio of the phosphine oxide-based photopolymerization initiator.
  • the wavelength of ultraviolet rays may be contained in the region of 350 nm to 405 nm from the viewpoint of curing the coated resin layer to the inside in the curing step.
  • FIG. 1 is a cross-sectional view showing the configuration of an optical fiber according to an embodiment.
  • FIG. 1 shows a cross section perpendicular to the central axis direction (optical axis direction) of the optical fiber 1.
  • the optical fiber 1 of the present embodiment includes a glass fiber 10 which is an optical transmitter and a coated resin layer 20 which is in contact with the glass fiber 10 and covers the glass fiber 10.
  • the glass fiber 10 includes a core 12 and a clad 14 covering the core 12.
  • the glass fiber 10 is a member made of glass, and is made of, for example, silica (SiO 2 ) glass.
  • the glass fiber 10 transmits the light introduced into the optical fiber 1.
  • the core 12 is provided, for example, in a region including the central axis of the glass fiber 10.
  • the core 12 is made of, for example, pure SiO 2 glass or SiO 2 glass containing GeO 2 and / or a fluorine element.
  • the clad 14 is provided in a region surrounding the core 12.
  • the clad 14 has a refractive index lower than that of the core 12.
  • the clad 14 is made of, for example, pure SiO 2 glass or SiO 2 glass to which an element of fluorine is added.
  • the coating resin layer 20 is an ultraviolet curable resin layer that covers the clad 14.
  • the coating resin layer 20 includes a primary resin layer 22 that covers the outer periphery of the glass fiber 10, and a secondary resin layer 24 that covers the outer periphery of the primary resin layer 22.
  • the primary resin layer 22 is in contact with the outer peripheral surface of the clad 14, and covers the entire clad 14.
  • the secondary resin layer 24 is in contact with the outer peripheral surface of the primary resin layer 22 and covers the entire primary resin layer 22.
  • the thickness of the primary resin layer 22 is, for example, 10 ⁇ m or more and 50 ⁇ m or less.
  • the thickness of the secondary resin layer 24 is, for example, 10 ⁇ m or more and 40 ⁇ m or less.
  • the coated resin layer 20 may further include a colored resin layer that covers the outer periphery of the secondary resin layer 24.
  • the primary resin layer 22 contains a cured product of the first resin composition containing a photopolymerizable compound and a phosphine oxide-based photopolymerization initiator.
  • the secondary resin layer 24 contains a cured product of the second resin composition containing a photopolymerizable compound and a phosphine oxide-based photopolymerization initiator.
  • the amount of the unreacted phosphine oxide-based photopolymerization initiator in the coating resin layer 20 is 0.5% by mass or less. As a result, it is possible to reduce the change over time in the coating removal property of the optical fiber.
  • the amount of the unreacted phosphine oxide-based photopolymerization initiator is preferably 0.49% by mass or less, more preferably 0.48% by mass or less, and further preferably 0.45% by mass or less. preferable.
  • the lower limit of the amount of the unreacted phosphine oxide-based photopolymerization initiator is not particularly limited, and may be 0.01% by mass or more, 0.03% by mass or more, or 0.05% by mass or more.
  • phosphine oxide-based photopolymerization initiator examples include 2,4,6-trimethylbenzoyldiphenylphosphine oxide (Omnirad TPO, manufactured by IGM Resins), bis (2,4,6-trimethylbenzoyl) phenylphosphine oxide (Omnirad 819,). IGM (manufactured by Resins) and bis (2,6-dimethoxybenzoyl) -2,4,4-trimethylpentylphosphine oxide.
  • TPO 2,4,6-trimethylbenzoyldiphenylphosphine oxide
  • IGM manufactured by Resins
  • bis (2,6-dimethoxybenzoyl) -2,4,4-trimethylpentylphosphine oxide examples include 2,4,6-trimethylbenzoyldiphenylphosphine oxide (Omnirad TPO, manufactured by IGM Resins), bis (2,4,6-trimethylbenzoyl) phenylphosphin
  • the first resin composition contains only a phosphine oxide-based photopolymerization initiator as a photopolymerization initiator. From the viewpoint of reducing the cost of the resin composition, the first resin composition and the second resin composition may contain only a phosphine oxide-based photopolymerization initiator as the photopolymerization initiator.
  • the second resin composition may further contain an acetophenone-based photopolymerization initiator from the viewpoint of improving the surface curability.
  • acetophenone-based photopolymerization initiator examples include 1-hydroxycyclohexylphenyl ketone (Omnirad 184, manufactured by IGM Resins), 2,2-dimethoxy-2-phenylacetophenone (Omnirad 651, manufactured by IGM Resins), 1- (4). -Isopropylphenyl) -2-hydroxy-2-methylpropane-1-one, and 2-methyl-1- [4- (methylthio) phenyl] -2-morpholino-propane-1-one (Omnirad 907, IGM Resins) Made).
  • the photopolymerizable compound according to this embodiment may contain an oligomer and a monomer.
  • the oligomer include urethane (meth) acrylate and epoxy (meth) acrylate.
  • the urethane (meth) acrylate may be a compound obtained by reacting a polyol compound, a polyisocyanate compound and a hydroxyl group-containing (meth) acrylate compound.
  • polyol compound examples include polytetramethylene glycol, polypropylene glycol, and bisphenol A / ethylene oxide-added diol.
  • the number average molecular weight (Mn) of the polyol compound may be 300 or more and 8000 or less from the viewpoint of adjusting the Young's modulus of the coated resin layer.
  • the Mn of the polyol compound constituting the urethane (meth) acrylate contained in the first resin composition is 1200 or more and 8000 or less, 2000 or more and 7000 or less, or 3000 or more and 6000 or less from the viewpoint of lowering the Young's modulus of the primary resin layer. May be.
  • the Mn of the polyol compound constituting the urethane (meth) acrylate contained in the second resin composition is 300 or more and less than 1200, 400 or more and 1100 or less, or 500 or more and 1000 or less from the viewpoint of increasing the Young's modulus of the secondary resin layer. May be.
  • polyisocyanate compound examples include 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, isophorone diisocyanate, and dicyclohexylmethane 4,4'-diisocyanate.
  • hydroxyl group-containing (meth) acrylate compound examples include 2-hydroxyethyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 1,6-hexanediol mono (meth) acrylate, and pentaerythritol tri (meth) acrylate. Examples thereof include 2-hydroxypropyl (meth) acrylate and tripropylene glycol (meth) acrylate.
  • An organotin compound is generally used as a catalyst for synthesizing urethane (meth) acrylate.
  • the organotin compound include dibutyltin dilaurate, dibutyltin diacetate, dibutyltinmalate, dibutyltinbis (2-ethylhexyl mercaptoacetate), dibutyltinbis (isooctyl mercaptoacetate), and dibutyltin oxide. From the viewpoint of easy availability or catalytic performance, it is preferable to use dibutyltin dilaurate or dibutyltin diacetate as the catalyst.
  • a lower alcohol having 5 or less carbon atoms may be used when synthesizing urethane (meth) acrylate.
  • the lower alcohol include methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl-2-propanol, 1-pentanol, 2-pentanol and 3-pentanol. Included are 2-methyl-1-butanol, 3-methyl-1-butanol, 2-methyl-2-butanol, 3-methyl-2-butanol, and 2,2-dimethyl-1-propanol.
  • epoxy (meth) acrylate a compound obtained by reacting an epoxy resin having two or more glycidyl groups with a compound having a (meth) acryloyl group can be used.
  • a monofunctional monomer having one polymerizable group and a polyfunctional monomer having two or more polymerizable groups can be used. Two or more kinds of monomers may be mixed and used.
  • Examples of the monofunctional monomer include methyl (meth) acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, n-butyl (meth) acrylate, s-butyl (meth) acrylate, and tert-butyl (meth) acrylate.
  • Carboxyl group-containing monomers such as acrylate, carboxypentyl (meth) acrylate, ⁇ -carboxy-polycaprolactone (meth) acrylate; N-acryloylmorpholin, N-vinylpyrrolidone, N-vinylcaprolactam, N-acryloylpiperidin, N-methacryloyl.
  • Heterocyclic ring-containing (meth) acrylates such as piperidine, N-acryloylpyrrolidine, 3- (3-pyridyl) propyl (meth) acrylate, cyclic trimethylolpropaneformal acrylate; maleimide, N-cyclohexylmaleimide, N-phenylmaleimide, etc.
  • Aminoalkyl (meth) acrylate monomers such as aminopropyl (meth) acrylate, N, N-dimethylaminoethyl (meth) acrylate, tert-butylaminoethyl (meth) acrylate; N- (meth) acryloyl.
  • Examples thereof include succinimide-based monomers such as oxymethylene succinimide, N- (meth) acrylamide-6-oxyhexamethylene succinimide, and N- (meth) acrylamide-8-oxyoctamethylene succinimide.
  • polyfunctional monomer examples include ethylene glycol di (meth) acrylate, polyethylene glycol di (meth) acrylate, polypropylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, and tripropylene glycol di (meth) acrylate.
  • Di (meth) acrylate of alkylene oxide adduct of bisphenol A tetraethylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate of hydroxypivalate, 1,4-butanediol di (meth) acrylate, 1,6 -Hexanediol di (meth) acrylate, 1,9-nonanediol di (meth) acrylate, 1,12-dodecanediol di (meth) acrylate, 1,14-tetradecanediol di (meth) acrylate, 1,16-hexadecane EO addition of diol di (meth) acrylate, 1,20-eicosane diol di (meth) acrylate, isopentyl diol di (meth) acrylate, 3-ethyl-1,8-octane diol di (meth) acrylate, bisphenol A
  • Nonylphenol polyethylene glycol acrylate may be contained as the monofunctional monomer, and it is preferable that the first resin composition contains nonylphenol polyethylene glycol acrylate.
  • the nonylphenol polyethylene glycol acrylate include nonylphenol ethylene oxide-modified (8 mol adduct) acrylate, nonylphenol ethylene oxide modified (1 mol adduct) acrylate, and nonylphenol ethylene oxide modified (4 mol adduct) acrylate.
  • the amount of unreacted nonylphenol polyethylene glycol acrylate in the coating resin layer may be less than 1.0% by mass, and may be 0.95% by mass or less, from the viewpoint of suppressing the change in coating removal property over time. It is more preferably 0.93% by mass or less, and even more preferably 0.90% by mass or less.
  • the lower limit of the amount of unreacted nonylphenol polyethylene glycol acrylate is not particularly limited and may be 0.1% by mass or more, 0.3% by mass or more, or 0.5% by mass or more.
  • the resin composition may further contain a silane coupling agent, a leveling agent, an antifoaming agent, an antioxidant, a sensitizer and the like.
  • the silane coupling agent is not particularly limited as long as it does not interfere with the curing of the resin composition.
  • examples of the silane coupling agent include tetramethyl silicate, tetraethyl silicate, mercaptopropyltrimethoxysilane, vinyltrichlorosilane, vinyltriethoxysilane, vinyltris ( ⁇ -methoxy-ethoxy) silane, and ⁇ - (3,4-epoxycyclohexyl).
  • -Ethyltrimethoxysilane dimethoxydimethylsilane, diethoxydimethylsilane, 3-acryloxypropyltrimethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, ⁇ -glycidoxypropylmethyldiethoxysilane, ⁇ -methacryloxypropyl Trimethoxysilane, N- ( ⁇ -aminoethyl) - ⁇ -aminopropyltrimethoxysilane, N- ( ⁇ -aminoethyl) - ⁇ -aminopropyltrimethyldimethoxysilane, N-phenyl- ⁇ -aminopropyltrimethoxysilane, ⁇ -Chloropropyltrimethoxysilane, ⁇ -mercaptopropyltrimethoxysilane, ⁇ -aminopropyltrimethoxysilane, bis- [3- (triethoxysilyl) prop
  • the method for manufacturing an optical fiber according to the present embodiment includes a coating step of applying a first resin composition and a second resin composition to the outer periphery of a glass fiber having a temperature of 80 ° C. or lower, and an ultraviolet ray after the coating step. Includes a curing step of curing the resin composition by irradiating with.
  • the first resin composition is applied to the surface of the glass fiber 10 and the first resin layer (the layer corresponding to the cured primary resin layer 22) made of the first resin composition is applied to the glass fiber 10.
  • a second resin layer made of the second resin composition by applying the second resin composition to the surface of the first resin layer (a layer corresponding to the cured secondary resin layer 24). Is formed on the surface of the first resin layer. That is, in the coating step, the first resin composition and the second resin composition are applied to the glass fiber 10 having a temperature of 80 ° C. or lower so as to be far from the glass fiber 10 in this order.
  • the temperature of the glass fiber is preferably 75 ° C. or lower, more preferably 70 ° C. or lower.
  • the lower limit of the temperature of the glass fiber is not particularly limited, and may be 30 ° C. or higher, 40 ° C. or higher, or 45 ° C. or higher.
  • the first resin layer and the second resin layer are cured by ultraviolet irradiation to form the primary resin layer 22 from the first resin layer and the secondary resin layer 24 from the second resin layer. do.
  • the ultraviolet light source examples include an ultraviolet LED and an ultraviolet lamp.
  • the wavelength of the ultraviolet light emitted from the ultraviolet LED is, for example, in the region of 300 nm to 450 nm, and the wavelength region of the ultraviolet light emitted from the ultraviolet lamp is, for example, 200 nm to 450 nm. Since it has high illuminance and can reduce power consumption, it is preferable to use an ultraviolet LED, and it is more preferable to use an ultraviolet LED containing an ultraviolet wavelength in the region of 350 nm to 405 nm.
  • the irradiation time of ultraviolet rays by the ultraviolet LED is, for example, 4 ⁇ 10 -3 seconds or more and 1 second or less.
  • the ultraviolet rays are irradiated in an inert gas atmosphere such as a nitrogen atmosphere.
  • urethane acrylate a 9 parts by mass of nonylphenol polyethylene glycol acrylate (trade name "SR504" manufactured by Sartomer), 7 parts by mass of N-vinylcaprolactam, 5 parts by mass of 1,6-hexanediol diacrylate, and
  • a resin composition P1 was prepared by mixing 1 part by mass of 2,4,6-trimethylbenzoyldiphenylphosphine oxide (Omnirad TPO).
  • the resin composition S2 was prepared by mixing 29 parts by mass of urethane acrylate b, 30 parts by mass of TPGDA, 40 parts by mass of PO-A, and 1 part by mass of TPO.
  • Example 1 In the coating step, a first resin layer having a thickness of 32.5 ⁇ m is formed on the outer periphery of a glass fiber having a diameter of 125 ⁇ m at a temperature of 80 ° C. using the resin composition P1, and the resin composition S1 is further formed on the outer periphery thereof. It was used to form a second resin layer with a thickness of 27.5 ⁇ m.
  • the irradiation amount is 29 mW / cm 2 seconds.
  • Example 2-5 and Comparative Example 1-2 An optical fiber was produced in the same manner as in Example 1 except that the temperature of the glass fiber and the irradiation conditions of ultraviolet rays were changed to the values shown in Table 1.
  • a first resin layer having a thickness of 32.5 ⁇ m is formed on the outer periphery of a glass fiber having a diameter of 125 ⁇ m at a temperature of 60 ° C. using the resin composition P1, and the resin composition S2 is further formed on the outer periphery thereof. It was used to form a second resin layer with a thickness of 27.5 ⁇ m.
  • the first layer and the second layer are cured by irradiating ultraviolet rays having an emission wavelength of 385 nm with an irradiation amount of 21 mW / cm 2 ⁇ sec using an ultraviolet LED to cure the primary resin layer and the secondary resin layer.
  • An optical fiber having a coated resin layer made of the above was produced.
  • Example 7-9 An optical fiber was produced in the same manner as in Example 6 except that the temperature of the glass fiber and the irradiation conditions of ultraviolet rays were changed to the values shown in Table 2.

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  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Optics & Photonics (AREA)
  • General Physics & Mathematics (AREA)
  • Medicinal Chemistry (AREA)
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PCT/JP2021/031878 2020-09-04 2021-08-31 光ファイバ及び光ファイバの製造方法 Ceased WO2022050257A1 (ja)

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JP2022546331A JP7771962B2 (ja) 2020-09-04 2021-08-31 光ファイバ及び光ファイバの製造方法
US17/789,287 US12111494B2 (en) 2020-09-04 2021-08-31 Optical fiber and method for manufacturing optical fiber
CN202180006832.2A CN114761853B (zh) 2020-09-04 2021-08-31 光纤以及光纤的制造方法

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JP2020-148903 2020-09-04

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