CN114578473A - Broadband low-dispersion optical fiber and preparation method thereof - Google Patents
Broadband low-dispersion optical fiber and preparation method thereof Download PDFInfo
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- CN114578473A CN114578473A CN202210172314.4A CN202210172314A CN114578473A CN 114578473 A CN114578473 A CN 114578473A CN 202210172314 A CN202210172314 A CN 202210172314A CN 114578473 A CN114578473 A CN 114578473A
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 96
- 239000006185 dispersion Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000919 ceramic Substances 0.000 claims abstract description 62
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000005137 deposition process Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- 238000012986 modification Methods 0.000 claims abstract description 13
- 230000004048 modification Effects 0.000 claims abstract description 13
- BCKOQWWRTRBSGR-UHFFFAOYSA-N octane-3,6-diol Chemical compound CCC(O)CCC(O)CC BCKOQWWRTRBSGR-UHFFFAOYSA-N 0.000 claims abstract description 13
- IOCLFIGHHOKNTE-UHFFFAOYSA-N 2,2,6,6-tetramethyl-n-(2,2,6,6-tetramethylpiperidin-4-yl)piperidin-4-amine Chemical compound C1C(C)(C)NC(C)(C)CC1NC1CC(C)(C)NC(C)(C)C1 IOCLFIGHHOKNTE-UHFFFAOYSA-N 0.000 claims abstract description 12
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 33
- 229910052582 BN Inorganic materials 0.000 claims description 29
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 29
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- DZPJVKXUWVWEAD-UHFFFAOYSA-N [C].[N].[Si] Chemical compound [C].[N].[Si] DZPJVKXUWVWEAD-UHFFFAOYSA-N 0.000 claims description 23
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 238000004528 spin coating Methods 0.000 claims description 12
- 239000012300 argon atmosphere Substances 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 10
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 9
- 230000005684 electric field Effects 0.000 claims description 9
- 239000005304 optical glass Substances 0.000 claims description 8
- 230000001678 irradiating effect Effects 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 7
- 229920000742 Cotton Polymers 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- 239000003599 detergent Substances 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 238000004544 sputter deposition Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000004050 hot filament vapor deposition Methods 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 238000002294 plasma sputter deposition Methods 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 239000011162 core material Substances 0.000 abstract description 86
- 239000010410 layer Substances 0.000 abstract description 52
- 230000032683 aging Effects 0.000 abstract description 12
- 239000011229 interlayer Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 4
- 230000003111 delayed effect Effects 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 238000009987 spinning Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 17
- 239000013077 target material Substances 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 4
- 229920006389 polyphenyl polymer Polymers 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- -1 polyethylene Polymers 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
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- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002829 nitrogen Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005491 wire drawing Methods 0.000 description 1
Classifications
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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
- G02B6/02—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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0647—Boron nitride
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges
- C23C16/511—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges using microwave discharges
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
Abstract
The invention discloses a broadband low-dispersion optical fiber and a preparation method thereof, and relates to the technical field of optical fibers. The invention uses low dispersion glass as a core material, and sequentially carries out a first deposition process, a second deposition process and a sintering process to form a uniform and compact interlayer ceramic layer on the surface of the core material, thereby effectively widening the frequency band of the optical fiber, simultaneously, the interlayer structure enables the reflection generated by the optical fiber to be mutually offset in a certain frequency band range, and being beneficial to improving the broadband performance of the optical fiber; after the ceramic layer is pretreated, a carbon quantum dot solution is coated on the surface in a spinning mode, and then 3, 6-octanediol, tert-butyl acrylate and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine are used for modification treatment to form an ultraviolet shielding film, so that the light aging phenomenon of the optical fiber is effectively delayed, the service life of the optical fiber is prolonged, meanwhile, the optical fiber can be stably regenerated, and the light aging resistance of the optical fiber is effectively improved. The optical fiber prepared by the invention has the effects of broadband and light aging resistance.
Description
Technical Field
The invention relates to the technical field of optical fibers, in particular to a broadband low-dispersion optical fiber and a preparation method thereof.
Background
The optical fiber communication is a technical basis of the information society, the significance of developing a new optical fiber communication technology is great, in order to meet the social demand, the low-dispersion optical fiber gradually enters the visual field of people, and the advantages of high gain, good noise performance, high output power and the like are well favored by people; however, because of the limited electrical conductivity of metal and the high absorption coefficient of dielectric, conventional low-dispersion optical fiber cannot be used for long-distance transmission of a wide range of wavelengths, and thus has a limitation in use.
In order to protect the normal use of the optical fiber and prevent the damage of the core of the optical fiber, polyethylene is currently used as a sheathing material. Polyethylene has the advantages of light weight, high bending strength, small friction coefficient and the like, but the pipe has the defects of poor light aging resistance, breakage, crosslinking and degradation of polyethylene molecular chains under long-term ultraviolet irradiation, short service life, frequent need of later maintenance, greatly increased cost and unnecessary waste.
Disclosure of Invention
The invention aims to provide a broadband low-dispersion optical fiber and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the broadband low-dispersion optical fiber is characterized by comprising a wire core, a ceramic layer and an ultraviolet shielding film in sequence from inside to outside; the wire core is low dispersion optical glass.
Further, the ceramic layer is prepared through the steps of a first deposition process, a second deposition process, a sintering process and the like in sequence.
Further, the first deposition process comprises: by utilizing hot wire chemical vapor deposition and with the help of microwave discharge, rapidly depositing a silicon-carbon-nitrogen film on the surface of the wire core to prepare a silicon-carbon-nitrogen film wire core; the second deposition process comprises the following steps: and depositing the boron nitride film by using a direct current electric field-plasma auxiliary pulse laser to prepare the boron nitride film wire core.
Further, the ultraviolet shielding film is prepared by a method that after a ceramic layer is pretreated, a carbon quantum dot solution is coated on the surface in a spinning mode, and the ceramic layer is modified by using 3, 6-octanediol, tert-butyl acrylate and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine.
Further, a preparation method of the broadband low-dispersion optical fiber comprises the following preparation steps:
(1) the first deposition process: polishing low-dispersion optical glass to obtain a wire core with the diameter of 5-15 mm, ultrasonically cleaning the wire core with acetone at 25-35 kHz for 18-30 min, placing the wire core in a microwave discharge system, vacuumizing to 0.02-0.1 Pa, introducing silane, methane, hydrogen and nitrogen according to the flow ratio of 1:1:10: 12-1: 1:15:18 until the air pressure is 20-40 MPa, heating to 400-600 ℃, and depositing for 22-41 min to obtain a silicon-carbon-nitrogen film wire core;
(2) and (3) a second deposition process: placing the silicon-carbon-nitrogen film wire core in plasma equipment, vacuumizing to 20-40 Pa, pre-sputtering for 10-13 min in an argon atmosphere, placing in laser equipment, connecting the laser equipment with a direct current electric field, and vacuumizing to 10 DEG-6～10-4In the atmosphere of Pa and argon, depositing for 15-22 min by using hexagonal boron nitride as a target to obtain a boron nitride film wire core;
(3) the sintering process comprises the following steps: placing the boron nitride film wire core in a container, heating to 400-650 ℃ at a speed of 10-20 ℃/min under the nitrogen atmosphere and a pressure of 10-50 MPa, preserving heat for 25-40 min, heating to 800-1000 ℃ at a speed of 1-10 ℃/min, and then drawing wires to obtain a wire core containing a ceramic layer;
(4) modification treatment: pretreating a ceramic layer-containing wire core, spin-coating a carbon quantum dot solution at 2000-2500 rmp/min, wherein the mass ratio of carbon quantum dots to methylbenzene in the carbon quantum dot solution is 1: 8-1: 12, after spin-coating for 40-60 s, drying at 70-80 ℃ for 1-2 h, soaking in absolute ethyl alcohol which is 10-15 times of the mass of the ceramic layer-containing wire core, adding 3, 6-octanediol which is 0.1-0.3 times of the mass of the ceramic layer-containing wire core, ultrasonically mixing at 30-40 kHz for 10-20 min, placing in a para-polystyrene lining hydrothermal reaction kettle, heating to 170-180 ℃, preserving heat for 1-2 h, and cooling to room temperature to obtain a modified optical fiber;
(5) and (3) secondary modification treatment: placing the modified optical fiber into a container, adding tert-butyl acrylate accounting for 0.8-1.2 times of the mass of the modified optical fiber and tetraisopropyl titanate accounting for 0.001-0.006 times of the mass of the modified optical fiber, heating to 170-180 ℃ under the protection of nitrogen, reacting for 8-10 hours, and washing with deionized water for 3-6 times; and then adding methanol which is 0.6-1.1 times of the mass of the modified optical fiber and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine which is 1.3-1.7 times of the mass of the modified optical fiber, uniformly stirring, heating to 40-50 ℃, reacting for 10-12 h, distilling at 50-60 ℃ for 1-3 h under 0.1-0.3 MPa, cooling to room temperature, and drying for 2-4 h at 70-80 ℃ to obtain the broadband low-dispersion optical fiber.
Further, the frequency of the microwave discharge system in the step (1) is 2400-2500 MHz, and the power is 100-200W.
Further, the plasma sputtering power in the step (2) is 100-150W.
Further, the laser device of step (2): the distance between the target and the substrate is 5-10 cm, and the laser density is 12-25J/cm2The laser wavelength is 532nm, and the voltage of the direct current electric field is 200-400V.
Further, the wire drawing speed in the step (3) is 1-4 mm/min; the diameter of the wire core of the ceramic-containing layer is 115-125 mu m.
Further, the pretreatment of the step (4): cleaning the ceramic layer-containing wire core for 3-6 times by using detergent and absorbent cotton, then carrying out ultrasonic treatment for 7-14 min at 25-30 kHz by using deionized water, acetone, isopropanol and absolute ethyl alcohol in sequence, drying for 30-45 min in vacuum at 60-80 ℃ and 0.01-0.03 MPa, placing in a container, introducing ozone at the rate of 30-40 mL/min, introducing for 20-30 min, irradiating 10-20 mm above the ceramic layer-containing wire core by using an ultraviolet lamp with the power of 5-10W and the wavelength of 253.7nm, and treating for 15-20 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention prepares the optical fiber through the steps of a first deposition process, a second deposition process, a discharge plasma sintering process, modification treatment and the like in sequence so as to realize the functions of light aging resistance and broadband.
Firstly, the method uses low dispersion glass as a core material, firstly carries out a first deposition process, uses hot filament chemical vapor deposition, generates non-magnetized high activated nitrogen reaction with the help of microwave discharge, and quickly deposits a silicon carbon nitrogen film on the surface of the low dispersion glass; then, carrying out a second deposition process, and depositing a boron nitride film by using a direct current electric field-plasma auxiliary pulse laser; under the action of an electric field, a large number of charged particles are generated on the surface of the boron nitride, and because the plasma provides an active gas environment, the charged particles react in the active environment, so that the surface has abundant active groups and is easy to deposit on the surface of the silicon carbon nitrogen film; and finally, sintering to ensure that boron nitride and silicon carbon nitrogen are fused and bonded to form a densified interlayer ceramic layer, wherein the silicon carbon nitrogen film and the boron nitride film have low dielectric constant and dielectric loss, the frequency band of the optical fiber is widened under the combined action, and simultaneously, the interlayer structure of the ceramic layer enables the reflection generated by the optical fiber to be mutually offset in a certain frequency band range, so that the broadband performance of the optical fiber is improved.
Secondly, after the ceramic layer is pretreated, the surface is coated with carbon quantum dot solution in a spinning mode to form an ultraviolet shielding film preliminarily, then modification treatment is carried out, hydroxyl of 3, 6-octanediol reacts with oxygen-containing groups on the surface of the carbon quantum dot to be grafted on the surface of the carbon quantum dot, the residual hydroxyl of the 3, 6-octanediol reacts with ester groups of tert-butyl acrylate, double bonds of the tert-butyl acrylate react with imino groups of bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine, so that a light stabilizing film is formed on the carbon quantum dot film, the absorption of ultraviolet rays by the optical fiber is further reduced, the light aging phenomenon of the optical fiber is effectively delayed, the service life of the optical fiber is prolonged, and in addition, a larger conjugated system formed by the 3, 6-octanediol, the tert-butyl acrylate and the bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine, the ultraviolet shielding film on the surface of the optical fiber is promoted to regenerate and stably exist, and the light aging resistance of the optical fiber is effectively improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
To more clearly illustrate the method of the present invention, the following examples are given, and the test methods for each index of the optical fiber manufactured in the following examples are as follows:
broadband: taking optical fibers with the same length to perform a broadband effect test, measuring the optical power of the tail end and the initial end of the optical fiber by using an optical power meter under the frequency of 0.2-2.0 GHz, calculating an absorption loss value, and taking the average value of the absorption loss values; the absorption loss value is initial end optical power-end optical power.
Light aging resistance: taking the optical fibers with the same length to carry out a light aging resistant effect test, irradiating the optical fibers at a distance of 3cm below an ultraviolet lamp for aging for 20 hours at room temperature, measuring by using a spectrum loss tester, and calculating the loss change rate; the loss change rate (loss after aging-loss of aged label)/loss before aging × 100%.
Example 1
A method for preparing a broadband low-dispersion optical fiber, which comprises the following preparation steps:
(1) the first deposition process: polishing low-dispersion optical glass to obtain a wire core with the diameter of 5mm, ultrasonically cleaning the wire core with acetone at 25kHz for 30min, placing the wire core in a microwave discharge system with the frequency of 2400MHz and the power of 100W, vacuumizing to 0.02Pa, introducing silane, methane, hydrogen and nitrogen according to the flow ratio of 1:1:10:12 until the pressure is 20MPa, heating to 400 ℃, and depositing for 41min to obtain a silicon-carbon-nitrogen film wire core;
(2) and (3) a second deposition process: placing the silicon-carbon-nitrogen film wire core in a plasma device with the power of 100W, vacuumizing to 20Pa, pre-sputtering for 10min in an argon atmosphere, placing in a laser device, connecting the laser device with a 200V direct current electric field, and vacuumizing to 10-6Pa, under the argon atmosphere, adopting hexagonal boron nitride as a target material, wherein the distance between the target material and the substrate is 5cm, and the laser density is 12J/cm2The laser wavelength is 532nm, and the boron nitride film is obtained by depositing for 22minA film wire core;
(3) the sintering process comprises the following steps: placing the boron nitride film wire core in a container, heating to 400 ℃ at a speed of 10 ℃/min under the nitrogen atmosphere and 10MPa, preserving heat for 40min, heating to 800 ℃ at a speed of 1 ℃/min, and drawing at a speed of 1mm/min to obtain a ceramic layer-containing wire core with the diameter of 115 mu m;
(4) modification treatment: cleaning a ceramic layer-containing wire core for 3 times by using detergent and absorbent cotton, then carrying out ultrasonic treatment for 14min at 25kHz by using deionized water, acetone, isopropanol and absolute ethyl alcohol in sequence, drying for 30min at 60 ℃ under 0.01MPa in vacuum, placing the ceramic layer-containing wire core in a container, introducing ozone at a rate of 30mL/min, introducing ozone for 30min, irradiating the ceramic layer-containing wire core 10mm above the ceramic layer-containing wire core by using an ultraviolet lamp with a power of 5W and a wavelength of 253.7nm, treating for 20min, spin-coating a carbon quantum dot solution at 2000rmp/min, wherein the mass ratio of carbon quantum dots to toluene in the carbon quantum dot solution is 1:8, drying for 60s at 70 ℃, soaking the ceramic layer-containing wire core in absolute ethyl alcohol 10 times of the mass of the ceramic layer-containing wire core, adding 3, 6-octanediol 0.1 time of the mass of the ceramic layer-containing wire core, carrying out ultrasonic mixing for 20min at 30kHz, placing the ceramic layer-containing wire core in a para-polyphenyl lining hydrothermal reaction kettle, heating to 170 ℃, keeping the temperature for 2h, cooling to room temperature to obtain the modified optical fiber;
(5) and (3) secondary modification treatment: placing the modified optical fiber into a container, adding tert-butyl acrylate with the mass 0.8 time of that of the modified optical fiber and tetraisopropyl titanate with the mass 0.001 time of that of the modified optical fiber, heating to 170 ℃ under the protection of nitrogen, reacting for 10h, and washing for 3 times by using deionized water; and then adding methanol which is 0.6 time of the mass of the modified optical fiber and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine which is 1.3 times of the mass of the modified optical fiber, uniformly stirring, heating to 40 ℃, reacting for 12h, distilling for 3h at 50 ℃ under 0.1MPa, cooling to room temperature, and drying for 4h at 70 ℃ to obtain the broadband low-dispersion optical fiber.
Example 2
A method for preparing a broadband low-dispersion optical fiber, comprising the following steps:
(1) the first deposition process comprises the following steps: polishing low-dispersion optical glass to obtain a wire core with the diameter of 15mm, ultrasonically cleaning the wire core with acetone at 35kHz for 18min, placing the wire core in a microwave discharge system with the frequency of 2500MHz and the power of 200W, vacuumizing to 0.1Pa, introducing silane, methane, hydrogen and nitrogen according to the flow ratio of 1:1:15:18 until the pressure is 40MPa, heating to 600 ℃, and depositing for 22min to obtain a silicon-carbon-nitrogen film wire core;
(2) and (3) a second deposition process: placing the silicon-carbon-nitrogen film wire core in plasma equipment with power of 150W, vacuumizing to 40Pa, pre-sputtering for 13min in argon atmosphere, placing in laser equipment, connecting the laser equipment with a 400V direct current electric field, and vacuumizing to 10 DEG-4Pa, under the argon atmosphere, adopting hexagonal boron nitride as a target material, wherein the distance between the target material and the substrate is 10cm, and the laser density is 25J/cm2Depositing for 15min to obtain a boron nitride film wire core, wherein the laser wavelength is 532 nm;
(3) the sintering process comprises the following steps: placing the boron nitride film wire core in a container, heating to 650 ℃ at a speed of 20 ℃/min under the nitrogen atmosphere and a pressure of 50MPa, preserving heat for 25min, heating to 1000 ℃ at a speed of 10 ℃/min, and drawing at a speed of 4mm/min to obtain a ceramic layer-containing wire core with a diameter of 125 mu m;
(4) modification treatment: cleaning a ceramic layer-containing wire core for 6 times by using detergent and absorbent cotton, then ultrasonically treating the ceramic layer-containing wire core for 7min at 30kHz by using deionized water, acetone, isopropanol and absolute ethyl alcohol in sequence, drying the ceramic layer-containing wire core for 45min at 80 ℃ under 0.03MPa in vacuum, placing the ceramic layer-containing wire core in a container, introducing ozone at a rate of 40mL/min, introducing ozone for 20min, irradiating the ceramic layer-containing wire core 20mm above the ceramic layer-containing wire core by using an ultraviolet lamp with the power of 10W and the wavelength of 253.7nm, treating the ceramic layer-containing wire core for 15min, spin-coating a carbon quantum dot solution at a rate of 2500rmp/min, wherein the mass ratio of carbon quantum dots to toluene in the carbon quantum dot solution is 1:12, after spin-coating for 40s, soaking the ceramic layer-containing wire core in absolute ethyl alcohol 15 times of the mass of the ceramic layer-containing wire core after drying for 1h at 80 ℃, adding 3, 6-octanediol 0.3 times of the ceramic layer-containing wire core mass, ultrasonically mixing for 10min at 40kHz, placing the ceramic layer-containing wire core in a para-polyphenyl lining hydrothermal reaction kettle, heating the kettle to 180 ℃, keeping the temperature for 1h, cooling to room temperature to obtain the modified optical fiber;
(5) and (3) secondary modification treatment: placing the modified optical fiber into a container, adding tert-butyl acrylate with the mass 1.2 times of that of the modified optical fiber and tetraisopropyl titanate with the mass 0.006 time of that of the modified optical fiber, heating to 180 ℃ under the protection of nitrogen, reacting for 8h, and washing for 6 times by using deionized water; then adding methanol which is 1.1 times of the mass of the modified optical fiber and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine which is 1.7 times of the mass of the modified optical fiber, stirring uniformly, heating to 50 ℃, reacting for 10h, distilling for 1h at 0.3MPa and 60 ℃, cooling to room temperature, and drying for 2h at 80 ℃ to obtain the broadband low-dispersion optical fiber.
Example 3
A method for preparing a broadband low-dispersion optical fiber, comprising the following steps:
(1) the first deposition process: polishing low-dispersion optical glass to obtain a wire core with the diameter of 10mm, ultrasonically cleaning the wire core with acetone at 30kHz for 24min, placing the wire core in a microwave discharge system with the frequency of 2450MHz and the power of 150W, vacuumizing to 0.07Pa, introducing monosilane, methane, hydrogen and nitrogen according to the flow ratio of 1:1:13:16, introducing the mixture to the pressure of 30MPa, heating to 540 ℃, and depositing for 31min to obtain a silicon-carbon-nitrogen film wire core;
(2) and (3) a second deposition process: placing the silicon-carbon-nitrogen film wire core in plasma equipment with power of 140W, vacuumizing to 30Pa, pre-sputtering for 12min in argon atmosphere, placing in laser equipment, connecting the laser equipment with a 300V direct current electric field, and vacuumizing to 10-5Pa, under the argon atmosphere, adopting hexagonal boron nitride as a target material, wherein the distance between the target material and the substrate is 7cm, and the laser density is 20J/cm2Depositing for 17min to obtain a boron nitride film wire core with the laser wavelength of 532 nm;
(3) the sintering process comprises the following steps: placing the boron nitride film wire core in a container, heating to 580 ℃ at a speed of 14 ℃/min under the nitrogen atmosphere and a pressure of 30MPa, preserving heat for 33min, heating to 900 ℃ at a speed of 4 ℃/min, and drawing at a speed of 2mm/min to obtain a ceramic layer-containing wire core with a diameter of 120 mu m;
(4) modification treatment: cleaning a ceramic layer-containing wire core with detergent and absorbent cotton for 5 times, then sequentially carrying out ultrasonic treatment for 12min at 28kHz with deionized water, acetone, isopropanol and absolute ethyl alcohol, drying for 39min at 72 ℃ under 0.02MPa in vacuum, placing the ceramic layer-containing wire core in a container, introducing ozone at 33mL/min, introducing ozone for 27min, irradiating the ceramic layer-containing wire core with an ultraviolet lamp with the power of 8W and the wavelength of 253.7nm, treating for 17min, spin-coating a carbon quantum dot solution at 2300rmp/min, wherein the mass ratio of carbon quantum dots to toluene in the carbon quantum dot solution is 1:10, after spin-coating for 53s, drying for 1.5h at 77 ℃, soaking in absolute ethyl alcohol 12 times of the mass of the ceramic layer-containing wire core, adding 3, 6-octanediol 0.24 times of the mass of the ceramic layer-containing wire core, ultrasonically mixing for 14min at 35kHz, placing the ceramic layer-containing wire core in a para-polyphenyl lining hydrothermal reaction kettle, heating to 176 ℃, preserving heat for 1.5h, cooling to room temperature to obtain the modified optical fiber;
(5) and (3) secondary modification treatment: placing the modified optical fiber in a container, adding tert-butyl acrylate with the mass of 1.07 times of that of the modified optical fiber and tetraisopropyl titanate with the mass of 0.004 time of that of the modified optical fiber, heating to 176 ℃ under the protection of nitrogen, reacting for 8-10 hours, and washing for 4 times by using deionized water; and then adding methanol which is 0.98 times of the mass of the modified optical fiber and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine which is 1.56 times of the mass of the modified optical fiber, uniformly stirring, heating to 46 ℃, reacting for 11h, distilling for 2h at the temperature of 55 ℃ under the pressure of 0.2MPa, cooling to room temperature, and drying for 3h at the temperature of 74 ℃ to obtain the broadband low-dispersion optical fiber.
Comparative example 1
Comparative example 1 differs from example 3 only in step (1), step (1) being changed to: polishing low-dispersion optical glass to obtain a wire core with the diameter of 10mm, ultrasonically cleaning the wire core with acetone at 30kHz for 24min, placing the wire core in a container, vacuumizing to 0.07Pa, introducing silane, methane, hydrogen and nitrogen according to the flow ratio of 1:1:13:16 until the air pressure is 30MPa, heating to 540 ℃, and depositing for 31min to obtain the silicon-carbon-nitrogen film wire core. The rest of the preparation steps are the same as example 3
Comparative example 2
Comparative example 2 differs from example 3 only in step (2), step (2) being changed to: placing the silicon-carbon-nitrogen film wire core in a laser device, connecting the laser device with a 300V direct current electric field, and vacuumizing to 10 DEG-5Pa, under the argon atmosphere, adopting hexagonal boron nitride as a target material, wherein the distance between the target material and the substrate is 7cm, and the laser density is 20J/cm2And the laser wavelength is 532nm, and the boron nitride film wire core is obtained by deposition for 17 min. The rest of the preparation steps are the same as example 3.
Comparative example 3
Comparative example 3 differs from example 3 only in step (2), step (2) being changed to: placing the silicon-carbon-nitrogen film wire core in plasma equipment with power of 140W, vacuumizing to 30Pa, pre-sputtering for 12min in argon atmosphere, placing in laser equipment, and vacuumizing to 10 DEG-5Pa, under the argon atmosphere, adopting hexagonal boron nitride as a target material, wherein the distance between the target material and the substrate is 7cm, and the laser density is 20J/cm2And the laser wavelength is 532nm, and the boron nitride film wire core is obtained by deposition for 17 min. The remaining preparation steps were as in example 3.
Comparative example 4
Comparative example 4 differs from example 3 only in that step (3) is not present, and the remaining preparation steps are the same as in example 3.
Comparative example 5
Comparative example 5 differs from example 3 only in step (4), which was changed to: soaking the ceramic layer-containing wire core in absolute ethyl alcohol with the mass of 12 times that of the ceramic layer-containing wire core, adding 3, 6-octanediol with the mass of 0.24 time that of the ceramic layer-containing wire core, ultrasonically mixing for 14min at 35kHz, placing in a p-polyphenyl lining hydrothermal reaction kettle, heating to 176 ℃, preserving heat for 1.5h, and cooling to room temperature to obtain the modified optical fiber. The remaining preparation steps were as in example 3.
Comparative example 6
Comparative example 6 differs from example 3 only in step (4), which was changed to: cleaning the ceramic layer-containing wire core for 5 times by using detergent and absorbent cotton, then carrying out ultrasonic treatment for 12min at 28kHz by using deionized water, acetone, isopropanol and absolute ethyl alcohol in sequence, drying for 39min at 72 ℃ under 0.02MPa in vacuum, placing the ceramic layer-containing wire core in a container, introducing ozone at 33mL/min, introducing 27min, irradiating 15mm above the ceramic layer-containing wire core by using an ultraviolet lamp with the power of 8W and the wavelength of 253.7nm, carrying out treatment for 17min, then spin-coating a carbon quantum dot solution at 2300rmp/min, wherein the mass ratio of carbon quantum dots to toluene in the carbon quantum dot solution is 1:10, and drying for 1.5h at 77 ℃ after 53s of spin-coating to obtain the modified optical fiber.
Comparative example 7
Comparative example 7 differs from example 3 only in step (5), which was changed to: putting the modified optical fiber into a container, adding methanol which is 0.98 time of the mass of the modified optical fiber and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine which is 1.56 times of the mass of the modified optical fiber, uniformly stirring, heating to 46 ℃, reacting for 11 hours, distilling at 0.2MPa and 55 ℃ for 2 hours, cooling to room temperature, and drying at 74 ℃ for 3 hours to obtain the broadband low-dispersion optical fiber. The rest of the preparation steps are the same as example 3.
Examples of effects
Table 1 below shows the results of performance analysis of optical fibers using examples 1 to 3 of the present invention and comparative examples 1 to 7.
TABLE 1
Comparing the absorption loss experimental data of the embodiment and the comparative example, it can be found that a uniform and compact interlayer ceramic layer is formed on the surface of the low-dispersion glass by the first deposition process, the second deposition process and the sintering process in sequence, the boron nitride film and the silicon carbon nitrogen film are fused and bonded, the cross-linking is tight, the dielectric constants and the dielectric losses of the silicon carbon nitrogen film and the boron nitride film are low, the frequency band of the optical fiber is widened under the combined action, and meanwhile, the interlayer structure of the ceramic layer enables the reflection generated by the optical fiber to be mutually offset in a certain frequency band range, so that the broadband performance of the optical fiber is improved; compared with the experimental data of the loss change rate of the embodiment and the comparative example, the carbon quantum dot film is introduced into the optical fiber film to form the ultraviolet shielding film, and the 3, 6-octanediol, the tert-butyl acrylate and the bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine are sequentially used for modifying the ultraviolet shielding film to form the light stabilizing film on the basis of the carbon quantum dot film, so that the absorption of ultraviolet rays by the optical fiber is further reduced, the light aging phenomenon of the optical fiber is effectively delayed, the service life of the optical fiber is prolonged, the regeneration and stable existence of the ultraviolet shielding film on the surface of the optical fiber can be promoted, and the light aging resistance of the optical fiber is effectively improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The broadband low-dispersion optical fiber is characterized by comprising a wire core, a ceramic layer and an ultraviolet shielding film in sequence from inside to outside; the wire core is low dispersion optical glass.
2. The broadband low dispersion optical fiber of claim 1, wherein said ceramic layer is formed by a first deposition process, a second deposition process, and a sintering process.
3. The broadband low dispersion optical fiber of claim 2, wherein said first deposition process: by utilizing hot wire chemical vapor deposition and with the help of microwave discharge, rapidly depositing a silicon-carbon-nitrogen film on the surface of the wire core to prepare a silicon-carbon-nitrogen film wire core; the second deposition process comprises the following steps: and depositing the boron nitride film by using a direct current electric field-plasma auxiliary pulse laser to prepare the boron nitride film wire core.
4. The broadband low-dispersion optical fiber of claim 3, wherein the UV-shielding film is prepared by pre-treating a ceramic layer, spin-coating a carbon quantum dot solution on the surface, and modifying the surface with 3, 6-octanediol, tert-butyl acrylate, and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine.
5. A method for preparing a broadband low-dispersion optical fiber is characterized by comprising the following preparation steps:
(1) the first deposition process: polishing low-dispersion optical glass to obtain a wire core with the diameter of 5-15 mm, ultrasonically cleaning the wire core with acetone at 25-35 kHz for 18-30 min, placing the wire core in a microwave discharge system, vacuumizing to 0.02-0.1 Pa, introducing silane, methane, hydrogen and nitrogen according to a flow ratio of 1:1:10: 12-1: 1:15:18 until the air pressure is 20-40 MPa, heating to 400-600 ℃, and depositing for 22-41 min to obtain a silicon-carbon-nitrogen film wire core;
(2) and (3) a second deposition process: placing the silicon-carbon-nitrogen film wire core in plasma equipment, vacuumizing to 20-40 Pa, pre-sputtering for 10-13 min in an argon atmosphere, placing in laser equipment, connecting the laser equipment with a direct current electric field, and vacuumizing to 10 DEG-6～10-4In the atmosphere of Pa and argon, depositing for 15-22 min by using hexagonal boron nitride as a target to obtain a boron nitride film wire core;
(3) the sintering process comprises the following steps: placing the boron nitride film wire core in a container, heating to 400-650 ℃ at a speed of 10-20 ℃/min under the nitrogen atmosphere and a pressure of 10-50 MPa, preserving heat for 25-40 min, heating to 800-1000 ℃ at a speed of 1-10 ℃/min, and then drawing wires to obtain a wire core containing a ceramic layer;
(4) modification treatment: pretreating a ceramic layer-containing wire core, spin-coating a carbon quantum dot solution at 2000-2500 rmp/min, wherein the mass ratio of carbon quantum dots to methylbenzene in the carbon quantum dot solution is 1: 8-1: 12, after spin-coating for 40-60 s, drying at 70-80 ℃ for 1-2 h, soaking in absolute ethyl alcohol which is 10-15 times of the mass of the ceramic layer-containing wire core, adding 3, 6-octanediol which is 0.1-0.3 times of the mass of the ceramic layer-containing wire core, ultrasonically mixing at 30-40 kHz for 10-20 min, placing in a para-polystyrene lining hydrothermal reaction kettle, heating to 170-180 ℃, preserving heat for 1-2 h, and cooling to room temperature to obtain a modified optical fiber;
(5) and (3) secondary modification treatment: placing the modified optical fiber into a container, adding tert-butyl acrylate accounting for 0.8-1.2 times of the mass of the modified optical fiber and tetraisopropyl titanate accounting for 0.001-0.006 times of the mass of the modified optical fiber, heating to 170-180 ℃ under the protection of nitrogen, reacting for 8-10 hours, and washing with deionized water for 3-6 times; and then adding methanol which is 0.6-1.1 times of the mass of the modified optical fiber and bis (2,2,6, 6-tetramethylpiperidin-4-yl) amine which is 1.3-1.7 times of the mass of the modified optical fiber, uniformly stirring, heating to 40-50 ℃, reacting for 10-12 h, distilling at 50-60 ℃ for 1-3 h under 0.1-0.3 MPa, cooling to room temperature, and drying for 2-4 h at 70-80 ℃ to obtain the broadband low-dispersion optical fiber.
6. The method as claimed in claim 5, wherein the microwave discharge system of step (1) has a frequency of 2400-2500 MHz and a power of 100-200W.
7. The method of claim 5, wherein the plasma sputtering power in step (2) is 100-150W.
8. The method according to claim 5, wherein the step (2) of the laser apparatus comprises: the distance between the target and the substrate is 5-10 cm, and the laser density is 12-25J/cm2The laser wavelength is 532nm, and the voltage of the direct current electric field is 200-400V.
9. The method of claim 5, wherein the drawing rate in step (3) is 1-4 mm/min; the diameter of the wire core of the ceramic-containing layer is 115-125 mu m.
10. The method of claim 5, wherein the step (4) of pretreating comprises: cleaning the ceramic layer-containing wire core for 3-6 times by using detergent and absorbent cotton, then carrying out ultrasonic treatment for 7-14 min at 25-30 kHz by using deionized water, acetone, isopropanol and absolute ethyl alcohol in sequence, drying for 30-45 min in vacuum at 60-80 ℃ and 0.01-0.03 MPa, placing in a container, introducing ozone at the rate of 30-40 mL/min, introducing for 20-30 min, irradiating 10-20 mm above the ceramic layer-containing wire core by using an ultraviolet lamp with the power of 5-10W and the wavelength of 253.7nm, and treating for 15-20 min.
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