CN109180023B - High-temperature-resistant optical fiber and preparation method thereof - Google Patents
High-temperature-resistant optical fiber and preparation method thereof Download PDFInfo
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- CN109180023B CN109180023B CN201811011940.5A CN201811011940A CN109180023B CN 109180023 B CN109180023 B CN 109180023B CN 201811011940 A CN201811011940 A CN 201811011940A CN 109180023 B CN109180023 B CN 109180023B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/104—Coating to obtain optical fibres
- C03C25/1065—Multiple coatings
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/48—Coating with two or more coatings having different compositions
- C03C25/50—Coatings containing organic materials only
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/10—Epoxy resins modified by unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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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
Abstract
The invention provides a high-temperature-resistant optical fiber and a preparation method thereof. The high-temperature resistant optical fiber comprises an optical fiber core layer, a cladding and a double-layer coating layer; the coating material of the inner coating consists of acrylate oligomer, 2-hydroxy-2-methyl propiophenone, vinyl tris (2-methoxyethoxy) silane and (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide; the outer coating is a high-temperature resistant acrylic resin outer coating. The high-temperature-resistant optical fiber can still maintain the reliability of optical fiber transmission in a high-temperature environment of 150 ℃ for a long time, and the phenomenon of aging failure such as yellowing and blackening of an optical fiber coating can not occur; the preparation method is simple, the optical fiber of the high-temperature resistant optical fiber prepared at the drawing speed of 2000-2200 m/min has low transmission loss, the attenuation value of the optical fiber at 1550nm is not more than 0.25dB/km, and the additional attenuation value of the optical fiber at 1550nm under the environment of 150 ℃ for a long time is not more than 0.05 dB/km.
Description
Technical Field
The invention belongs to the technical field of optical fiber processing, relates to an optical fiber and a preparation method thereof, in particular to a high-temperature resistant optical fiber and a preparation method thereof, and particularly relates to a low-loss high-temperature resistant optical fiber and a high-speed drawing preparation method thereof.
Background
With the rapid development of the optical communication field, optical fibers have been widely used as base materials in many fields. Different application scenes have different requirements on the performance of the optical fiber, for example, the high-temperature fields such as high-temperature sensing, oil and gas field wells and the like have special requirements on the temperature resistance of the optical fiber. The conventional optical fiber can only ensure the long-term service life at the ambient temperature of-60-85 ℃ at present, and cannot meet the use reliability at higher temperature. In order to meet the use requirements in high temperature environments, the optical fiber must maintain optical properties, mechanical strength, and reliability consistent or similar to those in normal temperature and normal use environments.
In the design of high-temperature resistant optical fibers, high-temperature resistant acrylic resin, silicone rubber, polyimide and the like are generally used as coating materials; and different coating processes are adopted for manufacturing, so that the service performance at different temperatures is met. Such fibers have low optical loss at optical wavelengths of 1310nm and 1550nm, typically less than 0.5 dB/km. Acrylate coated optical fibers are widely used for optical fiber communication and the maximum temperature at which they can operate normally is 85 ℃. However, when the temperature exceeds 85 ℃, the acrylate coating can be seriously aged or even failed, the color of the coating turns yellow or black, the mechanical strength is weakened until the protection effect on the optical fiber is lost, the optical fiber is easy to break, and the reliability requirement of optical fiber transmission in a high-temperature environment cannot be met.
CN102109636A discloses a high-temperature-resistant radiation-resistant optical fiber and a processing technology thereof, wherein the optical fiber comprises a fiber core, a cladding and a coating layer, the coating layer comprises a sputtering coating layer, and an electroplating coating layer is electroplated outside the sputtering coating layer. The sputter coating layer comprises one of a sputter aluminum coating film, a sputter copper coating film, a sputter nickel coating film, a sputter chromium coating film or a sputter gold coating film. The plating film layer includes one of an aluminum plating layer, a copper plating layer, a nickel plating layer, a chromium plating layer, a gold plating layer, a cobalt plating layer, or a lead plating layer. The invention uses metal material as coating, because the high-low temperature performance of the metal material is far better than that of the high molecular material, and can shield the irradiation well, and the optical fiber with the metal coating has good high temperature resistance, and can resist the high temperature of more than 400 ℃. However, since the hardness of the metal coating is much greater than that of the polymer coating and the coefficient of thermal expansion of the metal coating is much different from that of the glass cladding, a severe microbending effect is generated on the optical fiber, resulting in an increase in optical loss of the metal-coated optical fiber. The optical loss of metal coated fibers at 1310nm and 1550nm can be as high as 5dB/km or more, which limits the usable length of these metal coated fibers, typically only within 200 meters.
CN101726792A discloses a high temperature resistant optical fiber and a manufacturing method thereof, the high temperature resistant optical fiber comprises an optical fiber and a coating coated on the outer surface of the optical fiber, wherein the coating is a polyimide coating, is formed by dip-coating the outer surface of the optical fiber with a polyimide solution and heating and curing, and comprises pre-coating, pre-curing and secondary coating; the optical fiber can be used in high-temperature and severe working environment, the long-term use temperature can reach 300 ℃, the use characteristic is stable, and good durability can be maintained. However, the attenuation value of the high-temperature resistant optical fiber prepared by the invention at 1550nm is 0.5dB/km, the transmission loss of the optical fiber is large, and the high-temperature resistant optical fiber is not suitable for long-distance use.
CN103323906A discloses a high temperature resistant optical fiber, which is a single mode optical fiber, a multimode optical fiber, a polarization maintaining optical fiber, a rare earth doped optical fiber or a large numerical aperture optical fiber. The high-temperature resistant optical fiber has the screening strength of 100kpsi or 200kpsi, the typical Nd value is more than 20, and the high-temperature resistant optical fiber can provide commercial segment length more than 60km and is suitable for long-distance and long-span application. The invention adopts acrylic resin to carry out one-time single-layer coating, simplifies the optical fiber coating manufacturing process, and in addition, the uniformity of the single-coating material ensures the stability of the temperature resistance of the optical fiber at the environment temperature of 150 ℃, and can be used for a long time in a severe environment and used for a short time at the environment temperature of 200 ℃. However, when the optical fiber is prepared, the drawing speed is 200-1500 m/min, the drawing speed is too low, the productivity is low, the geometric parameters of the optical fiber can be influenced, and higher production cost can be brought, and although the single-layer coating simplifies the coating process, the optical fiber has large transmission loss and is not suitable for long-distance use.
Disclosure of Invention
In view of the defects of the prior art, an object of the present invention is to provide a high temperature resistant optical fiber, which does not suffer from aging failures such as yellowing and blackening of the optical fiber coating at a high temperature of 150 ℃, can maintain the reliability of optical fiber transmission even in a high temperature environment of 150 ℃ for a long time, and has low optical fiber transmission loss.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-temperature-resistant optical fiber comprises an optical fiber core layer, a cladding layer and a double-layer coating layer, wherein the double-layer coating layer comprises an inner coating and an outer coating; the coating material of the inner coating consists of acrylate oligomer, 2-hydroxy-2-methyl propiophenone, vinyl tris (2-methoxyethoxy) silane and (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide; the outer coating is a high-temperature-resistant acrylic resin outer coating.
The high temperature resistance in the high temperature resistant optical fiber is 150 ℃, the phenomenon of aging failure such as yellowing and blackening of an optical fiber coating can not occur, the loss of the protection effect on the optical fiber due to weakened mechanical strength can not occur, and the reliability of optical fiber transmission can still be maintained in the high temperature environment of 150 ℃ for a long time.
The low-loss high-temperature-resistant optical fiber means that the attenuation value of the optical fiber at 1550nm is not more than 0.25dB/km, and the additional attenuation value of the optical fiber at 1550nm is not more than 0.05dB/km in a 150 ℃ high-temperature environment.
The double-layer coating layer comprises an inner coating and an outer coating, wherein the inner coating enables the optical fiber to have higher toughness and strength, and the outer coating enables the optical fiber to still have low loss and reliable optical fiber transmission performance in a high-temperature environment of 150 ℃.
In the invention, the coating material of the inner coating comprises the following components in parts by weight:
preferably, the coating material of the high-temperature resistant acrylic resin outer coating consists of the following components in parts by weight:
specifically, the coating material of the inner coating comprises the following components in parts by weight:
20-80 parts of acrylate oligomer, for example, 20 parts, 30 parts, 40 parts, 50 parts, 60 parts, 70 parts and 80 parts of acrylate oligomer.
2-10 parts of 2-hydroxy-2-methyl propiophenone, for example, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts and 10 parts of 2-hydroxy-2-methyl propiophenone.
1-5 parts of vinyl tri (2-methoxyethoxy) silane, such as 1 part, 2 parts, 3 parts, 4 parts and 5 parts of vinyl tri (2-methoxyethoxy) silane.
1-8 parts of (2, 4, 6-trimethylbenzoyl) diphenylphosphine oxide, for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts of (2, 4, 6-trimethylbenzoyl) diphenylphosphine oxide.
Preferably, the coating material of the outer coating consists of the following components in parts by weight:
50-60 parts of epoxy acrylic resin, for example, 50 parts, 51 parts, 52 parts, 53 parts, 54 parts, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts and 60 parts of epoxy acrylic resin.
20-40 parts of trimethylolpropane triacrylate, for example, 20 parts, 25 parts, 30 parts, 35 parts and 40 parts of trimethylolpropane triacrylate.
10-20 parts of tripropylene glycol diacrylate, for example, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts and 20 parts of tripropylene glycol diacrylate by weight.
1-10 parts of benzophenone/tertiary amine system, such as 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts and 10 parts of benzophenone/tertiary amine system, wherein the benzophenone/tertiary amine system is a photoinitiator commonly used in the field.
Preferably, the thickness of the double-layer coating layer is 30-40 μm, for example, the thickness of the double-layer coating layer is 30 μm, 31 μm, 32 μm, 33 μm, 34 μm, 35 μm, 36 μm, 37 μm, 38 μm, 39 μm, 40 μm.
The optical fiber core layer and the cladding layer are both made of quartz glass.
In the invention, the high-temperature resistant optical fiber is one of a single-mode optical fiber and a multi-mode optical fiber.
The second purpose of the present invention is to provide a method for preparing a high temperature resistant optical fiber, which has the advantages of simple preparation process, high productivity of the optical fiber, and capability of preparing a high temperature resistant optical fiber with good appearance, stable and consistent diameter, high toughness, good strength and low loss, and the preparation method comprises the following steps:
1) melting and drawing the optical rod by using a graphite resistance furnace;
2) drawing, discharging, annealing and cooling, and entering a double-layer coating die for coating to obtain an optical fiber with a double-layer coating layer;
3) curing the coated optical fiber by using ultraviolet light;
4) and winding the optical fiber on an optical fiber disc by using a take-up device to finish the preparation of the high-temperature resistant optical fiber.
In the step 1), the melting temperature is 1900-2200 ℃, for example, the melting temperature is 1900 ℃, 2000 ℃, 2100 ℃, 2200 ℃.
Preferably, the drawing speed is 2000-2200 m/min, such as 2000m/min, 2010m/min, 2020m/min, 2030m/min, 2040m/min, 2050m/min, 2060m/min, 2070m/min, 2080m/min, 2090m/min, 2100m/min, 2110m/min, 2120m/min, 2130m/min, 2140m/min, 2150m/min, 2160m/min, 2170m/min, 2180m/min, 2190m/min, 2200 m/min. If the drawing speed is too low, which is lower than 2000m/min, the productivity is low, and the diameter of the optical fiber cannot be well controlled, and the diameter error is larger than 10 μm; if the drawing speed is too high, and the degree of polymerization of the coating is not high, the curing is not good, so that the strength of the optical fiber is poor, and the attenuation performance is poor.
Preferably, the light stick is one of a g.652 light stick, a g.654 light stick or a g.657 light stick. The optical rod comprises a core layer and a cladding layer, namely the optical fiber made by drawing the optical rod comprises the core layer and the cladding layer.
In the step 2), the coating pressure of the inner coating is 0.3-3 bar, for example, the coating pressure of the inner coating is 0.3bar, 0.5bar, 1bar, 1.5bar, 2bar, 2.5bar, 3 bar; the coating pressure of the external coating is 3-5.5 bar, for example, the coating pressure of the external coating is 3bar, 3.5bar, 4bar, 4.5bar, 5bar, 5.5 bar.
Preferably, the coating temperature is 20-45 ℃, for example, the coating temperature is 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃, 39 ℃, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃.
In addition, different coating diameters can be controlled by adjusting the double coating die, for example, adjusting the double coating die can provide high temperature resistant optical fibers of both 200 μm and 245 μm diameter sizes.
In the step 3), the curing is performed on the coated optical fiber by using 1-6 UV lamps.
When the preparation method disclosed by the invention is used for coating, the specific coating pressure, coating temperature and UV lamp power need to be adjusted and matched along with the specific drawing speed of the optical fiber, and the optical fiber is coated abnormally or even emits glue due to poor matching control, so that the quality of the optical fiber is influenced.
Preferably, the preparation method of the high temperature resistant optical fiber comprises the following steps:
1) melting the optical rod at 1900-2200 ℃ by using a graphite resistance furnace, and drawing at a drawing speed of 2000-2200 m/min;
2) drawing, discharging, annealing and cooling at normal temperature, and entering a double-layer coating die for coating to obtain an optical fiber with a double-layer coating layer, wherein the coating pressure of an inner coating layer is 0.3-3 bar, the coating pressure of an outer coating layer is 3-5.5 bar, and the coating temperature is 20-45 ℃;
3) curing the coated optical fiber by adopting ultraviolet light by adopting 1-6 UV lamps;
4) and winding the optical fiber on an optical fiber disc by using a take-up device to finish the preparation of the high-temperature resistant optical fiber.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the high-temperature-resistant optical fiber, the optical fiber coating does not have the aging failure phenomena of yellowing, blackening and the like at the high temperature of 150 ℃, the reliability of optical fiber transmission can be still maintained in the high-temperature environment of 150 ℃ for a long time, the optical fiber has the screening strength of more than 100kpsi and the dynamic fatigue parameter Nd value of more than 20 under the environment that the environmental temperature is 18-28 ℃ and the relative humidity is 40-60%; the high-temperature resistant optical fiber has low optical fiber transmission loss, the attenuation value of the optical fiber at 1550nm is not more than 0.25dB/km, and the additional attenuation value of the optical fiber at 1550nm under the environment of 150 ℃ for a long time is not more than 0.05 dB/km.
(2) The preparation method of the high-temperature-resistant optical fiber is simple in preparation process, has high productivity at the wire drawing speed of 2000-2200 m/min, and can prepare the high-temperature-resistant optical fiber with stable and consistent diameter, good toughness, good strength and low loss.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The high-temperature resistant optical fiber of the embodiment is prepared by the following process:
(1) carrying out high-temperature melt drawing on an online rod optical rod at 2000 ℃ in a graphite furnace, controlling the speed to 2200m/min, and allowing a certain error to exist in the diameter of the optical rod;
(2) the optical fiber subjected to melt drawing is annealed and cooled at normal temperature and then directly enters a double-layer coating die to be coated at one time, matching of gas at the melting end of an optical rod and speed is controlled through a PSU system, different coating diameters can be controlled by adjusting the die, the coating pressure of an inner coating is 2.5bar, the coating pressure of an outer coating is 5bar, and the coating temperature is 40 ℃;
(3) curing the coated optical fiber under the high power of 6 UV lamps;
(4) and (3) taking up the automatic take-up device to prepare the high-temperature-resistant optical fiber with the diameter of 200 mu m.
The coating material of the inner coating comprises the following components in parts by weight:
the coating material of the high-temperature-resistant acrylic resin outer coating comprises the following components in parts by weight:
example 2
The high-temperature resistant optical fiber of the embodiment is prepared by the following process:
(1) carrying out 2200 ℃ high-temperature melting and wire drawing on an online rod optical rod in a graphite furnace, controlling the speed to be 2100m/min, and allowing a certain error to exist in the diameter of the optical rod;
(2) the optical fiber subjected to melt drawing is annealed and cooled at normal temperature and then directly enters a double-layer coating die to be coated at one time, matching of gas at the melting end of an optical rod and speed is controlled through a PSU system, different coating diameters can be controlled by adjusting the die, the coating pressure of an inner coating is 1bar, the coating pressure of an outer coating is 4.5bar, and the coating temperature is 35 ℃;
(3) curing the coated optical fiber under the high power of 5 UV lamps;
(4) and (3) taking up the automatic take-up device to prepare the high-temperature-resistant optical fiber with the diameter of 200 mu m.
The coating material of the inner coating comprises the following components in parts by weight:
the coating material of the high-temperature-resistant acrylic resin outer coating comprises the following components in parts by weight:
example 3
The high-temperature resistant optical fiber of the embodiment is prepared by the following process:
(1) carrying out 1900 ℃ high-temperature melt wire drawing on an online rod optical rod in a graphite furnace, controlling the speed to be 2000m/min, and allowing the diameter of the optical rod to have a certain error;
(2) the optical fiber subjected to melt drawing is annealed and cooled at normal temperature and then directly enters a double-layer coating die to be coated at one time, matching of gas at the melting end of an optical rod and speed is controlled through a PSU system, different coating diameters can be controlled by adjusting the die, the coating pressure of an inner coating is 3bar, the coating pressure of an outer coating is 5.5bar, and the coating temperature is 45 ℃;
(3) curing the coated optical fiber under the high power of 6 UV lamps;
(4) and (3) taking up the optical fiber by using an automatic take-up device to prepare the high-temperature-resistant optical fiber with the diameter of 245 mu m.
The coating material of the inner coating comprises the following components in parts by weight:
the coating material of the high-temperature-resistant acrylic resin outer coating comprises the following components in parts by weight:
example 4
The high-temperature resistant optical fiber of the embodiment is prepared by the following process:
(1) melting and drawing an on-line rod polished rod at 1950 ℃ in a graphite furnace, controlling the speed to be 2050m/min, and allowing a certain error to exist in the diameter of the polished rod;
(2) the optical fiber subjected to melt drawing is annealed and cooled at normal temperature and then directly enters a double-layer coating die to be coated at one time, matching of gas at the melting end of an optical rod and speed is controlled through a PSU system, different coating diameters can be controlled by adjusting the die, the coating pressure of an inner coating is 1bar, the coating pressure of an outer coating is 3.5bar, and the coating temperature is 25 ℃;
(3) curing the coated optical fiber under the high power of 3 UV lamps;
(4) and (3) taking up the automatic take-up device to prepare the high-temperature-resistant optical fiber with the diameter of 200 mu m.
The coating material of the inner coating comprises the following components in parts by weight:
the coating material of the high-temperature-resistant acrylic resin outer coating comprises the following components in parts by weight:
example 5
The high-temperature resistant optical fiber of the embodiment is prepared by the following process:
(1) carrying out high-temperature melt drawing on an online rod optical rod at 2000 ℃ in a graphite furnace, controlling the speed to 2200m/min, and allowing a certain error to exist in the diameter of the optical rod;
(2) the optical fiber subjected to melt drawing is annealed and cooled at normal temperature and then directly enters a double-layer coating die to be coated at one time, matching of gas at the melting end of an optical rod and speed is controlled through a PSU system, different coating diameters can be controlled by adjusting the die, the coating pressure of an inner coating is 2bar, the coating pressure of an outer coating is 4bar, and the coating temperature is 20-4530 ℃;
(3) curing the coated optical fiber under the high power of 6 UV lamps;
(4) and (3) taking up the automatic take-up device to prepare the high-temperature-resistant optical fiber with the diameter of 200 mu m. The coating material of the inner coating comprises the following components in parts by weight:
the coating material of the high-temperature-resistant acrylic resin outer coating comprises the following components in parts by weight:
comparative example 1
The comparative example is different from example 1 in that the drawing speed was 1200m/min, and the others were the same as example 1.
Comparative example 2
The comparative example is different from example 1 in that the drawing speed was 2500m/min, and the others were the same as example 1.
Comparative example 3
This comparative example differs from example 1 in that the application pressure of the overcoat layer was 7bar and the application temperature was 50 ℃, all other things being equal to example 1.
Comparative example 4
This comparative example differs from example 1 in that the application pressure of the overcoat layer was 2bar and the application temperature was 10 ℃, all other things being equal to example 1.
Comparative example 5
This comparative example differs from example 1 in that the internal coating was applied at a pressure of 5bar and at a temperature of 50 c, all the same as in example 1.
Comparative example 6
The comparative example is different from example 1 in that the coating layer is a single layer and the coating material is an acrylic resin material, and the rest is the same as example 1.
Comparative example 7
This comparative example is different from example 1 in that the coating materials of the undercoat layer and the overcoat layer are both high temperature resistant acrylic resin coating materials, and the others are the same as example 1.
Comparative example 8
This comparative example differs from example 1 in that the coating materials of the undercoat layer and the overcoat layer are each a coating material composed of an acrylate oligomer, 2-hydroxy-2-methylpropiophenone, vinyltris (2-methoxyethoxy) silane and (2, 4, 6-trimethylbenzoyl) diphenylphosphine oxide, and the others are the same as in example 1.
The high temperature resistant optical fibers prepared in examples 1 to 5 and the optical fibers prepared in comparative examples 1 to 5 were subjected to performance tests under the environment of an ambient temperature of 18 ℃ to 28 ℃ and a relative humidity of 40% to 60%, wherein the screening strength test was performed according to GB-T15972.30-2008, part 30, the dynamic fatigue parameter test was performed according to GB-T15972.33-2008, part 33, the loss values of the optical fibers at 1310nm and 1550nm were measured by OTDR, and the additional attenuation typical value test was performed according to GB-T15972.40-2008, part 40.
Wherein, the screening strength of the high temperature resistant optical fiber prepared in example 1 is 100kpsi, the attenuation values of the optical fiber at 1310nm and 1550nm are 0.321dB/km and 0.183dB/km respectively, and the additional attenuation value at 1550nm under the long-term 150 ℃ environment is 0.01 dB/km.
The diameter of the optical fiber prepared in the comparative example 1 is more than 210 μm, the diameter size is unqualified, and the phenomenon of glue leakage occurs; the attenuation of the optical fiber prepared in the comparative example 2 at 1550nm is more than 0.25dB/km, and the loss is too large and is not qualified; the optical fibers prepared in comparative examples 3, 4, and 5 were coated abnormally and the attenuation at 1550nm was greater than 0.25dB/km, the loss was too large and failed; the attenuation of the optical fiber prepared in the comparative example 6 at 1550nm is 0.7dB/km, and the transmission loss of the optical fiber is large;
the optical fiber prepared in comparative example 7 has poor strength although it has good high temperature resistance, and it is difficult to prepare a 24km standard disc sample; the optical fiber prepared in comparative example 8 rapidly aged to yellow at 150 deg.C, and additionally attenuated more than 1dB/km at 1550nm and was not recoverable.
In conclusion, the high-temperature-resistant optical fiber provided by the invention has the advantages that the optical fiber coating does not have aging failure phenomena such as yellowing and blackening at the high temperature of 150 ℃, and the reliability of optical fiber transmission can be still maintained in the high-temperature environment of 150 ℃ for a long time; the high-temperature resistant optical fiber has low optical fiber transmission loss, the attenuation value of the optical fiber at 1550nm is not more than 0.25dB/km, and the additional attenuation value of the optical fiber at 1550nm under the environment of 150 ℃ for a long time is not more than 0.05 dB/km.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (9)
1. A high-temperature-resistant optical fiber consists of an optical fiber core layer, a cladding layer and a double-layer coating layer, and is characterized in that the double-layer coating layer consists of an inner coating and an outer coating; the coating material of the inner coating consists of acrylate oligomer, 2-hydroxy-2-methyl propiophenone, vinyl tris (2-methoxyethoxy) silane and (2, 4, 6-trimethylbenzoyl) diphenyl phosphine oxide; the outer coating is a high-temperature-resistant acrylic resin outer coating;
the preparation method of the high-temperature resistant optical fiber comprises the following steps:
1) melting and drawing the optical rod by using a graphite resistance furnace;
2) drawing, discharging, annealing and cooling, and entering a double-layer coating die for coating to obtain an optical fiber with a double-layer coating layer;
3) curing the coated optical fiber by using ultraviolet light;
4) winding the optical fiber on an optical fiber disc by using a take-up device to finish the preparation of the high-temperature resistant optical fiber;
in the step 1), the wire drawing speed is 2000-2200 m/min;
in the step 2), the coating pressure of the inner coating is 0.3-3 bar, the coating pressure of the outer coating is 3-5.5 bar, and the coating temperature is 20-45 ℃;
the coating material of the inner coating comprises the following components in parts by weight:
the coating material of the high-temperature-resistant acrylic resin outer coating comprises the following components in parts by weight:
2. the high-temperature-resistant optical fiber according to claim 1, wherein the thickness of the double coating layer is 30-40 μm.
3. The high temperature resistant optical fiber according to claim 1 or 2, wherein the core layer and the cladding layer are both made of quartz glass.
4. The high temperature resistant optical fiber according to claim 1 or 2, wherein the high temperature resistant optical fiber is one of a single mode optical fiber and a multimode optical fiber.
5. A method for preparing a high temperature resistant optical fiber according to any one of claims 1 to 4, comprising the steps of:
1) melting and drawing the optical rod by using a graphite resistance furnace;
2) drawing, discharging, annealing and cooling, and entering a double-layer coating die for coating to obtain an optical fiber with a double-layer coating layer;
3) curing the coated optical fiber by using ultraviolet light;
4) winding the optical fiber on an optical fiber disc by using a take-up device to finish the preparation of the high-temperature resistant optical fiber;
in the step 1), the wire drawing speed is 2000-2200 m/min;
in the step 2), the coating pressure of the inner coating is 0.3-3 bar, the coating pressure of the outer coating is 3-5.5 bar, and the coating temperature is 20-45 ℃.
6. The method according to claim 5, wherein the melting temperature in step 1) is 1900 to 2200 ℃.
7. The method according to claim 5 or 6, wherein in step 1), the optical rod is one of a G.652 optical rod, a G.654 optical rod or a G.657 optical rod.
8. The method of claim 5, wherein in the step 3), the curing is performed by using 1-6 UV lamps to cure the coated optical fiber.
9. The method of claim 5, wherein the method of manufacturing the high temperature resistant optical fiber comprises the steps of:
1) melting the optical rod at 1900-2200 ℃ by using a graphite resistance furnace, and drawing at a drawing speed of 2000-2200 m/min;
2) drawing, discharging, annealing and cooling at normal temperature, and entering a double-layer coating die for coating to obtain an optical fiber with a double-layer coating layer, wherein the coating pressure of an inner coating layer is 0.3-3 bar, the coating pressure of an outer coating layer is 3-5.5 bar, and the coating temperature is 20-45 ℃;
3) curing the coated optical fiber by adopting ultraviolet light by adopting 1-6 UV lamps;
4) and winding the optical fiber on an optical fiber disc by using a take-up device to finish the preparation of the high-temperature resistant optical fiber.
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| CN201811011940.5A CN109180023B (en) | 2018-08-31 | 2018-08-31 | High-temperature-resistant optical fiber and preparation method thereof |
| PCT/CN2019/102490 WO2020043042A1 (en) | 2018-08-31 | 2019-08-26 | High temperature resistant optical fiber and preparation method therefor |
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| CN110304821A (en) * | 2019-07-16 | 2019-10-08 | 成都中住光纤有限公司 | A kind of small diameter fiber and its manufacturing method of low attenuation change |
| CN111548004A (en) * | 2020-05-15 | 2020-08-18 | 中天超容科技有限公司 | Optical fiber production equipment and preparation method and optical fiber |
| CN114276026B (en) * | 2021-11-25 | 2024-03-22 | 中天科技光纤有限公司 | Optical fiber preparation method and equipment |
| CN115417592B (en) * | 2022-08-31 | 2023-11-28 | 中天科技光纤有限公司 | Temperature-resistant optical fiber, and preparation method and preparation equipment thereof |
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| EP1209132A1 (en) * | 2000-11-22 | 2002-05-29 | Dsm N.V. | Coated optical fibers, primary coating composition, method for curing, as well as an assembly and a method for measuring |
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