CN111635127B - Optical fiber preform with functional quartz cladding and preparation method thereof - Google Patents
Optical fiber preform with functional quartz cladding and preparation method thereof Download PDFInfo
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- CN111635127B CN111635127B CN202010380326.7A CN202010380326A CN111635127B CN 111635127 B CN111635127 B CN 111635127B CN 202010380326 A CN202010380326 A CN 202010380326A CN 111635127 B CN111635127 B CN 111635127B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
- C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/01466—Means for changing or stabilising the diameter or form of tubes or rods
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Abstract
The functional cladding optical fiber preform prepared by the method can meet the requirements of the preform on optical performance, and the production cost is reduced.
Description
Technical Field
The invention belongs to the technical field of optical fibers, and particularly relates to an optical fiber preform containing a functional quartz cladding and a preparation method thereof.
Background
When manufacturing an optical fiber, the purified raw material must be made into a glass rod meeting certain requirements, which is called an optical fiber preform, wherein the optical fiber preform is an original rod body material for drawing the optical fiber, the inner layer is a core layer with high refractive index (n 1), and the outer layer is a cladding layer with low refractive index (n 2), and the optical fiber preform has refractive index distribution and geometric dimension meeting the requirements. Typical optical fiber preforms are about 10 to 25nm in diameter and about 60 to 120nm in length.
In the process of manufacturing communication optical fibers, one of the important contents is the preparation of optical fiber preforms, which is divided into the manufacture of a core rod and the manufacture of an outer cladding, namely, the manufacture of the core rod (comprising a core layer and an optical cladding layer) first, and then the deposition of the cladding layer outside the core rod to obtain the optical fiber preform. Currently, technologies for manufacturing an optical fiber preform mainly include an in-tube method typified by a plasma chemical vapor deposition method (PCVD) and a modified chemical vapor deposition Method (MCVD) and an out-tube method typified by an axial vapor deposition method (VAD) and an out-vapor deposition method ((OVD).
When the optical fiber preform is prepared by deposition by an off-tube method, a certain negative pressure is required to be provided for the deposition cavity by using an exhaust gas treatment device because reaction exhaust gas in the deposition cavity needs to be extracted. In the extraction process, the tail gas treatment equipment can not only extract the reaction waste gas, but also extract certain reaction products, namely nano silicon dioxide powder. When the cloth bag dust type dry tail gas treatment equipment is used, the nano silicon dioxide powder cake with low relative water content and low salt content can be obtained, and dust pollution can be caused by directly discharging the particles into the air. At present, the main treatment mode of the waste is landfill, but the landfill mode still causes a certain harm to the environment, especially soil, and wastes resources.
The optical fiber preform is prepared by using the sleeve method, so that the manufacturing process of the optical fiber preform can be changed from a one-step method to a two-step method, and the production efficiency is improved. The sleeve preform is composed of a core rod and a sleeve which are prepared in advance, and is finally an optical fiber or an optical fiber preform by vacuum extraction from the tail end of a sleeve tail handle and fusion shrinkage operation in a wire drawing furnace or an extension furnace. A schematic structural diagram of the sleeve preform is shown in fig. 1.
The core rod of the sleeve preform comprises a core layer and an inner cladding layer, wherein the inner cladding layer is quartz glass with a certain doping and refractive index adjustment, and the sleeve is used as an outer cladding layer of the optical fiber preform, and the outer cladding layer is generally pure quartz glass. The light guide structure of the whole optical fiber preform is mainly realized by the design of the core rod, so the preparation requirement on the core rod is very high. However, for some deposition processes, it is difficult to produce a low attenuation, super bend resistant mandrel that is difficult to achieve directly through the thimble rod process.
Disclosure of Invention
The invention aims to solve the technical problems that the design of the core layer of the optical fiber preform with complex refractive index profile design (multiple layers of different refractive indexes) and certain doping concentration requirement on the doping agent is difficult to carry out one-time deposition molding through VAD or OVD equipment in the prior art, and provides a preparation method of the optical fiber preform with a functional quartz cladding, which can avoid carrying out multiple deposition operations, and the optical fiber preform prepared by the method.
The technical scheme adopted for solving the technical problems is as follows: the invention provides a preparation method of an optical fiber preform rod containing a functional quartz cladding, which comprises the following steps:
(T1) pickling a quartz cladding sleeve and a core rod, and then assembling, wherein the core rod is provided with a tail handle, and the quartz cladding sleeve is provided with a tail handle;
(T2) filling high-purity quartz powder into a gap between the cladding sleeve and the core rod after the quartz cladding sleeve and the core rod in the step (T1) are assembled; preferably, the purity of the high purity quartz powder is not less than 99.999%;
(T3) filling a high-purity quartz column in the tail pipe; preferably, the high purity quartz column refers to a high purity quartz column with a special structure, for example, a quartz column with a hole in the middle and a longitudinal shallow groove on one end as shown in fig. 5;
(T4) mounting a tail cover plate: the tail cover plate with the barometer, the air inlet, the air extraction opening and the Teflon sealing ring is arranged at the tail end of the tail handle of the optical fiber preform and used for fixing the position of the core rod;
and (T5) hanging the optical fiber preform on a fusion shrinkage device, doping quartz powder, and then fusion shrinkage sintering to obtain the transparent glass rod.
In the method, in the step (T4), the barometer is installed at the outlet position of the air extraction opening, the valve is installed at the rear part, positive pressure and negative pressure of the barometer can be displayed, the valve is installed on the air inlet, three sealing rings are respectively fixed at the tail end of the mandrel tail, the tail high-purity quartz column end and the tail end of the sleeve tail from inside to outside to form two annular gaps between the mandrel tail and the tail high-purity quartz column and between the tail high-purity quartz column and the sleeve tail, and the two annular gaps can be communicated with the quartz powder area through slotting on the outer surface of the other end of the tail high-purity quartz column.
Further, in the above method, the doping treatment of the quartz powder in step (T5) includes: closing a valve of the air outlet, introducing mixed gas consisting of doping gas, helium, argon or nitrogen into the air inlet, continuously introducing the gas, then placing the preform into a heating furnace, and heating to 1200-1400 ℃ to enable the doping gas to fully react with the quartz powder. Preferably, wherein the doping gas is silicon tetrachloride or silicon tetrafluoride.
In a further step, in the above method, the melt-shrinking sintering method in step (T5) includes: after fully reacting the doped gas with the quartz powder, cooling to 600-800 ℃, opening an air extraction valve, extracting mixed gas in the preform under negative pressure, then opening an air inlet end valve, feeding helium or mixed gas of helium and the doped gas into the preform, heating to a fusion shrinkage temperature after the pressure representation number is stable, and fusing and shrinking the cladding sleeve, the doped quartz powder and the core rod into a complete transparent glass rod;
preferably, wherein the doping gas of step (T5) is silicon tetrachloride or silicon tetrafluoride.
Wherein step (T5), the effect of the different doping gases is different, the silicon tetrafluoride is introduced to produce a functional cladding with a lower refractive index than undoped quartz glass; silicon tetrachloride is introduced in order to produce a functional cladding with a higher refractive index than undoped quartz glass. For example, the refractive index profile distribution of the functional-cladding optical fiber preform prepared by doping silicon tetrachloride is schematically shown in FIG. 6; a schematic of the emissivity profile of a functional-cladding-containing optical fiber preform prepared using silicon tetrafluoride doping is shown in FIG. 7.
The second aspect of the present invention also provides an optical fiber preform prepared by the aforementioned method of the present invention.
The third aspect of the present invention also provides an optical fiber preform, comprising, in order from the inside to the outside of the central axis: the high-purity quartz powder is filled in a gap between the cladding sleeve with the tail handle and the core rod with the tail handle, and the high-purity quartz column is filled in a tail pipe.
Further, preferably, the tail end of the tail handle of the preform is provided with a tail cover plate with a barometer, an air inlet, an air extraction opening and a Teflon sealing ring for fixing the position of the core rod,
furthermore, the barometer is arranged at the outlet position of the air extraction opening, the valve is arranged at the rear part, and the positive pressure and the negative pressure of the barometer can be displayed; the air inlet is provided with a valve; the sealing rings are respectively fixed at the tail end of the core rod tail handle, the tail end of the high-purity quartz column and the tail end of the sleeve tail handle from inside to outside to form two annular gaps between the core rod tail handle and the tail high-purity quartz column and between the tail high-purity quartz column and the sleeve tail handle, and through grooving on the outer surface of the other end of the tail high-purity quartz column, the two annular gaps can be communicated with a quartz powder area.
Furthermore, the gap between the cladding sleeve with the tail handle and the core rod with the tail handle is filled with high-purity quartz powder, and the purity of the high-purity quartz powder is not lower than 99.999%. The tail pipe is filled with a high-purity quartz column, preferably the high-purity quartz column is a high-purity quartz column with a special structure, for example, a quartz column with a hole in the middle and a longitudinal shallow groove on one end as shown in fig. 5.
The beneficial effects of the invention are as follows:
first, the present invention provides a method for manufacturing an optical fiber preform having a functional silica cladding, which can satisfy the optical performance requirements of the optical fiber preform, such as the functional cladding region having an elevated or reduced refractive index as shown in fig. 6 and 7, and can reduce the production cost.
Secondly, in the prior art, for the design of the core layer of the optical fiber preform with complex refractive index profile design (multiple layers of different refractive indexes) and with certain doping concentration requirement on the doping agent, the one-time deposition molding is difficult to carry out through VAD or OVD equipment.
Third, the present invention also provides a method for simplifying the manufacturing difficulty of a part of a preform of a special structure, for example, an ultra-low loss G652 optical fiber preform, a G654 optical fiber preform, and a G657 optical fiber preform, in order to realize the optical characteristics thereof, it is necessary to provide certain low refractive index regions or high refractive index regions, and it is difficult to increase the doping concentration or to realize the doping in the conventional VAD or OVD process, and the method for manufacturing an optical fiber preform containing a functional quartz cladding layer provided by the present invention can solve the problem.
Drawings
The technical scheme of the application is further described below with reference to the accompanying drawings and examples.
FIG. 1 is a schematic illustration of a sleeve preform construction;
FIG. 2 is a schematic illustration of components of the preform prior to assembly;
FIG. 3 is a schematic illustration of the preform of FIG. 2 after assembly of the components and filling with quartz powder;
FIG. 4 is a schematic diagram of a preform tail cover assembly;
FIG. 5 is a schematic illustration of a high purity quartz column surface grooving;
FIG. 6 is a schematic view of a refractive index profile of a functional-cladding-containing optical fiber preform prepared using silicon tetrachloride doping in example 1 of the present application;
FIG. 7 is a schematic view of the refractive index profile of a functional-cladding-containing optical fiber preform prepared using silicon tetrafluoride doping in example 1 of the present application.
Detailed Description
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The high-purity quartz powder provided by the invention is quartz powder with purity not lower than 99.999%, and the high-purity quartz column is a quartz column made of quartz materials meeting or higher than GE214 standard. Other terms used in connection with the present invention are to be construed as having their ordinary meaning in the art unless specifically indicated otherwise.
Example 1 preparation of an optical fiber preform containing a functional cladding
And (3) pickling the quartz cladding sleeve and the core rod which is designed in advance, assembling in a hundred-grade clean space, and filling high-purity quartz powder (the purity is not lower than 99.999%) into a gap between the cladding sleeve and the core rod after assembling.
After the assembly of the prefabricated rod is completed, a barometer (positive pressure and negative pressure can be displayed and arranged at the outlet position of the extraction opening and a valve is arranged at the rear part) is arranged at the tail end of the tail handle of the prefabricated rod, and an air inlet (the valve is required to be arranged), the extraction opening and a tail cover plate of the Teflon sealing ring are used for fixing the position of the core rod. The cover plate is cooled by cooling water, and the structure of the cover plate is shown in figure 4
The three sealing rings are respectively fixed at the tail end of the mandrel tail handle, the tail high-purity quartz column and the tail end of the sleeve tail handle from inside to outside to form two annular gaps between the mandrel tail handle and the tail high-purity quartz column and between the tail high-purity quartz column and the sleeve tail handle, and through grooving on the outer surface of the other end of the tail high-purity quartz column, as shown in fig. 5, the two annular gaps can be communicated with the quartz powder area.
After the tail cover plate is installed, the prefabricated rod is hung on a melting and shrinking device, a valve of an air outlet is closed, and mixed gas of doping gas (silicon tetrachloride or silicon tetrafluoride can be used), helium gas and other inert gases (argon, nitrogen and the like) according to a certain proportion is introduced into the air inlet. Continuously introducing gas, observing positive pressure indication of a barometer at the extraction opening, and closing the gas inlet after the pressure required by the process is reached. The preform is then slowly lowered into a furnace and slowly warmed to 1200 to 1400 c (which is determined by the process requirements of the doping source, the desired doping concentration, etc.) and maintained at a temperature for a time to ensure adequate reaction of the dopants. Then gradually cooling to 800 ℃, opening an air extraction valve, extracting mixed gas in the preform with a certain negative pressure, opening an air inlet end valve after a certain process pressure is reached, feeding helium (or mixed gas of helium and doping gas) into the preform, gradually heating to a melting and shrinking temperature after the pressure representation number is stable, and melting and shrinking the cladding sleeve, doped quartz powder and the core rod into a complete transparent glass rod.
In this process, the effect of the different dopant gases is different. Silicon tetrafluoride is introduced to produce a functional cladding having a lower refractive index than undoped silica glass; silicon tetrachloride is introduced in order to produce a functional cladding with a higher refractive index than undoped quartz glass. The refractive index profile distribution of the prepared optical fiber preform is schematically shown in fig. 6 and 7, respectively.
With the above-described preferred embodiments according to the present application as a teaching, the related workers can make various changes and modifications without departing from the scope of the technical idea of the present application. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of claims.
Claims (8)
1. A method for preparing an optical fiber preform comprising a functional silica cladding, comprising the steps of:
(T1) pickling a quartz cladding sleeve and a core rod, and then assembling, wherein the core rod is provided with a tail handle, and the quartz cladding sleeve is provided with a tail handle;
(T2) filling high-purity quartz powder into a gap between the cladding sleeve and the core rod after the quartz cladding sleeve and the core rod in the step (T1) are assembled;
(T3) filling a high-purity quartz column in the tail pipe;
(T4) mounting a tail cover plate: the tail cover plate with the barometer, the air inlet, the air extraction opening and the Teflon sealing ring is arranged at the tail end of the tail handle of the optical fiber preform and used for fixing the position of the core rod;
(T5) hanging the optical fiber preform on a shrinking device, doping quartz powder, and then shrinking and sintering to obtain a transparent glass rod;
step (T4) the barometer is installed in extraction opening exit position, and the rear portion installs the valve, and its malleation and negative pressure all can show, install the valve on the air inlet, the sealing washer is three, fix respectively at core rod tail handle end, afterbody high purity quartz column end and sleeve pipe tail handle end from inside to outside, form two annular gaps that are located between core rod tail handle and afterbody high purity quartz column and sleeve pipe tail handle, through fluting at afterbody high purity quartz column other end surface for two annular gaps homoenergetic and quartz powder regional UNICOM.
2. The method of claim 1, wherein the doping of the quartz powder of step (T5) comprises: and closing a valve of the air outlet, introducing mixed gas consisting of doping gas, helium, argon or nitrogen into the air inlet, continuously introducing the gas, then placing the preform into a heating furnace, and heating to 1200-1400 ℃ to enable the doping gas and quartz powder to fully react.
3. The method of claim 2, wherein the melt-shrinkage sintering method of step (T5) comprises: and after the doped gas and the quartz powder fully react, cooling to 600-800 ℃, opening an air extraction valve, extracting mixed gas in the preform under negative pressure, opening an air inlet end valve, feeding helium or mixed gas of helium and the doped gas into the preform, heating to a fusion shrinkage temperature after the pressure representation number is stable, and fusing and shrinking the cladding sleeve, the doped quartz powder and the core rod into a complete transparent glass rod.
4. A method according to any one of claims 2 to 3, wherein the doping gas is silicon tetrachloride or silicon tetrafluoride.
5. The method of claim 1, wherein the high purity quartz powder has a purity of not less than 99.999%.
6. An optical fiber preform, characterized by being prepared by the method of any one of claims 1 to 5.
7. An optical fiber preform, characterized by comprising, in order from the inside to the outside, from a central axis: the device comprises a core rod with a tail handle, a tail high-purity quartz column and a quartz cladding sleeve with a tail handle, wherein the core rod with the tail handle is assembled in the quartz cladding sleeve, high-purity quartz powder is filled in a gap between the cladding sleeve with the tail handle and the core rod with the tail handle, and the tail pipe is filled with the high-purity quartz column;
the tail cover plate with the barometer, the air inlet, the air extraction opening and the Teflon sealing ring is arranged at the tail end of the tail handle of the preform rod and used for fixing the position of the core rod,
the barometer is arranged at the outlet position of the air extraction opening, the valve is arranged at the rear part, and the positive pressure and the negative pressure of the barometer can be displayed; the air inlet is provided with a valve; the sealing rings are respectively fixed at the tail end of the core rod tail handle, the tail end of the high-purity quartz column and the tail end of the sleeve tail handle from inside to outside to form two annular gaps between the core rod tail handle and the tail high-purity quartz column and between the tail high-purity quartz column and the sleeve tail handle, and through grooving on the outer surface of the other end of the tail high-purity quartz column, the two annular gaps can be communicated with a quartz powder area.
8. The optical fiber preform according to claim 7, wherein a gap between the cladding sleeve with the butt and the core rod with the butt is filled with high purity quartz powder, and the purity of the high purity quartz powder is not lower than 99.999%.
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CN202010380326.7A CN111635127B (en) | 2020-05-08 | 2020-05-08 | Optical fiber preform with functional quartz cladding and preparation method thereof |
PCT/CN2020/102946 WO2021223326A1 (en) | 2020-05-08 | 2020-07-20 | Optical fiber preform containing functional quartz cladding and preparation method therefor |
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EP0718244A2 (en) * | 1994-12-20 | 1996-06-26 | Corning Incorporated | Method of making optical fiber having depressed index core region |
CN107082558A (en) * | 2017-04-27 | 2017-08-22 | 烽火通信科技股份有限公司 | Method for manufacturing the preform of single-mode fiber and manufacturing single-mode fiber |
CN107098578A (en) * | 2017-04-27 | 2017-08-29 | 烽火通信科技股份有限公司 | Method for manufacturing the preform of sandwich construction optical fiber and manufacturing optical fiber |
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US3932162A (en) * | 1974-06-21 | 1976-01-13 | Corning Glass Works | Method of making glass optical waveguide |
US6263706B1 (en) * | 1999-03-30 | 2001-07-24 | Deliso Evelyn M. | Method of controlling fluorine doping in soot preforms |
US8132429B2 (en) * | 2004-04-27 | 2012-03-13 | Silitec Fibers Sa | Method for fabricating an optical fiber, preform for fabricating an optical fiber, optical fiber and apparatus |
EP1942083A1 (en) * | 2006-12-07 | 2008-07-09 | Datwyler Fiber Optics S.A. | Method and apparatus for fabricating a preform for an active optical fiber, active optical fiber and amplifier |
EP2226301A1 (en) * | 2009-02-22 | 2010-09-08 | Silitec Fibers SA | Method for producing and processing a preform, preform and optical fiber |
US8925354B2 (en) * | 2009-11-04 | 2015-01-06 | Corning Incorporated | Methods for forming an overclad portion of an optical fiber from pelletized glass soot |
US9873629B2 (en) * | 2011-06-30 | 2018-01-23 | Corning Incorporated | Methods for producing optical fiber preforms with low index trenches |
US9108876B2 (en) * | 2011-11-30 | 2015-08-18 | Corning Incorporated | Pressed, multilayered silica soot preforms for the manufacture of single sinter step, complex refractive index profile optical fiber |
US9487428B2 (en) * | 2015-03-06 | 2016-11-08 | Ofs Fitel, Llc | Easy removal of a thin-walled tube in a powder-in-tube (PIT) process |
CN108117254A (en) * | 2017-12-29 | 2018-06-05 | 江苏通鼎光棒有限公司 | A kind of casing prefabricated rods and its manufacturing method |
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Publication number | Priority date | Publication date | Assignee | Title |
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EP0718244A2 (en) * | 1994-12-20 | 1996-06-26 | Corning Incorporated | Method of making optical fiber having depressed index core region |
CN107082558A (en) * | 2017-04-27 | 2017-08-22 | 烽火通信科技股份有限公司 | Method for manufacturing the preform of single-mode fiber and manufacturing single-mode fiber |
CN107098578A (en) * | 2017-04-27 | 2017-08-29 | 烽火通信科技股份有限公司 | Method for manufacturing the preform of sandwich construction optical fiber and manufacturing optical fiber |
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