CN106495463B - Method for preparing composite optical fiber with optical crystal or ceramic as core material and quartz as cladding - Google Patents
Method for preparing composite optical fiber with optical crystal or ceramic as core material and quartz as cladding Download PDFInfo
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- CN106495463B CN106495463B CN201610885073.2A CN201610885073A CN106495463B CN 106495463 B CN106495463 B CN 106495463B CN 201610885073 A CN201610885073 A CN 201610885073A CN 106495463 B CN106495463 B CN 106495463B
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- core material
- quartz
- preform
- optical fiber
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Classifications
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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
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
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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
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
- C03C13/046—Multicomponent glass compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/30—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi
- C03B2201/34—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers
- C03B2201/36—Doped silica-based glasses doped with metals, e.g. Ga, Sn, Sb, Pb or Bi doped with rare earth metals, i.e. with Sc, Y or lanthanides, e.g. for laser-amplifiers doped with rare earth metals and aluminium, e.g. Er-Al co-doped
Abstract
A method for preparing a composite optical fiber with optical crystal or ceramic as a core material and quartz as a cladding comprises the following steps: (1) processing the optical crystal or ceramic into a core material, so that the core material can be plugged into an inner hole of a hollow quartz preform, and cleaning and drying the core material; (2) processing a hollow quartz preform, and clamping the hollow quartz preform on a drawing tower by a long preform side clamping method, a reaming glass tube connecting method or a glass tube connecting and funnel connecting method; (3) and raising the temperature in the wire drawing furnace to be higher than the wire drawing temperature of the quartz glass and the melting point of the core material, and simultaneously drawing the composite optical fiber containing the core material while putting the core material into the hollow quartz preform rod being drawn. The on-line feeding method is simple and convenient to operate, the reaction time of the core material and the quartz cladding in the wire drawing process is short, and the problem of serious silica diffusion in the traditional melting core method is solved. The prepared optical fiber rare earth has high doping concentration and wide application range of the core material, and provides a new method for the development of composite optical fibers.
Description
Technical Field
The invention relates to a functional optical fiber, in particular to a preparation method of a composite optical fiber taking optical crystal or ceramic as a core material and quartz glass as a cladding.
Background
With the development of science and the demand of society, the application of optical fibers has been expanded from communication to a plurality of fields such as laser and sensing, and various functional optical fibers have come into play. In recent years, composite optical fibers are developed based on the combination of the drawability of glass and the functional characteristics of crystal and ceramic materials, the superior performance of various materials is exerted, and materials which cannot be drawn or are not suitable for drawing are drawn into optical fibers, such as crystal materials, ceramic materials and semiconductor materials, so that the functional characteristics and the application field of the optical fiber materials are expanded, and the optical fibers are becoming novel functional optical fiber materials.
The existing manufacturing methods of the composite optical fiber comprise a high-pressure chemical vapor deposition method, a laser heating base common-drawing method, a molten core and the like, and the optical fiber manufactured by the former two methods has high component purity, but has the defects of complex manufacturing process and short manufacturing length. The existing core melting method has two forms, namely a traditional tube-rod method and a powder-tube method, namely, a crystal core rod or powder is sealed in a glass tube, the glass tube is placed in a high-temperature furnace and heated until a core material is melted and cladding glass is softened, and then an optical fiber is drawn. Due to the requirement of the core cladding ratio of the optical fiber, the ratio of the outer diameter of the quartz tube to the aperture is 8-10, and the outer diameter is close to 20 mm. The large outer diameter results in a relatively long turn-around time of the preform, inevitable reaction of the liquid melted core with the softened quartz cladding, and a particularly rapid rate of such reaction. The silica of the cladding diffuses into the core material in a large amount, so that the composition of the core material is changed, the structure and the coordination field of the original material are damaged, the optical performance of the core material is damaged, and the performance of the obtained optical fiber is far different from that required by design.
Disclosure of Invention
The invention provides a method for preparing a composite optical fiber with an optical crystal and a quartz glass cladding taking ceramic as core materials, aiming at the existing method for drawing a fused core optical fiber. The method is also called an on-line feeding method, and has the key points that the on-line feeding operation is simple and convenient, the reaction time of the core material and the quartz cladding in the wire drawing process is short, and the problem of serious silica diffusion in the traditional molten core method is solved. The prepared optical fiber rare earth has high doping concentration and wide application range of the core material, and provides a new method for the development of composite optical fibers.
The technical solution of the invention is as follows:
a method for preparing a composite optical fiber with optical crystal or ceramic as a core material and quartz as a cladding, also called an on-line feeding method, is characterized by comprising the following steps:
(1) processing the optical crystal or ceramic into a core material, so that the core material can be plugged into an inner hole of a hollow quartz preform, and cleaning and drying the core material;
(2) processing a hollow quartz preform, and clamping the hollow quartz preform on a drawing tower by a long preform side clamping method, a reaming glass tube connecting method or a glass tube connecting and funnel connecting method;
(3) and raising the temperature in the wire drawing furnace to be higher than the wire drawing temperature of the quartz glass and the melting point of the core material, and simultaneously drawing the composite optical fiber containing the core material while putting the core material into the hollow quartz preform rod being drawn.
The core material comprises optical crystals or ceramics of yttrium aluminum garnet, aluminum oxide, yttrium oxide or spinel which are not doped with rare earth or doped with rare earth.
The long preform method side clamping method is that when the hollow preform is clamped on a drawing tower, an inner hole on the upper end surface is not blocked and is communicated with the outside.
The method for connecting the glass tube by reaming is to ream the upper end of the hollow quartz prefabricated rod and connect the end with another glass tube.
The glass receiving tube and funnel method is characterized in that the upper end of the hollow quartz prefabricated rod is connected with another glass tube, and the thin opening of a funnel is opposite to the inner hole at the upper end of the hollow quartz prefabricated rod.
The invention has the following advantages:
1, the operation is simple and convenient, and the cost is low;
2 the core material has wide selectable range.
3, the method is also called an on-line feeding method, the contact reaction time of the core material and the quartz cladding is short, the diffusion concentration of the silicon dioxide is low, and the functional characteristic of the core material is slightly changed;
4, because the practical use length of the functional optical fiber is short, even if the optical fiber has a core discontinuous part, a continuous optical fiber section with enough length can be selected to meet the requirement; the continuous fiber is typically selected to be longer than that produced by high pressure chemical vapor deposition, laser heated pedestal co-drawing.
Drawings
FIG. 1 is a schematic drawing of an optical fiber in a state of being drawn according to embodiment 1 of a method for manufacturing a composite optical fiber in which an optical crystal or ceramic is used as a core and silica glass is used as a cladding.
FIG. 2 is a schematic view of the preform tube-in-hole machining method of example 2 of the present invention.
FIG. 3 is a schematic view of the preform tube-to-glass tube and funnel processing of example 3 of the present invention.
FIG. 4 is a graph showing the composition distribution of an optical fiber according to example 1 of the present invention in comparison with a conventional Faraday method, wherein (a) is an in-line feeding method according to the present invention and (b) is a conventional method.
FIG. 5 is a distribution diagram of optical fiber components according to example 2 of the present invention.
Wherein 1 is a hollow quartz preform; 2 is a core material; 3 is a core melt; 4 is a composite optical fiber containing a core material; 5 is a graphite furnace of a wire drawing machine; 6 is a glass tube; 7 is the preform reaming position; 8 is a funnel; and 9 is a clamping fixture.
Detailed Description
The invention is further illustrated with reference to the following examples and figures, without thereby limiting the scope of protection of the invention.
Example 1
YAG transparent ceramic is cut and polished into granules with an outer diameter of about 2mm, preferably surface polished, then washed with dilute hydrochloric acid and deionized water, and dried. FIG. 1 is a schematic drawing of an optical fiber in a state of being drawn according to example 1 of the present invention. Selecting a hollow quartz preform 1 of a quartz tube with the length of 600mm, the outer diameter of 25mm and the inner diameter of 3.5mm, preferably cleaning, and plugging an inner hole at the lower end of the hollow quartz preform 1 by using a section of conical quartz rod to extend into a graphite furnace 5 of a wire drawing machine; the side surface of the upper end is clamped on the quartz optical fiber drawing tower through a clamping fixture 9, and the upper end surface of the hollow quartz prefabricated rod is leaked. And raising the temperature of the graphite furnace until the quartz tube is softened, dropping the lower head, starting to draw the hollow optical fiber, when the outer diameter of the optical fiber is adjusted to 200 mu m, putting one particle of YAG (yttrium aluminum oxide) particle 2 into the inner hole of the upper end face every 6min, enabling the core material particle 2 to fall into the lower part of the quartz tube which is drawn into a cone, melting the core material particle into a melt 3 at high temperature, and filling the melt into the inner hole of the quartz tube to form the yttrium aluminum silicon oxide core/quartz cladding composite optical fiber 4. And after the optical fiber is drawn, selecting the optical fiber containing the core material.
The drawn fiber was analyzed for composition by SEM test, and fig. 4 is a composition element distribution diagram of example 1 of the present invention compared with a conventional drawn fiber. It can be seen from the figure that the diffusion of silica in the core of the optical fiber prepared by the method of the present invention is reduced from 74 wt.% to 45 wt.% compared to the conventional method.
Example 2
Yb of2O3YAG transparent ceramic mixed with Yb 15 at.%, and cutting and polishing into 2mm long and external diameter0.5mm strip, polished surface, then washed with dilute hydrochloric acid and deionized water, and dried. One end of a thick-walled quartz tube of 10cm in length is reamed to form a reamed portion 7, and the end is connected to another thin-walled quartz tube to form a hollow preform shown in FIG. 2, which is drawn into a hollow optical fiber having an outer diameter of 170 μm, the temperature in the furnace is raised to 2000 ℃, and a core material is placed from the upper portion of the thin-walled quartz tube 6 every 3-5 min. Drawing to obtain Yb-doped yttrium aluminum silicon oxide core/quartz cladding composite optical fiber. FIG. 5 is a distribution diagram of optical fiber components according to example 2 of the present invention.
Example 3
The sapphire is cut and polished into strips with the length of 3mm and the outer diameter of 0.2mm, and then the strips are washed by deionized water and dried. A thick-walled quartz tube 50cm in length was connected to another thin-walled quartz tube with a funnel 8 interposed therebetween to constitute a hollow preform shown in FIG. 3, the temperature in the furnace was raised to 2200 ℃ to draw a hollow optical fiber having an outer diameter of 80 μm, and a core material was put from the thin-walled quartz tube 6 every 3 min. Drawing the quartz clad composite fiber with high alumina core.
Example 4
The Yb-doped transparent yttrium oxide ceramic and the Tm-Ho co-doped YAG are cut and polished into strips with the length of 3mm and the outer diameter of 0.2 mm. One end of a thick-walled quartz tube having a length of 20cm was enlarged and connected to the thin-walled quartz tube having a hole bored at the other side, to constitute a hollow preform. The temperature in the furnace is raised to be higher than 2100 ℃, the prefabricated rod is drawn into a hollow optical fiber with the outer diameter of 125 mu m, and 1 grain of yttrium oxide and 2 grains of YAG core material are put into the side hole of the thin-wall quartz tube. And drawing the Tm Ho Yb co-doped quartz cladding composite fiber.
Example 5
The YAG ceramics doped with Nd, alumina crystal and Yb-Ce are cut and polished into strips with the length of 3mm and the outer diameter of 0.1mm, and the strips are cleaned and dried. One end of a section of thick-wall quartz tube with the length of 80cm and the inner diameter of 2mm is extended into a graphite furnace; the side surface of the other end is clamped on the quartz optical fiber drawing tower, and the upper end surface of the quartz optical fiber drawing tower is leaked. And raising the temperature of the graphite furnace to 2100 ℃, drawing the hollow optical fiber, and putting 1 particle of each of the processed Nd: YAG crystal and YbCE: YAG ceramic into an inner hole on the upper end surface of the quartz tube to form the Nd, Ce and Yb co-doped composite optical fiber.
Example 6
Cutting and polishing spinel, alumina crystals and Er-doped YAG ceramic into strips with the length of 3mm and the outer diameter of 0.3mm, cleaning with deionized water, and drying. One end of a thick-wall quartz tube with the length of 80cm and the inner diameter of 4mm is plugged with a section of conical quartz rod with the length of 1cm and extends into the graphite furnace; the side surface of the other end is clamped on the quartz optical fiber drawing tower, and the upper end surface of the quartz optical fiber drawing tower is leaked. And raising the temperature of the graphite furnace to 2300 ℃ to soften the quartz tube, dropping the lower head, drawing the hollow optical fiber, and putting 1 grain of each of the processed spinel, the alumina crystal and the Er-doped YAG ceramic into an inner hole on the upper end face of the quartz tube to form the Er-doped composite optical fiber.
Claims (4)
1. A method for preparing a composite optical fiber with optical crystal or ceramic as a core material and quartz as a cladding is characterized by comprising the following steps:
(1) processing the optical crystal or ceramic into a core material, so that the core material can be plugged into an inner hole of a hollow quartz preform, and cleaning and drying the core material; the core material comprises optical crystals or ceramics of yttrium aluminum garnet, aluminum oxide, yttrium oxide or spinel which are not doped with rare earth or doped with rare earth;
(2) processing a hollow quartz preform, and clamping the hollow quartz preform on a drawing tower by a long preform side clamping method, a reaming glass tube connecting method or a glass tube connecting and funnel connecting method;
(3) and raising the temperature in the wire drawing furnace to be higher than the wire drawing temperature of the quartz glass and the melting point of the core material, and simultaneously drawing the composite optical fiber containing the core material while putting the core material into the hollow quartz preform rod being drawn.
2. The method of claim 1, wherein the long preform side clamping method is a method in which the inner hole of the upper end surface is not blocked and communicates with the outside when the hollow silica preform is clamped on the drawing tower.
3. The method for preparing a composite optical fiber with optical crystal or ceramic as core and quartz as cladding according to claim 1, characterized in that the method of reaming and connecting glass tube is to ream the upper end of the hollow quartz preform (1) and connect the end with another glass tube (6).
4. The method of claim 1, wherein the glass tube and funnel method is used to connect another glass tube to the upper end of the hollow silica preform, and the narrow opening of a funnel (8) is placed opposite to the inner hole of the upper end of the hollow silica preform.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610885073.2A CN106495463B (en) | 2016-10-11 | 2016-10-11 | Method for preparing composite optical fiber with optical crystal or ceramic as core material and quartz as cladding |
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| CN201610885073.2A CN106495463B (en) | 2016-10-11 | 2016-10-11 | Method for preparing composite optical fiber with optical crystal or ceramic as core material and quartz as cladding |
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| CN106495463B true CN106495463B (en) | 2019-12-20 |
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| CN107739152B (en) * | 2017-11-10 | 2020-06-02 | 上海欧感电气技术有限公司 | Intelligent heating device with adjusting function for optical fiber drawing |
| CN108411359B (en) * | 2018-02-27 | 2020-11-27 | 同济大学 | Method for growing crystal cladding in metal tube |
| CN108706865A (en) * | 2018-05-16 | 2018-10-26 | 上海大学 | A kind of more matrix method for preparing optical fiber of silica clad stick cored structure |
| CN108929032B (en) * | 2018-07-26 | 2021-08-31 | 杭州富通通信技术股份有限公司 | Optical fiber processing method |
| CN109143459B (en) * | 2018-09-04 | 2019-12-27 | 同济大学 | Cladding method of rare earth ion doped low-temperature garnet crystal bar |
| CN110294595B (en) * | 2019-06-10 | 2020-07-10 | 华中科技大学 | Miniaturized functional fiber drawing equipment |
| CN112851127B (en) * | 2021-01-16 | 2021-11-02 | 威海长和光导科技有限公司 | High-gain Ho3+/Tm3+/Yb3+Co-doped quartz optical fiber and preparation method thereof |
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| CN101328012A (en) * | 2007-06-21 | 2008-12-24 | 江苏亨通光纤科技有限公司 | Large size rock quartz optical fibre prefabricated bar manufacturing method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100378595B1 (en) * | 2000-08-22 | 2003-03-31 | 한국전자통신연구원 | Fabrication Method Of Fiber Preform via Melting Process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1884165A (en) * | 2006-06-30 | 2006-12-27 | 浙江富通光纤技术有限公司 | Method for preparing optical fiber by large-sized low-water-peak optical fiber preform and dedicated device therefor |
| CN101328012A (en) * | 2007-06-21 | 2008-12-24 | 江苏亨通光纤科技有限公司 | Large size rock quartz optical fibre prefabricated bar manufacturing method |
| CN102285758A (en) * | 2011-08-01 | 2011-12-21 | 江苏亨通光电股份有限公司 | Production method for large-size optical fiber prefabricated rod |
| CN203558972U (en) * | 2013-11-11 | 2014-04-23 | 江苏亨通光电股份有限公司 | Device for stretching optical fiber preform |
| CN104261670A (en) * | 2014-09-22 | 2015-01-07 | 江苏亨通光电股份有限公司 | Method for manufacturing optical fiber |
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