CN1187629C - Method of manufacturing high-performance ultraviolet optical fiber - Google Patents

Method of manufacturing high-performance ultraviolet optical fiber Download PDF

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Publication number
CN1187629C
CN1187629C CNB031155103A CN03115510A CN1187629C CN 1187629 C CN1187629 C CN 1187629C CN B031155103 A CNB031155103 A CN B031155103A CN 03115510 A CN03115510 A CN 03115510A CN 1187629 C CN1187629 C CN 1187629C
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China
Prior art keywords
optical fiber
ultraviolet light
ultraviolet
prefabricated rod
rod
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Expired - Fee Related
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CNB031155103A
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Chinese (zh)
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CN1455274A (en
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王廷云
陈振宜
郭强
沈育青
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Shanghai University
University of Shanghai for Science and Technology
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University of Shanghai for Science and Technology
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Priority to CNB031155103A priority Critical patent/CN1187629C/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01Manufacture of glass fibres or filaments
    • C03B37/012Manufacture of preforms for drawing fibres or filaments
    • C03B37/01205Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Surface Treatment Of Glass Fibres Or Filaments (AREA)
  • Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)

Abstract

The present invention relates to a method for manufacturing high-performance ultraviolet optical fibers, which belongs to the technical field of the manufacturing technology of optical glass fibers. The method of the present invention comprises the following steps: (1), an ultraviolet optical fiber preforming rod is made; 2), the optical fiber preforming rod is processed by ultraviolet light immunity radiation; (3), the optical fiber preforming rod enters a wire drawing operating system, and optical fiber heat processing is carried out to optical fiber preforming rod; (4), the optical fiber preforming rod is coated with coating and is heated and solidified. The method of the present invention proposes an immunity manufacturing technique for ultraviolet optical fibers, namely that firstly, ultraviolet light deliberately irradiates quartz glass materials for causing quartz glass materials to generating color center defects and multi-layer structure monstrosities; afterwards, a heat processing method is used for eliminating the defects; thereby, the ultraviolet light resisting capability of optical fibers are increased. The present invention eliminates the blocking effect of quartz glass optical fibers on ultraviolet light to a certain extent, and thereby, the present invention enhances the transmission capability of ultraviolet light in quartz optical fibers.

Description

Method for manufacturing high-performance ultraviolet optical fiber
Technical Field
The invention relates to a manufacturing method of a high-performance ultraviolet optical fiber, belonging to the technical field of manufacturing processes of optical glass fibers.
Background
The ultraviolet laser has the characteristics of short wavelength, high energy, no thermal effect, direct bond breaking through interaction with substances and the like. The ultraviolet laser is transmitted by the optical fiber, and can be introduced to a complex remote working target, so that the application range of the ultraviolet laser is greatly expanded. For example, with the use of ultraviolet optical fibers, ultraviolet quenching resin curing, mechanical micromachining and manufacturing, medical treatment, grating manufacturing, ultraviolet probing, environmental protection, and the like can be performed.
When an optical fiber is used for transmitting ultraviolet light, the ultraviolet light with short wavelength and high energy is required to be transmitted in many occasions, but when the ultraviolet light with short wavelength and high energy is transmitted in the quartz optical fiber, due to the action of the ultraviolet light and the quartz glass, color center defects are generated in the quartz glass, so that the structural change is generated, the transmission of the ultraviolet light is prevented, the loss is increased, and the transmission performance of the ultraviolet light is greatly reduced. When a standard high OH-The transmission performance of the ultraviolet silica fiber, after being continuously irradiated with an unfiltered deuterium lamp for 24 hours, is reduced by about 50%. The shorter the wavelength of the ultraviolet light and the higher the power, the more prominent this problem of reducing the transmission performance of the ultraviolet light, which may be referred to as the fiber ultraviolet suppression effect. Therefore, when an excimer laser is used as a light source, the transmission performance of the silica fiber is varied, particularly in the KrF excimer laser (wavelength: 248nm), F2Excimer lasers (wavelength: 157nm), ArF excimer lasers (wavelength: 193nm), and the like are more prominent as light sources.
In order to overcome the defect of the transmission performance variation of ultraviolet light in the silica glass optical fiber or improve the stopping effect of the silica glass optical fiber on the ultraviolet light, at present, when manufacturing the high-performance ultraviolet silica glass optical fiber, the following two methods are mainly adopted:
(1) the hydroxyl content (more than 500ppm) is increased in the quartz glass optical fiber core. However, in this method, when the hydroxyl group content is increased, the wavelength of the ultraviolet absorption edge is lengthened, and as a result, ultraviolet light of short wavelength (particularly, vacuum ultraviolet region) cannot be transmitted in the optical fiber. In addition, it is not the case that the higher the hydroxide content, the better the effect, but the improvement capability is limited, and when the hydroxide content is higher than a certain value (e.g., 2000ppm), the loss thereof is increased.
(2) Hydrogen loading in UV optical fibers also improves the transmission of short wavelength, high energy UV light through the fiber, however, hydrogen loading requires 1019cm-3The concentration of hydrogen gas, which can be completed only in a high-pressure container for several weeks, not only has large investment and long time, but also can cause a part of hydrogen-carrying gas to escape from the optical fiber due to environmental changes such as temperature and the like, and still can reduce the transmission performance of the optical fiber.
Disclosure of Invention
The invention aims to overcome the defect of transmission performance variation of ultraviolet light in a quartz glass optical fiber and improve the effect of the quartz glass optical fiber on preventing the ultraviolet light. Another objective of the present invention is to provide a high-performance uv optical fiber immune manufacturing technique, which addresses the problems in the prior art.
The purpose of the invention is realized by the following means:
the immune manufacturing technology is that ultraviolet light is used to deliberately irradiate quartz glass material to generate color center defect and multilayer structure variation, namely 'inoculation' color center defect; then, the heat treatment method is used for eliminating the defects, and the ultraviolet light resisting capability of the optical fiber is increased, so that the ultraviolet optical fiber has immunity when transmitting ultraviolet light with short wavelength and high energy, namely, serious defects can not occur.
However, there is a problem in how to irradiate the ultraviolet light in the above-mentioned ultraviolet light pre-irradiation. When one end face of the optical fiber is repeatedly irradiated with high-power ultraviolet light, structural defects are caused, which occur only at the irradiated end face, and the ultraviolet light cannot reach the other end face. Therefore, it is impossible to produce a long optical fiber except for a short optical fiber. If the low power uv light is used, the treatment time will be too long, which is not practical. Furthermore, if the finished optical fiber is laterally irradiated with ultraviolet light, the insulating coating layer formed of synthetic resin is melted by heating with ultraviolet light, and this irradiation causes damage to the ultraviolet optical fiber. For this reason, not the ultraviolet optical fiber but the ultraviolet optical fiber preform irradiated with ultraviolet light is used in the present invention, and then the silica optical fiber preform is drawn in a drawing operation system while being subjected to a heating treatment.
The method of the invention is characterized in that the ultraviolet light is used for pre-irradiating the quartz optical fiber preform and the quartz optical fiber manufactured by the preform is subjected to the thermal treatment.
The principle of the method of the invention is as follows:
in the method of the present invention, a silica glass optical fiber preform is irradiated with ultraviolet light in advance to make SiO in a silica glass material2In the initial structure (equivalent to Si-O-Si equivalent) and the initial defect particles (equivalent to Si-Si equivalent, and equivalent to Si-O-O-Si equivalent), multilayer structure variation and color center defects such as E 'color center (equivalent to Si) and NBOH color center (equivalent to Si-O.) are generated, and then the quartz glass material is subjected to heat treatment while being drawn by drawing by heat generated when the ultraviolet optical fiber is drawn by a drawing machine heating furnace, and a part of Si-O broken bonds during the heat treatment is recovered, so that the E' color center and NBOH color center defects are eliminated, namely (ii) a In addition, the average valence bond angle of the ≡ Si-O-Si ≡ network structure of the quartz glass material after heat treatment is larger than that of the quartz glass material before heat treatment, and the relaxation of the structure also provides a stable structural form for the quartz glass material, so that when the quartz glass material is irradiated by ultraviolet light again, the structure defects are prevented from being generated again, the immunity function is achieved, and the transmission performance of the ultraviolet light is improved.
The invention relates to a method for manufacturing a high-performance ultraviolet optical fiber, which is characterized by comprising the following steps of:
a. manufacturing an ultraviolet optical fiber preform: making UV fiber preforms by modified chemical vapor depositionSiCl is introduced into the quartz glass tube4、POCl3、C2F6、BBr3A compound of formula (I) and H2、O2The gases are mixed together and subjected to a chemical vapor reaction at elevated temperature to form soot in the tube, which soot forms SiO2、P2O5、B2O3The powdered oxide is deposited on the inner wall of the quartz tube and, in addition, OH is also present in the rod core-Generating; then raising the temperature to heat the quartz tube to about 2000 ℃ for collapsing the quartz tube containing the deposition layer into a solid prefabricated rod; the diameter of the prefabricated rod is 9-15 mm;
b. ultraviolet light immune irradiation treatment of the optical fiber preform: the preform is first deliberately irradiated with UV light and allowed to standGenerating multilayer structure variation and color center defects, placing the prefabricated rod on a rotating device, wherein the axis of the rotating device rotates along the axis of the prefabricated rod, so that ultraviolet light at the end can uniformly irradiate the whole prefabricated rod; the irradiation wavelength of the ultraviolet light is between 100 and 250nm, and the irradiation energy of the ultraviolet light to the preform is between 10 and 60mJ/cm2Within the range;
c. and (3) entering a wire drawing operation system and carrying out heat treatment on the optical fiber: placing the optical fiber preform subjected to ultraviolet light immune irradiation treatment into a clamping device, slowly feeding the optical fiber preform into a heating furnace, drawing and drawing the optical fiber by a traction wheel drawing machine, and simultaneously performing heat treatment on the optical fiber by utilizing heat generated by the heating furnace, wherein the drawing and the heat treatment are performed simultaneously, and the drawing temperature is 1600-2000 ℃;
d. optical fiber coating and heating curing: the method is carried out in the same wire drawing operation system, the optical fiber is coated with epoxy acrylic resin coating material through a coating cup and enters a curing furnace for heating and curing, and finally the ultraviolet quartz glass optical fiber is prepared.
The method has the advantages and effects that the optical fiber has higher ultraviolet optical fiber transmission performance, the output energy is obviously improved compared with the conventional optical fiber without immune treatment, the transmission is stable, the manufacturing is simple, and the realization is easy. In addition, the method of the invention is carried out in a conventional wire drawing operation system without adding traditional equipment, thereby being beneficial to the production of optical fibers and saving the cost.
Detailed Description
The first embodiment is as follows: now, the embodiment of the method of the present invention will be described, and the method of manufacturing a high performance ultraviolet optical fiber of the present invention is characterized by including the following steps:
a. manufacturing an ultraviolet optical fiber preform: making ultraviolet optical fiber preform by Modified Chemical Vapor Deposition (MCVD), introducing SiCl into quartz glass tube4、POCl3、C2F6、BBr3A compound of formula (I) and H2、O2The gases are mixed together and subjected to a chemical vapor reaction at elevated temperature to form soot in the tube, which soot forms SiO2、P2O5、B2O3The powdered oxide is deposited on the inner wall of the quartz tube and, in addition, OH is also present in the rod core-Generating; then raising the temperature to heat the quartz tube to about 2000 ℃ for collapsing the quartz tube containing the deposition layer into a solid prefabricated rod; the diameter of the preform is 9-15 mm.
b. Ultraviolet light immune irradiation treatment of the optical fiber preform: the method comprises the following steps of firstly, deliberately irradiating a prefabricated rod by ultraviolet light to cause the prefabricated rod to generate multilayer structure variation and color center defects, placing the prefabricated rod on a rotating device, and enabling the axis of the prefabricated rod to rotate along the axis of the prefabricated rod so that the ultraviolet light at the end part can uniformly irradiate the whole prefabricated rod; the irradiationwavelength of the ultraviolet light is between 100 and 250nm, and the irradiation energy of the ultraviolet light to the preform is between 10 and 60mJ/cm2Within the range.
The irradiation of ultraviolet light needs to be continuous, the irradiation time needs to be matched with the irradiation wavelength and intensity parameters, the wavelength is short, the energy is large, the required irradiation time can be short, and the irradiation time is dozens of minutes. In order to achieve good illumination of the entire rod, the preform is preferably less than 1 meter and is illuminated at both ends.
Usable ultraviolet light source F2(157nm), ArF (193nm), KrF (248nm) excimer lasers, deuterium lamps, mercury lamps, etc. may be used.
c. And (3) entering a wire drawing operation system and carrying out heat treatment on the optical fiber: placing the optical fiber preform subjected to ultraviolet light immune irradiation treatment into a clamping device, slowly feeding the optical fiber preform into a heating furnace, drawing the drawn fiber by a traction wheel, and simultaneously carrying out heat treatment on the optical fiber by using heat generated by the heating furnace, wherein the drawing and the heat treatment are carried out simultaneously, and the drawing temperature is 1600-2000 ℃;
d. optical fiber coating and heating curing: the method is carried out in the same wire drawing operation system, the optical fiber is coated with epoxy acrylic resin coating material through a coating cup and enters a curing furnace for heating and curing, and finally the ultraviolet quartz glass optical fiber is prepared.
The method is not only suitable for the manufacture of the quartz glass, but also suitable for the manufacture of multi-component glass and plastic silicon-coated core ultraviolet opticalfibers.

Claims (2)

1. A manufacturing method of a high-performance ultraviolet optical fiber is characterized by comprising the following steps:
a. manufacturing an ultraviolet optical fiber preform: the ultraviolet optical fiber preform is made by modified chemical vapor deposition method, i.e. SiCl is introduced into quartz glass tube4、POCl3、C2F6、BBr3A compound of formula (I) and H2、O2The gases are mixed together and subjected to a chemical vapor reaction at elevated temperature to form soot in the tube, which soot forms SiO2、P2O5、B2O3The powdered oxide is deposited on the inner wall of the quartz tube and, in addition, OH is also present in the rod core-Generating; then raising the temperature to heat the quartz tube to about 2000 ℃ for collapsing the quartz tube containing the deposition layer into a solid prefabricated rod; the diameter of the prefabricated rod is 9-15 mm;
b. ultraviolet light immune irradiation treatment of the optical fiber preform: the method comprises the following steps of firstly, deliberately irradiating a prefabricated rod by ultraviolet light to cause the prefabricated rod to generate multilayer structure variation and color center defects, placing the prefabricated rod on a rotating device, and enabling the axis of the prefabricated rod to rotate along the axis of the prefabricated rod so that the ultraviolet light at the end part can uniformly irradiate the whole prefabricated rod; the irradiation wavelength of the ultraviolet light is between 100 and 250nm, and the irradiation energy of the ultraviolet light to the preform is between 10 and 60mJ/cm2Within the range;
c. and (3) entering a wire drawing operation system and carrying out heat treatment on the optical fiber: placing the optical fiber preform subjected to ultraviolet light immune irradiation treatment into a clamping device, slowly feeding the optical fiber preform into a heating furnace, drawing and drawing the optical fiber by a traction wheel drawing machine, and simultaneously performing heat treatment on the optical fiber by utilizing heat generated by the heating furnace, wherein the drawing and the heat treatment are performed simultaneously, and the drawing temperature is 1600-2000 ℃;
d. optical fiber coating and heating curing: the method is carried out in the same wire drawing operation system, the optical fiber is coated with epoxy acrylic resin coating material through a coating cup and enters a curing furnace for heating and curing, and finally the ultraviolet quartz glass optical fiber is prepared.
2. The method of claim 1, wherein the method is applied to the manufacture of the high-performance UV optical fiber, such as the silica glass, the multicomponent glass, and the silicon-on-plastic core.
CNB031155103A 2003-02-25 2003-02-25 Method of manufacturing high-performance ultraviolet optical fiber Expired - Fee Related CN1187629C (en)

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Publication number Priority date Publication date Assignee Title
CN1317573C (en) * 2004-10-27 2007-05-23 上海大学 Ultraviolet optical fiber with high-transmission ability and producing method thereof, and deposition apparatus containing high-hydroxyl optical fibre prefabricated bar
CN102185252B (en) * 2011-03-15 2012-10-10 中国科学技术大学 Method for packaging single NV color center

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