CN114044627A - Method for preventing core element volatilization of rare earth ion-doped optical fiber preform - Google Patents
Method for preventing core element volatilization of rare earth ion-doped optical fiber preform Download PDFInfo
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- CN114044627A CN114044627A CN202111504626.2A CN202111504626A CN114044627A CN 114044627 A CN114044627 A CN 114044627A CN 202111504626 A CN202111504626 A CN 202111504626A CN 114044627 A CN114044627 A CN 114044627A
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 28
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 25
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 72
- 239000010453 quartz Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000012792 core layer Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 37
- 239000007787 solid Substances 0.000 claims description 12
- 239000002994 raw material Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 238000003466 welding Methods 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 3
- 239000010439 graphite Substances 0.000 claims description 3
- 239000002912 waste gas Substances 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 14
- 230000008021 deposition Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract 1
- -1 rare earth ion Chemical class 0.000 description 6
- 238000000151 deposition Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 210000001503 joint Anatomy 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C03B37/012—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]
- C03B37/018—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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
-
- 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]
- C03B37/018—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] by glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01853—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General 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)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The invention discloses a method for preventing core element volatilization of a rare earth ion-doped optical fiber preform, which comprises the steps of preparing the rare earth ion-doped optical fiber preform by adopting MCVD technology, and after the deposition of the core layer of the optical fiber preform prepared by MCVD is finished, burning out a section of quartz column with the length of about 2 cm from a reaction tube at a position of 1cm at a position of a port of the reaction tube connected with a tail gas end, and completely sealing a channel between the reaction tube and the tail gas end. Therefore, when the high-temperature rod is contracted for many times, elements in the core part of the prefabricated rod can not be discharged along with the carried gas after high-temperature volatilization, and can be remained in the reaction tube for continuous reaction and deposition, so that the problems of uneven fiber core doping of the prefabricated rod and low central doping element caused by element volatilization are effectively prevented, and the longitudinal and transverse uniformity of the fiber core doping element is ensured.
Description
Technical Field
The invention relates to the technical field of optical fiber manufacturing, in particular to a method for preventing core elements of a rare earth ion-doped optical fiber preform from volatilizing.
Background
The MCVD process is the most commonly used method in the process of manufacturing an optical fiber preform, and the method includes depositing on the inner wall of a quartz tube to manufacture a desired optical fiber preform, and then performing desired processing and drawing on the optical fiber preform to manufacture a desired optical fiber. In the process of preparing an optical fiber preform, particularly in the process of performing high-temperature rod shrinkage and rod contraction after the deposition of a core layer is finished, because the temperature is high (more than 2000 ℃), elements of a deposited fiber core can volatilize at high temperature, so that the central concentration of doping elements of the prepared fiber core of the optical fiber is low and even lost, and particularly for rare earth ion-doped optical fibers, if the doping elements of the fiber core are not uniformly doped, the optical fiber laser is low in efficiency, generates heat and even burns out when high-power laser is applied. At present, the traditional treatment method is to supplement a part of core elements to compensate the loss during the rod shrinkage, but for the rare earth ion doped optical fiber, the rare earth elements cannot be supplemented, so the loss of the rare earth ions in the center of the fiber core of the rare earth ion doped optical fiber is an important factor influencing the performance of the optical fiber. How to prevent the element volatilization loss during the rod shrinkage becomes an important research subject for preparing the rare earth ion doped optical fiber.
Disclosure of Invention
In view of the state of the art and the deficiencies of the prior art, the present invention provides a method for preventing volatilization of core elements of a rare earth ion doped optical fiber preform. The method can avoid the defect that the rare earth element at the center of the fiber core is lost because the volatilization of the rare earth element cannot be supplemented in the traditional MCVD core supplementing method, and can effectively prevent the problem of the loss of the rare earth element at the center of the fiber core caused by high-temperature volatilization in the preparation process of the rare earth ion doped optical fiber preform.
The technical scheme adopted by the invention for realizing the purpose is as follows: a method for preventing the volatilization of core elements of a rare earth ion-doped optical fiber preform is characterized by comprising the following steps:
selecting a quartz tube as a reaction tube and carrying out acid washing pretreatment.
And step two, selecting quartz tubes with the same diameter and wall thickness as the reaction tubes as an air inlet tube and a waste tube according to the selected diameters of the reaction tubes, and selecting quartz tubes with the diameter and the wall thickness larger than those of the reaction tubes as tail gas tubes.
Fixing one end of the air inlet pipe on an air inlet end fixing clamp of the MCVD system, welding the tail end of the air inlet pipe and one end of the reaction pipe, and ensuring the alignment of the air inlet pipe and the reaction pipe in the sintering process; fix exhaust pipe one end on the exhaust pipe fixing clamp of MCVD system to with the sealed fixing device cover of exhaust pipe of MCVD device at the afterbody of the exhaust pipe other end, carry out the high temperature with the reaction tube other end and soften, use graphite instrument with the reaction tube other end diameter expand to match with the exhaust pipe, with reaction tube and exhaust pipe butt fusion.
And step four, connecting the tail gas pipe into a tail gas exhaust system of the MCVD system.
And step five, after the MCVD system is started, the carrier gas and the reaction raw materials enter the reaction tube through the air inlet tube and react, and the unreacted gas, the unreacted raw materials, and the waste gas and impurities generated after the reaction in the reaction tube enter the tail gas exhaust system under the pressure action and are exhausted through the tail gas exhaust pipeline.
And sixthly, after the core layer is deposited, using oxyhydrogen flame to burn the reaction tube at a high temperature to obtain a section of solid quartz column at the interface of the reaction tube connected with the tail gas end, and completely sealing the channel between the reaction tube and the tail gas tube.
And step seven, introducing oxygen into the reaction tube, starting pressure control at the front end, controlling the gas pressure in the tube to prevent the reaction tube from collapsing, raising the temperature to perform rod shrinkage, and gradually reducing the tube diameter of the reaction tube at high temperature.
And step eight, further increasing the temperature, and completely burning the reaction tube to be solid to prepare the solid optical fiber perform.
The invention has the beneficial effects that: according to the method, after the deposition of the core layer of the preform rod is finished, a section of solid quartz column is subjected to high-temperature burning and shrinkage on the reaction tube at the front end of the joint of the reaction tube and the tail gas tube before the rod is shrunk, and the problem that the rare earth element in the center of the fiber core is lost due to the fact that the volatilization of the rare earth element cannot be supplemented in the traditional core supplementing method is effectively solved by means of sealing a channel between the reaction tube and the tail gas tube; the problems of nonuniform fiber core doping and low central doping element of the prefabricated rod caused by element volatilization are effectively prevented; thereby ensuring the longitudinal and transverse uniformity of the doped elements of the fiber core.
Drawings
FIG. 1 is a schematic view of the reaction tube and the like in depositing a core layer according to the present invention;
FIG. 2 is a schematic view of a portion of a solid quartz column fired after the end of the core layer deposition of the present invention;
FIG. 3 is a test chart showing the lack of the center of the uneven distribution of central elements in the core of a preform prepared by a conventional method;
FIG. 4 is a test chart showing that the central elements of the preform core prepared by the present invention are uniformly distributed without loss in the center.
Detailed Description
The invention is described in detail below with reference to the following figures and examples:
example (b): as shown in fig. 1 and fig. 2, the method for preventing volatilization of core elements of a rare earth ion-doped optical fiber preform comprises the following steps:
selecting a quartz tube with the diameter of 25mm and the wall thickness of 2mm as a reaction tube 3 and carrying out acid cleaning pretreatment, namely cleaning the reaction tube for many times by using hydrofluoric acid and deionized water to remove dust and impurities in the reaction tube.
And step two, selecting a quartz tube with the diameter of 25mm and the wall thickness of 2mm as an air inlet tube 2, and selecting a quartz tube with the diameter of 31mm and the wall thickness of 4mm as an exhaust tube 4.
Step three, fixing the air inlet pipe 2 on an air inlet end fixing clamp 1 of the MCVD, fixing the reaction pipe 3 on a tail gas pipe fixing clamp 5 of the MCVD, shaking the clamp to enable the end faces of the two pipes to be in butt joint, welding the air inlet pipe 2 and one end of the reaction pipe 3 by using an oxyhydrogen blowtorch, and checking the air tightness after welding.
Will fix and loosen tailpipe fixing clamp 5 on reaction tube 3, fix tailpipe 4 on tailpipe fixing clamp 5, and overlap the sealed fixing device 6 cover of tailpipe 4 one end with MCVD's tailpipe, fix and serve at the inboard one end of chuck of tailpipe fixing clamp 5, use oxyhydrogen blowtorch heat softening with the 3 other ends of reaction tube, use the graphite instrument to expand the 3 one end diameters of reaction tube that soften to match with 4 diameters of tailpipe, with reaction tube 3 and 4 butt fusions of tailpipe.
And step four, connecting the tail gas pipe 4 into a tail gas exhaust system 6 of the MCVD system.
After the MCVD system is started, carrier gas and reaction raw materials enter a reaction tube 3 through an air inlet tube 2 and react, and unreacted gas, raw materials, waste gas and impurities generated after the reaction in the reaction tube 3 enter a tail gas tube 4 and a tail gas exhaust system 6 under the action of pressure and are exhausted through a tail gas exhaust pipeline.
And sixthly, after the core layer is deposited, using oxyhydrogen flame to burn out a solid quartz column 7 with the length of about 2 centimeters from the reaction tube 2 on the reaction tube which is 1cm away from the interface of the reaction tube 3 and the tail gas tube 4 at the high temperature of about 2000 ℃, wherein the solid quartz column 7 is completely solid, so that the channel between the reaction tube 3 and the tail gas tube 4 can be completely sealed.
And seventhly, introducing oxygen with the flow of about 200sccm into the reaction tube 3, starting front end pressure control, controlling gas pressure in the tube to prevent the reaction tube 3 from collapsing, raising the temperature to over 2000 ℃ for collapsing, gradually reducing the tube diameter of the reaction tube 3 at high temperature, and finally collapsing to the tube inner bore diameter of about 2mm, wherein the tail gas end is completely sealed, and elements volatilized from the fiber core in the high-temperature collapsing process are still in the sealed reaction tube and cannot be discharged to the tail gas end, so that the elements can continuously react with the oxygen at high temperature and are deposited in the reaction tube.
And step eight, further increasing the temperature to about 2300 ℃, and completely compacting the reaction tube to prepare the solid optical fiber preform.
In the preparation process of the prefabricated rod, the core elements volatilized at high temperature are still deposited at the core, and after the preparation of the prefabricated rod is finished, the distribution condition of the rare earth elements of the fiber core of the prefabricated rod is tested and prepared by adopting a spectral absorption method, so that the optical fiber prefabricated rod master rod with the uniform distribution of the rare earth elements of the fiber core is obtained. FIG. 3 shows the preform without the method, in which rare-earth elements in the center of the core are lost seriously and have a large depression. FIG. 4 shows the distribution of rare earth elements in the core of the preform prepared by the method, which completely eliminates the loss of rare earth elements in the center of the core.
Claims (1)
1. A method for preventing the volatilization of core elements of a rare earth ion-doped optical fiber preform is characterized by comprising the following steps:
selecting a quartz tube as a reaction tube (3) and carrying out acid pickling pretreatment;
selecting a quartz tube with the same diameter and wall thickness as the reaction tube (3) as an air inlet tube (2) and a waste tube (6) according to the diameter of the selected reaction tube (3), and selecting a quartz tube with the diameter and wall thickness larger than that of the reaction tube (3) as an exhaust tube (4);
fixing one end of the air inlet pipe (2) on an air inlet end fixing clamp (1) of the MCVD system, welding the tail end of the air inlet pipe (2) with one end of the reaction pipe (3), and ensuring the collimation of the air inlet pipe (2) and the reaction pipe (3) in the sintering process;
one end of a tail gas pipe (4) is fixed on a tail gas pipe fixing clamp (5) of an MCVD system, a tail gas pipe sealing and fixing device (8) of the MCVD device is sleeved on the tail part of the other end of the tail gas pipe (4), the other end of a reaction pipe (3) is softened at high temperature, the diameter of the other end of the reaction pipe (3) is enlarged to be matched with the tail gas pipe (4) by using a graphite tool, and the reaction pipe (3) is welded with the tail gas pipe (4);
step four, the tail gas pipe (4) is connected into a tail gas exhaust system of the MCVD system;
after the MCVD system is started, carrier gas and reaction raw materials enter a reaction tube (3) through an air inlet tube (2) and react, and unreacted gas, raw materials, waste gas and impurities generated after the reaction in the reaction tube (3) enter a tail gas exhaust system (6) under the action of pressure and are exhausted through a tail gas exhaust pipeline;
sixthly, after the core layer is deposited, using oxyhydrogen flame to burn the reaction tube at a high temperature to form a section of solid quartz column (7) at the interface of the reaction tube connected with the tail gas end, and completely sealing the channel of the reaction tube (3) and the tail gas tube (4);
step seven, introducing oxygen into the reaction tube (3), starting front end pressure control, controlling gas pressure in the tube to prevent the reaction tube from collapsing, raising the temperature to perform rod shrinkage, and gradually reducing the tube diameter of the reaction tube at high temperature;
and step eight, further increasing the temperature, and completely burning the reaction tube (3) to be solid to prepare a solid optical fiber preform.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111504626.2A CN114044627A (en) | 2021-12-10 | 2021-12-10 | Method for preventing core element volatilization of rare earth ion-doped optical fiber preform |
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| CN202111504626.2A CN114044627A (en) | 2021-12-10 | 2021-12-10 | Method for preventing core element volatilization of rare earth ion-doped optical fiber preform |
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3961926A (en) * | 1974-12-27 | 1976-06-08 | International Telephone And Telegraph Corporation | Preparation of germania cores in optical fibers |
| DE2533040A1 (en) * | 1975-07-24 | 1977-02-10 | Licentia Gmbh | Quartz fibres for optical waveguides - made from internally coated tube collapsed by heat and pressure to form rod |
| JPS60176940A (en) * | 1984-02-23 | 1985-09-11 | Sumitomo Electric Ind Ltd | Production of fiber having constant polarization |
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| CN103922579A (en) * | 2014-04-17 | 2014-07-16 | 中天科技精密材料有限公司 | Device for manufacturing prefabricated optical fiber core rod based on base pipe outer diameter maintaining and correcting control and method for manufacturing prefabricated optical fiber core rod by device |
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| CN110903027A (en) * | 2019-12-10 | 2020-03-24 | 中国电子科技集团公司第四十六研究所 | Treatment method for preventing material path blockage of tail gas pipe in preparation process of optical fiber preform |
| CN112159095A (en) * | 2020-09-02 | 2021-01-01 | 烽火通信科技股份有限公司 | Optical fiber preform preparation device and preparation method |
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2021
- 2021-12-10 CN CN202111504626.2A patent/CN114044627A/en active Pending
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| US3961926A (en) * | 1974-12-27 | 1976-06-08 | International Telephone And Telegraph Corporation | Preparation of germania cores in optical fibers |
| DE2533040A1 (en) * | 1975-07-24 | 1977-02-10 | Licentia Gmbh | Quartz fibres for optical waveguides - made from internally coated tube collapsed by heat and pressure to form rod |
| JPS60176940A (en) * | 1984-02-23 | 1985-09-11 | Sumitomo Electric Ind Ltd | Production of fiber having constant polarization |
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