CN111116038A - Gas phase doping device and method for preparing rare earth doped optical fiber preform - Google Patents
Gas phase doping device and method for preparing rare earth doped optical fiber preform Download PDFInfo
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- CN111116038A CN111116038A CN202010030467.6A CN202010030467A CN111116038A CN 111116038 A CN111116038 A CN 111116038A CN 202010030467 A CN202010030467 A CN 202010030467A CN 111116038 A CN111116038 A CN 111116038A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 165
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 155
- 239000013307 optical fiber Substances 0.000 title claims abstract description 67
- 238000000034 method Methods 0.000 title claims abstract description 46
- 230000008021 deposition Effects 0.000 claims abstract description 129
- 238000001704 evaporation Methods 0.000 claims abstract description 113
- 238000010438 heat treatment Methods 0.000 claims abstract description 113
- 239000013522 chelant Substances 0.000 claims abstract description 110
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium chloride Substances Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 66
- 239000002994 raw material Substances 0.000 claims abstract description 59
- 230000008020 evaporation Effects 0.000 claims abstract description 57
- 230000005540 biological transmission Effects 0.000 claims abstract description 37
- 238000007740 vapor deposition Methods 0.000 claims abstract description 14
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000000151 deposition Methods 0.000 claims description 128
- 239000007789 gas Substances 0.000 claims description 102
- 239000012071 phase Substances 0.000 claims description 37
- 239000012159 carrier gas Substances 0.000 claims description 34
- 239000012808 vapor phase Substances 0.000 claims description 28
- 239000010410 layer Substances 0.000 claims description 21
- 239000000463 material Substances 0.000 claims description 20
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 16
- 239000001307 helium Substances 0.000 claims description 15
- 229910052734 helium Inorganic materials 0.000 claims description 15
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000005253 cladding Methods 0.000 claims description 14
- 239000012792 core layer Substances 0.000 claims description 14
- 239000000460 chlorine Substances 0.000 claims description 12
- 230000005587 bubbling Effects 0.000 claims description 9
- 238000005498 polishing Methods 0.000 claims description 9
- 229910019213 POCl3 Inorganic materials 0.000 claims description 8
- 238000002309 gasification Methods 0.000 claims description 8
- 229910003910 SiCl4 Inorganic materials 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000010926 purge Methods 0.000 claims description 6
- 229910006113 GeCl4 Inorganic materials 0.000 claims description 5
- 229910004014 SiF4 Inorganic materials 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 230000001681 protective effect Effects 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 description 15
- 239000010439 graphite Substances 0.000 description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 14
- 230000008569 process Effects 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 7
- -1 rare-earth ions Chemical class 0.000 description 7
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 238000005245 sintering Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 229910052769 Ytterbium Inorganic materials 0.000 description 2
- 238000005137 deposition process Methods 0.000 description 2
- 239000002019 doping agent Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 2
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000012495 reaction gas Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
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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
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/20—Specific substances in specified ports, e.g. all gas flows specified
- C03B2207/26—Multiple ports for glass precursor
- C03B2207/28—Multiple ports for glass precursor for different glass precursors, reactants or modifiers
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2207/00—Glass deposition burners
- C03B2207/42—Assembly details; Material or dimensions of burner; Manifolds or supports
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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)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
The invention discloses a gas phase doping device and a doping method for preparing a rare earth doped optical fiber preform rod3An evaporation unit and a rare earth chelate evaporation unit, wherein AlCl3The evaporation unit and the rare earth chelate evaporation unit both comprise a first heating furnace and an evaporation tank arranged in the first heating furnace; the gas phase transmission system comprises a high-temperature transmission pipeline, a common deposition raw material transmission pipeline and AlCl3A conveying pipeline, a conveying pipeline of the rare earth chelate, a conveying pipeline of common deposition raw materials and AlCl3The outlet sections of the conveying pipeline and the rare earth chelate conveying pipeline extend into a high-temperature conveying pipeline which can be heated; the vapor deposition system comprises a deposition unit and a second heating furnace which are connected with a high-temperature transmission pipeline of the vapor transmission system in a rotating and sealing mode. The method utilizes the device to prepare the rare earth doped optical fiber preform. The invention has high sealing performance and control repeatability.
Description
Technical Field
The invention relates to the technical field of optical fibers, in particular to a gas phase doping device and a gas phase doping method for preparing a rare earth doped optical fiber preform.
Background
At present, the rare earth doped special optical fiber is a research hotspot which is most concerned by people in the field of special optical fibers, and is regarded as a laser medium by people. Except for the commonly used Er3+As dopants, other rare-earth ions, e.g. Yb3+、Tm3+、Ho3+、Nd3+、Pr3+、Eu3+And the rare earth doped fiber is also used as a dopant to manufacture a rare earth doped special optical fiber. The rare earth doped optical fibers can be used for amplifying optical signals and manufacturing optical fiber devices such as optical fiber lasers and optical fiber sensors, and meanwhile, the application of various optical fiber devices and optoelectronic devices based on rare earth doping extends from optical fiber communication to the fields of sensing, medical treatment, material processing, national defense and the like.
The rare earth ion doping process of the rare earth doped optical fiber is generally divided into two types: liquid phase doping method of rare earth ions, and gas phase doping method of rare earth ions. The liquid phase doping method is used for manufacturing an optical fiber loose layer through deposition, and a rare earth doped optical fiber is manufactured by using a method of soaking in a doping solution. The liquid phase doping method is easy to cause the phenomena of uneven doping, separation layer falling and the like, and the soaking process needs to be separated from the lathe operation, so that the process flow is relatively complex.
Gas phase doping methods are further divided into two categories: rare earth chelate gas phase doping method and chloride gas phase doping method. Wherein the chloride gas phase doping method utilizes YbCl3And ErCl3When the chloride is generated to form certain saturated steam under the condition of higher temperature, the saturated steam is carried into the reaction tube through oxygen to carry out oxidation reaction to generate Yb2O3And Er2O3The oxides are incorporated into the core glass tube. The chelate gas phase doping method is that certain organic compound with suspended rare earth ions is volatilized and carries the rare earth ions to enter a reaction tube to carry out oxidation reaction under a high-temperature environment to generate oxide containing rare earth elements to be doped into a core layer glass tube, and other small molecular components are discharged out of a deposition tube after being fully reacted. Chloride gasThe temperature required by the phase doping method is higher, close to 1000 ℃, and the system is easy to generate condensation phenomenon, thereby influencing the rare earth doping control. The chelate gas-phase doping method for preparing the special optical fiber preform is more ideal, has stable and low volatilization, is easy to control, has the advantages of high deposition efficiency, uniform distribution, simple and convenient operation process, less tail gas pollution and the like, and becomes an excellent choice of the existing doping process.
Most of the rare earth chelate doping devices reported in the prior article are common crucible method rare earth chelate doping devices, the rare earth chelate is placed in a crucible in an air inlet pipe at the upper end of a reaction pipe, the rare earth raw material is generally only used for one experiment each time, the rare earth raw material needs to be added again in each experiment, the volatilization amount of the rare earth chelate is not only controlled by temperature and gas flow, but also influenced by factors such as rare earth surface area and capacity, the material is added again in each preparation, and the repeatability of the experiment is greatly reduced.
Therefore, how to ensure the stable volatilization flow of the rare earth chelate doping device and the high repeatability of the doping process is the key for preparing the high-performance doping prefabricated rod, and the high repeatability is the key for producing the stable prefabricated rod product.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a gas phase doping device and a doping method which adopt an MCVD process and improve the sealing property of the device and exert control repeatability through the integrated design of an evaporation tank and a high-temperature delivery pipeline, and improve the performance of an optical fiber preform and the product repeatability.
The invention provides a gas phase doping device for preparing a rare earth doped optical fiber preform rod, which comprises a gasification system, a gas phase transmission system and a gas phase deposition system, wherein the gasification system comprises a common deposition raw material supply unit and an AlCl3An evaporation unit and a rare earth chelate evaporation unit, wherein AlCl3The evaporation unit and the rare earth chelate evaporation unit both comprise a first heating furnace and an evaporation tank arranged in the first heating furnace;
the gas phase transmission system comprises a high-temperature transmission pipeline, a common deposition raw material transmission pipeline connected with a common deposition raw material supply unit and an AlCl3AlCl respectively connected with evaporating pots of evaporating unit and rare earth chelate evaporating unit3A conveying pipeline and a conveying pipeline of the rare earth chelate, the conveying pipeline of the common deposition raw material and AlCl3The outlet sections of the conveying pipeline and the rare earth chelate conveying pipeline extend into a high-temperature conveying pipeline which can be heated;
the vapor deposition system comprises a deposition unit and a second heating furnace, wherein the deposition unit is connected with a high-temperature transmission pipeline of the vapor transmission system in a rotating and sealing mode, an outlet of the high-temperature transmission pipeline is communicated with an air inlet pipe of the deposition unit, and the second heating furnace movably heats a deposition pipe of the deposition unit.
According to one embodiment of the vapor phase doping apparatus for fabricating a rare earth doped optical fiber preform according to the present invention, the AlCl is3The evaporating pot for evaporating the unit and rare-earth chelate includes AlCl3Or rare earth chelate bubbling device and annular pipeline arranged on the outer surface of the bubbling device in a surrounding manner, wherein the inlet of the annular pipeline is connected with a first carrier gas source, the outlet of the annular pipeline is connected with the gas inlet of the bubbling device, and the AlCl is filled in the annular pipeline3The gas outlets of the bubblers of the evaporation unit and the rare earth chelate evaporation unit are respectively connected with AlCl3The conveying pipeline is connected with the rare earth chelate conveying pipeline.
According to one embodiment of the vapor phase doping apparatus for fabricating a rare earth doped optical fiber preform according to the present invention, the AlCl is3The evaporating tanks of the evaporating unit and the rare earth chelate evaporating unit are made of quartz, high-temperature-resistant stainless steel or ceramic, and the volume of the evaporating tanks is not less than 250 ml; the length of the annular pipeline is not less than 2 m, and the inner diameter and AlCl which are defined by the annular pipeline3The outer diameters of the bubblers of the evaporation unit and the rare earth chelate evaporation unit are matched, and the center of each bubbler is provided with a temperature detector.
According to one embodiment of the vapor phase doping device for preparing the rare earth doped optical fiber preform rod, the high-temperature transmission pipeline comprises an inner heating layer, an outer heat insulation layer and a transmission cavity surrounded by the heating layer, and the common deposition raw material transmission pipeline and the AlCl are arranged in the transmission cavity3The outlet sections of the conveying pipeline and the rare earth chelate conveying pipeline both pass through the transmission cavity, wherein the common sinkAccumulated raw material conveying pipeline and AlCl3Control valves are arranged on the conveying pipeline and the rare earth chelate conveying pipeline, and the common deposition raw material conveying pipeline passes through AlCl3And the evaporation unit and the rare earth chelate evaporation unit enter a high-temperature conveying pipeline after entering a first heating furnace.
According to one embodiment of the vapor phase doping apparatus for fabricating a rare earth doped optical fiber preform according to the present invention, the AlCl is3The heating temperature of a first heating furnace in the evaporation unit is 50-300 ℃, the heating temperature of the first heating furnace in the rare earth chelate evaporation unit is 200-300 ℃, the heating temperature of a heating layer of the high-temperature transmission pipeline is 100-900 ℃, the heat insulation layer ensures that the external temperature of the high-temperature transmission pipeline is reduced to 50-100 ℃, and the heating temperature of a second heating furnace is 1200-2300 ℃.
According to one embodiment of the vapor phase doping apparatus for manufacturing a rare earth doped optical fiber preform according to the present invention, the deposition unit includes an inlet tube, a deposition tube, and an outlet tube connected in sequence and capable of rotating around a central axis thereof, one end of the inlet tube is connected and fixed to the high temperature delivery pipe by a rotary seal, and the tail gas tube is connected and fixed to the tail end of the MCVD lathe by a rotary seal.
According to an embodiment of the vapor phase doping apparatus for manufacturing a rare earth-doped optical fiber preform according to the present invention, the vapor phase doping apparatus further includes a gas control unit that controls flow and pressure of the carrier gas and/or each raw material gas, and a heating control unit that controls switching and temperature of each heating furnace.
In another aspect of the present invention, a vapor phase doping method for preparing a rare earth-doped optical fiber preform is provided, which comprises the steps of:
s1, connecting the gas phase doping device for preparing the rare earth doped optical fiber preform, adjusting the gas phase doping device to a state to be operated, introducing helium into the gas phase doping device through a common deposition raw material supply unit for replacement, introducing dehydrated gas for dehydration, and then heating a gasification system and a gas phase transmission system;
s2, heating a deposition unit in the vapor deposition system, introducing polishing gas into the deposition unit through a common deposition raw material supply unit to perform polishing treatment on a deposition tube, subsequently introducing cladding deposition raw material gas to perform cladding deposition, and introducing core deposition raw material gas to perform core deposition;
s3, continuously heating the deposition unit and keeping the temperature at O2And a small amount of Cl2Collapsing under atmosphere to obtain the rare earth doped prefabricated rod.
According to one embodiment of the vapor phase doping method for fabricating a rare earth-doped optical fiber preform according to the present invention, the cladding layer deposition raw material gas includes a second carrier gas and a common deposition raw material, and the core layer deposition raw material includes a first carrier gas and AlCl3Vapor and/or rare earth chelate vapor, a second carrier gas and common deposition raw materials, wherein the first carrier gas or the second carrier gas is nitrogen, oxygen or helium, and the common deposition raw materials are O2、SiCl4、GeCl4、POCl3、SiF4And/or SF6The common deposition material supply unit may further include nitrogen or helium as a purge gas, helium or argon as a protective gas for the first heating furnace, and O as a polishing gas2And SF6And chlorine as a moisture removal gas.
According to one embodiment of the vapor phase doping method for fabricating a rare earth-doped optical fiber preform of the present invention, AlCl is added in step S13Heating an evaporating pot of the evaporating unit to 100-150 ℃, heating the evaporating pot of the rare earth chelate evaporating unit to 200-300 ℃, and heating a high-temperature conveying pipeline to 100-400 ℃; in step S2, heating the deposition unit to 1600-2000 ℃; in step S3, the temperature of the deposition unit is raised to 2100-2200 ℃.
Compared with the prior art, the device has high tightness, can accurately control the concentration of doped rare earth, improves the stability of rare earth doping by the design of the evaporating pot of rare earth chelate, greatly improves the repeatability of the doping concentration for preparing the optical fiber perform and is a reliable guarantee for the continuous research and development of the optical fiber perform.
Drawings
Fig. 1 is a schematic view showing the overall structure of a vapor phase doping apparatus for fabricating a rare earth-doped optical fiber preform according to an exemplary embodiment of the present invention.
Fig. 2 is a schematic cross-sectional view illustrating a high-temperature transfer tube in a vapor-phase doping method for fabricating a rare-earth-doped optical fiber preform according to an exemplary embodiment of the present invention.
FIG. 3 illustrates AlCl in a vapor phase doping method for fabricating a rare earth doped optical fiber preform according to an exemplary embodiment of the present invention3The structure of the evaporation unit is shown schematically.
FIG. 4 illustrates AlCl in a vapor phase doping method for fabricating a rare earth doped optical fiber preform according to an exemplary embodiment of the present invention3Schematic diagram of the structure of the bubbler of the evaporation unit.
FIG. 5 illustrates AlCl in a vapor phase doping method for fabricating a rare earth doped optical fiber preform according to an exemplary embodiment of the present invention3Schematic diagram of the annular duct of the evaporation unit.
Description of reference numerals:
1-AlCl3evaporating pot, 2-rare earth chelate evaporating pot and 3-AlCl3A graphite resistance heating furnace, a 4-rare earth chelate graphite resistance heating furnace, a 5-high temperature transmission pipeline, a 6-rotary seal, a 7-air inlet pipe, an 8-common deposition raw material transmission pipeline and a 9-AlCl3The device comprises a conveying pipeline, a 10-rare earth chelate conveying pipeline, 11-a first annular pipeline, 12-a first temperature detector, 13-a first temperature detector tail wire, 14-an inlet of the first annular pipeline and 15-AlCl3Gas inlet of bubbler, 16-AlCl3The device comprises a gas outlet of a bubbler, a 17-second annular pipeline, a 18-second temperature detector, a 19-second temperature detector tail line, a 20-inlet of the second annular pipeline, a 21-gas inlet of a rare earth chelate bubbler, a 22-gas outlet of the rare earth chelate bubbler, a 23-heating layer, a 24-heat insulation layer, a 25-second heating furnace and a 26-deposition pipe.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
Fig. 1 is a schematic view showing the overall structure of a vapor phase doping apparatus for fabricating a rare earth-doped optical fiber preform according to an exemplary embodiment of the present invention.
As shown in fig. 1, the vapor doping apparatus for fabricating a rare earth-doped optical fiber preform according to an exemplary embodiment of the present invention includes a vaporization system for heating, vaporizing and transporting a raw material, a vapor transport system for transporting a vapor raw material, and a vapor deposition system for heating, oxidizing and depositing the raw material.
Wherein the gasification system of the present invention comprises a general deposition raw material supply unit (not shown), AlCl3An evaporation unit and a rare earth chelate evaporation unit, a common deposition raw material supply unit supplying SiCl to the vapor deposition system4、GeCl4、O2、He、POCl3、SiF4Equal to common deposition material, AlCl3The evaporation unit provides AlCl for the vapor deposition system3And (3) steam, wherein the rare earth chelate evaporation unit vapor deposition system provides rare earth chelate steam.
The AlCl of the invention3The evaporation unit and the rare earth chelate evaporation unit both comprise a first heating furnace and an evaporation tank arranged in the first heating furnace. Specifically, AlCl3The evaporating pot for evaporating the unit and rare-earth chelate includes AlCl3Or rare earth chelate bubbling device and annular pipeline arranged on the outer surface of the bubbling device in a surrounding manner, wherein the inlet of the annular pipeline is connected with a first carrier gas source, the outlet of the annular pipeline is connected with the gas inlet of the bubbling device, and AlCl is used for removing the first carrier gas3The gas outlets of the bubblers of the evaporation unit and the rare earth chelate evaporation unit are respectively connected with AlCl3The conveying pipeline is connected with the rare earth chelate conveying pipeline. Wherein, the first heating furnace is preferably a graphite resistance heating furnace.
That is, AlCl3Evaporating pot 1 and rare earth chelate evaporationThe hair pots 2 are respectively placed on AlCl3Heating in a graphite resistance heating furnace 3 and a rare earth chelate graphite resistance heating furnace 4 for generating high-temperature AlCl3And rare earth chelate vapors. AlCl3One end of the evaporating pot 1 and one end of the rare earth chelate evaporating pot 2 are connected with a gas phase transmission system for transmitting AlCl generated by volatilization of the evaporating pot3Vapor and rare earth chelate vapor, the other end of the vapor transport system being connected directly to the vapor deposition system.
AlCl3The evaporating pots of the evaporating unit and the rare earth chelate evaporating unit are made of quartz, high-temperature-resistant stainless steel or ceramic, and the volume of the evaporating pots is not less than 250 ml. The length of the annular pipeline is not less than 2 m, and the inner diameter and AlCl which are defined by the annular pipeline3The outer diameters of the bubblers of the evaporation unit and the rare earth chelate evaporation unit are matched, and then the bubblers are arranged in the middle of the annular pipeline.
FIG. 3 illustrates AlCl in a vapor phase doping method for fabricating a rare earth doped optical fiber preform according to an exemplary embodiment of the present invention3Fig. 4 illustrates AlCl in a vapor phase doping method for fabricating a rare earth-doped optical fiber preform according to an exemplary embodiment of the present invention3Fig. 5 illustrates an AlCl doping method for fabricating a rare earth doped optical fiber preform according to an exemplary embodiment of the present invention3Schematic diagram of the annular duct of the evaporation unit.
As shown in FIG. 3 to FIG. 5, with AlCl3An evaporation unit, for example, comprising AlCl3Evaporation pot 1 and AlCl3Graphite resistance heating furnace 3, AlCl3The evaporating pot 1 is arranged on AlCl3The graphite resistance heating furnace 3 is heated. AlCl3The evaporating pot 1 comprises AlCl3A bubbler and a first annular channel 11, AlCl surrounding the outer surface thereof3The bubbler is provided with an AlCl3Gas inlet 15 of the bubbler and an AlCl3A gas outlet 16 of the bubbler, an inlet 14 of the first annular pipe connected with a first carrier gas source for inputting the first carrier gas therein, an outlet of the first annular pipe connected with the AlCl3A gas inlet 15 of the bubbler is connected with AlCl3Gas outlet of bubbler16 are connected to a gas delivery system. Wherein, AlCl3The center of the bubbler is provided with a first temperature probe 12, the first temperature probe 12 being energised by a first temperature probe tail 13.
Similarly, the rare earth chelate evaporation unit comprises a rare earth chelate evaporation tank 2 and a rare earth chelate graphite resistance heating furnace 4, wherein the rare earth chelate evaporation tank 2 is arranged in the rare earth chelate graphite resistance heating furnace 4 for heating. The rare earth chelate evaporation tank 2 comprises a rare earth chelate bubbler and a second annular pipeline 17 arranged on the outer surface of the rare earth chelate bubbler in a surrounding mode, the rare earth chelate bubbler is provided with a gas inlet 21 of the rare earth chelate bubbler and a gas outlet 22 of the rare earth chelate bubbler, an inlet 20 of the second annular pipeline is connected with a first carrier gas source so as to input first carrier gas into the second annular pipeline, an outlet of the second annular pipeline is connected with the gas inlet 21 of the rare earth chelate bubbler, and the gas outlet 22 of the rare earth chelate bubbler is connected with a gas conveying system. Wherein, the center of the rare earth chelate bubbler is provided with a second temperature detector 18, and the second temperature detector 18 is electrified through a second temperature detector tail line 19.
The vapor phase transport system of the present invention comprises a high temperature transport pipe 5, a common deposition material transport pipe 8 connected to a common deposition material supply unit, and an AlCl3AlCl respectively connected with evaporating pots of evaporating unit and rare earth chelate evaporating unit3A conveying pipeline 9, a rare earth chelate conveying pipeline 10, a common deposition raw material conveying pipeline 8 and AlCl3The outlet sections of the conveying pipeline 9 and the rare earth chelate conveying pipeline 10 both extend into the high-temperature conveying pipeline 5 which can be heated. And, the common deposition material transfer line 8 passes through AlCl3The graphite resistance heating furnace 3 and the rare earth chelate graphite resistance heating furnace enter a high-temperature conveying pipeline 5.
Fig. 2 is a schematic cross-sectional view illustrating a high-temperature transfer tube in a vapor-phase doping method for fabricating a rare-earth-doped optical fiber preform according to an exemplary embodiment of the present invention.
As shown in FIG. 2, the high temperature transport pipeline 5 comprises an inner heating layer 23, an outer heat insulation layer 24 and a transport chamber surrounded by the heating layer 23, and the common deposition material is transportedPipeline 8, AlCl3The outlet sections of the conveying pipeline 9 and the rare earth chelate conveying pipeline 10 both pass through the conveying cavity. Wherein, the common deposition raw material conveying pipeline 8 and AlCl3The transfer pipe 9 and the rare earth chelate transfer pipe 10 are preferably provided with control valves for easy control. Moreover, the high-temperature conveying pipe 5 is preferably made of high-temperature resistant materials such as quartz, high-temperature resistant stainless steel, ceramics and the like.
Preferably, AlCl3First heating furnace in evaporation unit (i.e. AlCl)3The heating temperature of the graphite resistance heating furnace 3) is 50-300 ℃, the heating temperature of a first heating furnace (namely the rare earth chelate graphite resistance heating furnace 4) in the rare earth chelate evaporation unit is 200-300 ℃, the heating temperature of a heating layer 23 of the high-temperature transmission pipeline 5 is 100-400 ℃, and a heat insulation layer 24 ensures that the external temperature of the high-temperature transmission pipeline 5 is reduced to 50-100 ℃,
as shown in FIG. 1, the vapor deposition system of the present invention comprises a deposition unit and a second heating furnace 25 which are connected to a high-temperature transport pipe of the vapor transport system in a rotary sealed manner, the outlet of the high-temperature transport pipe 5 is communicated with the gas inlet pipe 7 of the deposition unit, and the second heating furnace 25 moves to heat the deposition pipe 26 of the deposition unit. The second heating furnace is preferably an oxyhydrogen flame heating furnace, and the heating temperature of the second heating furnace is preferably 1200-2300 ℃.
The deposition unit comprises an air inlet pipe 7, a deposition pipe 26 and an air outlet pipe which are sequentially connected and can rotate around a central shaft of the deposition unit, one end of the air inlet pipe 7 is connected and fixed with the high-temperature conveying pipeline 5 through a rotary seal 6, the tail air pipe is connected and fixed with the tail end of the MCVD lathe through a rotary seal, and high-temperature reaction gas raw materials conveyed by the high-temperature conveying pipeline 5 directly enter the deposition unit, so that the sealing performance and the effectiveness of the vapor deposition system are guaranteed.
The gas phase doping apparatus of the present invention actually further includes a gas control unit and a heating control unit (not shown), the gas control unit controls the flow rate and pressure of the carrier gas and/or each raw material gas, and the heating control unit controls the on-off and temperature of each heating furnace, which are not described herein as the prior art, and an operator can perform corresponding adjustment and improvement according to actual needs.
Referring to fig. 1, in the process of preparing the rare earth doped preform, AlCl3The evaporating pot 1 passes through AlCl3AlCl is generated by heating the graphite resistance heating furnace 23The vapor feed is carried into the deposition tubes of the deposition unit by a specific flow of a first carrier gas (e.g., helium) that enters the first annular channel 11 at the first annular channel inlet 14 and then passes through the AlCl3The gas inlet 15 of the bubbler enters AlCl3Bubbler and carrying AlCl with set flow3After the steam, the solution passes through AlCl3The gas outlet 16 of the bubbler enters AlCl3The delivery conduit 9, then the inlet pipe 7 and then the deposition pipe 26. The rare earth chelate evaporation tank 2 is heated by a rare earth chelate graphite resistance heating furnace 4 to generate a rare earth chelate vapor raw material, the raw material is carried by a first carrier gas (such as helium) with a specific flow rate to enter a deposition tube of a deposition unit, the first carrier gas enters a second annular pipeline 17 from an inlet 20 of the second annular pipeline, then enters the rare earth chelate bubbler 2 from a gas inlet 21 of the rare earth chelate bubbler and carries rare earth chelate vapor with a set flow rate, and then enters a rare earth chelate conveying pipeline 10 through a gas outlet 22 of the rare earth chelate bubbler, and then enters an air inlet pipe 7 and then enters a deposition tube 26. At the same time, common deposition materials (e.g., SiCl)4、GeCl4、O2He, etc.) enters the gas pipe 7 through the common deposition source material delivery pipe 8 and then enters the deposition pipe 26. AlCl3And after the steam, the rare earth chelate steam and the common raw material steam enter the deposition tube 26 together, the deposition preparation of the rare earth doped optical fiber preform is carried out under the heating action of the second heating furnace 25.
The invention also provides a gas phase doping method for preparing the rare earth doped optical fiber preform, which adopts the gas phase doping device for preparing the rare earth doped optical fiber preform to prepare the rare earth doped optical fiber preform and specifically comprises the following steps.
Step S1:
connecting a gas phase doping device for preparing the rare earth doped optical fiber preform and adjusting the gas phase doping device to a state to be operated, wherein the gas phase doping device comprises a system temperature, a program setting, an exhaust system, a welded gas inlet pipe, a deposition pipe and an exhaust pipe.
Introducing helium gas into the gas phase doping device for replacement through a common deposition raw material supply unit, introducing dehydrated gas for dehydration, and then heating a gasification system and a gas phase transmission system.
Because of the AlCl of the device at normal temperature3The evaporating pot, the rare earth chelate evaporating pot and the conveying pipeline thereof use N2Purging, wherein He is used for purging before the temperature of the doping device is raised, and N in the cavity and the pipeline2After the water is exhausted, the temperature of the device is raised. After the purging and dehydration are completed, the gas introduction is stopped and AlCl is added3And heating an evaporating pot of the evaporating unit to 100-150 ℃, heating the evaporating pot of the rare earth chelate evaporating unit to 200-300 ℃, and heating a high-temperature conveying pipeline to 100-400 ℃ so as to enable the raw materials to reach the melting point temperature.
Step S2:
and heating a deposition unit in the vapor deposition system, introducing polishing gas into the deposition unit through a common deposition raw material supply unit to perform polishing treatment on the deposition tube, subsequently introducing cladding deposition raw material gas to perform cladding deposition, and then introducing core deposition raw material gas to perform core deposition.
In the invention, the deposition unit is preferably heated to 1600-2000 ℃ for deposition. The cladding deposition material gas includes a second carrier gas and a common deposition material, and the second carrier gas carries the common deposition material into the vapor deposition system. Wherein the second carrier gas may be nitrogen, oxygen or helium, and the common deposition material may be O2、SiCl4、GeCl4、POCl3、SiF4And/or SF6. In addition, the common deposition material supply unit may be further capable of introducing nitrogen or helium as a purge gas, helium or argon as a shield gas of the first heating furnace, O as a polishing gas2And SF6And chlorine as the moisture removal gas, which can be specifically selected by the operator according to the preparation steps and controlled by a basic MCVD system.
The core layer deposition raw material comprises a first carrier gas and AlCl3Vapor and/or rare earth chelate vapor, a second carrier gas and common deposition raw materials, wherein the first carrier gas or the second carrier gas is nitrogen, oxygen or helium, and the common deposition raw materialsAs described above.
Step S3:
continuing to heat the deposition unit and keeping at O2And a small amount of Cl2Collapsing under atmosphere to obtain the rare earth doped prefabricated rod. Wherein the temperature of the deposition unit is preferably raised to 2100-2200 DEG C
The present invention will be further described with reference to the following specific examples.
The specific technical examples of the invention are as follows:
example 1: preparation of rare earth Yb doped YbAlPSi prefabricated rod
Preparation of rare earth YbAlPSi doped preform requiring AlCl in the doping apparatus of the present invention3Adding AlCl as raw material into evaporating pot3200 g and adding 200 g of raw material ytterbium chelate into a rare earth chelate evaporating pot.
The common raw material parameters in the preparation process of the prefabricated rod are controlled by an MCVD system as follows:
cladding parameter SiCl4：300sccm，O2：2000sccm，He：1000sccm，POCl3：80sccm，SF6: 1.5sccm, and the heated deposition temperature of the second heating furnace was 1960 ℃.
Core layer parameter SiCl4：150sccm，POCl3：85sccm，O2：1500sccm，He：1000sccm，AlCl3: 55sccm, Yb chelate: 260sccm, and the heating deposition temperature of the second heating furnace is 1850 ℃.
Before the optical fiber preform is prepared by experiment, the doping device is prepared according to the requirement, and the experimental parameters of the core layer deposition process are set as follows: AlCl3Flow rate (carrier gas He): 55sccm (AlCl)3Temperature of the evaporating pot: 150 deg.c), rare earth chelate flow rate (carrier gas He): 260scm (rare earth chelate evaporator temperature: 180 ℃).
After the core layer deposition is completed, at O2And Cl2And raising the heating temperature of the second heating furnace to 2250 ℃ in the atmosphere, and sintering the deposited tube with the deposited cladding and core layers. O is2And Cl2As the flow rate becomes smaller, and O is set2Flow rate between 1000sccm and 100sccm, Cl2The flow rate is between 100sccm and 10sccm, and the rare earth doping prefabricated rod is obtained after sintering, wherein the cladding comprises the following components: SiO 22-P2O5-F, core layer composition: yb of2O3-Al2O3-P2O5-SiO2。
Example 2: preparation of rare earth Yb doped YbPSi prefabricated rod
The raw material YbCl is required to be added into a rare earth chelate evaporation tank of the doping device for preparing the rare earth YbPSi doping prefabricated rod3200 g. AlCl in this example3The evaporation unit is closed and not needed.
The common raw material parameters are controlled by an MCVD system as follows:
cladding parameter SiCl4：300sccm，O2：2000sccm，He：1000sccm，POCl3: 80sccm, SF 6: 1.5sccm, and the heated deposition temperature of the second heating furnace was 1960 ℃.
Core layer parameter SiCl4：150sccm，POCl3：120sccm，O2：1500sccm，He：1000sccm，SiF4: 35sccm, Yb chelate: 180sccm and the heating deposition temperature of the second heating furnace is 1800 ℃.
Before the optical fiber preform is prepared by experiment, the doping device is prepared according to the requirement, and the experimental parameters of the core layer deposition process are set as follows: rare earth ytterbium chelate flow rate (carrier gas He): 180scm (rare earth chelate evaporator temperature: 180 ℃).
After the core layer deposition is completed, at O2And Cl2And raising the heating temperature of the second heating furnace to 2250 ℃ in the atmosphere, and sintering the deposition tube with the deposited core layer. O is2And Cl2As the flow rate becomes smaller, and O is set2Flow rate between 1000sccm and 100sccm, Cl2The flow rate is between 100sccm and 10 sccm. And (3) obtaining a rare earth doped preform after sintering, wherein the cladding comprises the following components: SiO 22-P2O5-F, core layer composition: yb of2O3-P2O5-SiO2-F。
In conclusion, the invention provides the doping device for effectively preparing the rare earth optical fiber preform, which is simple and convenient to operate and can be highly combined with an MCVD system. Meanwhile, the device has high tightness, the concentration of doped rare earth can be accurately controlled, the volatilization stability of chloride is effectively improved due to the integrated design of the evaporating pot and the high-temperature transmission pipeline, the repeatability of the doping concentration of the optical fiber perform rod is greatly improved, and the device is a reliable guarantee for the continuous research and development of the optical fiber perform rod.
The invention is not limited to the foregoing embodiments. The invention extends to any novel feature or any novel combination of features disclosed in this specification and any novel method or process steps or any novel combination of features disclosed.
Claims (10)
1. A gas phase doping device for preparing a rare earth doped optical fiber preform comprises a gasification system, a gas phase transmission system and a gas phase deposition system, and is characterized in that the gasification system comprises a common deposition raw material supply unit, an AlCl3An evaporation unit and a rare earth chelate evaporation unit, wherein AlCl3The evaporation unit and the rare earth chelate evaporation unit both comprise a first heating furnace and an evaporation tank arranged in the first heating furnace;
the gas phase transmission system comprises a high-temperature transmission pipeline, a common deposition raw material transmission pipeline connected with a common deposition raw material supply unit and an AlCl3AlCl respectively connected with evaporating pots of evaporating unit and rare earth chelate evaporating unit3A conveying pipeline and a conveying pipeline of the rare earth chelate, the conveying pipeline of the common deposition raw material and AlCl3The outlet sections of the conveying pipeline and the rare earth chelate conveying pipeline extend into a high-temperature conveying pipeline which can be heated;
the vapor deposition system comprises a deposition unit and a second heating furnace, wherein the deposition unit is connected with a high-temperature transmission pipeline of the vapor transmission system in a rotating and sealing mode, an outlet of the high-temperature transmission pipeline is communicated with an air inlet pipe of the deposition unit, and the second heating furnace movably heats a deposition pipe of the deposition unit.
2. The vapor phase doping apparatus for fabricating a rare earth doped optical fiber preform according to claim 1, wherein the apparatus is further characterized in thatAlCl3The evaporating pot for evaporating the unit and rare-earth chelate includes AlCl3Or rare earth chelate bubbling device and annular pipeline arranged on the outer surface of the bubbling device in a surrounding manner, wherein the inlet of the annular pipeline is connected with a first carrier gas source, the outlet of the annular pipeline is connected with the gas inlet of the bubbling device, and the AlCl is filled in the annular pipeline3The gas outlets of the bubblers of the evaporation unit and the rare earth chelate evaporation unit are respectively connected with AlCl3The conveying pipeline is connected with the rare earth chelate conveying pipeline.
3. The vapor phase doping apparatus for fabricating a rare earth doped optical fiber preform according to claim 2, wherein the AlCl is3The evaporating tanks of the evaporating unit and the rare earth chelate evaporating unit are made of quartz, high-temperature-resistant stainless steel or ceramic, and the volume of the evaporating tanks is not less than 250 ml; the length of the annular pipeline is not less than 2 m, and the inner diameter and AlCl which are defined by the annular pipeline3The outer diameters of the bubblers of the evaporation unit and the rare earth chelate evaporation unit are matched, and the center of each bubbler is provided with a temperature detector.
4. The vapor phase doping apparatus for preparing a rare earth doped optical fiber preform according to claim 1, wherein the high temperature transport pipe comprises an inner heating layer, an outer heat insulation layer and a transport cavity surrounded by the heating layer, and the common deposition material transport pipe, the AlCl3The outlet sections of the conveying pipeline and the rare earth chelate conveying pipeline both penetrate through the conveying cavity, wherein the common deposition raw material conveying pipeline and the AlCl3Control valves are arranged on the conveying pipeline and the rare earth chelate conveying pipeline, and the common deposition raw material conveying pipeline passes through AlCl3And the evaporation unit and the rare earth chelate evaporation unit enter a high-temperature conveying pipeline after entering a first heating furnace.
5. The vapor phase doping apparatus for fabricating a rare earth doped optical fiber preform according to claim 4, wherein the AlCl is3The heating temperature of the first heating furnace in the evaporation unit is 50-300 ℃, and the heating temperature of the first heating furnace in the rare earth chelate evaporation unit is200-300 ℃, the heating temperature of the heating layer of the high-temperature transmission pipeline is 100-400 ℃, the heat insulation layer ensures that the external temperature of the high-temperature transmission pipeline is reduced to 50-100 ℃, and the heating temperature of the second heating furnace is 1200-2300 ℃.
6. The vapor phase doping apparatus for fabricating a rare earth-doped optical fiber preform according to claim 1, wherein the deposition unit includes an inlet tube, a deposition tube and an outlet tube connected in sequence and capable of rotating around a central axis thereof, one end of the inlet tube is connected and fixed to the high temperature delivery tube by a rotary seal, and the tail gas tube is connected and fixed to a tail end of an MCVD lathe by a rotary seal.
7. The vapor phase doping apparatus for fabricating a rare earth-doped optical fiber preform according to claim 1, further comprising a gas control unit that controls flow and pressure of the carrier gas and/or each raw material gas, and a heating control unit that controls on/off and temperature of each heating furnace.
8. A vapor doping method for fabricating a rare earth-doped optical fiber preform, wherein the fabrication of the rare earth-doped optical fiber preform is performed using the vapor doping apparatus for fabricating a rare earth-doped optical fiber preform according to any one of claims 1 to 7 and comprises the steps of:
s1, connecting the gas phase doping device for preparing the rare earth doped optical fiber preform, adjusting the gas phase doping device to a state to be operated, introducing helium into the gas phase doping device through a common deposition raw material supply unit for replacement, introducing dehydrated gas for dehydration, and then heating a gasification system and a gas phase transmission system;
s2, heating a deposition unit in the vapor deposition system, introducing polishing gas into the deposition unit through a common deposition raw material supply unit to perform polishing treatment on a deposition tube, subsequently introducing cladding deposition raw material gas to perform cladding deposition, and introducing core deposition raw material gas to perform core deposition;
s3, continuously heating the deposition unit and keeping the temperature at O2And a small amount of Cl2Collapsing under atmosphere to obtain the rare earth doped prefabricated rod.
9. The vapor-phase doping method for fabricating a rare-earth-doped optical fiber preform according to claim 8, wherein the cladding layer deposition source gas comprises a second carrier gas and a common deposition source material, and the core layer deposition source material comprises a first carrier gas and AlCl3Vapor and/or rare earth chelate vapor, a second carrier gas and common deposition raw materials, wherein the first carrier gas or the second carrier gas is nitrogen, oxygen or helium, and the common deposition raw materials are O2、SiCl4、GeCl4、POCl3、SiF4And/or SF6The common deposition material supply unit may further include nitrogen or helium as a purge gas, helium or argon as a protective gas for the first heating furnace, and O as a polishing gas2And SF6And chlorine as a moisture removal gas.
10. The vapor-phase doping method for fabricating a rare-earth-doped optical fiber preform according to claim 8, wherein AlCl is added in step S13Heating an evaporating pot of the evaporating unit to 100-150 ℃, heating the evaporating pot of the rare earth chelate evaporating unit to 200-300 ℃, and heating a high-temperature conveying pipeline to 100-400 ℃; in step S2, heating the deposition unit to 1600-2000 ℃; in step S3, the temperature of the deposition unit is raised to 2100-2200 ℃.
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