CN114702239B - Fluorine-doped cladding-based irradiation-resistant erbium-doped optical fiber preform and preparation method thereof - Google Patents
Fluorine-doped cladding-based irradiation-resistant erbium-doped optical fiber preform and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a technology for manufacturing an optical fiber preform, in particular to an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer and a preparation method thereof. Solves the problem that the content of the co-doping agent of the prior erbium-doped optical fiber is highPoor irradiation resistance and Er not realized by nano-particle doping technology 3+ High concentration doping. The invention relates to an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding, which comprises a core region, a fluorine-doped cladding and a pure quartz barrier layer, wherein the fluorine-doped cladding and the pure quartz barrier layer are sequentially coated on the outer surface of the core region from inside to outside, and the relative refractive index difference delta n between the fluorine-doped cladding and the pure quartz barrier layer 1 The value range of (A) is 0.007-0.020; the core region sequentially comprises a central erbium-doped region and a non-erbium-doped region from inside to outside; the fluorine-doped cladding layer sequentially comprises a transition layer and a fluorine-doped quartz layer from inside to outside; the refractive indexes of the transition layer and the fluorine-doped quartz layer are equal, and the value range of the relative refractive index difference delta n between the core region and the fluorine-doped cladding layer is 0.013-0.021. Meanwhile, the invention also provides a preparation method for preparing the irradiation-resistant erbium-doped optical fiber preform.
Description
Technical Field
The invention relates to a technology for manufacturing an optical fiber preform, in particular to an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer and a preparation method thereof.
Background
With the continuous improvement of communication requirements in the space fields of satellite networking, constellation planning, deep space exploration and the like, the traditional radio communication cannot meet the communication requirements of human space exploration on large bandwidth, high speed and instantaneity due to bandwidth limitation. The spatial laser communication technology has become a development direction of a future spatial link due to its advantages of extremely high transmission rate, extremely high communication capacity, good confidentiality, no need of radio frequency permission, small volume, light weight and the like, and has become one of hot spots of worldwide research. The erbium-doped fiber amplifier is used as a key component of a space laser communication system, is mainly used for high-power amplification of an optical transmission system and pre-amplification of an optical receiving system, and plays an important role in space laser communication. However, because the erbium-doped fiber amplifier works in a severe irradiation environment of the outer space orbit for a long time, the erbium-doped fiber which is a key material of the erbium-doped fiber amplifier can be strongly irradiated by high-energy particles, so that the laser gain performance of the erbium-doped fiber amplifier is greatly reduced and even completely fails, and therefore, the radiation-resistant characteristic of the erbium-doped fiber needs to be improved besides a passive protection technology of radiation-proof shielding which is added on the surface of a device.
Usually, to increase Er 3+ The introduction of the co-doping agents can avoid concentration quenching effect caused by Er clusters, and simultaneously meet the requirement of a numerical aperture of 0.23 +/-0.02 to ensure the single-mode transmission of the pumping light and the signal light. However, the absorption band tail of the relevant color center formed by irradiation induction of these codoped agents in the short wavelength or visible light band causes additional loss in the near infrared region, which is also the most significant cause of the sharp decline of the laser performance of the erbium-doped fiber. In further studies by the German Frounhofu research institute, it was found that the Al component in the core has the greatest effect on radiation loss and that the optical fiber with the lowest A1 content has the lowest radiation loss (IEEE Transactions on Nuclear Science 1998, 45-439-444). Researches show that the radiation sensitivity of the Al component is mainly related to related defects of Al in a glass network, and the tails of 4 defect absorption peaks cover the laser working waveband of the erbium-doped fiber. Therefore, less Al doping is an effective means to improve the radiation resistance of erbium-doped fibers.
Currently, only Dutch Draka company adopts nanoparticle doping technology to prepare low-Al or even Al-free erbium-doped fiber with good irradiation resistance, but only relying on the technology can not effectively disperse Er 3+ Er to avoid the quenching effect of the ion concentration 3+ The doping concentration cannot be higher than 1000ppm (US 8467123B 2), which results in that the laser gain performance cannot be further improved, different gain requirements of the optical fiber cannot be met, and the application requirements of space laser communication are difficult to meet.
Disclosure of Invention
The invention provides a fluorine-doped silicon-based alloyThe radiation-resistant erbium-doped optical fiber preform of the cladding and the preparation method thereof solve the problems that the prior erbium-doped optical fiber has poor radiation resistance caused by high content of co-doping agent or the Er can not be realized by the nano-particle doping technology 3+ The technical problem of high-concentration doping effectively reduces the radiation sensitivity of the erbium-doped optical fiber, so that the erbium-doped optical fiber can better meet the application requirement of a space radiation environment.
The technical solution of the invention is as follows:
an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer is characterized in that: comprises a core region, a fluorine-doped cladding layer and a pure quartz barrier layer which are sequentially coated on the outer surface of the core region from inside to outside, wherein the relative refractive index difference delta n between the fluorine-doped cladding layer and the pure quartz barrier layer 1 The value range of (A) is 0.007-0.020;
the core region sequentially comprises a central erbium-doped region and a non-erbium-doped region from inside to outside;
the fluorine-doped cladding layer sequentially comprises a transition layer and a fluorine-doped quartz layer from inside to outside;
the refractive indexes of the transition layer and the fluorine-doped quartz layer are equal, and the value range of the relative refractive index difference delta n between the core region and the fluorine-doped cladding layer is 0.013-0.021.
Further, the components and the contents of the central erbium-doped region are respectively SiO 2 ：95.0～99.7Wt.％，Er 2 O 3 ：0.1～1.2Wt.％，Al 2 O 3 ：0.2～2.3Wt.％，Ce 2 O 3 : 0-1.5 Wt.%; the components and the contents of the non-erbium-doped regions are respectively SiO 2 ：95.0～98.5Wt.％，GeO 2 : 1.5-5.0 Wt.%; the components and the contents of the transition layer are respectively SiO 2 ：93.0～96.9Wt.％，GeO 2 : 1.0-2.5 Wt.%, F: 2.1-4.5 Wt.%; the fluorine-doped quartz layer comprises SiO as the component and the content 2 ：95.7～98.5Wt.％，F：1.5～4.3Wt.％。
Further, the ratio of the outer diameters of the central erbium-doped region and the non-erbium-doped region is 1: 1.05-1.3, the ratio of the outer diameter of the core region to the outer diameter of the transition layer is 1: 1.5-4, wherein the ratio of the outer diameter of the fluorine-doped quartz layer to the outer diameter of the pure quartz barrier layer is 1:1.05 to 1.2.
A preparation method of an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer is characterized by comprising the following steps:
step 1) preparing a germanium-fluorine co-doped quartz tube and a fluorine-doped quartz tube by adopting a plasma chemical vapor deposition method;
step 2) taking the germanium-fluorine co-doped quartz tube prepared in the step 1) as a deposition liner tube, sequentially depositing a non-erbium-doped region and a central erbium-doped region by adopting an improved chemical vapor deposition and chelate gas phase doping method, and sintering at high temperature to form a solid core rod;
step 3) removing the pure quartz layer on the outermost layer of the solid core rod obtained in the step 2);
step 4) according to the requirement of core cladding ratio, combining the core rod processed in the step 3) with the fluorine-doped quartz tube prepared in the step 1) by adopting one or more casing processes to prepare the erbium-doped optical fiber preform; and when the sleeve process is carried out for multiple times, removing the outer pure quartz barrier layer after the sleeve is sleeved for the last time.
Further, in the step 1), the germanium-fluorine co-doped quartz tube is sequentially arranged into a transition layer and a pure quartz layer from inside to outside, and the ratio of the outer diameters of the transition layer and the pure quartz layer is 1:1.05 to 1.2;
the fluorine-doped quartz tube is sequentially arranged into a fluorine-doped quartz layer and a pure quartz barrier layer from inside to outside, and the outer diameter ratio of the fluorine-doped quartz layer to the pure quartz barrier layer is 1:1.05 to 1.2.
Further, in step 2), the deposition parameters are: the deposition temperature is 1300-1900 ℃, the rotating speed is 30rpm/min, and the moving speed of oxyhydrogen flame is 80-100 mm/min.
Further, the step 3) is specifically to remove the pure quartz layer at the outermost layer of the solid core rod obtained in the step 2) by adopting a mechanical grinding or polishing method;
in the step 4), when the casing process is carried out for multiple times, the outer pure quartz barrier layer after the previous casing is removed by adopting a mechanical grinding or polishing method.
The invention has the beneficial effects that:
1) The radiation-resistant erbium-doped fiber of the invention introduces the fluorine-doped cladding design on the fiber structure, greatly reduces the requirement of single-mode transmission of the fiber on the absolute refractive index of the core region,ge. The Al content can be reduced by 5 to 20 times, and the content can be determined according to Er 3+ The concentration realizes the optimal matching, greatly reduces the doping of the core region codoping agent, effectively reduces the background transmission loss of the erbium-doped fiber, simultaneously effectively reduces the additional loss caused by the radiation color center related to the codoping agent, and greatly improves the irradiation resistance of the erbium-doped fiber.
2) Er in the irradiation-resistant erbium-doped fiber 3+ The Er in the central region can be made by doping the central region of the core region in a concentrated manner 3+ Is fully excited, and edge part with weak light intensity is prevented from being caused by Er 3+ The erbium-doped fiber is not fully excited to become an absorber, so that the gain is reduced, and meanwhile, the core region structure can also reduce the content of Al component, so that the radiation sensitivity of the erbium-doped fiber is further reduced.
3) The structure of the radiation-resistant erbium-doped fiber introduces the Ge-doped non-erbium doped region and the Ge-and-F-doped transition layer, which can be used as viscosity matching layers of the core region and the cladding layer, so that the stress loss of the fiber is reduced.
4) In the preparation method of the irradiation-resistant erbium-doped optical fiber preform, the introduction of the pure quartz layer in the germanium-fluorine co-doped quartz tube and the fluorine-doped quartz tube can effectively inhibit fluorine volatilization caused by high-temperature conditions in the processes of core rod deposition, sleeve and optical fiber drawing, and keep the stability of the optical fiber waveguide structure.
Drawings
FIG. 1 is a schematic cross-sectional view of a preform of an irradiation-resistant erbium-doped fiber prepared according to an embodiment of the present invention;
FIG. 2 is a schematic cross-sectional refractive index profile of an erbium-doped fiber preform fabricated according to an embodiment of the present invention;
FIG. 3 is a schematic view showing a cross-sectional refractive index profile of an erbium-doped optical fiber preform prepared in a comparative example;
fig. 4 is a graph comparing the gain attenuation of the radiation-resistant erbium-doped fiber prepared in the comparative example and the first and third examples of the present invention under different irradiation conditions.
Reference numerals: 1-central erbium-doped region, 2-non-erbium-doped region, 3-transition layer, 4-fluorine-doped quartz layer, 5-pure quartz barrier layer, 6-fiber core and 7-cladding layer.
Detailed Description
In order that the invention may be more readily understood, reference will now be made in detail to the present invention as illustrated in the accompanying drawings and specific examples. It is to be understood that these examples are illustrative only and are not intended to limit the present invention.
The invention is explained in more detail below with reference to the figures and examples.
The invention relates to an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding, which has a structure shown in figure 1 and comprises a core region, a fluorine-doped cladding and a pure quartz barrier layer 5, wherein the fluorine-doped cladding and the pure quartz barrier layer 5 are sequentially coated on the outer surface of the core region from inside to outside, and the relative refractive index difference delta n between the fluorine-doped cladding and the pure quartz barrier layer 5 1 The value range of (A) is 0.007-0.020; the core region comprises a central erbium-doped region 1 and a non-erbium-doped region 2 from inside to outside in sequence; the fluorine-doped cladding layer sequentially comprises a transition layer 3 and a fluorine-doped quartz layer 4 from inside to outside; the refractive index of the transition layer 3 is equal to that of the fluorine-doped quartz layer 4, the relative refractive index difference delta n between the core region and the fluorine-doped cladding layer is in the range of 0.013-0.021, and the schematic diagram of the relative refractive index distribution is shown in fig. 2.
Wherein, the components and the contents of the central erbium-doped region 1 are respectively SiO 2 ：95.0～99.7Wt.％，Er 2 O 3 ：0.1～1.2Wt.％，Al 2 O 3 ：0.2～2.3Wt.％，Ce 2 O 3 : 0-1.5 Wt.%; the component and content of the non-erbium-doped region 2 are respectively SiO 2 ：95.0～98.5Wt.％，GeO 2 : 1.5-5.0 Wt.%; the composition and content of the transition layer 3 are respectively SiO 2 ：93.0～96.9Wt.％，GeO 2 : 1.0-2.5 Wt.%, F: 2.1-4.5 Wt.%; the fluorine-doped quartz layer 4 comprises SiO 2 : 95.7-98.5 Wt.%, F: 1.5-4.3 Wt.%. The ratio of the outer diameters of the central erbium-doped region 1 and the non-erbium-doped region 2 is 1: 1.05-1.3, the ratio of the core area to the outer diameter of the transition layer 3 is 1: 1.5-4, the ratio of the outer diameter of the fluorine-doped quartz layer 4 to the outer diameter of the pure quartz barrier layer 5 is 1:1.05 to 1.2.
The invention also provides a preparation method of the radiation-resistant erbium-doped optical fiber preform based on the fluorine-doped cladding layer, and the detailed description is given below through examples and comparative examples.
Comparative example:
by common mixingErbium optical fiber is used as a comparison object, an F-300 quartz tube is used as a deposition liner tube, a common erbium-doped optical fiber preform is prepared by combining an improved chemical vapor deposition method with a chelate vapor phase doping method, the structure of the common erbium-doped optical fiber preform is that a cladding 7 is coated on the outer surface of a fiber core 6, and the schematic refractive index distribution diagram of the common erbium-doped optical fiber preform is shown in attached figure 3. Firstly, preheating and oxidizing impurity removal are carried out on an F-300 quartz tube in sequence; and is passed through SF 6 Gas erodes the inner wall of the F-300 quartz tube; after the etching was completed, the reaction material SiCl was set according to the flow rate of the fiber core 6 composition designed in Table 1 4 、Er(TMHD) 3 、AlCl 3 、GeCl 4 The flow rate of (a); introducing an F-300 quartz tube to start to deposit a core layer, wherein the deposition temperature is 1950 ℃, the rotating speed is 30rpm/min, and the moving speed of oxyhydrogen flame is 100mm/min; after the deposition is finished, introducing Cl of 5sccm 2 The quartz tube was sintered to a solid rod. The fiber core 6 of the common erbium-doped optical fiber preform is tested by adopting an electronic probe, and the test result shows that the components and the average content of the fiber core 6 are respectively about SiO 2 ：83.8Wt.％，Er 2 O 3 ：0.4Wt.％，Al 2 O 3 ：8.3Wt.％，GeO 2 :7.5Wt.%. A pure quartz tube is used as a sleeve, a proper sleeve process is selected to sleeve the preform to enable the preform to meet the requirement of the core-cladding ratio of the optical fiber, drawing and coating are carried out at the temperature of 2050 ℃, and the 4/125 mu m common erbium-doped optical fiber is obtained, wherein the basic performance parameters of the optical fiber are shown in a table 6.
TABLE 1 compositional flow rates (sccm) of the various deposits of the core in the comparative examples
| Number of deposited layers of core | SiCl 4 | Er(TMHD) 3 | GeCl 4 | AlCl 3 |
| 1～9 | 300 | 120 | 520 | 480 |
| 10 | 300 | 120 | 550 | 500 |
The first embodiment is as follows:
respectively preparing the germanium-fluorine co-doped quartz tube and the fluorine-doped quartz tube with quartz layers on the outer surfaces by adopting a plasma chemical vapor deposition method. The Ge-F co-doped quartz tube is sequentially arranged into a transition layer 3 and a pure quartz layer from inside to outside, and the external diameter ratio of the transition layer to the pure quartz layer is 1:1.1, the fluorine-doped quartz tube is sequentially arranged into a fluorine-doped quartz layer 4 and a pure quartz barrier layer 5 from inside to outside, and the external diameter ratio of the fluorine-doped quartz tube is 1:1.15; the transition layer 3 and the fluorine-doped quartz layer 4 have the same absolute refractive index, and the relative refractive index difference Deltan between the transition layer and the fluorine-doped quartz layer and the pure quartz layer 1 All of which are 0.015. The electronic probe test result shows that the components and the contents of the transition layer 3 are respectively SiO 2 ：94.6Wt.％，GeO 2 :1.3Wt.%, F:4.1Wt.%; the fluorine-doped quartz layer 4 comprises SiO 2 ：96.4Wt.％，F：3.6Wt.％。
The Ge-F co-doped quartz tube is used as a deposition liner tube, and an improved chemical vapor deposition and chelate gas phase doping method is adopted to prepare the erbium-doped optical fiber core rod, wherein the schematic cross-sectional diagram and the refractive index distribution diagram are respectively shown in the attached figures 1 and 2. Sequentially carrying out preheating, oxidation impurity removal and erosion treatment on the germanium-fluorine co-doped quartz tube; then, according to the non-erbium-doped region 2 and the central erbium-doped region in the core region of the optical fiber preform rodThe composition of the zone 1 requires that the reaction materials SiCl are respectively arranged 4 、Er(TMHD) 3 、AlCl 3 、GeCl 4 The flow rate of (2) is specifically shown in Table 2. Introducing the reaction materials into a germanium-fluorine codoped quartz tube to start to deposit a core layer, wherein the deposition temperature is 1680 ℃, the rotating speed is 30rpm/min, and the moving speed of oxyhydrogen flame is 100mm/min; after the deposition is finished, introducing Cl of 5sccm 2 The mixture is sintered and condensed into a solid core rod. Wherein the central erbium-doped region 1 and the non-erbium-doped region 2 of the solid core rod have outer diameters of 3.0mm and 3.3mm respectively (the ratio of outer diameters is 1. The electronic probe test result shows that the components and the average content of the central erbium-doped region 1 are respectively SiO 2 ：99Wt.％，Er 2 O 3 ：0.4Wt.％，Al 2 O 3 :0.6Wt.%; the composition and average content of the non-erbium-doped region 2 are respectively SiO 2 ：98.2Wt.％，GeO 2 ：1.8Wt.％。
Removing a pure quartz layer on the surface of the solid core rod by adopting a mechanical grinding method, then using the fluorine-doped quartz tube as a sleeve, selecting one or more sleeve processes to sleeve the erbium-doped core rod according to the requirement of the core cladding ratio of the optical fiber, and removing an outer pure quartz barrier layer 5 after the previous sleeve when the sleeve is sleeved for a plurality of times, thereby obtaining the final erbium-doped optical fiber preform. In the embodiment, the outer diameters of the fluorine-doped silica layer 4 and the pure silica barrier layer 5 in the erbium-doped optical fiber preform after sleeving the tube are 14.2mm and 15.6mm respectively (the outer diameter ratio is 1.1. Finally, the fiber was drawn and coated at 1950 ℃ to obtain 4/125 μm erbium-doped fiber, the basic performance parameters of which are shown in Table 6.
TABLE 2 composition flow rates (sccm) for each deposition layer in example one
| Core region composition | Number of deposited layers | SiCl 4 | Er(TMHD) 3 | AlCl 3 | GeCl 4 |
| Non erbium doped region | 1～3 | 300 | / | / | 100 |
| Central erbium doped region | 1～10 | 300 | 120 | 40 | / |
Example two:
the deposition method, preform size, jacket tube treatment method, fiber structure, etc. of the erbium-doped fiber core rod are the same as those of the first embodiment. The difference is the relative refractive index difference delta n of the transition layer 3 in the germanium-fluorine co-doped quartz tube, the fluorine-doped quartz layer 4 in the fluorine-doped quartz tube and the pure quartz layer 1 Are all 0.007; the deposition temperature was 1900 deg.C, the rotation speed was 30rpm/min, the moving speed of the oxyhydrogen flame was 90mm/min, and the setting of the reaction materials during the deposition of the core region was different, as shown in Table 3. The electronic probe test result shows that the components and the average content of the central erbium-doped region 1 are respectively SiO 2 ：95.0Wt.％，Er 2 O 3 ：1.2Wt.％，Al 2 O 3 ：2.3Wt.％，Ce 2 O 3 ：15Wt.%; the composition and average content of the non-erbium-doped region 2 are respectively SiO 2 ：95.0Wt.％，GeO 2 :5.0Wt.%; the composition and the content of the transition layer 3 are respectively SiO 2 ：96.9Wt.％，GeO 2 :1.0Wt.%, F:2.1Wt.%; the fluorine-doped quartz layer 4 comprises SiO 2 :98.5Wt.%, F:1.5Wt.%. After the core rod is manufactured, a fluorine-doped quartz tube with a pure quartz barrier layer 5 is used as a sleeve, a proper sleeve process is selected according to the geometric parameters of the optical fiber so as to meet the requirement of the core-cladding ratio of the optical fiber, drawing and coating are carried out at the temperature of 1950 ℃, and the 4/125 mu m erbium-doped optical fiber is obtained, wherein the basic performance parameters of the optical fiber are shown in table 6.
TABLE 3 compositional flow rates (sccm) for each deposition layer in example two
| Core region composition | Number of deposition layers | SiCl 4 | Er(TMHD) 3 | Ce(TMHD) 3 | AlCl 3 | GeCl 4 |
| Non erbium doped region | 1～3 | 300 | / | / | / | 240 |
| Central erbium doped region | 1～10 | 300 | 360 | 1200 | 190 | / |
Example three:
the deposition method, the sleeve treatment method, the optical fiber structure and the like of the erbium-doped optical fiber core rod are the same as those of the first embodiment. Different in that the relative refractive index difference delta n of the transition layer 3 in the germanium-fluorine co-doped quartz tube and the fluorine-doped quartz layer 4 in the fluorine-doped quartz tube and the pure quartz layer 1 All are 0.0142; the deposition temperature was 1750 ℃, the rotation speed was 30rpm/min, the moving speed of oxyhydrogen flame was 100mm/min, and the setting of the reaction materials was different when the core region was deposited, as shown in table 4. The electronic probe test result shows that the components and the average content of the central erbium-doped region 1 are respectively SiO 2 ：97.95Wt.％，Er 2 O 3 ：0.37Wt.％，Al 2 O 3 ：0.68Wt.％，Ce 2 O 3 :1.0Wt.%; the composition and average content of the non-erbium-doped region 2 are respectively SiO 2 ：97.5Wt.％，GeO 2 :2.5Wt.%; the composition and content of the transition layer 3 are respectively SiO 2 ：94.9Wt.％，GeO 2 :1.4Wt.%, F:3.7Wt.%; the fluorine-doped quartz layer 4 comprises SiO 2 :96.7Wt.%, F:3.3Wt.%. After the core rod is manufactured, a fluorine-doped quartz tube with a pure quartz barrier layer 5 is used as a sleeve, and a proper sleeve process is selected according to the geometric parameters of the optical fiber so as to meet the requirement of the core-cladding ratio of the optical fiber. Wherein the outer diameters of the central erbium-doped region 1 and the non-erbium-doped region 2 of the core region are respectively 2.3mm and 3.0mm (the ratio of the outer diameters is 1: 1.3), the outer diameters of the core region and the transition layer 3 are respectively 3.0mm and 4.5mm (the ratio of the outer diameters is 1The fluorine-doped quartz layer 4 and the pure quartz barrier layer 5 have outer diameters of 12.5mm and 15.0mm, respectively (the ratio of the outer diameters is 1. Finally, the fiber was drawn and coated at 1950 ℃ to obtain 4/125 μm erbium-doped fiber, the basic performance parameters of which are shown in Table 6.
TABLE 4 composition flow rates (sccm) for each deposition layer in example three
| Core region composition | Number of deposition layers | SiCl 4 | Er(TMHD) 3 | Ce(TMHD) 3 | AlCl 3 | GeCl 4 |
| Non erbium doped region | 1～6 | 300 | / | / | / | 120 |
| Central erbium doped region | 1～10 | 300 | 120 | 800 | 50 | / |
Example four:
the deposition method, the sleeve treatment method, the optical fiber structure and the like of the erbium-doped optical fiber core rod are the same as those of the first embodiment. The difference is the relative refractive index difference delta n of the transition layer 3 in the germanium-fluorine co-doped quartz tube, the fluorine-doped quartz layer 4 in the fluorine-doped quartz tube and the pure quartz layer 1 Are all 0.020; the deposition temperature was 1300 deg.C, the rotation speed was 30rpm/min, the moving speed of the oxyhydrogen flame was 80mm/min, and the setting of the reaction materials at the time of depositing the core region was different, as shown in Table 5. The electronic probe test result shows that the components and the average content of the central erbium-doped region 1 are respectively SiO 2 ：99.7Wt.％，Er 2 O 3 ：0.1Wt.％，Al 2 O 3 :0.2Wt.%; the composition and average content of the non-erbium-doped region 2 are respectively SiO 2 ：98.5Wt.％，GeO 2 :1.5Wt.%; the composition and content of the transition layer 3 are respectively SiO 2 ：94.5Wt.％，GeO 2 :1.0Wt.%, F:4.5Wt.%; the fluorine-doped quartz layer 4 comprises SiO 2 :95.7Wt.%, F:4.3Wt.%. After the core rod is manufactured, the fluorine-doped quartz tube with the pure quartz barrier layer 5 is used as a sleeve, and a proper sleeve process is selected according to the geometric parameters of the optical fiber so as to meet the requirement of the core-cladding ratio of the optical fiber, which is the same as the embodiment I. Wherein the outer diameters of the central erbium-doped region 1 and the non-erbium-doped region 2 of the core region are 1.0mm and 1.05mm respectively (the ratio of the outer diameters is 1.05. Finally, the fiber was drawn and coated at 1950 ℃ to obtain 4/125 μm erbium doped fiber, the basic performance parameters of which are shown in table 6.
TABLE 5 composition flow rates (sccm) for each deposition layer in example four
| Core region composition | Number of deposition layers | SiCl 4 | Er(TMHD) 3 | AlCl 3 | GeCl 4 |
| Non erbium doped region | 1 | 300 | / | / | 70 |
| Central erbium doped region | 1～10 | 300 | 30 | 5 | / |
The basic performance parameter pairs of the fibers obtained in comparative example and four examples are shown in table 6, and it can be seen that the background loss of the erbium-doped fiber obtained by the method of the present invention is reduced compared to the comparative example, and the background loss is reduced with the decrease of the content of the co-dopant, indicating that the decrease of the content of the core co-dopant contributes to the reduction of the background loss of the fiber. Fig. 4 shows the gain of the erbium-doped fiber obtained in the comparative example and the first and third examples as a function of the irradiation dose, and it can be seen that the gain attenuation of the erbium-doped fiber obtained by the preparation method of the present invention is significantly reduced compared to the conventional erbium-doped fiber, and the irradiation resistance of the Ce-doped fiber is improved compared to that of the Ce-undoped fiber, indicating that the erbium-doped fiber having excellent irradiation resistance can be obtained by the method of the present invention.
TABLE 6 comparison of the Performance parameters of the erbium-doped fibers prepared in the comparative example and the four examples
It is to be understood that the foregoing is only illustrative of the present invention and is not to be construed as limiting the scope of the invention, which is intended to cover any variations and modifications in the principles and methods disclosed herein or in the specification and drawings, or any other related fields of technology, which fall within the spirit and scope of the present invention.
Claims (6)
1. An irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer is characterized in that: comprises a core area, a fluorine-doped cladding and a pure quartz barrier layer (5) which are sequentially coated on the outer surface of the core area from inside to outside, and the relative refractive index difference delta n between the fluorine-doped cladding and the pure quartz barrier layer (5) 1 The value range of (a) is 0.007 to 0.020;
the core region sequentially comprises a central erbium-doped region (1) and a non-erbium-doped region (2) from inside to outside;
the fluorine-doped cladding layer sequentially comprises a transition layer (3) and a fluorine-doped quartz layer (4) from inside to outside;
the refractive indexes of the transition layer (3) and the fluorine-doped quartz layer (4) are equal, and the value range of the relative refractive index difference delta n between the core region and the fluorine-doped cladding is 0.013 to 0.021;
the central erbium-doped region (1) comprises SiO 2 ：95.0~99.7Wt.%，Er 2 O 3 ：0.1~1.2Wt.%，Al 2 O 3 ：0.2~2.3Wt.%，Ce 2 O 3 ：0~1.5Wt.%；
The components and the contents of the non-erbium-doped region (2) are respectively SiO 2 ：95.0~98.5Wt.%，GeO 2 ：1.5~5.0Wt.%；
The components and the contents of the transition layer (3) are respectively SiO 2 ：93.0~96.9Wt.%，GeO 2 ：1.0~2.5Wt.%，F：2.1~4.5Wt.%；
The fluorine-doped quartz layer (4) comprises SiO 2 ：95.7~98.5Wt.%，F：1.5~4.3Wt.%。
2. The preform of claim 1, wherein: the ratio of the outer diameters of the central erbium-doped region (1) to the non-erbium-doped region (2) is 1:1.05 to 1.3, wherein the ratio of the outer diameter of the core area to the outer diameter of the transition layer (3) is 1:1.5 to 4, wherein the ratio of the outer diameter of the fluorine-doped quartz layer (4) to the outer diameter of the pure quartz barrier layer (5) is 1:1.05 to 1.2.
3. A preparation method of an irradiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer is characterized by comprising the following steps:
step 1) preparing a germanium-fluorine co-doped quartz tube and a fluorine-doped quartz tube by adopting a plasma chemical vapor deposition method;
step 2) taking the germanium-fluorine co-doped quartz tube prepared in the step 1) as a deposition liner tube, sequentially depositing a non-erbium-doped region (2) and a central erbium-doped region (1) by adopting an improved chemical vapor deposition and chelate gas phase doping method, and sintering at high temperature to form a solid core rod;
step 3) removing the pure quartz layer on the outermost layer of the solid core rod obtained in the step 2);
step 4) according to the requirement of core cladding ratio, combining the core rod processed in the step 3) with the fluorine-doped quartz tube prepared in the step 1) by adopting one or more sleeve processes to prepare the erbium-doped optical fiber preform rod in any one of claims 1-2;
and in the multiple casing process, the outer pure quartz barrier layer after the previous casing is removed.
4. The method for preparing the fluorine-doped cladding-based irradiation-resistant erbium-doped optical fiber preform according to claim 3, wherein the method comprises the following steps:
in the step 1), the germanium-fluorine co-doped quartz tube is sequentially arranged into a transition layer (3) and a pure quartz layer from inside to outside, and the ratio of the outer diameters of the transition layer (3) to the pure quartz layer is 1:1.05 to 1.2;
the fluorine-doped quartz tube is sequentially arranged into a fluorine-doped quartz layer (4) and a pure quartz barrier layer (5) from inside to outside, and the outer diameter ratio of the fluorine-doped quartz layer (4) to the pure quartz barrier layer (5) is 1:1.05 to 1.2.
5. The method for preparing a radiation-resistant erbium-doped optical fiber preform based on a fluorine-doped cladding layer according to claim 4, wherein in the step 2), the deposition parameters are as follows: the deposition temperature is 1300 to 1900 ℃, the rotating speed is 30rpm/min, and the moving speed of the oxyhydrogen flame is 80 to 100mm/min.
6. The method for preparing the fluorine-doped cladding-based irradiation-resistant erbium-doped optical fiber preform according to claim 5, wherein the method comprises the following steps:
step 3) specifically, removing the pure quartz layer on the outermost layer of the solid core rod obtained in the step 2) by adopting a mechanical grinding or polishing method;
in the step 4), when the sleeve process is carried out for multiple times, the outer pure quartz barrier layer (5) after the sleeve is last sleeved is removed by adopting a mechanical grinding or polishing method.
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