CN116813207A - Anti-radiation polarization-maintaining erbium-doped fiber and preparation method and application thereof - Google Patents
Anti-radiation polarization-maintaining erbium-doped fiber and preparation method and application thereof Download PDFInfo
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- 230000003471 anti-radiation Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000013307 optical fiber Substances 0.000 claims abstract description 73
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000010453 quartz Substances 0.000 claims abstract description 38
- 238000005253 cladding Methods 0.000 claims abstract description 37
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- 238000000034 method Methods 0.000 claims abstract description 19
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- 239000000463 material Substances 0.000 claims abstract description 14
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052796 boron Inorganic materials 0.000 claims abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 10
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 9
- 230000005855 radiation Effects 0.000 claims description 35
- 238000007254 oxidation reaction Methods 0.000 claims description 20
- 229910052698 phosphorus Inorganic materials 0.000 claims description 15
- 238000012123 point-of-care testing Methods 0.000 claims description 13
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 5
- 239000011574 phosphorus Substances 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000013519 translation Methods 0.000 claims description 5
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- 150000002500 ions Chemical class 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 1
- KWMNWMQPPKKDII-UHFFFAOYSA-N erbium ytterbium Chemical compound [Er].[Yb] KWMNWMQPPKKDII-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
-
- 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
- C03B37/01205—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments
- C03B37/01211—Manufacture of preforms for drawing fibres or filaments starting from tubes, rods, fibres or filaments by inserting one or more rods or tubes into a tube
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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
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
- G02B6/024—Optical fibres with cladding with or without a coating with polarisation maintaining properties
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The application discloses an anti-radiation polarization-maintaining erbium-doped fiber and a preparation method and application thereof, wherein the fiber comprises a fiber core, an inner cladding, stress rods and an outer cladding, the fiber core is arranged in the center of the inner cladding, the stress rods are symmetrically and alternately distributed on two sides of the fiber core and are positioned in the inner cladding, the outer cladding is coated on the surface of the inner cladding, the background materials of the inner cladding and the outer cladding are both quartz materials, and the stress rods are boron rods; the core comprises mole percentages based on 100% of the sum of the mole percentages of the components in the coreSuch as the following components: 0.01-0.05% Er 2 O 3 、0.6‑1.2%Al 2 O 3 、0.6‑1.2%P 2 O 5 、0.1‑0.5%Ce 2 O 3 0.02-0.1% CoO, the balance being SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the The anti-radiation performance of the active optical fiber is enhanced.
Description
Technical Field
The application relates to the technical field of optical fibers, in particular to an anti-radiation polarization-maintaining erbium-doped optical fiber, and a preparation method and application thereof.
Background
The radiation-resistant optical fiber has extremely high application prospect, becomes an important space technology for space optical communication, and has the characteristics of high transmission rate, large communication capacity, high confidentiality and the like. Erbium-doped optical fibers or erbium-ytterbium co-doped optical fibers are used as important gain media for 1.5 mu m-band lasers, have received great attention in the field of space optical communication, and have been verified along with some satellite lift-off. Therefore, the anti-irradiation performance of the rare earth doped optical fiber is enhanced, and the stability and the reliability of the optical fiber are improved, so that the development of space communication is promoted.
The optical fiber is invalid in the space environment and is mainly caused by the action of cosmic rays. The mechanism of action of spatial irradiation on the fiber includes total ionization dose effect (TID) and displacement damage dose effect (DDD). Where in the low orbit region of the earth (generally referred to as the orbit height < 2000km region), the TID effect is a major factor affecting the operating life of the fiber laser source. In the related art, rare earth doped optical fibers are often used as gain materials, which is a key for improving the irradiation resistance of a space light source.
However, unlike passive optical fibers, rare earth doped optical fibers need to be filled with various co-doped ions to improve the amplification performance of the optical fibers, and complex fiber core components are more prone to generating unstable factors such as defects, non-bridging oxygen and the like, and are extremely prone to failure when irradiated rays act, so that research on how to improve the anti-irradiation performance of the rare earth doped optical fibers is very necessary.
Disclosure of Invention
In view of the above, the application provides an anti-radiation polarization-maintaining erbium-doped optical fiber, and a preparation method and application thereof, which enhance the anti-radiation performance of the active optical fiber.
In order to achieve the technical purpose, the application adopts the following technical scheme:
the application provides an anti-radiation polarization-maintaining erbium-doped fiber, which comprises a fiber core, an inner cladding, stress rods and an outer cladding, wherein the fiber core is arranged in the center of the inner cladding; the fiber core comprises the following components in percentage by mole based on the sum of the mole percentages of the components in the fiber core taken as 100 percent: 0.01-0.05% Er 2 O 3 、0.6-1.2 %Al 2 O 3 、0.6-1.2 %P 2 O 5 、0.1-0.5 %Ce 2 O 3 0.02-0.1% CoO, the balance being SiO 2 。
Preferably, al 2 O 3 And P 2 O 5 The molar ratio of (2) is 1-1.2:1.
In a second aspect, the application provides a preparation method of an anti-radiation polarization-maintaining erbium-doped fiber, comprising the following steps:
s1, depositing SiO on the inner wall of a quartz tube by using an MCVD process 2 A loose layer;
s2. Will be deposited with SiO 2 Soaking the quartz tube in the loose layer in the doping solution, and then leading out to obtain a doped quartz tube; the doping solution comprises Er 3+ 、Al 3+ 、Ce 3+ Co and Co 2+ ；
S3, introducing the doped quartz tube into Cl 2 Drying to obtain a reaction tube;
s4, introducing O into the reaction tube 2 Performing oxidation reaction to obtain an oxidation reaction tube;
s5, introducing O into the oxidation reaction tube 2 POCl (Point of care testing) 3 Performing phosphorus deposition and sintering on the gas to obtain a mother rod;
s6, collapsing and burning the mother rod into an optical fiber preform;
and S7, sleeving the optical fiber preform into a quartz sleeve, compacting and annealing to obtain a solid rod, inserting a boron rod into the solid rod, and carrying out combined wire drawing to obtain the anti-irradiation polarization-maintaining erbium-doped optical fiber.
Preferably, er in the doping solution 3+ The concentration of the (B) is 0.001-0.02mol/L, al 3+ The concentration of the (B) is 0.1-0.5mol/L, ce 3+ The concentration of the (B) is 0.01-0.3mol/L, co 2+ The concentration of the (B) is 0.001-0.1mol/L.
Preferably, the specific steps of step S1 are as follows: introducing 100-300sccm SiCl into quartz tube 4 The deposition temperature is 1400-1700 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotation speed is 20-60rmp.
Preferably, the specific steps of step S3 are as follows: introducing 50-200sccm of Cl into the doped quartz tube 2 The drying temperature is 900-1200 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotating speed is 20-60rmp.
Preferably, the specific steps of step S4 are as follows: introducing 300-1000sccm of O into the reaction tube 2 The oxidation temperature is 1300-1650 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotation speed is 20-60rmp.
Preferably, the specific steps of step S5 are as follows: introducing 100-200sccm POCl into oxidation reaction tube 3 O of 500-1200sccm 2 The sintering temperature is 1350-1650 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotating speed is 20-60rmp.
In a third aspect, the application provides an application of an anti-radiation polarization-maintaining erbium-doped fiber under the condition of 1500GY or more.
Preferably, the application wavelength range of the anti-irradiation polarization-maintaining erbium-doped fiber is 1450-1600nm.
The beneficial effects of the application are as follows:
the application improves the anti-irradiation performance of the polarization-maintaining erbium-doped fiber and can be applied to the field of enhancing the conventional erbium-doped fiber; the radiation resistance of the optical fiber is provided by optimizing the purity of the components, the components of the optical fiber and the ion co-doping, and the method can be completed on the existing production equipment without upgrading and reconstruction, and has the advantages of excellent performance and low cost.
The application improves the irradiation resistance of the optical fiber, does not change the basic physical and chemical properties of the optical fiber, and maintains good compatibility with commercial quartz optical fiber.
The anti-radiation polarization-maintaining erbium-doped fiber prepared by the scheme is suitable for medium-low order mode application and is beneficial to long-term stable operation of space equipment.
Drawings
FIG. 1 shows RIGV values for different fibers;
FIG. 2 is a graph of background loss before and after irradiation of different fibers;
fig. 3 shows the extinction ratio of the fibers before and after irradiation of the different fibers.
Detailed Description
The present application will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The improvement of the scheme starts from the following steps: the optical fiber comprises a fiber core and a cladding, wherein the cladding is made of pure quartz glass material, siO 2 Si-O in the structural network is combined into a covalent bond with larger combination energy, so that the influence of radiation particles is smaller, and the good anti-radiation performance can be kept. The core part is usually made of glass materials formed by various oxides, and particularly, because the non-glass network forming body elements exist in a large amount, the improvement of the radiation resistance of the core is the core and the root point of the development of the radiation resistant optical fiber.
The inventors have unexpectedly found that color center suppression is necessary for improving the radiation resistance of the optical fiber, because point defects in the optical fiber material trap charged particles and eventually form color centers; the color center makes the optical fiber material show strong absorption to ultraviolet band, and induces the optical fiber to generate excessive background loss in the whole transmission range, thereby influencing the near infrared band signal transmission. The color center is generated from defects of the optical fiber material, fatigue bonds in the glass network or oxygen displacement in the grid.
The application provides an anti-radiation polarization-maintaining erbium-doped fiber, which comprises a fiber core, an inner cladding, stress rods and an outer cladding, wherein the fiber core is arranged in the center of the inner cladding, the stress rods are symmetrically and alternately distributed at two sides of the fiber core and are positioned in the inner cladding, and the outer cladding is arranged on the outer side of the fiber coreThe surface of the inner cladding layer is coated with the background materials of the inner cladding layer and the outer cladding layer which are both made of quartz, and the stress rod is a boron rod; the fiber core comprises the following components in percentage by mole based on the sum of the mole percentages of the components in the fiber core taken as 100 percent: 0.01-0.05% Er 2 O 3 、0.6-1.2 %Al 2 O 3 、0.6-1.2 %P 2 O 5 、0.1-0.5 %Ce 2 O 3 0.02-0.1% CoO, the balance being SiO 2 . The mole percent may be expressed as "mol-%".
It will be appreciated that the component of the core is SiO 2 -Al 2 O 3 -P 2 O 5 -Ce 2 O 3 -CoO-Er 2 O 3 The method comprises the steps of carrying out a first treatment on the surface of the SiO on the premise that the sum of the molar ratios of the components is 100 percent 2 ：Al 2 O 3 ：P 2 O 5 ：Ce 2 O 3 ：CoO：Er 2 O 3 The molar ratio of (1) is (96.5-99): (0.6-1.2): (0.6-1.2): (0.1-0.5): (0.02-0.1): (0.01-0.05); preferably, siO 2 ：Al 2 O 3 ：P 2 O 5 ：Ce 2 O 3 ：CoO：Er 2 O 3 The molar ratio of (1) is (96.5-99): 0.6:0.6: (0.1-0.5): (0.02-0.1): (0.01-0.05); suitably, but not by way of limitation, the core comprises the following components in parts by mole, provided that the sum of the molar ratios of the components is 100%: 0.01-0.05 part Er 2 O 3 0.6-1.2 parts of Al 2 O 3 0.6-1.2 parts of P 2 O 5 0.1-0.5 part of Ce 2 O 3 0.02-0.1 part of CoO, 96.5-99 parts of SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the Suitably, but not by way of limitation, the core comprises 0.01 to 0.05mol Er, provided that the sum of the molar ratios of the components is 100% 2 O 3 、0.6-1.2mol Al 2 O 3 、0.6-1.2 mol P 2 O 5 、0.1-0.5 mol Ce 2 O 3 、0.02-0.1 mol CoO、96.5-99 mol SiO 2 。
The content of Er element is not too high, otherwise clusters are formed in the fiber core, and the amplification efficiency of the fiber is reduced. Al and P are not too small, otherwise, the solubility of Er element in glass is reduced, so that clusters are easy to occur; al and P are not easy to be excessive, otherwise, the glass properties (softening temperature, refractive index, density and the like) are greatly influenced, and loss is possibly increased. Ce. Co element is doped in the fiber core as valence-changing element, but excessive Ce can cause the increase of the optical fiber loss, so that the irradiation resistance of the optical fiber can be further increased by introducing a certain amount of Co on the basis of Ce doping, and the adverse effect on the optical fiber is reduced.
In the scheme, charge or hole generated by radiation induction is captured by doping valence-variable elements (Ce and Co elements), the generation of color centers is inhibited, and the radiation resistance of the active optical fiber is enhanced. Irradiation causes the core material to generate free electron and hole pairs that combine with defects in the material itself to create a color center. The radiation color center causes the change of the glass network structure, thereby changing the coordination environment of the rare earth ions, not only causing transmission loss, but also changing the luminous characteristic of the rare earth ions. Thus Ce is incorporated in the optical fiber component 3+ (in the glass in +3 or +4 valence state) and Co 2+ (in the glass in +2 and +3 valence states) for adjusting the free electron and hole pairs induced by irradiation. The higher cations being combined with free electrons to lower-valence ions, e.g. Ce 4+ /Co 3+ +e - →Ce 3+ /Co 2+ The method comprises the steps of carrying out a first treatment on the surface of the The combination of a lower cation and a hole is converted into a higher cation, e.g. Ce 3+ /Co 2+ +hole→Ce 4+ /Co 3+ . Ce doping is beneficial to improving the radiation resistance of the optical fiber, but also causes the increase of the optical fiber loss, and a larger amount of Ce also causes the problems of the increase of the sintering temperature of the preform or devitrification and crystallization of the fiber core. Therefore, a small amount of Co element is doped to replace Ce, the doping amount of the valence-changing element can be increased, the optical fiber loss is not obviously increased, and meanwhile, the optical fiber preparation process is not greatly influenced.
Co and Ce are Co-doped, the atomic number of Co is lower than that of other valence-changing elements (such as Se), and Co 2+ /Co 3+ The ion radius is closer to that of P, al, si, O and other elements, so that the distortion degree of the glass network is lower, the defects are reduced, and the radiation-resistant effect is better; and compared with other valence-changing elementsIn addition, the soluble salt serving as the raw material Co of the doping liquid is not easy to deliquesce and smoke in the air, and has low toxicity, low storage difficulty and environmental friendliness.
Al 2 O 3 And P 2 O 5 The molar ratio of (1) to (1.2) to (1); preferably, al 2 O 3 And P 2 O 5 The molar ratio of (2) is 1:1. The Al element and the P element have linkage effect, and when the doping concentration ratio of the Al element and the P element is close to 1, the glass network structure is the most stable, and the defects are the least, so that the glass has more ideal irradiation resistance.
In this scheme, the P/Al ratio is optimized to suppress defect centers. In order to adjust the refractive index distribution of the optical fiber, regulate and control the rare earth ion luminescence or inhibit the cluster rate, P, al is introduced into the fiber core component in the scheme. However, the inventors have unexpectedly found that P, al element is contained in SiO 2 Defect centers are induced in the network and result in significant increases in the radiation-induced losses in the 800-1600nm band. P is doped in SiO 2 P=O bonds are formed in the network, and P is caused by irradiation 1 、P 2 、P 4 And two POHC defect centers, where P 1 Belongs to the trapping hole type color center and may be an important defect causing radiation-induced loss in the 1.5 μm band. Al is doped in SiO 2 Formation of [ AlO ] in network 4 - ]And under irradiation conditions, the aluminum oxygen defect center (Al-OHC) is also a trapping hole type color center, consisting of [ AlO ] 4 - /H + ]Tetrahedra lose H upon high energy irradiation + And Al-OHC is generated. If Al and P elements are doped synchronously, P=O bond and [ AlO ] 4 - ]Will be broken and form Al-O-P bonds, respectively, thus reducing (Al-OHC) and P 1 Defects. However, when the P or Al is excessive, the excessive P or Al is still singly bonded and forms a defect center, so that the radiation resistance of the optical fiber is reduced to a certain extent.
The application provides a preparation method of an anti-radiation polarization-maintaining erbium-doped fiber, which comprises the following steps:
s1, depositing SiO on the inner wall of a quartz tube by using an MCVD process 2 A loose layer;
s2. Will be deposited with SiO 2 The quartz tube of the loose layer is soaked in the doping solution,then leading out to obtain a doped quartz tube; the doping solution comprises Er 3+ 、Al 3+ 、Ce 3+ Co and Co 2+ ；
S3, introducing the doped quartz tube into Cl 2 Drying to obtain a reaction tube;
s4, introducing oxygen into the reaction tube to perform oxidation reaction to obtain an oxidation reaction tube;
s5, introducing O into the oxidation reaction tube 2 POCl (Point of care testing) 3 Performing phosphorus deposition and sintering to obtain a mother rod;
s6, collapsing and burning the mother rod into an optical fiber preform;
and S7, sleeving the optical fiber preform into a quartz sleeve, compacting and annealing to obtain a solid rod, inserting a boron rod into the solid rod, and carrying out combined wire drawing to obtain the anti-irradiation polarization-maintaining erbium-doped optical fiber.
Preferably, er in the doping solution 3+ The concentration of the (B) is 0.001-0.02mol/L, al 3+ The concentration of the (B) is 0.1-0.5mol/L, ce 3+ The concentration of the (B) is 0.01-0.3mol/L, co 2+ The preparation concentration of the (B) is 0.001-0.1mol/L; when the preparation process parameters are fixed, the molar concentration of ions in the doping solution and the molar concentration of each oxide component in the fiber core are approximately in linear relation; in the scheme, the liquid phase doping solution contains Al 3+ 、Er 3+ 、Ce 3+ And Co 2+ The soluble compound of (2) has a purity of 5N or more. The vapor deposition material is SiCl 4 、POCl 3 And the purity of the raw materials reaches 5N or more, and when vapor deposition is adopted, the purity of bubbling gas can reach 99.999999%; the purity of the raw materials is improved, the content of coloring ions is strictly controlled, and the radiation resistance of the optical fiber can be further improved; the reason for this is that the optical fiber loss is increased because of the occurrence of "color center", and the elements which are extremely liable to form color center are mainly OH-and transition metal elements, so that the irradiation resistance of the optical fiber is improved and the introduction of coloring ions is reduced.
The specific steps of the step S1 are as follows: introducing 100-300sccm SiCl into quartz tube 4 The deposition temperature is 1400-1700 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotation speed is 20-60rmp, so as to deposit porous pure on the inner wall of the quartz tubeSiO 2 And (5) loosening the layer. The phosphorus silicate loose layer easily causes excessive doping of P, so that the proportion of P and Al is difficult to control, and the pure SiO is used in the application 2 And (5) loosening the layer.
The specific steps of the step S2 are as follows: will be deposited with SiO 2 Soaking the quartz tube in the loose layer in the doping solution for 1-2h, and then guiding out to obtain the doped quartz tube; the doping solution comprises Er 3+ 、Al 3+ 、Ce 3+ Co and Co 2+ 。
The step S3 comprises the following specific steps: the doped quartz tube is remounted on an MCVD lathe for drying, and 50-200sccm of Cl is introduced into the doped quartz tube 2 Residual hydroxyl and water are removed, the drying temperature is 900-1200 ℃, the translational speed of a main lamp is 50-150mm/min, and the rotating speed is 20-60rmp. The scheme improves the water removal process through the step S3, reduces the hydroxyl content and improves the radiation resistance of the optical fiber.
The specific steps of the step S4 are as follows: introducing 300-1000sccm O into the reaction tube at high temperature 2 Carrying out oxidation reaction at 1300-1650 ℃ and a main lamp translation speed of 50-150mm/min and a rotation speed of 20-60rmp; the purpose is to make Er 3+ 、Al 3+ 、Ce 3+ And Co 2+ Corresponding oxidation to Er 2 O 3 、Al 2 O 3 、Ce 2 O 3 And CoO.
The specific steps of the step S5 are as follows: introducing 100-200sccm POCl into oxidation reaction tube 3 O of 500-1200sccm 2 Sintering temperature is 1350-1650 ℃, main lamp translation speed is 50-150mm/min, and rotation speed is 20-60rmp; POCl in this range 3 The amount of (C) may be in a molar ratio of (1-1.2) to (0.8-1) with Al.
The specific steps of the step S7 are as follows: the optical fiber preform is sleeved into a quartz sleeve, is compacted by adopting a rod sleeving process, is then placed into an annealing furnace for annealing at 800-900 ℃ for 4-8 hours to obtain a solid rod, the solid rod after annealing is subjected to punching treatment, a boron rod is inserted, and the boron rod and the solid rod after punching are subjected to combined wire drawing to obtain the anti-radiation polarization-maintaining erbium-doped optical fiber.
The application provides application of an anti-radiation polarization-maintaining erbium-doped fiber under the condition of 1500GY or more, and in some embodiments, the application wavelength is 1450-1600nm.
The present application is further illustrated by the following specific examples.
Example 1
The anti-irradiation polarization-maintaining erbium-doped fiber comprises a fiber core, an inner cladding, stress rods and an outer cladding, wherein the fiber core is arranged in the center of the inner cladding, the stress rods are symmetrically and alternately distributed on two sides of the fiber core and are positioned in the inner cladding, the outer cladding is coated on the surface of the inner cladding, the background materials of the inner cladding and the outer cladding are both made of quartz, and the stress rods are boron rods; the fiber core comprises the following components in mole percent: 0.01% Er 2 O 3 ，0.6%Al 2 O 3 ，0.6%P 2 O 5 ，0.1%Ce 2 O 3 ，0.02%CoO ，98.67 %SiO 2 。
A preparation method of an anti-radiation polarization-maintaining erbium-doped fiber comprises the following steps:
s1, depositing SiO on the inner wall of a quartz tube by using an MCVD process 2 Loose layer: 100sccm of SiCl was introduced into a quartz tube 4 The deposition temperature is 1400 ℃, the translational speed of the main lamp is 50mm/min, and the rotation speed is 20rmp;
s2. Will be deposited with SiO 2 Soaking the quartz tube with loose layer in doping solution containing Er 3+ 、Al 3+ 、Ce 3+ And Co 2+ The solute is ErCl 3 0.004mol/L，AlCl 3 0.24mol/L，CeCl 3 0.04mol/L and CoCl 2 0.008mol/L, soaking for 1.5h, then leading out the solution, and drying to obtain a doped quartz tube;
s3, reinstalling the doped quartz tube on an MCVD lathe, and introducing 200sccm Cl 2 Drying at 900 deg.c with main lamp translation speed of 50mm/min and rotation speed of 20rmp to eliminate residual hydroxyl radical and obtain reaction tube;
s4, after the reaction tube is dried, 300sccm O is introduced at high temperature 2 The oxidation temperature is 1300 ℃, the translation speed of the main lamp is 50mm/min, the rotation speed is 20rmp, and the oxidation reaction is carried out to obtain an oxidation reaction tube;
s5, introducing 100sccm POCl into the oxidation reaction tube 3 And 800sccm O 2 Performing phosphorus deposition and sintering, wherein the sintering temperature is 1400 ℃, the translational speed of a main lamp is 50mm/min, and the rotating speed is 20rmp, so as to obtain a mother rod;
s6, collapsing and burning the mother rod into an optical fiber preform;
and S7, sleeving the optical fiber preform into a quartz sleeve, compacting by adopting a rod sleeving process, then placing the quartz sleeve into an annealing furnace for annealing at the annealing temperature of 800 ℃ for 4 hours to obtain a solid rod, punching the annealed solid rod, inserting a boron rod, and carrying out combined wire drawing on the boron rod and the punched solid rod to obtain the anti-radiation polarization-maintaining erbium-doped optical fiber.
Example 2
A radiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1, except that Er was included in the doping solution 3+ 、Al 3+ Ce3+ and Co 2+ The solute is ErCl 3 0.008mol/L，AlCl 3 0.24mol/L，CeCl 3 0.1mol/L and CoCl 2 0.035mol/L. The fiber core comprises the following components in mole percent: 0.02% Er 2 O，0.6%Al 2 O 3 ，0.6%P 2 O 5 ，0.25%Ce 2 O 3 ，0.0875%CoO，98.4425%SiO 2 。
Example 3
A radiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1, except that Er was included in the doping solution 3+ 、Al 3+ Ce3+ and Co 2+ The solute is ErCl 3 0.008mol/L，AlCl 3 0.48mol/L，CeCl 3 0.1mol/L and CoCl 2 0.04mol/L; in step S5, 200sccm POCl is introduced 3 The method comprises the steps of carrying out a first treatment on the surface of the The fiber core comprises the following components in mole percent: 0.02% Er 2 O 3 ，1.2%Al 2 O 3 ，1.2%P 2 O 5 ，0.25%Ce 2 O 3 ，0.1%CoO，97.23%SiO 2 。
Example 4
A radiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1 except that the dopant solution was wrapped in a bagEr is included 3+ 、Al 3+ 、Ce 3+ And Co 2+ The solute is ErCl 3 0.02mol/L，AlCl 3 0.24mol/L，CeCl 3 0.2mol/L and CoCl 2 0.04mol/L; the fiber core comprises the following components in mole percent: 0.05% Er 2 O 3 ，0.6%Al 2 O 3 ，0.6%P 2 O 5 ，0.5%Ce 2 O 3 ，0.1%CoO，98.15%SiO 2 。
Comparative example 1
A radiation-resistant polarization maintaining erbium doped fiber was the same as in example 1 except that the core comprised 0.2 mol% CoO.
Comparative example 2
A radiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1 except that the core comprised 0.6mol% of Ce 2 O 3 。
Comparative example 3
A radiation-resistant polarization-maintaining erbium-doped fiber is the same as in example 1 except that the core does not include P, al 2 O 3 The molar ratio of (2) was 0.6%.
Comparative example 4
A radiation-resistant polarization-maintaining erbium-doped fiber is the same as in example 1 except that the core does not include Al, P 2 O 5 The molar ratio of (2) was 0.6%.
Comparative example 5
A radiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1, except that the core comprised 0.5% Al, 0.1% P 2 O 5 。
Comparative example 6
A radiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1 except that the core comprised 0.5% P 2 O 5 ，0.1 % Al。
Comparative example 7
The irradiation-resistant polarization-maintaining erbium-doped fiber was the same as in example 1 except that step S3 was not included.
Evaluation test
The optical fibers obtained in each example and comparative example were tested, and the test results are shown in table 1, and the test contents are as follows:
RIGV test: the optical fibers prepared in each example and comparative example were subjected to 1500Gy total dose irradiation by the institute of irradiation processing in the national institute of sciences of Hubei province, and then the gain spectrum attenuation before and after the irradiation of the optical fibers was respectively tested, and the irradiation resistance of the optical fibers was characterized by mean radiation induced gain variation (RIGV, unit: dB/krad) at a wavelength of 1533.46 nm.
Optical fiber background loss test: each sample was subjected to loss testing prior to irradiation to monitor 1095nm wavelength loss as background loss of the fiber.
Polarization extinction ratio test: the optical fiber polarization maintaining performance test is carried out by adopting an extinction ratio tester, and the length of all samples to be tested is 5m.
TABLE 1 different fiber test results
Examples 1 to 4 were numbered 1 to 4, comparative examples 1 to 7 were numbered 5 to 11, and optical fibers 1 to 11 were tested according to the numbers listed, as shown in FIG. 1, which shows the results of the RIGV values of different optical fibers 1 to 11, FIG. 2, which shows the background loss before and after irradiation of different optical fibers 1 to 11, and FIG. 3, which shows the extinction ratio before and after irradiation of different optical fibers 1 to 11; it can be seen that in the range of the core component of the present application (examples 1-4), both the gain attenuation and the background loss due to the optical fiber radiation remain at low levels, indicating that the optical fiber has good radiation resistance. Comparative example 1 only increased CoO content compared to example 1, and the fiber background loss increased significantly due to excessive induced glass network structure changes. Comparative example 2 Ce is increased compared to example 1 2 O 3 Content, again, causes a substantial increase in the background loss of the fiber. Comparative example 3 and comparative example 4 cancel P separately from example 1 2 O 5 And Al 2 O 3 Doping, because of the formation of groups each susceptible to radiation particles, results in a serious decrease in the radiation resistance of the optical fiber. Comparative examples 5 and 6 are doped with Al, respectively, as compared with example 1 2 O 3 Excess and P 2 O 5 Excessive, small portions of Al-O-P bonds are formed, which to some extent improves the resistance to irradiation, but due to the presence of a large amount of [ AlO ] 4 - ]Or p=o, the irradiation resistance is not improved at all. Comparative example 7 uses exactly the same composition as example 1, but eliminates drying, so that a large amount of-OH remains, not only the irradiation resistance is weakened, but also a significant increase in the loss of the optical fiber is caused, and there is a serious problem even in the conventional environmental use.
According to the application, the polarization maintaining performance of the optical fiber sample before and after irradiation is synchronously tested, and the irradiation has no obvious influence on the polarization maintaining performance of the optical fiber according to the extinction ratio test result. Therefore, examples 1 to 4 have good irradiation resistance, low background loss and polarization maintaining performance, and are expected to play an important role in the irradiation severe environment.
The present application is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present application are intended to be included in the scope of the present application.
Claims (10)
1. The anti-radiation polarization-maintaining erbium-doped fiber is characterized by comprising a fiber core, an inner cladding, stress rods and an outer cladding, wherein the fiber core is arranged in the center of the inner cladding, the stress rods are symmetrically distributed at intervals on two sides of the fiber core and are positioned in the inner cladding, the outer cladding is coated on the surface of the inner cladding, the background materials of the inner cladding and the outer cladding are both quartz materials, and the stress rods are boron rods; the fiber core comprises the following components in percentage by mole based on the sum of the mole percentages of the components in the fiber core taken as 100 percent: 0.01-0.05% Er 2 O 3 、0.6-1.2 %Al 2 O 3 、0.6-1.2%P 2 O 5 、0.1-0.5%Ce 2 O 3 0.02-0.1% CoO, the balance being SiO 2 。
2. The radiation-resistant polarization-maintaining erbium-doped fiber according to claim 1, wherein said Al 2 O 3 With said P 2 O 5 The molar ratio of (2) is 1-1.2:1.
3. A method for preparing the radiation-resistant polarization-maintaining erbium-doped fiber according to any one of claims 1 to 2, comprising the steps of:
s1, depositing SiO on the inner wall of a quartz tube by using an MCVD process 2 A loose layer;
s2. Will be deposited with SiO 2 Soaking the quartz tube in the loose layer in the doping solution, and then leading out to obtain a doped quartz tube; the doping solution comprises Er 3+ 、Al 3+ 、Ce 3+ Co and Co 2+ ；
S3, introducing Cl into the doped quartz tube 2 Drying to obtain a reaction tube;
s4, introducing O into the reaction tube 2 Performing oxidation reaction to obtain an oxidation reaction tube;
s5, introducing O into the oxidation reaction tube 2 POCl (Point of care testing) 3 Performing phosphorus deposition and sintering on the gas to obtain a mother rod;
s6, collapsing and burning the mother rod into an optical fiber preform;
and S7, sleeving the optical fiber preform into a quartz sleeve, compacting and annealing to obtain a solid rod, inserting a boron rod into the solid rod, and carrying out combined wire drawing to obtain the anti-radiation polarization-maintaining erbium-doped optical fiber.
4. The method for preparing radiation-resistant polarization-maintaining erbium-doped fiber according to claim 3, wherein Er in the doping solution 3+ The concentration of the (B) is 0.001-0.02mol/L, al 3+ The concentration of the (B) is 0.1-0.5mol/L, ce 3+ The concentration of the Co is 0.01-0.3mol/L 2+ The concentration of the (B) is 0.001-0.1mol/L.
5. The method for preparing the anti-radiation polarization-maintaining erbium-doped fiber according to claim 3, wherein the specific steps of the step S1 are as follows: introducing 100-300sccm SiCl into the quartz tube 4 The deposition temperature is 1400-1700 ℃, and the translation speed of the main lampThe degree is 50-150mm/min, and the rotating speed is 20-60rmp.
6. The method for preparing the anti-radiation polarization-maintaining erbium-doped fiber according to claim 3, wherein the step S3 comprises the following specific steps: introducing 50-200sccm of Cl into the doped quartz tube 2 The drying temperature is 900-1200 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotating speed is 20-60rmp.
7. The method for preparing the anti-radiation polarization-maintaining erbium-doped fiber according to claim 3, wherein the step S4 comprises the following specific steps: introducing 300-1000sccm of O into the reaction tube 2 The oxidation temperature is 1300-1650 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotation speed is 20-60rmp.
8. The method for preparing the anti-radiation polarization-maintaining erbium-doped fiber according to claim 3, wherein the step S5 comprises the following specific steps: introducing 100-200sccm POCl into the oxidation reaction tube 3 O of 500-1200sccm 2 The sintering temperature is 1350-1650 ℃, the translational speed of the main lamp is 50-150mm/min, and the rotating speed is 20-60rmp.
9. Use of the radiation-resistant polarization-maintaining erbium-doped fiber obtained by the preparation method according to any one of claims 3 to 8 under the condition of 1500GY or more.
10. The use according to claim 9, wherein the radiation-resistant polarization-maintaining erbium-doped fiber has an application wavelength in the range 1450-1600nm.
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