CN117585895A - Secondary carrier gas-based radiation-resistant three-cladding erbium-ytterbium co-doped fiber and preparation method thereof - Google Patents
Secondary carrier gas-based radiation-resistant three-cladding erbium-ytterbium co-doped fiber and preparation method thereof Download PDFInfo
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- 239000012159 carrier gas Substances 0.000 title claims abstract description 75
- 238000005253 cladding Methods 0.000 title claims abstract description 45
- KWMNWMQPPKKDII-UHFFFAOYSA-N erbium ytterbium Chemical compound [Er].[Yb] KWMNWMQPPKKDII-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 239000000835 fiber Substances 0.000 title claims abstract description 43
- 230000005855 radiation Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000013307 optical fiber Substances 0.000 claims abstract description 108
- 239000007789 gas Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 38
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 claims abstract description 27
- 229910052805 deuterium Inorganic materials 0.000 claims abstract description 27
- 238000004061 bleaching Methods 0.000 claims abstract description 22
- -1 erbium ions Chemical class 0.000 claims abstract description 22
- 230000008569 process Effects 0.000 claims abstract description 13
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 8
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 7
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 57
- 235000012239 silicon dioxide Nutrition 0.000 claims description 52
- 239000010453 quartz Substances 0.000 claims description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000001307 helium Substances 0.000 claims description 8
- 229910052734 helium Inorganic materials 0.000 claims description 8
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 238000007740 vapor deposition Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000004017 vitrification Methods 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 abstract description 12
- 230000000052 comparative effect Effects 0.000 description 17
- 239000010410 layer Substances 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 9
- 230000003471 anti-radiation Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 230000002829 reductive effect Effects 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 241000473945 Theria <moth genus> Species 0.000 description 3
- 230000001965 increasing effect Effects 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052754 neon Inorganic materials 0.000 description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052775 Thulium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005491 wire drawing Methods 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
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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
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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)
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- Organic Chemistry (AREA)
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Abstract
The invention discloses a radiation-resistant three-cladding erbium-ytterbium co-doped fiber based on secondary carrier gas and a preparation method thereof, comprising the following steps: s1, obtaining an optical fiber preform, wherein the optical fiber preform is doped with erbium ions, ytterbium ions and cerium ions; s2, introducing mixed gas containing deuterium into the optical fiber preform for carrying out primary carrier gas, and then sequentially carrying out irradiation treatment and thermal bleaching treatment to obtain a post-treatment optical fiber preform; s3, manufacturing the post-treatment optical fiber preform into a three-cladding optical fiber by utilizing a tube rod drawing process; s4, introducing mixed gas containing deuterium into the three-cladding optical fiber for secondary carrier gas, and obtaining the radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber; according to the scheme, through twice carrier gas treatment, the anti-irradiation performance of the three-cladding optical fiber is improved, and meanwhile, the optical performance is not affected.
Description
Technical Field
The invention relates to the technical field of erbium-ytterbium co-doped fibers, in particular to an irradiation-resistant three-cladding erbium-ytterbium co-doped fiber based on secondary carrier gas and a preparation method thereof.
Background
The optical fiber has the advantages of high transmission efficiency, low loss, light weight, static interference resistance and the like, and has been widely applied in the field of communication. The rare earth (such as Yb, er and Tm) doped quartz fiber laser or amplifier has the advantages of light weight, small volume, high electro-optical conversion efficiency, high peak power, narrow line width and the like, and has important application value in the aspects of space communication, laser radar, space garbage treatment, airborne laser weapons and the like.
However, lasers or amplifiers are subject to harsh particle radiation (e.g., protons, electrons, X-rays, and gamma rays) when performing space tasks. Particle radiation can lead to a sharp increase in the loss of the active fiber in the laser or amplifier, a significant drop in the laser slope efficiency, and even no laser output in severe cases. Related technology, more commonly used technology is to improve the anti-radiation performance of the optical fiber by compounding different anti-radiation ions.
However, the efficiency of erbium ytterbium anti-radiation optical fiber is generally about 35%, and if the anti-radiation performance of the optical fiber is improved by means of component optimization under the requirement, only partial optical performance can be sacrificed, so that a method for balancing the optical performance and the anti-radiation performance of the optical fiber is urgently needed.
Disclosure of Invention
In view of the above, the application provides a radiation-resistant three-cladding erbium-ytterbium co-doped fiber based on secondary carrier gas and a preparation method thereof, which solve the problem of balancing the radiation resistance and the optical performance of the three-cladding erbium-ytterbium co-doped fiber.
In order to achieve the technical purpose, the application adopts the following technical scheme:
in a first aspect, the present application provides a method for preparing an irradiation-resistant tri-clad erbium ytterbium co-doped fiber based on a secondary carrier gas, including the following steps:
s1, obtaining an optical fiber preform, wherein the optical fiber preform is doped with erbium ions, ytterbium ions and cerium ions;
s2, introducing mixed gas containing deuterium into the optical fiber preform for carrying out primary carrier gas, and then sequentially carrying out irradiation treatment and thermal bleaching treatment to obtain a post-treatment optical fiber preform;
s3, manufacturing the post-treatment optical fiber preform into a three-cladding optical fiber by utilizing a tube rod drawing process;
s4, introducing mixed gas containing deuterium into the three-cladding optical fiber for secondary carrier gas, and obtaining the radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber.
Preferably, in step S2, the primary carrier gas has a carrier gas pressure of 2.1-2.5MPa, a carrier gas temperature of 100-200deg.C, and a carrier gas time of 0.5-5h.
Preferably, in step S4, the carrier gas pressure of the secondary carrier gas is 0.5-1.6Mpa, the carrier gas temperature is 20-80 ℃ and the carrier gas time is 8-10h.
Preferably, in step S2, the ratio of deuterium in the mixed gas is 84.6-100%; in the step S4, the ratio of deuterium in the mixed gas is 30-75%.
Preferably, in the step S2, the irradiation treatment dose is 50-5000Gy, and the irradiation rate is 10-200Gy/h.
Preferably, in step S2, the temperature of the thermal bleaching is 500-1200 ℃.
Preferably, the preparation process of the optical fiber preform comprises the following steps:
s11, depositing a silicon dioxide porous layer on the inner wall of the pure quartz tube by using a vapor deposition method to obtain a reaction tube;
s12, soaking the reaction tube in a doping solution containing erbium ions, ytterbium ions and cerium ions, and drying by utilizing nitrogen to obtain a doped quartz tube;
s13, introducing chlorine into the doped quartz tube at 500-1200 ℃, and then passing phosphorus oxychloride and oxygen at 1200-1400 ℃ to obtain a deposited quartz tube;
s14, introducing oxygen and helium into the deposited quartz tube at 1900-2200 ℃ for vitrification, and then collapsing by a collapse method to obtain the optical fiber preform.
Preferably, the process of step S3 is:
s31, inserting the post-treatment optical fiber preform into an inner layer sleeve, sleeving the inner layer sleeve into an outer layer sleeve, and drawing by using a tube rod method to obtain drawn optical fibers; the inner sleeve is made of octagonal pure quartz, and the outer sleeve is made of fluorine-doped quartz;
s32, coating a low refractive index coating on the outer wall of the drawn optical fiber to obtain the three-clad optical fiber.
In a second aspect, the present application provides a radiation-resistant triple-clad erbium ytterbium co-doped fiber.
In a third aspect, the application provides an application of an irradiation-resistant three-cladding erbium-ytterbium co-doped fiber under an irradiation condition of more than or equal to 1000 Gy.
The beneficial effects of this application are as follows: the method improves the irradiation resistance of the three-cladding erbium-ytterbium co-doped optical fiber by matching the procedures of primary carrier gas, pre-irradiation, thermal bleaching and secondary carrier gas, and simultaneously ensures that the optical fiber efficiency of the three-cladding erbium-ytterbium co-doped optical fiber is not reduced under the same condition.
Detailed Description
The present invention 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 invention 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 invention.
Interpretation of the terms
And (3) thermal bleaching: and (3) preserving the heat of the irradiated optical fiber preform for 1-2 hours at the temperature of 500-1200 ℃.
Low refractive index coating: a coating having a refractive index lower than 1.38.
In a first aspect, the present application provides a method for preparing an irradiation-resistant tri-clad erbium ytterbium co-doped fiber based on a secondary carrier gas, including the following 4 steps:
s1, obtaining an optical fiber preform, wherein the optical fiber preform is doped with erbium ions, ytterbium ions and cerium ions;
the specific process of the optical fiber preform in the step S1 is as follows:
s11, depositing a porous layer of silicon dioxide on the inner wall of a pure quartz tube by a vapor deposition method to obtain a reaction tube;
s12, introducing a doping solution into the treated reaction tube, wherein the doping solution comprises but is not limited to Er 3+ (0.5～2g/L)、Yb 3+ (0.05～5.0g/L)、Ce 3+ (0.22-0.8 g/L), soaking the quartz tube in the doping solution at 20-60 ℃ for 2-10h, wherein the rotation speed of the quartz tube is 10-50r/min during soaking, guiding the doping solution out of the quartz tube, drying the quartz tube by nitrogen, and controlling the flow rate of the nitrogen to be 15-30m 3 Obtaining a doped quartz tube; the book is provided withThe porous structure in the quartz tube adsorbs ions in the doping solution, and the absorption of the porous structure to the ions is further promoted under the heating and rotating conditions;
s13, introducing chlorine into the doped quartz tube, heating at 500-1200 ℃ to remove water and hydroxyl in the tube; introducing phosphorus oxychloride and oxygen into the quartz tube after introducing chlorine, and heating the quartz tube at 1200-1400 ℃ to enable P to be P 2 O 5 Is deposited into the quartz tube in the form of (a) to obtain a deposited quartz tube;
s14, introducing oxygen and helium into the deposited quartz tube, vitrifying at 1900-2200 ℃ to enable rare earth ions in the doping solution to be converted into a glass structure through melting vitrification of the porous structure; then the quartz tube is collapsed into a solid optical fiber preform doped with anti-radiation ions by a collapse method;
s2, introducing mixed gas containing deuterium into the optical fiber preform obtained in the step S1 for carrying out primary carrier gas, and then sequentially carrying out irradiation treatment and thermal bleaching treatment to obtain a post-treatment optical fiber preform;
in the step, deuterium and other gases are included in the mixed gas, wherein the other gases include but are not limited to inert gases such as nitrogen, helium, neon and the like, and the optical fiber preform is taken out for irradiation treatment and then for thermal bleaching treatment; the dose of the irradiation treatment is 50-5000Gy, and the irradiation rate is 10-200Gy/h; the temperature of the thermal bleaching is 500-1200 ℃; the irradiation dose and the irradiation rate are high, so that irreversible damage can be generated on the preform, and the treatment effect can be affected.
The specific step of carrying gas is that the optical fiber preform is put into a high-pressure tank, mixed gas containing deuterium gas is introduced to carry out primary carrying gas, the carrying gas pressure of the primary carrying gas is 2.1-2.5Mpa, the carrying gas temperature is 100-200 ℃ and the carrying gas time is 0.5-5h in step S2.
After primary carrier gas, irradiation treatment and thermal bleaching treatment are also carried out, and the effect is that on one hand, the irradiation sensitivity of the optical fiber preform is reduced and the irradiation performance is improved by pre-irradiation; on the other hand, the preform can form a color center after irradiation, which is a defect, the color center can be repaired by thermal bleaching, and the primary carrier gas is carried out before irradiation so as to reduce the damage of irradiation rays to the preform and reduce the generation of the color center.
S3, manufacturing the post-treatment optical fiber preform into a three-cladding optical fiber by utilizing a tube rod drawing process;
the specific preparation process of the step S3 three-cladding optical fiber is as follows:
s31, inserting the post-treatment optical fiber preform into an inner layer sleeve, sleeving the inner layer sleeve into an outer layer sleeve, and drawing by using a tube rod method to obtain drawn optical fibers; the inner sleeve is made of octagonal pure quartz, and the outer sleeve is made of fluorine-doped quartz; controlling the wiredrawing speed to be 100-200m/min, the tension to be 10-150g, and controlling the temperature to be 1900-2100 ℃;
s32, coating a low refractive index coating on the outer wall of the drawn optical fiber, and coating the optical fiber under the pressure of 1-100pa to obtain the three-clad optical fiber.
The three-cladding optical fiber obtained in the step S3 takes an optical fiber preform as a fiber core, the fiber core size is controlled to be 9-12 mu m in the drawing process of the step S31, the first cladding is an octagonal pure quartz layer, the second cladding is a fluorine-doped quartz layer, and the third layer is a low-refractive-index coating.
S4, introducing mixed gas containing deuterium into the three-cladding optical fiber for secondary carrier gas, and obtaining the radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber.
The specific step of carrying gas is that the three-cladding optical fiber is put into a high-pressure tank, mixed gas containing deuterium is introduced to carry out secondary carrying gas, and in the step S4, the carrying gas pressure of the secondary carrying gas is 0.5-1.6Mpa, the carrying gas temperature is 20-80 ℃, and the carrying gas time is 8-10h.
In this step, deuterium and other gases are included in the mixed gas, and other gases include, but are not limited to, inert gases such as nitrogen, helium, neon, and the like.
The scheme improves the irradiation resistance of the three-cladding erbium-ytterbium co-doped fiber through twice carrier gas, and has the following mechanism: after the optical fiber preform doped with the anti-irradiation ions is obtained, carrying out primary carrier gas, wherein the primary carrier gas aims at eliminating material defects in quartz glass on the whole, inhibiting the condition of uneven stress distribution in the optical fiber preform, reducing the attenuation of the post-treatment preform to be drawn, and simultaneously effectively reducing the irradiation sensitivity of the optical fiber; after drawing, a three-clad optical fiber is obtained, and secondary carrier gas is carried out, wherein the purpose of the secondary carrier gas is to further improve the irradiation resistance of the optical fiber without affecting the optical performance.
It is noted that, the primary carrier gas condition of step S2 is different from the secondary carrier gas condition of step S4, and the primary carrier gas is low in temperature and long in time compared with the secondary carrier gas, and the reason is that the secondary carrier gas is used for the three-clad optical fiber, the coating layer of the three-clad optical fiber is aged due to the fact that the temperature is too high, the strength of the optical fiber is damaged, the deuterium gas permeability effect is poor due to the fact that the temperature is too low, the improvement of the permeation amount of the carrier gas is facilitated by increasing the duration of the secondary carrier gas, and finally the irradiation resistance of the three-clad optical fiber is further improved.
In the step S2, the ratio of deuterium in the mixed gas is 84.6-100%; in the step S4, the ratio of deuterium in the mixed gas is 30-75%, and in the range, the deuterium permeation effect is good.
In a second aspect, the application provides an irradiation-resistant three-cladding erbium-ytterbium co-doped optical fiber, wherein the three-cladding optical fiber uses an optical fiber preform as a fiber core, the first cladding is an octagonal pure quartz layer, the second cladding is a fluorine-doped quartz layer, and the third layer is a low refractive index coating.
In a third aspect, the application provides an application of an irradiation-resistant three-cladding erbium-ytterbium co-doped fiber under an irradiation condition of more than or equal to 1000 Gy.
Further description will be given below by way of specific examples.
Example 1
A preparation method of a radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber based on secondary carrier gas comprises the following steps:
s1, obtaining an optical fiber preform, wherein the optical fiber preform is doped with erbium ions, ytterbium ions and cerium ions:
s11, depositing a porous layer of silicon dioxide on the inner wall of a pure quartz tube by a vapor deposition method to obtain a reaction tube;
s12, introducing a doping solution into the treated reaction tube, wherein the doping solution comprises but is not limited to Er 3+ (0.45g/L)、Yb 3+ (0.52g/L)、Ce 3+ (0.22 g/L), quartzSoaking the tube in the doping solution at 25deg.C for 2.5 hr at rotation speed of 25r/min, guiding the doping solution out of the quartz tube, blowing nitrogen gas to dry the quartz tube, and controlling nitrogen flow to 15-30m 3 Obtaining a doped quartz tube;
s13, introducing chlorine into the doped quartz tube, heating at 1125 ℃ to remove water and hydroxyl in the tube; introducing phosphorus oxychloride and oxygen into the quartz tube after introducing chlorine, and heating the quartz tube to 1330 ℃ to enable phosphorus to be in the form of P 2 O 5 Is deposited into the quartz tube to obtain a deposited quartz tube;
s14, introducing oxygen and helium into a deposition quartz tube, and vitrifying at 1950 ℃; then the quartz tube is collapsed into a solid optical fiber preform doped with anti-radiation ions by a collapse method;
s2, placing the optical fiber preform obtained in the S1 into a high-pressure tank, introducing deuterium and helium, wherein the deuterium accounts for 84.6% of the mixed gas, adjusting the pressure in the tank to 2.1Mpa, heating the tank to 110 ℃, preserving heat and pressure for 7.5 hours, taking out the optical fiber preform, performing pre-irradiation treatment with the total radiation dose of 1000Gy, and performing thermal bleaching treatment at the temperature of 1000 ℃ on the irradiated preform to obtain a post-treatment optical fiber preform;
s3, manufacturing the post-treatment optical fiber preform into a three-clad optical fiber by utilizing a tube rod drawing process:
s31, inserting the post-treatment optical fiber preform into a sleeve with an octagonal inner pure quartz layer and a fluorine-doped quartz outer layer, drawing by a tube rod method, controlling the drawing speed to be 110m/min, controlling the tension to be 100g, and controlling the temperature to be 1900 ℃;
s32, coating a low refractive index coating on the outer wall of the drawn optical fiber, controlling the size of the fiber core to be 9 mu m, controlling the distance between opposite sides of the octagonal inner cladding to be 105 mu m, and drawing the outer cladding to be 125 mu m to obtain the three-clad optical fiber.
S4, placing the three-cladding optical fiber into a high-pressure tank, and introducing deuterium and helium, wherein the ratio of the deuterium to the mixed gas is 75%, adjusting the pressure in the tank to 1.6Mpa, heating the tank to 65 ℃, and preserving heat and pressure for 8.5 hours to obtain the radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber.
The slope efficiency was measured to be 36.75% and the absorption coefficient @1530nm was 41.27dB/m. After the optical fiber is subjected to irradiation treatment with the total dose of 1000Gy, the absorption coefficient is measured to be 39.07dB/m at 1530nm, and the radiation absorption change RIA is calculated to be=0.022 dB/m/kRad.
Example 2
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber is the same as that of example 1 except that Ce 3+ The concentration of (C) was 0.5g/L.
Example 3
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber is the same as that of example 1 except that Ce 3+ The concentration of (C) was 0.8g/L.
Example 4
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber is the same as that of the embodiment 1 except that deuterium concentration, tank pressure, temperature and time of the secondary carrier gas of the triple-clad fiber in the step S4 are the same as those of the primary carrier gas of the optical fiber preform in the step S2.
Comparative example 1
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber is the same as that of example 1 except that the secondary carrier gas of step S4 is not included and the irradiation and bleaching treatment are not performed after the primary carrier gas of step S2.
Comparative example 2
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber was the same as in example 1 except that the secondary carrier gas of step S4 was not included and the bleaching treatment was not performed after the primary carrier gas of step S2.
Comparative example 3
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber was the same as in example 1 except that the secondary carrier gas of step S4 was not included.
Comparative example 4
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber was the same as in example 1 except that the irradiation and bleaching treatment were not performed after the primary carrier gas in step S2.
Comparative example 5
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber is the same as that of example 1 except that the secondary carrier gas of step S4 is not included, and the primary carrier gas of step S2 and the irradiation and bleaching treatment process are not included.
Comparative example 6
The irradiation-resistant triple-clad erbium ytterbium co-doped fiber was the same as in example 1 except that the carrier gas treatment of step S2 was not included.
Testing and evaluation
Slope test and radiation-induced absorption change RIA values are carried out on the radiation-resistant three-cladding erbium-ytterbium co-doped optical fibers obtained in the examples and the comparative examples.
The efficiency is the ratio of pump power to optical fiber power, reflects the optical performance of the optical fiber, is tested by utilizing a cut-off method, and is subjected to linear fitting by drawing points on the coordinate axes of pump power (X) and optical fiber power (Y), the slope of a fitted linear equation is the slope efficiency, and the higher the slope efficiency is, the better the optical performance effect is.
Ria= |absorption before fiber irradiation-absorption after fiber irradiation|irradiation dose; the absorption value is an absorption coefficient@1530 nm value directly read by test equipment, the irradiation dose is 1000Gy (10Gy=1 krad), and the radiation-resistant effect is better when the RIA value is lower.
The test results are shown in Table 1.
TABLE 1 irradiation resistance test results
From the test results, it can be seen that examples 1-3 follow Ce 3+ The content was increased and the RIA of the fiber tended to decrease, indicating Ce 3+ The higher the concentration of (c) the better the irradiance performance of the fiber. But with Ce 3+ The slope efficiency of the optical fiber decreases sharply and the optical performance becomes weaker.
Compared with example 1 and example 4, the RIA value of example 1 is larger than that of example 4, and the irradiation resistance effect of example 4 is slightly improved, because the secondary carrier gas condition in the step S4 increases the deuterium proportion and increases the pressure in the tank and the temperature, deuterium element can be loaded into the optical fiber more, and the irradiation resistance performance of the optical fiber is improved. However, the slope efficiency of example 1 is higher than that of example 4, and the optical performance of example 4 is greatly reduced, which means that the optical performance of the optical fiber can be deteriorated at high temperature, and the secondary carrier gas is more beneficial to ensuring the anti-irradiation performance and the optical performance at the same time in a low-temperature and long-time mode.
Comparative example 5 does not include the primary carrier gas, secondary carrier gas, irradiation and bleaching treatment process, comparative example 1 has a RIA reduced by 0.01 compared with that of comparative example 1, comparative example 6 has a RIA reduced by 0.11 compared with that of comparative example 1, and comparative example 2 has a sum of RIA reduced values lower than that of comparative example 5 and example 1, which means that there is a synergistic effect of improving the anti-irradiation performance between the primary carrier gas and the irradiation, bleaching and secondary carrier gases, and in addition, the process (example 1) used in combination has less influence on the fiber efficiency.
Comparative example 1 has a larger RIA value and slope efficiency than comparative example 2, indicating that irradiation treatment can improve irradiation resistance but can reduce optical properties. Comparative example 2, which does not include a bleaching process but has an increased RIA value and a reduced slope efficiency, compared to example 1, shows that the thermal bleaching treatment can further reduce the irradiation sensitivity of the optical fiber, thereby enhancing the irradiation performance of the optical fiber, and that the degradation of the slope efficiency of the optical fiber due to carrier gas and irradiation after the thermal bleaching treatment is significantly repaired.
The present invention 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 invention are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber based on the secondary carrier gas is characterized by comprising the following steps of:
s1, obtaining an optical fiber preform, wherein the optical fiber preform is doped with erbium ions, ytterbium ions and cerium ions;
s2, introducing mixed gas containing deuterium into the optical fiber preform for carrying out primary carrier gas, and then sequentially carrying out irradiation treatment and thermal bleaching treatment to obtain a post-treatment optical fiber preform;
s3, manufacturing the post-treatment optical fiber preform into a three-cladding optical fiber by utilizing a tube rod drawing process;
s4, introducing mixed gas containing deuterium into the three-cladding optical fiber for secondary carrier gas, and obtaining the radiation-resistant three-cladding erbium-ytterbium co-doped optical fiber.
2. The method for preparing the radiation-resistant three-clad erbium-ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein in the step S2, the carrier gas pressure of the primary carrier gas is 2.1-2.5Mpa, the carrier gas temperature is 100-200 ℃ and the carrier gas time is 0.5-5h.
3. The method for preparing the radiation-resistant three-clad erbium-ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein in the step S4, the carrier gas pressure of the secondary carrier gas is 0.5-1.6Mpa, the carrier gas temperature is 20-80 ℃ and the carrier gas time is 8-10h.
4. The method for preparing the radiation-resistant three-cladding erbium-ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein in the step S2, the ratio of deuterium in the mixed gas is 84.6-100%; in the step S4, the ratio of deuterium in the mixed gas is 30-75%.
5. The method for preparing the radiation-resistant three-cladding erbium-ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein in the step S2, the radiation treatment dose is 50-5000Gy, and the radiation rate is 10-200Gy/h.
6. The method for preparing the radiation-resistant three-clad erbium ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein in the step S2, the temperature of thermal bleaching is 500-1200 ℃.
7. The method for preparing the radiation-resistant three-cladding erbium-ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein in the step S1, the preparation process of the optical fiber preform is as follows:
s11, depositing a silicon dioxide porous layer on the inner wall of the pure quartz tube by using a vapor deposition method to obtain a reaction tube;
s12, soaking the reaction tube in a doping solution containing erbium ions, ytterbium ions and cerium ions, and drying by utilizing nitrogen to obtain a doped quartz tube;
s13, introducing chlorine into the doped quartz tube at 500-1200 ℃, and then passing phosphorus oxychloride and oxygen at 1200-1400 ℃ to obtain a deposited quartz tube;
s14, introducing oxygen and helium into the deposited quartz tube at 1900-2200 ℃ for vitrification, and then collapsing by a collapse method to obtain the optical fiber preform.
8. The method for preparing the radiation-resistant three-cladding erbium-ytterbium co-doped fiber based on the secondary carrier gas according to claim 1, wherein the process of the step S3 is as follows:
s31, inserting the post-treatment optical fiber preform into an inner layer sleeve, sleeving the inner layer sleeve into an outer layer sleeve, and drawing by using a tube rod method to obtain drawn optical fibers; the inner sleeve is made of octagonal pure quartz, and the outer sleeve is made of fluorine-doped quartz;
s32, coating a low refractive index coating on the outer wall of the drawn optical fiber to obtain the three-cladding optical fiber.
9. A radiation-resistant triple-clad erbium ytterbium co-doped fiber obtained by the production method according to any one of claims 1 to 8.
10. The use of the radiation-resistant triple-clad erbium-ytterbium co-doped fiber according to claim 9 under the irradiation condition of 1000Gy or more.
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