CN117185644A - Ytterbium-doped optical fiber preform, ytterbium-doped active optical fiber and preparation method thereof - Google Patents
Ytterbium-doped optical fiber preform, ytterbium-doped active optical fiber and preparation method thereof Download PDFInfo
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- 239000013307 optical fiber Substances 0.000 title claims abstract description 70
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 33
- -1 ytterbium ion Chemical class 0.000 claims abstract description 29
- 239000012792 core layer Substances 0.000 claims abstract description 24
- 150000003747 ytterbium compounds Chemical class 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims description 77
- 230000008021 deposition Effects 0.000 claims description 39
- 239000010453 quartz Substances 0.000 claims description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 35
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 22
- 239000007789 gas Substances 0.000 claims description 20
- 238000002791 soaking Methods 0.000 claims description 19
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 150000002910 rare earth metals Chemical class 0.000 claims description 13
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 claims description 13
- 229910052734 helium Inorganic materials 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 239000000460 chlorine Substances 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 8
- 239000012266 salt solution Substances 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 239000002019 doping agent Substances 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 230000018044 dehydration Effects 0.000 claims description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical group CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical group OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims description 2
- ZMIGMASIKSOYAM-UHFFFAOYSA-N cerium Chemical compound [Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce][Ce] ZMIGMASIKSOYAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 125000005473 octanoic acid group Chemical group 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical group OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 125000000542 sulfonic acid group Chemical group 0.000 claims description 2
- 125000005922 tert-pentoxy group Chemical group 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims 1
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 claims 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 claims 1
- 238000009826 distribution Methods 0.000 abstract description 14
- 238000009792 diffusion process Methods 0.000 abstract description 3
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 abstract description 2
- 229940075624 ytterbium oxide Drugs 0.000 abstract description 2
- 229910003454 ytterbium oxide Inorganic materials 0.000 abstract description 2
- 238000000151 deposition Methods 0.000 description 33
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 24
- 239000000835 fiber Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000010410 layer Substances 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 4
- HDGGAKOVUDZYES-UHFFFAOYSA-K erbium(iii) chloride Chemical compound Cl[Er](Cl)Cl HDGGAKOVUDZYES-UHFFFAOYSA-K 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000005491 wire drawing Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
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- 230000010287 polarization Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
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- Manufacture, Treatment Of Glass Fibers (AREA)
- Lasers (AREA)
Abstract
The invention discloses an ytterbium-doped optical fiber preform, an ytterbium-doped active optical fiber and a preparation method thereof. And in the liner tube shrinking stage, introducing steam containing ytterbium compound into the tube to reduce loss caused by outward diffusion and volatilization of ytterbium oxide in the liner tube shrinking stage, thereby obtaining the uniformly doped ytterbium-doped optical fiber preform. The prepared preform rod has uniform core layer ytterbium ion concentration distribution, and the ytterbium-doped optical fiber obtained by drawing has high laser slope efficiency.
Description
Technical Field
The invention belongs to the field of optical fiber manufacturing, relates to an ytterbium-doped optical fiber preparation technology, and in particular relates to an ytterbium-doped optical fiber preform, an ytterbium-doped active optical fiber and a preparation method thereof.
Background
The rare earth doped optical fiber preform is a key material for producing an optical fiber amplifier and an optical fiber laser. Compared with the traditional semiconductor laser amplifier, the optical fiber amplifier can directly amplify the signal in full light without the complex processes of photoelectric conversion, electro-optical conversion, signal regeneration and the like, has the characteristics of high gain, large bandwidth, low noise, polarization insensitivity gain and low lead-in loss in the working wavelength range, has good transparency, and is particularly suitable for relay amplification of long-distance optical communication. It can be said that the optical fiber amplifier lays an important technical foundation for realizing high-capacity all-optical communication. Rare earth doped fiber is used as an important component of high power fiber laser and is a main factor for determining the performance of high power fiber laser.
At present, the rare earth element doping method for producing the rare earth doped optical fiber preform mainly comprises a gas phase method, including rare earth chloride gas phase deposition and rare earth chelate gas phase deposition; the solution method comprises soaking rare earth solution in a tube and soaking rare earth solution outside the tube; a nano ion direct deposition method and a gel method. The solution method is the main preparation method of the doped optical fiber preform at present and comprises the following steps of: depositing a powder rod by a VAD method, soaking the powder rod in a solution containing rare earth elements, and vitrifying the soaked powder rod in a high-temperature furnace to prepare a rare earth element doped optical fiber preform core layer (CN 102108008B); in-tube method: and sequentially depositing an inner cladding layer and a loose ash core layer in a deposition tube, and injecting a solution containing rare earth chloride into the deposition tube, wherein the fused deposition tube, the inner cladding layer and the loose ash core layer are solid prefabricated rods (CN 102515501B, CN1500069, US 5711782A and US 5262365A).
The rare earth ions and the co-doping agent are easy to volatilize in a large amount in a high-temperature melting stage, so that the rare earth ions on the cross section of the core rod are unevenly distributed, the lower the content of the intermediate rare earth ions is, the distribution is in a V shape, and the refractive index profile of the finally drawn optical fiber is concave, so that the matching of an active optical fiber and a passive optical fiber is influenced, the thermal stability of a laser is reduced, the quality of a light beam is deteriorated, and the central dark spot is reduced, and therefore, the uniform distribution of the rare earth ions is very critical in the process of preparing the active optical fiber preform by a liquid phase method.
Disclosure of Invention
The invention aims to provide a preparation method of an ytterbium-doped optical fiber preform based on an in-tube method, aiming at the defects of the prior art, and the ytterbium-doped optical fiber preform produced by the method has uniform ytterbium ions distribution in a core layer of the optical fiber preform, and the obtained optical fiber laser has high slope efficiency.
The invention also aims to provide a preparation method of the ytterbium-doped active optical fiber, which is obtained by adopting the ytterbium-doped optical fiber preform rod and performing sleeve rod wire drawing or direct wire drawing; the obtained ytterbium-doped active optical fiber has stable refractive index of transverse section, and has the characteristics of high gain, large bandwidth, low noise, polarization insensitivity gain and low introduction loss in the working wavelength range.
The invention adopts the technical proposal for solving the problems that:
in one aspect, the invention provides a preparation method of an ytterbium-doped optical fiber preform based on an in-tube method, comprising the following steps:
preparing a quartz deposition tube with a loose core layer deposited on the inner surface by adopting an MCVD process;
heating and breaking one end of the tail pipe, injecting ytterbium-containing rare earth salt solution into the quartz deposition tube, and soaking for a period of time;
pouring out the residual solution in the quartz deposition tube after soaking, introducing nitrogen or inert gas for purging, and then introducing first process gas for drying and dehydration;
and introducing a second process gas doped with ytterbium compound steam into the quartz deposition tube, oxidizing and shrinking the quartz deposition tube, and cooling to obtain the ytterbium-doped optical fiber preform.
According to the invention, ytterbium-containing compound steam is introduced into the quartz deposition tube in the shrinking stage, and the partial pressure of the ytterbium-containing compound steam is controlled to balance outward diffusion volatilization of ytterbium oxide in the deposition layer, so that the uniformly doped ytterbium-doped optical fiber preform is obtained, and the ytterbium-doped active optical fiber with uniform refractive index on the cross section can be obtained by utilizing the preform for drawing, so that the requirement of a high-power optical fiber laser is met.
As a preferable technical scheme, the deposition temperature of the loose core layer on the inner surface of the quartz deposition tube is 1200-1400 ℃; by controlling proper deposition temperature, a deposition layer with good looseness and uniform density is obtained, and when rare earth elements are doped, the adsorption capacity to ytterbium-containing rare earth salt and co-doping agent is strong, and the rare earth distribution is uniform.
As a preferable technical scheme, anions in the ytterbium-containing rare earth salt solution are selected from any one or a combination of a plurality of chloride ions, nitrate radicals, benzenesulfonic acid groups, tert-pentoxy groups, trifluoro sulfonic acid groups, methylsulfonic acid groups, octanoic acid groups and perfluorooctanoic acid groups.
As a preferable technical scheme, the ytterbium-containing rare earth salt solution is also doped with a co-doping agent during soaking.
Further preferably, the co-admixture is any one or a combination of several compounds containing phosphorus, cerium and aluminum.
As a preferable technical scheme, the soaking time of the ytterbium rare earth salt solution in the quartz deposition tube is 1-6 hours, and the optimal time is 3.5 hours; the soaking temperature is 0-70 deg.c, and most preferably 40 deg.c.
As a preferred embodiment, the first process gas includes helium, oxygen, and chlorine, and the drying dehydration temperature is 600 ℃ to 1000 ℃.
As a preferred solution, the second process gas comprises helium, oxygen, and the second process gas type may be adapted according to the actual process.
As a preferred embodiment, the ytterbium-containing compound of the second process gas into which the ytterbium compound steam is introduced comprises Yb (thmd) 3 、Yb(NO 3 ) 3 The ytterbium-containing compound is not limited to these two, and may be any ytterbium-containing compound capable of forming steam at the condensation temperature.
As a preferable technical scheme, in the mixed gas consisting of the second process gas and ytterbium compound steam, the volume ratio of the ytterbium compound steam is 5-15%, and under the volume ratio, volatilization and adsorption of the ytterbium compound in the loose layer can reach an equilibrium state, so that uniformity of ytterbium ion distribution of the core rod after melting and shrinking is maintained.
As a preferable technical scheme, in the process of melting and shrinking, the fluctuation range of the steam volume ratio of the ytterbium compound in the mixed gas is not more than 2%, maintaining the stability of the steam volume ratio of the ytterbium compound is beneficial to improving the uniformity of the distribution of the ytterbium compound in the loose layer of the preform after melting and shrinking, and the fluctuation range is not more than 2% means that the difference between the maximum value and the minimum value of the steam volume ratio of the ytterbium compound is controlled to be not more than 2% in the whole process of melting and shrinking.
As a preferable technical scheme, the temperature of oxidizing and shrinking the quartz deposition tube is 1600-2200 ℃, the pressure in the tube is controlled to be-1000 Pa-500 Pa, and proper shrinking temperature and pressure are selected, so that the roundness of the fiber core and the uniformity of ytterbium compound distribution can be improved.
As a preferable technical scheme, in the ytterbium-doped optical fiber preform obtained after oxidation and shrinkage, the mass concentration of ytterbium ions in the core layer is 500-30000ppm, in the concentration range, the ytterbium-doped optical fiber performance is obviously improved, and the uniformity of the mass concentration distribution of ytterbium ions in the core layer can be easily controlled.
On the other hand, the invention also provides an ytterbium-doped optical fiber preform which is prepared by adopting the preparation method.
On the other hand, the invention also provides an ytterbium-doped active optical fiber, which is obtained by adopting the ytterbium-doped optical fiber preform rod and performing sleeve rod wire drawing or direct wire drawing.
On the premise of not increasing the existing solution method production equipment, the optical fiber preform and the ytterbium-doped optical fiber with even ytterbium ion doping can be prepared by a shrinking process.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, by improving the shrinking process and supplementing ytterbium compound steam in the shrinking stage, the loss caused by outward diffusion and volatilization of ytterbium ions in the shrinking stage of the optical fiber preform can be solved, and the existing production equipment can be utilized, so that the universality and the adaptability are strong. The ytterbium-doped optical fiber preform produced by the method has the advantages that ytterbium ions are uniformly distributed in the optical fiber preform, and the obtained optical fiber laser has high slope efficiency.
Drawings
FIG. 1 is a graph showing the slope efficiency of ytterbium-doped fiber laser drawn from the preform of example 1 and comparative example 1.
FIG. 2 is a graph showing the slope efficiency of ytterbium-doped fiber laser drawn from the preform obtained in example 2 and comparative example 2.
FIG. 3 is a graph showing the slope efficiency of ytterbium-doped fiber laser drawn from the preform obtained in example 3 and comparative example 3.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the invention further, but are not to be construed as limiting the invention.
Example 1: preparing a quartz deposition tube with a loose core layer deposited on the inner surface by adopting an MCVD process, injecting 0.3L of ethanol solution containing ytterbium chloride, cerium chloride and aluminum chloride into the deposition tube, wherein the ytterbium chloride content is 0.023mol/L, the cerium chloride content is 0.007mol/L, the aluminum chloride content is 0.16mol/L, soaking for 3 hours at 40 ℃, pouring out the solution, introducing nitrogen into a quartz liner tube for purging for 3 hours, and then introducing He and O between 650 ℃ and 950 DEG C 2 ，Cl 2 Dewatering the loose core layer, finally smelting the quartz tube at 1800-2100 deg.c, and introducing Yb (thmd) in smelting stage 3 Steam, and Yb (thmd) 3 The volume percentage of the steam in the liner tube is between 10 percent and 11.5 percent, and finally the ytterbium-doped active optical fiber preform is obtained.
Comparative example 1: preparing a quartz deposition tube with a loose core layer deposited on the inner surface by adopting an MCVD process, injecting 0.3L of ethanol solution containing ytterbium chloride, cerium chloride and aluminum chloride into the deposition tube, wherein the ytterbium chloride content is 0.023mol/L, the cerium chloride content is 0.007mol/L, the aluminum chloride content is 0.16mol/L, soaking for 3 hours at 40 ℃, pouring out the solution, introducing nitrogen into a quartz liner tube for purging for 3 hours, and then introducing He and O between 650 ℃ and 950 DEG C 2 ，Cl 2 Dehydrating the loose core layer, and finally shrinking the quartz tube at 1800-2100 ℃ to obtain ytterbium-doped active lightA fiber preform.
The two core rod ytterbium ion concentration test distributions are shown in table 1, and it can be seen that the ytterbium ion concentration distribution of the preform prepared in example 1 is uniform compared with the comparative example.
Table 1 shows ytterbium ion concentration profiles of example 1 and comparative example 1
Example 1 preform drawing resulted in a fiber laser slope efficiency of 75.1% (as shown in fig. 1). The slope efficiency of the fiber laser obtained in comparative example 1 is only 55.6%, and it can be seen that the ytterbium-doped fiber prepared by this example can significantly improve the fiber performance.
Example 2: preparing a quartz deposition tube with a loose core layer deposited on the inner surface by adopting an MCVD process, injecting 0.3L of ethanol solution containing ytterbium chloride, aluminum chloride and erbium chloride into the deposition tube, wherein the ytterbium chloride content is 0.021mol/L, the aluminum chloride content is 0.15mol/L, the erbium chloride content is 0.005mol/L, soaking for 3.5 hours at 45 ℃, pouring out the solution, introducing nitrogen into a quartz liner tube for purging for 3 hours, and then introducing He and O between 650 ℃ and 950 DEG C 2 ，Cl 2 Dewatering the loose core layer, finally smelting the quartz tube at 1800-2100 deg.c, and introducing Yb (NO) 3 ) 3 Steam, and Yb (NO) 3 ) 3 The volume percentage of the steam in the liner tube is between 13.5% and 14.7%, and finally the ytterbium-doped optical fiber preform is obtained.
Comparative example 2: preparing a quartz deposition tube with a loose core layer deposited on the inner surface by an MCVD process, injecting 0.3L of ethanol solution containing ytterbium chloride, aluminum chloride and erbium chloride into the deposition tube, wherein the ytterbium chloride content is 0.021mol/L, the aluminum chloride content is 0.15mol/L, the erbium chloride content is 0.005mol/L, soaking for 3.5 hours at 45 ℃, pouring out the solution, introducing nitrogen into a quartz liner tube for purging for 3 hours, and then introducing He and O between 650 ℃ and 950 DEG C 2 ，Cl 2 And (3) dehydrating the loose core layer, and finally, shrinking the quartz tube at 1800-2100 ℃ to finally obtain the ytterbium-doped optical fiber preform.
The two core rod ytterbium ion concentration test distributions are shown in Table 2, and it can be seen that the preform ytterbium ion concentration distribution prepared in example 2 is uniform compared with the comparative example.
Table 2 shows ytterbium ion concentration profiles of example 2 and comparative example 2
Example 2 preform drawing resulted in a fiber laser slope efficiency of 73.8% (as shown in fig. 2). The slope efficiency of the fiber laser obtained in comparative example 2 is only 54.9%, and it can be seen that the ytterbium-doped fiber prepared by this example can significantly improve the fiber performance.
Example 3: preparing a quartz deposition tube with a loose core layer deposited on the inner surface by adopting an MCVD process, injecting 0.31L of ethanol solution containing ytterbium chloride, aluminum chloride and phosphoric acid into the deposition tube, wherein the ytterbium chloride content is 0.025mol/L, the aluminum chloride content is 0.17mol/L, the phosphoric acid content is 0.15mol/L, soaking for 4 hours at 43 ℃, pouring out the solution, introducing nitrogen into a quartz liner tube for purging for 3.5 hours, and then introducing He and O between 650 ℃ and 950 DEG C 2 ，Cl 2 Dewatering the loose core layer, finally smelting the quartz tube at 1800-2100 deg.c, and introducing Yb (NO) 3 ) 3 Steam, and Yb (NO) 3 ) 3 The volume percentage of the steam in the liner tube is between 5.2% and 6.9%, and finally the ytterbium-doped optical fiber preform is obtained.
Comparative example 3: preparing a quartz deposition tube with a loose core layer deposited on the inner surface by an MCVD process, injecting 0.31L of ethanol solution containing ytterbium chloride, aluminum chloride and phosphoric acid into the deposition tube, wherein the ytterbium chloride content is 0.025mol/L, the aluminum chloride content is 0.17mol/L, the phosphoric acid content is 0.15mol/L, soaking for 4 hours at 43 ℃, pouring out the solution, introducing nitrogen into a quartz liner tube for purging for 3.5 hours, and then introducing He and O between 650 ℃ and 950 DEG C 2 ，Cl 2 And (3) dehydrating the loose core layer, and finally, shrinking the quartz tube at 1800-2100 ℃ to finally obtain the ytterbium-doped optical fiber preform.
The two core rod ytterbium ion concentration test distributions are shown in Table 3, and it can be seen that the preform ytterbium ion concentration distribution prepared in example 3 is uniform compared with the comparative example.
Table 3 shows ytterbium ion concentration profiles of example 3 and comparative example 3
Example 3 preform drawing resulted in a fiber laser slope efficiency of 78.6% (as shown in fig. 3). The slope efficiency of the fiber laser obtained in comparative example 3 is only 56.1%, and it can be seen that the ytterbium-doped fiber prepared by this example can significantly improve the fiber performance.
The foregoing is merely a preferred embodiment of the present invention, and it should be noted that modifications and changes can be made by those skilled in the art without departing from the inventive concept and remain within the scope of the invention.
Claims (15)
1. The preparation method of the ytterbium-doped optical fiber preform based on the in-pipe method is characterized by comprising the following steps of:
preparing a quartz deposition tube with a loose core layer deposited on the inner surface by adopting an MCVD process;
heating and breaking one end of the tail pipe, injecting ytterbium-containing rare earth salt solution into the quartz deposition tube, and soaking for a period of time;
pouring out the residual solution in the quartz deposition tube after soaking, introducing nitrogen or inert gas for purging, and then introducing first process gas for drying and dehydration;
and introducing a second process gas doped with ytterbium compound steam into the quartz deposition tube, oxidizing and shrinking the quartz deposition tube, and cooling to obtain the ytterbium-doped optical fiber preform.
2. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: the deposition temperature of the loose core layer on the inner surface of the quartz deposition tube is 1200-1400 ℃.
3. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: the anions in the ytterbium-containing rare earth salt solution are selected from any one or a combination of a plurality of chloridion, nitrate radical, benzenesulfonic acid group, tert-pentyloxy, trifluoro sulfonic acid group, methylsulfonic acid group, octanoic acid group and perfluorooctanoic acid group.
4. The method for preparing an ytterbium-doped optical fiber preform based on the in-tube method according to claim 3, wherein: during soaking, the ytterbium-containing rare earth salt solution is also doped with a co-doping agent.
5. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 4, wherein the method comprises the following steps: the co-doping agent is any one or a combination of a plurality of compounds containing phosphorus, cerium, aluminum and erbium.
6. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: the soaking time of ytterbium rare earth salt solution in the quartz deposition tube is 1-6h, and the soaking temperature is 0-70 ℃.
7. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: the first process gas comprises helium, oxygen and chlorine, and the drying dehydration temperature is 600 ℃ to 1000 ℃.
8. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: the second process gas comprises helium, oxygen.
9. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1 or 8, wherein the method comprises the following steps: the second process gas is doped with steam of ytterbium-containing compound including Yb (thmd) 3 、Yb(NO 3 ) 3 。
10. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1 or 8, wherein the method comprises the following steps: the mixed gas composed of the second process gas and ytterbium compound steam has the volume ratio of ytterbium compound steam of 5% to 15%.
11. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 10, wherein the method comprises the following steps: in the process of melting and shrinking, the fluctuation range of the steam volume ratio of ytterbium compound in the mixed gas is not more than 2 percent.
12. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: the temperature of oxidizing and shrinking the quartz deposition tube is 1600-2200 deg.c, and the pressure inside the tube is controlled at-1000 Pa-500 Pa.
13. The method for preparing the ytterbium-doped optical fiber preform based on the in-tube method according to claim 1, wherein the method comprises the following steps: in the ytterbium-doped optical fiber preform obtained after oxidation and shrinkage, the mass concentration of ytterbium ions in the core layer is 500-30000ppm.
14. An ytterbium-doped optical fiber preform, characterized in that: a preparation process according to any one of claims 1 to 13.
15. Ytterbium-doped active optical fiber, characterized in that it is obtained by using the ytterbium-doped optical fiber preform according to any one of claims 1 to 14, through a jacket rod drawing or a direct drawing.
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