CN112266174A - Preparation and test method of aluminum fluoride 2.9 mu m high-power optical fiber laser - Google Patents
Preparation and test method of aluminum fluoride 2.9 mu m high-power optical fiber laser Download PDFInfo
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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
- C03C13/041—Non-oxide glass compositions
- C03C13/042—Fluoride glass compositions
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- 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
- C03B37/01265—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt
- C03B37/01268—Manufacture of preforms for drawing fibres or filaments starting entirely or partially from molten glass, e.g. by dipping a preform in a melt by casting
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- 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
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- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M11/00—Testing of optical apparatus; Testing structures by optical methods not otherwise provided for
- G01M11/02—Testing optical properties
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- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M11/00—Testing of optical apparatus; Testing structures by optical methods not otherwise provided for
- G01M11/30—Testing of optical devices, constituted by fibre optics or optical waveguides
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Abstract
The invention discloses a preparation and test method of aluminum fluoride 2.9 mu m high-power fiber laser, which relates to the technical field of fiber lasers, and provides the following scheme aiming at the existing realization of different functions and problems, and comprises the following steps: s1: placing the dried raw materials into an ultra-fine grinding machine for mixing and grinding; s2: the raw material ground in the step S1 is put into a platinum crucible dried at high temperature and is fired in a glove box electric furnace by a melting method; s3: and pouring the liquid fired in the step S2 in a mold for annealing until the liquid is cooled to room temperature to prepare a prefabricated rod, and the invention realizes the high-power laser emission of the aluminum fluoride fiber at 2.9 mu m and simultaneously obtains higher laser slope efficiency and lower pumping threshold. The method is more beneficial to laser communication and sensing of middle infrared wave bands in the future, and simultaneously realizes good balance between high-power fiber laser and mechanicalness and different functions.
Description
Technical Field
The invention relates to the technical field of fiber lasers, in particular to a method for preparing and testing an aluminum fluoride 2.9 mu m high-power fiber laser.
Background
Mid-infrared fiber lasers are receiving more and more attention because of their important application values, such as national defense industry, medical instruments, chemical detection, etc. The glass materials currently dedicated to the transmission of mid-infrared bands and laser generation are mainly concentrated on tellurite glasses, chalcogenide glasses and fluoride glasses. The tellurite glass has good fiber forming performance and strong anti-crystallization capability, but the phonon energy is higher, the high phonon energy inevitably increases the inter-energy-level multi-phonon non-radiative relaxation rate, reduces the radiation quantum efficiency of luminescent ions, and limits the generation and transmission of laser in the middle infrared field; the chalcogenide glass has low phonon energy, but has poor thermal stability and low mechanical strength, and the difficulty of drawing optical fiber is improved in the optical fiber drawing process due to the complex preparation process, so that the chalcogenide glass is not beneficial to practical application. Among fluoride materials, zirconium fluoride-based glass, indium fluoride-based glass, and aluminum fluoride-based glass are mainly focused.
Zirconium fluoride-based glasses, mainly focused on the ZBLAN component, have received wide attention due to their low phonon energy and transmission window width, and in 2018, YIGIT ozanadyn et al, using an Er3+ ion doped ZBLAN fiber, achieved a high power mid-infrared laser output of 2.82 μm at 41.6W
The transmission window of the indium fluoride material is wider than that of the zirconium fluoride material, so that in the middle infrared field, the optical fiber of the indium fluoride material is further explored, and in 2018, Jia et al achieve the preparation of a 2.87 μm doped Ho3+ indium fluoride optical fiber, the maximum output power is 54.5mW, the slope efficiency is 6%, and the threshold power is up to 278 mW. In the same year, FR É D É RIC MAES et al realized a laser output of 3.92 μm with an output power of 200mW in a Ho3+ doped indium fluoride fiber with a 888nm semiconductor laser pumping.
However, zirconium fluoride-based glass and indium fluoride-based glass have poor mechanical properties and thermal stability (the glass transition temperature of ZBLAN is 267 ℃ and the glass transition temperature of indium fluoride material is 260 ℃), and the optical fiber itself is more susceptible to damage and deliquescence in high-power laser transmission, resulting in further degradation of the optical fiber quality over time, limiting their development in high-power laser transmission.
The aluminum fluoride-based glass is more beneficial to the development of the intermediate infrared band optical fiber due to the excellent mechanical property, thermal stability and chemical stability. In 2018, Jia et al characterized the thermal stability and the anti-deliquescence capability of a fluorine-aluminum glass material, realized the preparation of a 2.8 μm Ho3+ doped aluminum fluoride optical fiber and tested the laser performance thereof, but the optical fiber has lower slope efficiency and output power, only 57mW, and is insufficient in the generation capability of high-power optical fiber laser.
The Pr3+ ion sensitized Ho3+ doped optical fiber prepared by the aluminum fluoride based glass material has better laser performance, the maximum output power of 156.3mW is obtained when the length of 193.3mm is obtained, the laser power is improved by nearly 3 times, the slope efficiency is 9.843%, and higher output power and slope efficiency can be realized when the length of the optical fiber is shorter.
Disclosure of Invention
The invention provides a method for preparing and testing an aluminum fluoride 2.9 mu m high-power fiber laser, which solves the existing problem that the high-power fiber laser and the mechanical property cannot be well balanced.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of aluminum fluoride 2.9 mu m high-power optical fiber laser comprises the following steps:
s1: placing the dried raw materials into an ultra-fine grinding machine for mixing and grinding;
s2: the raw material ground in the step S1 is put into a platinum crucible dried at high temperature and is fired in a glove box electric furnace by a melting method;
s3: pouring the liquid fired in the step S2 into a mold for annealing until the liquid is cooled to room temperature to prepare a preform;
s4: polishing the surface of the preform rod prepared in the step S3 by using an automatic polishing machine, and then performing surface decontamination;
s5: the product obtained in step S4 was loaded on a drawing tower and drawn into an optical fiber in a nitrogen atmosphere.
Preferably, the feedstock in step S1 comprises AlF3、BaF2、YF3、PbF2、MgF2And doping Pr and Ho elements therein, grinding the powder in step S1 to 3000-6000 mesh for 10-40 min.
Preferably, the concentration of doped Pr is 10000-30000 ppm, and the concentration of doped Ho is 1000-3000 ppm.
Preferably, in the step S2, the temperature in the glove box is 850-1000 ℃, and the firing time is 1-3 h.
Preferably, the temperature of the die in the step S3 is 300-450 ℃, the annealing time is 1-5 h, and the cooling mode adopts natural cooling.
Preferably, in step S4, polishing is performed to optical grade, and the cleaning agent is alcohol with an alcohol concentration of 80-99%.
The utility model provides a testing arrangement of aluminium fluoride 2.9 mu m high power fiber laser, includes the laser instrument, two coupling lens that one side of laser instrument was provided with, one side of coupling lens is provided with the space beam isolator, one side of space beam isolator is provided with focusing lens (5), one side of focusing lens is provided with the dichroscope, one side of dichroscope is provided with finished product optic fibre, the other end of finished product optic fibre is connected with the InF2 jumper wire, the other end of InF2 jumper wire connects is connected with the spectrum appearance.
Preferably, the coupling lens is a CaF2 coupling lens, the focal lengths of the two coupling lenses are respectively 100mm and 40mm, and the focusing lens is a CaF2 focusing lens with the focal length of 6 mm.
A test method of aluminum fluoride 2.9 mu m high-power fiber laser comprises the following steps:
s1, installing and fixing a laser, adjusting two coupling lenses, sequentially installing a space beam isolator and a focusing lens, placing the drawn finished optical fiber, the dichroic mirror and the InF2 jumper at a specified position, and adjusting all devices to reach the specified position;
s2, starting a laser, outputting the laser, shrinking the laser after passing through two CaF2 coupling lenses, enabling the shrunk laser to pass through a space beam isolator and then reach a focusing lens, converging the laser in a fiber core area of a finished product optical fiber which is cut vertically after passing through a dichroic mirror, outputting the laser after passing through the finished product optical fiber, receiving the laser by an InF2 jumper and then inputting the laser into a spectrometer;
and S3, recording the data in the step S2, drawing a chart and analyzing the chart.
Preferably, the laser is used at a wavelength of 1150nm, and the test experiment is carried out under the protection of nitrogen or inert gas.
The invention has the beneficial effects that:
1: the high-power laser emission of the aluminum fluoride fiber at 2.9 mu m is realized by proportioning the components of the fiber, and simultaneously, higher laser slope efficiency and lower pumping threshold are also obtained. The method is more beneficial to laser communication and sensing of middle infrared wave bands in the future.
2: through different proportions of the components of the optical fiber, various optical fibers with different properties can be realized, different working environments are adapted, high-power optical fiber laser and mechanical property are well balanced, and different functions are realized.
Drawings
FIG. 1 is a laser spectrum obtained for a 193.3mm length Ho3+/Pr3+ co-doped fiber with a 1739.2mW pump;
FIG. 2 is a diagram of the spectral emission mechanism;
FIG. 3 is an experimental graph of experimental slope efficiency as a function of fiber length in accordance with the present invention;
FIG. 4 is a graph of 2.9 μm laser power with pump spectra for a fiber length of 193.3 mm;
FIG. 5 is a graph showing the experimental slope efficiency of the present invention gradually increasing with decreasing fiber length
Reference numbers in the figures: 1 laser, 3 coupling lenses, 4 space beam isolators, 5 focusing lenses, 6 focusing lenses, 7 finished optical fibers, 8InF2 jumper wires and 9 spectrometers.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.
Example 1:
drying AlF3、BaF2、YF3、PbF2、MgF2Placing the mixture into an ultrafine grinding machine according to the molar ratio of 30, 15, 20, 25 and 10, adding a compound with Pr and Ho elements at the same time to enable the concentrations of the Pr and Ho elements to be 2000ppm and 20000ppm respectively, mixing and grinding the mixture for 20min, then putting the ground raw materials into a high-temperature dried platinum crucible, firing the raw materials in a glove box electric furnace by using a melting method, maintaining the temperature of the glove box electric furnace at 930 ℃ for 2h, pouring the fired liquid into a mold at 380 ℃ for annealing until the temperature is reduced to room temperature to prepare a prefabricated rod, then polishing the surface of the prepared prefabricated rod to a academic level by using an automatic polishing machine, performing surface decontamination by using 99% alcohol, installing the prefabricated rod after decontamination on a drawing tower, drawing an optical fiber in a nitrogen environment, and enabling the core component of the optical fiber to be 30AlF3-15BaF2-20YF3-25PbF2-10MgF2 due to element replacement, and after the drawing is finished, placing the device on an installed testing machine for testing and recording.
Example 2: drying AlF3、BaF2、YF3、PbF2、MgF2Placing the mixture into an ultra-fine grinding machine according to the molar ratio of 38, 10, 20, 24 and 8, adding a compound with Pr and Ho elements at the same time to enable the concentrations of the Pr and Ho elements to be 3000ppm and 30000ppm respectively, then mixing and grinding the mixture for 40min, then putting the ground raw materials into a high-temperature drying platinum crucible, firing the raw materials in a glove box electric furnace by using a melting method, maintaining the temperature of the glove box electric furnace at 1000 ℃ for 3h, pouring the fired liquid into a mold at 450 ℃ for annealing until the temperature is reduced to room temperature to prepare a prefabricated rod, then polishing the surface of the prepared prefabricated rod to a chemical level by using an automatic polishing machine, performing surface decontamination by using 99% alcohol, installing the prefabricated rod after decontamination on a drawing tower, drawing the prefabricated rod into an optical fiber in a nitrogen environment, and enabling the core of the finally drawn optical fiber to have the main component of 50AlF3-10BaF2-12YF3-14 MgF 2-14MgF2 due to the replacement of the component, and after the drawing is finished, placing the device on an installed testing machine for testing and recording.
Example 3:
will dryDried AlF3、BaF2、YF3、PbF2、MgF2Placing the mixture into an ultrafine grinding machine according to the molar ratio of 25, 20, 30 and 5, adding a compound with Pr and Ho elements at the same time to ensure that the concentrations of the Pr and Ho elements are 1000ppm and 10000ppm respectively, then mixing and grinding the mixture for 10min, then putting the ground raw materials into a high-temperature dried platinum crucible, firing the raw materials in a glove box electric furnace by using a melting method, maintaining the temperature of the glove box electric furnace at 850 ℃ for 1h, pouring the fired liquid into a mold at 300 ℃ for annealing until the temperature is reduced to room temperature to prepare a prefabricated rod, then polishing the surface of the prepared prefabricated rod to a chemical grade by using an automatic polishing machine, performing surface decontamination by using 80% alcohol, installing the prefabricated rod after decontamination on a drawing tower, drawing the prefabricated rod into an optical fiber in a nitrogen environment, and enabling the core of the finished optical fiber to be 27AlF3-20BaF2-10YF 3-27F 2 due to the replacement of elements and subsequent overflow in the high-temperature environment 6MgF2, and after the drawing is finished, the device is placed on a mounted testing machine for testing and recording.
In the process of multiple experiments, the comprehensive performance of the optical fiber in example 1 is the most excellent, in example 2, the mechanical strength and the thermal stability are slightly improved for smaller but lower slope efficiency and output power, and in example 3, the mechanical strength and the thermal stability are better but lower but slightly lower, and the optical fiber can be selected and used under different use conditions.
Referring to fig. 1-4, experiments were validated for the formulation of example 1;
fig. 1 shows a laser spectrum obtained when a finished optical fiber with a length of 193.3mm (hereinafter, referred to as Ho3+/Pr3+ co-doped optical fiber) is pumped at 1739.2mW, the laser center is 2.866 μm, the development of an optical fiber laser with a length of more than 3 μm is more favorably realized by utilizing a nonlinear effect, and when the optical fiber is pumped at high power, multimode laser is obtained near 2.9 μm, and then the optical fiber laser with the energy level wider due to the wider energy level in the spectral emission from 5I6 to 5I7 is more favorably obtained by 2.9 μm laser.
Fig. 2 is a spectral emission mechanism, when the Ho3+/Pr3+ co-doped fiber is pumped with 1150nm LD, Ho3+ ions of 5I8 level are excited to 5I6 level via Ground State Absorption (GSA), where an energy transfer up-conversion process occurs, some Ho3+ ions of 5I6 level are concentrated to a higher 5F5 level (5I6 + 5I6 → 5F5 + 5I8), 656nm emission is due to the relaxation of 5F5 level particles down to 5I8 level, and 1.43 μm emission is due to the relaxation of particles at 5F5 level down to 5I6 level. The laser emission of 2.9 μm which is transited from 5I6 energy level to 5I7 energy level is carried out through the energy transfer 1 and 2 processes of Ho3+ particle sum of 5I7 energy level, the energy is transferred to Pr3+ of 3F2 and 3H6, the concentration number of 5I7 energy level is reduced, the laser emission of 2.9 μm is improved, and the laser threshold is reduced (5I7+3H4 → 5I8+3F2, 5I7+3H4 → 5I8+ 3H 6). In addition, a part of particles at Ho3+:5I7 energy level will decay to 5I8 energy level.
Fig. 3 shows that the slope efficiency gradually increases with decreasing fiber length. A2.4 μm long pass filter is added at the output end of the fiber to filter out the pump light (transmittance 90% @2.9 μm), and the laser is finally input into an optical power meter. The back cutting method is utilized to test the optical fiber under different lengths and different pumping powers, when the length of the optical fiber is longer, the pumping light and the 2.9 mu m laser are consumed by the self absorption loss of the optical fiber in the resonant cavity and are transmitted to the surrounding medium in the form of heat, and along with the reduction of the length of the optical fiber, the pumping light and the 2.9 mu m laser realize effective laser transmission in the resonant cavity, so that higher slope efficiency can be obtained, and when the length of the optical fiber is reduced to 193.3mm, the slope efficiency of the 2.9 mu m laser reaches 9.843%.
Fig. 4 shows that the 2.9 μm laser power increases with increasing pump light at a fiber length of 193.3 mm. The laser threshold is 154mW, when the pump power is 1739.2mW, the laser power of 2.9 μm reaches 156.3mW, which is improved by 3 times compared with the previously reported laser power of 2.9 μm fiber using aluminum fluoride fiber and indium fluoride fiber as resonant cavities respectively, and when the length of the fiber is shorter, it has the potential to obtain higher laser output power.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of aluminum fluoride 2.9 mu m high-power optical fiber laser is characterized by comprising the following steps:
s1: placing the dried raw materials into an ultra-fine grinding machine for mixing and grinding;
s2: the raw material ground in the step S1 is put into a platinum crucible dried at high temperature and is fired in a glove box electric furnace by a melting method;
s3: pouring the liquid fired in the step S2 into a mold for annealing until the liquid is cooled to room temperature to prepare a preform;
s4: polishing the surface of the preform rod prepared in the step S3 by using an automatic polishing machine, and then performing surface decontamination;
s5: the product obtained in step S4 was loaded on a drawing tower and drawn into an optical fiber in a nitrogen atmosphere.
2. The method for preparing aluminum fluoride 2.9 μm high power fiber laser as claimed in claim 1, wherein the raw material in step S1 comprises AlF3、BaF2、YF3、PbF2、MgF2And doping Pr and Ho elements therein, grinding the powder in step S1 to 3000-6000 mesh for 10-40 min.
3. The method for preparing aluminum fluoride 2.9 μm high power fiber laser according to claim 2, wherein the doped Pr concentration is 10000-30000 ppm, and the doped Ho concentration is 1000-3000 ppm.
4. The method for preparing high power fiber laser of aluminum fluoride 2.9 μm according to claim 1, wherein the temperature in the glove box in step S2 is 850-1000 ℃, and the firing time is 1-3 h.
5. The method for preparing the aluminum fluoride 2.9 μm high-power fiber laser according to claim 1, wherein the temperature of the die in the step S3 is 300-450 ℃, the annealing time is 1-5 h, and the cooling mode adopts natural cooling.
6. The method for preparing high power fiber laser of aluminum fluoride 2.9 μm according to claim 1, wherein in step S4, polishing is performed to optical grade, and the cleaning agent is alcohol with an alcohol concentration of 80-99%.
7. The utility model provides a testing arrangement of aluminium fluoride 2.9 mu m high power fiber laser, includes laser instrument (1), its characterized in that, two coupling lens (3) that one side of laser instrument (1) was provided with, one side of coupling lens (3) is provided with space beam isolator (4), one side of space beam isolator (4) is provided with focusing lens (5), one side of focusing lens (5) is provided with dichroic mirror (6), one side of dichroic mirror (6) is provided with finished product optic fibre (7), the other end of finished product optic fibre (7) is connected with InF2 jumper (8), the other end of InF2 jumper connection is connected with spectrum appearance (9).
8. The test preparation of the aluminum fluoride 2.9 μm high-power fiber laser as claimed in claim 7, wherein said coupling lens (3) is CaF2 coupling lens, the focal lengths of two said coupling lenses (3) are 100mm and 40mm respectively, and said focusing lens (5) is CaF2 focusing lens with focal length of 6 mm.
9. A test method of aluminum fluoride 2.9 mu m high-power fiber laser is characterized by comprising the following steps:
s1, installing and fixing a laser (1), adjusting two coupling lenses (3), sequentially installing a space beam isolator (4) and a focusing lens (5), placing a drawn finished optical fiber (7), a dichroic mirror (6) and an InF2 jumper (8) at a specified position, and adjusting all devices to reach the specified position;
s2, starting a laser (1), outputting laser, shrinking the laser after passing through two CaF2 coupling lenses, enabling the shrunk laser to pass through a space beam isolator (4) and then reach a focusing lens (5), converging the laser in a fiber core area of a finished product optical fiber (7) which is cut vertically after passing through a dichroic mirror (6), outputting the laser after passing through the finished product optical fiber (7), receiving the laser by an InF2 jumper (8), and inputting the laser into a spectrometer (9);
and S3, recording the data in the step S2, drawing a chart and analyzing the chart.
10. The test method of the aluminum fluoride 2.9 μm high-power fiber laser according to claim 9, wherein the laser (1) has a wavelength of 1150nm, and the test experiment is performed under the protection of nitrogen or inert gas.
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Cited By (2)
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CN112919814A (en) * | 2021-02-23 | 2021-06-08 | 威海长和光导科技有限公司 | Pr (Pr) powder3+/Ho3+ZAlFB-doped optical fiber glass and preparation method thereof |
CN112960905A (en) * | 2021-03-11 | 2021-06-15 | 哈尔滨工程大学 | Ho3+Doped fluoroaluminium glasses |
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CN110896192A (en) * | 2019-11-13 | 2020-03-20 | 江苏师范大学 | Non-quartz glass-based medium-infrared special fiber Raman DFB fiber laser |
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CN110896192A (en) * | 2019-11-13 | 2020-03-20 | 江苏师范大学 | Non-quartz glass-based medium-infrared special fiber Raman DFB fiber laser |
Non-Patent Citations (2)
Title |
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S J JIA: "Ho3+ doped fluoroaluminate glass fibers for 2.9 μm lasing", 《LASER PHYSICS》 * |
SHUNBIN WANG: "2.9 μm lasing from a Ho3+/Pr3+ co-doped AlF3-based glass fiber pumped by a 1150 nm laser", 《OPTICS LETTERS》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112919814A (en) * | 2021-02-23 | 2021-06-08 | 威海长和光导科技有限公司 | Pr (Pr) powder3+/Ho3+ZAlFB-doped optical fiber glass and preparation method thereof |
CN112919814B (en) * | 2021-02-23 | 2021-08-31 | 威海长和光导科技有限公司 | Pr (Pr) powder3+/Ho3+ZAlFB-doped optical fiber glass and preparation method thereof |
CN112960905A (en) * | 2021-03-11 | 2021-06-15 | 哈尔滨工程大学 | Ho3+Doped fluoroaluminium glasses |
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