CN116354598A - Bismuth-gallium co-doped gain fiber serving as gain medium and preparation method thereof - Google Patents
Bismuth-gallium co-doped gain fiber serving as gain medium and preparation method thereof Download PDFInfo
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- XTPMURFLEDRBCW-UHFFFAOYSA-N bismuth gallium Chemical compound [Ga].[Bi] XTPMURFLEDRBCW-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000000835 fiber Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 59
- 239000013307 optical fiber Substances 0.000 claims abstract description 55
- 239000002994 raw material Substances 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000005253 cladding Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000010453 quartz Substances 0.000 claims abstract description 18
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims abstract description 14
- 229910005191 Ga 2 O 3 Inorganic materials 0.000 claims abstract description 12
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 11
- 239000003365 glass fiber Substances 0.000 claims abstract description 11
- 230000003287 optical effect Effects 0.000 claims abstract description 9
- 229910052797 bismuth Inorganic materials 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000005491 wire drawing Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000012856 weighed raw material Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000002269 spontaneous effect Effects 0.000 abstract description 13
- 230000000191 radiation effect Effects 0.000 abstract description 4
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 239000008358 core component Substances 0.000 abstract 1
- 230000004927 fusion Effects 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 17
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 11
- 229910052733 gallium Inorganic materials 0.000 description 11
- 239000005368 silicate glass Substances 0.000 description 9
- 238000000295 emission spectrum Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- LEHUDBPYSAPFFO-UHFFFAOYSA-N alumane;bismuth Chemical compound [AlH3].[Bi] LEHUDBPYSAPFFO-UHFFFAOYSA-N 0.000 description 7
- 229910052710 silicon Inorganic materials 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 238000004891 communication Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000003825 pressing Methods 0.000 description 5
- 239000010431 corundum Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000323 aluminium silicate Inorganic materials 0.000 description 1
- 239000005354 aluminosilicate glass Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- AJNVQOSZGJRYEI-UHFFFAOYSA-N digallium;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Ga+3].[Ga+3] AJNVQOSZGJRYEI-UHFFFAOYSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001195 gallium oxide Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
- C03B37/02718—Thermal treatment of the fibre during the drawing process, e.g. cooling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
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- General Life Sciences & Earth Sciences (AREA)
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Abstract
The invention belongs to the technical field of gain fibers, and discloses a bismuth-gallium co-doped glass fiber serving as a gain medium and a preparation method thereof. The gain fiber mainly comprises a fiber core and a cladding, the cladding is a quartz cladding, and the fiber core is prepared from raw material SiO 2 ,Bi 2 O 3 Ga 2 O 3 Is prepared by the steps of; the fiber core is mainly prepared from the following raw materials in percentage by mol: siO (SiO) 2 :95~99%,Bi 2 O 3 :0.01~0.1%,Ga 2 O 3 :0.05 to 4 percent. The invention uses high-power laser to fuse the core rod to prepare the fiber core component which can not be fused by the traditional fusion quenching method. The optical fiber is easy to weld, has high luminous efficiency, obvious spontaneous radiation effect of optical fiber amplification, covers the near infrared wave band of 1.0-1.55 mu m, and has wave length of 1250-1550 nmThe segments have a switching gain. The bismuth gallium co-doped glass optical fiber is used as a gain medium in an optical amplifier and an optical fiber laser.
Description
Technical Field
The invention belongs to the technical field of optical fiber communication, and particularly relates to a bismuth-gallium co-doped gain optical fiber serving as a gain medium and a preparation method thereof.
Background
Bismuth doped glass has broadband near infrared photoluminescence characteristic and long fluorescence lifetime, and has important significance in optical application as a next generation amplifier material of a large-capacity optical communication system. As such, bismuth doped glass materials have received increasing attention since the near infrared luminescence of bismuth doped glass was first discovered in the early part of the century. Among them, bismuth-doped silicate glass is one of the most promising candidate materials because of its excellent high temperature resistance, optical transparency, chemical stability and ingredient adjustability.
In order to improve the optical response of bismuth doped silicate glasses, a great deal of research has been conducted. Alumina is considered as a dopant that is advantageous in improving near infrared emission intensity of bismuth-doped silicate glass and adjusting emission properties. However, the near infrared luminous intensity of the bismuth doped aluminosilicate glass still needs to be improved, and the effective gain range of the bismuth doped aluminosilicate optical fiber prepared by the traditional MCVD method can only be between 1000 and 1200nm (refer to article: [1 ]]Dianov,E.M.,A.V.Shubin,M.A.Melkumov,O.I.Medvedkov and I.A.Bufetov.High-power cw bismuth-fiber lasers.Journal of the Optical Society of America B-Optical Physics24 1749-1755.) the gain interval is small and cannot reach the use range of the communication band.
Disclosure of Invention
In order to improve the near infrared luminous intensity of the bismuth-doped silicate glass material and expand the gain bandwidth of the bismuth-doped silicate optical fiber, the invention aims to provide the bismuth-gallium co-doped gain optical fiber serving as a gain medium. The invention selects a small amount of bismuth oxide and gallium oxide doped high silicon component and uses high-power CO 2 The laser fuses the gallium bismuth co-doped silicate glass optical fiber preform, and the fiber core fusion method is used for successfully drawing the optical fiber, so that the glass optical fiber has the characteristics of obvious spontaneous radiation effect, wide gain range and the like.
In the invention, gallium is a better doping choice for improving the near infrared luminous intensity and adjusting the emission performance of bismuth doped silicate glass, the near infrared luminous intensity of bismuth gallium co-doped silicate glass is far greater than that of bismuth aluminum co-doped silicate glass, the gain range of the optical fiber almost can cover a plurality of communication wave bands from O to C (1260 to 1565 nm), and the gain range of the optical fiber is wider than that of bismuth aluminum co-doped silicate glass.
The aim of the invention is achieved by the following technical scheme:
a bismuth-gallium co-doped gain optical fiber used as a gain medium is prepared by drawing a bismuth-gallium co-doped glass fiber through a fiber core melting method.
The bismuth-gallium co-doped glass fiber core is mainly prepared from the following raw materials in percentage by mol:
SiO 2 :95~99.5%
Ga 2 O 3 :0.45~4.5%
Bi 2 O 3 :0.05~0.5%
the cladding of the bismuth gallium co-doped glass fiber serving as the gain medium is a high-purity quartz tube;
the fiber core melting method is to uniformly mix raw materials, press-form, sinter, heat to a molten state, cool and process into a rod shape to obtain a fiber core glass rod; the core glass rod is then placed in a hollow cladding and drawn into an optical fiber.
The preparation method of the bismuth gallium co-doped glass optical fiber serving as the gain medium comprises the following steps:
1) SiO is made of 2 、Ga 2 O 3 Bi and Bi 2 O 3 Weighing according to the mole ratio;
2) Fully and uniformly grinding the weighed raw materials, and then performing compression molding;
3) Sintering the pressed sample;
4) Heating the sintered block to a molten state by using high-power laser; closing the laser, and cooling to room temperature to obtain bismuth-gallium co-doped glass blocks;
5) Processing the obtained bismuth-gallium co-doped glass block into a fiber core glass rod, and placing the fiber core glass rod into a hollow cladding to prepare a preform;
6) The preform is drawn into an optical fiber.
The pressing and forming in the step 2) means that the weighed raw materials are placed in a strip-shaped die, pressurized to 10MPa, and taken out after standing for 5 minutes.
The sintering in the step 3) means that the obtained strip sample is placed in a muffle furnace, the temperature is raised to 900-1000 ℃ per minute at 5 ℃, and the temperature is kept for 2-4 hours and then cooled to the room temperature.
The melting in the step 4) refers to heating the sample to 2000-2100 ℃ by using a high-power laser.
The size of the fiber core glass rod in the step 5) is 2-5 mm in diameter and 30-40 mm in length;
in the step 5), the inner diameter of the cladding (quartz rod) is 0.05-0.10 mm larger than that of the fiber core rod, the outer diameter is 30-35 mm, and the length is 200-300 mm.
And 5) after the fiber core glass rod in the step 5) is placed in the cladding, sealing the bottom of the cladding by adopting a solid quartz rod. When the solid quartz rod is adopted for sealing, the solid quartz rod is sintered by oxyhydrogen flame to be adhered together.
The drawing in the step 6) refers to drawing, wherein the temperature of drawing is 2030-2100 ℃, and the speed of drawing is 2-5 m per minute.
The drawing tower is quickly heated to the drawing temperature of the cladding at 200 ℃/min, and the drawing speed and the feeding speed are adjusted to draw the size which can be matched with the commercial quartz optical fiber.
And (3) preserving heat of the prefabricated rod in the step 6) for 30-60 min before wiredrawing.
The diameter of the optical fiber produced in step 6) is 125 to 150. Mu.m.
The bismuth gallium co-doped glass fiber is used as a gain medium in optical amplifiers and fiber lasers.
According to the invention, the gallium-bismuth co-doped optical fiber is successfully prepared by using the method of melting the core rod by using the high-power laser, the spontaneous radiation effect of the optical fiber is good, and the switching gain is successfully measured. No prior art has developed a gain fiber of this composition.
The optical fiber obtained by the invention obtains a broadband amplified spontaneous emission signal by pumping at 808nm after welding, and can realize 5.5dB switching gain at maximum by using 5cm optical fiber, and the gain range is from 1250 to 1550nm, thereby realizing broadband optical amplification.
Compared with the prior art, the invention has the following advantages and effects:
(1) The component of the invention has the broadband near infrared luminescence of 1000-1700 nm under 808nm pumping, and the luminescence property is better than that of bismuth aluminum co-doped component.
(2) The optical fiber drawn by the components has good spontaneous radiation effect, and the gain interval is 1250nm to 1550nm, and covers a plurality of communication wave bands such as O, E, S, C and the like.
(3) The bismuth gallium co-doped gain optical fiber with high-efficiency near infrared fluorescence performance prepared by the invention not only can be used for preparing an optical fiber amplifier, but also can be used for preparing a laser, and the transmission capacity of an optical fiber communication system is improved.
Drawings
FIG. 1 is a spontaneous emission spectrum of the optical fiber of example 1;
FIG. 2 is a spontaneous emission spectrum of the optical fiber of example 2;
FIG. 3 is a graph of the optical fiber switch gain of example 2 using a test fiber length of 5cm;
FIG. 4 is a spontaneous emission spectrum of the optical fiber of example 3;
fig. 5 is a graph showing the comparison of near infrared emission spectra of the bismuth-gallium co-doped high silicon glass material prepared in example 1 and the bismuth-aluminum co-doped high silicon glass material prepared in comparative example 1 under the excitation of 808nm laser.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto. The following processes, unless otherwise specified, are all accomplished or understood by those skilled in the art with reference to the prior art. The reagents or apparatus used were not manufacturer-specific and were considered conventional products commercially available.
Example 1
The embodiment is a preparation method of bismuth gallium co-doped glass optical fiber, comprising the following steps:
(1) Selecting high-purity SiO 2 、Ga 2 O 3 、Bi 2 O 3 As a raw material, wherein SiO 2 :Ga 2 O 3 :Bi 2 O 3 The molar ratio of (2) is 95:4.5:0.5, the raw materials with the total weight of 30g are weighed, and the raw materials are ground in an agate mortar for 30 minutes to obtain fully mixed raw materials;
(2) Pressing the ground mixture into strips by using a mould, then filling the strips into a crucible, heating to 900 ℃ at 5 ℃ per minute by using a muffle furnace, preserving heat for 2 hours at 900 ℃, and cooling to room temperature;
(3) Placing the sintered strip block in a corundum crucible, heating by using laser, heating to 2000 ℃ at 400 ℃ per second, standing for a plurality of seconds, and turning off the laser to cool to room temperature;
(4) Processing the glass prepared in the step (3) into a glass core rod with the diameter of 2mm and the length of 30mm on a cold processing machine tool, and polishing the surface of the glass core rod;
(5) Acid cleaning is carried out on the gallium bismuth co-doped glass core rod prepared in the step (4), the gallium bismuth co-doped glass core rod is placed into a cladding quartz tube (the inner diameter is 2.05mm, the outer diameter is 30 mm), and the bottom of the quartz tube is sealed by a solid quartz rod (oxyhydrogen flame treatment), so that a complete gallium bismuth co-doped glass optical fiber preform is obtained;
(6) And (3) placing the prefabricated rod prepared in the step (5) in a high-temperature wire drawing tower, rapidly heating to 2000 ℃ at 200 ℃/min, preserving heat for 30 minutes, softening the prefabricated rod, controlling the wire drawing speed to be 2 m/min, and drawing the gallium-bismuth co-doped glass optical fiber with the diameter of 125 mu m.
Fig. 1 is a spontaneous emission spectrum of the optical fiber of example 1, and it can be seen that the spontaneous emission spectrum covers a range of 1000 to 1600nm.
Example 2
The embodiment is a preparation method of bismuth gallium co-doped glass optical fiber, comprising the following steps:
(1) Selecting high-purity SiO 2 、Ga 2 O 3 、Bi 2 O 3 As a raw material, wherein SiO 2 :Ga 2 O 3 :Bi 2 O 3 The molar ratio of (2) is 99:0.9:0.1, weighing the raw materials with the total weight of 30g, and grinding the raw materials in an agate mortar for 30 minutes to obtain fully mixed raw materials;
(2) Pressing the ground mixture into strips by using a mould, then filling the strips into a crucible, heating to 900 ℃ at 5 ℃ per minute by using a muffle furnace, preserving heat for 2 hours at 900 ℃, and cooling to room temperature;
(3) Placing the sintered strip block in a corundum crucible, heating by using laser, heating to 2030 ℃ at 400 ℃ per second, standing for several seconds, and turning off the laser to cool to room temperature;
(4) Processing the glass prepared in the step (3) into a glass core rod with the diameter of 4mm and the length of 30mm on a cold processing machine tool, and polishing the surface of the glass core rod;
(5) Acid cleaning is carried out on the gallium bismuth co-doped glass core rod prepared in the step (4), the gallium bismuth co-doped glass core rod is placed into a cladding quartz tube (the inner diameter is 4.05mm, the outer diameter is 30 mm), and the bottom of the quartz tube is sealed by a solid quartz rod (oxyhydrogen flame treatment), so that a complete gallium bismuth co-doped glass optical fiber preform is obtained;
(6) And (3) placing the prefabricated rod prepared in the step (5) in a high-temperature wire drawing tower, rapidly heating to 2000 ℃ at 200 ℃/min, preserving heat for 45 minutes, softening the prefabricated rod, controlling the wire drawing speed to be 2.5 m/min, and drawing the gallium-bismuth co-doped glass optical fiber with the diameter of 125 mu m.
Fig. 2 is a graph of spontaneous emission of the optical fiber of example 2, which shows the spontaneous emission range from 1000nm to 1600nm, and fig. 3 is a graph of the optical fiber switch gain of example 2, which shows the wide gain range, covering O, E, S, C and other wavebands, using a test fiber length of 5 cm.
Example 3
The embodiment is a preparation method of bismuth gallium co-doped glass optical fiber, comprising the following steps:
(1) Selecting high-purity SiO 2 、Ga 2 O 3 、Bi 2 O 3 As a raw material, wherein SiO 2 :Ga 2 O 3 :Bi 2 O 3 The molar ratio of (2) is 95:4.5:0.5, the raw materials with the total weight of 30g are weighed, and the raw materials are ground in an agate mortar for 30 minutes to obtain fully mixed raw materials;
(2) Pressing the ground mixture into strips by using a mould, then filling the strips into a crucible, heating to 900 ℃ at 5 ℃ per minute by using a muffle furnace, preserving heat for 2 hours at 900 ℃, and cooling to room temperature;
(3) Placing the sintered strip block in a corundum crucible, heating by using laser, heating to 2100 ℃ at 400 ℃ per second, standing for a plurality of seconds, and turning off the laser to cool to room temperature;
(4) Processing the glass prepared in the step (3) into a glass core rod with the diameter of 3mm and the length of 30mm on a cold processing machine tool, and polishing the surface of the glass core rod;
(5) Acid cleaning is carried out on the gallium bismuth co-doped glass core rod prepared in the step (4), the gallium bismuth co-doped glass core rod is placed into a cladding quartz tube (the inner diameter is 5.05mm, the outer diameter is 30 mm), and the bottom of the quartz tube is sealed by a solid quartz rod (oxyhydrogen flame treatment), so that a complete gallium bismuth co-doped glass optical fiber preform is obtained;
(6) And (3) placing the prefabricated rod prepared in the step (5) in a high-temperature wire drawing tower, rapidly heating to 2000 ℃ at 200 ℃/min, preserving heat for 60 minutes, softening the prefabricated rod, controlling the wire drawing speed to be 5 m/min, and drawing the gallium-bismuth co-doped glass optical fiber with the diameter of 125 mu m.
FIG. 4 is a spontaneous emission spectrum of the optical fiber of example 3, which covers 1000 to 1600nm.
Comparative example 1
The embodiment is a preparation method of bismuth-aluminum co-doped glass, which comprises the following steps:
(1) Selecting high-purity SiO 2 、Al 2 O 3 、Bi 2 O 3 As a raw material, wherein SiO 2 :Al 2 O 3 :Bi 2 O 3 The molar ratio of (2) is 99.5:4.5:0.5, the raw materials with the total weight of 30g are weighed, and the raw materials are ground in an agate mortar for 30 minutes to obtain fully mixed raw materials;
(2) Pressing the ground mixture into strips by using a mould, then filling the strips into a crucible, heating to 900 ℃ at 5 ℃ per minute by using a muffle furnace, preserving heat for 2 hours at 900 ℃, and cooling to room temperature;
(3) Placing the sintered strip block in a corundum crucible, heating by using laser, heating to 2100 ℃ at 400 ℃ per second, standing for several seconds, and then turning off the laser to cool to room temperature to obtain a glass block;
fig. 5 is a graph showing the comparison of near infrared emission spectra of the bismuth-gallium co-doped high silicon glass material prepared in example 1 and the bismuth-aluminum co-doped high silicon glass material prepared in comparative example 1 under the excitation of 808nm laser.
As compared with example 1, the near infrared emission intensity of the bismuth-gallium co-doped high silicon glass is more than twice that of the bismuth-aluminum co-doped high silicon glass under the excitation of the 808nm laser, and the peak position is red shifted.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the examples. Any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the invention are intended to be equivalent substitutes for those that do not depart from the spirit and principles of the invention.
Claims (8)
1. A bismuth gallium co-doped glass optical fiber used as a gain medium is characterized in that: the bismuth gallium co-doped glass fiber consists of a bismuth gallium co-doped glass fiber core and a quartz cladding, and is prepared by fiber core melting wire drawing;
the bismuth-gallium co-doped glass fiber core is mainly prepared from the following raw materials in percentage by mol:
SiO 2 :95~99.5%
Ga 2 O 3 :0.45~4.5%
Bi 2 O 3 :0.05~0.5%
the fiber core melting method is to uniformly mix raw materials, press-form, sinter, heat to a molten state, cool and process into a rod shape to obtain a fiber core glass rod; the core glass rod is then placed in a hollow cladding and drawn into an optical fiber.
2. The method for preparing the bismuth gallium co-doped glass optical fiber used as the gain medium according to claim 1, comprising the following steps:
1) SiO is made of 2 、Ga 2 O 3 Bi and Bi 2 O 3 Weighing according to the mole ratio;
2) Fully and uniformly grinding the weighed raw materials, and then performing compression molding;
3) Sintering the pressed sample;
4) Heating the sintered block to a molten state by using high-power laser, and cooling to room temperature to obtain a bismuth-gallium co-doped glass block;
5) Processing the obtained bismuth-gallium co-doped glass block into a fiber core glass rod, placing the fiber core glass rod in a hollow cladding,
manufacturing a prefabricated rod;
6) The preform is drawn into an optical fiber.
3. The method for preparing the bismuth gallium co-doped glass optical fiber serving as the gain medium according to claim 2, wherein the method comprises the following steps:
the sintering in the step 3) means that the pressed and molded sample is placed in a muffle furnace, the temperature is raised to 900-1000 ℃ per minute at 5 ℃, and the sample is cooled to room temperature after heat preservation for 2-4 hours.
4. The method for preparing the bismuth gallium co-doped glass optical fiber serving as the gain medium according to claim 2, wherein the method comprises the following steps:
the melting in the step 4) refers to heating the sample to 2000-2100 ℃ by using a high-power laser.
5. The method for preparing the bismuth gallium co-doped glass optical fiber serving as the gain medium according to claim 2, wherein the method comprises the following steps:
the size of the fiber core glass rod in the step 5) is 2-5 mm in diameter and 30-40 mm in length;
the cladding in the step 5) is a high-purity quartz tube; the inner diameter of the cladding is 0.05-0.1 mm larger than that of the core rod, the outer diameter is 30-35 mm, and the length is 200-300 mm.
6. The method for preparing the bismuth gallium co-doped glass optical fiber serving as the gain medium according to claim 2, wherein the method comprises the following steps:
the drawing in the step 6) refers to drawing, wherein the temperature of drawing is 2030-2100 ℃, and the speed of drawing is 2-5 m per minute;
the heat preservation time of the prefabricated rod in the step 6) before wiredrawing is 30-60 min;
the diameter of the optical fiber produced in step 6) is 125 to 150. Mu.m.
7. The use of bismuth gallium co-doped glass fiber as gain medium according to claim 1, characterized in that: the bismuth gallium co-doped glass fiber serving as the gain medium is used for preparing an optical amplifier and an optical fiber laser.
8. The use according to claim 7, characterized in that: the bismuth gallium co-doped glass fiber is used as a gain medium in an amplifier and a fiber laser.
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