CN108483899A - One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof - Google Patents

One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof Download PDF

Info

Publication number
CN108483899A
CN108483899A CN201810230656.0A CN201810230656A CN108483899A CN 108483899 A CN108483899 A CN 108483899A CN 201810230656 A CN201810230656 A CN 201810230656A CN 108483899 A CN108483899 A CN 108483899A
Authority
CN
China
Prior art keywords
glass
optical fiber
semiconductor
nanocrystal
active optical
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201810230656.0A
Other languages
Chinese (zh)
Inventor
钱奇
张琪
杨中民
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South China University of Technology SCUT
Original Assignee
South China University of Technology SCUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by South China University of Technology SCUT filed Critical South China University of Technology SCUT
Priority to CN201810230656.0A priority Critical patent/CN108483899A/en
Publication of CN108483899A publication Critical patent/CN108483899A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/02—Optical fibres with cladding with or without a coating
    • G02B6/0229—Optical fibres with cladding with or without a coating characterised by nanostructures, i.e. structures of size less than 100 nm, e.g. quantum dots

Abstract

The invention discloses one kind mixed with semiconductor β Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof, fibre core is using poreless high silica glass as matrix, semiconductor β Ga2O3Nanocrystal Uniform Doped is in the substrate.The preparation method of the present invention obtains cellular glass after split-phase acidleach processing with the borosilicate glass of specific composition first, cellular glass is then immersed in Ga3+Through hydrothermal deposition in solion, then cellular glass is placed in tube furnace and obtains core material after high temperature sintering, preform is prepared with above-mentioned core material and pure quartz glass later, finally, Active Optical Fiber is made in prepared preform drawing.One aspect of the present invention is difficult to the laser wavelength generated supplemented with rear-earth-doped Active Optical Fiber, on the other hand avoid active microcrystalline glass optical fiber easy crystal in drawing process grow up even crystallization technology of preparing problem.

Description

One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof
Technical field
The present invention relates to a kind of Active Optical Fibers and preparation method thereof, more particularly to one kind is mixed with semiconductor β-Ga2O3It is nanocrystalline Active Optical Fiber of body and preparation method thereof.
Background technology
Active Optical Fiber has a wide range of applications in the fields such as optical fiber laser, fiber amplifier, Fibre Optical Sensor, currently, Active Optical Fiber is mainly rare-earth doped optical fibre, but since rare earth ion stimulated radiation generates fluorescent light source layer electron transition in the inner Radiation makes rear-earth-doped Active Optical Fiber be only capable of generating the laser of specific band, it is difficult to by the variation in ligand field adjust rare earth from The fluorescent characteristic of son, and then limit the application field of Active Optical Fiber.
Semiconductor doping devitrified glass has some unique optical properties, can supplement what rare-earth doped optical fibre was difficult to generate Laser wavelength.Lot of domestic and foreign scholar has carried out extensive research to devitrified glass, but is the failure to realize the active crystallite of low-loss The preparation of glass optical fiber.It is prefabricated to microcrystalline glass optical fiber because needing when its major technical difficulty is that microcrystalline glass optical fiber is drawn The reheating that stick carries out causes in glass crystal grain to be grown up or even glass entirety crystallization, to make prepared Active Optical Fiber Quality is severely impacted.
Nano semiconductor material is a kind of novel semiconductor material of rising in recent years, since its material dimension and structure are special The nano-scale of sign, and quantum size effect, quantum confined effect, macroscopic quantum tunneling effect and skin effect are shown, from And it is made to show different from physical characteristics such as electricity, magnetic, light, the heat of conventional body material, show many peculiar new phenomenons.
β-Ga2O3It is a kind of broad stopband transparent conductive oxide semi-conducting material of stabilization, energy gap is about 4.8~ 5.l eV are the quality materials for manufacturing the light emitting devices such as high brightness blue, green light LED and laser diode, in photoelectricity Have broad application prospects in terms of sub- device.Due to β-Ga2O3Itself existing defects, in addition to generation exciton is compound and band-to-band transition It shines outer, several intraband transitions can also be generated and shone, β-Ga have thus been expanded2O3Application field.It is introduced in vitreum β-Ga2O3Nano microcrystalline, since quantum confined effect and quantum size effect often generate weight to the optical property of nano material It influences.
The doping techniques of Active Optical Fiber include mainly two kinds of common process of liquid and gas, however, both technologies are deposited It is mostly sub-micron in the size of some problems, dopant material, amplification performance and amplification efficiency are vulnerable to restriction.In recent years, There is researcher to propose that a kind of technique for atomic layer deposition prepares novel doping Active Optical Fiber, but the technology for the deficiency of above-mentioned technique Mainly for the preparation of film rather than nano particle；Many research groups both domestic and external are also to the technology of preparing of mixed nanometer optical fiber A large amount of research has been carried out with relevant problem in science.
Won-Tack Han of Gwangju, Korea Technological research institute (GIST) etc. are using solution immersion process and combine at high temperature Reason, is prepared into mixed with the semiconductor compound nanos particle Active Optical Fiber such as PbTe, the Amplified Spontaneous for realizing 1537nm wave bands is penetrated It radiates (ASE), but its doping efficiency is very low, dispersibility is also poor.
The Liekki companies of Finland propose that direct nano-particle deposits (DND) technology, which is mainly used for rare earth element Doping cannot achieve broadband amplification.
Research group where Brazilian Jacob has studied incorporation PbTe quantum dots in tellurate glass optical fiber, in 1100nm Wave band observes apparent exciton absorption peak, and observes nano-particle using high-resolution TEM, but since the uniformity of doping is asked Topic, does not measure light radiation characteristic.
The incorporation of semiconductor PbTe quantum dots is had periodical porous structure by S.Kawanishi of Japanese NTT companies etc. Photonic crystal fiber is seen using the semiconductor laser that wavelength is 1535nm, power is 10mW as pumping in 1554nm wave bands Significant photoluminescence spectra is measured, but this technology needs photonic crystal fiber, cost is higher, and doping techniques also lack Consistency and long-term stability.
The preparation of domestic Active Optical Fiber mainly uses modified chemical vapor deposition process (MCVD), the Duan Yuwen of Beijing University of Post ＆ Telecommunication logical Cross this method and successfully prepare and mix InP nanoparticle optical fiber, grain size is about 15-20nm, but its prepare preform and Wire drawing required temperature is very high, more than 1600 DEG C.
In conclusion in order to which the performance for further increasing Active Optical Fiber and the existing technology of preparing for solving Active Optical Fiber are asked Topic, this patent propose a kind of new Active Optical Fiber and preparation method thereof.By nanoscale aperture, pore size distribution uniformly and mutually interconnect Ga is impregnated in logical cellular glass3+Solution and after obtained through hydrolytic precipitation sintering process it is fine and close transparent mixed with semiconductor β- Ga2O3Nanocrystalline vagcor, and light is made with the pure quartz glass as clad material using this glass as core material Fine prefabricated rods are finally prepared into mixed with semiconductor β-Ga2O3It is active to solve doped rare earth element with this for nanocrystalline Active Optical Fiber The technology of preparing problem of the limitation of the emission band of optical fiber, active microcrystalline glass optical fiber and existing doped semiconductor Active Optical Fiber.
Invention content
The purpose of the present invention is that solve the above-mentioned problems and provides one kind mixed with semiconductor β-Ga2O3Nanocrystal Active Optical Fiber and preparation method thereof.
The present invention is achieved through the following technical solutions above-mentioned purpose：
One kind of the invention is mixed with semiconductor β-Ga2O3The Active Optical Fiber of nanocrystal, fibre core are with poreless high silica glass Matrix, semiconductor β-Ga2O3Nanocrystal is entrained in fibre core Medium Culture.
Further, the semiconductor β-Ga2O3Nanocrystal Uniform Doped is in the fibre core Medium Culture.Half in the fibre core Conductor β-Ga2O3Nanocrystal size is 2~3nm.
One kind of the invention is mixed with semiconductor β-Ga2O3The preparation method of the Active Optical Fiber of nanocrystal, includes the following steps：
(1) become SiO according to group263.5%-B2O328%-Na2O 8.5% (wt%) with electronic balance weigh analysis it is pure SiO2、H3BO3、Na2CO3Reagent amounts to 100g；Batch is fully ground, after mixing, is put into the platinum crucible of 200ml, waits for silicon After molybdenum stove is warming up to 1550 DEG C, the platinum crucible for filling batch is placed on silicon molybdenum stove inside holding 2 hours；Then by platinum crucible Interior melt is poured on pre-warmed stainless steel grinding tool and is molded, and molding glass blocks is placed on temperature rapidly and has risen to 480 DEG C Annealing furnace in keep the temperature 1h, last furnace cooling；The mother glass of water white transparency is pressed into institute with precision gas cutting machine after annealing Size is needed to be cut into sheet；
(2) some are kept flat on lightweight refracrory liner is melted that uniformities are good, mother glass piece of bubble-free flawless, And be put into the Muffle furnace of precise temperature control, 560 DEG C of heat preservation 48h are warming up to the heating rate of 4 DEG C/min, are then powered off with stove It is cooled to room temperature；
(3) the mother glass piece after taking out heat treatment in Muffle furnace, it is with sand paper that 6 surfaces of these sheet glass are manual It polishes, deionized water ultrasonic cleaning is then used to dry slide in case Acid Leaching；
(4) to the hydrochloric acid and saturation NH filled with 2mol/L4It is put into through step in the beaker for the Acid Leaching liquid that Cl solution is prepared Suddenly the sheet glass of (3) processing, beaker mouth is sealed with preservative film, then beaker is placed in water-bath and is warming up to 95 DEG C, heat preservation 24h；Then the sheet glass leached burin-in process in 95 DEG C of deionized waters is put into for 24 hours, again to use sheet glass after aging It is 7 that deionized water and absolute ethyl alcohol, which are cleaned by ultrasonic repeatedly to the pH value of cleaning solution, and then sheet glass is placed in 120 in constant temperature oven After DEG C dry 5h, and it is put in drier and preserves；Obtained sheet glass final in this way is that nanoscale aperture, pore size distribution are uniform And the cellular glass of mutual unicom；
(5) it takes out the cellular glass immersion prepared and fills 0.015molL-1GaCl3In the beaker of solution, guarantor is used in combination Fresh film sealing and standing 1 day, so that Ga3+It is sufficiently submerged in the duct of cellular glass；
(6) it takes out and is soaked with Ga3+Cellular glass and be put into and fill 150ml 0.015molL-1GaCl3The beaker of solution In, it is used in combination preservative film to seal, then the beaker for being placed with porous glass disks is put into water-bath, 5h is kept the temperature at 70 DEG C；It kept the temperature Afterwards, porous glass disks are taken out rapidly, deionized water and absolute ethyl alcohol is used in combination to clean repeatedly, are remained in cellular glass with removing GaCl3Porous glass disks are then placed in clean culture dish in baking oven in 120 DEG C of dry 5h by solution；
It (7) will be through in step (6) treated porous glass disks are placed on clean aluminium oxide Noah's ark, then Noah's ark be put into In tube furnace, in high-purity Ar atmosphere, 900 DEG C of heat preservation 1h is risen to the heating rate of 5 DEG C/min, are then rapidly heated to 1100 DEG C heat preservation 1h after slowly cool to room temperature with the furnace；
(8) after tube furnace is cooled to room temperature, sheet glass is taken out, finally obtains water white transparency, closely knit glass sample is Mixed with semiconductor β-Ga2O3Nanocrystalline vagcor；
(9) fibre core is made in sheet glass in step (8), pure quartz glass is used in combination that covering is made, is finally prepared into optical fiber Prefabricated rods；
(10) Active Optical Fiber is made in prepared preform drawing.
Further, it is prepared mixed with semiconductor β-Ga using the method for hydrolytic precipitation sintering in step (8)2O3Nanocrystal Vagcor.Preform is drawn into mixed with semiconductor β-Ga using wire-drawer-tower in step (10)2O3Nanocrystal Active Optical Fiber.
The beneficial effects of the present invention are：
The present invention is one kind mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof, with the prior art It compares, Active Optical Fiber of the present invention is difficult to the laser wavelength generated supplemented with rare-earth doped optical fibre, has widened Active Optical Fiber Application field；It is long that the preparation method of the Active Optical Fiber avoids active microcrystalline glass optical fiber easy crystal in drawing process The technology of preparing problem of big even crystallization；The preparation method of Active Optical Fiber of the present invention it is simple for process easily-controllable, it is used to set It is standby simple, reduce manufacturing cost.
Description of the drawings
Fig. 1 is mixed with semiconductor β-Ga2O3Nanocrystalline Active Optical Fiber section and index distribution schematic diagram；
Fig. 2 is mixed with semiconductor β-Ga2O3The preparation flow schematic diagram of nanocrystalline Active Optical Fiber.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings：
Fig. 1 is in the embodiment of the present invention mixed with semiconductor β-Ga2O3Nanocrystalline Active Optical Fiber section and index distribution are shown It is intended to, there is the Active Optical Fiber new fibre core to form, and the fibre core is using poreless high silica glass as matrix, semiconductor β-Ga2O3It receives Rice crystal doping is in fibre core Medium Culture.
The fibre core Medium Culture is uniformly mixed with semiconductor β-Ga2O3Nanocrystal.Wherein it is entire to refer to fibre core for fibre core Uniform Doped Semiconductor β-Ga in region2O3Nanocrystal has identical percent by volume.
Semiconductor β-Ga2O3 the nanocrystal sizes being distributed in the fibre core are 2~3nm.
Semiconductor β-Ga are mixed in Active Optical Fiber2O3Nanocrystal, due to semiconductor β-Ga2O3Crystal is a kind of dark purple Outer transparent wide bandgap semiconductor oxide, energy gap is about 4.8~5.1eV, it may be observed that Strong indigo plants, green light are manufactures The quality material of the light emitting devices such as high brightness blue, green light LED and laser diode, has in terms of opto-electronic device Wide application prospect.Due to β-Ga2O3Itself existing defects can be in addition to occurring other than exciton is compound and band-to-band transition shines Several intraband transitions are generated to shine；In addition, β-Ga2O3Also there is good gas sensing property and catalytic, thus expanded β- Ga2O3Application field.And β-Ga2O3Nanocrystal, since quantum confined effect and quantum size effect are often to nanometer material The optical property of material has an important influence on, to show excellent physics and chemical property, therefore, mixed with semiconductor β- Ga2O3On the one hand nanocrystalline Active Optical Fiber is difficult to the laser wavelength generated supplemented with rear-earth-doped Active Optical Fiber, on the other hand The Active Optical Fiber is set to be applied more broadly in the fields such as optical fiber laser, fiber amplifier, Fibre Optical Sensor.
The present invention mixed with semiconductor β-Ga2O3The preparation method of nanocrystalline Active Optical Fiber is based on hydrolytic precipitation sintering system Technique is made, is specifically comprised the following steps：
(1) become SiO according to group263.5%-B2O328%-Na2O 8.5% (wt%) with electronic balance weigh analysis it is pure SiO2、H3BO3、Na2CO3Reagent amounts to 100g.Batch is fully ground, after mixing, is put into the platinum crucible of 200ml, waits for silicon After molybdenum stove is warming up to 1550 DEG C, the platinum crucible for filling batch is placed on silicon molybdenum stove inside holding 2 hours.Then by platinum crucible Interior melt is poured on pre-warmed stainless steel grinding tool and is molded, and molding glass blocks is placed on temperature rapidly and has risen to 480 DEG C Annealing furnace in keep the temperature 1h, last furnace cooling.The mother glass of water white transparency is pressed into institute with precision gas cutting machine after annealing Size is needed to be cut into sheet.
(2) some are kept flat on lightweight refracrory liner is melted that uniformities are good, mother glass piece of bubble-free flawless, And be put into the Muffle furnace of precise temperature control, 560 DEG C of heat preservation 48h are warming up to the heating rate of 4 DEG C/min, are then powered off with stove It is cooled to room temperature.
(3) the mother glass piece after taking out heat treatment in Muffle furnace, it is with sand paper that 6 surfaces of these sheet glass are manual It polishes, deionized water ultrasonic cleaning is then used to dry slide in case Acid Leaching.
(4) to the hydrochloric acid and saturation NH filled with 2mol/L4It is put into through step in the beaker for the Acid Leaching liquid that Cl solution is prepared Suddenly the sheet glass of (3) processing, beaker mouth is sealed with preservative film, then beaker is placed in water-bath and is warming up to 95 DEG C, heat preservation 24h.Then the sheet glass leached burin-in process in 95 DEG C of deionized waters is put into for 24 hours, again to use sheet glass after aging It is 7 that deionized water and absolute ethyl alcohol, which are cleaned by ultrasonic repeatedly to the PH values of cleaning solution, and then sheet glass is placed in constant temperature oven After 120 DEG C of dry 5h, and it is put in drier and preserves.Obtained sheet glass final in this way is nanoscale aperture, pore size distribution The cellular glass of uniform and mutual unicom.
(5) it takes out the cellular glass immersion prepared and fills 0.015molL-1GaCl3In the beaker of solution, guarantor is used in combination Fresh film sealing and standing 1 day, so that Ga3+It is sufficiently submerged in the duct of cellular glass.
(6) it takes out and is soaked with Ga3+Cellular glass and be put into and fill 150ml 0.015molL-1GaCl3The beaker of solution In, it is used in combination preservative film to seal, then the beaker for being placed with porous glass disks is put into water-bath, 5h is kept the temperature at 70 DEG C.It kept the temperature Afterwards, porous glass disks are taken out rapidly, deionized water and absolute ethyl alcohol is used in combination to clean repeatedly, are remained in cellular glass with removing GaCl3Porous glass disks are then placed in clean culture dish in baking oven in 120 DEG C of dry 5h. by solution
It (7) will be through in step (6) treated porous glass disks are placed on clean aluminium oxide Noah's ark, then Noah's ark be put into In tube furnace, in high-purity Ar atmosphere, with the heating rate of 5 DEG C/min rise to 900 DEG C heat preservation 1h, be then rapidly heated to Room temperature is slowly cooled to the furnace after 1100 DEG C of heat preservation 1h.
(8) after tube furnace is cooled to room temperature, sheet glass is taken out, finally obtains water white transparency, closely knit glass sample is Mixed with semiconductor β-Ga2O3Nanocrystalline vagcor.
(9) fibre core is made in sheet glass in step (8), pure quartz glass is used in combination that covering is made, is finally prepared into optical fiber Prefabricated rods.
(10) prepared preform drawing is made by Active Optical Fiber using wire-drawer-tower.
The present invention mixed with semiconductor β-Ga2O3The principle of the preparation method of nanocrystalline Active Optical Fiber is with cellular glass For template, there is big specific surface area using the nano grade pore road of cellular glass, to have stronger adsorption capacity, in this way will Cellular glass is immersed in a concentration of 0.015molL-1GaCl3In solution, make Ga3+Channel surfaces are adsorbed on, it then will be porous Glass is put into the GaCl of same concentrations3In solution, heating water bath is to 70 DEG C and keeps the temperature 5h.At this moment, Ga3+Water occurs in channel surfaces Solution precipitation generates GaOOH precipitations, and is deposited on channel surfaces.Then by cellular glass in tube furnace and in high-purity Ar gas In atmosphere, in temperature ramp de, GaOOH precipitations are thermally decomposed, and Ga is generated2O3And Ga occurs2O3Crystal transfer, finally Form β-Ga2O3Nanocrystal, and hole is closed completely during cellular glass keeps the temperature 1h at 1100 DEG C, β-Ga2O3It is nanocrystalline Body is by SiO2Package, obtains closely knit transparent mixed with β-Ga2O3The vagcor of nanocrystal.Then with mixed with β-Ga2O3 Fibre core is made in the vagcor of nanocrystal, is used in combination pure quartz glass that covering is made, and is prepared into preform.Finally adopt Active Optical Fiber is made in prepared preform drawing with wire-drawer-tower.
The present invention mixed with semiconductor β-Ga2O3The preparation method of nanocrystalline Active Optical Fiber, on the one hand, avoid active Microcrystalline glass optical fiber easy crystal in drawing process is grown up or even the technology of preparing problem of crystallization；On the other hand, the technique letter Single easily-controllable, device therefor is simple, reduces manufacturing cost.
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its Equivalent thereof.

Claims (6)

1. one kind is mixed with semiconductor β-Ga2O3The Active Optical Fiber of nanocrystal, it is characterised in that：Its fibre core is with poreless high silica glass Glass is matrix, semiconductor β-Ga2O3Nanocrystal is entrained in fibre core Medium Culture.
2. according to claim 1 mixed with semiconductor β-Ga2O3The Active Optical Fiber of nanocrystal, which is characterized in that semiconductor β-Ga2O3Nanocrystal Uniform Doped is in the fibre core Medium Culture.
3. according to claim 1 mixed with semiconductor β-Ga2O3The Active Optical Fiber of nanocrystal, which is characterized in that the fibre Semiconductor β-Ga in core2O3Nanocrystal size is 2~3nm.
4. one kind is mixed with semiconductor β-Ga2O3The preparation method of the Active Optical Fiber of nanocrystal, it is characterised in that：Including following step Suddenly：
(1) become SiO according to group263.5%-B2O328%-Na2O 8.5% (wt%) with electronic balance weigh analysis it is pure SiO2、H3BO3、Na2CO3Reagent amounts to 100g；Batch is fully ground, after mixing, is put into the platinum crucible of 200ml, waits for silicon After molybdenum stove is warming up to 1550 DEG C, the platinum crucible for filling batch is placed on silicon molybdenum stove inside holding 2 hours；Then by platinum crucible Interior melt is poured on pre-warmed stainless steel grinding tool and is molded, and molding glass blocks is placed on temperature rapidly and has risen to 480 DEG C Annealing furnace in keep the temperature 1h, last furnace cooling；The mother glass of water white transparency is pressed into institute with precision gas cutting machine after annealing Size is needed to be cut into sheet；
(2) some are kept flat on lightweight refracrory liner and is melted that uniformities are good, mother glass piece of bubble-free flawless, and are put In the Muffle furnace for entering precise temperature control, 560 DEG C of heat preservation 48h are warming up to the heating rate of 4 DEG C/min, then power-off cools to the furnace Room temperature；
(3) the mother glass piece after taking out heat treatment in Muffle furnace, is ground on 6 surfaces of these sheet glass with sand paper manually It is flat, then use deionized water ultrasonic cleaning to dry slide in case Acid Leaching；
(4) to the hydrochloric acid and saturation NH filled with 2mol/L4It is put into through step (3) in the beaker for the Acid Leaching liquid that Cl solution is prepared The sheet glass of processing seals beaker mouth with preservative film, then beaker is placed in water-bath and is warming up to 95 DEG C, and heat preservation is for 24 hours；Then The sheet glass leached is put into 95 DEG C of deionized waters burin-in process for 24 hours, again by sheet glass deionized water after aging It is 7 to be cleaned by ultrasonic repeatedly with absolute ethyl alcohol to the pH value of cleaning solution, and sheet glass is then placed in 120 DEG C of dry 5h in constant temperature oven Afterwards, and it is put in preservation in drier；Obtained sheet glass final in this way is nanoscale aperture, pore size distribution uniformly and mutually interconnects Logical cellular glass；
(5) it takes out the cellular glass immersion prepared and fills 0.015molL-1GaCl3In the beaker of solution, preservative film is used in combination Sealing and standing 1 day, so that Ga3+It is sufficiently submerged in the duct of cellular glass；
(6) it takes out and is soaked with Ga3+Cellular glass and be put into and fill 150ml 0.015molL-1GaCl3In the beaker of solution, It is used in combination preservative film to seal, then the beaker for being placed with porous glass disks is put into water-bath, 5h is kept the temperature at 70 DEG C；After heat preservation, It is rapid to take out porous glass disks, it is used in combination deionized water and absolute ethyl alcohol to clean repeatedly, is remained in cellular glass with removing GaCl3Porous glass disks are then placed in clean culture dish in baking oven in 120 DEG C of dry 5h by solution；
It (7) will be through in step (6) treated porous glass disks are placed on clean aluminium oxide Noah's ark, Noah's ark be then put into tubular type In stove, in high-purity Ar atmosphere, 900 DEG C of heat preservation 1h is risen to the heating rate of 5 DEG C/min, is then rapidly heated to 1100 DEG C and protects Room temperature is slowly cooled to the furnace after warm 1h；
(8) after tube furnace is cooled to room temperature, take out sheet glass, finally obtain water white transparency, closely knit glass sample i.e. mixed with Semiconductor β-Ga2O3Nanocrystalline vagcor；
(9) fibre core is made in sheet glass in step (8), pure quartz glass is used in combination that covering is made, is finally prepared into optical fiber prefabricating Stick；
(10) Active Optical Fiber is made in prepared preform drawing.
5. preparation method according to claim 2, which is characterized in that using the method for hydrolytic precipitation sintering in step (8) It prepares mixed with semiconductor β-Ga2O3The vagcor of nanocrystal.
6. preparation method according to claim 2, which is characterized in that use wire-drawer-tower by preform in step (10) It is drawn into mixed with semiconductor β-Ga2O3The Active Optical Fiber of nanocrystal.
CN201810230656.0A 2018-03-20 2018-03-20 One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof Pending CN108483899A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810230656.0A CN108483899A (en) 2018-03-20 2018-03-20 One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810230656.0A CN108483899A (en) 2018-03-20 2018-03-20 One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof

Publications (1)

Publication Number Publication Date
CN108483899A true CN108483899A (en) 2018-09-04

Family

ID=63318778

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810230656.0A Pending CN108483899A (en) 2018-03-20 2018-03-20 One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof

Country Status (1)

Country Link
CN (1) CN108483899A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110187432A (en) * 2019-04-30 2019-08-30 上海大学 A kind of preparation method and device of active microcrystal fiber
CN113024126A (en) * 2021-03-17 2021-06-25 山东海富光子科技股份有限公司 Preparation method of glass microstructure with nanoscale holes

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110187432A (en) * 2019-04-30 2019-08-30 上海大学 A kind of preparation method and device of active microcrystal fiber
US11502475B2 (en) 2019-04-30 2022-11-15 Shanghai University Method and device for processing active microcrystalline fiber by magnetic field induction and lasering
CN113024126A (en) * 2021-03-17 2021-06-25 山东海富光子科技股份有限公司 Preparation method of glass microstructure with nanoscale holes
CN113024126B (en) * 2021-03-17 2023-03-14 山东海富光子科技股份有限公司 Preparation method of glass microstructure with nanoscale holes

Similar Documents

Publication Publication Date Title
Reza Dousti et al. Enhanced frequency upconversion in Er 3+-doped sodium lead tellurite glass containing silver nanoparticles
Dong et al. Quantum dot-doped glasses and fibers: fabrication and optical properties
Qiao et al. Spectroscopic properties of neodymium doped high silica glass and aluminum codoping effects on the enhancement of fluorescence emission
Hu et al. Femtosecond-laser-induced precipitation of CsPbBr3 perovskite nanocrystals in glasses for solar spectral conversion
CN109516679B (en) Intermediate infrared luminescent material of rare earth ion doped microcrystalline glass and preparation method thereof
Wu et al. Tunable upconversion luminescence of monodisperse Y2O3: Er3+/Yb3+/Tm3+ nanoparticles
Murugadoss ZnO/CdS nanocomposites: synthesis, structure and morphology
Iskhakova et al. Microstructure, composition, and luminescent properties of bismuth-doped porous glass and optical fiber preforms
Gunji et al. Efficiency enhancement of silicon solar cells covered by GeO2-PbO glasses doped with Eu3+ and TiO2 nanoparticles
Cheng et al. An optical fiber glass containing PbSe quantum dots
CN108483899A (en) One kind is mixed with semiconductor β-Ga2O3Active Optical Fiber of nanocrystal and preparation method thereof
Chen et al. Effects of In2O3 nanoparticles doping on the photoluminescent properties of Eu2+/Eu3+ ions in silica glasses
Du et al. Enhance the Er 3+ upconversion luminescence by constructing NaGdF 4: Er 3+@ NaGdF 4: Er 3+ active-core/active-shell nanocrystals
Chen et al. Growth of SnO 2 nanocrystals co-doped with Eu 3+ for highly enhanced photoluminescence in mesoporous silica glasses
Mattos et al. Performance improvement of Si solar cell via down-Conversion and plasmonic processes using Eu3+ doped TeO2-GeO2-PbO glasses with silver nanoparticles as cover layer
Tran et al. A review on rare-earth activated SnO2-based photonic structures: Synthesis, fabrication and photoluminescence properties
Li et al. Enhanced tunable mid-infrared emissions by controlling rare earth ion energy transfer processes in multifunctional multiphase solids
Kim et al. Lead sulfide quantum dots in glasses containing rare-earth ions
CN109354497B (en) Ho-doped transparent scandium oxide ceramic and preparation method thereof
Li et al. Fluorescent optical fiber intensity ratio temperature sensor based on polymer matrix using down-conversion from ZnS: Cu
CN109023524B (en) Erbium-holmium-praseodymium tri-doped lead fluoride mid-infrared laser crystal and preparation method thereof
Chen et al. A study on the growth of Yb: YVO4 single crystal
Pei et al. Sol–gel synthesis of silver nanocrystals embedded in sodium borosilicate monolithic transparent glass with giant third-order optical nonlinearities
Podhorodecki et al. 1.54 μm photoluminescence from Er-doped sol–gel derived In2O3 films embedded in porous anodic alumina
CN104891572A (en) A micro-nano potassium yttrium tungstate film and a preparing method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination