CN104591535A - Method for preparing rare earth-doped quartz glass microstructure optical fibers by laser melting technology - Google Patents

Method for preparing rare earth-doped quartz glass microstructure optical fibers by laser melting technology Download PDF

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CN104591535A
CN104591535A CN201410617663.8A CN201410617663A CN104591535A CN 104591535 A CN104591535 A CN 104591535A CN 201410617663 A CN201410617663 A CN 201410617663A CN 104591535 A CN104591535 A CN 104591535A
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optical fibers
powder
laser
microstructured optical
doped
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CN104591535B (en
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张卫
周桂耀
夏长明
侯峙云
刘建涛
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Guangzhou Huarenyihe Specialty Fiber Technology Co ltd
South China Normal University
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Guangzhou Huarenyihe Specialty Fiber Technology Co ltd
South China Normal University
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Abstract

The invention discloses a method for preparing rare earth-doped quartz glass microstructure optical fibers by a laser melting technology. The method comprises the following steps of powder preparation, melting, doped rod treatment and optical fiber precast rod preparation, and rare earth-doped quartz glass microstructure optical fiber drawing. The invention discloses a use of the uniformly doped quartz glass rod in an all solid state laser and a microstructure optical fiber. The invention discloses a laser melting system. The laser melting system comprises a powder feeding device, a laser source, a mother rod, a clamp, a motor and a guide rail. The prepared rare earth-doped powder and the quartz glass microstructure optical fibers realize uniform doping of a plurality of rare earth ions. The prepared doped microstructure optical fibers have a rare earth ion effective-doping concentration more than 10000ppm.

Description

Laser melting technology is adopted to prepare the method for rear-earth-doped silica glass microstructured optical fibers
Technical field
The present invention relates to the method adopting laser melting technology to prepare rear-earth-doped silica glass microstructured optical fibers.
Background technology
Compared with traditional solid statelaser, optical fiber laser has the plurality of advantages such as efficient, compact, tunable, beam quality is excellent, heat radiation is good, gain is high, laser threshold is low, is therefore widely used in the fields such as industrial processes, material processing, military and national defense.But, along with the development and application of the industrial processes such as laser cutting, welding and high energy laser weapon, the more high-power output of optical fiber laser and laser beam quality are had higher requirement, but high-capacity optical fiber laser also brings the new problems such as the damage from laser of fiber optic materials and non-linear effect simultaneously, the optical fiber of large core diameter is adopted can effectively to improve damage from laser problem, and shorten fiber lengths, improve doping content and then effectively can reduce non-linear effect.For traditional large core diameter doped fiber, due to enough low clad/core refringence cannot be obtained, more difficultly realize single-mode output.Large mould field high-concentration dopant microstructured optical fibers (MSF) has while maintenance big mode field area, keeps the superiority of endless single mode, plays conclusive effect to high-capacity optical fiber laser development.And the preparation of rear-earth-doped microstructured optical fibers, the preparation of especially rear-earth-doped plug is again the core determining MSF function and performance, and can also determine MSF finally practical.Along with the appearance of the optical fiber designs such as large mould field, new requirement is proposed to the technique preparing preform, as larger sized plug, higher doping content, being uniformly distributed of dopant ion, the accurate control of dopant material specific refractory power, many rare earth ions are mixed altogether, this is for currently used technology, as: improve vapour deposition process (MCVD), foreign minister's vapour deposition process (OVD), vapour phase axial deposition technique (VAD) and plasma activated chemical vapour deposition technique (PCVD), sol-gel method (SOL-GEL) etc. will be difficult to realize, thus limit further developing of the MSF of high-dopant concentration.
Summary of the invention
The object of the present invention is to provide the method adopting laser melting technology to prepare rear-earth-doped silica glass microstructured optical fibers.
The technical solution used in the present invention is:
Adopt laser melting technology to prepare the method for rear-earth-doped silica glass microstructured optical fibers, step is as follows:
1) powder process: take the muriate of rare earth ion and mix thing altogether, soluble in water, be mixed with the aqueous solution, utilize carrier gas to be transported in the aqueous solution by quantitative silicon tetrachloride, corresponding chemical reaction occurs, after reaction terminates, removing moisture, obtain powder, powder is fully added heat abstraction hydroxyl under chlorine and oxidizing atmosphere, obtains uniform rear-earth-doped mixed powder;
2) melting: utilize shielding gas to be blowed by powder to the excellent top of mother, after powder arrives female excellent top, the effect of carbon dioxide laser is utilized to make it melt formation vitreous state, in the process, along with the rising of temperature, the viscosity degradation of glass metal, in glass metal, the diameter of bubble increases gradually and constantly rises and finally removes from glass metal; Meanwhile, female rod rotates and declines, and glass metal leaves smelting zone gradually, and temperature reduces, and makes glass metal cool formation glass stick gradually, finally obtains the quartz glass bar of uniform doping;
3) process of doping rod and the preparation of preform: it is 10-30cm that the doping quartz pushrod prepared is cut into length, namely can be made into the Uniform Doped quartz pushrod that external diameter is 5-30mm after grinding and buffing; It can be used as the fibre core of microstructured optical fibers prefabricated rods, adopt to pile up and prepare the method for microstructured optical fibers prefabricated rods: choose external diameter be 15-50mm, internal diameter 10-35mm, length 20-100cm silica tube as outer tube, at endoporus circumferentially-periodic arrangement quartz capillary centered by the quartz pushrod that adulterates respectively, thus the prefabricated rods of obtained doping microstructured optical fibers;
4) drawing of rear-earth-doped silica glass microstructured optical fibers: the microstructured optical fibers prefabricated rods upper step prepared, is arranged on fiber drawing tower, by being heated to 1800-2000 DEG C; Finally draw out the rear-earth-doped silica glass microstructured optical fibers that external diameter is 100-1000 μm.
In step 1), described carrier gas is oxygen or air.
In step 1), described rare earth ion is Er 3+, Tm 3+, Yb 3+, Ho 3+, Nd 3+in at least one; Described thing of mixing altogether is at least one in the compound of aluminum chloride, phosphorus and fluorine.
In step 1), the concentration of rear-earth-doped mixed powder Rare Earth Ion is 3000-20000ppm.
In step 1), the air flow of carrier gas is at 0.1m 3/ h-4.8m 3/ h, SiCl 4operational throughput is 1 ~ 4 times of solution quality.
Step 2) in, described shielding gas is oxygen, nitrogen or air; Powder operational throughput is 1-50g/min, and the lowering speed of female rod is 0.1-5mm/min; Under the effect of carbon dioxide laser, the temperature at female excellent top rises to 1800-2500 DEG C, and powder smelting becomes vitreous state.
Above-mentioned steps 2) quartz glass bar of uniform doping that obtains preparing the application in all solid state laser and microstructured optical fibers.
A kind of laser melting system, comprises powder feeder, LASER Light Source, female rod, fixture, motor, guide rail; Wherein, the doping powder that powder feeder is used for step 1) to obtain is transported to female excellent top; The heat energy that LASER Light Source adulterates powder for providing melting; Fixture is used for clamping female rod; Motor is used for driving female rod to rotate; Guide rail is used to provide the track that power supply machine falls.
Described LASER Light Source is one and arrives multiple.
When described LASER Light Source is single beam laser light source, then described laser melting system also comprises laser beam expanding system, for adjusting the size of laser facula.
The invention has the beneficial effects as follows:
Rear-earth-doped powder prepared by the present invention and silica glass microstructured optical fibers, can realize the Uniform Doped of multiple rare earth ion, and in doping microstructured optical fibers prepared by the present invention, the Effective Doping concentration of rare earth ion is more than 10000ppm.
Specifically:
Rear-earth-doped powder prepared by the present invention and microstructured optical fibers thereof, can realize multiple rare earth ion, as Yb 3+, Er 3+, Ho 3+and Tm 3+deng Uniform Doped, and mixing altogether of many rare earth ions can be realized, not only can make up the shortcoming of MCVD, dopant species also has better handiness.Silica glass Uniform Doped can be realized, high-concentration dopant, the accurate control of specific refractory power and variation doping, and effectively can reduce the hydroxy radical content of dopant material, adopt and pile up capillary tube technique and to arrange out flexile prefabricated rods, draw can obtain single mode by high temperature wire-drawer-tower, the high-concentration dopant microstructured optical fibers of large mould field, the Effective Doping concentration of rare earth ion is more than 10000ppm, new approach is opened for preparing special optical fiber, for the development of high-capacity optical fiber laser, the stability of Rear Earth Doped Fiber Laser can be improved, and improve the power of laser apparatus.
Accompanying drawing explanation
The Yb of Fig. 1 prepared by embodiment 1 3+the pictorial diagram of doped silica glass rod;
Fig. 2 is the Yb adopting embodiment 1 to prepare 3+the end view drawing of the large mould field high density single mode microstructured optical fibers that doped silica glass draws;
Fig. 3 is Yb dosed optical fiber loss figure;
Fig. 4 is multicore microstructured optical fibers end view drawing;
Fig. 5 is erbium and ytterbium codoping microstructured optical fibers end view drawing;
Fig. 6 is erbium and ytterbium codoping microstructured optical fibers loss spectra;
Fig. 7 is 980nm LD laser pumping erbium-ytterbium co-doped fiber fluorescence spectrum figure;
Fig. 8 is for mixing thulium microstructured optical fibers end view drawing;
Fig. 9 is for mixing thulium microstructured optical fibers loss figure.
Figure 10 is the structural representation of the laser melting system that the present invention relates to.
Embodiment
Adopt laser melting technology to prepare the method for rear-earth-doped silica glass microstructured optical fibers, step is as follows:
1) powder process: using rare earth ion as doped source, takes the muriate of rare earth ion and mixes thing altogether, and being dissolved in deionized water, being mixed with the aqueous solution, and wherein, the concentration of doped source is: 1000-12000ppm, and the concentration of mixing thing is altogether 3000-20000ppm; Then with oxygen or air as carrier gas by SiCl 4(or organism of silicon) is delivered in above-mentioned solution, and the air flow of carrier gas is at 0.1m 3/ h-4.8m 3/ h, SiCl 4operational throughput is 1 ~ 4 times of solution quality, SiCl 4can produce with water and react as follows:
SiCl 4+2H 2O=SiO 2↓+4HCl↑
2RCl 3+3H 2O=R 2O 3↓+6HCl↑
Wherein, R represents rare earth ion or mixes thing ion altogether.
Then by water evaporate to dryness, obtain powder, loaded in quartz container by powder, and under chlorine atmosphere, be heated to 800-1100 degree with eliminating hydroxide, heat-up time is 1-6 hour;
Wherein:
Described rare earth ion is Er 3+, Tm 3+, Yb 3+, Ho 3+, Nd 3+in at least one; Preferably, be Er 3+, Tm 3+, Yb 3+, Ho 3+in one.
Described thing of mixing altogether is at least one in the compound of aluminum chloride, phosphorus and fluorine; Preferably, be aluminum chloride;
2) melting: adopt single or multiple carbon dioxide laser as thermal source, selects laser power, adjustment Laser beam energy distribution, thus keeps smelting zone temperature between 1800-2500 degree.Then the doping powder prepared is added powder feeder, utilize shielding gas (oxygen, nitrogen or air) powder to be delivered to female rod (being preferably quartz pushrod) top (being smelting zone), powder operational throughput is 1-50g/min ,the flow of conveying protection gas is 500-5000ml/min; after powder arrives female excellent top, under the effect of carbon dioxide laser, fusing forms vitreous state; along with the rising of temperature; the viscosity degradation of glass metal; bubble in glass metal also increases thereupon; the speed that bubble rises is accelerated, thus promotes the elimination of bubble and striped.And rotate while decline along with female rod, glass metal leaves smelting zone gradually, the reduction of temperature, glass metal is made to cool formation glass stick gradually, in addition, regulate the speed of rotation (10-300rpm/min) of the scram speed (0.1-5mm/min) of female rod and female rod, to get rid of the phase mutual diffusion of bubble and glass component, thus reach the object of homogenizing; Along with rotation and the lasting decline thereof of female rod, the final quartz glass bar forming uniform doping;
In this step, adopt multiple (or single) carbon dioxide laser as thermal source, in protective atmosphere, fast melting is carried out to dopant mixture, because laser processing is non-contact type processing, effectively can reduce the foreign matter content in dopant material, and the optical density of hydroxyl to carbon dioxide laser is higher, adopt carbon dioxide laser as thermal source, effectively can reduce the content of hydroxyl in material, the temperature of carbon dioxide laser thermal source and thermo parameters method thereof can regulate arbitrarily according to laser power and laser facula distribution thereof; According to single beam laser as thermal source, its thermo parameters method in conjunction with laser beam shaping technology, can be regulated by beam expanding lens adjustment laser facula size (6-20mm);
3) process of doping rod and the preparation of preform: the doping quartz pushrod prepared is cut into the rod that length is 10-30cm, namely can be made into the Uniform Doped quartz pushrod that external diameter is 5-30mm after grinding and buffing; It is as the fibre core of microstructured optical fibers prefabricated rods, adopt to pile up and prepare the method for microstructured optical fibers prefabricated rods: choose external diameter be 15-50mm, internal diameter 10-35mm, length 20-100cm silica tube as outer tube, at endoporus circumferentially-periodic arrangement quartz capillary centered by the quartz pushrod that adulterates respectively, thus the prefabricated rods of obtained doping microstructured optical fibers;
4) drawing of rear-earth-doped silica glass microstructured optical fibers: the microstructured optical fibers prefabricated rods that upper step is prepared, be arranged on fiber drawing tower, at the temperature of 1800-2000 DEG C, finally draw out the rear-earth-doped silica glass microstructured optical fibers that external diameter is 100-2000 μm, preferably, draw in microstructured optical fibers process, photocuring processes can be adopted simultaneously at the skin coating 1-2 layer silicone protective layer of described microstructured optical fibers;
The step 2 of above-mentioned method) quartz glass bar of uniform doping that obtains preparing the application in all solid state laser and microstructured optical fibers;
Preparing the embody rule method in all solid state laser be: the quartz glass bar of the uniform doping prepared is cut into the rod that length is 10-30cm, namely the Uniform Doped quartz pushrod that external diameter is 5-30mm is can be made into after grinding and buffing, adopt precise polished equipment, excellent two ends polishing of adulterating simultaneously.The kind rear-earth-doped according to quartz pushrod, selects suitable pumping source, carries out the development of all solid state laser.
Through detecting, in finally prepd doping microstructured optical fibers, the Effective Doping concentration of rare earth ion is more than 10000ppm.
As shown in Figure 10, be the structural representation of laser melting system that the present invention relates to, laser melting system: comprise powder feeder 2, LASER Light Source 9, female rod 4, fixture 5, motor 6, guide rail 7;
Wherein, powder feeder 2 is transported to female excellent 4 ends for the doping powder 1 step 1) obtained; The heat energy that LASER Light Source 9 adulterates powder 1 for providing melting; Fixture 5 is used for clamping female rod 4; Motor 6 is used for driving female rod 4 to rotate; Guide rail 7 is used to provide the track that power supply machine 6 falls.
Described LASER Light Source is one and arrives multiple; Preferably, be 1-5; Preferably, with carbon dioxide laser as thermal source, provide the heat energy that powder is adulterated in melting; If described LASER Light Source is single beam laser light source, then preferably, native system also comprises laser beam expanding system 8, for adjusting the size of laser facula;
Through the processing step of melting, being preferably quartz pushrod at the excellent 4(of mother) quartz glass bar 3 of uniform doping is formed on top.
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1:
Consisting of (mass percent) of doping powder: Yb 2o 3: 1.28%, Al 2o 3: 2.49%, SiO 2: 96.23%; The raw material dosage of preparation doping powder is determined by forming; Select more following precursor to prepare and mix ytterbium silica glass: six water Ytterbium trichlorides, Aluminum Chloride Hexahydrate, silicon tetrachloride (solution).Select deionized water as solvent.In silica glass beaker, add deionized water, Aluminum Chloride Hexahydrate and six water Ytterbium trichlorides are dissolved in deionized water, stirs 30 minutes, be prepared into doped solution.Then utilize dry oxygen as the carrier gas (air flow of carrier gas: 0.1-4.8 m 3/ h) silicon tetrachloride (intake of silicon tetrachloride is 1-4 times of doped solution quality) is carried in doped solution, and ceaselessly stir, form the material of similar gels shape.Then this material is added the unnecessary moisture of heat abstraction at the temperature of 200 degree, after 6 hours, be prepared into dry powder.Then by dried powder under chlorine atmosphere, under the heat of 1100 degree, remove remaining hydroxyl, after 6 hours, prepare anhydrous drying doping powder;
Then the dried powder of preparation is loaded in powder feeder, under the protection of oxygen as shielding gas, powder is delivered to smelting zone, oxygen ventilation amount is (500-5000) ml/min, powder melts after arriving smelting zone (top of the female rod of quartz) and forms vitreous state under the effect of carbon dioxide laser, ytterbium silica glass is mixed in formation, female rod rotates (speed is 10-300rpm/min) while decline (speed is 0.1-5mm/min), glass metal leaves smelting zone gradually, the reduction of temperature, glass metal is made to cool formation glass stick gradually, finally preparing diameter is 8mm, length be 300mm mix ytterbium quartz glass bar,
Ytterbium quartz glass bar sanding and polishing will be mixed, form the fibre core of 7.2mm preform, then the method for piling up kapillary is utilized to prepare preform, the external diameter of kapillary is 0.7mm, the external diameter of preform is 30mm, the prepared ytterbium quartz glass bar of mixing of which floor airport of prefabricated rods center is replaced, so just prepares complete Yb-doping microstructure preform;
What afterwards prefabricated rods is fixed on wire-drawer-tower send in bar system, is drawn into the Yb dosed optical fiber of 0.3mm under the hot conditions of 1800 degree.
The Yb of Fig. 1 prepared by this example 3+the pictorial diagram of doped silica glass rod, its Effective Doping concentration is 12000ppm;
Fig. 2 is the Yb adopting this example to prepare 3+the end view drawing of the large mould field high density single mode microstructured optical fibers that doped silica glass draws;
The background loss of Yb dosed optical fiber is low, and background loss is less than 0.25dB/m 1200nm, and as shown in Figure 3, the background loss value that Yb-doping microstructure optical fiber is being positioned at 1200 nm wavelength places is less than 0.25 dB/m.In addition, also observe two obvious absorption peaks, lay respectively at 1390 nm and 2235 nm wavelength places, it is all caused by hydroxyl group absorption.
Meanwhile, multicore microstructured optical fibers can also be prepared in this way, as shown in Figure 4.
In addition, the rare earth doped material prepared in this way and microstructured optical fibers thereof, can realize mixing altogether of different rare earth ions and see as embodiment 2, not only can make up the shortcoming of MCVD, dopant species also has better handiness.Silica glass Uniform Doped can be realized, high-concentration dopant, the accurate control of specific refractory power and variation doping, and effectively can reduce the hydroxy radical content of dopant material, adopt and pile up capillary tube technique and to arrange out flexile prefabricated rods, draw can obtain single mode by high temperature wire-drawer-tower, the high-concentration dopant microstructured optical fibers of large mould field, the Effective Doping concentration of rare earth ion is more than 12000ppm, new approach is opened for preparing special optical fiber, for the development of high-capacity optical fiber laser, the stability of Rear Earth Doped Fiber Laser can be improved, and improve the power of laser apparatus.
embodiment 2:
Consisting of (mass percent) of doping powder: Yb 2o 3: 2.53%, Er 2o 3: 0.61%, Al 2o 3: 2.46%, SiO 2: 94.40%; The raw material dosage of preparation doping powder is determined by forming; In silica glass beaker, add deionized water, Aluminum Chloride Hexahydrate, Erbium trichloride, six water Ytterbium trichlorides are dissolved in deionized water, form erbium and ytterbium codoping solution, this solution is stirred 30 minutes at ambient temperature.Then utilize dry oxygen as the carrier gas (air flow of carrier gas: 0.1-4.8 m 3/ h) silicon tetrachloride (intake of silicon tetrachloride is 1-4 times of doped solution quality) is carried in doped solution, and ceaselessly stir, form the material of similar gels shape.Then this material is added the unnecessary moisture of heat abstraction at the temperature of 200 degree, after 6 hours, obtain dry doping powder.Then by dried powder under chlorine atmosphere, under the heat of 900 degree, remove remaining hydroxyl, after 6 hours, prepare anhydrous drying doping powder;
Then the anhydrous dried powder of preparation is loaded in powder feeder, dry oxygen as shielding gas protection under by powder to smelting zone, oxygen ventilation amount is (500-5000) ml/min, after powder arrives smelting zone (top of the female rod of quartz), under the effect of carbon dioxide laser, fast melt forms vitreous state, form erbium and ytterbium codoping silica glass, female rod rotates (speed is 10-300rpm/min) while decline (speed is 0.1-5mm/min), glass metal leaves smelting zone gradually, the reduction of temperature, glass metal is made to cool formation glass stick gradually, finally preparing diameter is 8mm, length is the erbium and ytterbium codoping quartz glass bar of 300mm,
By erbium and ytterbium codoping quartz glass bar sanding and polishing, form the fibre core of 7.2mm preform, then the method for piling up kapillary is utilized to prepare preform, the external diameter of kapillary is 0.7mm, the external diameter of preform is 30mm, the prepared erbium and ytterbium codoping quartz glass bar of which floor airport of prefabricated rods center is replaced, so just prepares complete Yb-doping microstructure preform;
What afterwards prefabricated rods is fixed on wire-drawer-tower send in bar system, and under the hot conditions of 1800 degree, be drawn into the erbium and ytterbium codoping microstructured optical fibers of 0.3mm, as shown in Figure 5, Fig. 6 is erbium and ytterbium codoping microstructured optical fibers loss spectra to its structure, and 977nm absorption loss is up to 7dB/m.Fig. 7 is 980nm LD laser pumping erbium and ytterbium codoping microstructured optical fibers fluorescence spectrum figure, as can be seen from the figure achieves ytterbium erbium energy conversion process with optical fiber prepared by this method.
embodiment 3:
Consisting of (mass percent) of doping powder: Tm 2o 3: 1.26%, Al 2o 3: 2.5%, SiO 2: 96.24%; The raw material dosage of preparation doping powder is determined by forming; In silica glass beaker, add deionized water, Aluminum Chloride Hexahydrate, thulium chloride are dissolved in deionized water, formed and mix thulium solution, this solution is stirred 30 minutes at ambient temperature.Then utilize dry oxygen as the carrier gas (air flow of carrier gas: 0.1-4.8 m 3/ h) silicon tetrachloride (intake of silicon tetrachloride is 1-4 times of doped solution quality) is carried in doped solution, and ceaselessly stir, form the material of similar gels shape.Then this material is added the unnecessary moisture of heat abstraction at the temperature of 200 degree, after 6 hours, obtain dry doping powder.Then by dried powder under chlorine atmosphere, under the heat of 1050 degree, remove remaining hydroxyl, after 6 hours, prepare anhydrous drying doping powder;
Then the anhydrous dried powder of preparation is loaded in powder feeder, dry oxygen shielding gas protection under by powder to smelting zone, oxygen ventilation amount is 500-5000ml/min, after powder arrives smelting zone (top of the female rod of quartz), under the effect of carbon dioxide laser, fast melt forms vitreous state, thulium silica glass is mixed in formation, female rod rotates (speed is 10-300rpm/min) while decline (speed is 0.1-5mm/min), glass metal leaves smelting zone gradually, the reduction of temperature, glass metal is made to cool formation glass stick gradually, finally preparing diameter is 8mm, length be 300mm mix thulium quartz glass bar,
Thulium quartz glass bar sanding and polishing will be mixed, form the fibre core of 7.2mm preform, then the method for piling up kapillary is utilized to prepare preform, the external diameter of kapillary is 0.7mm, the external diameter of preform is 30mm, the prepared thulium quartz glass bar of mixing of which floor airport of prefabricated rods center is replaced, so just prepares and complete mix thulium microstructured optical fibers prefabricated rods;
What afterwards prefabricated rods is fixed on wire-drawer-tower send in bar system, be drawn under the hot conditions of 1800 degree external diameter be 0.3mm mix thulium microstructured optical fibers.Fig. 8 be draw by this method mix thulium microstructured optical fibers end view drawing.Fig. 9 is for mixing thulium microstructured optical fibers loss figure.Optical fiber is very strong to the receptivity of pumping wavelength, and the absorption loss of 793nm is up to 14dB/m, and the optical fiber standby with MCVD legal system matches in excellence or beauty even better.

Claims (10)

1. adopt laser melting technology to prepare the method for rear-earth-doped silica glass microstructured optical fibers, it is characterized in that: step is as follows:
1) powder process: take the muriate of rare earth ion and mix thing altogether, soluble in water, be mixed with the aqueous solution, utilize carrier gas to be transported in the aqueous solution by quantitative silicon tetrachloride, corresponding chemical reaction occurs, after reaction terminates, removing moisture, obtain powder, powder is fully added heat abstraction hydroxyl under chlorine and oxidizing atmosphere, obtains uniform rear-earth-doped mixed powder;
2) melting: utilize shielding gas to be blowed by powder to the excellent top of mother, after powder arrives female excellent top, the effect of carbon dioxide laser is utilized to make it melt formation vitreous state, in the process, along with the rising of temperature, the viscosity degradation of glass metal, in glass metal, the diameter of bubble increases gradually and constantly rises and finally removes from glass metal; Meanwhile, female rod rotates and declines, and glass metal leaves smelting zone gradually, and temperature reduces, and makes glass metal cool formation glass stick gradually, finally obtains the quartz glass bar of uniform doping;
3) process of doping rod and the preparation of preform: it is 10-30cm that the doping quartz pushrod prepared is cut into length, namely can be made into the Uniform Doped quartz pushrod that external diameter is 5-30mm after grinding and buffing; It can be used as the fibre core of microstructured optical fibers prefabricated rods, adopt to pile up and prepare the method for microstructured optical fibers prefabricated rods: choose external diameter be 15-50mm, internal diameter 10-35mm, length 20-100cm silica tube as outer tube, at endoporus circumferentially-periodic arrangement quartz capillary centered by the quartz pushrod that adulterates respectively, thus the prefabricated rods of obtained doping microstructured optical fibers;
4) drawing of rear-earth-doped silica glass microstructured optical fibers: the microstructured optical fibers prefabricated rods upper step prepared, is arranged on fiber drawing tower, by being heated to 1800-2000 DEG C; Finally draw out the rear-earth-doped silica glass microstructured optical fibers that external diameter is 100-1000 μm.
2. employing laser melting legal system according to claim 1 is for the method for rear-earth-doped silica glass microstructured optical fibers, it is characterized in that: in step 1), and described carrier gas is oxygen or air.
3. employing laser melting legal system according to claim 1 is for the method for rear-earth-doped silica glass microstructured optical fibers, it is characterized in that: in step 1), and described rare earth ion is Er 3+, Tm 3+, Yb 3+, Ho 3+, Nd 3+in at least one; Described thing of mixing altogether is at least one in the compound of aluminum chloride, phosphorus and fluorine.
4. employing laser melting legal system according to claim 1 is for the method for rear-earth-doped silica glass microstructured optical fibers, it is characterized in that: in step 1), and the concentration of rear-earth-doped mixed powder Rare Earth Ion is 3000-20000ppm.
5. employing laser melting legal system according to claim 1 is for the method for rear-earth-doped silica glass microstructured optical fibers, and it is characterized in that: in step 1), the air flow of carrier gas is at 0.1m 3/ h-4.8m 3/ h, SiCl 4operational throughput is 1 ~ 4 times of solution quality.
6. employing laser melting legal system according to claim 1 is for the method for rear-earth-doped silica glass microstructured optical fibers, it is characterized in that: step 2) in, described shielding gas is oxygen, nitrogen or air; Powder operational throughput is 1-50g/min, and the lowering speed of female rod is 0.1-5mm/min; Under the effect of carbon dioxide laser, the temperature at female excellent top rises to 1800-2500 DEG C, and powder smelting becomes vitreous state.
7. the step 2 of method according to claim 1) quartz glass bar of uniform doping that obtains preparing the application in all solid state laser and microstructured optical fibers.
8. a laser melting system, is characterized in that: comprise powder feeder, LASER Light Source, female rod, fixture, motor, guide rail;
Wherein, the doping powder that powder feeder is used for step 1) in claim 1 to obtain is transported to female excellent top; The heat energy that LASER Light Source adulterates powder for providing melting; Fixture is used for clamping female rod; Motor is used for driving female rod to rotate; Guide rail is used to provide the track that power supply machine falls.
9. a kind of laser melting system according to claim 8, is characterized in that: described LASER Light Source is one and arrives multiple.
10. a kind of laser melting system according to claim 8, is characterized in that: when described LASER Light Source is single beam laser light source, then described laser melting system also comprises laser beam expanding system, for adjusting the size of laser facula.
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CN109085674A (en) * 2018-08-31 2018-12-25 华南理工大学 All-glass fiber derived from 2 micron waveband monocrystalline of one kind and preparation method thereof
CN111253074A (en) * 2020-01-21 2020-06-09 华南师范大学 Erbium-ytterbium co-doped quartz substrate up-conversion luminescent fiber and preparation method thereof
CN112645584A (en) * 2020-12-11 2021-04-13 华南师范大学 Laser drawing tower for drawing special optical fiber
CN112645584B (en) * 2020-12-11 2023-08-08 华南师范大学 Laser drawing tower for drawing special optical fiber

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