CN104692656A - 2mu m silica fiber core rod glass and preparation method thereof - Google Patents
2mu m silica fiber core rod glass and preparation method thereof Download PDFInfo
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- CN104692656A CN104692656A CN201510054242.3A CN201510054242A CN104692656A CN 104692656 A CN104692656 A CN 104692656A CN 201510054242 A CN201510054242 A CN 201510054242A CN 104692656 A CN104692656 A CN 104692656A
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Abstract
The invention provides 2mu m silica fiber core rod glass, including a thulium-doped or holmium-doped silica fiber core rod glass, and a preparation method of the glass. The core rod glass is prepared by virtue of the following steps: preparing an evenly doped high-concentration rare-earth silicon oxide powder by use of a sol-gel method from a solution; and performing decarbonization, dehydroxylation and ball milling processing on the powder, and then burning the processed powder to obtain the core rod glass. The large-size, high-rare earth ion doped core rod glass is applicable to preparing large-size and high-uniformity Tm or Ho doped double-clad photonic crystal silica fiber; and as a result, relatively high laser efficiency can be obtained.
Description
Technical field
The present invention relates to the preparation of preform, particularly a kind of 2 μm of quartz optical fibre core glass comprise Tm
3+or Ho
3+doping quartz optical fibre core glass and preparation method thereof.
Background technology
2 μm of laser be widely used in opticfiber communication, military weapon, in the field such as infrared pumping source and laser medicine.For meeting civilian and military demand, the development of 2 μm of laser is very meaningful.From 1988, people (the Electronics Letters such as the D.C.Hanna of Southampton, Britain university, 1988, Vol.24, No.19, pp.1222-1223), since reported first mixes Tm3+ quartz fiber laser, the evolution that Tm3+ silica fibre experienced by single covering, double clad, triple clad (publication number: US6941053 B2) and photonic crystal fiber has been mixed.
The preparation method of rear-earth-doped prefabricated quartz fiber rod more ripe is at present chemical vapour deposition (MCVD) the binding soln infusion method improved.From technique, MCVD has the advantages such as loss is low, good uniformity for preparing Traditional dopant optical fiber, but exist doping content on the low side, be difficult to be prepared into the shortcomings such as large core diameter.Larger difficulty is had to the preparation of the prefabricated rod mandrel of large mould field, high-concentration dopant PCF.Therefore, employing MCVD method is difficult to realize large mould field, prepared by high-concentration dopant PCF, and this becomes the bottleneck problem of restriction ultra high power, the development of multi-wavelength tunable fiber laser, limits the further raising of high-capacity optical fiber laser performance.
A patent (publication number: US 2002/0073739A1) of the U.S. discloses a kind of method of " mixing gas phase process (HVP) " that uses and realizes rare earth doped fiber high-concentration dopant, the method can realize online rare earth ion doped function, but the rare earth doped compound used due to it is organic compound, the carbon introduced and a certain amount of hydroxyl fail effectively to remove, cause the carbide concentration of preform hydroxyl and silicon to raise, increase considerably the non-pumped absorption loss of optical fiber.Although the silicon source of this patent is also organic compound, after being through a series of process of tube furnace, eliminate residual carbon and hydroxyl well.Patent of invention " a kind of manufacture method of rare-earth-doped fiber precast rod plug " (publication number: CN 102875019A) of flames of war sharp Micron Technology Co., Ltd in Wuhan disclosed in January, 2013.The method utilize rare earth material mineral compound together doping metals mineral compound be mixed rare earth material prefabricated target rod, on this prefabricated target rod, its high temperature ablation is made to evaporate prefabricated target material laser focusing, pass into the mixed gas of the carbide composition of oxygen, chlorine, silicon tetrachloride gas, germanium tetrachloride gas and fluorine, carry out formation of deposits fibre-optical mandrel prefabricated component, finally this plug prefabricated component high temperature melting is contracted, form transparent preform.But the rare earth material prefabricated target of this invention rod is obtained by physical mixed, is not prepare powder from pure solution method, is difficult to fundamentally to solve the homogeneity question in multiple dopant ion situation.In addition, this invention mixes rare earth silica glass plug clearly not obtaining large size.
Summary of the invention
The present invention is directed to deficiency and the defect of above-mentioned existing fiber core technology of preparing, according to the demand of high-capacity optical fiber laser development, there is provided a kind of 2 μm of quartz optical fibre core glass to comprise to mix the preparation method of thulium or holmium doping quartz optical fibre core glass, adopt the Tm3+ that sol-gel method is obtained, the silica glass that Ho3+ or high density Tm3+, Al3+ mix altogether or Ho3+, Al3+ mix altogether has the feature of low hydroxy radical content, high uniformity, meets the application requiring of preparation large size, high rare earth ion doped quartz optical fibre core glass.The plug that application the method obtains can be used for preparing large size, the double clad of high uniformity is mixed Tm or mixed Ho quartz optical fibre core glass, and highly doped, large core diameter is mixed Tm or mixed double clad or the PCF silica fibre of Ho, obtains higher lasing efficiency.
Technical solution of the present invention is:
A kind of 2 μm of quartz optical fibre core glass, comprise and mix thulium or mix holmium quartz optical fibre core glass, its feature is, the molar percentage compositing range of this plug glass is as follows:
Thulium-doped silica fib plug glass:
SiO
2： 91～98.4mol％
Tm
2O
3： 0.1～0.8mol％
Al
2O
3： 1.5～8mol％
Or
Mix holmium quartz optical fibre core glass:
SiO
2： 93.6～98.32mol％
Ho
2O
3： 0.08～0.4mol％
Al
2O
3： 1.6～6mol％。
The preparation method of above-mentioned 2 μm of quartz optical fibre core glass, its feature is, the method comprises the following steps:
1. the selected molar percentage mixed thulium or mix holmium quartz optical fibre core glass composition, by selected molar percentage weighing raw materials silicon alkoxide, six hydrous thulium chlorides or six chloride hydrate holmiums, Aluminium chloride hexahydrate, wherein silicon alkoxide introduces SiO
2, six hydrous thulium chlorides introduce Tm
2o
3or six chloride hydrate holmiums introduce Ho
2o
3, Aluminium chloride hexahydrate introduces Al
2o
3;
2. silicon alkoxide is pressed: water: the proportions water of organic solvent=1:2 ~ 10:4 ~ 20 and the mixing solutions of organic solvent, then six described hydrous thulium chlorides or six chloride hydrate holmiums, Aluminium chloride hexahydrate are added in this mixing solutions successively, add the hydrolysis of catalyst silicon alkoxide, at room temperature fully stirred through 1 ~ 24 hour, obtain Tm
3+or Ho
3+, Al
3+the silicon oxide vitreosol liquid mixed altogether, leaves standstill 1 ~ 10 day to its gelation;
3. described silica gel is placed in tube furnace, under oxygen atmosphere, under the condition of 600 ~ 1000 DEG C, insulation 5 ~ 12 hours removing residual carbons and hydroxyl, form Tm
3+or Ho
3+, Al
3+the silicon oxide powder mixed altogether;
4. adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 140 ~ 160 object polytetrafluoros;
5. described powder is placed in corundum crucible, at the High Temperature Furnaces Heating Apparatus 10 of 1600 ~ 2000 DEG C
-1~ 10
-3carry out melting in 1 ~ 8 hour under Pa vacuum tightness, furnace cooling forms bubble-free transparent glass;
6. described bubble-free transparent glass is processed as diameter and is more than or equal to 3.0mm, length is more than or equal to the plug of 50mm, optical polish, is placed in mass concentration after the HF acid acid treatment 5 ~ 15min of 5 ~ 20%, takes out dry, obtains and mix Tm
3+or Ho
3+prefabricated quartz fiber rod core.
Described silicon alkoxide is Si (OC
2h
5)
4or Si (OCH
3)
4.
Described step 2. middle organic solvent is C
2h
5oH or CH
3oH.
7. described step 2. middle silicon alkoxide hydrolyst is hydrochloric acid or ammoniacal liquor, and when adopting hydrochloric acid catalysis, the hydrochloric acid content added makes solution ph be 1 ~ 3; When adopting ammonia-catalyzed, the ammonia vol added makes solution ph be 8 ~ 10.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) adopt sol-gel method from solution, realize the Uniform Doped of molecular level, adopt sol-gel method can prepare the doping of higher rare earth ion concentration, and Tm
3+or Ho
3+, Al
3+the silicon oxide vitreosol liquid mixed altogether;
(2) adopt the thermal treatment process of dehydration, decarburization, in conjunction with ball grinding technique, realize low hydroxyl concentration, Tm without residual carbon and distributed components
3+or Ho
3+, Al
3+the preparation of the silicon oxide powder mixed altogether;
(3) adopt high-temperature vacuum sintering, obtain bubble-free, low hydroxy radical content, uniform Tm3+ or Ho
3+, Al
3+the silica glass mixed altogether, in glass, OH content is less than 10ppm, rare earth oxide Tm
2o
3doping content reach 5.0wt%; Ho
2o
3doping content reach 2.5wt%, according to Tm
2o
3and Al
2o
3doping, the specific refractory power of plug glass can in 1.448 ~ 1.476 range regulation, according to Ho
2o
3and Al
2o
3doping, the specific refractory power of plug glass in 1.446 ~ 1.459 range regulation, can be conducive to the numerical aperture realized required for optical fiber designs.Can obtain diameter through processing and be more than or equal to 3.0mm, length is more than or equal to the doping rock quartz core rod of 50mm;
(4) the plug glass adopting the present invention to prepare, and quartz glass tube or quartz glass capillary, utilize rod-in-tube technique and Dutch stack process, can prepare that back end loss is little, hydroxy radical content is low, fiber core refractive index is evenly distributed mixes Tm or Ho double clad or photonic crystal silica fibre, the core refractive index fluctuation of doubly clad optical fiber is less than 5 × 10
-4, also can prepare the laser fiber of other structure.
Accompanying drawing explanation
Fig. 1 is the Tm prepared by the embodiment of the present invention 2
3+, Al
3+mix the refractive index profile of clad silica fiber altogether.
Fig. 2 is the Tm prepared by the embodiment of the present invention 2
3+, Al
3+mix the absorption loss spectrum of clad silica fiber altogether.
Fig. 3 is the Tm prepared by inventive embodiments 3
3+, Al
3+the laser spectrum of co-doped double-clad silica fibre.
Fig. 4 is the Tm prepared by the embodiment of the present invention 3
3+, Al
3+the laser input-output curve of co-doped double-clad silica fibre.
Fig. 5 is the Ho prepared by the embodiment of the present invention 5
3+, Al
3+the laser input-output curve of co-doped double-clad silica fibre.
Fig. 6 is the Ho prepared by the embodiment of the present invention 5
3+, Al
3+mix the absorption loss spectrum of clad silica fiber altogether.
Embodiment
Below in conjunction with drawings and Examples to comprise with regard to 2 μm of quartz optical fibre core glass mix Tm or Ho quartz optical fibre core method for glass preparation, plug glass preparation doubly clad optical fiber, the present invention will be further described for optical fiber property, but should not limit the scope of the invention with this.
Embodiment 1:
Described plug glass formula: 0.1Tm
2o
3-1.5Al
2o
3-98.4SiO
2(mol%).The preparation method of this plug glass is: under room temperature and magnetic agitation effect, according to Si (OCH
3)
4: C
2h
5oH:H
2the mol ratio of O=1:4:2 take ammoniacal liquor as catalyzer, preparation vitreosol liquid, regulator solution pH=8.Then according to the plug glass formula of design, AlCl is added
36H
2o and TmCl
36H
2o.Stirred at ambient temperature forms transparent doping colloidal sol for 24 hours, leaves standstill to gelation in encloses container; This gel is placed in tube furnace insulation 12 hours removing residual carbons and hydroxyl under the condition of oxygen atmosphere and 600 DEG C, obtains Tm
3+, Al
3+the silicon oxide powder mixed altogether; Adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 150 object polytetrafluoros; It is 10 that the powder that will sieve is placed in vacuum tightness
-3in 1800 DEG C of melting 8h under the High Temperature Furnaces Heating Apparatus of Pa, furnace cooling forms bubble-free transparent glass.This doped silica glass is 1.448 in 1552nm place specific refractory power, and density is 2.22g/cm3; Described bubble-free transparent glass is processed as diameter 3.2mm, the plug of long 50mm, optical polish, be placed in mass concentration 5% HF acid carry out acid treatment 15min after, take out dry, obtain and mix Tm
3+prefabricated quartz fiber rod core.
Embodiment 2:
Described plug glass formula: 0.1Tm
2o
3-1.5Al
2o
3-98.4SiO
2(mol%).Under room temperature and magnetic agitation effect, according to Si (OC
2h
5)
4: C
2h
5oH:H
2the mol ratio of O=1:4:2 take hydrochloric acid as catalyzer, preparation vitreosol liquid, regulator solution pH=1.Then according to the plug glass formula of design, AlCl is added
36H
2o and TmCl
36H
2o, stirred at ambient temperature forms doping colloidal sol for 12 hours, leaves standstill to gelation in encloses container; This gel is placed in tube furnace insulation 8 hours removing residual carbons and hydroxyl under the condition of oxygen atmosphere and 1000 DEG C, obtains Tm
3+, Al
3+the silicon oxide powder mixed altogether; Adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 150 object polytetrafluoros; It is 10 that the powder that will sieve is placed in vacuum tightness
-1in 1600 DEG C of melting 8h under the High Temperature Furnaces Heating Apparatus of Pa, furnace cooling forms bubble-free transparent glass.This doped silica glass is 1.447 in 1552nm place specific refractory power, and density is 2.21g/cm3; Described bubble-free transparent glass is processed as diameter 3.2mm, the plug of long 50mm, optical polish, be placed in mass concentration 10% HF acid carry out acid treatment 8min after, take out dry, obtain and mix Tm
3+prefabricated quartz fiber rod core.
Adopt conventional rod-in-tube technique to prepare prefabricated rods afterwards, draw Tm at 1800 DEG C
3+, Al
3+single clad silica fiber of doping, adopts index distribution tester (S14 Refractive Index Profiler, Photon Kinetics) to test its index distribution, the results are shown in Figure 2.Core segment refractive index fluctuation is less than 5 × 10
-4, show the optical homogeneity that this optical fiber has had.
Embodiment 3:
Described plug glass formula: 0.3Tm
2o
3-4.5Al
2o
3-95.2SiO
2(mol%).Under room temperature and magnetic agitation effect, according to Si (OC
2h
5)
4: C
2h
5oH:H
2the mol ratio of O=1:20:10 take hydrochloric acid as catalyzer, preparation vitreosol liquid, regulator solution pH=3.Then according to the plug glass formula of design, AlCl is added
36H
2o and TmCl
36H
2o, stirred at ambient temperature forms doping colloidal sol for 10 hours, leaves standstill to gelation in encloses container; This gel is placed in tube furnace insulation 8 hours removing residual carbons and hydroxyl under the condition of oxygen atmosphere and 800 DEG C, obtains Tm
3+, Al
3+the silicon oxide powder mixed altogether; Adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 150 object polytetrafluoros; It is 10 that the powder that will sieve is placed in vacuum tightness
-3in 1750 DEG C of melting 5h under the High Temperature Furnaces Heating Apparatus of Pa, furnace cooling forms bubble-free transparent glass.This doped silica glass is 1.454 in 1552nm place specific refractory power, and density is 2.25g/cm3; Described bubble-free transparent glass is processed as diameter 3.2mm, the plug of long 50mm, optical polish, be placed in mass concentration 20% HF acid carry out acid treatment 5min after, take out dry, obtain and mix Tm
3+prefabricated quartz fiber rod core.
Embodiment 4:
Described plug glass formula: 0.8Tm
2o
3-8Al
2o
3-91.2SiO
2(mol%).Under room temperature and magnetic agitation effect, according to Si (OCH
3)
4: CH
3oH:H
2the mol ratio of O=1:20:10, preparation transparent liquid.Then according to the plug glass formula of design, AlCl is added
36H
2o and TmCl
36H
2o take ammoniacal liquor as catalyzer, preparation vitreosol liquid, regulator solution pH=10.Stirred at ambient temperature forms doping colloidal sol for 1 hour, leaves standstill to gelation in encloses container; This gel is placed in tube furnace insulation 5 hours removing residual carbons and hydroxyl under the condition of oxygen atmosphere and 1000 DEG C, obtains Tm
3+, Al
3+the silicon oxide powder mixed altogether; Adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 150 object polytetrafluoros; It is 10 that the powder that will sieve is placed in vacuum tightness
-2in 1700 DEG C of melting 5h under the High Temperature Furnaces Heating Apparatus of Pa, furnace cooling forms bubble-free transparent glass.This doped silica glass is 1.476 in 1552nm place specific refractory power, and density is 2.39g/cm3; Described bubble-free transparent glass is processed as diameter 3.2mm, the plug of long 50mm, optical polish, be placed in mass concentration 5% HF acid carry out acid treatment 10min after, take out dry, obtain and mix Tm
3+prefabricated quartz fiber rod core.
Embodiment 5:
Described plug glass formula: 0.08Ho
2o
3-1.6Al
2o
3-98.32SiO
2(mol%).Under room temperature and magnetic agitation effect, according to Si (OC
2h
5)
4: C
2h
5oH:H
2the mol ratio of O=1:4:2 take hydrochloric acid as catalyzer, preparation vitreosol liquid, regulator solution pH=1.Then according to the plug glass formula of design, AlCl is added
36H
2o and HoCl
36H
2o, stirred at ambient temperature forms doping colloidal sol for 24 hours, leaves standstill to gelation in encloses container; This gel is placed in tube furnace insulation 8 hours removing residual carbons and hydroxyl under the condition of oxygen atmosphere and 600 DEG C, obtains Ho
3+, Al
3+the silicon oxide powder mixed altogether; Adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 150 object polytetrafluoros; It is 10 that the powder that will sieve is placed in vacuum tightness
-2in 2000 DEG C of melting 1h under the High Temperature Furnaces Heating Apparatus of Pa, furnace cooling forms bubble-free transparent glass.This doped silica glass is 1.446 in 1552nm place specific refractory power, and density is 2.22g/cm3; Described bubble-free transparent glass is processed as diameter 3.0mm, the plug of long 50mm, optical polish, be placed in mass concentration 15% HF acid carry out acid treatment 5min after, take out dry, obtain and mix Ho3+ prefabricated quartz fiber rod core.
Embodiment 6:
Described plug glass formula: 0.4Ho
2o
3-6.0Al
2o
3-93.6SiO
2(mol%).Under room temperature and magnetic agitation effect, according to Si (OC
2h
5)
4: C
2h
5oH:H
2the mol ratio of O=1:5:8 take hydrochloric acid as catalyzer, preparation vitreosol liquid, regulator solution pH=3.Then according to the plug glass formula of design, AlCl is added
36H
2o and HoCl
36H
2o, stirred at ambient temperature forms doping colloidal sol for 12 hours, leaves standstill to gelation in encloses container; This gel is placed in tube furnace insulation 10 hours removing residual carbons and hydroxyl under the condition of oxygen atmosphere and 800 DEG C, obtains Ho
3+, Al
3+the silicon oxide powder mixed altogether; Adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 150 object polytetrafluoros; It is 10 that the powder that will sieve is placed in vacuum tightness
-1in 1750 DEG C of melting 3h under the High Temperature Furnaces Heating Apparatus of Pa, furnace cooling forms bubble-free transparent glass.This doped silica glass is 1.459 in 1552nm place specific refractory power, and density is 2.30g/cm3; Described bubble-free transparent glass is processed as diameter 3.0mm, the plug of long 50mm, optical polish, be placed in mass concentration 10% HF acid carry out acid treatment 8min after, take out dry, obtain and mix Ho
3+prefabricated quartz fiber rod core.
Application examples 1: mix Tm quartz doubly clad optical fiber
The plug glass of plug embodiment 2 is inserted in quartz socket tube, is prepared into a single covering prefabricated rods; By this prefabricated rods 1800 DEG C of high temperature wire drawings, adopt specific refractory power be 1.37 organic gel it is applied.Prepare double clad and mix Tm quartz glass optical fibre.Adopt the wideband light source of NKT company, the fiber spectrometer of Yokogawa company and conventional intercept method, test this optical fiber and compose in the absorption loss of 850-1450nm scope, see Fig. 3.The loss of 1333nm back end is 1.1dB/m, 1385nm hydroxyl group absorption loss is 2.0dB/m, shows that Tm optical fiber of mixing prepared by the method has lower hydroxy radical content.The plug glass of plug embodiment 3 is obtained pure silica tube as inner cladding according to identical method above, fibre core diameter 45um, inner cladding diameter is 450um, and inner cladding is that octagonal double clad mixes Tm quartz glass optical fibre.Fig. 4 is the laser spectrum of this optical fiber, and illustration is inner cladding is octagonal fiber cross-sections figure.793nmLD is adopted to carry out Laser Experiments to this optical fiber.Testing laser result is as Fig. 5, and its slope efficiency is 12.2%, when pump laser power is limited, obtains the Laser output of the highest 2.4W.
Application examples 2: mix Ho quartz doubly clad optical fiber
The plug glass of plug embodiment 5 is inserted in quartz socket tube, is prepared into a single covering prefabricated rods; By this prefabricated rods 1800 DEG C of high temperature wire drawings, and adopt specific refractory power be 1.37 organic gel it is applied.Prepare double clad and mix Ho quartz glass optical fibre.Employing output wavelength is that the thulium optical fiber laser of 1.9um carries out Laser Experiments to this pumped fiber, and testing laser result is as Fig. 6.Its slope efficiency reaches 48.46%, when pump laser power is limited, obtains the Laser output of the highest 320mW.Adopt the wideband light source of NKT company, the fiber spectrometer of Yokogawa company and conventional intercept method, test this optical fiber and compose in the absorption loss of 900-1650nm scope.1383nm hydroxyl group absorption loss is 2.5dB/m, shows that Ho optical fiber of mixing prepared by the method has lower hydroxy radical content.
Claims (5)
1. 2 μm of quartz optical fibre core glass, comprise and mix thulium or mix holmium quartz optical fibre core glass, it is characterized in that, the molar percentage compositing range of this plug glass is as follows:
Thulium-doped silica fib plug glass:
SiO
2： 91～98.4mol％
Tm
2O
3： 0.1～0.8mol％
Al
2O
3： 1.5～8mol％
Mix holmium quartz optical fibre core glass:
SiO
2： 93.6～98.32mol％
Ho
2O
3： 0.08～0.4mol％
Al
2O
3： 1.6～6mol％。
2. the preparation method of 2 μm of quartz optical fibre core glass according to claim 1, it is characterized in that, the method comprises the following steps:
1. the selected molar percentage mixed thulium or mix holmium quartz optical fibre core glass composition, by selected molar percentage weighing raw materials silicon alkoxide, six hydrous thulium chlorides or six chloride hydrate holmiums, Aluminium chloride hexahydrate, wherein silicon alkoxide introduces SiO
2, six hydrous thulium chlorides introduce Tm
2o
3or six chloride hydrate holmiums introduce Ho
2o
3, Aluminium chloride hexahydrate introduces Al
2o
3;
2. silicon alkoxide is pressed: water: the proportions water of organic solvent=1:2 ~ 10:4 ~ 20 and the mixing solutions of organic solvent, then six described hydrous thulium chlorides or six chloride hydrate holmiums, Aluminium chloride hexahydrate are added in this mixing solutions successively, add the hydrolysis of catalyst silicon alkoxide, at room temperature fully stirred through 1 ~ 24 hour, obtain Tm
3+or Ho
3+, Al
3+the silicon oxide vitreosol liquid mixed altogether, leaves standstill 1 ~ 10 day to its gelation;
3. described silica gel is placed in tube furnace, under oxygen atmosphere, under the condition of 600 ~ 1000 DEG C, insulation 5 ~ 12 hours removing residual carbons and hydroxyl, form Tm
3+or Ho
3+, Al
3+the silicon oxide powder mixed altogether;
4. adopt ball-grinding machine to carry out ball milling to described silicon oxide powder, filter out the powder of particle diameter below 100 microns by 140 ~ 160 object polytetrafluoros;
5. described powder is placed in corundum crucible, at the High Temperature Furnaces Heating Apparatus 10 of 1600 ~ 2000 DEG C
-1~ 10
-3carry out melting in 1 ~ 8 hour under Pa vacuum tightness, furnace cooling forms bubble-free transparent glass;
6. described bubble-free transparent glass is processed as diameter and is more than or equal to 3.0mm, length carries out optical polish after being more than or equal to the plug of 50mm, is then placed in mass concentration after the HF acid acid treatment 5 ~ 15min of 5 ~ 20%, takes out dry, obtains and mix Tm
3+or Ho
3+prefabricated quartz fiber rod core.
3. the preparation method of 2 μm of quartz optical fibre core glass according to claim 2, is characterized in that, described silicon alkoxide is Si (OC
2h
5)
4or Si (OCH
3)
4.
4. the preparation method of 2 μm of quartz optical fibre core glass according to claim 2, is characterized in that, described step 2. middle organic solvent is C
2h
5oH or CH
3oH.
5. the preparation method of 2 μm of quartz optical fibre core glass according to claim 2, is characterized in that, described step 2. middle silicon alkoxide hydrolyst is hydrochloric acid or ammoniacal liquor, and when adopting hydrochloric acid catalysis, the hydrochloric acid content added makes solution ph be 1 ~ 3; When adopting ammonia-catalyzed, the ammonia vol added makes solution ph be 8 ~ 10.
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| CN104932054A (en) * | 2015-07-20 | 2015-09-23 | 富通集团有限公司 | Three-wrapping-layer thulium-doped optical fiber and preparation method thereof |
| CN112851127A (en) * | 2021-01-16 | 2021-05-28 | 威海长和光导科技有限公司 | High-gain Ho3+/Tm3+/Yb3+Co-doped quartz optical fiber and preparation method thereof |
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| 王欣等: "Tm3+掺杂Bi2O3-SiO2-PbO玻璃的~2μm发光光谱性质", 《无机材料学报》 * |
Cited By (4)
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| CN104932054A (en) * | 2015-07-20 | 2015-09-23 | 富通集团有限公司 | Three-wrapping-layer thulium-doped optical fiber and preparation method thereof |
| CN104932054B (en) * | 2015-07-20 | 2018-02-23 | 富通集团有限公司 | A kind of triple clad thulium doped fiber and preparation method thereof |
| CN112851127A (en) * | 2021-01-16 | 2021-05-28 | 威海长和光导科技有限公司 | High-gain Ho3+/Tm3+/Yb3+Co-doped quartz optical fiber and preparation method thereof |
| CN112851127B (en) * | 2021-01-16 | 2021-11-02 | 威海长和光导科技有限公司 | High-gain Ho3+/Tm3+/Yb3+Co-doped quartz optical fiber and preparation method thereof |
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