CN102023318B - Composition of silicate optical fiber with super large mode area and preparation method thereof - Google Patents
Composition of silicate optical fiber with super large mode area and preparation method thereof Download PDFInfo
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- CN102023318B CN102023318B CN 200910023895 CN200910023895A CN102023318B CN 102023318 B CN102023318 B CN 102023318B CN 200910023895 CN200910023895 CN 200910023895 CN 200910023895 A CN200910023895 A CN 200910023895A CN 102023318 B CN102023318 B CN 102023318B
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- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000013307 optical fiber Substances 0.000 title abstract description 37
- 239000000203 mixture Substances 0.000 title abstract description 5
- 239000000835 fiber Substances 0.000 claims abstract description 96
- 239000011521 glass Substances 0.000 claims abstract description 33
- 238000005253 cladding Methods 0.000 claims abstract description 27
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052810 boron oxide Inorganic materials 0.000 claims abstract description 11
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 33
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 30
- 238000000137 annealing Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000005491 wire drawing Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 14
- 241001397173 Kali <angiosperm> Species 0.000 claims description 10
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(iii) oxide Chemical compound O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 10
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 10
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 9
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims description 9
- 229940075624 ytterbium oxide Drugs 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 5
- 238000005352 clarification Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 5
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 abstract description 7
- 229910000464 lead oxide Inorganic materials 0.000 abstract 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 abstract 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 abstract 1
- 229910001950 potassium oxide Inorganic materials 0.000 abstract 1
- 229910052814 silicon oxide Inorganic materials 0.000 abstract 1
- 239000011162 core material Substances 0.000 description 55
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 8
- 230000003287 optical effect Effects 0.000 description 5
- -1 rare earth ion Chemical class 0.000 description 4
- 239000005368 silicate glass Substances 0.000 description 3
- 150000004760 silicates Chemical class 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 239000004038 photonic crystal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
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Abstract
The invention provides a composition of a silicate optical fiber with an ultra-large mode area and a preparation method thereof. The fiber comprises a fiber core part and a fiber cladding part, wherein the formula comprises silicon oxide, boron oxide, aluminum oxide, lead oxide, potassium oxide, lanthanum oxide, yttrium oxide and rare earth oxide, the structure of the fiber is gain guide-refractive index reverse guide, the diameter of the fiber core of the gain guide-refractive index reverse guide fiber is far larger than that of the fiber core (4-10 mu m) of a common single mode fiber, and the area of a mode field can reach tens of thousands of square microns. The core diameter is within the range of 100-500 um; the cladding consists of multi-component glass, and the diameter of the cladding is about 250-650 um; the refractive index difference delta n between the fiber core and the cladding is less than 0.05-0.28%, and the problems of more than 100 mu m of mode field diameter and single-mode transmission characteristic are solved.
Description
Technical field
The invention belongs to optical material and laser technology field, be specifically related to composition of the long-pending silicate fibers of a kind of super large die face and preparation method thereof.
Background technology
High-power fiber amplifier and laser instrument are widely used in fields such as Laser Processings.Under high-power pumping, when the optical fiber core diameter hour, fibre core and fiber end face easily produce calamitous optical damage; And when the optical fiber core diameter was larger, optical fiber can produce serious nonlinear effect due to stimulated Raman scattering and stimulated Brillouin scattering, thereby affects the beam quality of Laser output.
Adopt optical fiber and restraint technology or large mould field optical fiber, the restriction that can avoid above-mentioned factor to cause in theory, but the core diameter maximum of the large mould of the step change type field optical fiber of the single-mode laser of having realized at present output is only 40 μ m, and the maximum core diameter of photonic crystal fiber is 100 μ m, greater than 100 μ m, near field diffraction pattern can have a strong impact on the beam quality of laser instrument when core diameter.
In addition, optical fiber and the technology of restrainting do not make a breakthrough yet.Therefore, a kind of super large die face of exploitation is long-pending, the single-mode laser output optical fibre is significant.
In conventional art, realize that large mould field optical fiber mainly adopts methods such as reducing numerical aperture and design Refractive Index Profile o.Reduce that numerical aperture will cause that the leaded light effect dies down, loss increases; The design Refractive Index Profile o may be brought the multimode oscillation problem; These two kinds of methods are all to obtain big mode field area by the design optical fiber structure, and the mode field area that can realize at present only has the hundreds of square micron.Therefore, more than realizing mode field diameter 100 μ m, and satisfy simultaneously the single mode transport characteristic, the optical fiber structure of design is difficult to realize traditionally.
Siegman had proposed a kind of new ideas optical fiber in 2003, and is namely gain guided---refractive index inverse-guiding type optical fiber (gain-guided, index-antiguided, GG+IAG).The fiber core refractive index of this optical fiber is less than cladding index (Δ n＜0), and the fiber core refractive index of general single mode fiber is greater than cladding index.
Therefore, at GG+IAG fiber core and covering at the interface, light can not transmit according to total internal reflection principle.In GG+IAG optical fiber, the wide part of fibre core transmission leaks in covering, and the gain media in fibre core is with optical signal amplification, with the compensation leakage loss simultaneously.
Abroad developed in 2006 and mixed Nd
3+Phosphate GG+IAG optical fiber, and realized the single-mode laser output of profile pump and end pumping in 2007, its core diameter is 100 μ m～400 μ m.
Summary of the invention
The invention provides composition of the long-pending silicate fibers of a kind of super large die face and preparation method thereof, mainly solved the problem that optical fiber of the prior art can't satisfy the above and single mode transport characteristic of mode field diameter 100 μ m simultaneously.
Technical solution of the present invention is as follows:
The fibre core of this silicate fibers, its formula contains by mole% meter:
Monox 48～60
Boron oxide 1～6
Aluminium oxide 1～4
Massicot 21～28
Kali 15～25
Lanthana 0～5
Yttria 0～5
Rare earth oxide 0.1～1
The above-mentioned more suitable formula of the present invention contains by mole% meter:
Monox 50～58.5
Boron oxide 1.2～5.5
Aluminium oxide 1.3～3.9
Massicot 22～27.8
Kali 15.5～24.5
Lanthana 0.3～4.8
Yttria 0.3～4.5
Rare earth oxide 0.11～1
The above-mentioned better formula of the present invention contains by mole% meter:
Monox 50.8～58
Boron oxide 1.25～5.5
Aluminium oxide 1.35～3.5
Massicot 22.3～27.5
Kali 15.7～24.5
Lanthana 0.35～4.5
Yttria 0.35～4.3
Rare earth oxide 0.12～0.98
The above monox, aluminium oxide, massicot are introduced with oxide form, and boron oxide is introduced with boric acid, and kali is introduced with potassium nitrate, and each oxide or compound purity are all greater than 99.6%; Lanthana, yttria purity are greater than 99.99%, and described rare earth oxide is the arbitrary replacement of ytterbium oxide, erbium oxide, neodymia or thulium oxide, and take ytterbium oxide as good, purity is greater than 99.99%.
The covering formula of this silicate fibers contains by mole% meter:
Monox 51～58
Boron oxide 2～8
Aluminium oxide 2～7
Massicot 21～28
Kali 14～20
Lanthana 0～5
Yttria 0～5
Above-mentioned better formula contains by mole% meter:
Monox 52.5～57.2
Boron oxide 2.2～6.8
Aluminium oxide 2.2～5.4
Massicot 22.5～27.8
Kali 14.5～19.6
Lanthana 0.3～4.8
Yttria 0.3～4.8
The method of the long-pending silicate fibers preparation of this super large die face comprises the following steps:
(1) preparation fibre core prefabricated rods
Successively add in silica crucible after raw material is mixed and heat, heating-up temperature is 900～980 ℃, be 1.0～1.5h heat time heating time, and then molten mass is poured in the Pt crucible heated, heating-up temperature is 1100～1150 ℃, be 2.5～3.5h heat time heating time, obtains the glass metal of high temperature homogenizing through stirring, clarification, homogenizing; After temperature is reduced to 890 ℃, the glass metal of high temperature homogenizing is cast in mould, carries out fine annealing after casting complete and process, annealing temperature is 450 ℃, after completing, annealing is cooled to room temperature with 1.5～2 ℃/min again, the treated silicate fibers fibre core prefabricated rods that obtains;
(2) preparation covering prefabricated rods
Determine the raw material of covering prefabricated rods according to the selected raw material of preparation fibre core prefabricated rods, after raw material is mixed, according to the preparation method of step (1) preparation fibre core prefabricated rods, preparation covering prefabricated rods;
(3) synthetic fibre-optical
To be socketed fibre core prefabricated rods and covering prefabricated rods, fusion, surface working and wire drawing process, and obtains silicate fibers.
During the wire drawing of the above step (3) synthetic fibre-optical was processed, wire-drawing temperature was 780～820 ℃, and charging rate is 1～2mm/min, and drawing speed is 5～10cm/min.
During the above step (1) preparation gain core prefabricated rods, heating is first to put into silica crucible to be heated by Elema, and heating-up temperature is 900～980 ℃, and be 1.0～1.5h heat time heating time; After put into the Pt crucible and heated by Elema, heating-up temperature is 1100～1150 ℃, be 2.5～3.5h heat time heating time.
The invention has the advantages that:
1, the structure of silicate fibers provided by the invention is gain guided-refractive index inverse-guiding, and gain guided and refractive index inverse-guiding fibre core diameter is much larger than the core diameter (4～10 μ m) of general single mode fiber, and mode field area can reach square microns up to ten thousand.
2, the core material of silicate fibers provided by the invention forms by having the active rare earth ion of gain, and core diameter is in 100～500um scope; Covering is comprised of multicomponent glass, and cladding diameter is 250～650um approximately; Refractive indices n＜0.05%～0.28% between fibre core-covering.
3, silicate fibers provided by the invention has good thermal property, optical property, mechanical property and mechanical property, is expected to be applied in high-capacity optical fiber laser.
4, contain gain media in the fibre core of silicate fibers provided by the invention, so when the fibre core gain coefficient is enough large, but the just tunnelling ray transmission of partial-compensation from the sandwich layer to the covering of the fibre core of GG+IAG optical fiber gain, part is used for realizing LP
01Mode oscillation.
Description of drawings
Fig. 1 light gain guided transmitting procedure in refractive index inverse-guiding optical fiber;
Fig. 2 is big core diameter single-mode fiber end face of the present invention;
Fig. 3 is the large mould field single-mode fiber Laser output quality that the present invention relates to.
Embodiment
The present invention
Table 1-1: glass of fiber core forms: (by mole% meter)
Table 1-2: cladding glass forms: (by mole% meter)
According to the silicate fibers of group 1～group 12 preparations, have a very high technology stability, super large die face long-pending, and be single-mode fiber, suitable large-scale production.
Add the purpose of PbO to be to improve glass structure in formula, improve the glass light spectral property; Add K
2The purpose of O is to reduce glass viscosity, makes glass be easy to melting.
Because containing gain media (being gain guided optical fiber), flashlight can be amplified fibre core, thus the loss that compensating light leaks.When the gain coefficient of fibre core was enough large, part energy can compensate the tunnelling ray transmission from the fibre core to the covering, and another part energy can be in order to realize LP
01The mould transmission, this moment, the gain coefficient of GG+IAG optical fiber did not reach LP
11The laser generation threshold value of mould, thus realized single-mode laser output.
The optical fiber that formula by this silicate fibers and preparation method thereof is prepared, structure is gain guided-refractive index inverse-guiding (GG+IAG), be that the fiber core refractive index of optical fiber is less than cladding index Δ n＜0 (refractive index inverse-guiding optical fiber), therefore, the transmission of light between fibre core and covering interface is not to adopt total internal reflection principle.In GG+IAG optical fiber, except having a small amount of glancing light, the wide part of fibre core transmission leaks in covering, as shown in Figure 1; Fig. 2 is big core diameter single-mode fiber end face of the present invention, and the large mould field single-mode fiber Laser output quality that the present invention relates to as shown in Figure 3.
Because this optical fiber has good thermal property, optical property and mechanical property, be expected to be applied to the high energy fiber laser and amplifier, and the key areas such as information industry.
Embodiment 1:
According to the design feature of GG+IAG optical fiber, get the table 1-1 with the table 1-2 in the 1st assembly side process.
In raw material, monox, aluminium oxide, massicot are introduced with oxide form, and boron oxide is introduced with boric acid, and kali is introduced with potassium nitrate, and each oxide or compound purity are all greater than 99.6%; Lanthana, yttria purity are greater than 99.99%, and described rare earth oxide is the arbitrary replacement of ytterbium oxide, erbium oxide, neodymia or thulium oxide, and take ytterbium oxide as good, purity is greater than 99.99%.Adopt high-temperature fusion technique to prepare the Yb3+ doped silicate glasses.
Successively add in silica crucible after raw material is mixed and heat, heating-up temperature is 910 ℃, and be 1.0h heat time heating time, and then molten mass is poured in the Pt crucible heated, heating-up temperature is 1100 ℃, and be 2.5h heat time heating time, obtains the glass metal of high temperature homogenizing through stirring, clarification, homogenizing; After temperature is reduced to 890 ℃, the glass metal of high temperature homogenizing is cast in mould, carries out fine annealing after casting complete and process, annealing temperature is 450 ℃, after completing, annealing is cooled to room temperature with 1.5～2 ℃/min again, the treated silicate fibers fibre core prefabricated rods that obtains.
Adjust respective process gain of parameter inner cladding glass and surrounding layer glass on the preparation technology basis of glass of fiber core.
Adopt the rod in tube method drawing optical fiber.At first, adopt mechanical processing method that glass of fiber core rod and inner cladding glass bar, surrounding layer glass bar are processed into the required actual geometric configuration of fiber draw process and physical dimension.
The prefabricated rods that processes is carried out wire drawing on wire drawing machine, wire-drawing temperature is 780 ℃, and charging rate is 1mm/min, and drawing speed is 7.5cm/min.
The fiber core refractive index n1=1.57387 of the big core diameter single-mode optical fiber for preparing according to the method described above, core diameter is 100 μ m; Inner cladding refractive index n2=1.57432, inner cladding diameter are 250 μ m; Cladding refractive index n3 is 1.50613; Fibre core and inner cladding refractive index are poor is Δ n=-0.0045.
Embodiment 2:
According to the design feature of GG+IAG optical fiber, get the table 1-1 with the table 1-2 in the 6th assembly side process.
In raw material, monox, aluminium oxide, massicot are introduced with oxide form, and boron oxide is introduced with boric acid, and kali is introduced with potassium nitrate, and each oxide or compound purity are all greater than 99.6%; Lanthana, yttria purity are greater than 99.99%, and described rare earth oxide is the arbitrary replacement of ytterbium oxide, erbium oxide, neodymia or thulium oxide, and take ytterbium oxide as good, purity is greater than 99.99%.Adopt high-temperature fusion technique to prepare the Yb3+ doped silicate glasses.
Successively add in silica crucible after raw material is mixed and heat, heating-up temperature is 940 ℃, and be 1.5h heat time heating time, and then molten mass is poured in the Pt crucible heated, heating-up temperature is 1100 ℃, and be 2.5h heat time heating time, obtains the glass metal of high temperature homogenizing through stirring, clarification, homogenizing; After temperature is reduced to 890 ℃, the glass metal of high temperature homogenizing is cast in mould, carries out fine annealing after casting complete and process, annealing temperature is 450 ℃, after completing, annealing is cooled to room temperature with 1.5～2 ℃/min again, the treated silicate fibers fibre core prefabricated rods that obtains;
Adjust respective process gain of parameter inner cladding glass and surrounding layer glass on the preparation technology basis of glass of fiber core.
Adopt the rod in tube method drawing optical fiber.At first, adopt mechanical processing method that glass of fiber core rod and inner cladding glass bar, surrounding layer glass bar are processed into the required actual geometric configuration of fiber draw process and physical dimension.
The prefabricated rods that processes is carried out wire drawing on wire drawing machine, wire-drawing temperature is 800 ℃, and charging rate is 1.5mm/min, and drawing speed is 5cm/min.
The fiber core refractive index n of the big core diameter single-mode optical fiber for preparing according to the method described above
1Be 1.57224, core diameter is 300 μ m; Inner cladding refractive index n
2Be 1.57318, the inner cladding diameter is 460 μ m; Cladding refractive index n
3Be 1.50552, the surrounding layer diameter is 520 μ m; Fibre core and inner cladding refractive index are poor is-0.00094.
Embodiment 3:
According to the design feature of GG+IAG optical fiber, get the table 1-1 with the table 1-2 in the 10th assembly side process.
In raw material, monox, aluminium oxide, massicot are introduced with oxide form, and boron oxide is introduced with boric acid, and kali is introduced with potassium nitrate, and each oxide or compound purity are all greater than 99.6%; Lanthana, yttria purity are greater than 99.99%, and described rare earth oxide is the arbitrary replacement of ytterbium oxide, erbium oxide, neodymia or thulium oxide, and take ytterbium oxide as good, purity is greater than 99.99%.Adopt high-temperature fusion technique to prepare the Yb3+ doped silicate glasses.
Successively add in silica crucible after raw material is mixed and heat, heating-up temperature is 960 ℃, and be 1.5h heat time heating time, and then molten mass is poured in the Pt crucible heated, heating-up temperature is 1100 ℃, and be 3.5h heat time heating time, obtains the glass metal of high temperature homogenizing through stirring, clarification, homogenizing; After temperature is reduced to 890 ℃, the glass metal of high temperature homogenizing is cast in mould, carries out fine annealing after casting complete and process, annealing temperature is 450 ℃, after completing, annealing is cooled to room temperature with 1.5～2 ℃/min again, the treated silicate fibers fibre core prefabricated rods that obtains.
Adjust respective process gain of parameter inner cladding glass and surrounding layer glass on the preparation technology basis of glass of fiber core.
The prefabricated rods that processes is carried out wire drawing on wire drawing machine, wire-drawing temperature is 810 ℃, and charging rate is 1.5mm/min, and drawing speed is 6cm/min.
The fiber core refractive index n of the big core diameter single-mode stripping pattern optical fiber for preparing according to the method described above
1Be 1.57286, core diameter is 200 μ m; Inner cladding refractive index n
2Be 1.57402, the inner cladding diameter is 320 μ m; Cladding refractive index n
3Be 1.50564, the surrounding layer diameter is 340 μ m; Fibre core and inner cladding refractive index are poor is-0.00116.
Claims (7)
1. the long-pending silicate fibers of super large die face, comprise fibre core and covering, and it is characterized in that: the formula of described fibre core contains by mole% meter:
The formula of described covering contains by mole% meter:
Described rare earth oxide is the arbitrary replacement of ytterbium oxide, erbium oxide, neodymia or thulium oxide; Described core diameter is 100 ~ 500 μ m, and cladding diameter is 250 ~ 650 μ m.
2. the long-pending silicate fibers of super large die face according to claim 1, is characterized in that, the formula of described fibre core contains by mole% meter:
3. the long-pending silicate fibers of super large die face according to claim 1, is characterized in that, the formula of described fibre core contains by mole% meter:
4. the long-pending silicate fibers of arbitrary described super large die face of according to claim 1 to 3, it is characterized in that: in described fibre core, monox, aluminium oxide, massicot are introduced with oxide form, boron oxide is introduced with boric acid, and kali is introduced with potassium nitrate, and each oxide or compound purity are all greater than 99.6%; Lanthana, yttria purity are greater than 99.99%, and the purity of described rare earth oxide is greater than 99.99%.
5. a method for preparing the long-pending silicate fibers of super large die face of formula that any one is put down in writing in claim 1 to 4, is characterized in that, comprises the following steps:
(1) preparation fibre core prefabricated rods
Successively add in silica crucible after raw material is mixed and heat, heating-up temperature is 900 ~ 980 ℃, be 1.0 ~ 1.5h heat time heating time, and then molten mass is poured in the Pt crucible heated, heating-up temperature is 1100 ~ 1150 ℃, be 2.5 ~ 3.5h heat time heating time, obtains the glass metal of high temperature homogenizing through stirring, clarification, homogenizing; After temperature is reduced to 890 ℃, the glass metal of high temperature homogenizing is cast in mould, carries out fine annealing after casting complete and process, annealing temperature is 450 ℃, after completing, annealing is cooled to room temperature with 1.5 ~ 2 ℃/min again, the treated silicate fibers fibre core prefabricated rods that obtains;
(2) preparation covering prefabricated rods
Determine the raw material of covering prefabricated rods according to the selected raw material of preparation fibre core prefabricated rods, after raw material is mixed, according to the preparation method of step (1) preparation fibre core prefabricated rods, preparation covering prefabricated rods;
(3) synthetic fibre-optical
To be socketed fibre core prefabricated rods and covering prefabricated rods, fusion, surface working and wire drawing process, and obtains silicate fibers.
6. the method for preparing silicate fibers according to claim 5 is characterized in that: during the wire drawing of described step (3) synthetic fibre-optical was processed, wire-drawing temperature was 780 ~ 820 ℃, and charging rate is 1 ~ 2mm/min, and drawing speed is 5 ~ 10cm/min.
7. the method for preparing silicate fibers according to claim 6, it is characterized in that: during described step (1) preparation gain core prefabricated rods, first put into silica crucible and heated by Elema, heating-up temperature is 900 ~ 980 ℃, and be 1.0 ~ 1.5h heat time heating time; After put into the Pt crucible and heated by Elema, heating-up temperature is 1100 ~ 1150 ℃, be 2.5 ~ 3.5h heat time heating time.
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| CN103011607A (en) * | 2012-12-27 | 2013-04-03 | 南京邮电大学 | Long-distance micro/nano-core glass optical fiber and preparation method thereof |
| CN103964696B (en) * | 2014-05-26 | 2017-09-15 | 山东海富光子科技股份有限公司 | The full glass of phosphate silicate for high-capacity optical fiber laser mixes optical fiber |
| CN104402236A (en) * | 2014-10-28 | 2015-03-11 | 中国科学院上海光学精密机械研究所 | Lead silicate glass used in double-clad optical fiber, and double-clad optical fiber preparation method |
| CN106772778B (en) * | 2016-12-14 | 2019-04-16 | 中国人民解放军国防科学技术大学 | Thermotropic super large mode field optical fiber |
| CN109061795A (en) * | 2018-09-28 | 2018-12-21 | 镇江微芯光子科技有限公司 | A kind of preparation method of optical fiber |
| CN109164535A (en) * | 2018-09-29 | 2019-01-08 | 镇江微芯光子科技有限公司 | A kind of high-power glass optical fiber |
| CN111170628B (en) * | 2020-01-17 | 2021-04-20 | 中国科学院西安光学精密机械研究所 | Preparation method of tensile optical fiber |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108961A (en) * | 1989-12-29 | 1992-04-28 | Circon Corporation | Etchable core glass compositions and method for manufacturing a high performance microchannel plate |
| CN1457326A (en) * | 2001-02-05 | 2003-11-19 | 皇家菲利浦电子有限公司 | Multicomponent glass, glass fiber, twister and taper |
| CN101405232A (en) * | 2006-03-14 | 2009-04-08 | 肖特公开股份有限公司 | Optical glass as core glass for a fibre-optic light guide and fibre-optic stepped-index fibre with this core glass |
| CN101475309A (en) * | 2007-12-20 | 2009-07-08 | 肖特公开股份有限公司 | Core glass in alkali-zinc-glass system and fibre optic cable |
-
2009
- 2009-09-11 CN CN 200910023895 patent/CN102023318B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5108961A (en) * | 1989-12-29 | 1992-04-28 | Circon Corporation | Etchable core glass compositions and method for manufacturing a high performance microchannel plate |
| CN1457326A (en) * | 2001-02-05 | 2003-11-19 | 皇家菲利浦电子有限公司 | Multicomponent glass, glass fiber, twister and taper |
| CN101405232A (en) * | 2006-03-14 | 2009-04-08 | 肖特公开股份有限公司 | Optical glass as core glass for a fibre-optic light guide and fibre-optic stepped-index fibre with this core glass |
| CN101475309A (en) * | 2007-12-20 | 2009-07-08 | 肖特公开股份有限公司 | Core glass in alkali-zinc-glass system and fibre optic cable |
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