CN103896494A - Glass optical fiber and preparation method thereof - Google Patents
Glass optical fiber and preparation method thereof Download PDFInfo
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- CN103896494A CN103896494A CN201410085300.4A CN201410085300A CN103896494A CN 103896494 A CN103896494 A CN 103896494A CN 201410085300 A CN201410085300 A CN 201410085300A CN 103896494 A CN103896494 A CN 103896494A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
- C03C3/17—Silica-free oxide glass compositions containing phosphorus containing aluminium or beryllium
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/045—Silica-containing oxide glass compositions
- C03C13/046—Multicomponent glass compositions
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a glass optical fiber and a preparation method thereof. The glass optical fiber comprises the following raw materials in parts by weight: 10-20 parts of silicon dioxide, 30-40 parts of calcium oxide, 40-50 parts of alumina, 30-50 parts of potassium oxide, 60-80 parts of sodium peroxide, 50-60 parts of methyl acrylic acid, 20-30 parts of antimonous oxide, 22-28 parts of ammonium dihydrogen phosphate, 50-60 parts of calcium hydrophosphate, 20-60 parts of calcium phosphate, 30-45 parts of monocalcium phosphate, 40-55 parts of potassium dihydrogen phosphate, 20-55 parts of nicotinic acid and 30-40 parts of dioctyl phthalate. The preparation method comprises the following steps of weighing 60-70% of mixed raw materials, placing the mixed raw materials in a platinum crucible for heating, and annealing to obtain a fiber core preform; completely melting the residual raw materials and stirring; drawing the fiber core preform to obtain a glass optical fiber. The glass optical fiber disclosed by the invention has excellent physical properties and mechanical properties.
Description
Technical field
The present invention relates to a kind of optical fiber, relate in particular to a kind of glass optical fiber and preparation method thereof.
Background technology
Glass optical fiber is that silicon-dioxide does, so because and material and the similar glass optical fiber that cries again of character of glass.Up to now, external existing many companies have developed commercial glass optical fiber (mainly comprise erbium-doped tellurite glass fiber, er-doped phosphoric acid salt optical fiber, er-doped bismuthate optical fiber and mix thulium, praseodymium fluoride fiber etc.) and corresponding glass fiber amplifier, and rear-earth-doped glass optical fiber develops rapidly in recent years in WDM transmission system.The spectrum of glass optical fiber is often compared with more smooth in quartz substrate and roomy; Glass optical fiber preparation technology is simple, and cost is low.The component of tellurate glass will directly affect formation ability, thermostability, specific refractory power size, doping concentration of rare earth ion and the Spectrum of Rare Earth Ions characteristic etc. of glass.Thermostability is usually weighed by the difference DELTA T size that the crystallization of glass starts between temperature T x and glass transformation temperature Tg, generally uses differential scanning calorimeter (DSC) or differential thermal analyzer (DTA) to measure.Δ T is larger, represents that glass optical fiber does not produce the can operating temperature range wider of crystallization while drawing, and its thermostability is better, otherwise Δ T difference is less, and thermal stability is poorer, the inner crystallization that easily produces when fibre-optical drawing.Generally speaking, the better heat stability of glass when Δ T>100 ° of C.Mixing Er3+ optical fiber or mixing Tm3+ optical fiber of employing tellurate glass matrix can make signal realize effectively amplification at C+L wave band (1530～1610nm) or S-band (1420～1520nm) broad band region.Some famous fiber optic materials research units are one after another using the er-doped of tellurate matrix or thulium doped fiber as research emphasis in the world.
Application number is the patent of CN200910024128 composition of disclosing the long-pending metaphosphate optical fiber of a kind of super large die face and preparation method thereof, and this metaphosphate optical fiber comprises the fibre core being made up of Vanadium Pentoxide in FLAKES, aluminum oxide, potassium oxide, barium oxide, calcium oxide, magnesium oxide and the rare earth oxide of certain molar percentage and the fibre core covering being made up of Vanadium Pentoxide in FLAKES, aluminum oxide, potassium oxide, barium oxide, calcium oxide and the magnesium oxide of certain molar percentage.By the fibre core prefabricated rods making and covering prefabricated rods be socketed, fusion, surface working and wire drawing processing can obtain this metaphosphate optical fiber.But the performance of this metaphosphate optical fiber is general.
Summary of the invention
The object of this invention is to provide a kind of glass optical fiber and preparation method thereof, specific refractory power is large, and gain guided and refractive index inverse-guiding fibre core diameter, much larger than the core diameter of general single mode fiber, has good optical property.
A kind of glass optical fiber, comprises the raw material of following weight part meter: 0～20 part of silica 1,30～40 parts, calcium oxide, 40～50 parts, aluminum oxide, 30～50 parts of potassium oxides, 60～80 parts of sodium peroxides, 50～60 parts of Methyl methyacrlates, 20～30 parts of antimonous oxides, 22～28 parts of primary ammonium phosphates, 50～60 parts of secondary calcium phosphates, 20～60 parts, calcium phosphate, 30～45 parts of monocalcium phosphates, 40～55 parts of potassium primary phosphates, 20～55 parts, nicotinic acid, 30～40 parts of dioctyl phthalate (DOP)s.
As preferably, 0～18 part of silica 1,30～35 parts, calcium oxide, 40～48 parts, aluminum oxide, 30～48 parts of potassium oxides, 60～70 parts of sodium peroxides, 50～55 parts of Methyl methyacrlates, 20～25 parts of antimonous oxides, 22～27 parts of primary ammonium phosphates, 50～55 parts of secondary calcium phosphates, 20～40 parts, calcium phosphate, 30～40 parts of monocalcium phosphates, 40～50 parts of potassium primary phosphates, 20～30 parts, nicotinic acid, 30～35 parts of dioctyl phthalate (DOP)s.
As preferably, 5 parts of silica 1s, 35 parts, calcium oxide, 45 parts, aluminum oxide, 35 parts of potassium oxides, 70 parts of sodium peroxides, 55 parts of Methyl methyacrlates, 25 parts of antimonous oxides, 27 parts of primary ammonium phosphates, 55 parts of secondary calcium phosphates, 40 parts, calcium phosphate, 40 parts of monocalcium phosphates, 45 parts of potassium primary phosphates, 30 parts, nicotinic acid, 35 parts of dioctyl phthalate (DOP)s.
The preparation method of glass optical fiber, comprises the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 60～70% mixing raw material, put into platinum crucible and heat, Heating temperature is 500～600 DEG C, be 1～2h heat-up time, then stirs with platinum stirrer, and churning time is 100～110 minutes; Be cooled to after 200～300 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 100～150 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 500～600 DEG C, after fusing, stir with platinum stirrer completely, churning time is 100～110 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 60～80 DEG C, be drawn into glass optical fiber.
As preferably, the initial Heating temperature of step (1) is 550～560 DEG C.
As preferably, the temperature of fusion of step (2) is 500～550 DEG C.
Fiber core refractive index n1 of the present invention is 1.539～1.579, inner cladding refractive index n2 is 1.543～1.583, cladding refractive index n3,1.505～1.545, illustrates that glass optical fiber of the present invention has good thermal property, optical property, mechanical property and mechanical property.
Embodiment
Further illustrate the present invention below by specific embodiment.
embodiment 1
A kind of glass optical fiber, comprises the raw material of following weight part meter: 0 part of silica 1,30 parts, calcium oxide, 40 parts, aluminum oxide, 30 parts of potassium oxides, 60 parts of sodium peroxides, 50 parts of Methyl methyacrlates, 20 parts of antimonous oxides, 22 parts of primary ammonium phosphates, 50 parts of secondary calcium phosphates, 20 parts, calcium phosphate, 30 parts of monocalcium phosphates, 40 parts of potassium primary phosphates, 20 parts, nicotinic acid, 30 parts of dioctyl phthalate (DOP)s.
The preparation method of above-mentioned glass optical fiber, comprises the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 60% mixing raw material, put into platinum crucible and heat, Heating temperature is 500 DEG C, and be 1h heat-up time, then stirs with platinum stirrer, and churning time is 100 minutes; Be cooled to after 200 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 100 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 500 DEG C, after fusing, stir with platinum stirrer completely, churning time is 100 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 60 DEG C, be drawn into glass optical fiber.
embodiment 2
A kind of glass optical fiber, comprises the raw material of following weight part meter: 20 parts of silicon-dioxide, 40 parts, calcium oxide, 50 parts, aluminum oxide, 50 parts of potassium oxides, 80 parts of sodium peroxides, 60 parts of Methyl methyacrlates, 30 parts of antimonous oxides, 28 parts of primary ammonium phosphates, 60 parts of secondary calcium phosphates, 60 parts, calcium phosphate, biphosphate Ca45 part, 55 parts of potassium primary phosphates, 55 parts, nicotinic acid, 40 parts of dioctyl phthalate (DOP)s.
The preparation method of above-mentioned glass optical fiber, comprises the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 70% mixing raw material, put into platinum crucible and heat, Heating temperature is 600 DEG C, and be 2h heat-up time, then stirs with platinum stirrer, and churning time is 110 minutes; Be cooled to after 300 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 150 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 600 DEG C, after fusing, stir with platinum stirrer completely, churning time is 110 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 80 DEG C, be drawn into glass optical fiber.
embodiment 3
A kind of glass optical fiber, comprises the raw material of following weight part meter: 5 parts of silica 1s, 35 parts, calcium oxide, 45 parts, aluminum oxide, 35 parts of potassium oxides, 70 parts of sodium peroxides, 55 parts of Methyl methyacrlates, 25 parts of antimonous oxides, 27 parts of primary ammonium phosphates, 55 parts of secondary calcium phosphates, 40 parts, calcium phosphate, 40 parts of monocalcium phosphates, 45 parts of potassium primary phosphates, 30 parts, nicotinic acid, 35 parts of dioctyl phthalate (DOP)s.
The preparation method of above-mentioned glass optical fiber, comprises the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 65% mixing raw material, put into platinum crucible and heat, Heating temperature is 550 DEG C, and be 1.5h heat-up time, then stirs with platinum stirrer, and churning time is 105 minutes; Be cooled to after 250 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 120 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 550 DEG C, after fusing, stir with platinum stirrer completely, churning time is 105 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 70 DEG C, be drawn into glass optical fiber.
embodiment 4
A kind of glass optical fiber, comprises the raw material of following weight part meter: 1 part of silica 1,31 parts, calcium oxide, 41 parts, aluminum oxide, 31 parts of potassium oxides, 61 parts of sodium peroxides, 51 parts of Methyl methyacrlates, 21 parts of antimonous oxides, 24 parts of primary ammonium phosphates, 51 parts of secondary calcium phosphates, 21 parts, calcium phosphate, 31 parts of monocalcium phosphates, 41 parts of potassium primary phosphates, 21 parts, nicotinic acid, 31 parts of dioctyl phthalate (DOP)s.
The preparation method of above-mentioned glass optical fiber, comprises the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 61% mixing raw material, put into platinum crucible and heat, Heating temperature is 510 DEG C, and be 1.1h heat-up time, then stirs with platinum stirrer, and churning time is 101 minutes; Be cooled to after 201 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 101 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 501 DEG C, after fusing, stir with platinum stirrer completely, churning time is 101 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 61 DEG C, be drawn into glass optical fiber.
embodiment 5
A kind of glass optical fiber, comprises the raw material of following weight part meter: 2 parts of silica 1s, 32 parts, calcium oxide, 42 parts, aluminum oxide, 32 parts of potassium oxides, 62 parts of sodium peroxides, 52 parts of Methyl methyacrlates, 22 parts of antimonous oxides, 24 parts of primary ammonium phosphates, 52 parts of secondary calcium phosphates, 22 parts, calcium phosphate, 32 parts of monocalcium phosphates, biphosphate K42 part, 22 parts, nicotinic acid, 32 parts of dioctyl phthalate (DOP)s.
The preparation method of above-mentioned glass optical fiber, comprises the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 62% mixing raw material, put into platinum crucible and heat, Heating temperature is 510 DEG C, and be 1.2h heat-up time, then stirs with platinum stirrer, and churning time is 103 minutes; Be cooled to after 213 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 110 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 510 DEG C, after fusing, stir with platinum stirrer completely, churning time is 103 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 63 DEG C, be drawn into glass optical fiber.
reference examples
Raw material and method are with embodiment 1, different: phosphoric acid ammonium dihydrogen not in raw material.
performance test: the glass optical fiber that embodiment 1～3, reference examples are made carries out performance test.
| ? | Embodiment 1 | Embodiment 2 | Embodiment 3 | Contrast |
| Fiber core refractive index n1 | 1.559 | 1.569 | 1.579 | 1.321 |
| Inner cladding refractive index n2 | 1.553 | 1.573 | 1.583 | 1.231 |
| Cladding refractive index n3 | 1.515 | 1.535 | 1.545 | 1.334 |
Fiber core refractive index n1 of the present invention is 1.559～1.579, inner cladding refractive index n2 is 1.553～1.583, cladding refractive index n3,1.515～1.545, illustrates that glass optical fiber of the present invention has good thermal property, optical property, mechanical property and mechanical property.This is due to the adding of primary ammonium phosphate, and has changed the lattice field intensity of the surrounding of silicon crystal in glass optical fiber, has strengthened the specific refractory power of silicon crystal; And to make its structure be gain guided refractive index inverse-guiding, gain guided and refractive index inverse-guiding fibre core diameter is much larger than the core diameter of general single mode fiber, and mode field area can reach square microns up to ten thousand, has greatly improved mechanics and the optical property of optical fiber.
Claims (6)
1. a glass optical fiber, is characterized in that: the raw material that comprises following weight part meter: 0～20 part of silica 1,30～40 parts, calcium oxide, 40～50 parts, aluminum oxide, 30～50 parts of potassium oxides, 60～80 parts of sodium peroxides, 50～60 parts of Methyl methyacrlates, 20～30 parts of antimonous oxides, 22～28 parts of primary ammonium phosphates, 50～60 parts of secondary calcium phosphates, 20～60 parts, calcium phosphate, 30～45 parts of monocalcium phosphates, 40～55 parts of potassium primary phosphates, 20～55 parts, nicotinic acid, 30～40 parts of dioctyl phthalate (DOP)s.
2. glass optical fiber according to claim 1, is characterized in that: 0～18 part of silica 1,30～35 parts, calcium oxide, 40～48 parts, aluminum oxide, 30～48 parts of potassium oxides, 60～70 parts of sodium peroxides, 50～55 parts of Methyl methyacrlates, 20～25 parts of antimonous oxides, 22～27 parts of primary ammonium phosphates, 50～55 parts of secondary calcium phosphates, 20～40 parts, calcium phosphate, 30～40 parts of monocalcium phosphates, 40～50 parts of potassium primary phosphates, 20～30 parts, nicotinic acid, 30～35 parts of dioctyl phthalate (DOP)s.
3. glass optical fiber according to claim 1, is characterized in that: 5 parts of silica 1s, 35 parts, calcium oxide, 45 parts, aluminum oxide, 35 parts of potassium oxides, 70 parts of sodium peroxides, 55 parts of Methyl methyacrlates, 25 parts of antimonous oxides, 27 parts of primary ammonium phosphates, 55 parts of secondary calcium phosphates, 40 parts, calcium phosphate, 40 parts of monocalcium phosphates, 45 parts of potassium primary phosphates, 30 parts, nicotinic acid, 35 parts of dioctyl phthalate (DOP)s.
4. the preparation method of glass optical fiber claimed in claim 1, is characterized in that: comprise the following steps:
(1) fibre core prefabricated rods preparation: after each raw material is mixed, take 60～70% mixing raw material, put into platinum crucible and heat, Heating temperature is 500～600 DEG C, be 1～2h heat-up time, then stirs with platinum stirrer, and churning time is 100～110 minutes; Be cooled to after 200～300 DEG C, the glass metal of high temperature homogenizing is cast in mould, then carry out anneal, annealing temperature is 100～150 DEG C, is then cooled to room temperature, obtains fibre core prefabricated rods;
(2) prepare covering prefabricated rods: remaining raw material is put into platinum crucible and melt in the globars electric furnace of 500～600 DEG C, after fusing, stir with platinum stirrer completely, churning time is 100～110 minutes;
(3) fibre-optical drawing: described preform is placed on fiber-pulling machine, is cooled to 60～80 DEG C, be drawn into glass optical fiber.
5. the preparation method of glass optical fiber according to claim 4, is characterized in that: the initial Heating temperature of step (1) is 550～560 DEG C.
6. the preparation method of glass optical fiber according to claim 4, is characterized in that: the temperature of fusion of step (2) is 500～550 DEG C.
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| CN201410085300.4A CN103896494A (en) | 2014-03-10 | 2014-03-10 | Glass optical fiber and preparation method thereof |
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| CN201410085300.4A CN103896494A (en) | 2014-03-10 | 2014-03-10 | Glass optical fiber and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108333673A (en) * | 2018-01-04 | 2018-07-27 | 南京邮电大学 | A kind of heterogeneous fragmented packets layer large mould field single mode 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 |
| CN111138082A (en) * | 2020-01-13 | 2020-05-12 | 苏州众为光电有限公司 | High-stability glass optical fiber and preparation method thereof |
| CN112341001A (en) * | 2020-11-17 | 2021-02-09 | 临沂昊泉硅业科技有限公司 | High silica glass fiber, preparation method thereof and fireproof equipment |
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| CN108333673A (en) * | 2018-01-04 | 2018-07-27 | 南京邮电大学 | A kind of heterogeneous fragmented packets layer large mould field single mode optical fiber |
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Application publication date: 20140702 |