CN108947233A - A kind of titanium-doped sapphire amorphous optical fiber and its preparation method and application - Google Patents
A kind of titanium-doped sapphire amorphous optical fiber and its preparation method and application Download PDFInfo
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- CN108947233A CN108947233A CN201810687229.5A CN201810687229A CN108947233A CN 108947233 A CN108947233 A CN 108947233A CN 201810687229 A CN201810687229 A CN 201810687229A CN 108947233 A CN108947233 A CN 108947233A
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- sapphire
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- doped sapphire
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- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 55
- 239000010980 sapphire Substances 0.000 title claims abstract description 55
- 239000013307 optical fiber Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 28
- 239000011162 core material Substances 0.000 claims abstract description 20
- 238000005253 cladding Methods 0.000 claims abstract description 16
- 239000000835 fiber Substances 0.000 claims abstract description 16
- 238000012681 fiber drawing Methods 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 10
- 230000008018 melting Effects 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000011521 glass Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000003780 insertion Methods 0.000 claims abstract description 3
- 230000037431 insertion Effects 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005491 wire drawing Methods 0.000 claims description 8
- 239000010453 quartz Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910052593 corundum Inorganic materials 0.000 claims description 5
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000003754 machining Methods 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 4
- 238000007500 overflow downdraw method Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 7
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 239000010437 gem Substances 0.000 description 11
- 229910001751 gemstone Inorganic materials 0.000 description 11
- FPSFKBGHBCHTOE-UHFFFAOYSA-N sodium 3-hydroxy-4-[(3-methyl-5-oxo-1-phenyl-4H-pyrazol-4-yl)diazenyl]naphthalene-1-sulfonic acid Chemical compound [Na+].O=C1C(N=NC=2C3=CC=CC=C3C(=CC=2O)S(O)(=O)=O)C(C)=NN1C1=CC=CC=C1 FPSFKBGHBCHTOE-UHFFFAOYSA-N 0.000 description 11
- 238000002189 fluorescence spectrum Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 description 2
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/025—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from reheated softened tubes, rods, fibres or filaments, e.g. drawing fibres from preforms
- C03B37/027—Fibres composed of different sorts of glass, e.g. glass optical fibres
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
-
- 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
-
- 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
- C03C13/048—Silica-free oxide glass compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/10—Internal structure or shape details
- C03B2203/22—Radial profile of refractive index, composition or softening point
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/32—Eccentric core or cladding
Abstract
The invention discloses a kind of preparation methods of titanium-doped sapphire amorphous optical fiber, comprising the following steps: (1) ti sapphire crystal is processed into plug；(2) plug is obtained to step (1) to clean；(3) by the plug insertion cladding after cleaning, prefabricated rods are made；The material of the cladding is the glass material that melting temperature is higher than core material；(4) fibre-optical drawing: the prefabricated rods prepared are put into wire-drawer-tower, and heating makes the temperature of fiber drawing furnace rise above the melting temperature of ti sapphire crystal, keep the temperature 15~20min, drawing optical fiber, obtaining fibre core is amorphous titanium-doped sapphire amorphous optical fiber.The invention also discloses above-mentioned optical fiber and its applications.The preparation method simple process of titanium-doped sapphire amorphous optical fiber of the present invention, standby obtained titanium-doped sapphire amorphous optical fiber and ti sapphire crystal have similar luminescence feature.
Description
Technical field
The present invention relates to the preparation of optical fiber, in particular to a kind of titanium-doped sapphire amorphous optical fiber and preparation method thereof and answer
With.
Background technique
Ti sapphire crystal is one of laser medium most important so far, it not only has good heat conductivity
Energy, mechanical performance and higher saturation flux, it is often more important that the tunable wave length range that it is wider than 400nm is existing at present
Any laser medium is incomparable.Using different pumping source and pump mode, people have successfully developed various
Ti sapphire crystal laser, femtosecond laser are exactly an important utilization of sapphire laser.In addition, by frequency multiplication skill
Art, optical parametric oscillation and amplifying technique, people are extended to the output wavelength range of sapphire laser from ultraviolet to red
Outside.There are one important advantages to be that its structure is simple and the operation is stable for sapphire laser simultaneously, therefore, in recent ten years
Ti sapphire crystal solid-state laser is widely studied and applied.
So far, the laser of nearly all ti sapphire crystal preparation is solid-state laser, it is difficult to which realization is mixed
The miniaturization of titanium sapphire laser device, although now can be by the direct pulling monocrystal optical fiber of growth method, this preparation be single
The comparable complexity of the technique of brilliant optical fiber.The miniaturization for how realizing ti sapphire crystal laser is urgently to be resolved at present
Problem.If titanium-doped sapphire optical fiber can be prepared using more mature glass optical fiber drawing technology, for solving above-mentioned ask
Topic and development of new optical fiber laser all have a very important significance.
Summary of the invention
In order to overcome the disadvantages mentioned above and deficiency of the prior art, the purpose of the present invention is to provide a kind of titanium-doped sapphire is non-
The preparation method of brilliant optical fiber, preparation process is simple, and the titanium-doped sapphire amorphous optical fiber being prepared and ti sapphire crystal have
There is similar luminescence feature.
Another object of the present invention is to provide the titanium-doped sapphire amorphous optical fiber that above-mentioned preparation method is prepared.
A further object of the present invention is to provide the applications of above-mentioned titanium-doped sapphire amorphous optical fiber.
The purpose of the present invention is achieved through the following technical solutions:
One kind mixing chrome red jewel amorphous optical fiber, and the chrome red jewel amorphous optical fiber of mixing is core-pack arrangement optical fiber, using crystalline state
Chrome red jewel is mixed as core material, is prepared into fibre core through fibre core fusion method wire drawing and is mixed chrome red jewel amorphous light to be amorphous
It is fine.
The clad material is high purity quartz pipe.
The application for mixing chrome red jewel amorphous optical fiber in optical fiber laser and optical fiber sensing.
A kind of preparation method for mixing chrome red jewel amorphous optical fiber, comprising the following steps:
(1) chrome red gem crystal will be mixed and is processed into plug；
The chrome red gem crystal chemistry of mixing contains by mass percentage:
Cr2O3: 0.01~4%；
Surplus is Al2O3；
(2) plug is obtained to step (1) to clean；
(3) by the plug insertion cladding after cleaning, prefabricated rods are made；The material of the cladding is that wire-drawing temperature is high
In the glass material of core material melting temperature；
(4) fibre-optical drawing:
The prefabricated rods prepared are put into wire-drawer-tower, are heated up, the temperature of fiber drawing furnace is risen above and mixes chrome red jewel crystalline substance
The melting temperature of body, keeps the temperature 15~20min, and drawing optical fiber obtains fibre core to be amorphous and mixes chrome red jewel amorphous optical fiber.
It is described plug is obtained to step (1) to clean, specifically:
It is cleaned up with ultrasonic cleaning, then with deionized water and absolute alcohol.
Step (4) described heating, specifically:
Fiber drawing furnace is set to be raised to wire-drawing temperature with 5~10 DEG C of heating rates per minute.
The temperature for making fiber drawing furnace rises above the melting temperature for mixing chrome red gem crystal, specifically:
The temperature of fiber drawing furnace is set to be raised to 2050~2200 DEG C.
Step (1) described processing, specifically: it is cold worked on machining tool.
Compared with prior art, the present invention has the following advantages and beneficial effects:
The present invention is by using the high purity quartz stick of high melt temperature as covering, and ti sapphire crystal is as fibre core material
Material, successfully draws out amorphous sapphire fiber using fibre core fusion method, and realize in fiber core derived from Ti3+Width
Band shines, and preparation process is simple, proves that the fiber core of preparation is in amorphous state by Raman Characterization, mainly organizing becomes
Al2O3, testing the optical fiber that discovery is drawn by fluorescence spectrum characterization has similar luminescence feature with ti sapphire crystal.This
This optical fiber of preparation is invented in development of new wideband adjustable optical fiber laser and realizes the miniaturization of broadband tunable laser device
Etc. have a very important significance with potential application value, be ti sapphire crystal laser field application propose
A kind of new approach.
Detailed description of the invention
Fig. 1 is the section microphoto of the titanium-doped sapphire amorphous optical fiber of the embodiment of the present invention.
Fig. 2 is the fluorescence spectra of the titanium-doped sapphire amorphous optical fiber of the embodiment of the present invention.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, embodiments of the present invention are not limited thereto.
Embodiment 1
1. the selection of core material: selecting the sapphire crystal mixed with titanium as core material.
The component of ti sapphire crystal, by mass percentage, each component and content are as follows:
TiO2: 0.1%；
Surplus is Al2O3。
2. choosing cladding:
Cladding uses F300 high purity quartz pipe.Internal diameter 3.1mm, outer diameter 25mm, length 200mm, surfaces externally and internally are thrown
Light is in mirror surface.
3. prepared by prefabricated rods:
(1) ti sapphire crystal is cold worked into diameter 3mm on machining tool, is about the microlite stick of 50mm.
(2) the ti sapphire crystal plug and cladding that process are placed in the box for fill water and use ultrasonic cleaning
About 10min, then cleaned 2~3 times with deionized water, finally cleaned up with absolute alcohol.
(3) plug is inserted into cladding, the taper quartz that cladding lower part is polished with the end face of 2.8~3.2mm of diameter
Glass bar stoppers, and prevents plug from falling, and prefabricated rods are made.
4. fibre-optical drawing:
The prefabricated rods prepared are put into wire-drawer-tower, are slowly heated up, the temperature of fiber drawing furnace is made to rise above sapphire crystalline substance
The melting temperature (about 2100 DEG C) of body keeps the temperature 15min.By adjusting the speed and prefabricated rods blanking velocity of wire drawing, draw out not
With the optical fiber of size.
5. pair optical fiber prepared characterizes, Fig. 1 is fiber cross-sections figure manufactured in the present embodiment, can from figure
To apparent core-pack arrangement.
Embodiment 2
1. the selection of core material: selecting the sapphire crystal mixed with titanium as core material.
The component of ti sapphire crystal, by mass percentage, each component and its content are as follows:
TiO2: 0.3%；
Surplus is Al2O3。
2. choosing cladding:
Cladding uses F300 high purity quartz pipe.Internal diameter 3.6mm, outer diameter 25mm, length 200mm, surfaces externally and internally are thrown
Light is in mirror surface.
3. prepared by prefabricated rods:
(1) ti sapphire crystal is cold worked into diameter 3.5mm on machining tool, is about the microlite stick of 50mm.
(2) the ti sapphire crystal plug and cladding that process are placed in the box for fill water and use ultrasonic cleaning
About 10min, then cleaned 2~3 times with deionized water, finally cleaned up with absolute alcohol.
(3) plug is inserted into cladding, the taper quartz that cladding lower part is polished with the end face of 3.4~3.8mm of diameter
Glass bar stoppers, and prevents plug from falling, and prefabricated rods are made.
4. fibre-optical drawing:
The prefabricated rods prepared are put into wire-drawer-tower, are slowly heated up, the temperature of fiber drawing furnace is made to rise above sapphire crystalline substance
The melting temperature (about 2100 DEG C) of body keeps the temperature 20min.By adjusting the speed and prefabricated rods blanking velocity of wire drawing, draw out not
With the optical fiber of size.
5. pair optical fiber prepared characterizes, Fig. 2 is the fluorescence spectrum of optical fiber manufactured in the present embodiment.From Fig. 2
It will be seen that the optical fiber and ti sapphire crystal of preparation have essentially identical fluorescence spectrum, under 532nm laser excitation
There is broad-band illumination within the scope of 600~900nm, which is derived from Ti3+Energy level transition.It can be seen that the optical fiber exists
Novel titanium-doped sapphire tunable laser etc. is prepared to have potential application.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by the embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of titanium-doped sapphire amorphous optical fiber, which is characterized in that the titanium-doped sapphire amorphous optical fiber is core-pack arrangement light
Fibre selects crystalline state titanium-doped sapphire as core material, is prepared into fibre core by fibre core fusion method wire drawing and mixes titanium to be amorphous
Sapphire fiber.
2. titanium-doped sapphire amorphous optical fiber according to claim 1, which is characterized in that the clad material is high purity quartz
Pipe.
3. the answering in terms of tunable optical fiber laser and laser miniaturization of titanium-doped sapphire amorphous optical fiber described in claim 1
With.
4. a kind of preparation method of titanium-doped sapphire amorphous optical fiber, which comprises the following steps:
(1) ti sapphire crystal is processed into plug；
The chemistry of ti sapphire crystal contains by mass percentage:
TiO2: 0.01~3%；
Surplus is Al2O3；
(2) plug is obtained to step (1) to clean；
(3) by the plug insertion cladding after cleaning, prefabricated rods are made；The material of the cladding is that wire-drawing temperature is higher than fibre
The glass material of core material melting temperature；
(4) fibre-optical drawing:
The prefabricated rods prepared are put into wire-drawer-tower, heats up, the temperature of fiber drawing furnace is made to rise above ti sapphire crystal
Melting temperature keeps the temperature 15~20min, and drawing optical fiber, obtaining fibre core is amorphous titanium-doped sapphire amorphous optical fiber.
5. the preparation method of titanium-doped sapphire amorphous optical fiber according to claim 4, which is characterized in that specifically:
It is cleaned up with ultrasonic cleaning, then with deionized water and absolute alcohol.
6. the preparation method of titanium-doped sapphire amorphous optical fiber according to claim 4, which is characterized in that step (4) is described
Heating, specifically:
Fiber drawing furnace is set to be raised to wire-drawing temperature with 5~10 DEG C of heating rates per minute.
7. the preparation method of titanium-doped sapphire amorphous optical fiber according to claim 4, which is characterized in that described to make fiber drawing furnace
Temperature rise above the melting temperature of ti sapphire crystal, specifically:
The temperature of fiber drawing furnace is set to be raised to about 2050~2200 DEG C.
8. the preparation method of titanium-doped sapphire amorphous optical fiber according to claim 4, which is characterized in that step (1) is described
Processing, specifically: it is cold worked on machining tool.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810687229.5A CN108947233B (en) | 2018-06-28 | 2018-06-28 | Titanium-doped sapphire amorphous optical fiber and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810687229.5A CN108947233B (en) | 2018-06-28 | 2018-06-28 | Titanium-doped sapphire amorphous optical fiber and preparation method and application thereof |
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| Publication Number | Publication Date |
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| CN108947233A true CN108947233A (en) | 2018-12-07 |
| CN108947233B CN108947233B (en) | 2021-09-21 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112729601A (en) * | 2020-12-08 | 2021-04-30 | 北京信息科技大学 | Sapphire F-P optical fiber temperature sensor prepared by femtosecond laser |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080047303A1 (en) * | 2006-08-25 | 2008-02-28 | National Sun Yat-Sen University | Indirect heat type double-clad crystal fiber fabrication method |
| CN101710193A (en) * | 2009-11-27 | 2010-05-19 | 电子科技大学 | Method for manufacturing microstructure fiber |
| CN101799572A (en) * | 2010-03-15 | 2010-08-11 | 阮双琛 | Titanium gem photonic crystal fiber and preparation method thereof |
| CN102073099A (en) * | 2009-11-25 | 2011-05-25 | 德拉克通信科技公司 | High-Bandwidth Multimode Optical Fiber |
| CN104556671A (en) * | 2015-01-19 | 2015-04-29 | 华南理工大学 | Preparation method of transition metal ion doped microcrystalline glass fibers |
-
2018
- 2018-06-28 CN CN201810687229.5A patent/CN108947233B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080047303A1 (en) * | 2006-08-25 | 2008-02-28 | National Sun Yat-Sen University | Indirect heat type double-clad crystal fiber fabrication method |
| CN102073099A (en) * | 2009-11-25 | 2011-05-25 | 德拉克通信科技公司 | High-Bandwidth Multimode Optical Fiber |
| CN101710193A (en) * | 2009-11-27 | 2010-05-19 | 电子科技大学 | Method for manufacturing microstructure fiber |
| CN101799572A (en) * | 2010-03-15 | 2010-08-11 | 阮双琛 | Titanium gem photonic crystal fiber and preparation method thereof |
| CN104556671A (en) * | 2015-01-19 | 2015-04-29 | 华南理工大学 | Preparation method of transition metal ion doped microcrystalline glass fibers |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112729601A (en) * | 2020-12-08 | 2021-04-30 | 北京信息科技大学 | Sapphire F-P optical fiber temperature sensor prepared by femtosecond laser |
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