CN106316138A - Near-infrared emitting tellurium quantum dot doped fiber and preparing method thereof - Google Patents
Near-infrared emitting tellurium quantum dot doped fiber and preparing method thereof Download PDFInfo
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- CN106316138A CN106316138A CN201610715964.3A CN201610715964A CN106316138A CN 106316138 A CN106316138 A CN 106316138A CN 201610715964 A CN201610715964 A CN 201610715964A CN 106316138 A CN106316138 A CN 106316138A
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- glass
- tellurium
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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
- C03C13/048—Silica-free oxide glass compositions
-
- 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
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
-
- 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
- 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
- C03C2213/00—Glass fibres or filaments
- C03C2213/04—Dual fibres
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Glass Compositions (AREA)
Abstract
The invention discloses a near-infrared emitting tellurium quantum dot doped fiber, comprising fibre core glass and cladding glass, the described fibre core glass covers Li2O, Na2O, K2O, Al2O3, MgO, CaO, SrO, BaO, ZnO, TeO2, P2O5; and cladding glass covers La2O3, Li2O, Na2O, K2O, Al2O3,MgO, CaO, SrO, BaO, ZnO, TeO2, P2O5. The invention also discloses a preparing method for the near-infrared emitting tellurium quantum dot fiber, adopting rod-in-tube technique for preparing. Optical fiber of the invention can be prepared under low temperature, and can avoid tellurium volatilization, achieve high concentration adulteration of tellurium and efficient luminescence, the best adulteration concentration is 5 mol %, which is three order of magnitudes above higher than the tellurium adulteration concentration in the silica fiber; the optical fiber luminescence coverage is 900-1,500nm, and the luminescence full width at half maximum is more than 200nm.
Description
Technical field
The present invention relates to the preparation field of optical fiber, particularly to a kind of quantum dot-doped optical fiber of near-infrared light-emitting tellurium and preparation
Method.
Background technology
Quantum dot-doped optical fiber is a class New Active glass optical fiber, has broadband near-infrared luminous, it is possible to achieve adjustable
Humorous laser exports.Quantum dot shows local order in glass structure, and the structure of this local order material often has
Unique root.In recent years, Quantum Dot Glass is studied by Many researchers.But Quantum Dot Glass optical fiber also exists very
The most challenging problem, on the one hand, Quantum Dot Glass will carry out annealing or secondary heat treatment could obtain quantum dot.But
Quantum Dot Glass is during secondary heat treatment and fibre-optical drawing, and due to dimensional effect, crystal grain is grown up again, split-phase, oxidation
Reduction reactions etc. cause glass devitrification blackening, and cause light scattering and absorb increase, thus cause glass luminescence significantly to weaken
Even disappear.The character of quantum dot uniqueness disappears the most immediately, is difficult to prepare high-quality Quantum Dot Glass optical fiber.The opposing party
Face, the tellurite fiber of report is tellurium doping silica fibre at present, uses modified chemical vapor deposition (MCVD) to prepare.But this system
Preparation Method must be carried out under the high temperature more than 2000 degree, and otherwise quartz cannot soften, it is impossible to prepares optical fiber.The highest temperature
Tellurium will be caused to volatilize in a large number, so the tellurium silica fibre prepared, tellurium doping content is low, only 0.02at%, and gain is low.This or
Permitted to be because tellurium concentration extremely low time the reason that cannot be formed of tellurium cluster ions luminophore.Tellurium silica fibre gain is low, utilizes short
Optical fiber cannot realize laser generation, is unfavorable for device miniaturization, intensive.Thermal stability is good, it is possible to stablize tellurium near-infrared
Luminescence, highly doped tellurium concentration is to prepare high-quality tellurium quanta point optical fiber key.But currently without can near-infrared luminous, can adopt
With the report of tellurium Quantum Dot Glass optical fiber prepared by rod-in-tube technique.
Summary of the invention
In order to overcome the disadvantages mentioned above of prior art with not enough, it is an object of the invention to provide a kind of near-infrared light-emitting tellurium
Quantum dot-doped optical fiber, highly doped tellurium concentration, illumination effect is good, is expected to swash at broadband optical fiber amplifier, wideband adjustable optical fiber
The field such as light, ultra-short pulse laser obtains application.
Another object of the present invention is to provide the preparation method of the quantum dot-doped optical fiber of a kind of near-infrared light-emitting tellurium, use
Rod-in-tube technique, preparation temperature is low, can be prevented effectively from tellurium volatilization, and the glass of fiber core tellurium quantum dot size of the optical fiber prepared reduces also
Stable existence.
The purpose of the present invention is achieved through the following technical solutions:
A kind of quantum dot-doped optical fiber of near-infrared light-emitting tellurium, including glass of fiber core and cladding glass, in described glass of fiber core
The molar percentage of each oxide component is:
In described cladding glass, the molar percentage of each oxide component is:
TeO in described glass of fiber core2Molar percentage be 5mol%.
The preparation method of the quantum dot-doped optical fiber of a kind of near-infrared light-emitting tellurium, comprises the following steps:
(1) use melted-quenching method, found glass of fiber core and cladding glass respectively at 1000～1250 DEG C, and 450～
500 DEG C of annealing；
In described glass of fiber core, the molar percentage of each oxide component is:
In described cladding glass, the molar percentage of each oxide component is:
(2) glass of fiber core step (1) obtained and cladding glass are processed into glass of fiber core rod and cladding glass rod respectively,
Surface finish；
(3) at cladding glass rod centrally along axially punching, hole inwall is polished；
(4) glass of fiber core rod is filled in cladding glass rod central duct, prepare preform；
(5) preform is put into fiber drawing tower, draws, obtain optical fiber.
Drawing described in step (5), particularly as follows:
Draw at 750～900 DEG C.
TeO in described glass of fiber core2Molar content be 5mol%.
Step is founded described in (1), specifically, found 1～5 hour.
Step (1) described annealing, particularly as follows: anneal 100-200 hour.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) the quantum dot-doped optical fiber of the near-infrared light-emitting tellurium of the present invention, highly doped tellurium concentration, illumination effect is good, is expected to
The fields such as broadband optical fiber amplifier, wideband adjustable optical-fiber laser, ultra-short pulse laser obtain application.
(2) preparation method of the quantum dot-doped optical fiber of the near-infrared light-emitting tellurium of the present invention, after the glass of fiber core annealing of preparation
Tellurium quantum dot size reduces and stable existence, along with the increase luminescence enhancement of annealing time and temperature.
(3) present invention is controlled by the component of glass of fiber core and cladding glass, can prepare at low temperature (1000～1350 DEG C),
Being avoided that tellurium volatilizees, can realize tellurium high-concentration dopant, doping content is more than three orders of magnitude of tellurium doping silica fibre.
Accompanying drawing explanation
Fig. 1 (a) is the high-resolution-ration transmission electric-lens figure before the annealing of glass of fiber core prepared by embodiments of the invention.
Fig. 1 (b) is the high-resolution-ration transmission electric-lens figure after the annealing of glass of fiber core prepared by embodiments of the invention.
Fig. 2 is the illuminated diagram of the quantum dot-doped optical fiber of tellurium prepared by embodiments of the invention.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
Embodiment
The preparation process of the quantum dot-doped optical fiber of near-infrared light-emitting tellurium of the present embodiment is as follows:
(1) with lanthana, magnesium oxide, calcium carbonate, strontium carbonate, brium carbonate, zinc oxide, phosphorus pentoxide (or biphosphate
Ammonium), aluminium oxide (or aluminium hydroxide), lithium carbonate, sodium carbonate, potassium carbonate etc. be raw material, use traditional melted-quenching method, press
Fiber core glass described in table 1 and mole composition of cladding glass, melting technology condition prepare structural glass sample respectively；
Glass sample is made annealing treatment by annealing process as described in table 1, eliminates residual stress in glass, prevents glass in the course of processing
In broken.
(2) covering prepared in step (1) and glass of fiber core are processed into respectively bar-shaped, polishing.
(3) at cladding glass rod centrally along axially punching, hole inwall is polished.
(4) glass of fiber core rod is filled in cladding glass rod central duct, prepare preform.
(5) preform being put into fiber drawing tower, drawing condition as described in table 1 prepares optical fiber.
Multicomponent fibre cladding glass prepared by table 1 the present embodiment, the Mole percent of each oxide component of glass of fiber core
Ratio (mol%), glass melting condition, glass annealing process condition, drawing condition and luminous situation
Optical fiber prepared by the present embodiment, TeO2Optimum molar percentage ratio when being 5mol%, luminous situation is optimal.This enforcement
Fibre diameter prepared by example～200 microns, fibre core/cladding diameter is than for 1:15.Fibre diameter can control drawing speed regulation.Figure
1 (a), Fig. 1 (b) are respectively the high-resolution-ration transmission electric-lens figure before and after glass of fiber core (sample 5 glass of fiber core in table 1) annealing, and it shows
Before showing annealing, tellurium quantum dot size is mainly between 5～12 nanometers, and after annealing, tellurium quantum dot size is mainly received between 2～7
Between meter, other samples are similar to therewith, and after annealing, nano-particle substantially diminishes and stable existence.Glass prepared by the present embodiment
Heat treatment at 500～650 DEG C, glass keeps red and transparent, without crystallize, Heat stability is good.Fig. 2 is that the present embodiment prepares tellurium
The illuminated diagram of quantum dot-doped optical fiber (sample 5 in table 1), TeO in glass of fiber core2Molar percentage be 5%, it is luminous covers
900-1500nm, luminous halfwidth 266nm；The optical fiber being made up of this glass of fiber core, luminous similar to glass of fiber core, cover
900-1500nm, luminous halfwidth 270nm.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (7)
1. the quantum dot-doped optical fiber of near-infrared light-emitting tellurium, including glass of fiber core and cladding glass, it is characterised in that described fibre
In core glass, the molar percentage of each oxide component is:
In described cladding glass, the molar percentage of each oxide component is:
A kind of quantum dot-doped optical fiber of near-infrared light-emitting tellurium the most according to claim 1, it is characterised in that described fibre core glass
TeO in glass2Molar percentage be 5mol%.
3. the preparation method of the quantum dot-doped optical fiber of near-infrared light-emitting tellurium, it is characterised in that comprise the following steps:
(1) use melted-quenching method, found glass of fiber core and cladding glass respectively at 1000～1250 DEG C, and 450～500
DEG C annealing；
In described glass of fiber core, the molar percentage of each oxide component is:
In described cladding glass, the molar percentage of each oxide component is:
(2) glass of fiber core step (1) obtained and cladding glass are processed into glass of fiber core rod and cladding glass rod, surface respectively
Polishing；
(3) at cladding glass rod centrally along axially punching, hole inwall is polished；
(4) glass of fiber core rod is filled in cladding glass rod central duct, prepare preform；
(5) preform is put into fiber drawing tower, draws, obtain optical fiber.
The preparation method of the quantum dot-doped optical fiber of near-infrared light-emitting tellurium the most according to claim 3, it is characterised in that step
(5) drawing described in, particularly as follows:
Draw at 750～900 DEG C.
The preparation method of the quantum dot-doped optical fiber of near-infrared light-emitting tellurium the most according to claim 3, it is characterised in that described
TeO in glass of fiber core2Molar content be 5mol%.
The preparation method of near-infrared light-emitting tellurium quanta point optical fiber the most according to claim 3, it is characterised in that step (1)
Described found, specifically, found 1～5 hour.
The preparation method of the quantum dot-doped optical fiber of near-infrared light-emitting tellurium the most according to claim 3, it is characterised in that step
(1) described annealing, particularly as follows: anneal 100-200 hour.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610715964.3A CN106316138A (en) | 2016-08-24 | 2016-08-24 | Near-infrared emitting tellurium quantum dot doped fiber and preparing method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610715964.3A CN106316138A (en) | 2016-08-24 | 2016-08-24 | Near-infrared emitting tellurium quantum dot doped fiber and preparing method thereof |
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| CN106316138A true CN106316138A (en) | 2017-01-11 |
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ID=57790337
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| CN201610715964.3A Pending CN106316138A (en) | 2016-08-24 | 2016-08-24 | Near-infrared emitting tellurium quantum dot doped fiber and preparing method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407478A (en) * | 2019-08-04 | 2019-11-05 | 五邑大学 | A kind of cluster doped borate glass of near-infrared light-emitting tellurium and preparation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1402028A (en) * | 2002-09-06 | 2003-03-12 | 中国科学院上海光学精密机械研究所 | Rare-earth element doped glass double-clad optic fibre and mfg. method thereof |
| CN102515512A (en) * | 2010-08-06 | 2012-06-27 | 肖特公司 | Broadening of rare earth ion emission bandwidth in phosphate based laser glasses |
| CN104556678A (en) * | 2015-01-19 | 2015-04-29 | 华南理工大学 | Preparation method of quantum dot doped microcrystalline glass optical fiber |
| CN105198213A (en) * | 2015-08-17 | 2015-12-30 | 华南理工大学 | Near-infrared luminescence tellurium quantum dot doped red glass and preparing method thereof |
-
2016
- 2016-08-24 CN CN201610715964.3A patent/CN106316138A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1402028A (en) * | 2002-09-06 | 2003-03-12 | 中国科学院上海光学精密机械研究所 | Rare-earth element doped glass double-clad optic fibre and mfg. method thereof |
| CN102515512A (en) * | 2010-08-06 | 2012-06-27 | 肖特公司 | Broadening of rare earth ion emission bandwidth in phosphate based laser glasses |
| CN104556678A (en) * | 2015-01-19 | 2015-04-29 | 华南理工大学 | Preparation method of quantum dot doped microcrystalline glass optical fiber |
| CN105198213A (en) * | 2015-08-17 | 2015-12-30 | 华南理工大学 | Near-infrared luminescence tellurium quantum dot doped red glass and preparing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407478A (en) * | 2019-08-04 | 2019-11-05 | 五邑大学 | A kind of cluster doped borate glass of near-infrared light-emitting tellurium and preparation method |
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