CN110412681A - A kind of quantum dot-doped fiber preparation apparatus and method - Google Patents
A kind of quantum dot-doped fiber preparation apparatus and method Download PDFInfo
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- CN110412681A CN110412681A CN201810394432.3A CN201810394432A CN110412681A CN 110412681 A CN110412681 A CN 110412681A CN 201810394432 A CN201810394432 A CN 201810394432A CN 110412681 A CN110412681 A CN 110412681A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 39
- 239000013307 optical fiber Substances 0.000 claims abstract description 32
- 238000002347 injection Methods 0.000 claims abstract description 30
- 239000007924 injection Substances 0.000 claims abstract description 30
- 239000002096 quantum dot Substances 0.000 claims description 67
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- 239000000243 solution Substances 0.000 claims description 24
- 229910002475 Cu2ZnSnS4 Inorganic materials 0.000 claims description 21
- 238000005119 centrifugation Methods 0.000 claims description 17
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- 238000006243 chemical reaction Methods 0.000 claims description 13
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- -1 octadecylene Chemical group 0.000 claims description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
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- 239000005642 Oleic acid Substances 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 3
- 238000001723 curing Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
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- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 3
- 238000001935 peptisation Methods 0.000 claims 1
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- 229910000238 buergerite Inorganic materials 0.000 description 2
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 2
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- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 description 1
- 229910004613 CdTe Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/661—Chalcogenides
- C09K11/662—Chalcogenides with zinc or cadmium
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/02—Optical fibres with cladding with or without a coating
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
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- Optics & Photonics (AREA)
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Abstract
The invention discloses a kind of quantum dot-doped fiber preparation apparatus and methods, belong to optical communication and technical field of nano material.Described device includes: multiple card slots, injection needle, microscope device, light curring unit and rotating device, the multiple card slot is linearly distributed setting, for fixing hollow-core fiber, the position near the card slot of end is arranged in the multiple card slot in the injection needle, the microscope device is arranged in the mode opposite with the hollow periphery of the hollow-core fiber, and the periphery of the hollow-core fiber is arranged in the light curring unit.Quantum dot-doped fiber preparation apparatus provided by the invention and method, it is simple and easy to do, the preparation of different type, different sizes, the quantum dot-doped optical fiber of various concentration can be met.
Description
Technical field
The present invention relates to optical communication and technical field of nano material, in particular to a kind of quantum dot-doped optical fiber preparation dress
It sets and method.
Background technique
Quantum dot is the nanocrystal of size 1-20nm, and internal electron or hole are limited on three-dimensional space, energy level knot
Structure is discrete, has quantum size effect, quantum confined effect, skin effect etc., is widely used to biological fluorescent labelling, light is urged
The fields such as change, solar battery.The absorption of quantum dot, radiation spectrum almost cover 490-2300nm wave band, therefore quantum dot-doped
Optical fiber is the preferable selection for realizing broad-band illumination；Absorption (radiation) peak can be realized by change quantum vertex type, size simultaneously
Controllably, simple process is opened to realize that wideband adjustable shines in quantum dot-doped microcrystalline glass optical fiber for position, overall with half high (FWHM)
New approach is warded off.Therefore, quantum dot is applied to silica fibre and quantum dot-doped optical fiber is made, to New Generation Optical fiber amplifier
Research be of great significance, a kind of quantum dot-doped fiber preparation apparatus that simplicity is handy is provided and method just seems and especially must
It wants.
Typical quanta point material has II-VI group binary compound (CdS, CdSe) and I-III-VI race ternary compound
(CuInS2、CuInSe2).Compared with binary compound, quaternary Cu2ZnSnS4The absorption coefficient of light (> 10 with higher4cm-1)
With suitable forbidden bandwidth (1.5eV), and component abundance is big, safe and non-toxic.Reported quantum dot-doped optical fiber is adopted
It is adulterated with binary compounds such as PbSe, CdSe, CdTe, CdS, introduces rare and dispersed element even heavy metal member in a fiber
Element, material cost is high and toxic, runs counter to green optical communication theory.Cu2ZnSnS4Quantum dot has absorption spectra blue shift, width
FWHM fluorescent characteristic and big absorption cross-section, with Cu2ZnSnS4Quantum dot prepares doped fiber, be conducive to develop high efficiency, it is low at
Originally, environment-friendly optical fiber amplifier.
Currently, binary, the technology of preparing of ternary quantum dots have tended to be mature, and quaternary Cu2ZnSnS4Comprising multiple element,
The increase of element species increases its chemical component and the Degree of Structure Freedom, ZnS, SnS easily occurs in synthesis processx、CuxS、
Cu2SnS3Equal miscellaneous phases, therefore pure phase Cu2ZnSnS4The synthesis of quantum dot is always the difficult point of research.
Summary of the invention
In order to solve problems in the prior art, the embodiment of the invention provides a kind of quantum dot-doped fiber preparation apparatus and
Method.The technical solution is as follows:
On the one hand, a kind of quantum dot-doped fiber preparation apparatus is provided, described device includes:
Multiple card slots, injection needle, microscope device, light curring unit and rotating device, the multiple card slot are linear
Distribution setting, for fixing hollow-core fiber, the attached of the card slot for being located at end in the multiple card slot is arranged in the injection needle
Near position, the microscope device are arranged in the mode opposite with the hollow periphery of the hollow-core fiber, the light curring unit
The periphery of the hollow-core fiber is set.
Preferably, the card slot is V-groove.
Preferably, the quantity of the card slot is 2.
Preferably, the microscope device includes microscope and the micro-image display device connecting with the microscope.
Preferably, the light curring unit includes UV light reflecting cover and UV lamp pipe.
Preferably, the injection needle is micron syringe needle.
Preferably, the injection needle is also connected with the control device of its injection of control.
On the other hand, the quantum dot-doped optical fiber preparation side according to above-mentioned quantum dot-doped fiber preparation apparatus is provided
Method, comprising:
Hollow-core fiber is placed in multiple card slots；
Microscope device is opened, the Cu prepared using injection needle from the injection of hollow-core fiber one end2ZnSnS4Quantum dot/UV
Sol solution；
After the completion of injection, light curring unit is opened；
The rotating device connecting with optical fiber, at the uniform velocity spin fiber are opened, keeps UV glue uniform curing.
Preferably, the method also includes:
According to Cu (CH3COO)2: Zn (CH3COO)2=(1~10): 1, Zn (CH3COO)2: SnCl2=1:(1~5) rub
You are added into the octadecylene of 10~100mL than weighing reagent, under vacuum or atmosphere of inert gases, solution is heated to 100~
150 DEG C, uniform stirring, until metal salt is completely dissolved；
0.5~5mL n- dodecyl mereaptan, 100~150 DEG C of heat preservation 10min or more are added；
0.2~2mL oleic acid, 100~150 DEG C of heat preservation 10min or more, to remove the moisture and dissolved oxygen in solution are added；
It is rapidly heated to 200~300 DEG C of reaction temperature, keeps the temperature 2~50min, obtain dark brown and generate liquid；
Liquid to be generated is cooled to room temperature, according to generate liquid: methanol=1:3 volume ratio mix strongly shake up, 6000~
8000rmp centrifugation, obtains sediment i.e. Cu2ZnSnS4Quantum dot.
Preferably, the method also includes:
Appropriate n-hexane dissolution Cu is added2ZnSnS4Quantum dot, 4000~6000rmp centrifugation, obtains upper solution；
According to solution: the mixing of methanol=1:1 volume ratio shakes up, and 6000~8000rmp centrifugation repeats above step 3~7
It is secondary, to remove the impurity for being attached to quantum dot surface；
It measures ultraviolet cured adhesive and is placed in test tube, the Cu after purification is added2ZnSnS4Quantum dot is placed in supersonic oscillations instrument
Middle oscillation keeps quantum dot evenly dispersed, by controlling the quality of quantum dot or the volume acquisition respective concentration of ultraviolet cured adhesive
Cu2ZnSnS4Quantum dot/UV sol solution.
Technical solution provided in an embodiment of the present invention has the benefit that
1, the quantum dot-doped fiber preparation apparatus provided, structure is simple, can meet different type, different sizes, difference
The preparation of the quantum dot-doped optical fiber of concentration；
2, accordingly with the preparation method of the quantum dot-doped fiber preparation apparatus, the process behaviour for preparing optical fiber is easy easily
Row；
3, Cu is prepared using the thermal decomposition method provided in the embodiment of the present invention2ZnSnS4Quantum dot knot may be implemented in quantum dot
The controlledly synthesis of structure, size, and product has polymolecularity and homogeneity, miscellaneous phase is few, can be directly used for preparing quantum dot-doped
Optical fiber.
Detailed description of the invention
To describe the technical solutions in the embodiments of the present invention more clearly, make required in being described below to embodiment
Attached drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for
For those of ordinary skill in the art, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is quantum dot-doped fiber preparation apparatus structural schematic diagram provided in an embodiment of the present invention；
Fig. 2 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4The X of quantum dot
X ray diffration pattern x；
Fig. 3 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4Quantum dot it is saturating
Penetrate electron microscope；
Fig. 4 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4Quantum dot it is saturating
Penetrate electron microscope；
Fig. 5 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4Quantum dot it is saturating
Penetrate electron microscope；
Fig. 6 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4Quantum dot it is saturating
Penetrate electron microscope；
Fig. 7 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4Quantum dot it is saturating
Penetrate electron microscope；
Fig. 8 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4Quantum dot it is saturating
Penetrate electron microscope.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with attached in the embodiment of the present invention
Figure, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is only this
Invention a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art exist
Every other embodiment obtained under the premise of creative work is not made, shall fall within the protection scope of the present invention.
It should be noted that the present invention " near " etc. in orientation as described in description be all based on orientation or position shown in the drawings
The contextual definition set, it is merely for convenience of description of the present invention and simplification of the description, rather than device described in indication or suggestion must
It must be constructed and operated in a specific orientation, therefore be not considered as limiting the invention.In the description of the present invention, " multiple "
It is meant that two and two or more, unless otherwise specifically defined.
Quantum dot-doped fiber preparation apparatus provided in an embodiment of the present invention and method, it is simple and easy to do, inhomogeneity can be met
The preparation of type, different sizes, the quantum dot-doped optical fiber of various concentration.
Combined with specific embodiments below and attached drawing, to quantum dot-doped fiber preparation apparatus provided in an embodiment of the present invention and
Method is described further.
Quantum dot-doped fiber preparation apparatus provided in an embodiment of the present invention, including multiple card slots, injection needle, microscope
Equipment, light curring unit, rotating device and mounting platform.
Wherein, multiple card slots linearly distribution setting on mounting platform, for solid before preparing quantum dot doped fiber
Determine hollow-core fiber, the quantity of card slot can be two or more here, and multiple card slots can guarantee the balance of hollow-core fiber
Stability.The shape of card slot is preferably V-groove, also can choose other any type in the cards of U-type groove such as and fixes
Structure, the embodiment of the present invention do not limit it especially.The fixing stability of V-groove is preferable, facilitate it is handy, also just due to
This, when card slot is V-groove, selection is also just firm enough using two.Injection needle, which is arranged in multiple card slots, is located at end
Card slot near position injection behaviour is carried out to hollow-core fiber convenient for injection needle in this way when hollow-core fiber is placed in card slot
Make.Injection needle is also connected with the control device of its injection of control, is preferably fixed by mounting platform, and when operation passes through adjusting
The x y location of mounting platform controls injection needle.Additionally preferably, injection needle here is preferably chosen a micron syringe needle.It is aobvious
Micro-mirror device is arranged in the mode opposite with the hollow periphery of hollow-core fiber, preferably with the hollow periphery face of hollow-core fiber
Mode, the effect for preparing for quantum dot-doped optical fiber observe and record.Preferably microscope device includes microscope
And the micro-image display device being connect with the microscope, such as computer etc..Hollow-core fiber is arranged in light curring unit
Periphery preferably includes UV light reflecting cover and UV lamp pipe for carrying out photocuring to optical fiber.
Fig. 1 is quantum dot-doped fiber preparation apparatus structural schematic diagram provided in an embodiment of the present invention.As shown in Figure 1, empty
Core fibre 1 is placed on two V-grooves 2,4, and two V-grooves 2,4 are set on mounting platform with a fixed spacing, and spacing here can root
It is adjusted according to the hollow-core fiber segment length of interception.Micron syringe needle 3 is located at position near V-groove 2, and micron syringe needle 3 is installed on
Control the control device (not shown) of its injection.Microscope 5 is set to the position of the hollow periphery in face hollow-core fiber one end
It sets, microscope 5 is connected with micro-image display device 6.The periphery of hollow-core fiber 1 is provided with UV light reflecting cover 7 and UV lamp pipe
8。
In addition, the embodiment of the invention also provides a kind of quantum dot-doped light of above-mentioned quantum dot-doped fiber preparation apparatus
Fine preparation method, the preparation method the following steps are included:
Hollow-core fiber is placed on multiple card slots；
Microscope device is opened, the Cu prepared using injection needle from the injection of hollow-core fiber one end2ZnSnS4Quantum dot/UV
Sol solution；
After the completion of injection, light curring unit is opened；
The rotating device connecting with optical fiber, at the uniform velocity spin fiber are opened, keeps UV glue uniform curing.
Additionally preferably, above-mentioned preparation method further includes Cu2ZnSnS4Quantum dot preparation process, the preparation process are as follows:
1) according to Cu (CH3COO)2: Zn (CH3COO)2=(1~10): 1, Zn (CH3COO)2: SnCl2=1:(1~5)
Vacuum or atmosphere of inert gases into the octadecylene (Octadecene, ODE) of 10~100mL is added in molar ratio weighing reagent
Under, solution is heated to 100~150 DEG C, uniform stirring, until metal salt is completely dissolved；
2) 0.5~5mL n- dodecyl mereaptan (Dodecanethiol, DDT) is added, 100~150 DEG C of heat preservation 10min or more；
3) 0.2~2mL oleic acid (Oleic acid, OA) is added, 100~150 DEG C of heat preservation 10min or more, to remove solution
In moisture and dissolved oxygen；
4) it is rapidly heated to 200~300 DEG C of reaction temperature, keeps the temperature 2~50min, obtain dark brown and generate liquid；
5) liquid to be generated is cooled to room temperature, according to generate liquid: methanol=1:3 volume ratio mix strongly shake up, 6000~
8000rmp centrifugation, obtains sediment i.e. Cu2ZnSnS4Quantum dot.
Fig. 2 is the Cu of quantum dot-doped method for preparing optical fiber preparation provided in an embodiment of the present invention2ZnSnS4The X of quantum dot
X ray diffration pattern x.Fig. 2 is shown, obtains the mutually single buergerite Cu of object using above-mentioned preparation method2ZnSnS4Structure.Gained
Cu2ZnSnS4The X-ray diffractogram of quantum dot such as Fig. 1.In figure, diffraction peak and buergerite Cu2ZnSnS4Map (100),
(002), (101), (102), (110), (103) and (112) crystal face correspond, and Cu is not presentxS、ZnS、SnSx、Cu2SnS3
Etc. binary or ternaries compound miscellaneous phase peak position, show products therefrom be pure phase Cu2ZnSnS4Structure.
Below in conjunction with specific embodiment to above-mentioned Cu2ZnSnS4Quantum dot preparation method is described further.
Embodiment 1
Take the pure 1mmol Cu (CH of analysis3COO)2、0.5mmol Zn(CH3COO)2、0.5mmol SnCl2And 20mL ODE
Be placed in three-neck flask, vacuum condition, at 120 DEG C uniform stirring until metal salt is completely dissolved；1mL DDT, 120 DEG C of heat preservations are added
10min；0.5mL OA is added, solution is heated to 120 DEG C of heat preservation 10min；It is rapidly heated to 220 DEG C of reaction temperature, keeps the temperature
20min, liquid to be generated are cooled to room temperature, according to generate liquid: methanol=1:3 volume ratio mix strongly shake up, 6000~
8000rmp centrifugation obtains 3.6nm Cu after centrifugation purification2ZnSnS4Quantum dot.Fig. 3 is quantum dot provided in an embodiment of the present invention
The Cu of doped fiber preparation method preparation2ZnSnS4The transmission electron microscope picture of quantum dot, the Cu which obtains2ZnSnS4Quantum
Point transmission electron microscope picture is as shown in Figure 3.
Embodiment 2
In the present embodiment, in addition to reaction temperature is 240 DEG C, 20min is kept the temperature, obtains 5.3nm after centrifugation purification
Cu2ZnSnS4Quantum dot, other reaction conditions and implementation process are same as Example 1.Fig. 4 is amount provided in an embodiment of the present invention
The Cu of son point doped fiber preparation method preparation2ZnSnS4The transmission electron microscope picture of quantum dot, the Cu which obtains2ZnSnS4
Quantum dot transmission electron microscope picture is as shown in Figure 4.
Embodiment 3
In the present embodiment, in addition to reaction temperature is 270 DEG C, 20min is kept the temperature, obtains 10.5nm after centrifugation purification
Cu2ZnSnS4Quantum dot, other reaction conditions and implementation process are same as Example 1.Fig. 5 is amount provided in an embodiment of the present invention
The Cu of son point doped fiber preparation method preparation2ZnSnS4The transmission electron microscope picture of quantum dot, the Cu which obtains2ZnSnS4
Quantum dot transmission electron microscope picture is as shown in Figure 5.
Embodiment 4
Take the pure 5mmol Cu (CH of analysis3COO)2、0.5mmol Zn(CH3COO)2、2.5mmol SnCl2And 100mL
ODE is placed in three-neck flask, vacuum condition, at 150 DEG C uniform stirring until metal salt is completely dissolved；Be added 5mL DDT, 150 DEG C
Keep the temperature 15min；2mL OA is added, solution is heated to 150 DEG C of heat preservation 15min；It is rapidly heated to 240 DEG C of reaction temperature, protects
Warm 5min.Liquid to be generated is cooled to room temperature, according to generate liquid: methanol=1:3 volume ratio mix strongly shake up, 6000~
8000rmp centrifugation obtains 3.2nm Cu after centrifugation purification2ZnSnS4Quantum dot.Fig. 6 is quantum dot provided in an embodiment of the present invention
The Cu of doped fiber preparation method preparation2ZnSnS4The transmission electron microscope picture of quantum dot, the Cu which obtains2ZnSnS4Quantum
Point transmission electron microscope picture is as shown in Figure 6.
Embodiment 5
In the present embodiment, in addition to reaction temperature is 240 DEG C, 20min is kept the temperature, obtains 4.8nm after centrifugation purification
Cu2ZnSnS4Quantum dot, other reaction conditions and implementation process are same as Example 4.Fig. 7 is amount provided in an embodiment of the present invention
The Cu of son point doped fiber preparation method preparation2ZnSnS4The transmission electron microscope picture of quantum dot, the Cu which obtains2ZnSnS4
Quantum dot transmission electron microscope picture is as shown in Figure 7.
Embodiment 6
In the present embodiment, in addition to reaction temperature is 240 DEG C, 50min is kept the temperature, obtains 9.7nm after centrifugation purification
Cu2ZnSnS4Quantum dot, other reaction conditions and implementation process are same as Example 4.Fig. 8 is amount provided in an embodiment of the present invention
The Cu of son point doped fiber preparation method preparation2ZnSnS4The transmission electron microscope picture of quantum dot, the Cu which obtains2ZnSnS4
Quantum dot transmission electron microscope picture is as shown in Figure 8.
In addition, obtaining Cu using above scheme2ZnSnS4After quantum dot, Cu2ZnSnS4Quantum dot/UV sol solution system
It is standby preferably to use following steps:
Appropriate n-hexane dissolution Cu is added2ZnSnS4Quantum dot, 4000~6000rmp centrifugation, obtains upper solution；
According to solution: the mixing of methanol=1:1 volume ratio shakes up, and 6000~8000rmp centrifugation repeats above step 3~7
It is secondary, to remove the impurity for being attached to quantum dot surface；
It measures ultraviolet cured adhesive and is placed in test tube, the Cu after purification is added2ZnSnS4Quantum dot is placed in supersonic oscillations instrument
Middle oscillation keeps quantum dot evenly dispersed, by controlling the quality of quantum dot or the volume acquisition respective concentration of ultraviolet cured adhesive
Cu2ZnSnS4Quantum dot/UV sol solution.
All the above alternatives can form alternative embodiment of the invention using any combination, herein no longer
It repeats one by one.
It should be noted that quantum dot-doped method for preparing optical fiber provided by the above embodiment and quantum dot-doped optical fiber system
Standby Installation practice belongs to same design, and specific implementation process is detailed in Installation practice, and which is not described herein again.
In conclusion quantum dot-doped fiber preparation apparatus provided in an embodiment of the present invention and method, compared with prior art,
It has the advantages that
1, the quantum dot-doped fiber preparation apparatus provided, structure is simple, can meet different type, different sizes, difference
The preparation of the quantum dot-doped optical fiber of concentration；
2, accordingly with the preparation method of the quantum dot-doped fiber preparation apparatus, the process behaviour for preparing optical fiber is easy easily
Row；
3, Cu is prepared using the thermal decomposition method provided in the embodiment of the present invention2ZnSnS4Quantum dot knot may be implemented in quantum dot
The controlledly synthesis of structure, size, and product has polymolecularity and homogeneity, miscellaneous phase is few, can be directly used for preparing quantum dot-doped
Optical fiber.
Those of ordinary skill in the art will appreciate that realizing that all or part of the steps of above-described embodiment can pass through hardware
It completes, relevant hardware can also be instructed to complete by program, the program can store in a kind of computer-readable
In storage medium, storage medium mentioned above can be read-only memory, disk or CD etc..
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of quantum dot-doped fiber preparation apparatus characterized by comprising multiple card slots, injection needle, microscope are set
Standby, light curring unit and rotating device, the multiple card slot are linearly distributed setting, for fixing hollow-core fiber, the injection
Syringe needle be arranged in the multiple card slot positioned at end card slot near position, the microscope device with the hollow light
The opposite mode of fine hollow periphery is arranged, and the periphery of the hollow-core fiber is arranged in the light curring unit.
2. the apparatus according to claim 1, which is characterized in that the card slot is V-groove.
3. the apparatus of claim 2, which is characterized in that the quantity of the card slot is 2.
4. the apparatus according to claim 1, which is characterized in that the microscope device includes microscope and micro- with this
The micro-image display device of mirror connection.
5. the apparatus according to claim 1, which is characterized in that the light curring unit includes UV light reflecting cover and UV lamp
Pipe.
6. the apparatus according to claim 1, which is characterized in that the injection needle is micron syringe needle.
7. device according to claim 1 or 6, which is characterized in that the injection needle, which is also connected with, controls its injection
Control device.
8. a kind of quantum dot-doped method for preparing optical fiber of device according to claim 1 characterized by comprising
Hollow-core fiber is placed in multiple card slots；
Microscope device is opened, the Cu prepared using injection needle from the injection of hollow-core fiber one end2ZnSnS4Quantum dot/UV peptization
Liquid；
After the completion of injection, light curring unit is opened；
The rotating device connecting with optical fiber, at the uniform velocity spin fiber are opened, keeps UV glue uniform curing.
9. according to the method described in claim 8, it is characterized in that, the method also includes:
According to Cu (CH3COO)2: Zn (CH3COO)2=(1~10): 1, Zn (CH3COO)2: SnCl2=1:(1~5) molar ratio claim
Reagent is measured, is added into the octadecylene of 10~100mL, under vacuum or atmosphere of inert gases, solution is heated to 100~150 DEG C,
Uniform stirring, until metal salt is completely dissolved；
0.5~5mL n- dodecyl mereaptan, 100~150 DEG C of heat preservation 10min or more are added；
0.2~2mL oleic acid, 100~150 DEG C of heat preservation 10min or more, to remove the moisture and dissolved oxygen in solution are added；
It is rapidly heated to 200~300 DEG C of reaction temperature, keeps the temperature 2~50min, obtain dark brown and generate liquid；
Liquid to be generated is cooled to room temperature, according to generate liquid: methanol=1:3 volume ratio mix strongly shake up, 6000~8000rmp
Centrifugation, obtains sediment i.e. Cu2ZnSnS4Quantum dot.
10. method according to claim 8 or claim 9, which is characterized in that the method also includes:
Appropriate n-hexane dissolution Cu is added2ZnSnS4Quantum dot, 4000~6000rmp centrifugation, obtains upper solution；
According to solution: the mixing of methanol=1:1 volume ratio shakes up, and 6000~8000rmp centrifugation repeats above step 3~7 times,
To remove the impurity for being attached to quantum dot surface；
It measures ultraviolet cured adhesive and is placed in test tube, the Cu after purification is added2ZnSnS4Quantum dot is placed in supersonic oscillations instrument and shakes
It swings, keeps quantum dot evenly dispersed, respective concentration is obtained by the quality of control quantum dot or the volume of ultraviolet cured adhesive
Cu2ZnSnS4Quantum dot/UV sol solution.
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