CN109456757A - A kind of up-conversion luminescent material and preparation method thereof of up-conversion luminescence Selective long-range DEPT - Google Patents
A kind of up-conversion luminescent material and preparation method thereof of up-conversion luminescence Selective long-range DEPT Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 129
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- XILIYVSXLSWUAI-UHFFFAOYSA-N 2-(diethylamino)ethyl n'-phenylcarbamimidothioate;dihydrobromide Chemical compound Br.Br.CCN(CC)CCSC(N)=NC1=CC=CC=C1 XILIYVSXLSWUAI-UHFFFAOYSA-N 0.000 title abstract description 29
- 239000010931 gold Substances 0.000 claims abstract description 69
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052737 gold Inorganic materials 0.000 claims abstract description 47
- 239000002105 nanoparticle Substances 0.000 claims abstract description 45
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/58—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing copper, silver or gold
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Abstract
The present invention provides a kind of this up-conversion luminescent materials of up-conversion luminescence Selective long-range DEPT, belong to up-conversion luminescent material technical field.The preparation of the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT provided by the invention selects micron optical fiber glass core as substrate, on its surface, deposition gold nanometer film is as phasmon structure, by upper conversion nano even particulate dispersion on gold nanometer film surface, the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT is formed.The up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT provided by the invention is excited by waveguide, using the interaction between incident light, gold nanometer film, upper conversion nano particle, realizes the Selective long-range DEPT of up-conversion luminescence.
Description
Technical field
The present invention relates to up-conversion luminescent material technical field, in particular to a kind of up-conversion luminescence Selective long-range DEPT it is upper
Changing luminous material and preparation method thereof.
Background technique
Stokes' law thinks that material can only be excited by the light of high-energy, issues the light of low energy, i.e. wavelength is short
The low light of the high frequency for inspiring wavelength length of frequency.But some materials may be implemented with above-mentioned law it is exactly the opposite shine
Effect, we are called anti-Stokes luminescence, also known as up-conversion luminescence.So far, up-conversion luminescence all occurs adulterating
In the compound of rare earth ion, mainly there are fluoride, oxide, sulfur-containing compound, oxyfluoride and halide etc..
Solar energy is that the utilizable the most abundant clean energy resource of the mankind occupies sunlight major part energy so far
Infrared light be not fully utilized also, the development of up-conversion luminescence nanomaterial provides new think of to improve solar energy utilization ratio
Road.Lanthanide-doped upper conversion nano particle (UCNPs) due to it with high s/n ratio, toxicity is low, emission peak is narrow, light is steady
The features such as qualitative good, has been widely used in the necks such as solar battery, bio-imaging, upconversion laser and three-dimensional full-color display
Domain.However, the poor efficiency of up-conversion luminescence greatly limits further applying for conversion nano particle.Further, since group of the lanthanides
Multiple peaks can occur simultaneously in the emission spectrum of upper conversion nano particle in the multipotency level structure of ion.Lanthanide ion it is this
Multimodal property will limit conversion nano particle further applying in display and upconversion laser production.It is so far
Only, many researchers are by introducing photonic crystal, grating, noble metal nano particles and array, the knot such as metal nucleocapsid and tip
Structure, the efficiency of Lai Tigao up-conversion luminescence.
However, the above method needs to introduce complicated optical device, fine array structure prepares complex, operation
On less flexibly, it is not easy of integration.In addition, these methods are all to whole or multiple emission peaks for the enhancing of up-conversion luminescence
Whole enhancing, the multimodality of up-conversion luminescence is not significantly improved.
Summary of the invention
In view of this, it is an object of that present invention to provide a kind of up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT and
The Selective long-range DEPT of up-conversion luminescence may be implemented in preparation method, up-conversion luminescent material provided by the invention.
The present invention provides a kind of up-conversion luminescent materials of up-conversion luminescence Selective long-range DEPT, cylindric in solid core, by
It is interior to outside successively include micron optical fiber glass core, gold nanometer film and the upper conversion nano for being dispersed in gold nanometer film surface
Particle；The diameter of the micron optical fiber glass core is 0.05~10 μm.
Preferably, the micron optical fiber glass core is to remove the buffer layer of optical fiber and polymer interlayers, by gained fibre core
Heating is elongated to required diameter and obtains.
Preferably, the gold nanometer film with a thickness of 10~25nm.
Preferably, the upper conversion nano particle is six side's β phase NaYF4:Yb3+,Er3+。
Preferably, the up-conversion luminescence nanometer is elliposoidal, a length of 35~41nm of the long axis of the elliposoidal, short axle
A length of 29~35nm.
Preferably, the load density of the upper conversion nano particle is (1.0~5.0) × 1014A/square metre.
The present invention also provides the preparation method of the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT, including it is following
Step:
One layer of gold nanometer film is deposited in micron optical fiber glass wicking surface, upper conversion nano particle solution is soaked into gold nano
Film surface obtains the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT after dry.
Preferably, the method for the deposition is sputter coating.
Preferably, the sputtering current of the sputter coating is 15mA.
Preferably, the concentration of the upper conversion nano particle solution is 0.02~2mg/mL.
Advantageous effects: the present invention selects micron optical fiber glass core as substrate, deposits gold nanometer film on its surface
Up-conversion luminescence selection is formed by upper conversion nano even particulate dispersion on gold nanometer film surface as phasmon structure
Property enhancing up-conversion luminescent material.The up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT provided by the invention passes through wave
Excitation is led, using incident light, the choosing of up-conversion luminescence is realized in gold nanometer film, the interaction between upper conversion nano particle
The enhancing of selecting property.Such as 980nm wavelength laser is transferred in micron optical fiber to excite the phasmon characteristic in gold nanometer film.
Due to the interaction of gold nanometer film surface phasmon and incident light, the local electric field of incident light can be made to be increased
By force, to improve the utilization efficiency of incident light, and then effectively enhance up-conversion luminescence.In addition, gold nanometer film upper plasma swashs
The fuel factor of member induction, which acts on, to be covered on the upper conversion nano particle of gold nano film surface, and conversion particles can be caused
2H11/2Population increases on energy level, (corresponds to 2H in 523nm to selectively enhance11/2→4I15/2Energy level transition) at
Fluorescent emission.By the experimental data of specific embodiment it is found that up-conversion luminescence Selective long-range DEPT that the present invention is prepared
The fluorescence spectrum of up-conversion luminescent material has strongest emission peak at 523 nanometers (green lights).
Detailed description of the invention:
Fig. 1 is the preparation process schematic diagram of the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT；
Fig. 2 is the scanning electron microscope diagram of UCNPs/Au sample obtained in embodiment 1；
Fig. 3 is the enlarged drawing of dashed rectangle part in Fig. 2；
Fig. 4 is the absorption spectrum of UCNPs/Au sample obtained in embodiment 1；
Fig. 5 is the schematic diagram of UCNPs/Au sample up-conversion fluorescence Selective long-range DEPT obtained in embodiment 1；
Fig. 6 be UCNPs sample obtained in UCNPs/Au sample and comparative example 1 obtained in embodiment 1 610 milliwatts,
Illuminated diagram under the excitation of 960nm wavelength；
Fig. 7 be UCNPs sample obtained in UCNPs/Au sample and comparative example 1 obtained in embodiment 1 610 milliwatts,
Fluorescence spectrum under the excitation of 960nm wavelength；
Fig. 8 is up-conversion fluorescence spectrum of the UCNPs/Au sample under different excitation light powers obtained in embodiment 1；
Fig. 9 is UCNPs/Au sample I obtained in embodiment 1523/I655And I523/I545With the variation diagram of power；
Figure 10 is different-thickness gold nanometer film UCNPs/Au sample obtained in Examples 1 to 3 in identical exciting power
Normalization fluorescence spectrum under 610 milliwatts.
Specific embodiment
The present invention provides a kind of up-conversion luminescent materials of up-conversion luminescence Selective long-range DEPT, cylindric in solid core, by
It is interior to outside successively include micron optical fiber glass core, gold nanometer film and the upper conversion nano for being dispersed in gold nanometer film surface
Particle；The diameter of the micron optical fiber glass core is 0.05~10 μm.
In the present invention, the diameter of the micron optical fiber glass core is preferably 1~8 μm, and more preferably 3~5 μm.In this hair
In bright, fibre diameter crosses conference and is unfavorable for waveguide excitation, and the too small meeting of diameter is so that incident light has before reaching excitation area
Too many loss, therefore its diameter is limited to 0.05~10 μm.
In the present invention, the micron optical fiber glass core preferably removes the buffer layer of optical fiber and polymer interlayers, will
The heating of gained fibre core is elongated to required diameter and obtains.The present invention is not particularly limited the source of optical fiber, selects art technology
Commercially available optical fiber known to personnel.The present invention is not particularly limited the method for the removing, selects those skilled in the art
Well known stripping means is preferably removed using optical fiber ablation device in the present invention.The present invention adds gained fibre core
The long method of hot-drawn is not particularly limited, and selects method well known to those skilled in the art.In the present invention, specifically excellent
It is selected as clamping one end of gained fibre core with tweezers and placing it in alcohol blast burner flame envelope heating 0.5~1.5 minute, it is molten to reach it
Point, slowly pulling tweezers to stretch fiber elongates it until fibre diameter is decreased to required length.
In the present invention, the thickness of the gold nanometer film is preferably 10~25nm, more preferably 15~20nm, most
Preferably 18nm.In the present invention, gold nanometer film excitating surface phasmon characteristic under 980nm incident light, so that
The local electric field of incident light is greatly enhanced, to improve the utilization efficiency of incident light, and then effectively enhances up-conversion luminescence.Separately
Outside, the fuel factor of gold nanometer film upper plasma excimer induction acts on the upper conversion nano particle for being covered in gold nano film surface
On, cause conversion particles 2H11/2Population increases on energy level, (corresponds to 2H in 523nm to selectively enhance11/2→
4I15/2Energy level transition) at fluorescent emission.
In the present invention, the upper conversion nano particle is preferably six side's β phase NaYF4:Yb3+,Er3+Nano particle.
In the present invention, the load density of the upper conversion nano particle is preferably (1~5) × 1014A/square metre, more preferably
(2.0~3.0) × 1014A/square metre, most preferably 2.50 × 1014A/square metre.
In the present invention, when the upper conversion nano particle is preferably six side's β phase NaYF4:Yb3+,Er3+When, it is described
NaYF4, Yb and Er molar ratio be preferably 78:20:2.In the present invention, the upper conversion nano particle is preferably elliposoidal,
The long axial length of the elliposoidal is preferably 35~41nm, more preferably 38nm；The long short axle of elliposoidal is preferably 29~35nm, more
Preferably 32nm.The present invention is not particularly limited the source of upper conversion nano particle, selects well known to those skilled in the art
Commercial goods.
The present invention is excited by waveguide, utilizes the phase interaction between incident light, gold nanometer film, upper conversion nano particle
With realizing the Selective long-range DEPT of up-conversion luminescence.
The present invention also provides the preparation methods of the up-conversion luminescent material of above-mentioned up-conversion luminescence Selective long-range DEPT, including
Following steps:
One layer of gold nanometer film is deposited in micron optical fiber glass wicking surface, upper conversion nano particle solution is soaked into gold nano
Film surface obtains the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT after dry.
In the present invention, the method for the deposition is preferably sputter coating.In the present invention, the sputtering of the sputter coating
Electric current is preferably 10~20mA, more preferably 15mA, and the time of the sputtering is preferably 1~5min, more preferably 2min.At this
In invention, the equipment of the sputter coating is preferably ETD2000/3000 sputter coating machine.
In the present invention, the concentration of the upper conversion nano particle solution is preferably 0.02~2mg/mL, more preferably
0.05~0.15mg/mL；In the present invention, changing the solvent of nanoparticles solution on described is preferably water or ethyl alcohol.
The present invention is not particularly limited the method soaked, and selects soaking procedure well known to those skilled in the art.
In the present invention, it is preferred to for upper conversion nano particle solution is added drop-wise to gold nanometer film surface.
In the present invention, it is described upper conversion nano particle solution is dripped into gold nanometer film surface after be further preferably included in room
Lower stand of temperature is dried.The present invention dries removing solvent by standing, and upper conversion nano particle and gold pass through electrostatic attraction steadily
It is coupled together, obtains the up-conversion luminescent material of up-conversion luminescence Selective long-range DEPT.
Fig. 1 is the up-conversion luminescent material preparation process schematic diagram of up-conversion luminescence Selective long-range DEPT.
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
1) buffer layer of optical fiber and polymer interlayers are removed using optical fiber ablation device, obtains fibre core；Then it is pressed from both sides with tweezers
One end of fibre core simultaneously places it in the heating of alcohol blast burner flame envelope 1 minute to reach its fusing point, and slowly pulling tweezers to stretch fiber makes
Its elongation is decreased to 3 microns up to diameter, obtains micron optical fiber glass core.
2) micron optical fiber made is fixed on the glass substrate, place it in 2000/3000 sputter coating of ETD
In machine, sputtering current and sputtering time are respectively set as 15 milliamperes and 2 minutes, gold nanometer film is just successfully deposited on micron
Optical fiber surface, with a thickness of 18 nanometers.
3) sample in step 2) is removed and placed on experimental bench, it is with syringe that upper conversion nano particle is water-soluble
Liquid, upper conversion nano particle water are six sides (β) phase NaYF4:Yb3+,Er3+Nano particle (NaYF4/ Yb/Er=78:20:2), it is dense
Degree is 0.05mg/mL, takes out and is dripped on gold nanometer film surface dropwise.It is placed 10 minutes at room temperature finally, sample is placed in
After solvent evaporation, the up-conversion luminescent material (hereinafter referred to as UCNPs/Au sample) of up-conversion luminescence Selective long-range DEPT is obtained.
Comparative example 1
Buy the amido modified upper conversion nano particle of PEG- in Hefei Heng Na Biotechnology Co., Ltd, product code numbering
103-35-X-NH2, six sides (β) phase NaYF4:Yb3+,Er3+Nano particle (NaYF4/ Yb/Er=78:20:2).
Fig. 2 is the scanning electron microscope diagram of UCNPs/Au sample obtained in embodiment 1.Micron optical fiber as shown in Figure 2
The diameter of glass core is about 3.0 μm.
Fig. 3 is the enlarged drawing of corresponding region in Fig. 2.Upper conversion nano particle is successful and more uniform heavy as shown in Figure 3
For product on the surface of Au nano thin-film and micron optical fiber, grain density is 2.50 × 1014A/square metre.
Fig. 4 is the absorption spectrum of UCNPs/Au sample obtained in embodiment 1.Fig. 4 in embodiment 1 the results show that obtain
UCNPs/Au sample there is good absorbance (0.97) for the light of 980 nanometers of excitation wavelengths, and for up-conversion fluorescence
Absorbance it is lower (absorbance for 523,545,655 nanometers is respectively 0.32,0.31,0.42), be to be conducive to upper conversion
Fluorescence enhancement.
Fig. 5 is the schematic diagram of UCNPs/Au sample up-conversion fluorescence Selective long-range DEPT obtained in embodiment 1.980 nanometers
The laser of wavelength is transferred to micron optical fiber glass in the heart to excite the plasma in gold nanometer film, due to gold nanometer film table
The interaction of face phasmon and incident light can make incident local electric field be greatly enhanced, to improve the benefit of incident light
With efficiency, and then up-conversion fluorescence efficiency can be improved.In addition, with the increase of laser power, since gold nanometer film powers on
The nonradiative transition of son can generate strong fuel factor, and the fuel factor of plasmon induction, which acts on, is covered in gold nano film table
On the upper conversion nano particle in face, population on high level can be caused to increase, to selectively enhance in the glimmering of 523 nanometers
Light emitting.
The laser of 980 nano wave lengths is inputted into the micron optical fiber glass core in embodiment 1 and comparative example 1, with 610 milliwatts
For excitation light power, result is as shown in Figure 6.UCNPs/Au sample is excited and issues shown in green light such as Fig. 6 (a), UCNPs
Sample is excited at identical conditions and emits yellow light, as shown in figure four (b).Fig. 7 is the fluorescence spectrum detected, by Fig. 7
It is found that the fluorescence spectrum of UCNP/Au sample has a strongest emission peak at 523 nanometers (green lights), and the luminous light of UCNPs sample
Occur three main emission peaks centered on 523,545 and 655 nanometers in spectrum, due to the presence of multimodal, the hair of UCNPs sample
Light color is penetrated in yellow.In addition, the emitted luminescence intensity ratio UCNPs sample of UCNPs/Au sample enhances in 523 nanometers of wavelength
36 times.
Intensity rate between three emission peaks of UCNPs/Au sample obtained in embodiment 1 can be with exciting power
Change and change, as shown in Figure 8.When exciting power is 40 milliwatt, 523 and 655 nanometers of (I523/I655), 523 and 545 nanometers
(I523/I545) at the ratio of fluorescence intensity be respectively 1.99 and 0.98.With the increase of exciting power, institute in up-conversion fluorescence
The intensity of some emission peaks has enhancing, wherein 523 nanometers of emission peak intensity increase is most fast.It is 460 milliwatts in exciting power
When, fluorescence intensity ratio I between peak value523/I655And I523/I545Respectively 22.79 and 5.34, this shows that the green of 523 nanometers is glimmering
Light emitting peak has obtained selectively enhancing with the increase of exciting power.
Exciting power progressively increases to 610 milliwatts, the intensity at UCNPs/Au sample difference up-conversion fluorescence peak from 40 milliwatts
Ratio (I523/I655And I523/I545) as shown in Figure 9 with the result of the variation of power.The result shows that up-conversion fluorescence peak strength
Than that can increase with the increase of exciting power, up-conversion fluorescence accounts in entire fluorescence spectrum in the fluorescence peak of 523 nanometers
Ratio it is increasing, i.e., up-conversion fluorescence spectrum unimodality be improved.The Selective long-range DEPT of this fluorescence emission peak with
Fuel factor caused by gold nanometer film phasmon is related.
Embodiment 2
1) buffer layer of optical fiber and polymer interlayers are removed using optical fiber ablation device, obtains fibre core；Then it is pressed from both sides with tweezers
One end of fibre core simultaneously places it in the heating of alcohol blast burner flame envelope 1 minute to reach its fusing point, and slowly pulling tweezers to stretch fiber makes
It is elongated until 3 microns of diameter reduction, obtains micron optical fiber glass core.
2) the micron optical fiber glass heart made is fixed on the glass substrate, place it in ETD2000/3000 sputtering
In coating machine, sputtering current and sputtering time are respectively set as 15 milliamperes and 1 minute, gold nanometer film is just successfully deposited on
Micron optical fiber surface, with a thickness of 10 nanometers.
3) sample in step 2) is removed and placed on experimental bench, it is with syringe that upper conversion nano particle is water-soluble
Liquid, upper conversion nano particle water are six sides (β) phase NaYF4:Yb3+,Er3+Nano particle (NaYF4/ Yb/Er=78:20:2), it is dense
Degree is 0.05mg/mL, takes out and is dripped on gold nanometer film surface dropwise.It is placed 10 minutes at room temperature finally, sample is placed in
After solvent evaporation, the up-conversion luminescent material (hereinafter referred to as UCNPs/Au sample) of up-conversion luminescence Selective long-range DEPT is obtained.
Embodiment 3
1) buffer layer of optical fiber and polymer interlayers are removed using optical fiber ablation device, obtains fibre core；Then it is pressed from both sides with tweezers
One end of fibre core simultaneously places it in the heating of alcohol blast burner flame envelope 1 minute to reach its fusing point, and slowly pulling tweezers to stretch fiber makes
It is elongated until 3 microns of diameter reduction, obtains micron optical fiber glass core.
2) the micron optical fiber glass heart made is fixed on the glass substrate, place it in ETD2000/3000 sputtering
In coating machine, sputtering current and sputtering time are respectively set as 15 milliamperes and 2.5 minutes, gold nanometer film just successfully deposits
On micron optical fiber surface, with a thickness of 25 nanometers.
3) sample in step 2) is removed and placed on experimental bench, it is with syringe that upper conversion nano particle is water-soluble
Liquid, upper conversion nano particle water are six sides (β) phase NaYF4:Yb3+,Er3+Nano particle (NaYF4/ Yb/Er=78:20:2), it is dense
Degree is 0.05mg/mL, takes out and is dripped on gold nanometer film surface dropwise.It is placed 10 minutes at room temperature finally, sample is placed in
After solvent evaporation, the up-conversion luminescent material (hereinafter referred to as UCNPs/Au sample) of up-conversion luminescence Selective long-range DEPT is obtained.
Figure 10 is different-thickness gold nanometer film UCNPs/Au sample obtained in Examples 1 to 3 in identical exciting power
Normalization fluorescence spectrum under 610 milliwatts.As shown in Figure 10 gold nanometer film with a thickness of 18nm when, up-conversion fluorescence intensity
Be it is strongest, show that the gold nano film of 18nm thickness provides best up-conversion fluorescence Selective long-range DEPT for upper conversion nano particle
Effect.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
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| CN116285989A (en) * | 2022-12-15 | 2023-06-23 | 浙江大学杭州国际科创中心 | Rare earth doped nanocomposite and preparation method and application thereof |
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| CN107321392A (en) * | 2017-07-28 | 2017-11-07 | 重庆理工大学 | Photocatalysis hollow quartz fiber and preparation method |
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| CN102544177A (en) * | 2011-03-30 | 2012-07-04 | 郑州大学 | Plasma strengthening upconverter for solar cells and preparation method thereof |
| CN107321392A (en) * | 2017-07-28 | 2017-11-07 | 重庆理工大学 | Photocatalysis hollow quartz fiber and preparation method |
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