CN105219379A - A kind of method of quencher up-conversion luminescence - Google Patents
A kind of method of quencher up-conversion luminescence Download PDFInfo
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- CN105219379A CN105219379A CN201510726266.9A CN201510726266A CN105219379A CN 105219379 A CN105219379 A CN 105219379A CN 201510726266 A CN201510726266 A CN 201510726266A CN 105219379 A CN105219379 A CN 105219379A
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Abstract
A method for quencher up-conversion luminescence, belongs to field of luminescent technology.It is at inorganic Yb
3+mix other metallic cation in ion fluorescence cluster, destroy the fluorophore clustering architecture in material, thus cause the structure deteriorate quencher of cluster fluorescence; Inorganic Yb
3+the matrix of ion fluorescence cluster is alkaline-earth metal fluoride; With the volumetric molar concentration of whole metallic cation be 100% calculating, trivalent group of the lanthanides ytterbium ion Yb
3+doping content be 0.05mol% ~ 10mol%, the doping content of other metallic cation is 0.1mol% ~ 14mol%.The positively charged ion mixed can be do not have the rare earth ion of fluorescent characteristic or the ion of other kind.Utilize this quenching of fluorescence method, effectively can regulate the intensity of cooperative luminescence, also effectively can regulate the Up-conversion Intensity because cooperative sensitization produces.Therefore, this method for quenching has good use range.
Description
Technical field
The invention belongs to field of luminescent technology, be specifically related to a kind of method of quencher up-conversion luminescence.
Background technology
Cooperative luminescence is the comparatively effective up-conversion luminescence of one.It is the luminescence produced by two or more lanthanide ion cooperation transition of the same race.The fluorescence cluster that cooperative luminescence is normally made up of adjacent very near lanthanide ion of the same race emits.In addition, by lanthanide ion of the same race (as Yb
3+) cluster that the forms ion that also other can be caused to have high level by cooperative sensitization produces up-conversion luminescence.Such as, by Yb
3+and Pb
2+codoped enters CaF
2in, excite at 980nm near infrared light and can to launch down ~ broadband ultraviolet the up-conversion luminescence of 382nm.
But cooperative luminescence likely becomes the obstacle affecting material and device performance in the application that some are important.Such as, Er is mixed high-power
3+in amplifier, if the Yb mixed altogether in material
3+ion defines ion pair or fluorescence cluster, under the exciting of 980nm laser, and Yb
3+ion pair and fluorescence cluster just have very high probability to produce cooperation transition, and by Yb
3+the 980nm photon energy of ionic absorption is launched with the form of high-energy photon, thus reduces Yb
3+ion is to Er
3+transmission ofenergy, cause mixing Er
3+image intensifer decrease in efficiency.
Summary of the invention
The object of this invention is to provide the method for the up-conversion luminescence that a kind of effective quencher is caused by cooperative effect, destroy fluorescence cluster particular by suitable cation doping, cause the structure deteriorate quencher of cluster fluorescence.Such as, at CaF
2: Yb
3+adulterate in cluster fluorescent material Y
3+ion, Y
3+ion is by displacement Yb
3+ion, Yb
3+fluorescence cluster is destroyed, and causes Yb
3+the structure destruction quencher of cluster fluorescence.
The present invention compared with prior art, under the exciting of 980nm light, CaF
2: Yb
3+cluster fluorescent material can be launched peak value and be positioned at Green upconversion luminescent near the ultraviolet conversion luminous of 343nm and 520nm.When in material doped with suitable metallic cation (as Y
3+, La
3+, Al
3+, Pb
2+deng) after, these two kinds of up-conversion luminescences all can weaken, until disappear.Such quenching of fluorescence method is non-existent in prior art.More precisely, the method for the structure quench fluorescence destroying fluorescence cluster is not passed through in prior art.Therefore, method provided by the invention has unique function and characteristic.
Advantage of the present invention is, destroys the structure of fluorescence cluster by mixing suitable positively charged ion, thus the up-conversion luminescence that quencher is relevant to fluorescence cluster.The positively charged ion mixed can be do not have the rare earth ion of fluorescent characteristic or the ion of other kind, and its effect is exactly substitute Yb in lattice
3+ion, destroys Yb
3+ion fluorescence cluster.The method can be avoided mixing ion and participate in transition process, and the physical process producing quenching of fluorescence is relatively simple; Utilize this quenching of fluorescence method, effectively can regulate the intensity of cooperative luminescence, also effectively can regulate the Up-conversion Intensity because cooperative sensitization produces.Therefore, this method for quenching has good use range.
The method of a kind of quencher up-conversion luminescence provided by the present invention not only can quencher Yb
3+the cooperative luminescence of ion, but also can effectively quencher by Yb
3+the up-conversion luminescence of ion cluster sensitization, is characterized in that:
(1) at inorganic Yb
3+mix except Yb in ion fluorescence cluster
3+outside other metallic cation, destroy the fluorophore clustering architecture in material, cause the structure deteriorate quencher of cluster fluorescence; Inorganic Yb
3+the matrix of ion fluorescence cluster is that alkaline-earth metal fluoride is (as CaF
2, SrF
2, BaF
2, MgF
2or ZnF
2); With whole metallic cation (Yb
3+metallic cation in ion, other metallic cation, alkaline-earth metal fluoride) volumetric molar concentration and be 100% calculating, trivalent group of the lanthanides ytterbium ion (Yb
3+) doping content be 0.05mol% ~ 10mol%, except Yb
3+the doping content of other metallic cation (not comprising the metallic cation in alkaline-earth metal fluoride) outside ion is 0.1mol% ~ 14mol%;
(2) under the exciting of 980nm near infrared light, the inorganic Yb of not doping
3+ion fluorescence cluster transmitting green Yb
3+the cooperation up-conversion luminescence of ion pair (~ 520nm, as shown in Figure 1) and ultraviolet cooperation up-conversion luminescence (~ 343nm, as shown in Figure 2).After other metallic cation mixes, above-mentioned two kinds of cooperation up-conversion luminescences can weaken and until disappear, produce the destructive quencher of obvious fluorophore clustering architecture;
(3) ion for quench fluorescence can be rare earth ion RE
3+(as Y
3+, La
3+, Lu
3+deng, but do not comprise Yb
3+with the metallic cation in alkaline-earth metal fluoride), transition-metal ion (Mn
2+, Cr
2+) or other main group metal ion (as Pb
2+, Al
3+deng).These cationic common traits are can displacement Yb in the material
3+ion, destroys Yb
3+ion fluorescence cluster.
Accompanying drawing explanation
Fig. 1: under 980nm laser excitation, CaF
2: 1%Yb
3+yb in sample
3+the cooperative luminescence spectrum of ion pair, probe temperature is 100K.
Fig. 2: under 980nm near infrared light excites, CaF
2: 1%Yb
3+ultraviolet conversion luminous spectrum.The peak value of spectrum is 343nm, and probe temperature is 13K.
Fig. 3: the Yb of different volumetric molar concentration of adulterating
3+during ion, CaF
2: x%Yb
3+green upconversion luminescent integrated intensity and Yb
3+the variation diagram of ion doping volumetric molar concentration, wherein, x=0.01,0.05,0.1,0.5,2,5,10.
Fig. 4: the Y of different volumetric molar concentration of adulterating
3+during ion, CaF
2: 2%Yb
3+, x%Y
3+greening collaboration up-conversion luminescence spectrum with Y
3+the variation diagram of ion doping volumetric molar concentration, wherein, x=0,0.5,1,2.
Fig. 5: the Y of different volumetric molar concentration of adulterating
3+during ion, CaF
2: 2%Yb
3+, x%Y
3+ultraviolet cooperation up-conversion luminescence spectrum with Y
3+the variation diagram of ion doping volumetric molar concentration, wherein, x=0,0.5,1,2.
Fig. 6: the Pb of different volumetric molar concentration of adulterating
2+during ion, CaF
2: 1%Yb
3+, x%Pb
2+greening collaboration up-conversion luminescence spectrum with Pb
2+the variation diagram of ion doping volumetric molar concentration, wherein, x=0,0.3,0.8,1,2,4,6.
Fig. 7: the Pb of different volumetric molar concentration of adulterating
2+during ion, CaF
2: 1%Yb
3+, x%Pb
2+ultraviolet cooperation up-conversion luminescence spectrum with Pb
2+the variation diagram of ion doping volumetric molar concentration, wherein, x=0,0.3,0.5,1,2,3,4.
Fig. 8: the Al of different volumetric molar concentration of adulterating
3+during ion, CaF
2: 2%Yb
3+, x%Al
3+greening collaboration up-conversion luminescence spectrum with Al
3+the variation diagram of ion doping volumetric molar concentration, wherein, x=0,0.1,0.5, Isosorbide-5-Nitrae, 9,14.
Fig. 9: the Al of different volumetric molar concentration of adulterating
3+during ion, CaF
2: 2%Yb
3+, x%Al
3+ultraviolet cooperation up-conversion luminescence spectrum with Al
3+the variation diagram of ion doping volumetric molar concentration, wherein, x=0,0.1,0.3,0.5,1,2,6,8.
Embodiment
Embodiment 1:
A certain amount of CaF is taken respectively according to mol ratio
2and YbF
3, contain into platinum or other non-corrosiveness crucible after fully grinding makes it mix, the vacuum environment being placed in 1450 DEG C is calcined 4 hours, takes out, obtain white mixed crystal material after naturally cooling to room temperature.Under the exciting of 980nm near infrared light, the CaF prepared under hot conditions
2: 0.5mol%Yb
3+mixed crystal material can launch bright green fluorescence; Spectroscopic analysis shows, this green fluorescence is from Yb
3+the cooperative luminescence of ion pair.Along with the reduction of probe temperature, greening collaboration luminescence is more and more stronger, and Fig. 1 is the emmission spectrum recorded under 100K low temperature.Under 13K low temperature, sample launches ultraviolet cooperative luminescence in UV spectrum district; Spectroscopic analysis shows, this Ultraluminescence is from Yb
3+the cooperative luminescence of triple ion, as shown in Figure 2.Repeat above-mentioned preparation, obtain the sample of different levels of doping, its Yb
3+the doping content of ion is respectively: 0.01mol%, 0.05mol%, 0.1mol%, 0.5mol%, 2mol%, 5mol%, 10mol%.Fig. 3 be under the exciting of 980nm near infrared light the luminous light intensity of greening collaboration along with Yb
3+the change of ion doping concentration; Result shows, works as Yb
3+when ion doping concentration is between 0.5mol% ~ 2mol%, cooperative luminescence intensity is maximum.
Embodiment 2:
Yb is prepared by coprecipitation method
3+(2mol%) and Y
3+the CaF of (0,0.5,1,2mol%) codoped
2powder.Testing the raw material adopted is Ca (NO
3)
2, Yb (NO
3)
3, Y (NO
3)
3and NH
4hF
2.First Yb (the NO of 0.5mol/L is mixed with
3)
3, 0.01mol/L Y (NO
3)
3, 0.5mol/L Ca (NO
3)
2standard aqueous solution.Stoichiometrically Yb (the NO of measured amounts
3)
3, Y (NO
3)
3with Ca (NO
3)
2solution is put in beaker and is stirred 30min, then solution is added drop-wise to NH
4hF
2the aqueous solution (15mol/L) in stir 1 hour, make it mix.Stirred mixed solution filter paper filters, gained precipitation after deionized water wash at 95 DEG C dry 12 hours, roasting 2 hours at 1200 DEG C, obtained a series of different Y
3+the CaF of doping molar fraction
2: Yb
3+, Y
3+sample.
XRD research shows, is CaF by matrix of materials prepared by aforesaid method
2, there is cubic crystal structure.XRD diffraction peak is very strong, and halfwidth is very narrow, and interpret sample all has good crystallization degree.The position of the diffraction peak of all samples and intensity all match with the data of standard card (PDF#35-0816), show that these materials are cubic crystal structure, and doping does not cause the change of cubic crystal structure.
Under 980nm optical excitation, we measure the CaF of four kinds of different doping
2: 2%Yb
3+, x%Y
3+the Room temperature emission spectra of sample, as shown in Figure 4 and Figure 5.Green upconversion luminescent in figure and ultraviolet conversion luminous respectively from Yb
3+ion pair and Yb
3+the cooperative luminescence of triple ion.Along with Y
3+mixing of ion increases with doping content, and cooperative luminescence weakens until disappear, and there occurs Fluorescence-quenching.Due to Y
3+ion is not fluoride ions, does not exist by Yb
3+ion is to Y
3+the transmission ofenergy of ion.These analyses show, this Fluorescence-quenching is derived from Y
3+to Yb
3+ion pair and Yb
3+the destruction of triple ion Cluster Structures.Work as Y
3+when the doping content of ion reaches 2mol%, Yb
3+the ultraviolet cooperative luminescence almost completely dissolve of triple ion; In other words, Y is worked as
3+when the doping content of ion reaches 2mol%, Yb
3+triple ion is almost all destroyed.
Embodiment 3:
Yb is prepared by coprecipitation method
3+(1mol%) and Pb
2+the CaF of (0,0.3,0.5,0.8,1,2,3,4,6mol%) codoped
2powder.Testing the raw material adopted is Ca (NO
3)
2, Yb (NO
3)
3, Pb (NO
3)
2and NH
4hF
2.First Yb (the NO of 0.5mol/L is mixed with
3)
3, 0.01mol/L Pb (NO
3)
2, 0.5mol/L Ca (NO
3)
2standard aqueous solution.Stoichiometrically Yb (the NO of measured amounts
3)
3, Pb (NO
3)
2with Ca (NO
3)
2solution is put in beaker and is stirred 30min, then solution is added drop-wise to NH
4hF
2the aqueous solution (15mol/L) in stir 1 hour, make it mix.Stirred mixed solution filter paper filters, gained precipitation after deionized water wash at 95 DEG C dry 12 hours, roasting 2 hours at 1200 DEG C, obtained a series of different Pb
2+the CaF of doping molar fraction
2: Yb
3+, Pb
2+sample.
Under 980nm optical excitation, we measure CaF
2: 0.5%Pb
2+and CaF
2: 1%Yb
3+, x%Pb
2+the visible region of (x=0,0.3,0.5,0.8,1,2,3,4) sample and ultraviolet region room temperature Up-conversion emission spectrum, as shown in Figure 6 and Figure 7.For the Yb that do not adulterate
3+ion and the 0.5%Pb that only adulterates
2+the sample CaF of ion
2: 0.5%Pb
2+, under 980nm near infrared light excites, do not find any luminescence, as shown in the solid-line curve in Fig. 7.Doped with 1%Yb
3+ion and a small amount of Pb
2+ion samples, has a ultraviolet cooperative luminescence peak near 343nm, in addition, has occurred that is derived from a Pb at 382nm place
2+the ultraviolet Up-conversion emission peak of ion; And the Yb that do not adulterate
3+the sample of ion does not have this Up-conversion emission peak.Work as Pb
2+when the doping content of ion is 0.5%, this emission peak reaches maximum value, as shown in Fig. 7 curve.Obviously, the emission peak being centrally located at 382nm is derived from 3 Yb
3+the common sensitization of ion.Along with Pb
2+the increase of ion doping concentration, two cooperative luminescence peaks all present the trend of monotonic decreasing, and ultraviolet cooperation emission peak is at Pb
2+ion doping concentration disappears when reaching 4%; Greening collaboration emission peak is at Pb
2+ion doping concentration disappears when reaching 6%.While ultraviolet cooperation emission peak disappears, Pb
2+the Up-conversion emission peak of ion also disappears, and presents obvious fluorophore clustering architecture destructive characteristics.
Embodiment 4:
Yb is prepared by coprecipitation method
3+(2mol%) and Al
3+the CaF of (0,0.1,0.3,0.5,1,2,4,6,8,9,14mol%) codoped
2powder.Testing the raw material adopted is Ca (NO
3)
2, Yb (NO
3)
3, Al (NO
3)
3and NH
4hF
2.First Yb (the NO of 0.5mol/L is mixed with
3)
3, 0.01mol/L Al (NO
3)
3, 0.5mol/L Ca (NO
3)
2standard aqueous solution.Stoichiometrically Yb (the NO of measured amounts
3)
3, Al (NO
3)
3with Ca (NO
3)
2solution is put in beaker and is stirred 30min, then solution is added drop-wise to NH
4hF
2the aqueous solution (15mol/L) in stir 1 hour, make it mix.Stirred mixed solution filter paper filters, gained precipitation after deionized water wash at 95 DEG C dry 12 hours, roasting 2 hours at 1200 DEG C, obtained a series of different al
3+the CaF of doping molar fraction
2: Yb
3+, Al
3+sample.
Under 980nm near infrared light excites, we measure CaF
2: 0.5%Al
3+and CaF
2: 2%Yb
3+, x%Al
3+the visible region of (x=0,0.1,0.3,0.5,1,2,4,6,8,9,14) sample and ultraviolet region room temperature Up-conversion emission spectrum, as shown in Figure 8 and Figure 9.For the Yb that do not adulterate
3+ion and the 0.5%Al that only adulterates
3+the sample CaF of ion
2: 0.5%Al
3+, under 980nm near infrared light excites, do not find any luminescence.Doped with 1%Yb
3+ion and a small amount of Al
3+ion samples, has a ultraviolet cooperative luminescence peak, occurs greening collaboration glow peak near 520nm near 343nm.Obviously, along with Al
3+the increase of ion doping concentration, two cooperative luminescence peaks all present the trend of monotonic decreasing.Ultraviolet cooperation emission peak is at Al
3+ion doping concentration disappears when reaching 8%; Greening collaboration emission peak is at Al
3+ion doping concentration disappears when reaching 14%, presents obvious fluorophore clustering architecture destructive characteristics.
Claims (5)
1. a method for quencher up-conversion luminescence, is characterized in that: at inorganic Yb
3+mix except Yb in ion fluorescence cluster
3+outside other metallic cation, destroy the fluorophore clustering architecture in material, thus cause the structure deteriorate quencher of cluster fluorescence; Inorganic Yb
3+the matrix of ion fluorescence cluster is alkaline-earth metal fluoride; With the volumetric molar concentration of whole metallic cation be 100% calculating, trivalent group of the lanthanides ytterbium ion Yb
3+doping content be 0.05mol% ~ 10mol%, except Yb
3+outside the doping content of other metallic cation be 0.1mol% ~ 14mol%.
2. the method for a kind of quencher up-conversion luminescence as claimed in claim 1, is characterized in that: alkaline-earth metal fluoride is CaF
2, SrF
2, BaF
2, MgF
2or ZnF
2.
3. the method for a kind of quencher up-conversion luminescence as claimed in claim 1, is characterized in that: except Yb
3+outside metallic cation be rare earth ion RE
3+, transition-metal ion or other main group metal ion, wherein RE
3+represent rare earth ion.
4. the method for a kind of quencher up-conversion luminescence as claimed in claim 3, is characterized in that: except Yb
3+outside metallic cation be Y
3+, La
3+, Lu
3+, Mn
2+, Cr
2+, Pb
2+or Al
3+.
5. the method for a kind of quencher up-conversion luminescence as claimed in claim 1, is characterized in that: quencher Yb
3+the cooperative luminescence of ion or quencher are by Yb
3+the up-conversion luminescence of ion cluster sensitization.
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Cited By (3)
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| CN105969347A (en) * | 2016-05-31 | 2016-09-28 | 吉林大学 | Method for acquiring up-conversion white light |
| CN106010538A (en) * | 2016-06-01 | 2016-10-12 | 中国计量大学 | Method for inhibiting concentration quenching effect in Yb/Er:NaGdF4 up-conversion luminescent nanocrystals |
| CN114479840A (en) * | 2021-12-28 | 2022-05-13 | 吉林大学 | Yb enhanced by zirconia modification3+Cluster cooperative luminescent material, preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105969347A (en) * | 2016-05-31 | 2016-09-28 | 吉林大学 | Method for acquiring up-conversion white light |
| CN106010538A (en) * | 2016-06-01 | 2016-10-12 | 中国计量大学 | Method for inhibiting concentration quenching effect in Yb/Er:NaGdF4 up-conversion luminescent nanocrystals |
| CN106010538B (en) * | 2016-06-01 | 2018-02-13 | 中国计量大学 | One kind is used to suppress Yb/Er:NaGdF4The method of concentration quenching effect in up-conversion luminescence nanometer crystal |
| CN114479840A (en) * | 2021-12-28 | 2022-05-13 | 吉林大学 | Yb enhanced by zirconia modification3+Cluster cooperative luminescent material, preparation method and application thereof |
| CN114479840B (en) * | 2021-12-28 | 2022-12-30 | 吉林大学 | Yb enhanced by zirconia modification 3+ Cluster cooperative luminescent material, preparation method and application thereof |
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