CN105969358A - Gd<3+> ultraviolet up-conversion luminescent material and preparation method for same - Google Patents
Gd<3+> ultraviolet up-conversion luminescent material and preparation method for same Download PDFInfo
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7766—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing two or more rare earth metals
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Abstract
The invention discloses a Gd<3+> ultraviolet up-conversion luminescent material. A chemical general formula of the Gd<3+> ultraviolet up-conversion luminescent material is KGdxLu0.795-xYb0.2Tm0.005F4, wherein x is more than or equal to 0.3 and less than or equal to 0.795. The invention also provides a preparation method for the material. The preparation method comprises the following steps: 1, weighing a Lu<3+>-containing compound, a Gd<3+>-containing compound, a Yb<3+>-containing compound and a Tm<3+>-containing compound according to a stoichiometric ratio respectively; 2, dispersing the Lu<3+>-containing compound, the Gd<3+>-containing compound, the Yb<3+>-containing compound and the Tm<3+>-containing compound in de-ionized water, adding nitric acid, and performing heating to obtain an RE(NO3)3 solution; 3, weighing KF according to a stoichiometric ratio of F-:RE<3+> of (6-10):1, and dissolving the KF in de-ionized water to obtain a KF solution; 4, adding dropwise the KF solution into the RE(NO3)3 solution to obtain a white turbid solution with stirring; 5, transferring the white turbid solution into a reaction kettle, and preserving heat for 1 to 20h at 150 to 200 DEG C; 6, cooling a product obtained in step 5 to room temperature, performing centrifugation to obtain white precipitates, washing the white precipitates, and performing drying under a vacuum condition.
Description
Technical field
The present invention relates to field of light emitting materials, it is provided that a kind of Gd3+Ultraviolet conversion luminous material and preparation method thereof.
Background technology
The report of up-conversion luminescence has been occurred as soon as far back as nineteen fifty-nine.Up-conversion luminescence, it may be assumed that anti-Stokes luminescence (Anti-Stokes),
Refer to utilize the light of long wavelength, during exciting irradiation luminescent material, launch the light conversion phenomena of the light of short wavelength.Up-conversion luminescence
The main application of material is infrared acquisition, and upconversion laser, 3 D stereo show, biological fluorescent labelling, the aspect such as false proof.
Up-conversion luminescence host material is mainly the material of low phonon energy, and such as fluoride, halogenide, oxyfluoride etc., low
Phonon contributes to reducing radiationless relaxation rate and improves up-conversion luminescence efficiency.Fluoride particularly hexagonal phase NaYF4Study more,
Hexagonal phase NaYF4The upper conversion host material that the upper conversion efficiency that is well recognized as is the highest.It is related to hexagonal phase NaLuF in recent years4:Yb3+,
Tm3+Report, under 980nm excites, can produce strong ultraviolet and blue up-conversion luminous (CrystEngComm, 2011,
13,3782-3787).About Gd3+Infrared sharp lower ultraviolet Up-conversion emission (Opt.Lett.2008,33,857-859) rarely has report.
Gd3+Relatively big (the about 32,000cm of first excited state and ground state energy difference-1), it is commonly used as matrix ion.Additionally, Gd3+Can
Contrast medium as magnetic resonance (MRI) imaging.
Explore novel Gd3+Ultraviolet conversion luminous material is also developed its application and can be widened rare earth luminescent material research range, improves
Conversion luminous mechanism, is a new research direction.
Summary of the invention
It is an object of the invention to overcome the shortcoming of prior art, it is provided that a kind of Gd3+Ultraviolet conversion luminous material and preparation side thereof
Method.
For solving above-mentioned technical problem, present invention employs techniques below measure:
A kind of Gd3+Ultraviolet conversion luminous material, it is rice krispies flower-shaped nanoscale fluoride, and chemical general formula is:
KGdxLu0.795-xYb0.2Tm0.005F4(1), wherein, 0.3≤x≤0.795.
Further, described Gd3+Ultraviolet conversion luminous material is cubic system, has α-NaGdF4Structure.
Further, described Gd3+Ultraviolet conversion luminous material is positioned at infrared 980nm laser excitation, Up-conversion emission peak
In the range of 250nm to 850nm.
Further, described Gd3+Ultraviolet conversion luminous material, under infrared 980nm laser excitation, has Gd3+In ultraviolet
Switching emission and Tm3+Up-conversion emission.
A kind of above-mentioned Gd3+The preparation method of ultraviolet conversion luminous material, comprises the following steps:
S1, weighs containing Lu according to the stoichiometric proportion in formula (1) respectively3+Compound, containing Gd3+Compound, containing Yb3+
Compound and containing Tm3+Compound；
S2, by Lu3+Compound, containing Gd3+Compound, containing Yb3+Compound and containing Tm3+Compound be scattered in
In deionized water, and add nitric acid post-heating, it is thus achieved that RE (NO3)3Solution；
S3, stoichiometrically F-:RE3+=6～10:1 weigh KF, are dissolved in deionized water, form KF solution；
S4, under conditions of stirring, by KF solution with being added dropwise over RE (NO3)3In solution, obtain white turbid solution；
S5, transfers in reactor by described white turbid solution, is incubated 1～20h at 150～200 DEG C；And
S6, after the product that step S5 obtains is cooled to room temperature, centrifugal acquisition white precipitate, cleans described white precipitate vacuum
Lower dry.
Further, step S2 farther includes,
S21, adds deionized water and heats；And
S22, repeat the above steps 2-4 time.
Further, stoichiometrically F-:RE3+=7～9:1 weigh KF.
Further, in step s 5, at 170～190 DEG C, it is incubated 10～15h.
Further, the step of described cleaning white precipitate includes cleaning 2～4 times with deionized water respectively, and uses ethanol purge 1-2
Secondary.
Further, Lu3+Compound, containing Gd3+Compound, containing Yb3+Compound and containing Tm3+Compound respectively
For the oxide containing above-mentioned ion.
The Gd that the present invention provides3+Ultraviolet conversion luminous material and preparation thereof have the advantage that one, the Gd of the present invention3+
Ultraviolet conversion luminous material 980nm laser excitation, can be observed to launch wavelength and is positioned at the rare earth of 250nm to 850nm
Gd3+Ultraviolet and Tm3+Ultraviolet-visible-infrared up conversion luminous；Its two, the preparation method of the present invention is with water as reaction media
Hydro-thermal method, the method is green, and environmental protection simply, easily operates, easily batch synthetic material.
Accompanying drawing explanation
Fig. 1 is that the present invention prepares Gd3+The method flow diagram of ultraviolet conversion luminous material.
The various KGd that Fig. 2 provides for the embodiment of the present inventionxLu0.795-xYb0.2Tm0.005F4The XRD figure of sample.
The KGd that Fig. 3 provides for one embodiment of the invention0.3Lu0.495Yb0.2Tm0.005F4Stereoscan photograph.
The KGd that Fig. 4 provides for one embodiment of the invention0.3Lu0.495Yb0.2Tm0.005F4Sample under infrared 980nm excites upper turn
Change emission spectrum.
The KGd that Fig. 5 provides for one embodiment of the invention0.3Lu0.495Yb0.2Tm0.005F4Sample exciting under infrared 980nm excites
Power relies on Up-conversion emission spectrum.
The KGd that Fig. 6 provides for another embodiment of the present invention0.795Yb0.2Tm0.005F4The stereoscan photograph of sample.
The KGd that Fig. 7 provides for another embodiment of the present invention0.795Yb0.2Tm0.005F4The sample upper conversion under infrared 980nm excites
Emission spectrum.
Detailed description of the invention
With detailed description of the invention, the present invention is described in further detail below in conjunction with the accompanying drawings.
The embodiment of the present invention provides a kind of Gd3+Ultraviolet conversion luminous material, it is rice krispies flower-shaped nanoscale fluoride, and chemistry is logical
Formula is:
KGdxLu0.795-xYb0.2Tm0.005F4(1), wherein, 0.3≤x≤0.795.
Wherein, described Gd3+Ultraviolet conversion luminous material is cubic system, has α-NaGdF4Structure.
Described Gd3+Ultraviolet conversion luminous material is positioned at 250nm to 850 at infrared 980nm laser excitation, Up-conversion emission peak
In the range of nm.It addition, described Gd3+Ultraviolet conversion luminous material, under infrared 980nm laser excitation, has Gd3+Ultraviolet
Up-conversion emission and Tm3+Up-conversion emission.
Refer to Fig. 1, the embodiment of the present invention provides and also provides for a kind of above-mentioned Gd3+The preparation method of ultraviolet conversion luminous material,
Comprise the following steps:
S1, weighs containing Lu according to the stoichiometric proportion in formula (1) respectively3+Compound, containing Gd3+Compound, containing Yb3+
Compound and containing Tm3+Compound；
S2, by Lu3+Compound, containing Gd3+Compound, containing Yb3+Compound and containing Tm3+Compound be scattered in
In deionized water, and add nitric acid post-heating, it is thus achieved that RE (NO3)3Solution；
S3, stoichiometrically F-:RE3+=6～10:1 weigh KF, are dissolved in deionized water, form KF solution；
S4, under conditions of stirring, by KF solution with being added dropwise over RE (NO3)3In solution, obtain white turbid solution；
S5, transfers in reactor by described white turbid solution, is incubated 1～20h at 150～200 DEG C；And
S6, after the product that step S5 obtains is cooled to room temperature, centrifugal acquisition white precipitate, cleans described white precipitate vacuum
Lower dry.
In step sl, Lu3+Compound, containing Gd3+Compound, containing Yb3+Compound and containing Tm3+Compound
It is respectively the oxide containing above-mentioned ion.
Step S2 farther includes,
S21, adds deionized water and heats；And
S22, repeat the above steps 2-4 time.
In step s3, it is preferred that stoichiometrically F-:RE3+=7～9:1 weigh KF.
In step s 5, it is preferred that at 170～190 DEG C, be incubated 10～15h.
In step s 6, it is preferred that the step of described cleaning white precipitate includes cleaning 2～4 times with deionized water, and use respectively
Ethanol purge 1-2 time.
This example uses rare earth oxide Lu2O3(99.99%), Gd2O3(99.99%), Yb2O3(99.99%), Tm2O3
(99.99%) prepare the rare earth nitrate used in each embodiment in the present invention as raw material, rare earth oxide is bought and is jumped from Chinese Shanghai
Dragon new material company limited.KF (99.9%), HNO3(A.R.) buy from Chemical Reagent Co., Ltd., Sinopharm Group of China.
Embodiment 1
KGd0.3Lu0.495Yb0.2Tm0.005F4Preparation
Stoichiometrically according to molecular formula KGd0.3Lu0.495Yb0.2Tm0.005F4Weigh a certain amount of reagent: 0.99mmol
Lu2O3, 0.60mmol Gd2O3, 0.40mmol Yb2O3, 0.01mmol Tm2O3；By load weighted raw material with deionized water
Dispersion, adds HNO3, heating, add deionized water, heating, the most repeatedly for three times, be finally configured to 15mL RE (NO3)3；
Weigh 32mmol KF (99.9%), be made into 20mL KF solution；Gained KF solution is added dropwise over magnetic agitation RE (NO3)3
In solution, obtain white turbid solution；By gained turbid solution magnetic agitation 15min；White turbid solution is transferred to 50mL
In politef stainless steel cauldron, 180 DEG C, keep 12h；Question response still is cooled to room temperature, the supernatant is outwelled,
By 7000 revs/min of deionized water wash white precipitates of centrifuge 3 times, washing with alcohol 1 time, in vacuum drying oven, 60 DEG C are dried
12h, obtains target luminescent material and is KGd0.3Lu0.495Yb0.2Tm0.005F4Up-conversion luminescent material.
Embodiment 2
KGd0.5Lu0.295Yb0.2Tm0.005F4Preparation
Stoichiometrically according to molecular formula KGd0.5Lu0.295Yb0.2Tm0.005F4Weigh a certain amount of reagent: 0.59mmol
Lu2O3, 1.00mmol Gd2O3, 0.40mmol Yb2O3, 0.01mmol Tm2O3；By load weighted raw material with deionized water
Dispersion, adds HNO3, heating, add deionized water, heating, the most repeatedly for three times, be finally configured to 15mL RE (NO3)3；
Weigh 32mmol KF (99.9%), be made into 20mL KF solution；Gained KF solution is added dropwise over magnetic agitation RE (NO3)3
In solution, obtain white turbid solution；By gained turbid solution magnetic agitation 15min；White turbid solution is transferred to 50mL
In politef stainless steel cauldron, 180 DEG C, keep 12h；Question response still is cooled to room temperature, the supernatant is outwelled,
By 7000 revs/min of deionized water wash white precipitates of centrifuge 3 times, washing with alcohol 1 time, in vacuum drying oven, 60 DEG C are dried
12h, obtains target luminescent material and is KGd0.3Lu0.495Yb0.2Tm0.005F4Up-conversion luminescent material.
Embodiment 3
KGd0.7Lu0.095Yb0.2Tm0.005F4Preparation
Stoichiometrically according to molecular formula KGd0.5Lu0.295Yb0.2Tm0.005F4Weigh a certain amount of reagent: 0.19mmol
Lu2O3, 1.40mmol Gd2O3, 0.40mmol Yb2O3, 0.01mmol Tm2O3；By load weighted raw material with deionized water
Dispersion, adds HNO3, heating, add deionized water, heating, the most repeatedly for three times, be finally configured to 15mL RE (NO3)3；
Weigh 32mmol KF (99.9%), be made into 20mL KF solution；Gained KF solution is added dropwise over magnetic agitation RE (NO3)3
In solution, obtain white turbid solution；By gained turbid solution magnetic agitation 15min；White turbid solution is transferred to 50mL
In politef stainless steel cauldron, 180 DEG C, keep 12h；Question response still is cooled to room temperature, the supernatant is outwelled,
By 7000 revs/min of deionized water wash white precipitates of centrifuge 3 times, washing with alcohol 1 time, in vacuum drying oven, 60 DEG C are dried
12h, obtains target luminescent material and is KGd0.3Lu0.495Yb0.2Tm0.005F4Up-conversion luminescent material.
Embodiment 4
Molecular formula: KGd0.795Yb0.2Tm0.005F4
Stoichiometrically according to molecular formula KGd0.5Lu0.295Yb0.2Tm0.005F4Weigh a certain amount of reagent: 1.59mmol
Gd2O3, 0.40mmol Yb2O3, 0.01mmol Tm2O3；Load weighted raw material is disperseed with deionized water, adds HNO3,
Heating, adds deionized water, heating, the most repeatedly for three times, is finally configured to 15mL RE (NO3)3；Weigh 32mmol KF
(99.9%) 20mL KF solution, it is made into；Gained KF solution is added dropwise over magnetic agitation RE (NO3)3In solution, obtain
White turbid solution；By gained turbid solution magnetic agitation 15min；White turbid solution is transferred to 50mL politef
In stainless steel cauldron, 180 DEG C, keep 12h；Question response still is cooled to room temperature, the supernatant is outwelled, with centrifuge 7000
Rev/min deionized water wash white precipitate 3 times, washing with alcohol 1 time, in vacuum drying oven, 60 DEG C of dry 12h, obtain mesh
Mark luminescent material is KGd0.3Lu0.495Yb0.2Tm0.005F4Up-conversion luminescent material.
As can be seen from Figure 2: each sample KGdxLu0.795-xYb0.2Tm0.005F4Diffraction maximum and standard JCPDS 27-0697
Emission in Cubic NaGdF4The intrinsic characteristic diffraction peak of card is basically identical, illustrate the material of synthesis for and Emission in Cubic NaGdF4Isomorphism
Emission in Cubic KGd0.3Lu0.495Yb0.2Tm0.005F4；Standard of comparison spectrum JCPDS 27-0697, the XRD of synthetic composes along with x
Increase i.e. Gd3+Content increase is moved to little angular direction.K+Radius is more than Na+Radius, therefore sample XRD moves to little angular direction.
Lu simultaneously3+Radius is less than Gd3+Radius, so that with Lu3+The i.e. x of content minimizing increases, and diffraction maximum moves to little angle.Additionally, also
Occur without other diffraction maximum, the KGd synthesized by explanationxLu0.795-xYb0.2Tm0.005F4It it is pure Emission in Cubic.
Fig. 3 is the scanning electron microscope FE-SEM picture of this embodiment sample, it will thus be seen that synthesis KGd0.3Lu0.495Yb0.2Tm0.005F4
Sample is the flower-shaped nano-particle of rice krispies.
Fig. 4 is the Up-conversion emission spectrum of this embodiment sample, as can be seen from the figure: under 980nm is infrared ray excited,
KGd0.3Lu0.495Yb0.2Tm0.005F4Sample can detect that the up-conversion luminescence of 250nm to 850nm.Up-conversion emission spectrum is observed
To being positioned at the ultraviolet conversion luminous of 277nm and 313nm, derive from Gd3+'s6IJ→8S7/2And6P7/2→8S7/2Transition.
The strong up-conversion luminescence being positioned at 476nm and 802nm derives from Tm3+'s1G4→3H6And3H4→3H6Transition.Weak
The light sources being positioned at 650nm in Tm3+'s1G4→3F4Transition.It is positioned at the purple of 290nm, 350nm and 365nm
Outside upper conversion light sources is in Tm3+'s1I6→3H6,1I6→3F4And1D2→3H6Transition luminescence..
Fig. 5 is the exciting power dependence Up-conversion emission spectrum of this embodiment sample, as can be seen from the figure: same sample, along with
The increase of exciting power, under 980nm excites, Gd3+Ultraviolet and Tm3+Ultraviolet-visible-infrared up conversion is transmitted in enhancing.
Fig. 6 is the scanning electron microscope FE-SEM picture of this embodiment sample, for the flower-shaped nano-particle of rice krispies.Contrast
KGd0.3Lu0.495Yb0.2Tm0.005F4FE-SEM Fig. 3 of sample, granular size increased, and Gd is described3+When content increases,
Granule becomes big.
Fig. 7 is the Up-conversion emission spectrum of this embodiment sample, is visually observed bright bluish violet up-conversion luminescence.Right
Compare KGd0.3Lu0.495Yb0.2Tm0.005F4The Up-conversion emission spectrogram 4, Gd of sample3+Ultraviolet conversion luminous die down, explanation
Gd3+When increasing to a certain extent, it is unfavorable for obtaining its up-conversion luminescence.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all spirit in the present invention and former
Within then, any modification, equivalent substitution and improvement etc. done, within should be included in the scope of protection of the invention.
Claims (10)
1. a Gd3+Ultraviolet conversion luminous material, it is characterised in that: described Gd3+Ultraviolet conversion luminous material is that rice krispies is flower-shaped to be received
Meter level fluoride, its chemical general formula is:
KGdxLu0.795-xYb0.2Tm0.005F4(1), wherein, 0.3≤x≤0.795.
Gd the most according to claim 13+Ultraviolet conversion luminous material, it is characterised in that: described Gd3+Ultraviolet conversion luminous
Material is cubic system, has α-NaGdF4Structure.
Gd the most according to claim 13+Ultraviolet conversion luminous material, it is characterised in that: described Gd3+Ultraviolet conversion luminous
Material is in infrared 980nm laser excitation, in the range of Up-conversion emission peak is positioned at 250nm to 850nm.
Gd the most according to claim 13+Ultraviolet conversion luminous material, it is characterised in that: described Gd3+Ultraviolet conversion luminous
Material, under infrared 980nm laser excitation, has Gd3+Ultraviolet Up-conversion emission and Tm3+Up-conversion emission.
5. a Gd as claimed in claim 13+The preparation method of ultraviolet conversion luminous material, it is characterised in that include following step
Rapid:
S1, weighs containing Lu according to the stoichiometric proportion in formula (1) respectively3+Compound, containing Gd3+Compound, containing Yb3+
Compound and containing Tm3+Compound；
S2, by Lu3+Compound, containing Gd3+Compound, containing Yb3+Compound and containing Tm3+Compound be scattered in
In deionized water, and add nitric acid post-heating, it is thus achieved that RE (NO3)3Solution；
S3, stoichiometrically F-:RE3+=6～10:1 weigh KF, are dissolved in deionized water, form KF solution；
S4, under conditions of stirring, by KF solution with being added dropwise over RE (NO3)3In solution, obtain white turbid solution；
S5, transfers in reactor by described white turbid solution, is incubated 1～20h at 150～200 DEG C；And
S6, after the product that step S5 obtains is cooled to room temperature, centrifugal acquisition white precipitate, cleans described white precipitate vacuum
Lower dry.
Preparation method the most according to claim 5, it is characterised in that: step S2 farther includes,
S21, adds deionized water and heats；And
S22, repeat the above steps 2-4 time.
Preparation method the most according to claim 5, it is characterised in that: stoichiometrically F-:RE3+=7～9:1 weigh KF.
Preparation method the most according to claim 5, it is characterised in that: in step s 5, at 170～190 DEG C, it is incubated 10～15
h。
Preparation method the most according to claim 5, it is characterised in that: the step of described cleaning white precipitate include spending respectively from
Sub-water cleans 2～4 times, and with ethanol purge 1-2 time.
Preparation method the most according to claim 1, it is characterised in that: Lu3+Compound, containing Gd3+Compound, containing Yb3+
Compound and containing Tm3+Compound be respectively containing the oxide of above-mentioned ion.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965112A (en) * | 2012-12-07 | 2013-03-13 | 东北林业大学 | Intense ultraviolet up-converting micron fluoride material and preparation method thereof |
| CN103846097A (en) * | 2013-11-27 | 2014-06-11 | 上海大学 | NaLuF4:Gd, Yb, Tm/TiO2 nano composite material and preparation method thereof |
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2016
- 2016-05-11 CN CN201610307762.5A patent/CN105969358B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965112A (en) * | 2012-12-07 | 2013-03-13 | 东北林业大学 | Intense ultraviolet up-converting micron fluoride material and preparation method thereof |
| CN103846097A (en) * | 2013-11-27 | 2014-06-11 | 上海大学 | NaLuF4:Gd, Yb, Tm/TiO2 nano composite material and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| L. W. YANG ET AL.: "Magnetic and upconverted luminescent properties of multifunctional lanthanide doped cubic KGdF4 nanocrystals", 《NANOSCALE》 * |
| WEIYE SONG ET AL.: "Ultraviolet Upconversion Emissions of Gd3+ in β-NaLuF4:Yb3+,Tm3+,Gd3+ Nanocrystals", 《JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY》 * |
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