CN108865146A - A kind of up-conversion phosphor, preparation method and application emitting high-intensitive feux rouges - Google Patents
A kind of up-conversion phosphor, preparation method and application emitting high-intensitive feux rouges Download PDFInfo
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- CN108865146A CN108865146A CN201810938416.6A CN201810938416A CN108865146A CN 108865146 A CN108865146 A CN 108865146A CN 201810938416 A CN201810938416 A CN 201810938416A CN 108865146 A CN108865146 A CN 108865146A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—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
- C09K11/7772—Halogenides
- C09K11/7773—Halogenides with alkali or alkaline earth metal
Abstract
The invention discloses a kind of up-conversion phosphor for emitting high-intensitive feux rouges, the chemical expression of the up-conversion phosphor is NaLuF4:(1-x) Er/xTm, wherein the Lu:Er:Tm is 1:(1-x):X, x are 0~0.04.Application the invention also discloses the up-conversion phosphor of a kind of preparation method of up-conversion phosphor for emitting high-intensitive feux rouges and the transmitting high intensity feux rouges in fields such as solar battery, bio-imaging, solid state lasers.The present invention emits the up-conversion phosphor of high-intensitive feux rouges, by with NaLuF4As host material, Er3+It is used as sensitized ions and active ions, Tm simultaneously3+As energy capture center, can obtain under 980nm excitation with high-intensitive, high-purity red emission up-conversion.
Description
Technical field
The present invention relates to luminescent material technical field more particularly to a kind of up-conversion phosphor for emitting high-intensitive feux rouges,
The preparation method and applications of the up-conversion phosphor of the transmitting high intensity feux rouges.
Background technique
In recent years, since rear-earth-doped up-conversion is in bio-imaging, solar battery, anti-fake, 3D FPD etc.
There is huge application prospect in field, has received significant attention.Up-conversion can be by nonlinear optical process, by low energy
The exciting light of amount is converted into the transmitting light of high-energy.Relative to short-wavelength light (600nm or less), red spectral band (600-700nm)
With near infrared band (700-1100nm) due to being known as " optical window " with very strong biological tissue's penetrability.Due to
The excitation wavelength of 980nm is in biological window ranges, it is thus possible to depth penetrates biological tissue.However, up-conversion is logical
Often show multiple emission peaks.It falls into its emission peak in " optical window " range, can just make conversion material
Material is more efficiently applied to biological field.In addition, the luminous efficiency of up-conversion is low at present, this limits its significantly and practical answers
With.Therefore, it prepares with high-intensitive, high-purity red emission up-conversion, its reality in fields such as biologies is answered
With being of great significance.Traditional up-conversion is all with Yb3+As sensitized ions, and this mode is easy to cause concentration
Quenching effect.Developing a kind of becomes current luminescent material technology with high-intensitive, high-purity red emission up-conversion
The a great problem in field.
Summary of the invention
For overcome the deficiencies in the prior art, emit the upper of high-intensitive feux rouges one of the objects of the present invention is to provide a kind of
Conversion phosphor typically exhibits multiple emission peaks, the impure and intensity that shines to solve existing up-conversion and not enough etc. asks
Topic.
The second object of the present invention is to provide a kind of preparation method of up-conversion phosphor for emitting high-intensitive feux rouges, lead to
It crosses this method and prepares a kind of up-conversion phosphor for emitting high-intensitive feux rouges, typically exhibited with solving existing up-conversion
The problems such as multiple emission peaks, the inadequate impure and intensity that shines.
The third object of the present invention is to provide a kind of up-conversion phosphor of high-intensitive feux rouges of transmitting as described above
Application in fields such as solar battery, bio-imaging, solid state lasers exists to solve existing rear-earth-doped up-conversion
Influence its application because of the problems such as impure and intensity that shines is inadequate.
An object of the present invention adopts the following technical scheme that realization：
A kind of up-conversion phosphor emitting high-intensitive feux rouges, the chemical expression of the up-conversion phosphor are
NaLuF4:(1-x) Er/xTm, wherein the Lu:Er:Tm is 1:(1-x):X, x are 0~0.04.
Further, the x is 0.02.
The second object of the present invention adopts the following technical scheme that realization：
A kind of preparation method for the up-conversion phosphor emitting high-intensitive feux rouges, includes the following steps：
Prepare turbid solution：Based on volume parts, by 1~2 part of the citric acid solution of 1~4mol/L, the hydrogen-oxygen of 2~8mol/L
Change 1~2 part of sodium solution and 5~20 parts of deionized water are uniformly mixed so as to obtain mixed system, then sequentially adds nitric acid into mixed system
Lutetium solution, nitric acid bait solution and thulium nitrate solution, 8~33 parts of Fluorinse that 0.5~2mol/L is added after mixing, mix
Milky turbidity liquid is formed afterwards；
Hydro-thermal reaction：Hydro-thermal reaction 10h is carried out under the conditions of milky turbidity liquid is transferred to 200 DEG C, is made and has been reacted muddy
Turbid；
It isolates and purifies：It will react after turbid solution is successively centrifuged, washed, dried, and obtain emitting high-intensitive feux rouges
Up-conversion phosphor；
According to molar ratio computing, Lu in the milky turbidity liquid:Er:Tm is 1:(1-x):X, the x are 0~0.04.
Further, in preparing turbid solution step, 1.5 parts of citric acid solution by 2mol/L, the hydrogen of 4mol/L
1.25 parts of sodium hydroxide solution and 10 parts of deionized water are uniformly mixed so as to obtain mixed system.
Further, in preparing turbid solution step, the lutecium nitrate that 0.5~2mol/L is sequentially added into mixed system is molten
1 part of liquid, 0.96~1 part of the nitric acid bait solution of 0.5~2mol/L and the thulium nitrate solution 0~0.04 of 0.05~0.2mol/L
Part.
Further, in preparing turbid solution step, the lutecium nitrate solution 1 of 1mol/L is sequentially added into mixed system
Part, 0.02 part of thulium nitrate solution of 0.98 part of the nitric acid bait solution of 1mol/L and 1mol/L.
Further, 10 parts of Fluorinse that 1mol/L is added in preparing turbid solution step, after mixing.
Further, in the separation and purification step, it is described centrifugation be 10000r/min be centrifuged 10min, it is described washing for according to
Secondary alternately to be washed with water and alcohol, the drying dries 12h under the conditions of being 60 DEG C.
The third object of the present invention adopts the following technical scheme that realization：
A kind of up-conversion phosphor of the high-intensitive feux rouges of transmitting as described above is in solar battery, bio-imaging, solid
The application in the fields such as body laser.
Compared with prior art, the beneficial effects of the present invention are：
(1) a kind of up-conversion phosphor for emitting high-intensitive feux rouges of the present invention, by with NaLuF4As host material, Er3 +It is used as sensitized ions and active ions, Tm simultaneously3+As energy capture center, it can obtain that there is height under 980nm excitation
The up-conversion of intensity, high-purity red emission.
(2) a kind of preparation method for the up-conversion phosphor for emitting high-intensitive feux rouges of the present invention, citric acid as chelating agent,
Sodium hydroxide is used to adjust the pH value of solution, by the proportion of Lu ion, Er ion and Tm ion in adjusting solution, then passes through water
Thermal response prepares a kind of up-conversion phosphor with high intensity, high-purity red emission, and preparation process is simple, equipment cost
Low, easy to operate, non-environmental-pollution, short preparation period is suitble to produce in enormous quantities.
(3) a kind of up-conversion phosphor for emitting high-intensitive feux rouges of the present invention swashs in solar battery, bio-imaging, solid
The application in the fields such as light device, red spectral band (600-700nm) and near infrared band (700-1100nm) are due to very strong life
Object penetration into tissue is known as " optical window ".Since the excitation wavelength of 980nm is in biological window ranges, it is thus possible to
Depth penetrates biological tissue, therefore, the up-conversion phosphor that the present invention can be emitted to high-intensitive feux rouges are applied to bio-imaging
Field also can be used for solar cell power generation, solid state laser by the longer light of absorbing wavelength and the shorter light of launch wavelength
Equal fields.
Detailed description of the invention
Fig. 1 is hexagonal phase NaLuF prepared by embodiment 24:The X-ray diffractogram of (1-x) Er/xTm crystal；
Fig. 2 is the hexagonal phase NaLuF of embodiment 1-4 preparation4:(1-x) Er/xTm crystal is under the excitation of 980nm near infrared light
Up-conversion fluorescence spectrogram.
Specific embodiment
In the following, being described further in conjunction with attached drawing and specific embodiment to the present invention, it should be noted that not
Under the premise of conflicting, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
Hereinafter, by the preparation that the present invention emits the up-conversion phosphor of high-intensitive feux rouges is elaborated by Examples 1 to 4
Method and up-conversion phosphor obtained.
Embodiment 1
Prepare turbid solution：By 1.5mL concentration be 2mol/L citric acid solution, 1.25mL concentration be 4mol/L hydroxide
Sodium solution and 10mL deionized water stir 30min, obtain mixed system.0.5mL concentration is added into mixed system again is
The lutecium nitrate solution and 0.5mL concentration of 1mol/L is the nitric acid bait solution of 1mol/L, after stirring 30min, continues to add 10mL
Concentration is the Fluorinse of 1mol/L, continuously adds 6mL deionized water after being again stirring for 30min and stirs 30min, and cream is made
White opacity liquid.
Hydro-thermal reaction：Milky turbidity liquid is transferred in white bushing, it is then that 50 milliliters of white bushing loading is stainless
It puts baking oven in steel reaction kettle, after encapsulation into and carries out 200 DEG C hydro-thermal reaction 10 hours.
It isolates and purifies：Reacted turbid solution is successively carried out to 10000 revs/min twice of centrifugation, and each centrifugation time
For 10min, after being washed respectively with the alcohol of deionized water and 90%, dries 12 hours, that is, collect last in the environment of 60 DEG C
Powder sample, obtain up-conversion phosphor.
Embodiment 2
Prepare turbid solution：By 1.5mL concentration be 2mol/L citric acid solution, 1.25mL concentration be 4mol/L hydroxide
Sodium solution and 10mL deionized water stir 30min, obtain mixed system.0.5mL concentration is added into mixed system again is
The nitric acid bait solution and 0.05mL concentration that the lutecium nitrate solution of 1mol/L, 0.495mL concentration are 1mol/L are 0.1mol/L's
Thulium nitrate solution after stirring 30min, continues to add the Fluorinse that 10mL concentration is 1mol/L, it is subsequent to be again stirring for 30min
It is continuous that 6mL deionized water is added and stirs 30min, milky turbidity liquid is made.
Hydro-thermal reaction：Milky turbidity liquid is transferred in white bushing, it is then that 50 milliliters of white bushing loading is stainless
It puts baking oven in steel reaction kettle, after encapsulation into and carries out 200 DEG C hydro-thermal reaction 10 hours.
It isolates and purifies：Reacted turbid solution is successively carried out to 10000 revs/min twice of centrifugation, and each centrifugation time
For 10min, after being washed respectively with the alcohol of deionized water and 90%, dries 12 hours, that is, collect last in the environment of 60 DEG C
Powder sample, obtain up-conversion phosphor.
Embodiment 3
Prepare turbid solution：By 1.5mL concentration be 2mol/L citric acid solution, 1.25mL concentration be 4mol/L hydroxide
Sodium solution and 10mL deionized water stir 30min, obtain mixed system.0.5mL concentration is added into mixed system again is
The nitre that the nitric acid bait solution and 0.1mL concentration that the lutecium nitrate solution of 1mol/L, 0.49mL concentration are 1mol/L are 0.1mol/L
Sour thulium solution after stirring 30min, continues to add the Fluorinse that 10mL concentration is 1mol/L, continue after being again stirring for 30min
6mL deionized water is added and stirs 30min, milky turbidity liquid is made.
Hydro-thermal reaction：Milky turbidity liquid is transferred in white bushing, it is then that 50 milliliters of white bushing loading is stainless
It puts baking oven in steel reaction kettle, after encapsulation into and carries out 200 DEG C hydro-thermal reaction 10 hours.
It isolates and purifies：Reacted turbid solution is successively carried out to 10000 revs/min twice of centrifugation, and each centrifugation time
For 10min, after being washed respectively with the alcohol of deionized water and 90%, dries 12 hours, that is, collect last in the environment of 60 DEG C
Powder sample, obtain the up-conversion phosphor.
Embodiment 4
Prepare turbid solution：By 1.5mL concentration be 2mol/L citric acid solution, 1.25mL concentration be 4mol/L hydroxide
Sodium solution and 10mL deionized water stir 30min, obtain mixed system.0.5mL concentration is added into mixed system again is
The nitre that the nitric acid bait solution and 0.2mL concentration that the lutecium nitrate solution of 1mol/L, 0.48mL concentration are 1mol/L are 0.1mol/L
Sour thulium solution after stirring 30min, continues to add the Fluorinse that 10mL concentration is 1mol/L, continue after being again stirring for 30min
6mL deionized water is added and stirs 30min, milky turbidity liquid is made.
Hydro-thermal reaction：Milky turbidity liquid is transferred in white bushing, it is then that 50 milliliters of white bushing loading is stainless
It puts baking oven in steel reaction kettle, after encapsulation into and carries out 200 DEG C hydro-thermal reaction 10 hours.
It isolates and purifies：Reacted turbid solution is successively carried out to 10000 revs/min twice of centrifugation, and each centrifugation time
For 10min, after being washed respectively with the alcohol of deionized water and 90%, dries 12 hours, that is, collect last in the environment of 60 DEG C
Powder sample, obtain the up-conversion phosphor.
Effect test one
Up-conversion phosphor prepared by embodiment 2 is detected by X-ray diffraction, X-ray diffraction peak.Peak figure is shown in Fig. 1.
As can be seen from Figure, the hexagonal phase NaLuF at the X-ray diffraction peak of the sample and standard4Diffraction maximum (JCPDS27-
0726) it fits like a glove.
Effect test two
Four kinds of up-conversion phosphor (hexagonal phase NaLuF prepared by embodiment 1-44:Er/xTm) crystal is closely red in 980nm
Up-conversion fluorescence spectrogram under outer light excitation, is shown in Fig. 2.As seen from Figure 2, under 980nm excitation, by with NaLuF4As base
Material, Er3+It is used as sensitized ions and active ions, Tm simultaneously3+As energy capture center, Er can be greatly improved3+'s
660nm red Up-conversion Intensity simultaneously obtains high-purity red emission.Hexagonal phase NaLuF4It is a kind of efficient upper conversion base
Material, by with NaLuF4As host material, Er3+It is used as sensitized ions and active ions, Tm simultaneously3+As energy capture
Center can obtain under 980nm excitation with high-intensitive, high-purity red emission up-conversion.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (9)
1. a kind of up-conversion phosphor for emitting high-intensitive feux rouges, which is characterized in that the chemistry expression of the up-conversion phosphor
Formula is NaLuF4:(1-x) Er/xTm, wherein the Lu:Er:Tm is 1:(1-x):X, x are 0~0.04.
2. up-conversion phosphor as described in claim 1, which is characterized in that the x is 0.02.
3. a kind of preparation method for the up-conversion phosphor for emitting high-intensitive feux rouges, which is characterized in that include the following steps：
Prepare turbid solution：Based on volume parts, by 1~2 part of the citric acid solution of 1~4mol/L, the sodium hydroxide of 2~8mol/L
1~2 part of solution and 5~20 parts of deionized water are uniformly mixed so as to obtain mixed system, then to sequentially add into mixed system lutecium nitrate molten
Liquid, nitric acid bait solution and thulium nitrate solution, 8~33 parts of Fluorinse that 0.5~2mol/L is added after mixing, shape after mixing
At milky turbidity liquid；
Hydro-thermal reaction：Hydro-thermal reaction 10h is carried out under the conditions of milky turbidity liquid is transferred to 200 DEG C, is made and has been reacted turbid solution；
It isolates and purifies：To react after turbid solution is successively centrifuged, washed, dried, obtain emitting high-intensitive feux rouges upper turn
Change fluorescent powder；
According to molar ratio computing, Lu in the milky turbidity liquid:Er:Tm is 1:(1-x):X, the x are 0~0.04.
4. the preparation method of up-conversion phosphor as claimed in claim 3, which is characterized in that in preparing turbid solution step,
1.5 parts of citric acid solution by 2mol/L, 1.25 parts of the sodium hydroxide solution of 4mol/L and 10 parts of deionized water mixings
Obtain mixed system.
5. the preparation method of up-conversion phosphor as claimed in claim 3, which is characterized in that in preparing turbid solution step,
1 part of the lutecium nitrate solution of 0.5~2mol/L, the nitric acid bait solution 0.96~1 of 0.5~2mol/L are sequentially added into mixed system
Part and 0~0.04 part of thulium nitrate solution of 0.05~0.2mol/L.
6. the preparation method of up-conversion phosphor as claimed in claim 5, which is characterized in that in preparing turbid solution step,
1 part of the lutecium nitrate solution of 1mol/L, 0.98 part of the nitric acid bait solution of 1mol/L and 1mol/L are sequentially added into mixed system
0.02 part of thulium nitrate solution.
7. the preparation method of up-conversion phosphor as claimed in claim 3, which is characterized in that in preparing turbid solution step,
10 parts of Fluorinse that 1mol/L is added after mixing.
8. the preparation method of up-conversion phosphor as claimed in claim 3, which is characterized in that in the separation and purification step, institute
Stating centrifugation is that 10000r/min is centrifuged 10min, and successively alternately to be washed with water and alcohol, the drying is 60 DEG C of items for the washing
12h is dried under part.
9. a kind of as claimed in claim 1 or 2 up-conversion phosphor for emitting high-intensitive feux rouges solar battery, biology at
The application in the fields such as picture, solid state laser.
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| CN105670628A (en) * | 2016-01-19 | 2016-06-15 | 中山大学 | Up-conversion fluorescent powder with greatly improved red light and excellent monochromaticity and method for preparing up-conversion fluorescent powder |
| CN105713612A (en) * | 2016-01-19 | 2016-06-29 | 中山大学 | Up-conversion fluorescent powder with substantially increased red-green ratio and preparation method of up-conversion fluorescent powder with substantially increased red-green ratio |
| CN107722967A (en) * | 2017-10-31 | 2018-02-23 | 西安邮电大学 | It is a kind of to strengthen the method that red fluorescence is launched in ytterbium/holmium/cerium codope fluorine lutetium natrium nanocrystalline body |
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2018
- 2018-08-17 CN CN201810938416.6A patent/CN108865146A/en active Pending
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| US20150362432A1 (en) * | 2013-01-22 | 2015-12-17 | University Of Massachusetts Medical School | Compositions and methods for upconverting luminescence with engineered excitation and applications thereof |
| CN105670628A (en) * | 2016-01-19 | 2016-06-15 | 中山大学 | Up-conversion fluorescent powder with greatly improved red light and excellent monochromaticity and method for preparing up-conversion fluorescent powder |
| CN105713612A (en) * | 2016-01-19 | 2016-06-29 | 中山大学 | Up-conversion fluorescent powder with substantially increased red-green ratio and preparation method of up-conversion fluorescent powder with substantially increased red-green ratio |
| CN107722967A (en) * | 2017-10-31 | 2018-02-23 | 西安邮电大学 | It is a kind of to strengthen the method that red fluorescence is launched in ytterbium/holmium/cerium codope fluorine lutetium natrium nanocrystalline body |
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| Title |
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| HAN LIN ET AL.,: "Upconversion luminescence and Visible-Infrared Properties of β-NaLuF4:Er3+ Microcrystals Synthesized by the Surfactant-Assisted Hydrothermal Method", 《JOURNAL OF NANOMATERIALS》 * |
| WEI WEI ET AL.,: "Cross Relaxation Induced Pure Red Upconversion in Activator- and Sensitizer-Rich Lanthanide Nanoparticles", 《CHEM. MATER.》 * |
| XIUMEI YIN ET AL.,: "Single red up-conversion emission of Er3+, Tm3+ co-doped NaYF4 nano-particles under 1510 nm excitation", 《MATERIALS RESEARCH BULLETIN》 * |
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Application publication date: 20181123 |