CN103980903A - YPO4.0.8H2O crystal powder and preparation method thereof as well as method for improving luminescence property - Google Patents
YPO4.0.8H2O crystal powder and preparation method thereof as well as method for improving luminescence property Download PDFInfo
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- CN103980903A CN103980903A CN201410206360.7A CN201410206360A CN103980903A CN 103980903 A CN103980903 A CN 103980903A CN 201410206360 A CN201410206360 A CN 201410206360A CN 103980903 A CN103980903 A CN 103980903A
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Abstract
The invention discloses YPO4.0.8H2O crystal powder and a preparation method thereof as well as a method for improving luminescence property. The preparation method comprises the following steps: mixing and stirring a YNO3 solution and an EuNO3 solution, and then dropwise adding an NH4H2PO4 solution to form a liquid precursor; adjusting the pH value of the liquid precursor; transferring the liquid precursor to a reaction kettle after stirring, sealing and cooling after reacting at 120-180 DEG C; centrifuging, washing and drying to obtain the product; controlling the doping density of Eu<3+> at 12-22%, reacting with the NH4H2PO4 solution by using YNO3 and EuNO3 solutions to synthesize a hexagonal YPO4.0.8H2O crystal powder, and improving the luminescence property by a calcination method. The luminescence property can be greatly improved by virtue of a PL spectrogram. The YPO4.0.8H2O powder with the hexagonal structure is synthesized, and the YPO4.0.8H2O crystal powder is simple in preparation process, mild in synthesis condition, and beneficial to large-scale popularization.
Description
Technical field
The present invention relates to the preparation field of crystal powder, be specifically related to a kind of YPO
40.8H
2o crystal powder and preparation method thereof and luminescent properties method for improving.
Background technology
Rare earth ion is a huge mine of luminescent materials, and in the various luminescent materials of human development, rare earth element is being brought into play very important effect.Because rare earth element has special electron structure, make rare earth compound show the physics and chemistry performance of many uniquenesses, be used widely in many fields such as illumination, demonstration, information storage and medical radioactives.Wherein rare-earth phosphate phosphor is the important luminescent material of a class, has very high luminous efficiency under the exciting of vacuum-ultraviolet light, and chemical stability and good thermal stability, thereby has caused the favor of researcher.Y in rare earth yttrium phosphate
3+4f track be complete empty, thereby there is not f-f transition, so just can loss of energy, thereby there are the potentiality of the relative higher luminescent properties of other RE phosphate.
As everyone knows, the structure of crystal powder, pattern, doping all can affect its luminescent properties.For this reason, numerous investigators have done a large amount of trials at its pattern of control and structure aspects.Hua Lai etc. with different synthesis of surfactants the YPO of different-shape
40.8H
2o (Ceramics International, 2014,40 (1), 1885).Jiangchao Chen etc. utilizes the method for LSS (liquid-solid-solution) to synthesize YPO by changing ligand
4: xH
2o (x=0.5-1) (The Journal of PHysical Chemistry, 2013,117 (11), 5953).Up to now, also not by controlling Eu
3+the synthetic YPO of doping content
40.8H
2o crystal powder also promotes the relevant report of its luminescent properties by calcining.
Summary of the invention
The object of the invention is to overcome the shortcoming existing in above-mentioned prior art, a kind of YPO is provided
40.8H
2o crystal powder and preparation method thereof and luminescent properties method for improving, have synthesis condition gentleness, is conducive to the advantages such as spread.
For achieving the above object, the present invention is by the following technical solutions:
A kind of YPO
40.8H
2the preparation method of O crystal powder, comprises the following steps:
Step 1): join Y (NO
3)
3, Eu (NO
3)
3solution and NH
4h
2pO
4solution for standby;
Step 2): measure respectively Eu (NO
3)
3and Y (NO
3)
3taking mol ratio as (12-22): (88-78) mix, be uniformly mixed liquid and obtain Y
xeu
1-xnO
3solution, rear dropping NH
4h
2pO
4solution, and Y after dripping
xeu
1-xnO
3and NH
4h
2pO
4mol ratio be (1:1)-(2:1);
Step 3): regulating step 2) the pH value of mixing solutions of gained is to 0.5-3, after stirring, move on in reactor and seal, at 120 DEG C-180 DEG C reaction to producing precipitation, after by reactor cool to room temperature;
Step 4): by step 3) the throw out centrifugation that obtains, rear washing is dry, obtains by Eu
3+synthetic YPO
40.8H
2o crystal powder.
Described step 1) in, Y (NO
3)
3, Eu (NO
3)
3the preparation process of solution is: respectively by Y
2o
3and Eu
2o
3be dissolved in concentrated nitric acid, add after the unnecessary concentrated nitric acid of heat abstraction, add respectively deionized water to mix, being finally made into concentration is 0.2molL
-1y (NO
3)
3with concentration be 0.2molL
-1eu (NO
3)
3solution.
Described step 1) in, NH
4h
2pO
4the solvent of solution is deionized water, and concentration is 0.2molL
-1.
Described step 3) in to regulate the reagent of pH be that massfraction is rare nitric acid of 40%.
Described step 3), the churning time of mixing solutions is 40min.
Described step 3) in, reactor is stainless steel cauldron, and reactor volume compactedness is 60%-80%, step 3) in, the reaction times at 180 DEG C is 6h, the mode that cooling mode is naturally cooling.
Described step 4) in, washing drying process is: by obtain centrifugal after the dried up and washing with alcohol of throw out, the dry environment after having washed is: loft drier, the temperature of loft drier is 70 DEG C, be 12h time of drying.
A kind of YPO
40.8H
2the YPO that the preparation method of O crystal powder makes
40.8H
2the optical property method for improving of O crystal powder, by the YPO obtaining
40.8H
2after the calcining of O crystal powder, obtain the YPO of non-structure water
4matrix.
Described calcination environment is retort furnace, and calcining temperature is 200 DEG C-600 DEG C, calcination time 2-6h.
A kind of YPO
40.8H
2the YPO that the preparation method of O crystal powder makes
40.8H
2o crystal powder, Eu
3+doping content be 12%-22%, YPO
40.8H
2the structure of O powder is the structure with six side's phases.
The present invention has following beneficial effect: the prior art of comparing, the present invention is by adopting hydrothermal method, by controlling Eu
3+doping content be controlled at 12%-22%, utilize YNO
3and EuNO
3solution and NH
4h
2pO
4solution reaction synthesizes six side's phase YPO
40.8H
2o crystal powder also promotes its luminescent properties by method for calcinating.By YNO
3solution and EuNO
3after solution mix and blend, drip NH
4h
2pO
4solution, forms precursor liquid, regulates the pH value of precursor liquid; After stirring, precursor liquid is transferred in reactor to sealing, cool to room temperature after reaction at 120 DEG C-180 DEG C; Through centrifugal, washing, is dried and obtains product again.The sample obtaining, through calcining, can be found to its luminescent properties is without significantly improving before calcining by PL spectrogram.The present invention is by Eu
3+doping content be controlled at 12%-22% and synthesized the YPO with six side's phase structures
40.8H
2o powder, and can draw through spectrogram, by later stage thermal treatment, luminescent properties increases substantially.Preparation technology of the present invention is simple, and synthesis condition gentleness is environmentally friendly, is conducive to large-scale promotion.
Brief description of the drawings
Fig. 1 is Eu prepared by the present invention
3+doping content is 13% YPO
40.8H
2o powder X-ray RD collection of illustrative plates;
Fig. 2 is Eu prepared by the present invention
3+doping content is 13% YPO
40.8H
2o FE-SEM photo;
Fig. 3 is Eu prepared by the present invention
3+doping content is 13% YPO
40.8H
2o and calcined the PL spectrogram after 200 DEG C.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
A kind of YPO
40.8H
2the preparation method of O crystal powder: comprise the following steps:
Step 1): respectively by Y
2o
3and Eu
2o
3be dissolved in concentrated nitric acid, add after the unnecessary concentrated nitric acid of heat abstraction, add respectively deionized water and mix, being finally made into concentration is 0.2molL
-1y (NO
3)
3with concentration be 0.2molL
-1eu (NO
3)
3solution, by NH
4h
2pO
4be dissolved in that in deionized water, to be made into concentration be 0.2molL
-1nH
4h
2pO
4solution;
Step 2): measure respectively Eu (NO
3)
3and Y (NO
3)
3solution mixes, and Eu (NO
3)
3and Y (NO
3)
3mol ratio be (12-22): (88-78), be uniformly mixed liquid and obtain Y
xeu
1-xnO3 solution, rear dropping NH
4h
2pO
4solution, and Y after dripping
xeu
1-xnO3 and NH
4h
2pO
4mol ratio be (1:1)-(2:1);
Step 3): the rare nitric acid regulating step 2 that is 40% with massfraction) the pH value of mixing solutions of gained is to 0.5-3;
Step 4): step 3) mixing solutions of gained stirs after 40min, transfer in band teflon-lined stainless steel cauldron, and reactor volume compactedness is 60-%80%, encapsulation process, at 120 DEG C-180 DEG C reaction to produce precipitation capacity do not increase, after reactor is naturally cooled to room temperature;
Step 5): by step 4) the throw out centrifugation that obtains, by obtain centrifugal after the dried up and washing with alcohol of throw out three times, after wash, put in 70 DEG C of loft drier and be dried 12h, obtain by Eu
3+synthetic YPO
40.8H
2o crystal powder.
A kind of YPO
40.8H
2o crystal powder luminescent properties method for improving, by the YPO making
40.8H
2o crystal powder is positioned over 200 DEG C-600 DEG C calcining 2-6h in retort furnace, finally obtains the YPO of non-structure water
4matrix.
A kind of YPO
40.8H
2the YPO that the method for O crystal powder makes
40.8H
2o crystal powder, Eu
3+doping content be 12%-22%, YPO
40.8H
2the structure of O powder is the structure with six side's phases.
Be elaborated below in conjunction with embodiment:
Embodiment 1:
(1) get the 0.2molL of 19.575ml
-1y (NO
3)
3solution and Eu (NO
3)
3solution fully mixes, and Eu
3+doping content account for 12% of strength of solution;
(2) weigh 0.522 gram of NH
4h
2pO
4be dissolved in 18ml deionized water, be added dropwise in the mixing solutions of step (1) gained, stir 30min, ensure that it mixes;
(3) under agitation condition, regulate the pH=0.5 of mixing solutions with rare nitric acid;
(4) will after above-mentioned mixing solutions stirring 40min, transfer in the stainless steel cauldron with tetrafluoroethylene liner and seal, reactor compactedness be 60%, after reaction to precipitation does not increase at 180 DEG C, naturally cools to room temperature;
(5) by the throw out centrifugation obtaining, when centrifugal, rotating speed is 10000r/min, and centrifugation time is 5min, and washes throw out with water three times, and dry 12h in the loft drier of 70 DEG C is put in centrifugation, obtains YPO
40.8H
2o crystal powder;
In order further to strengthen YPO
40.8H
2the luminescent properties of O crystal powder, by the YPO obtaining
40.8H
2o crystal powder is positioned over 200 DEG C of calcining 6h in retort furnace, finally obtains the YPO of non-structure water
4matrix.
Embodiment 2:
(1) get the 0.2molL of 19.575ml
-1y (NO
3)
3solution and Eu (NO
3)
3solution fully mixes, Eu
3+doping content account for 17% of strength of solution;
(2) weigh 0.522 gram of NH
4h
2pO
4be dissolved in 18ml deionized water, be added dropwise in the mixing solutions of step (1) gained, stir 30min, ensure that it mixes;
(3) under agitation condition, regulate the pH=1 of mixing solutions with rare nitric acid;
(4) will after above-mentioned mixing solutions stirring 40min, transfer in the stainless steel cauldron with tetrafluoroethylene liner and seal, reactor compactedness be 60%, after reaction to precipitation does not increase at 160 DEG C, naturally cools to room temperature;
(5) by the throw out centrifugation obtaining, when centrifugal, rotating speed is 10000r/min, and centrifugation time is 5min, and washes throw out with water three times, and dry 12h in the loft drier of 70 DEG C is put in centrifugation, obtains YPO
40.8H
2o crystal powder;
In order further to strengthen YPO
40.8H
2the luminescent properties of O crystal powder, by the YPO obtaining
40.8H
2o crystal powder is positioned over 400 DEG C of calcining 4h in retort furnace, finally obtains the YPO of non-structure water
4matrix.
Embodiment 3:
(1) get the 0.2molL of 19.575ml
-1y (NO
3)
3solution and Eu (NO
3)
3solution fully mixes, Eu
3+doping content account for 22% of strength of solution;
(2) weigh 0.522 gram of NH
4h
2pO
4be dissolved in 18ml deionized water, be added dropwise in the mixing solutions of step (1) gained, stir 30min, ensure that it mixes;
(3) under agitation condition, regulate the pH=3 of mixing solutions with rare nitric acid;
(4) will after above-mentioned mixing solutions stirring 40min, transfer in the stainless steel cauldron with tetrafluoroethylene liner and seal, reactor compactedness be 60%, and at 180 DEG C, reaction to precipitation does not increase, and naturally cools to room temperature;
(5) by the throw out centrifugation obtaining, when centrifugal, rotating speed is 10000r/min, and centrifugation time is 5min, and washes throw out with water three times, centrifugation; After put into dry 12h in the loft drier of 70 DEG C, obtain YPO
40.8H
2o crystal powder;
In order further to strengthen YPO
40.8H
2the luminescent properties of O crystal powder, by the YPO obtaining
40.8H
2o crystal powder is positioned over 600 DEG C of calcining 2h in retort furnace, finally obtains the YPO of non-structure water
4matrix.
Embodiment 4:
(1) get the 0.2molL of 19.575ml
-1y (NO
3)
3solution and Eu (NO
3)
3solution fully mixes, Eu
3+doping content account for 13% of strength of solution; ;
(2) weigh 0.522 gram of NH
4h
2pO
4be dissolved in 18ml deionized water, be added dropwise in the mixing solutions of step (1) gained, stir 30min, ensure that it mixes.
(3) under agitation condition, regulate the pH=1 of mixing solutions with rare nitric acid;
(4) will after above-mentioned mixing solutions stirring 40min, transfer in the stainless steel cauldron with tetrafluoroethylene liner and seal, reactor compactedness be 60%, after reaction to precipitation does not increase at 180 DEG C, naturally cools to room temperature;
(5), by the throw out centrifugation obtaining, when centrifugal, rotating speed is 10000r/min,, centrifugation time is 5min, and washes throw out with water three times, centrifugation.Put into dry 12h in the loft drier of 70 DEG C, obtain YPO
40.8H
2o crystal powder.
In order further to strengthen YPO
40.8H
2the luminescent properties of O crystal powder, by the YPO obtaining
40.8H
2o crystal powder is positioned over 200 DEG C of calcining 2h in retort furnace, finally obtains the YPO of non-structure water
4matrix.
Fig. 1 utilizes the Eu that prepared by method described in the embodiment of the present invention 4
3+synthetic YPO when doping content is 13%
40.8H
2o crystal powder, all diffraction peaks position in figure can be all YPO with six sides mutually
40.8H
2(JCPDS Card42-0082) is corresponding for O standard diffracting spectrum, shows that prepared sample is YPO
40.8H
2o.
Fig. 2 utilizes the Eu that prepared by method described in the embodiment of the present invention 4
3+synthetic YPO when doping content is 13%
40.8H
2the field emission scanning electron microscope photo of O crystal powder.Can find out and work as Eu from this width figure
3+when doping content is 13%, product is club shaped structure, and length is approximately 1-2 μ m, the about 0.1-0.4 μ of diameter m.
Fig. 3 utilizes the Eu that prepared by method described in the embodiment of the present invention 4
3+synthetic YPO when doping content is 13%
40.8H
2o crystal powder (a) and calcined the PL spectrum of 200 DEG C (b).Main emission peak lays respectively at 590nm, 618nm, and 650nm and 697nm place, correspond respectively to Eu
3+'s
5d
0-
7f
j(J=1,2,34) transition, from scheming obviously can find out YPO
40.8H
2o crystal powder luminous intensity after calcining increases substantially.
The present invention adopts Hydrothermal Synthesis system, by controlling Eu
3+doping content synthesized the YPO with six side's phase structures
40.8H
2o powder, and after the calcination processing of 200 DEG C, its luminescent properties increases substantially.Preparation method of the present invention is simple, and synthesis condition gentleness is conducive to large-scale popularization.
The foregoing is only one embodiment of the present invention, is not unique embodiment, this area scientific research, and technician, by reading the present invention, not deviating from any equivalent transformation doing under this technological process, is claim of the present invention and contains.
Claims (10)
1. a YPO
40.8H
2the preparation method of O crystal powder, is characterized in that: comprise the following steps:
Step 1): join Y (NO
3)
3, Eu (NO
3)
3solution and NH
4h
2pO
4solution for standby;
Step 2): measure respectively Eu (NO
3)
3and Y (NO
3)
3taking mol ratio as (12-22): (88-78) mix, be uniformly mixed liquid and obtain Y
xeu
1-xnO
3solution, rear dropping NH
4h
2pO
4solution, and Y after dripping
xeu
1-xnO
3and NH
4h
2pO
4mol ratio be (1:1)-(2:1);
Step 3): regulating step 2) the pH value of mixing solutions of gained is to 0.5-3, after stirring, move on in reactor and seal, at 120 DEG C-180 DEG C reaction to producing precipitation, after by reactor cool to room temperature;
Step 4): by step 3) the throw out centrifugation that obtains, rear washing is dry, obtains by Eu
3+synthetic YPO
40.8H
2o crystal powder.
2. a kind of YPO according to claim 1
40.8H
2the preparation method of O crystal powder, is characterized in that: described step 1) in, Y (NO
3)
3, Eu (NO
3)
3the preparation process of solution is: respectively by Y
2o
3and Eu
2o
3be dissolved in concentrated nitric acid, add after the unnecessary concentrated nitric acid of heat abstraction, add respectively deionized water to mix, being finally made into concentration is 0.2molL
-1y (NO
3)
3with concentration be 0.2molL
-1eu (NO
3)
3solution.
3. a kind of YPO according to claim 1
40.8H
2the preparation method of O crystal powder, is characterized in that: described step 1) in, NH
4h
2pO
4the solvent of solution is deionized water, and concentration is 0.2molL
-1.
4. a kind of YPO according to claim 1
40.8H
2the preparation method of O crystal powder, is characterized in that: described step 3) in to regulate the reagent of pH be that massfraction is rare nitric acid of 40%.
5. a kind of YPO according to claim 1
40.8H
2the preparation method of O crystal powder, is characterized in that: described step 3), the churning time of mixing solutions is 40min.
6. a kind of YPO according to claim 1
40.8H
2the preparation method of O crystal powder, is characterized in that: described step 3) in, reactor is stainless steel cauldron, and reactor volume compactedness is 60%-80%, step 3) in, the reaction times at 180 DEG C is 6h, the mode that cooling mode is naturally cooling.
7. a kind of YPO according to claim 1
40.8H
2the preparation method of O crystal powder, it is characterized in that: described step 4) in, washing drying process is: by obtain centrifugal after the dried up and washing with alcohol of throw out, the dry environment after having washed is: loft drier, the temperature of loft drier is 70 DEG C, and be 12h time of drying.
8. according to a kind of YPO described in claim 1-7 any one
40.8H
2the YPO that the preparation method of O crystal powder makes
40.8H
2the luminescent properties method for improving of O crystal powder, is characterized in that: by the YPO obtaining
40.8H
2after the calcining of O crystal powder, obtain the YPO of non-structure water
4matrix.
9. a kind of YPO according to claim 8
40.8H
2the luminescent properties method for improving of O crystal powder, is characterized in that: described calcination environment is retort furnace, and calcining temperature is 200 DEG C-600 DEG C, calcination time 2-6h.
10. according to a kind of YPO described in claim 1-7 any one
40.8H
2the YPO that the preparation method of O crystal powder makes
40.8H
2o crystal powder, is characterized in that: Eu
3+doping content be 12%-22%, YPO
40.8H
2the structure of O powder is the structure with six side's phases.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104893726A (en) * | 2015-05-27 | 2015-09-09 | 陕西科技大学 | Self-assembly Eu<3+> doping YPO4 microspheres and preparation method thereof |
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CN101591539A (en) * | 2009-07-06 | 2009-12-02 | 浙江理工大学 | Preparation method of a rare earth phosphate LnPO4: ce, tb Green fluorescent powder |
CN103074064A (en) * | 2013-01-30 | 2013-05-01 | 东华大学 | Preparation method of rare-earth doped phosphate LnPO4:RE<3+> luminous nanoparticle |
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2014
- 2014-05-15 CN CN201410206360.7A patent/CN103980903A/en active Pending
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CN101591539A (en) * | 2009-07-06 | 2009-12-02 | 浙江理工大学 | Preparation method of a rare earth phosphate LnPO4: ce, tb Green fluorescent powder |
CN103074064A (en) * | 2013-01-30 | 2013-05-01 | 东华大学 | Preparation method of rare-earth doped phosphate LnPO4:RE<3+> luminous nanoparticle |
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Title |
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HEJUAN SONG ET AL: "EDTA-assisted hydrothermal synthesis, characterization, and luminescent properties of YPO4·nH2O:Eu3+(n = 0, 0.8) microflakes and microbundles", 《MATERIALS SCIENCE AND ENGINEERING B》, vol. 178, 21 June 2013 (2013-06-21) * |
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CN104893726A (en) * | 2015-05-27 | 2015-09-09 | 陕西科技大学 | Self-assembly Eu<3+> doping YPO4 microspheres and preparation method thereof |
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Application publication date: 20140813 |