CN104830339A - Method for converting rare-earth-doped YPO4 (yttrium phosphate) crystal from hexagonal phase to tetragonal phase and improving luminescence property of rare-earth-doped YPO4 crystal - Google Patents

Method for converting rare-earth-doped YPO4 (yttrium phosphate) crystal from hexagonal phase to tetragonal phase and improving luminescence property of rare-earth-doped YPO4 crystal Download PDF

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CN104830339A
CN104830339A CN201510278354.7A CN201510278354A CN104830339A CN 104830339 A CN104830339 A CN 104830339A CN 201510278354 A CN201510278354 A CN 201510278354A CN 104830339 A CN104830339 A CN 104830339A
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earth
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tetragonal
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CN104830339B (en
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刘运
李朋
王晨昱
郭雅欣
史晓磊
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Shaanxi University of Science and Technology
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Abstract

The invention relates to a method for converting a rare-earth-doped YPO4 (yttrium phosphate) crystal from hexagonal phase to tetragonal phase and improving a luminescence property of the rare-earth-doped YPO4 crystal. The method includes the steps of synthesizing a hexagonal-phase rare-earth-Eu-ion-doped YPO4 crystal by means of adopting a water heating method and taking Na3cit or EDTA (ethylene diamine tetraacetic acid) as a chelating agent; regulating proportion of PO4<3->, RE<3+> and Cit<3->/ the EDTA in a reaction solution to obtain the YPO4; performing controllable conversion of crystalline phase from the hexagonal phase to the tetragonal phase of the Eu crystal. The method has the advantages that the luminescence property of the YPO4 is improved substantially, crystalline phase conversion of the YPO4 crystal is achieved by the water heating method, operation is simple, the Eu-doped YPO4 crystals in different crystalline phases can be synthesized selectively, the tetragonal-phase Eu-doped YPO4 crystal is higher than the hexagonal-phase rare-earth-Eu-ion-doped YPO4 crystal in luminescence property, and the method is suitable for extensive popularization.

Description

A kind of rear-earth-doped YPO 4crystal crystalline phase is from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof
Technical field
The invention belongs to rare earth luminescent material preparing technical field, be specifically related to a kind of rear-earth-doped YPO 4crystal crystalline phase is from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof.
Background technology
Rare earth luminescent material occupies very consequence in whole solid luminescence field, because special electron structure makes rare earth element have the incomparable character of general element.In recent years, because have the advantages such as receptivity is strong, luminosity is high, synthesis temperature is moderate, RE phosphate was widely used at illumination, quantum optics, colour television set and thermoluminescence detection field, caused researcher interest widely.
YPO 4in RE phosphate, occupy critical role, be widely used in the doped substrate of rare earth ion.According to the difference of synthesis condition and synthetic method, yttrium phosphate (YPO 4) two kinds of different isomr crystalline structure can be obtained, be respectively Tetragonal and six side's phases.Research before shows, compared to the rare earth doping phosphoric acid yttrium crystal of Tetragonal, the crystal of six side's phases shows lower luminescent properties, and reason has luminous cancellation person (OH in the crystal due to six side's phases -).But in the ordinary course of things, the yttrium phosphate crystal of six side's phases easily obtains all the better.Therefore, for obtaining for its higher luminescent properties, how to go the transformation realized from hexagonal crystal to tetragonal phase to become very important study hotspot.Up to now, general after the product obtaining six side's phases, can realize being Tetragonal crystal (Journal of the American Chemical Society by six side's phase crystalline transformation by the method for high-temperature calcination process, 2011,133,2998, Journal of theAmerican Chemical Society, 2010,132,2759).But this method not only needs two steps to complete, being first obtaining of six side's phase products, is then the heat treatment process of six side's phase products, and limits the research to the transformation of its crystalline phase and the transformation of pattern thereof.
So, seek a simple method to realize research that the transformation of yttrium phosphate crystal crystalline phase is the transition process of isomr for its crystal or all to have very important significance for the raising of its potential performance.
Summary of the invention
The object of the invention is to overcome the shortcoming existed in above-mentioned prior art, a kind of rear-earth-doped YPO is provided 4crystal crystalline phase is from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof.
For achieving the above object, the present invention is by the following technical solutions: comprise the following steps:
(1) Y (NO is prepared 3) 3, Eu (NO 3) 3ion is water-soluble rear for subsequent use; By Na 3cit or EDTA joins in deionized water and heated and stirred makes it dissolve, and forms Na 3cit or EDTA solution, naturally cools to room temperature for subsequent use; By NH 4h 2pO 4be dissolved in deionized water and be made into NH 4h 2pO 4solution;
(2) with solute mol ratio 9:1 ~ 4:1 mixing Y (NO 3) 3solution and Eu (NO 3) 3solution, backward mixed solution and dripping Na 3cit or EDTA solution, drips NH after being uniformly mixed liquid 20 ~ 30min 4h 2pO 4solution, Y in the solution finally obtained xeu 1-xnO 3, Na 3cit/EDTA, NH 4h 2pO 4the mol ratio of three is 1:1:1 ~ 1:1:13;
(3) by the solution ph to 1 that dust technology regulating step (2) obtains;
(4) will the solution stirring 40 ~ 60min of pH value be regulated, after transfer in band teflon-lined stainless steel cauldron and seal, react after 6 ~ 12 hours at 160 ~ 180 DEG C, naturally cool to room temperature, be precipitated thing;
(5) the throw out centrifugation will obtained, and with water and washing with alcohol several times, after washed material to be put into 70 ~ 80 DEG C of loft drier dry, finally obtain six side's phases, six side's phases mix with Tetragonal, and the YPO of Tetragonal 4crystal.
In described step (1), Y (NO 3) 3with Eu (NO 3) 3the preparation method of solution is: respectively by Y 2o 3and Eu 2o 3be dissolved in concentrated nitric acid, add the concentrated nitric acid that heat abstraction is unnecessary, then add deionized water and be made into Y (NO 3) 3with Eu (NO 3) 3solution.
In described step (2), NH 4h 2pO 4the dropping mode of solution is slowly drip.
In described step (4), churning time is 40 ~ 60min, and reactor volume compactedness is 80%.
The rear-earth-doped YPO of pure Tetragonal will be obtained in described step (5) 4crystal, the NH in initial action solution 4h 2pO 4, Y xeu 1-xnO 3, Na 3the mol ratio of cit/EDTA three must be greater than 9:1:1.
The number of times of described step (5) middle water and washing with alcohol is three times.
Time of drying in described step (5) is 9 ~ 12h.
The present invention has following beneficial effect: prior art of comparing, and the present invention adopts hydrothermal method by the present invention, uses Na 3cit or EDTA, as sequestrant, has first synthesized the rare earth Eu ion doping YPO of six side's phases 4crystal.By regulating PO in initial action solution 4 3-: RE 3+: Cit 3-the ratio of/EDTA, achieves YPO 4: the controlled transformation of crystalline phase from six sides to Tetragonal of Eu crystal.Meanwhile, the luminescent properties of product also increases substantially.Hydrothermal method is adopted to realize YPO 4the transformation of crystal crystalline phase, simple to operate, optionally synthesize the Eu doping YPO of different crystalline phase 4crystal.The YPO and the Eu of obtained Tetragonal adulterates 4crystal increases substantially compared with the crystallo-luminescence performance of six side's phases, and present method is applicable to spread.
Accompanying drawing explanation
Fig. 1 is different Eu doping YPO prepared by the present invention 4the XRD figure spectrum of crystal;
Fig. 2 is different Eu doping YPO prepared by the present invention 4the PL spectrum of crystal.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in further detail.
The present invention includes following steps:
(1) Y (NO is prepared 3) 3, Eu (NO 3) 3ion is water-soluble rear for subsequent use; By Na 3cit or EDTA joins in deionized water and heated and stirred makes it dissolve, and forms Na 3cit or EDTA solution, naturally cools to room temperature for subsequent use; By NH 4h 2pO 4be dissolved in deionized water and be made into NH 4h 2pO 4solution; Y (NO 3) 3with Eu (NO 3) 3the preparation method of solution is: respectively by Y 2o 3and Eu 2o 3be dissolved in concentrated nitric acid, add the concentrated nitric acid that heat abstraction is unnecessary, then add deionized water and be made into Y (NO 3) 3with Eu (NO 3) 3solution;
(2) with solute mol ratio 9:1 ~ 4:1 mixing Y (NO 3) 3solution and Eu (NO 3) 3solution, backward mixed solution and dripping Na 3cit or EDTA solution, drips NH after being uniformly mixed liquid 20 ~ 30min 4h 2pO 4solution, Y in the solution finally obtained xeu 1-xnO 3, Na 3cit/EDTA, NH 4h 2pO 4the mol ratio of three is 1:1:1 ~ 1:1:13; NH 4h 2pO 4the dropping mode of solution is slowly drip;
(3) by the solution ph to 1 that dust technology regulating step (2) obtains;
(4) will the solution stirring 40 ~ 60min of pH value be regulated, after transfer in band teflon-lined stainless steel cauldron and seal, react after 6 ~ 12 hours at 160 ~ 180 DEG C, naturally cool to room temperature, be precipitated thing; Churning time is 40 ~ 60min, and reactor volume compactedness is 80%;
(5) the throw out centrifugation will obtained, and by water and washing with alcohol three times, after washed material is put into the dry 9 ~ 12h of 70 ~ 80 DEG C of loft drier, finally obtain six side's phases, six side's phases mix with Tetragonal, and the YPO of Tetragonal 4crystal (see accompanying drawing 1).
Embodiment:
Embodiment 1:
(1) 0.4molL of 5.95ml is got -1y (NO 3) 3solution, then adds Eu (NO 3) 3solution fully mixes (Eu5%, mol ratio);
(2) 2mmolNa is weighed 3cit puts in 15ml deionized water, stirs and makes it dissolve, it slowly joined in the mixing solutions of step (1) gained after its cool to room temperature, and additional stirring 20min, to ensure Na 3cit completely by positively charged ion parcel evenly;
(3) 2mmol NH is weighed 4h 2pO 4be dissolved in 15ml deionized water, be added dropwise in the mixing solutions of step (2) gained, stir 20min, ensure that it mixes;
(4) pH=1 of mixing solutions is regulated under agitation with dust technology;
(5) above-mentioned mixing solutions is stirred 40min, transfer in band teflon-lined stainless steel cauldron, sealing, after reacting 6h, naturally cools to room temperature at 180 DEG C;
(6) by the throw out centrifugation obtained (rotating speed is 10000r/min), centrifugation time is 5min, and with water and ethanol repeated washing throw out, centrifugation.Put into 70 DEG C of dry 12h of loft drier, obtain six side phase Eu doping YPO 4crystal.
Embodiment 2:
(1) 0.4molL of 5.95ml is got -1y (NO 3) 3solution, then adds Eu (NO 3) 3solution fully mixes (Eu5%, mol ratio);
(2) 2mmolNa is weighed 3cit puts in 15ml deionized water, and heated and stirred makes it dissolve, and it is slowly joined in the mixing solutions of step (1) gained after its cool to room temperature, and additional stirring 20min, to ensure Na 3cit completely by positively charged ion parcel evenly;
(3) NH of 10mmol is weighed 4h 2pO 4be dissolved in 15ml deionized water, be added dropwise in the mixing solutions of step (2) gained, stir 25min, ensure that it mixes;
(4) pH=1 of final gained mixing solutions is regulated under agitation with dust technology;
(5) above-mentioned mixing solutions is stirred 50min, transfer in band teflon-lined stainless steel cauldron, sealing, after reacting 9h, naturally cools to room temperature at 170 DEG C;
(6) by the throw out centrifugation obtained (rotating speed is 10000r/min), centrifugation time is 5min, and with water and ethanol repeated washing throw out, centrifugation, put into 75 DEG C of dry 9h of loft drier, obtain the Eu doping YPO of six side's phases and Tetragonal mixing 4crystal.
Embodiment 3:
(1) 0.4molL of 5.95ml is got -1y (NO 3) 3solution, then adds Eu (NO 3) 3solution fully mixes (Eu5%, mol ratio);
(2) 2mmolNa is weighed 3cit puts in 15ml deionized water, and heated and stirred makes it dissolve, and it is slowly joined in the mixing solutions of step (1) gained after its cool to room temperature, and additional stirring 30min, to ensure Na 3cit completely by positively charged ion parcel evenly;
(3) NH of 22mmol is weighed 4h 2pO 4be dissolved in 15ml deionized water, be added dropwise in the mixing solutions of step (2) gained, stir 20min, ensure that it mixes;
(4) pH=1 of final gained mixing solutions is regulated under agitation with dust technology;
(5) above-mentioned mixing solutions is stirred 60min, transfer in band teflon-lined stainless steel cauldron, sealing, after reacting 6h, naturally cools to room temperature at 180 DEG C;
(6) by the throw out centrifugation obtained (rotating speed is 10000r/min), centrifugation time is 5min, and with water and ethanol repeated washing throw out, centrifugation.Put into 80 DEG C of dry 12h of loft drier, obtain the Eu doping YPO of Tetragonal 4crystal.
Fig. 1 is the Eu doping YPO of the different crystalline phases utilizing the method for the invention to prepare 4crystal X-Ray Diffraction collection of illustrative plates, as can be seen from the figure, along with increase PO 4 3-concentration, the crystalline phase of crystal there occurs the transformation from six sides to Tetragonal.
Fig. 2 is the Eu doping YPO of the different crystalline phases utilizing the method for the invention to prepare 4crystal PL spectrum.Therefrom can find out the transformation along with crystalline phase, its luminous intensity increases substantially.
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, is not deviating from any equivalent transformation done under this technological process, is being claim of the present invention and contains.

Claims (6)

1. a rear-earth-doped YPO 4crystal crystalline phase, is characterized in that: comprise the following steps from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof:
(1) Y (NO is prepared 3) 3, Eu (NO 3) 3ion is water-soluble rear for subsequent use; By Na 3cit or EDTA joins deionized water for stirring makes it dissolve, and forms Na 3cit or EDTA solution, naturally cools to room temperature for subsequent use; By NH 4h 2pO 4be dissolved in deionized water and be made into NH 4h 2pO 4solution;
(2) with solute mol ratio 9:1 ~ 4:1 mixing Y (NO 3) 3solution and Eu (NO 3) 3solution, backward mixed solution and dripping Na 3cit or EDTA solution, drips NH after being uniformly mixed liquid 20 ~ 30min 4h 2pO 4solution, Y in the solution finally obtained xeu 1-xnO 3, Na 3cit/EDTA, NH 4h 2pO 4the mol ratio of three is 1:1:1 ~ 1:1:13;
(3) by the solution ph to 1 that dust technology regulating step (2) obtains;
(4) will the solution stirring 40 ~ 60min of pH value be regulated, after transfer in band teflon-lined stainless steel cauldron and seal, react after 6 ~ 12 hours at 160 ~ 180 DEG C, naturally cool to room temperature, be precipitated thing;
(5) the throw out centrifugation will obtained, and with water and washing with alcohol several times, after washed material to be put into 70 ~ 80 DEG C of loft drier dry, finally obtain six side's phases, six side's phases mix with Tetragonal, and the YPO of Tetragonal 4crystal.
2. the rear-earth-doped YPO of one according to claim 1 4crystal crystalline phase, is characterized in that from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof, in described step (1), and Y (NO 3) 3with Eu (NO 3) 3the preparation method of solution is: respectively by Y 2o 3and Eu 2o 3be dissolved in concentrated nitric acid, add the concentrated nitric acid that heat abstraction is unnecessary, then add deionized water and be made into Y (NO 3) 3with Eu (NO 3) 3solution.
3. the rear-earth-doped YPO of one according to claim 1 4crystal crystalline phase, is characterized in that from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof, in described step (2), and NH 4h 2pO 4the dropping mode of solution is slowly drip.
4. the rear-earth-doped YPO of one according to claim 1 4crystal crystalline phase, is characterized in that from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof, and in described step (4), churning time is 40 ~ 60min, and reactor volume compactedness is 80%.
5. the rear-earth-doped YPO of one according to claim 1 4crystal crystalline phase is from six sides to the method for improving of the transformation of Tetragonal and luminescent properties thereof, and it is characterized in that, the number of times of described step (5) middle water and washing with alcohol is three times.
6. the rear-earth-doped YPO of one according to claim 1 4crystal crystalline phase to the method for improving of the transformation of Tetragonal and luminescent properties thereof from six sides, is characterized in that, will obtain the rear-earth-doped YPO of pure Tetragonal in described step (5) 4crystal, the NH in initial action solution 4h 2pO 4,y xeu 1-xnO 3, Na 3the mol ratio of cit/EDTA three must be greater than 9:1:1.
CN201510278354.7A 2015-05-27 2015-05-27 A kind of rear-earth-doped YPO4The method for improving of transformation and its luminescent properties of the crystal crystalline phase from hexagonal phase to Tetragonal Active CN104830339B (en)

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* Cited by examiner, † Cited by third party
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CN103979515A (en) * 2014-05-15 2014-08-13 陕西科技大学 YPO4 nano particle synthesized by assist of surfactant cetyltrimethyl ammonium bromide (CTAB) and preparation method of YPO4 nano particle

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CN103979515A (en) * 2014-05-15 2014-08-13 陕西科技大学 YPO4 nano particle synthesized by assist of surfactant cetyltrimethyl ammonium bromide (CTAB) and preparation method of YPO4 nano particle

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