CN105295913A - Yellow monodispersible spherical rare earth oxide fluorescent powder and preparation method thereof - Google Patents

Yellow monodispersible spherical rare earth oxide fluorescent powder and preparation method thereof Download PDF

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CN105295913A
CN105295913A CN201510908152.6A CN201510908152A CN105295913A CN 105295913 A CN105295913 A CN 105295913A CN 201510908152 A CN201510908152 A CN 201510908152A CN 105295913 A CN105295913 A CN 105295913A
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fluorescent powder
yellow
earth oxide
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fluorescent material
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李金凯
侯青月
刘宗明
滕鑫
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University of Jinan
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University of Jinan
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Abstract

The invention provides yellow monodispersible spherical rare earth oxide fluorescent powder with the chemical formula as follows: [(YyGd1-y)1-xDyx)]2O3. The fluorescent powder is prepared by the steps of synthesizing a precursor of a target product by taking rare earth nitrate as a mother salt and urea as a precipitating agent through a uniform precipitation technology, and then, calcining at high temperature. The fluorescent powder particles provided by the invention has extremely high sphericility and favorable dispersibility; due to the doping of Y<3+>, the crystal structure of the fluorescent powder can be improved, and the stability of the fluorescent powder can be improved; and the yellow monodispersible spherical rare earth oxide fluorescent powder can emit excellent yellow and blue lights, an energy transfer effect from Gd<3+> to Dy<3+> exists, the light intensity of Dy<3+> is remarkably improved, and the fluorescent powder with excellent performances and a preparation method of the fluorescent powder are provided for actual production application.

Description

A kind of yellow monodisperse spherical rare-earth oxide phosphor and preparation method thereof
Technical field
The invention belongs to rare-earth luminescent material field, be specifically related to a kind of yellow monodisperse spherical rare-earth oxide phosphor and preparation method thereof.
Background technology
Rare earth oxide refers to generally have the oxide compound that rare earth element is formed stronger fluorescent characteristic, and possess photoluminescence property.
Yttrium oxide (Y 2o 3) and gadolinium sesquioxide (Gd 2o 3) be all very important rare-earth oxide, be often applied in fluorescent material as starting material.The crystalline structure of yttrium oxide belongs to isometric system, and have good chemical stability and heat-resisting, corrosion resistance nature, specific inductivity is high, and to advantages such as reducing medium good stabilities.Gadolinium sesquioxide (Gd 2o 3) structure relative complex, undergoing phase transition under about normal pressure 1300-1400 DEG C, is monoclinic phase by cubic phase transition, and Gd 3+radius is Y comparatively 3+bigger.Therefore, by admixture Y 3+improve Gd 2o 3crystalline structure.
Y 2o 3and Gd 2o 3being all excellent luminous host material, is Eu about rare earth ion doped research at present the most widely 3+.Wherein, Y 2o 3: Eu 3+there is excellent luminescent properties, be important three-color light-emitting material, can be used as the red fluorescence powder of colour television set picture tube.Meanwhile, nanometer Y 2o 3: Eu 3+there is the excellent properties such as high brightness, high stability, low applied voltage, can be used in high-resolution projection, low pressure display, field-emission display device.Gd 2o 3: Eu 3+also be a kind of red fluorescence powder of high-quality, there is higher luminous quantum efficiency and good spectral response curve, be widely used in the fields such as high definition television, projection TV, flat pannel display, Green Lighting Project.And (Y, Gd) 2o 3: Eu 3+also be the fluorescent material that a kind of luminous efficiency is higher, can be applicable to the fields such as photoluminescence, cathodoluminescence, X-ray luminescence.
Research finds, Dy 3+there are two main emission bands at visible-range, are stimulated and produce stronger blue light and yellow emission, correspond respectively to Dy 3+'s 4f 9/2→ 6h 15/2(near 484nm) and 4f 9/2→ 6h 13/2(near 575nm) transition, can be used for three-color light-emitting assembly and white light LEDs, is a kind of potential white emitting fluorescent powder.But, rarely have about Dy 3+doping Y 2o 3/ Gd 2o 3the research of monodisperse spherical fluorescent material synthesis.Therefore, Dy is utilized 3+doping Y 2o 3/ Gd 2o 3prepare rare-earth oxide phosphor and there is larger researching value and meaning.
Summary of the invention
The object of the present invention is to provide a kind of sphericity high, favorable dispersity and the stable yellow rare-earth oxide fluorescent powder of crystalline network and preparation method.
The preparation method of the yellow monodisperse spherical rare-earth oxide phosphor that the present invention proposes comprises the following steps:
(1) form according to the chemical formula of this fluorescent material, take reagent according to stoichiometric, described reagent comprises Gd 2o 3(purity 99.99%), Dy 2o 3(purity 99.99%), Y 2o 3(purity 99.99%), urea (CO (NH 2) 212H 2o, >99%) and concentrated nitric acid (HNO 3, analytical pure) etc.;
(2) by the powdery RE in step (1) 2o 3(RE=Gd, Dy and Y) is dissolved in the Gd (NO that hot nitric acid is mixed with 0.5mol/L 3) 3, Y (NO 3) 3with the Dy (NO of 0.1mol/L 3) 3rare earth nitrate solution;
(3) rare earth nitrate solution that step (2) obtains is mixed with female salts solution according to certain mixed in molar ratio, (urea add-on is rare-earth cation RE to add precipitation agent urea wherein 3+40 times of concentration), add deionized water and obtain 500mL question response solution;
(4) the question response solution of preparation in step (3) is moved into water bath with thermostatic control heated and stirred, make its precipitation from homogeneous solution, products therefrom is through repeatedly centrifugation, washing and alcohol wash, finally the throw out that dehydrated alcohol disperses is placed in beaker, obtains 80 DEG C of oven dry the white precursor powder that this is fluorescent material;
(5) calcined at different temperatures by gained white presoma in step (4), after grinding, obtain this is fluorescent powder grain.
Heating and temperature control described in step (4) is 90 ± 1 DEG C, and soaking time is 2h, and drying time is 6h.
Heating rate when calcining described in step (5) is 5 DEG C/min, and calcination time is 4h.
Fluorescent material prepared by the present invention, tool has the following advantages:
(1) fluorescent powder grain prepared by the present invention has good dispersiveness and sphericity, can reduce exciting scattering of light, is easy to self-assembly, film forming, effectively improves luminous efficiency;
(2) Y 3+add and can improve the crystalline structure that this is fluorescent material, improve stability;
(3) this be fluorescent material under 275nm optical excitation, present excellent blue light and yellow emission;
(4) there is Gd 3+→ Dy 3+between transmission ofenergy effect, significantly improve Dy 3+luminous intensity.
Accompanying drawing explanation
Fig. 1 is [(Y ygd 1-y) 1-xdy x)] 2o 3the FE-SEM shape appearance figure of series phosphor powder presoma.
Fig. 2 is through 1000 DEG C of calcining gained [(Y ygd 1-y) 1-xdy x)] 2o 3the FE-SEM shape appearance figure of series phosphor powder.
Fig. 3 is through 1000 DEG C of calcining gained [(Y ygd 1-y) 1-xdy x)] 2o 3the XRD curve of series phosphor powder.
Fig. 4 calcines gained [(Y through 1000 ° of C 0.05gd 0.95) 0.98dy 0.02)] 2o 3the fluorescence emission spectrum of fluorescent material.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention will be described in detail.
Embodiment 1
The present invention tests required reagent and comprises Gd 2o 3(purity 99.99%), Dy 2o 3(purity 99.99%), Y 2o 3(purity 99.99%), urea (CO (NH 2) 212H 2o, >99%) and concentrated nitric acid (HNO 3, analytical pure) etc.; According to the chemical formula [(Y of fluorescent material ygd 1-y) 1-xdy x)] 2o 3, get x=0.02, y=0.05, i.e. [(Y 0.05gd 0.95) 0.98dy 0.02)] 2o 3; Powdery rare earth oxide compound Y is accurately taken according to stoichiometric ratio 2o 3, Gd 2o 3and Dy 2o 3, be dissolved in the rare earth nitrate solution that hot nitric acid is mixed with 0.5mol/L, 0.5mol/L and 0.1mol/L respectively; According to chemical formula composition, measure the Y (NO of preparation 3) 3solution 0.735mL, Gd (NO 3) 3solution 13.965mL, Dy (NO 3) 3solution 1.5mL, taking urea 18.018g(urea concentration is 0.6mol/L, rare-earth cation RE 3+concentration is 0.015mol/L); Above reagent mix is added deionized water, is formulated as the mixing solutions of 500mL; Then, this solution is moved into water bath with thermostatic control heated and stirred, first at 25 DEG C of insulation 2h, then in 1h, be warming up to 90 DEG C, at 90 ± 1 DEG C of insulation 2h to reacting end; Solution is cooled to rapidly less than 30 DEG C after taking out, and through repeatedly centrifugal, washes 2 times, alcohol wash 1 time; Then this is precipitated ultrasonic disperse in dehydrated alcohol, be placed in air dry oven, dry 6h at 80 DEG C and make precipitation dry, obtaining this is fluorescent material precursor powder; This presoma is carried out high-temperature calcination, and calcining temperature is 1000 DEG C, and temperature rise rate is 5 DEG C/min, and soaking time is 4h; Fluorescent powder grain after calcining grinds through agate mortar, can obtain target fluorescent powder.
Embodiment 2
The present invention tests required reagent and comprises Gd 2o 3(purity 99.99%), Dy 2o 3(purity 99.99%), Y 2o 3(purity 99.99%), urea (CO (NH 2) 212H 2o, >99%) and concentrated nitric acid (HNO 3, analytical pure) etc.; According to the chemical formula [(Y of fluorescent material ygd 1-y) 1-xdy x)] 2o 3, get x=0.02, y=0.10, i.e. [(Y 0.10gd 0.90) 0.98dy 0.02)] 2o 3; Powdery rare earth oxide compound Y is accurately taken according to stoichiometric ratio 2o 3, Gd 2o 3and Dy 2o 3, be dissolved in the rare earth nitrate solution that hot nitric acid is mixed with 0.5mol/L, 0.5mol/L and 0.1mol/L respectively; According to chemical formula composition, measure the Y (NO of preparation 3) 3solution 1.47mL, Gd (NO 3) 3solution 13.23mL, Dy (NO 3) 3solution 1.5mL, taking urea 18.018g(urea concentration is 0.6mol/L, rare-earth cation RE 3+concentration is 0.015mol/L); Above reagent mix is added deionized water, is formulated as the mixing solutions of 500mL; Then, this solution is moved into water bath with thermostatic control heated and stirred, first at 25 DEG C of insulation 2h, then in 1h, be warming up to 90 DEG C, at 90 ± 1 DEG C of insulation 2h to reacting end; Solution is cooled to rapidly less than 30 DEG C after taking out, and through repeatedly centrifugal, washes 2 times, alcohol wash 1 time; Then this is precipitated ultrasonic disperse in dehydrated alcohol, be placed in air dry oven, dry 6h at 80 DEG C and make precipitation dry, obtaining this is fluorescent material precursor powder; This presoma is carried out high-temperature calcination, and calcining temperature is 1000 DEG C, and temperature rise rate is 5 DEG C/min, and soaking time is 4h; Fluorescent powder grain after calcining grinds through agate mortar, can obtain target fluorescent powder.
Embodiment 3
The present invention tests required reagent and comprises Gd 2o 3(purity 99.99%), Dy 2o 3(purity 99.99%), Y 2o 3(purity 99.99%), urea (CO (NH 2) 212H 2o, >99%) and concentrated nitric acid (HNO 3, analytical pure) etc.; According to the chemical formula [(Y of fluorescent material ygd 1-y) 1-xdy x)] 2o 3, get x=0.02, y=0.15, i.e. [(Y 0.15gd 0.85) 0.98dy 0.02)] 2o 3; Powdery rare earth oxide compound Y is accurately taken according to stoichiometric ratio 2o 3, Gd 2o 3and Dy 2o 3, be dissolved in the rare earth nitrate solution that hot nitric acid is mixed with 0.5mol/L, 0.5mol/L and 0.1mol/L respectively; According to chemical formula composition, measure the Y (NO of preparation 3) 3solution 2.205mL, Gd (NO 3) 3solution 12.495mL, Dy (NO 3) 3solution 1.5mL, taking urea 18.018g(urea concentration is 0.6mol/L, rare-earth cation RE 3+concentration is 0.015mol/L); Above reagent mix is added deionized water, is formulated as the mixing solutions of 500mL; Then, this solution is moved into water bath with thermostatic control heated and stirred, first at 25 DEG C of insulation 2h, then in 1h, be warming up to 90 DEG C, at 90 ± 1 DEG C of insulation 2h to reacting end; Solution is cooled to rapidly less than 30 DEG C after taking out, and through repeatedly centrifugal, washes 2 times, alcohol wash 1 time; Then this is precipitated ultrasonic disperse in dehydrated alcohol, be placed in air dry oven, dry 6h at 80 DEG C and make precipitation dry, obtaining this is fluorescent material precursor powder; This presoma is carried out high-temperature calcination, and calcining temperature is 1000 DEG C, and temperature rise rate is 5 DEG C/min, and soaking time is 4h; Fluorescent powder grain after calcining grinds through agate mortar, can obtain target fluorescent powder.
Embodiment 4
The present invention tests required reagent and comprises Gd 2o 3(purity 99.99%), Dy 2o 3(purity 99.99%), Y 2o 3(purity 99.99%), urea (CO (NH 2) 212H 2o, >99%) and concentrated nitric acid (HNO 3, analytical pure) etc.; According to the chemical formula [(Y of fluorescent material ygd 1-y) 1-xdy x)] 2o 3, get x=0.03, y=0.05, i.e. [(Y 0.05gd 0.95) 0.97dy 0.03)] 2o 3; Powdery rare earth oxide compound Y is accurately taken according to stoichiometric ratio 2o 3, Gd 2o 3and Dy 2o 3, be dissolved in the rare earth nitrate solution that hot nitric acid is mixed with 0.5mol/L, 0.5mol/L and 0.1mol/L respectively; According to chemical formula composition, measure the Y (NO of preparation 3) 3solution 0.7275mL, Gd (NO 3) 3solution 13.8225mL, Dy (NO 3) 3solution 2.25mL, taking urea 18.018g(urea concentration is 0.6mol/L, rare-earth cation RE 3+concentration is 0.015mol/L); Above reagent mix is added deionized water, is formulated as the mixing solutions of 500mL; Then, this solution is moved into water bath with thermostatic control heated and stirred, first at 25 DEG C of insulation 2h, then in 1h, be warming up to 90 DEG C, at 90 ± 1 DEG C of insulation 2h to reacting end; Solution is cooled to rapidly less than 30 DEG C after taking out, and through repeatedly centrifugal, washes 2 times, alcohol wash 1 time; Then this is precipitated ultrasonic disperse in dehydrated alcohol, be placed in air dry oven, dry 6h at 80 DEG C and make precipitation dry, obtaining this is fluorescent material precursor powder; This presoma is carried out high-temperature calcination, and calcining temperature is 1000 DEG C, and temperature rise rate is 5 DEG C/min, and soaking time is 4h; Fluorescent powder grain after calcining grinds through agate mortar, can obtain target fluorescent powder.
Fig. 1 prepares [(Y by present method ygd 1-y) 1-xdy x)] 2o 3the FE-SEM shape appearance figure of series phosphor powder presoma, wherein (a) x=0.02, y=0.05; (b) x=0.02, y=0.10; (c) x=0.02, y=0.15; (d) x=0.03, y=0.05.As can be seen from Figure 1 Y 3+and Dy 3+interpolation and content the pattern of fluorescent material presoma and size are not all made a significant impact.All granular precursors all present excellent monodisperse spherical pattern, illustrate that the precipitation from homogeneous solution technology that the present invention adopts has good feasibility.
Fig. 2 is through 1000 DEG C of calcining gained [(Y by presoma ygd 1-y) 1-xdy x)] 2o 3the FE-SEM shape appearance figure of series phosphor powder, wherein (a) x=0.02, y=0.05; (b) x=0.02, y=0.10; (c) x=0.02, y=0.15; (d) x=0.03, y=0.05.As can be seen from Figure 2, this be fluorescent material presoma after 1000 DEG C of high-temperature calcinations, gained fluorescent material still can keep excellent sphericity and dispersiveness.
Fig. 3 is through 1000 DEG C of calcining gained [(Y by presoma ygd 1-y) 1-xdy x)] 2o 3the XRD curve of series phosphor powder, wherein S1 (x=0.02, y=0.05), S2 (x=0.02, y=0.10), S3 (x=0.02, y=0.15), S4 (x=0.03, y=0.05).As can be seen from Figure 3 at the calcination temperature, the rare earth oxide pure phase that this is fluorescent material can all be obtained.
Fig. 4 calcines gained [(Y by presoma through 1000 ° of C ygd 1-y) 1-xdy x)] 2o 3the emmission spectrum (wherein x=0.02, y=0.05) of series phosphor powder.Under 275nm optical excitation, emmission spectrum comprises two dominant emission peaks: be positioned at the blue emission at 489nm place and be positioned at the yellow emission at 577nm place, corresponding respectively to Dy 3+'s 4f 9/2→ 6h 15/2transition and 4f 9/2→ 6h 13/2transition.

Claims (7)

1. a yellow monodisperse spherical rare-earth oxide phosphor, is characterized in that: this is that fluorescent material has high sphericity and excellent dispersiveness, and chemical formula is [(Y ygd 1-y) 1-xdy x)] 2o 3(wherein x=0.02,0.03, y=0.05,0.10,0.15).
2. the yellow monodisperse spherical rare-earth oxide phosphor of one according to claim 1, is characterized in that: this is that fluorescent material presents excellent blue light and yellow emission (corresponding to Dy under 275nm optical excitation 3+'s 4f 9/2→ 6h 15/2transition and 4f 9/2→ 6h 13/2transition).
3. the yellow monodisperse spherical rare-earth oxide phosphor of one according to claim 1 and 2, is characterized in that: Y 3+admixture effectively can improve the stability that this is fluorescent material crystalline network.
4. the preparation method of a kind of yellow monodisperse spherical rare-earth oxide phosphor as claimed in claim 1, is characterized in that, comprise the following steps:
(1) according to the chemical formula composition that this is fluorescent material, take reagent according to stoichiometric, described reagent comprises Y 2o 3(purity 99.99%), Gd 2o 3(purity 99.99%), Dy 2o 3(purity 99.99%), urea (CO (NH 2) 212H 2o, purity >99%) and concentrated nitric acid (HNO 3, analytical pure) etc.;
(2) by the powdery rare earth oxide compound RE in step (1) 2o 3(RE=Y, Gd, Dy) is dissolved in hot nitric acid and is mixed with corresponding rare earth nitrate solution;
(3) according to stoichiometric, the rare earth nitrate solution measuring preparation in step (2) mixes with acclimatization agent urea, obtained reaction soln is also moved into water bath with thermostatic control heated and stirred, and precipitin reaction products therefrom obtains through centrifugation, washing, oven dry the white precursor powder that this is fluorescent material;
(4) white for gained in step (3) granular precursor being obtained this through high-temperature calcination is fluorescent material.
5. preparation method according to claim 4, is characterized in that: in described step (3), heating and temperature control is 90 ± 1 DEG C, and the insulation reaction time is 2h.
6. preparation method according to claim 4, is characterized in that: in described step (3), bake out temperature is 80 DEG C, and the time is 6h.
7. preparation method according to claim 4, is characterized in that: in described step (4), heating rate is 5 DEG C/min.
CN201510908152.6A 2015-12-10 2015-12-10 Yellow monodispersible spherical rare earth oxide fluorescent powder and preparation method thereof Pending CN105295913A (en)

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Application publication date: 20160203