CN103725285B - Single-substrate white-light fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof - Google Patents

Single-substrate white-light fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof Download PDF

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CN103725285B
CN103725285B CN201310718318.9A CN201310718318A CN103725285B CN 103725285 B CN103725285 B CN 103725285B CN 201310718318 A CN201310718318 A CN 201310718318A CN 103725285 B CN103725285 B CN 103725285B
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white
fluorescent powder
light
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powder
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CN103725285A (en
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宁青菊
李向龙
代旭飞
胡昌志
刘斐
董成思
常方
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Shaanxi University of Science and Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention discloses a single-substrate white-light fluorescent powder for white-light LEDs (light-emitting diodes) and a preparation method thereof, belonging to the technical field of preparation of LED fluorescent powder. The composition expression of the white-light fluorescent powder is NaLaMgWO6:xTm<3+>,yDy<3+>,zEu<3+>, wherein x=0.07-0.2, y=0.01-0.07, and z=0.01-0.07. The preparation method comprises the following steps: 1) mixing Na2CO3, La2O3, Mg(NO3)2.6H2O, WO3, Tm2O3, Dy2O3 and Eu2O3 in a mole ratio of (0.5-2):(0.5-2):(0.5-2):1:x/2:y/2:z/2, and grinding uniformly to obtain a powder mixture; and 2) carrying out solid-phase sintering on the powder mixture in a weakly reducing atmosphere to obtain the white-light fluorescent powder. The method is simple to operate, has the advantages of low facility request and environment friendliness, and is suitable for industrialized large-scale production.

Description

A kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof
Technical field
The invention belongs to technical field of preparation of LED fluorescent powder, be specifically related to a kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof.
Background technology
White light LEDs (Light Emitting Diode) have nontoxic, energy-efficient, the life-span is long, all solid state, operating voltage is low, shock resistance and the various features such as security is good, instead of existing incandescent light and luminescent lamp becomes lighting source of new generation, be widely used in illumination and display field.
At present, the realization of business-like white light LEDs mainly contains two schemes, one is that blue chip excites yellow fluorescent powder, residue blue light and gold-tinted compound send white light, but the glow color of device with driving voltage and fluorescent coating thickness change and change, color reducibility is poor, the low and non-refractory of colour rendering index.Another kind is that ultraviolet-near ultraviolet (350 ~ 4l0nm) excites red-green-blue fluorescent material to realize white light LEDs, but, absorb again and proportioning regulation and control problem owing to there is color between mixed fluorescent powder, the luminous efficiency of fluorescent material and color reducibility are a greater impact.Single-matrix white fluorescent powder is as novel fluorescence powder material, and due to colour stable, the advantages such as color reducibility is good have become study hotspot, and therefore the applicable near ultraviolet excitated efficient single-matrix white fluorescent powder tool of development is of great significance.
In recent years, the research of relevant fluorescence powder, existing lot of documents report, the matrix compounds related to mainly contains silicate, phosphoric acid salt, borate, vanadate, aluminate, tungstate etc.Wherein, tungstate is typical self-activating luminescent material, and luminescent spectrum is very stable, and intrinsic photoluminescent band is very wide, occupies the major part of visible region, and the positively charged ion in tungstate affects the position of emission band consumingly.Tungstate can by some impurity activation, and these impurity can make it have the luminescence of special property after being impregnated in tungstate dot matrix.Therefore, tungstate is a kind of substrate material of luminescent properties excellence.
In addition, along with developing rapidly of LED industry, the research of its luminescent material synthetic method is also become popular.Preparation method has high temperature solid-state method, combustion synthesis method, sol-gel method, spray pyrolysis, hydrothermal synthesis method etc.At present, the material dephasign of the wet chemical method synthesis such as such as sol-gel method, spray pyrolysis, hydrothermal synthesis method is more, and luminous efficiency is lower.High temperature solid-state method is a kind of traditional method in synthesizing luminescent material, and this method technical process is simple, easy to operate, and the crystalline structure of synthesis resulting materials is more intact, and stable performance, brightness is high.So far, most of business-like luminescent material still uses this method to prepare.
Summary of the invention
The object of the present invention is to provide a kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof, the method adopts high temperature solid-phase sintering, and obtained product granularity is even, crystal property good, can realize white light emission.
The present invention is achieved through the following technical solutions:
For a single-matrix white fluorescent powder for white light LEDs, the composition expression formula of this white emitting fluorescent powder is NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+, wherein x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07.
The colour rendering index of described white emitting fluorescent powder is 80.
The median size of described white emitting fluorescent powder is 1 ~ 5 μm.
The emission wavelength coverage of described white emitting fluorescent powder is 450nm ~ 650nm.
A preparation method for white light LEDs single-matrix white fluorescent powder, comprises the following steps:
1) according to (0.5 ~ 2): (0.5 ~ 2): the mol ratio of (0.5 ~ 2): 1:x/2:y/2:z/2, x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07, gets Na respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, after mixing, grinding evenly, obtains mixed powder;
2) by mixed powder through solid state sintering, obtain NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07;
Described solid state sintering system is: by mixed powder from room temperature, with 1 ~ 3 DEG C/min ramp to 100 ~ 300 DEG C, again with 2 ~ 4 DEG C/min ramp to 300 ~ 600 DEG C, then with 3 ~ 7 DEG C/min ramp to 1000 ~ 1200 DEG C, cool after insulation 3 ~ 9h.
Described solid state sintering is that mixed powder is placed in alumina crucible, sinters in resistance furnace.
Described is cooled to furnace cooling.
Compared with prior art, the present invention has following useful technique effect:
The present invention is with Na 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3for raw material, after solid state sintering, the NaLaMgWO of obtained uniform particle sizes 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder.By the testing and analyzing of X-ray diffractometer and fluorescence spectrum, known by the NaLaMgWO prepared by solid phase method 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder powder and NaLaMgWO 6standard card is consistent, and powder granularity is even, crystal property good and realize white light emission, and obtained white emitting fluorescent powder median size is 1 ~ 5 μm, and colour rendering index is up to 80, and emission wavelength coverage is at 450nm ~ 650nm.Present method is simple to operate, low for equipment requirements, environmental friendliness, is applicable to industrialization scale operation.
Accompanying drawing explanation
Fig. 1 is the NaLaMgWO that the embodiment of the present invention 1 obtains 6: xTm 3+, yDy 3+, zEu 3+the XRD figure of white emitting fluorescent powder;
Fig. 2 is the NaLaMgWO that the embodiment of the present invention 2 obtains 6: xTm 3+, yDy 3+, zEu 3+the utilizing emitted light spectrogram of white emitting fluorescent powder;
Fig. 3 is the NaLaMgWO that the embodiment of the present invention 3 obtains 6: xTm 3+, yDy 3+, zEu 3+the CIE figure of white emitting fluorescent powder.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
The preparation method of white light LEDs white emitting fluorescent powder provided by the invention, specifically with Na 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3for raw material, after solid state sintering, the NaLaMgWO of obtained uniform particle sizes 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder powder.Concrete grammar is:
According to (0.5 ~ 2): (0.5 ~ 2): the mol ratio (x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07) of (0.5 ~ 2): 1:x/2:y/2:z/2, takes Na respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, and above raw material is carried out mix, grind, obtain raw material powder;
Raw material powder is placed in alumina crucible, sinters in resistance furnace.In described resistance furnace sintering schedule for by mixed powder from room temperature, with 1 ~ 3 DEG C/min ramp to 100 ~ 300 DEG C, again with 2 ~ 4 DEG C/min ramp to 300 ~ 600 DEG C, then with 3 ~ 7 DEG C/min ramp to 1000 ~ 1200 DEG C, cool after insulation 3 ~ 9h.
Embodiment 1
A kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof, comprises the following steps:
1) according to the mol ratio (x=0.07, y=0.01, z=0.01) of 0.5:0.5:1:1:x/2:y/2:z/2, Na is taken respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, and above raw material is carried out mix, grind, obtain mixed powder;
2) mixed powder is placed in alumina crucible, sinters in resistance furnace.In described resistance furnace, sintering schedule is with 1 DEG C/min ramp to 200 DEG C, then with 3 DEG C/min ramp to 500 DEG C, then with 5 DEG C/min ramp to 1000 DEG C, insulation 3h, last furnace cooling, obtains NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.07, y=0.01, z=0.01.
See Fig. 1, NaLaMgWO as can be seen from Figure 1 6: xTm 3+, yDy 3+, zEu 3+powder and NaLaMgWO 6standard card JCPDS#37-0243 be consistent completely, and peak shape is sharp-pointed, and the sample of synthesis belongs to AA ' BB ' X 6type monoclinic structure, spacer is P21 (4), and lattice parameter is a=5.524nm, b=5.525nm, c=7.894nm.This illustrates NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+the crystallization degree of sample is high, and a small amount of Tm 3+, Dy 3+, Eu 3+doping do not change NaLaMgWO 6host lattice structure.
Embodiment 2
A kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof, comprises the following steps:
1) according to the mol ratio (x=0.15, y=0.03, z=0.03) of 0.5:0.5:2:1:x/2:y/2:z/2, Na is taken respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, and above raw material is carried out mix, grind, obtain mixed powder;
2) mixed powder is placed in alumina crucible, sinters in resistance furnace.In described resistance furnace, sintering schedule is with 1 DEG C/min ramp to 100 DEG C, then with 2 DEG C/min ramp to 300 DEG C, then with 7 DEG C/min ramp to 1100 DEG C, insulation 3h, last furnace cooling, obtains NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.15, y=0.03, z=0.03.
See Fig. 2, the emission band of fluorescent material is distributed within the scope of 450nm ~ 650nm as can be seen from Figure 2, and emmission spectrum launches strong peak composition primarily of 3, and respectively at 485nm, 575nm, 615nm place, wherein, 485nm place is due to Tm 3+'s 1g 4- 3h 6energy level transition launches blue green light, and 575nm place is due to Dy 3+'s 4f 9/2- 6h 13/2energy level transition launches gold-tinted, and 615nm place is due to Eu 3+'s 5d 0- 7f 2energy level transition red-emitting.Tm 3+, Dy 3+, Eu 3+in same matrix, there is transmission ofenergy thus realize white light emission.
Embodiment 3
A kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof, comprises the following steps:
1) according to the mol ratio (x=0.2, y=0.05, z=0.05) of 1:2:0.5:1:x/2:y/2:z/2, Na is taken respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, and above raw material is carried out mix, grind, obtain mixed powder;
2) mixed powder is placed in alumina crucible, sinters in resistance furnace.In described resistance furnace, sintering schedule is with 3 DEG C/min ramp to 300 DEG C, then with 4 DEG C/min ramp to 600 DEG C, then with 5 DEG C/min ramp to 1100 DEG C, insulation 5h, last furnace cooling, obtains NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.2, y=0.05, z=0.05.
See Fig. 3, as can be seen from Figure 3, NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+fluorescent material is transmitting white under near ultraviolet excitation, colour temperature Tc=2947K, and this is due to Tm 3+, yDy 3+, zEu 3+in near ultraviolet excitated lower generation transmission ofenergy.
Embodiment 4
A kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof, comprises the following steps:
1) according to the mol ratio (x=0.1, y=0.03, z=0.01) of 2:1:2:1:x/2:y/2:z/2; Take Na respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, and above raw material is carried out mix, grind, obtain mixed powder;
2) mixed powder is placed in alumina crucible, sinters in resistance furnace.In described resistance furnace, sintering schedule is with 2 DEG C/min ramp to 200 DEG C, then with 4 DEG C/min ramp to 600 DEG C, then with 3 DEG C/min ramp to 1200 DEG C, insulation 7h, last furnace cooling, obtains NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.1, y=0.03, z=0.01.
Embodiment 5
A kind of single-matrix white fluorescent powder for white light LEDs and preparation method thereof, comprises the following steps:
1) according to the mol ratio (x=0.2, y=0.07, z=0.07) of 0.5:0.5:1:1:x/2:y/2:z/2, Na is taken respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, and above raw material is carried out mix, grind, obtain mixed powder
2) mixed powder is placed in alumina crucible, sinters in resistance furnace.In described resistance furnace, sintering schedule is with 2 DEG C/min ramp to 200 DEG C, then with 3 DEG C/min ramp to 500 DEG C, then with 5 DEG C/min ramp to 1150 DEG C, insulation 9h, last furnace cooling, obtains NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.2, y=0.07, z=0.07.

Claims (4)

1. for a single-matrix white fluorescent powder for white light LEDs, it is characterized in that, the composition expression formula of this white emitting fluorescent powder is NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+, wherein x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07;
The colour rendering index of described white emitting fluorescent powder is 80, and median size is 1 ~ 5 μm, and emission wavelength coverage is 450nm ~ 650nm.
2. a preparation method for white light LEDs single-matrix white fluorescent powder, is characterized in that, comprises the following steps:
1) according to (0.5 ~ 2): (0.5 ~ 2): the mol ratio of (0.5 ~ 2): 1:x/2:y/2:z/2, x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07, gets Na respectively 2cO 3, La 2o 3, Mg (NO 3) 26H 2o, WO 3, Tm 2o 3, Dy 2o 3and Eu 2o 3, after mixing, grinding evenly, obtains mixed powder;
2) by mixed powder through solid state sintering, obtain NaLaMgWO 6: xTm 3+, yDy 3+, zEu 3+white emitting fluorescent powder, wherein x=0.07 ~ 0.2, y=0.01 ~ 0.07, z=0.01 ~ 0.07;
Described solid state sintering system is: by mixed powder from room temperature, with 1 ~ 3 DEG C/min ramp to 100 ~ 300 DEG C, again with 2 ~ 4 DEG C/min ramp to 300 ~ 600 DEG C, then with 3 ~ 7 DEG C/min ramp to 1000 ~ 1200 DEG C, cool after insulation 3 ~ 9h.
3. the preparation method of a kind of white light LEDs single-matrix white fluorescent powder according to claim 2, is characterized in that, described solid state sintering is that mixed powder is placed in alumina crucible, sinters in resistance furnace.
4. the preparation method of a kind of white light LEDs single-matrix white fluorescent powder according to claim 2, it is characterized in that, described is cooled to furnace cooling.
CN201310718318.9A 2013-12-20 2013-12-20 Single-substrate white-light fluorescent powder for white-light LEDs (light-emitting diodes) and preparation method thereof Expired - Fee Related CN103725285B (en)

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CN104277850A (en) * 2014-09-01 2015-01-14 陕西科技大学 Yellow fluorescent powder for white LED (light-emitting diode) and preparation method of yellow fluorescent powder
CN104694126A (en) * 2014-12-25 2015-06-10 陕西科技大学 Rare earth-doped NaLaMgTeO6-based green fluorescent powder and preparation method thereof
CN104694128B (en) * 2014-12-25 2016-11-30 陕西科技大学 A kind of single-matrix WLED fluorescent material and preparation method thereof
CN104877680A (en) * 2015-04-22 2015-09-02 南方科技大学 White-light fluorescent powder and preparation method thereof and white light-emitting device
CN110218562A (en) * 2019-07-11 2019-09-10 陕西科技大学 A kind of rare earth ion codope magnesium tungstate lanthanum sodium luminescent material and preparation method thereof

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