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CN101519589A - High-luminance finely ground particle red fluorescent powder and preparation method thereof - Google Patents

High-luminance finely ground particle red fluorescent powder and preparation method thereof Download PDF

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CN101519589A
CN101519589A CN200910061326A CN200910061326A CN101519589A CN 101519589 A CN101519589 A CN 101519589A CN 200910061326 A CN200910061326 A CN 200910061326A CN 200910061326 A CN200910061326 A CN 200910061326A CN 101519589 A CN101519589 A CN 101519589A
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fluorescent material
high brightness
small particle
red emitting
preparation
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袁曦明
谢安
尹海斌
王永钱
王娟娟
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China University of Geosciences
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Abstract

The invention relates to high-luminance finely ground particle red fluorescent powder and a preparation method thereof. The empirical formula of the red fluorescent powder is LiEu1-xYx(WO4) y(MoO4)2-y, wherein x is equal to 0, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, and 0.8 series; and y is equal to 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.8 and 1.0 series. The red fluorescent powder can be respectively and effectively excited to give off the red light with the emission peak of 615nm by the near ultraviolet light with the wavelength of 396nm and the blue light with the wavelength of 466nm. H3BO3, BaF2, AlF3 or NH4F is taken as a flux and the ultrasonic post-treatment is also adopted so as to effectively solve the agglomeration problem of the prepared red fluorescent powder and meet the technical requirements on the finely ground particle red fluorescent powder used for a white light LED. The sample has high luminous efficiency, fine and even particles, and an average grain diameter of 2 to 3 mu m. The luminous performance is remarkably improved.

Description

A kind of high-luminance finely ground particle red fluorescent powder and preparation method thereof
Technical field
The present invention relates to the required fluor of purposes, particularly a kind of high-luminance finely ground particle red fluorescent powder and preparation method thereof such as semi-conductor solid state lighting (white light LEDs), the novel background light source of liquid-crystal display.
Background technology
White light LEDs is energy-conservation because of it, efficient and environmental protection is referred to as solid state lighting lamp of new generation and receives much concern and enter fields such as automobile, personal communication apparatus, LCD backlight and illumination rapidly.First LED lamp results from July 29th, 1996, and Ri Ya chemical company discovers that the white light that the yttrium aluminium garnet fluorescent powder of jaundice light cooperates photodiode to produce can be used to illumination.It is to utilize blue-ray LED irradiation fluorescent substance to produce and blue light complementary gold-tinted, utilizes lens principle that complementary blue light, gold-tinted are mixed again, produces white light.Nowadays, the colour rendering index of general white LED lamp all about 85, can satisfy general lighting.Yet these white LED lamps can not be used for some specific area such as medical use and architectural lighting etc. because of it lacks red emission.In order to reach the output of high brightness, should make as far as possible that spectral line of emission half-breadth value is little.Commercial colour rendering index and the adjusting colour temperature of utilizing red-light fluorescent powder to improve white light LEDs still is confined to sulfide sill such as CaS:Eu 2+, SrY 2S 4: Eu 2+And ZnCdS:Cu, Al etc.Yet use its physical and chemical performance of sulfide sill very unstable, easily deliquescence easily produces the strong H of corrodibility 2S.During improper use, with the metal lead wire among the LED, reverberation bowl, even chip produces chronic corrosive nature and intoxicating phenomenon, causes the LED device performance to be badly damaged and damages, and its spectral line of emission half-breadth value is also high and efficient is lower in addition.Therefore, exploitation high stability and can be seemed very important by the red fluorescence powder that near-ultraviolet light and blue light effectively excite.
Summary of the invention
Problem to be solved by this invention is to propose a kind of high brightness, small particle red emitting fluorescent material and preparation method thereof at above-mentioned prior art, and this fluorescent powder grain is evenly tiny, luminance purity height, good luminous performance.
The present invention addresses the above problem the technical scheme that is adopted to be: a kind of high brightness, small particle red emitting fluorescent material, its empirical formula is: LiEu 1-xY x(WO 4) y(MoO 4) 2-y, x=0 wherein, 0.1,0.2,0.3,0.4,0.5,0.6,0.8 series; Y=0.1,0.2,0.3,0.4,0.5,0.6,0.8,1.0 series; The mean particle size of fluorescent material is 2～3 μ m; It can effectively be excited by the blue light of the near-ultraviolet light of wavelength 396nm and wavelength 466nm respectively, and emission peak is positioned at the ruddiness of 615nm.
Press such scheme, described high brightness, small particle red emitting fluorescent material, the optimization experiment formula is: LiEu 1-xY x(WO 4) 0.5(MoO 4) 1.5, x=0 wherein, 0.1,0.2,0.3,0.4,0.5,0.6,0.8 series.
Press such scheme, described high brightness, small particle red emitting fluorescent material, best empirical formula is: LiEu 0.5Y 0.5(WO 4) 0.5(MoO 4) 1.5
High brightness, small particle red emitting fluorescent material is the preparation method may further comprise the steps successively:
1) accurately takes by weighing reagent rare earth oxide Eu according to molecular formula by stoichiometric ratio 2O 3, Y 2O 3, WO 3, MoO 3And Li 2CO 3
2) load weighted mentioned reagent is fully ground, after mixing, in the ceramic crucible of packing into;
3) with step 2) the gained sample puts into the high temperature experimental furnace and carries out calcination, and design temperature 700-850 degree are incubated 3-6 hours;
4) after the calcination EP (end of program), treat that the sample furnace cooling takes out to room temperature;
5) sample that is taken out is ground again and sieve, select the fluorescent material that particle diameter is 2～3 μ m;
6) fluorescent material with step 5) gained 2～3 μ m places distilled water, and the volume ratio of distilled water and fluorescent material powder is 5-15:1, carries out dispersion treatment 5-15min with ultrasonic wave, leave standstill, the elimination supernatant liquid repeats to add distilled water again, stir, ultrasonic dispersing 5-15min leaves standstill, so triplicate, be electric neutrality to solution, be throw out that sample takes out then, drying, fluorescent material gets product.
Press such scheme, described reagent also includes fusing assistant, and described fusing assistant is H 3BO 3, BaF 2, AlF 3Or NH 4F.
Press such scheme, step 2) described process of lapping is to be placed in the agate mortar, milling time is 20-60min.
Press such scheme, preferred holding temperature is 750 degree, soaking time 5 hours.
Press such scheme, the described drying of step 6) is at 80-100 ℃ of down dry 2-3h.
The present invention is in order to improve Eu in the fluorescent material matrix molybdate 3+Ion 615nm ( 5D 0→ 7F 2Transition) therefore luminescent properties is introduced and Mo 6+(0.41
Figure A200910061326D0004155201QIETU
) W that ionic radius is close 6+(0.42
Figure A200910061326D0004155201QIETU
) change around luminescence center ionic time crystalline network so that improve the center luminosity.
The present invention prepares, produces red fluorescence powder LiEu with the ultrasonic wave aftertreatment in conjunction with high temperature solid-state method 1-xY x(WO 4) y(MoO 4) 2-y, optimized the preparation production technique.Owing to adopting H in the process for preparing product at high temperature solid-state method 3BO 3, BaF 2, AlF 3Or NH 4Solubility promoters such as F, and in conjunction with the ultrasonic wave aftertreatment, overcome the agglomeration traits of prepared red fluorescence powder effectively, satisfied the technical requirements of the finely ground particle red fluorescent powder that white light LEDs uses, sample luminous efficiency height, particle is tiny, even, and median size has improved luminescent properties significantly at 2-3 μ m.
Description of drawings
Fig. 1 is an embodiment of the invention schema;
Fig. 2 is the powder crystal diffractogram of twinkler of the present invention;
Fig. 3 is the picture of twinkler of the present invention under scanning electronic microscope;
Fig. 4 is twinkler LiEu of the present invention 1-xY x(WO 4) 0.5(MoO 4) 1.5(x=0,0.1,0.2,0.3,0.4,0.5,0.6,0.8) emmission spectrum figure when 396nm excites.
Fig. 5 is twinkler LiEu of the present invention 1-xY x(WO 4) 0.5(MoO 4) 1.5(x=0,0.1,0.2,0.3,0.4,0.5,0.6,0.8) emmission spectrum figure when 466nm excites.
Embodiment
High brightness, small particle red emitting fluorescent material is the preparation method may further comprise the steps successively:
1) accurately takes by weighing reagent rare earth oxide Eu according to molecular formula by stoichiometric ratio 2O 3, Y 2O 3, WO 4, MoO 3, Li 2CO 3And fusing assistant;
2) load weighted mentioned reagent is fully ground, after mixing, in the ceramic crucible of packing into;
3) with step 2) the gained sample puts into the high temperature experimental furnace and carries out calcination, and design temperature 700-850 degree are incubated 3-6 hours;
4) after the calcination EP (end of program), treat that the sample furnace cooling takes out to room temperature;
5) sample that is taken out is ground again and sieve, select the fluorescent material that particle diameter is 2～3 μ m;
6) fluorescent material with step 5) gained 2～3 μ m places distilled water, and the volume ratio of distilled water and fluorescent material powder is 5-15:1, carries out dispersion treatment 5-15min with ultrasonic wave, leave standstill, the elimination supernatant liquid repeats to add distilled water again, stir, ultrasonic dispersing 5-15min leaves standstill, so triplicate, be electric neutrality to solution, be throw out that sample takes out then, drying, fluorescent material gets product.
Further introduce the present invention below by embodiment, but embodiment can not be construed as limiting the invention.
Embodiment 1
Molecular formula: LiEu (WO 4) y(MoO 4) 2-y(y=0.1,0.2,0.3,0.4,0.5,0.6,0.8,1.0)
(1) presses proportioning type LiEu (WO 4) y(MoO 4) 2-y(y=0.1,0.2,0.3,0.4,0.5,0.6,0.8,1.0) stoichiometric ratio takes by weighing MoO respectively 3(99.99wt.%), Eu 2O 3(99.99wt.%), Li 2CO 3(99.9wt.%), WO 3(99.99wt.%);
(2) load weighted reagent is placed on the 40min that mills in the agate mortar, after mixing, in the ceramic crucible of packing into;
(3) sample is put into the high temperature experimental furnace, set heating schedule, under 750 degree, be incubated several 5 hours;
(4) after the calcination EP (end of program), treat that the sample furnace cooling takes out to room temperature;
(5) sample that is taken out is ground again and sieve, select the fluorescent material that particle diameter is 2～3 μ m;
(6) aftertreatment of sample: putting into beaker through the fluorescent material of screening, add distilled water and fully stir, the volume ratio of distilled water and fluorescent material powder is 15:1, ultrasonic dispersing 5min, leave standstill and treat the solution layering, after the basic clear liquid in upper strata, the elimination supernatant liquid adds distilled water again, stir, ultrasonic dispersing 5min leaves standstill, so triplicate.When solution was electric neutrality, the elimination supernatant liquid was put into far infrared drying oven with beaker, dry 3h under 100 ℃, and fluorescent material gets product.
(7) the relative brightness value by spectrophotofluorometer F-4500 measure sample, and definite WO 4 2-And MoO 4 2-Optimum ratio be WO 4 2-/ MoO 4 2-=1/3.
Embodiment 2
Molecular formula: LiEu 1-xY x(WO 4) 0.5(MoO 4) 1.5(x=0,0.1,0.2,0.3,0.4,0.5,0.6,0.8)
(1) presses proportioning type LiEu 1-xY x(WO 4) 0.5(MoO 4) 1.5(x=0,0.1,0.2,0.3,0.4,0.5,0.6,0.8) stoichiometric ratio takes by weighing MoO respectively 3(99.99wt.%), Eu 2O 3(99.99wt.%), Li 2CO 3(99.9wt.%), WO 3(99.99wt.%), Y 2O 3(99.99wt.%),
(2) load weighted reagent is placed on the 0.5h that mills in the agate mortar, after mixing, in the ceramic crucible of packing into;
(3) sample is put into the high temperature experimental furnace, set heating schedule, under 800 degree, be incubated several 4 hours;
(4) after the calcination EP (end of program), treat that the sample furnace cooling takes out to room temperature;
(5) sample that is taken out is ground again and sieve, select the fluorescent material that particle diameter is 2～3 μ m;
(6) aftertreatment of sample: putting into beaker through the fluorescent material of screening, add distilled water and fully stir, the volume ratio of distilled water and fluorescent material powder is 5:1, ultrasonic dispersing 10min, leave standstill and treat the solution layering, after the basic clear liquid in upper strata, the elimination supernatant liquid adds distilled water again, stir, ultrasonic dispersing 10min leaves standstill, so triplicate.When solution was electric neutrality, the elimination supernatant liquid was put into far infrared drying oven with beaker, dry 3h under 90 ℃, and fluorescent material gets product.
(7) the relative brightness value by spectrophotofluorometer F-4500 measure sample, and definite Y 3+Optimum doping concentration be 50mol%.
Embodiment 3
Molecular formula: LiEu 0.5Y 0.5(WO 4) 0.5(MoO 4) 1.5
(1) presses embodiment 1 and the 2 best proportioning type LiEu that determine 0.5Y 0.5(WO 4) 0.5(MoO 4) 1.5Stoichiometric ratio takes by weighing reagent MoO respectively 3(99.99wt.%), Eu 2O 3(99.99wt.%), Li 2CO 3(99.9wt.%), WO 3(99.99wt.%); Y 2O 3(99.99wt.%)., and take by weighing 1wt.% fusing assistant H 3BO 3, H wherein 3BO 3Get the 0.1%-3% of reagent total mass for accounting for;
(2) load weighted reagent is placed on the 0.5h that mills in the agate mortar, after mixing, in the ceramic crucible of packing into;
(3) sample is put into the high temperature experimental furnace, set heating schedule, under 750 degree, be incubated several 5 hours;
(4) after the calcination EP (end of program), treat that the sample furnace cooling takes out to room temperature;
(5) sieve pulverizing fluorescent material later, select the fluorescent material that particle diameter is 2～3 μ m;
(6) aftertreatment of sample: putting into beaker through the fluorescent material of screening, add distilled water and fully stir, the volume ratio of distilled water and fluorescent material powder is 10:1, ultrasonic dispersing 5min, leave standstill and treat the solution layering, after the basic clear liquid in upper strata, the elimination supernatant liquid adds distilled water again, stir, ultrasonic dispersing 5min leaves standstill, so triplicate.When solution was electric neutrality, the elimination supernatant liquid was put into far infrared drying oven with beaker, dry 3h under 100 ℃, and fluorescent material gets product.
(7) measure its brightness and particle diameter.
Embodiment 4-6
Solubility promoter is replaced with BaF respectively 2, AlF 3And NH 4F; All the other steps are identical with embodiment 3, and by measuring its brightness and particle diameter, comparing embodiment 2-6 selects the influence of different flux to this fluorescent material powder for use:
The fluorescent material powder median size of embodiment 2-6 and relative luminous intensity (wherein embodiment 2 gets no fusing assistant brightness optimum value)
Can know that by above form its illumination effect is behind the adding fusing assistant: H 3BO 3NH 4F〉no solubility promoter〉AlF 3BaF 2Its median size behind the adding fusing assistant: no solubility promoter〉NH 4F〉BaF 2AlF 3H 3BO 3
The sample that the present invention is made utilizes Japanese RIGAKU.D/max-3B powder crystal diffraction (XRD) analysis, result such as Fig. 2;
Twinkler LiEu of the present invention 1-xY x(WO 4) 0.5(MoO 4) 1.5(x=0,0.1,0.5) XRD illustrates: although introduced WO in this experiment 4 2-With the Y that mixed 3+But it still belongs to the scheelite mineral phase, and Fig. 2 is powder LiEu 1-xY x(WO 4) 0.5(MoO 4) 1.5The XRD comparison diagram of (x=0,0.1,0.5) is not significantly observed the position of diffraction peak and is moved the appearance of yet not observing new diffraction peak along with the increase sample XRD figure shape of x value.The diffraction peak of all samples all with JCPDS standard card No.54-0978 tetragonal system LiEu (MoO 4) 2Structure inherent characteristic diffraction peak is consistent; Do not observe and starting material WO 3, MoO 3, Eu 2O 3, Li 2CO 3And Y 2O 3Corresponding assorted peak; Just unit cell parameters is along with the increase of x value reduces slightly, and major cause is because adulterated Y 3+(0.83
Figure A200910061326D0004155201QIETU
) replacement Eu 3+(0.88
Figure A200910061326D0004155201QIETU
) enter due to the lattice; This series phosphor powder perfect crystalline of preparation is described, is tetragonal system, spacer: 141/a (88).
The sample that the present invention is made utilizes NEC JSM-35CF type scanning electron microscope (SEM) pattern to detect, and the results are shown in Figure 3;
The sample that the present invention is made utilizes FDAC F-4500 type luminoscope to detect, and the luminescent properties test result is seen Fig. 4.
Each cited raw material of the present invention can both be realized the present invention, and the bound value of each raw material, interval value can both realize the present invention; Do not enumerate embodiment one by one at this.Bound value, the interval value of processing parameter of the present invention (as temperature, time etc.) can both be realized the present invention, all can realize in the 700-850 scope such as the heat tracing temperature, do not enumerate embodiment one by one at this.

Claims (8)

1, a kind of high brightness, small particle red emitting fluorescent material, its empirical formula is: LiEu 1-xY x(WO 4) y(MoO 4) 2-y, x=0 wherein, 0.1,0.2,0.3,0.4,0.5,0.6,0.8 series; Y=0.1,0.2,0.3,0.4,0.5,0.6,0.8,1.0 series; The mean particle size of fluorescent material is 2～3 μ m; It can effectively be excited by the blue light of the near-ultraviolet light of wavelength 396nm and wavelength 466nm respectively, and emission peak is positioned at the ruddiness of 615nm.
2, by the described high brightness, small particle red emitting fluorescent material of claim 1, it is characterized in that the empirical formula of described high brightness, small particle red emitting fluorescent material is: LiEu 1-xY x(WO 4) 0.5(MoO 4) 1.5, x=0 wherein, 0.1,0.2,0.3,0.4,0.5,0.6,0.8 series.
3, by the described high brightness, small particle red emitting fluorescent material of claim 1, it is characterized in that the empirical formula of described high brightness, small particle red emitting fluorescent material is: LiEu 0.5Y 0.5(WO 4) 0.5(MoO 4) 1.5
4, the described high brightness, small particle red emitting fluorescent material of claim 1 preparation method is characterized in that may further comprise the steps successively:
1) accurately takes by weighing reagent rare earth oxide Eu according to molecular formula by stoichiometric ratio 2O 3, Y 2O 3, WO 3, MoO 3And Li 2CO 3
2) load weighted mentioned reagent is fully ground, after mixing, in the ceramic crucible of packing into;
3) with step 2) the gained sample puts into the high temperature experimental furnace and carries out calcination, and design temperature 700-850 degree are incubated 3-6 hours;
4) after the calcination EP (end of program), treat that the sample furnace cooling takes out to room temperature;
5) sample that is taken out is ground again and sieve, select the fluorescent material that particle diameter is 2～3 μ m;
6) fluorescent material with step 5) gained 2～3 μ m places distilled water, and the volume ratio of distilled water and fluorescent material powder is 5-15:1, carries out dispersion treatment 5-15min with ultrasonic wave, leave standstill, the elimination supernatant liquid repeats to add distilled water again, stir, ultrasonic dispersing 5-15min leaves standstill, so triplicate, be electric neutrality to solution, be throw out that sample takes out then, drying, fluorescent material gets product.
5, by the described high brightness, small particle red emitting fluorescent material of claim 4 preparation method, it is characterized in that described reagent also includes fusing assistant, described fusing assistant is H3BO 3, BaF 2, AlF 3Or NH 4F.
6,, it is characterized in that step 2 by the described high brightness, small particle red emitting fluorescent material of claim 4 preparation method) described process of lapping is to be placed in the agate mortar, milling time is 20-60min.
7,, it is characterized in that holding temperature is 750 degree, soaking time 5 hours by the described high brightness, small particle red emitting fluorescent material of claim 4 preparation method.
8,, it is characterized in that the described drying of step 6) is at 80-100 ℃ of down dry 2-3h by the described high brightness, small particle red emitting fluorescent material of claim 4 preparation method.
CN200910061326A 2009-03-27 2009-03-27 High-luminance finely ground particle red fluorescent powder and preparation method thereof Pending CN101519589A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102120931A (en) * 2010-12-03 2011-07-13 深圳职业技术学院 Red fluorophor and preparation method thereof
CN106520117A (en) * 2016-10-31 2017-03-22 陕西科技大学 A preparing method of LiLa(MoO4)2:Eu<3+> fluorescent powder
CN107033897A (en) * 2017-05-08 2017-08-11 陕西科技大学 The tungsten salt luminescent material and synthetic method of a kind of Fluorin doped of near ultraviolet excitation
CN107033898A (en) * 2017-05-08 2017-08-11 陕西科技大学 A kind of high thermal stability doping Sm tungsten salt luminescent material and preparation method thereof
CN109793266A (en) * 2019-01-30 2019-05-24 湖北中烟工业有限责任公司 A kind of cigarette light-emitting particles and preparation method thereof and the filter stick containing the light-emitting particles
WO2021093567A1 (en) * 2019-11-12 2021-05-20 深圳市绎立锐光科技开发有限公司 Fluorescent ceramic and light source device

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102120931A (en) * 2010-12-03 2011-07-13 深圳职业技术学院 Red fluorophor and preparation method thereof
WO2012071746A1 (en) * 2010-12-03 2012-06-07 深圳职业技术学院 Red fluorescent materials and preparation methods thereof
CN102120931B (en) * 2010-12-03 2013-06-19 深圳职业技术学院 Red fluorophor and preparation method thereof
CN106520117A (en) * 2016-10-31 2017-03-22 陕西科技大学 A preparing method of LiLa(MoO4)2:Eu<3+> fluorescent powder
CN107033897A (en) * 2017-05-08 2017-08-11 陕西科技大学 The tungsten salt luminescent material and synthetic method of a kind of Fluorin doped of near ultraviolet excitation
CN107033898A (en) * 2017-05-08 2017-08-11 陕西科技大学 A kind of high thermal stability doping Sm tungsten salt luminescent material and preparation method thereof
CN107033897B (en) * 2017-05-08 2020-02-21 陕西科技大学 Fluorine-doped tungsten molybdate luminescent material excited by near ultraviolet light and synthesis method
CN109793266A (en) * 2019-01-30 2019-05-24 湖北中烟工业有限责任公司 A kind of cigarette light-emitting particles and preparation method thereof and the filter stick containing the light-emitting particles
WO2021093567A1 (en) * 2019-11-12 2021-05-20 深圳市绎立锐光科技开发有限公司 Fluorescent ceramic and light source device

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Application publication date: 20090902