CN103525422A - Fluorescent powder used for white-light LED (light emitting diode) and preparation method of fluorescent powder - Google Patents
Fluorescent powder used for white-light LED (light emitting diode) and preparation method of fluorescent powder Download PDFInfo
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- CN103525422A CN103525422A CN201310452776.2A CN201310452776A CN103525422A CN 103525422 A CN103525422 A CN 103525422A CN 201310452776 A CN201310452776 A CN 201310452776A CN 103525422 A CN103525422 A CN 103525422A
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Abstract
The invention discloses fluorescent powder used for a white-light LED and a preparation method of the fluorescent powder. A chemical structural formula of the fluorescent powder is (Y3-x-y-z-w CexBiyGdzLaw) Al5012, wherein x is larger than or equal to 0.01 and is smaller than or equal to 0.03, y is larger than or equal to 0.01 and is smaller than or equal to 0.08, z is larger than or equal to 0.02 and is smaller than or equal to 0.50, and w is larger than or equal to 0.02 and is smaller than or equal to 0.05. According to the fluorescent powder used for the white-light LED and the preparation method of the fluorescent powder, a mixed solution of ammonium bicarbonate and ammonium hydroxide is used as a precipitator, and an intermediate product is obtained with a coprecipitation method and is heated in reducing atmosphere after steps of water washing, alcohol washing and drying, so that the fluorescent powder is obtained; and the prepared fluorescent powder has high luminous efficiency and is warm-toned.
Description
Technical field
The present invention relates to a kind of fluorescent material and preparation method thereof, relate in particular to a kind of fluorescent powder for white LED and preparation method thereof.
Background technology
Apart from modern LED commodity the earliest, in nineteen sixty-eight, come out, yet, until after the GaInN that Japanese Ya company in 1993 successfully develops greater efficiency is blue-ray LED, side is achieved the LED product of true color.Photodiode (Light-emitting kiode, LED) relatively there are many advantages with conventional light source, comprise that volume is little, luminous efficiency is high, energy consumption is low, the life-span long (reaching more than 1000 hours), without warm lamp time, operant response speed be exceedingly fast, reliability is high, not cracky, the element that is easily prepared into various size or array, non-thermal radiation and the advantage such as pollution-free.
On blue-light LED chip, coating can be by blue-light excited yellow fluorescent powder, gold-tinted and the remaining blue light of fluorescent material transmitting are combined into white light, this is the technique that current white light LEDs is the most often used, the efficient yellow fluorescent powder being excited by blue-ray LED is the important component part of white light LEDs, so carried out a large amount of research work aspect the fluorescent material that people excite at development blue-ray LED, and constantly had patent in succession open.As, United States Patent (USP) 5998925 discloses a kind of blue-light excited yellow fluorescent powder, they consist of (Y, Gd)<sub TranNum="56">3</sub>(A1, Ga)<sub TranNum="57">5</sub>0<sub TranNum="58">12</sub>: Ce, combines and obtains white light LEDs with blue chip.Although it has higher luminous efficiency, in its emission wavelength, lack ruddiness and cannot obtain the warm white light LEDs from light and high-color rendering.In Chinese patent CN01120498.2, disclose a kind of Yttrium aluminium garnet (YAG) type fluorescent powder, its molecular formula is (Y<sub TranNum="59">3-x-y</sub>ce<sub TranNum="60">x</sub>z<sub TranNum="61">y</sub>) Al<sub TranNum="62">5</sub>0<sub TranNum="63">12</sub>or (Y<sub TranNum="64">3</sub>ce<sub TranNum="65">x</sub>z<sub TranNum="66">y</sub>) Al<sub TranNum="67">5</sub>0<sub TranNum="68">12</sub>, 0<x≤0.8 wherein, 0.5<y≤2.5, Z is the group that gadolinium element forms.Chinese patent CN02103950 discloses a kind of preparation method of yttrium aluminium garnet white light powder of cerium activation, usings oxyaluminum compound as start material, and its chemical formula is: Y<sub TranNum="69">3-x</sub>al<sub TranNum="70">5</sub>0<sub TranNum="71">12</sub>: xCe; With oxyaluminum compound, yttrium oxide is raw material, and the cerous nitrate of x=0.001-0.04 of take is exciting agent, the fusing assistant that adds again 5% mole of chemical formula, obtains mixture, after mixed grinding, at 1400-1600 ℃, heat-treat again, obtain qualified fluorescent material.Chinese patent CN031527094 discloses the preparation method of the adjustable white light emitting diode fluorescent material of a kind of high brightness wavelength, it is characterized in that: according to chemical formula Y<sub TranNum="72">3-x</sub>al<sub TranNum="73">5</sub>0<sub TranNum="74">12</sub>: xCe<sup TranNum="75">3+</sup>stoichiometric ratio relation, takes aluminum oxide, yttrium oxide, activator ceria, x=0.01-0.05; The fusing assistant that adds 1%-5% mole, obtains mixture; This mixture is ground and is mixed, be placed in calcination vessel; At this container, put into carbon-point outward, then put in the lump High Temperature Furnaces Heating Apparatus heating, make High Temperature Furnaces Heating Apparatus by room temperature, rise to 900 ℃ fast, and at 900 ℃ of constant temperature 30min, then make High Temperature Furnaces Heating Apparatus be raised to 1550 ℃ from 900 ℃, roasting 3-5 hour, obtains white emitting fluorescent powder of the present invention after cooling.With it, be packaged into white light LEDs, its luminous intensity is greater than lOcd.It can be scattered in transparent silica gel uniformly, has changed the emission wavelength of fluorescent material, can make full use of the InGaN blue chip of 430-480nm, improves colour temperature and the chromaticity coordinates of white light LEDs.
Although the emission efficiency of above-mentioned fluorescent material is higher, emission wavelength also has certain Red Shift Phenomena, and its synthetic method bothers relatively, and its emission efficiency can also further improve in addition.
Summary of the invention
Technical problem for above-mentioned existence, the object of the invention is: proposed fluorescent powder for white LED that a kind of luminous efficiency is higher and preparation method thereof.
Technical solution of the present invention is achieved in that a kind of fluorescent powder for white LED, and its chemical structural formula is: (Y
3-x-y-z-wce
xbi
ygd
zla
w) Al
50
12, wherein, 0.03≤x≤0.01,0.01≤y≤0.08,0.02≤z≤0.50,0.02≤w≤0.05.
Preferably, described material powder is selected from metal nitrate or muriate.
The preparation method of aforesaid fluorescent powder for white LED, comprises the following steps:
1) according to chemical formula (Y
3-x-y-z-wce
xbi
ygd
zla
w) Al
50
12stoichiometric ratio relation, 0.03≤x≤0.01 wherein, 0.01≤y≤0.08,0.02≤z≤0.50,0.02≤w≤0.05; Take in proportion Y (NO
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use.
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the ratio of bicarbonate of ammonia and ammoniacal liquor is 1:3～6, and concentration is 0.01～2M.In B solution, add 0.5～2% dispersion agent and 10～30% ethanol simultaneously.
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=10～14, rapid stirring is 20～35 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product.
4), after intermediate product is dried, in reducing atmosphere, l000～l550 ℃ of thermal treatment is 5～8 hours, is cooled to room temperature, obtains fluorescent material.
Preferably, step 1) each described material purity is 99.9～99.999%.
Preferably, step 3), the pH value of reaction mixture is adjusted to 10.5～12.5.
Preferably, step 4) in, the intermediate product after drying is placed in High Temperature Furnaces Heating Apparatus, at N
2-H
2in the High Temperature Furnaces Heating Apparatus that mixed gas or carbon dust participate in, be heated to l000～l550 ℃, be incubated 5～8 hours, come out of the stove after cooling to room temperature with the furnace, obtain fluorescent material.
Due to the utilization of technique scheme, the present invention compared with prior art has following advantages:
Fluorescent powder for white LED of the present invention is mixed altogether by rare earth ion, changed the emission wavelength of fluorescent material, can make full use of the InGaN blue chip of 430-480nm, improve colour temperature and the chromaticity coordinates of white light emitting diode, and is improved its work-ing life; By changing the content of Partial Elements, make its white light emitting diode being packaged into, the white light emitting diode that its luminous intensity becomes close to the external similar fluorescent powder packaging with selling in the market.The preparation method of fluorescent powder for white LED of the present invention adopts liquid-phase coprecipitation, various elements are mixed at molecule, atomic size, more even than solid phase mixing, its grain-size is generally 20～50nm, offspring median size is 0.5 μ m left and right, tiny particle diameter, can be scattered in transparent silica gel uniformly, is conducive to evenly apply encapsulation.The preparation method of fluorescent powder for white LED of the present invention, technique is simple, with low cost, is suitable for large-scale mass production.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, technical solution of the present invention is described further:
Accompanying drawing 1 is the excitation and emission spectra figure of the fluorescent material described in embodiment mono-;
Accompanying drawing 2 is the excitation and emission spectra figure of the fluorescent material described in embodiment bis-;
Accompanying drawing 3 is the excitation and emission spectra figure of the fluorescent material described in embodiment tri-;
Accompanying drawing 4 is the XRD figure spectrum of the fluorescent material described in embodiment tetra-;
Accompanying drawing 5 is the SEM photo of the fluorescent material described in embodiment five;
Accompanying drawing 6 is the Laser particle-size distribution figure of the fluorescent material described in embodiment five.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Implement one:
, its chemical structural formula is: (Y
2.94ce
0.03bi
0.02gd
0.02la
0.02) Al
50
12.
A preparation method for fluorescent powder for white LED, comprises the following steps:
1) according to chemical formula (Y
2.94ce
0.03bi
0.02gd
0.02la
0.02) Al
50
12stoichiometric ratio relation, takes Y (NO in proportion
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use.
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1:3, and concentration is 0.01M.In B solution, add 0.5% dispersion agent and 10% ethanol simultaneously.
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=10.5, rapid stirring is 20 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product.
4), after intermediate product is dried, in reducing atmosphere, l000 ℃ of thermal treatment is 5 hours, is cooled to room temperature, obtains fluorescent material.Its excitation and emission spectra figure as shown in Figure 1.
Implement two:
, its chemical structural formula is: (Y
2.86ce
0.05bi
0.03gd
0.03la
0.03) Al
50
12.
A preparation method for fluorescent powder for white LED, comprises the following steps:
1) according to chemical formula (Y
2.86ce
0.05bi
0.03gd
0.03la
0.03) Al
50
12stoichiometric ratio relation, takes Y (NO in proportion
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use.
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1:3, and concentration is 0.01M.In B solution, add 0.5% dispersion agent and 10% ethanol simultaneously.
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=10.5, rapid stirring is 20 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product.
4), after intermediate product is dried, in reducing atmosphere, l450 ℃ of thermal treatment is 5 hours, is cooled to room temperature, obtains fluorescent material.Its excitation and emission spectra figure as shown in Figure 2
Implement three:
, its chemical structural formula is: (Y
2.84ce
0.06bi
0.04gd
0.03la
0.03) Al
50
12.
A preparation method for fluorescent powder for white LED, comprises the following steps:
1) according to chemical formula (Y
2.84ce
0.06bi
0.04gd
0.03la
0.03) Al
50
12stoichiometric ratio relation, takes Y (NO in proportion
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use.
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1:3, and concentration is 0.01M.In B solution, add 0.5% dispersion agent and 10% ethanol simultaneously.
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=10.5, rapid stirring is 20 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product.
4), after intermediate product is dried, in reducing atmosphere, l550 ℃ of thermal treatment is 5 hours, is cooled to room temperature, obtains fluorescent material.Its excitation and emission spectra figure as shown in Figure 3
Implement four:
, its chemical structural formula is: (Y
2.81ce
0.06bi
0.06gd
0.04la
0.03) Al
50
12.
A preparation method for fluorescent powder for white LED, comprises the following steps:
1) according to chemical formula (Y
2.81ce
0.06bi
0.06gd
0.04la
0.03) Al
50
12stoichiometric ratio relation, takes Y (NO in proportion
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use.
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1:3, and concentration is 0.01M.In B solution, add 0.5% dispersion agent and 10% ethanol simultaneously.
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=10.5, rapid stirring is 20 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product.
4), after intermediate product is dried, in reducing atmosphere, l500 ℃ of thermal treatment is 5 hours, is cooled to room temperature, obtains fluorescent material.Fig. 4 is the XRD test pattern of the fluorescent material that obtains of this method.
Implement five:
, its chemical structural formula is: (Y
2.69ce
0.07bi
0.08gd
0.08la
0.08) Al
50
12.
A preparation method for fluorescent powder for white LED, comprises the following steps:
1) according to chemical formula (Y
2.69ce
0.07bi
0.08gd
0.08la
0.08) Al
50
12stoichiometric ratio relation, takes Y (NO in proportion
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use.
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1:4.5, and concentration is 1.005M.In B solution, add 1.25% dispersion agent and 20% ethanol simultaneously.
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=11.5, rapid stirring is 27.5 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product.
4), after intermediate product is dried, in reducing atmosphere, l475 ℃ of thermal treatment is 6.5 hours, is cooled to room temperature, obtains fluorescent material.Fig. 5 and Fig. 6 are its stereoscan photograph and particle size distribution figure.
The preparation method of the fluorescent powder for white LED of above-described embodiment, step 1) each described material purity is 99.9～99.999%.
The preparation method of the fluorescent powder for white LED of above-described embodiment, step 4) in, the intermediate product after drying is placed in High Temperature Furnaces Heating Apparatus, at N
2-H
2in the High Temperature Furnaces Heating Apparatus that mixed gas or carbon dust participate in, be heated to l000～l550 ℃, be incubated 5～8 hours, come out of the stove after cooling to room temperature with the furnace, obtain fluorescent material.
Fluorescent powder for white LED of the present invention is mixed altogether by rare earth ion, changed the emission wavelength of fluorescent material, can make full use of the InGaN blue chip of 430-480nm, improve colour temperature and the chromaticity coordinates of white light emitting diode, and is improved its work-ing life; By changing the content of aluminium, make it be packaged into white light emitting diode, the white light emitting diode that its luminous intensity becomes close to the similar fluorescent powder packaging of the external use of selling in the market.The preparation method of fluorescent powder for white LED of the present invention adopts liquid-phase coprecipitation, various elements are mixed at molecule, atomic size, more even than solid phase mixing, its grain-size is generally 20～50nm, offspring median size is 0.5 μ m left and right, tiny particle diameter, can be scattered in transparent silica gel uniformly, is conducive to evenly apply encapsulation.The preparation method of fluorescent powder for white LED of the present invention, technique is simple, with low cost, is suitable for large-scale mass production.
Above-described embodiment is only explanation technical conceive of the present invention and feature; its object is to allow person skilled in the art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; all equivalences that spirit is done according to the present invention change or modify, and all should be encompassed in protection scope of the present invention.
Claims (6)
1. a fluorescent powder for white LED, is characterized in that: its chemical structural formula is: (Y
3-x-y-z-wce
xbi
ygd
zla
w) Al
50
12, wherein, 0.03≤x≤0.01,0.01≤y≤0.08,0.02≤z≤0.50,0.02≤w≤0.05.
2. fluorescent powder for white LED according to claim 1, is characterized in that: described material powder is selected from metal nitrate or muriate.
3. the preparation method of fluorescent powder for white LED according to claim 1 and 2, is characterized in that: comprise the following steps:
1) according to chemical formula (Y
3-x-y-z-wce
xbi
ygd
zla
w) Al
50
12stoichiometric ratio relation, 0.03≤x≤0.01 wherein, 0.01≤y≤0.08,0.02≤z≤0.50,0.02≤w≤0.05; Take in proportion Y (NO
3)
3.6H
2o, Ce (NO
3)
3.6H
2o, Bi (NO
3)
3.5H
2o, Gd (NO
3)
3.6H
2o, La (NO
3)
3.6H
2o, Al (NO
3)
3.9H
2o, joins in deionized water and dissolves and form A solution for later use;
2) take bicarbonate of ammonia and ammoniacal liquor mixed dissolution forms B solution in deionized water, wherein the molar ratio of bicarbonate of ammonia and ammoniacal liquor is 1:3～6, and concentration is 0.01～2M; In B solution, add 0.5～2% dispersion agent and 10～30% ethanol simultaneously;
3) after stirring, A solution is poured in B solution lentamente, adjusted PH=10～14, rapid stirring is 20～35 minutes simultaneously, filters white precipitate washing, alcohol wash, obtains fluorescent material intermediate product;
4), after intermediate product being dried, grinding, in reducing atmosphere, l000～l550 ℃ of thermal treatment is 2～8 hours, is cooled to room temperature, obtains fluorescent material.
4. the preparation method of fluorescent powder for white LED according to claim 3, is characterized in that: step 1) each described material purity is 99.9～99.999%.
5. according to the preparation method of the fluorescent powder for white LED described in claim 4, it is characterized in that: step 3) in the pH value of reaction mixture be adjusted to 10.5～12.5.
6. according to the preparation method of the fluorescent powder for white LED described in claim 5, it is characterized in that: step 4) in the intermediate product after drying is placed in High Temperature Furnaces Heating Apparatus, at N
2-H
2in the High Temperature Furnaces Heating Apparatus that mixed gas or carbon dust participate in, be heated to l000～l550 ℃, be incubated 5～8 hours, come out of the stove after cooling to room temperature with the furnace, obtain fluorescent material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194785A (en) * | 2014-08-21 | 2014-12-10 | 西安交通大学 | Method for improving luminous intensity of (Y,Gd)AG:Ce fluorescent powder through modification of bismuth nitrate pentahydrate |
| CN110041933A (en) * | 2019-04-10 | 2019-07-23 | 济南大学 | A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission |
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| JPH10298550A (en) * | 1997-04-28 | 1998-11-10 | Hitachi Maxell Ltd | Infrared light-emitting fluorescent material |
| CN1364851A (en) * | 2002-02-27 | 2002-08-21 | 北京大学 | Process for preparing cerium activated yttrium aluminium garnet white light powder |
| CN1718669A (en) * | 2005-07-14 | 2006-01-11 | 上海交通大学 | Method of preparing cerium activated yttrium aluminium garnet ultrafine fluorescent powder using coprecipitation |
| CN100999662A (en) * | 2006-12-29 | 2007-07-18 | 中国科学院长春应用化学研究所 | Preparation process of fluorescent powder for white light LED excited by blue light |
| CN101602944A (en) * | 2009-07-09 | 2009-12-16 | 宁波大学 | A kind of production method of rare earth ion doped yttrium aluminum garnet nano phosphor powder |
| CN101973569A (en) * | 2010-10-15 | 2011-02-16 | 河南理工大学 | Method for synthesizing fluorescent powder of yttrium aluminum garnet |
-
2013
- 2013-09-26 CN CN201310452776.2A patent/CN103525422A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10298550A (en) * | 1997-04-28 | 1998-11-10 | Hitachi Maxell Ltd | Infrared light-emitting fluorescent material |
| CN1364851A (en) * | 2002-02-27 | 2002-08-21 | 北京大学 | Process for preparing cerium activated yttrium aluminium garnet white light powder |
| CN1718669A (en) * | 2005-07-14 | 2006-01-11 | 上海交通大学 | Method of preparing cerium activated yttrium aluminium garnet ultrafine fluorescent powder using coprecipitation |
| CN100999662A (en) * | 2006-12-29 | 2007-07-18 | 中国科学院长春应用化学研究所 | Preparation process of fluorescent powder for white light LED excited by blue light |
| CN101602944A (en) * | 2009-07-09 | 2009-12-16 | 宁波大学 | A kind of production method of rare earth ion doped yttrium aluminum garnet nano phosphor powder |
| CN101973569A (en) * | 2010-10-15 | 2011-02-16 | 河南理工大学 | Method for synthesizing fluorescent powder of yttrium aluminum garnet |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104194785A (en) * | 2014-08-21 | 2014-12-10 | 西安交通大学 | Method for improving luminous intensity of (Y,Gd)AG:Ce fluorescent powder through modification of bismuth nitrate pentahydrate |
| CN110041933A (en) * | 2019-04-10 | 2019-07-23 | 济南大学 | A kind of Bi3+Doping enhancing Ce3+The fluorescent powder of yellow emission |
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