CN102533266A - Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder - Google Patents

Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder Download PDF

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CN102533266A
CN102533266A CN2011104195611A CN201110419561A CN102533266A CN 102533266 A CN102533266 A CN 102533266A CN 2011104195611 A CN2011104195611 A CN 2011104195611A CN 201110419561 A CN201110419561 A CN 201110419561A CN 102533266 A CN102533266 A CN 102533266A
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red fluorescent
preparation
white light
europium
fluorescent powder
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韦波
顾国华
袁荣鑫
刘海燕
张咪
张明明
於晓菁
孙笑
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CHANGSHU ASIA-PACIFIC FLUORESCENT MATERIAL Co Ltd
Changshu Institute of Technology
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CHANGSHU ASIA-PACIFIC FLUORESCENT MATERIAL Co Ltd
Changshu Institute of Technology
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    • Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps

Abstract

The invention provides europium-activated tungsten molybdate red fluorescent powder for a white LED (Light Emitting Diode) and a preparation method of the europium-activated tungsten molybdate red fluorescent powder, relating to fluorescent powder. The chemical formula of the europium-activated tungsten molybdate red fluorescent powder is R3<1>R2<2>R3<3-x>Eux(R4O4)8, wherein R<1> is one or more of Li, Na, K, Rb, Cs and Ag, R<2> is one or more of Mg, Ca, Sr, Ba and Zn, R<3> is one or more of Y, Gd, La, Lu, Pr, Sm, Ce, Tb, Bi, Al and Cr, R<4> is either Mo or W or both the Mo and the W, and x is not less than 0 and not more than 3. The preparation method comprises the following steps of: evenly mixing and grinding raw materials containing the R<1>, the R<2>, the R<3>, the R<4> and Eu<3+>, carrying out high-temperature synthesis, and carrying out aftertreatment. The europium-activated tungsten molybdate red fluorescent powder provided by the invention can be effectively activated by near ultraviolet or blue light and emits red light with high color purity. The preparation method of the europium-activated tungsten molybdate red fluorescent powder has the advantages of simplicity, easiness in operation and environment-friendliness.

Description

White light LEDs is with silicate red fluorescent material of europkium-activated tungsten and preparation method thereof
Technical field
The invention belongs to rare earth luminescent material technical field, be specifically related to a kind of can by near-ultraviolet light or blue-ray LED effectively excite with the silicate red fluorescent material of europium ion activated tungsten, and relate to the preparation method of this fluorescent material.
Background technology
1996, Japanese Ri Ya company was with GaN base blue-light LED chip and Ce 3+Activated yttrium aluminum garnet yellow fluorescent powder is combined, and has prepared first white light LEDs.White light LEDs is a kind of semi-conductor solid state lighting new light sources of efficient, less energy-consumption; It has that volume is little, the life-span is long, antidetonation is not fragile, WV is low, start characteristics such as fast, energy-conservation, pollution-free and reduce power consumption of time of response, and being acknowledged as is the green illumination light source of complete following replace fluorescent lamps and incandescent light at present.
At present, the form that obtains white light LEDs mainly contains two kinds: the one, with three kinds of led chip combination results of red, green, blue white light; The 2nd, form white light with mixing with other luminescent materials of LED de excitation; The fluorescent material and the red light fluorescent material that promptly cooperate jaundice coloured light with blue-ray LED; The fluorescent material that perhaps cooperates glow green and burn red with blue-ray LED is perhaps with purple light or three kinds of fluorescent material of ultraviolet LED de excitation red, green, blue etc.
Second method through fluor conversion hysteria LED have simple in structure, light efficiency is high with become the low advantage of wood, be the main path that obtains white light LEDs now, and its key problem is a development high-efficiency fluorescence powder.Because fluorescent material can determine the key property and the parameters such as light conversion efficiency, luminous efficiency, colour temperature, chromaticity coordinates value and colour rendering index of white light LEDs.So the development white light LEDs is significant with the high-efficiency fluorescence powder.The red fluorescence powder that current commerce is used for ultraviolet InGaN base LED chip is Y 2O 2S:Eu 3+Yet, red fluorescence powder Y 2O 2S:Eu 3+Can not effectively absorb to blue light range near ultraviolet, its luminous intensity has only 1/8th of blue colour fluorescent powder and green emitting phosphor brightness.In addition, red fluorescence powder Y under the exciting of near-ultraviolet light or blue light 2O 2S:Eu 3+Chemical property is unstable, decompose easily and produce harmful SO 2Gas.These deficiencies of red fluorescence powder have become the bottleneck that improves the white light LEDs development.Research to red fluorescent powder for white LED has obtained certain progress, and its kind is a lot, has their own characteristics each, and shortcoming is also respectively arranged, and in general, can't reach the target that current LED technology is expected red fluorescence powder.Therefore, exploitation can be become a urgent task by the red fluorescent powder for white radiation LED that near-ultraviolet light and blue light effectively excite.
Summary of the invention
The purpose of this invention is to provide a kind of that can effectively be excited by near-ultraviolet light or blue light, good luminous performance and stable chemical performance and red light color purity ideal tungsten Barbiturates red fluorescence powder.
Another object of the present invention provides the preparation method of above-mentioned red fluorescence powder.This method preparation method technological process is simple, easy handling, pollution-free, cost is low.
For realizing above-mentioned purpose, the present invention takes following technical scheme:
White light LEDs is used europkium-activated red fluorescence powder, and its chemical expression is: R 3 1R 2 2R 3 3-xEu x(R 4O 4) 8R wherein 1Be among Li, Na, K, Rb, Cs, the Ag one or more; R 2Be among Mg, Ca, Sr, Ba, the Zn one or more; R 3Be among Y, Gd, La, Lu, Pr, Sm, Ce, Tb, Bi, Al, the Cr one or more; R 4Be among Mo, the W one or more; 0≤x≤3 wherein.
White light LEDs of the present invention is with the preparation method of europkium-activated red fluorescence powder, and this method may further comprise the steps:
1. with R 1, R 2, R 3And Eu 3+Carbonate, nitrate salt or organic acid salt, and R 4Oxide compound, oxygen acid or oxysalt be raw material, desired raw material is placed the baking oven thorough drying, accurately take by weighing corresponding raw material and porphyrize respectively according to the mol ratio in the chemical expression.
2. the powder stock mixed grinding that 1. step is obtained is even.
3. the mixture that 2. step is obtained places retort furnace, under air atmosphere, 600 ℃～1200 ℃ sintering temperatures 1 hour～12 hours.
4. the product of roasting that 3. step is obtained carries out aftertreatment and promptly makes red fluorescence powder of the present invention.
Above-mentioned steps 2. in, can add volatile solvents such as zero(ppm) water or ethanol, acetone during mixed grinding, also can under the situation of solubilizing agent not, grind;
Above-mentioned steps 3. in, also can adopt two step calcination methods, can be earlier 500-900 ℃ of sintering temperature 1 hour～8 hours, then with powder mixed grinding once more, again 600 ℃ of-1200 ℃ of sintering temperatures 1 hour～12 hours.
Above-mentioned steps 4. in aftertreatment comprised broken, select powder, removal of impurities, oven dry and classification.Removal of impurities comprises one or more in pickling, alkali cleaning, the washing; Classification process can adopt one or more in the methods such as settling process, method of sieving, hydraulic classification or air classification
The positively effect that the present invention has: red fluorescence powder physicochemical property 1. of the present invention are stable, and are nontoxic, nuisanceless, do not react with oxygen, carbonic acid gas and steam in the environment.2. red fluorescence powder of the present invention can be about near-ultraviolet light about 394nm and 465nm blue-light excited purity of color red light preferably of launching down about 617nm; The output wavelength coupling of its excitation wavelength and near ultraviolet LED chip or blue-light LED chip meets the requirement of the solid-state photo device of white light LEDs with powder.3. preparing method's technological process of red fluorescence powder of the present invention is simple, and preparation cost is low, and can not produce pollution.
Description of drawings
Fig. 1 is the excitation spectrum of red fluorescence powder of the present invention
Fig. 2 is the emmission spectrum of red fluorescence powder of the present invention
Embodiment
Embodiment 1
Preparation Li 3Ba 2Gd 1.2Eu 1.8(WO 4) 8Red fluorescence powder
Desired raw material is placed the baking oven thorough drying, take by weighing Eu then 2O 33.1674g, Gd 2O 32.1750g, WO 318.5470g, Li 2CO 31.1082g, BaCO 33.9466g above raw material middle-weight rare earths oxide compound purity is 99.99% (quality), remaining all is an analytical pure.With the above-mentioned raw materials mixed grinding evenly after, put into crucible, be placed in the retort furnace in 600 ℃ and carry out pre-burning 5 hours, with the powder regrinding after the pre-burning to evenly, sintering 6 hours under 1000 ℃ of conditions in retort furnace.With the sintered product that obtains carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, promptly obtain the red fluorescence powder of above-mentioned chemical expression.
The resulting white light LEDs of present embodiment with the excitation spectrum of molybdate red phosphor and emmission spectrum respectively by illustrated in figures 1 and 2; Wherein: main emission peak is near 617nm; Two main excitation peaks are respectively near 394nm and 465nm; Hence one can see that, and this fluorescent material can effectively be excited and sends ruddiness by near-ultraviolet light and blue light, can be used for white light LEDs.
Embodiment 2
Preparation Li 3Ba 2Y 0.9Eu 2.1(WO 4) 8Red fluorescence powder
Desired raw material is placed the baking oven thorough drying, take by weighing Eu then 2O 33.6953g, Y 2O 31.0161g, WO 318.5470g, Li 2CO 31.1082g, BaCO 33.9466g above raw material middle-weight rare earths oxide compound purity is 99.99% (quality), remaining all is an analytical pure.With the above-mentioned raw materials mixed grinding evenly after, put into crucible, be placed in the retort furnace in 600 ℃ and carry out pre-burning 5 hours, with the powder regrinding after the pre-burning to evenly, sintering 6 hours under 900 ℃ of conditions in retort furnace.With the sintered product that obtains carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, promptly obtain the red fluorescence powder of above-mentioned chemical expression.
Embodiment 3
Preparation Li 3Ba 2La 1.5Eu 1.5(WO 4) 8Red fluorescence powder
Desired raw material is placed the baking oven thorough drying, take by weighing Eu then 2O 32.6395g, La 2O 32.4435g, WO 318.5470g, Li 2CO 31.1082g, BaCO 33.9466g above raw material middle-weight rare earths oxide compound purity is 99.99% (quality), remaining all is an analytical pure.With the above-mentioned raw materials mixed grinding evenly after, put into crucible, be placed in the retort furnace in 600 ℃ and carry out pre-burning 5 hours, with the powder regrinding after the pre-burning to evenly, sintering 6 hours under 1000 ℃ of conditions in retort furnace.With the sintered product that obtains carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, promptly obtain the red fluorescence powder of above-mentioned chemical expression.
Embodiment 4
Preparation Li 3Ba 2Gd 2.4Eu 0.6(MoO 4) 8Red fluorescence powder
Desired raw material is placed the baking oven thorough drying, take by weighing Eu then 2O 30.5279g, Gd 2O 32.1750g, MoO 35.7575g, Li 2CO 30.5541g, BaCO 31.9733g above raw material middle-weight rare earths oxide compound purity is 99.99% (quality), remaining all is an analytical pure.With the above-mentioned raw materials mixed grinding evenly after, put into crucible, be placed in the retort furnace in 600 ℃ and carry out pre-burning 5 hours, with the powder regrinding after the pre-burning to evenly, sintering 6 hours under 1000 ℃ of conditions in retort furnace.With the sintered product that obtains carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, promptly obtain the red fluorescence powder of above-mentioned chemical expression.
Embodiment 5
Preparation Li 3Ba 2Y 1.8Eu 1.2(MoO 4) 8Red fluorescence powder
Desired raw material is placed the baking oven thorough drying, take by weighing Eu then 2O 31.0558g, Y 2O 31.0161g, MoO 35.7575g, Li 2CO 30.5541g, BaCO 31.9733g above raw material middle-weight rare earths oxide compound purity is 99.99% (quality), remaining all is an analytical pure.With the above-mentioned raw materials mixed grinding evenly after, put into crucible, be placed in the retort furnace in 600 ℃ and carry out pre-burning 5 hours, with the powder regrinding after the pre-burning to evenly, sintering 6 hours under 950 ℃ of conditions in retort furnace.With the sintered product that obtains carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, promptly obtain the red fluorescence powder of above-mentioned chemical expression.
Embodiment 6
Preparation Na 3Ba 2Gd 1.5Eu 1.5(MoO 4) 8The red fluorescence powder red fluorescence powder
Desired raw material is placed the baking oven thorough drying, take by weighing Eu then 2O 31.3198g, Gd 2O 31.3594g, MoO 35.7575g, Na 2CO 30.7949g, BaCO 31.9733g above raw material middle-weight rare earths oxide compound purity is 99.99% (quality), remaining all is an analytical pure.With the above-mentioned raw materials mixed grinding evenly after, put into crucible, be placed in the retort furnace in 600 ℃ and carry out pre-burning 5 hours, with the powder regrinding after the pre-burning to evenly, sintering 6 hours under 1000 ℃ of conditions in retort furnace.With the sintered product that obtains carry out fragmentation, select powder, pickling, washing, oven dry, cross 200 mesh sieves, promptly obtain the red fluorescence powder of above-mentioned chemical expression.

Claims (7)

1. white light LEDs is characterized in that with the silicate red fluorescent material of europkium-activated tungsten, and its chemical expression is: R 3 1R 2 2R 3 3-xEu x(R 4O 4) 8R wherein 1Be among Li, Na, K, Rb, Cs, the Ag one or more; R 2Be among Mg, Ca, Sr, Ba, the Zn one or more; R 3Be among Y, Gd, La, Lu, Pr, Sm, Ce, Tb, Bi, Al, the Cr one or more; R 4Be among Mo, the W one or more; 0≤x≤3 wherein.
2. white light LEDs is characterized in that with the preparation method of the silicate red fluorescent material of europkium-activated tungsten, and this method comprises the steps:
1. with R 1, R 2, R 3And Eu 3+Carbonate, nitrate salt or organic acid salt, and R 4Oxide compound, oxygen acid or oxysalt be raw material, desired raw material is placed the baking oven thorough drying, accurately take by weighing corresponding raw material and porphyrize respectively according to the mol ratio in the chemical expression.
2. the powder stock mixed grinding that 1. step is obtained is even.
3. the mixture that 2. step is obtained places retort furnace, under air atmosphere, 600 ℃～1200 ℃ sintering temperatures 1 hour～12 hours.
4. the product of roasting that 3. step is obtained carries out aftertreatment and promptly makes white light LEDs with the silicate red fluorescent material of tungsten.
3. white light LEDs according to claim 2 is with the preparation method of the silicate red fluorescent material of europkium-activated tungsten; It is characterized in that: above-mentioned steps 2. in; Can add volatile solvents such as zero(ppm) water or ethanol, acetone during mixed grinding, also can under the situation of solubilizing agent not, grind.
4. white light LEDs according to claim 2 is with the preparation method of the silicate red fluorescent material of europkium-activated tungsten; It is characterized in that: above-mentioned steps 3. in; Also can adopt two step calcination methods; Can be earlier 500～900 ℃ of sintering temperatures 1 hour～8 hours, then with powder mixed grinding once more, again 600 ℃～1200 ℃ sintering temperatures 1 hour～12 hours.
5. white light LEDs according to claim 2 is characterized in that with the preparation method of the silicate red fluorescent material of europkium-activated tungsten: above-mentioned steps 4. in, that aftertreatment has comprised is broken, select powder, removal of impurities, oven dry and classification.
6. white light LEDs according to claim 5 is characterized in that with the preparation method of the silicate red fluorescent material of europkium-activated tungsten: said removal of impurities comprises one or more in pickling, alkali cleaning, the washing.
According to claim 5 or 6 described white light LEDs with the preparation method of the silicate red fluorescent material of europkium-activated tungsten, it is characterized in that: said classification process can adopt one or more in the methods such as settling process, method of sieving, hydraulic classification or air classification.
CN2011104195611A 2011-12-15 2011-12-15 Europium-activated tungsten molybdate red fluorescent powder for white LED (Light Emitting Diode) and preparation method of europium-activated tungsten molybdate red fluorescent powder Pending CN102533266A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104078537A (en) * 2014-06-25 2014-10-01 南京工业大学 Method for preparing LED by means of quantum dot composite fluorescent particles
CN104371719A (en) * 2014-11-18 2015-02-25 安徽理工大学 Double-perovskite tungsten molybdate red fluorescent powder for white light LED and preparation method of double-perovskite tungsten molybdate red fluorescent powder
CN105400512A (en) * 2015-10-28 2016-03-16 常熟理工学院 Red tungstate fluorescent powder as well as preparation method and application thereof
CN107112397A (en) * 2014-09-10 2017-08-29 西博勒Ip I私人有限公司 Light-emitting device
CN107338051A (en) * 2017-06-28 2017-11-10 陕西科技大学 Samarium red fluorescence powder and preparation method thereof is mixed suitable for the molybdic acid alkali of white light LEDs
CN107365582A (en) * 2017-06-28 2017-11-21 陕西科技大学 Europium red fluorescence powder and preparation method thereof is mixed suitable for the molybdic acid alkali of white light LEDs
CN109943330A (en) * 2019-03-25 2019-06-28 常州工程职业技术学院 A kind of Cr3+The near-infrared fluorescent powder of activation, preparation method and application
CN110184060A (en) * 2019-06-19 2019-08-30 齐齐哈尔大学 Lithium molybdate doped yttrium samarium emitting red light powder and preparation method thereof
CN110862822A (en) * 2019-12-06 2020-03-06 成都理工大学 Molybdate-based red fluorescent powder and preparation method and application thereof
CN113462390A (en) * 2021-07-27 2021-10-01 上海同晔科技有限公司 Europium-doped tungsten molybdate red fluorescent powder and preparation method and application thereof
CN113481010A (en) * 2021-07-27 2021-10-08 上海同晔科技有限公司 Europium-doped tungstate red fluorescent powder and preparation method and application thereof
CN115820254A (en) * 2022-12-08 2023-03-21 广西贺源科技发展有限责任公司 Synthesis and application of near ultraviolet light excited molybdate red fluorescent powder

Non-Patent Citations (1)

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YEE-CHENG CHANG ET AL: "Synthesis and Photoluminescence Characteristics of High Color Purity and Brightness Li3Ba2Gd3(MoO4)8Eu3+ Red Phosphors", 《JOURNAL OF PHYSICAL CHEMISTRY C》 *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104078537A (en) * 2014-06-25 2014-10-01 南京工业大学 Method for preparing LED by means of quantum dot composite fluorescent particles
CN107112397B (en) * 2014-09-10 2019-12-17 西博勒Ip I私人有限公司 Light emitting device
CN107112397A (en) * 2014-09-10 2017-08-29 西博勒Ip I私人有限公司 Light-emitting device
CN104371719A (en) * 2014-11-18 2015-02-25 安徽理工大学 Double-perovskite tungsten molybdate red fluorescent powder for white light LED and preparation method of double-perovskite tungsten molybdate red fluorescent powder
CN105400512A (en) * 2015-10-28 2016-03-16 常熟理工学院 Red tungstate fluorescent powder as well as preparation method and application thereof
CN107338051A (en) * 2017-06-28 2017-11-10 陕西科技大学 Samarium red fluorescence powder and preparation method thereof is mixed suitable for the molybdic acid alkali of white light LEDs
CN107365582A (en) * 2017-06-28 2017-11-21 陕西科技大学 Europium red fluorescence powder and preparation method thereof is mixed suitable for the molybdic acid alkali of white light LEDs
CN109943330A (en) * 2019-03-25 2019-06-28 常州工程职业技术学院 A kind of Cr3+The near-infrared fluorescent powder of activation, preparation method and application
CN110184060A (en) * 2019-06-19 2019-08-30 齐齐哈尔大学 Lithium molybdate doped yttrium samarium emitting red light powder and preparation method thereof
CN110862822A (en) * 2019-12-06 2020-03-06 成都理工大学 Molybdate-based red fluorescent powder and preparation method and application thereof
CN113462390A (en) * 2021-07-27 2021-10-01 上海同晔科技有限公司 Europium-doped tungsten molybdate red fluorescent powder and preparation method and application thereof
CN113481010A (en) * 2021-07-27 2021-10-08 上海同晔科技有限公司 Europium-doped tungstate red fluorescent powder and preparation method and application thereof
CN115820254A (en) * 2022-12-08 2023-03-21 广西贺源科技发展有限责任公司 Synthesis and application of near ultraviolet light excited molybdate red fluorescent powder

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Application publication date: 20120704