CN102676152A - Flux for preparing green fluorescent powder for light emitting diode (LED) - Google Patents

Flux for preparing green fluorescent powder for light emitting diode (LED) Download PDF

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CN102676152A
CN102676152A CN201210141987XA CN201210141987A CN102676152A CN 102676152 A CN102676152 A CN 102676152A CN 201210141987X A CN201210141987X A CN 201210141987XA CN 201210141987 A CN201210141987 A CN 201210141987A CN 102676152 A CN102676152 A CN 102676152A
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led
grams
green fluorescent
fluorescent powder
flux
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CN102676152B (en
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师丽丽
顾竟涛
翟辉
杨勇
谢玉明
李依群
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SUZHOU INTERCHINA LIGHTING CO Ltd
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SUZHOU INTERCHINA LIGHTING CO Ltd
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Abstract

The invention discloses a flux for preparing green fluorescent powder for a light emitting diode (LED). The flux composition comprises the following components in part by weight: 5 to 20 parts of Li2CO3, 40 to 75 parts of Na3AlF6 and 20 to 40 parts of SrCO3; the green fluorescent powder for the LED can be prepared by mixing raw materials for the green fluorescent powder for the LED and the flux uniformly and sintering at a high temperature in a reductive atmosphere; through the green fluorescent powder for the LED, the initial brightness of the LED is improved; and the particle size distribution of the powder is improved, namely the particle size distribution is narrowed.

Description

A kind of fusing assistant for preparing LED with green emitting phosphor
Technical field
The invention belongs to LED fluorescent material technical field, relate to the fusing assistant of preparation LED fluorescent material, be specifically related to the fusing assistant of a kind of LED of preparation with green emitting phosphor.
Background technology
Along with developing rapidly of green light LED, also increasingly high to the requirement of fluorescent material, require fluorescent material to have higher brightness and good use properties.Except conditions such as purity of raw materials and calcination technology to the brightness of fluorescent material and use properties influential, the selection of fusing assistant also has very big shadow noon to the brightness and the use properties of fluorescent material.The effect of fusing assistant is: be used to reduce calcination temperature and improve percent crystallinity.Present fusing assistant is generally carbonate, fluorochemical, the muriate of basic metal or earth alkali metal etc., and boric acid and borate reduce sintering temperature and can be beneficial to aftertreatment, have also improved the optical property such as the light decay of fluorescent material.There is report to disclose MgF 2, AlF 3, Li 2CO 3And H 3BO 3Four kinds of materials prepare green emitting phosphor as fusing assistant, and its crystalline structure, granule-morphology and luminous intensity are compared Li 2CO 3And H 3BO 3All obtained good effect.
Summary of the invention
In order to reduce LED with the calcination temperature of green emitting phosphor and improve its percent crystallinity, the invention provides the flux composition of a kind of new preparation LED with green emitting phosphor.
According to the parts by weight meter, it contains the Li of 5-20 part to described preparation LED with the flux composition of green emitting phosphor 2CO 3, 40-75 part Na 3AlF 6, 20-40 part SrCO 3
Described flux composition usage quantity accounts for the 3%-20% of LED with the green emitting phosphor raw material weight.
Through adding above-mentioned flux composition, the LED of gained had both improved original intensity with green emitting phosphor, had improved the powder granule size-grade distribution again when preparing LED with green emitting phosphor; Make size distribution narrow, raw material sources of the present invention are extensive, and technology is simple; Cycle is short; Pollution-free, cost is low, is suitable for industrialized production.
Description of drawings
Fig. 1 uses the LED of fusing assistant according to the invention front and back with green emitting phosphor luminescent spectrum figure;
Fig. 2 is for using the preceding LED of fusing assistant according to the invention with green emitting phosphor particulate scan Electronic Speculum figure;
Fig. 3 is for using LED behind the fusing assistant according to the invention with a green emitting phosphor sem photograph.
Embodiment
Below in conjunction with embodiment and accompanying drawing preparation LED of the present invention is set forth with the fusing assistant of green emitting phosphor in detail; Thereby protection scope of the present invention is made more explicit defining so that advantage of the present invention and characteristic can be easier to it will be appreciated by those skilled in the art that.
Embodiment 1
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 3% of total batch mixing, respectively takes by weighing 1.5 grams, 5 grams, 7.5 grams respectively, amounts to 14 grams.Evenly the back is at 1350oC for batch mixing, and sintering is 4 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 2
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 5% of total batch mixing, respectively takes by weighing 4 grams, 5 grams, 14 grams respectively, amounts to 23 grams.Evenly the back is at 1200oC for batch mixing, and sintering is 5 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 3
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 8% of total batch mixing, respectively takes by weighing 3 grams, 8 grams, 25 grams respectively, amounts to 36 grams.Evenly the back is at 1300oC for batch mixing, and sintering is 3 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 4
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 10% of total batch mixing, respectively takes by weighing 4.5 grams, 16 grams, 24.5 grams respectively, amounts to 45 grams.Evenly the back is at 1200oC for batch mixing, and sintering is 3 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 5
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 10% of total batch mixing, respectively takes by weighing 3.5 grams, 17 grams, 24.5 grams respectively, amounts to 45 grams.Evenly the back is at 1250oC for batch mixing, and sintering is 2.5 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 6
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 13% of total batch mixing, respectively takes by weighing 6 grams, 16 grams, 37 grams respectively, amounts to 59 grams.Evenly the back is at 1200oC for batch mixing, and sintering is 3 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 7
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 16% of total batch mixing, respectively takes by weighing 13 grams, 20 grams, 39 grams respectively, amounts to 72 grams.Evenly the back is at 1250oC for batch mixing, and sintering is 3 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Embodiment 8
Take by weighing LED with total batch mixing 450 grams of green fluorescence powder raw material, fusing assistant is Li 2CO 3, SrCO 3, Na 3AlF 6Mixture, consumption is 20% of total batch mixing, respectively takes by weighing 10 grams, 21 grams, 59 grams respectively, amounts to 90 grams.Evenly the back is at 1280oC for batch mixing, and sintering is 4 hours under the reducing atmosphere, and aftertreatment promptly gets LED and uses the green emitting phosphor product after accomplishing.
Use particle diameter D10, D50, the D90 of LS-POP (6) laser particle size analyzer (Zhuhai OMEC Technology Co., Ltd.) specimen coating front and back; With the photoluminescence intensity of the fluorescent powder grain before and after the QP600-1-SR spectrum analyzer analysis of control coating, with the fluorescent powder grain before and after the KYKY-2800 type scanning electron microscope analysis coating.
Use the variation of fusing assistant according to the invention front and back LED with the green emitting phosphor grain diameter:
Figure BDA0000162084721
The LED of gained had both improved original intensity with green emitting phosphor, had improved the powder granule size-grade distribution again, made size distribution narrow.

Claims (2)

1. fusing assistant for preparing LED with green emitting phosphor, it is characterized in that: according to the parts by weight meter, it contains the Li of 5-20 part 2CO 3, 40-75 part Na 3AlF 6, 20-40 part SrCO 3
2. fusing assistant according to claim 1 is characterized in that: described fusing assistant usage quantity accounts for the 3%-20% of LED with the green emitting phosphor raw material weight.
CN201210141987.XA 2012-05-09 2012-05-09 Flux for preparing green fluorescent powder for light emitting diode (LED) Active CN102676152B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106544023A (en) * 2016-10-21 2017-03-29 北京宇极科技发展有限公司 A kind of preparation method of white light LEDs with the green powder of small particle LuAG

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1290199A (en) * 1998-12-08 2001-04-04 品川白炼瓦株式会社 Molding powder for continuous casting of steel and method for continuous casting of steel
CN101565613A (en) * 2009-06-01 2009-10-28 彩虹集团电子股份有限公司 Method for producing zinc-manganese silicate green fluorescent powder for PDP
CN101845303A (en) * 2010-05-29 2010-09-29 兰州大学 Method for preparing vacuum ultraviolet excited green aluminate fluorescent powder

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1290199A (en) * 1998-12-08 2001-04-04 品川白炼瓦株式会社 Molding powder for continuous casting of steel and method for continuous casting of steel
CN101565613A (en) * 2009-06-01 2009-10-28 彩虹集团电子股份有限公司 Method for producing zinc-manganese silicate green fluorescent powder for PDP
CN101845303A (en) * 2010-05-29 2010-09-29 兰州大学 Method for preparing vacuum ultraviolet excited green aluminate fluorescent powder

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
文小强: "助熔剂种类对绿色荧光粉(Ce0.67,Tb0.33)MgAl11O19晶体结构、形貌及发光强度的影响", 《江西有色金属》 *
郭美券: "助熔剂和还原气氛对掺铕硅酸锶荧光粉发光性能的影响", 《化工新型材料》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106544023A (en) * 2016-10-21 2017-03-29 北京宇极科技发展有限公司 A kind of preparation method of white light LEDs with the green powder of small particle LuAG

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