CN100575453C - A kind of orange light phosphor powder for white light LED and preparation method thereof - Google Patents

A kind of orange light phosphor powder for white light LED and preparation method thereof Download PDF

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CN100575453C
CN100575453C CN200610131687A CN200610131687A CN100575453C CN 100575453 C CN100575453 C CN 100575453C CN 200610131687 A CN200610131687 A CN 200610131687A CN 200610131687 A CN200610131687 A CN 200610131687A CN 100575453 C CN100575453 C CN 100575453C
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phosphor powder
white light
orange light
molar concentration
volumetric molar
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CN101168670A (en
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张家骅
郝振东
张霞
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Changchun Institute of Optics Fine Mechanics and Physics of CAS
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Abstract

The invention belongs to the luminescent material technical field, relate to a kind of orange light phosphor powder for white light LED, general formula is M 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, M is a kind of or any two kinds of combinations among Ca, Sr, the Ba; 0.001≤x≤0.05,0.04≤y≤0.16,0≤z≤0.05.This orange light phosphor powder preparation method: the oxide compound or the salt that take by weighing each element by the general formula stoichiometric ratio, and abundant porphyrize mixing, insert crucible, under 1200 ℃ of-1300 ℃ of temperature and carbon or hydrogen and nitrogen reductive condition, obtained sintered compact in roast 2-4 hour and be ground into powder promptly getting orange light phosphor powder.This orange light phosphor powder can be complementary with the near-ultraviolet light photodiode, is applied to the three primary colours white light LEDs as the orange light phosphor powder composition, and its preparation method is simple, and is pollution-free, and cost is low.

Description

A kind of orange light phosphor powder for white light LED and preparation method thereof
Technical field
The invention belongs to the luminescent material technical field, relate to a kind of white light LEDs orange light phosphor powder that is suitable near ultraviolet excitation and preparation method thereof.
Background technology
That white light LEDs (Light Emitting Diode) has is nontoxic, overlong service life (100,000 hours), energy-efficient, all solid state, plurality of advantages such as operating voltage is low, shock resistance and security are good, can be widely used on the various lighting installations, comprising indoor lamp, stop-light, street lamp, automobile with taillight, indicator, brake lamp, outdoor ultra-large type screen, display screen and billboard etc., is a kind of environmental protection, energy-conservation green illumination light source.
Realize that at present white light LEDs has multiple scheme, but most based on following three kinds of schemes.1. the blue led chip is formed white light LEDs with being organically combined by the gold-tinted fluorescent material that blue light effectively excites.The gold-tinted of fluorescent material emission and the blue light of tube core become white light.2. utilize the near-ultraviolet light led chip to launch the red, green, blue three primary colors fluorescent powder with can effectively being excited and organically combine the composition white light LEDs by UV-light.3. red, green, blue three-primary color LED chip or luminotron are assembled into a pixel (pixel), realize white light.Scheme 1. in because white light is to be formed by the yellow fluorescence of fluorescent material and the blue light of tube core, the glow color of device can change with the variation of driving voltage and fluorescent coating thickness, color reducibility is poor, colour rendering index is lower.Recently the 2. described near-ultraviolet light led chip that utilizes of scheme is launched the development of red, green, blue three primary colors fluorescent powder bonded white light LEDs rapidly with can effectively being excited by UV-light, this scheme has many advantages, particularly shows chromaticity matter and choosing at random property, high color rendering index (CRI) Ra＞90, light efficiency is high and selects aspects such as the high-efficiency fluorescence body is of a great variety for use.Yet the fluor that light conversion efficiency and thermal stability are good particularly can extremely be lacked by blue light and the efficient fluorescent red-orange body that nearly UV light effectively excites.
The end of the year 2004, the Korea S researchist has reported a kind of single-phase white-emitting phosphor (J.S.Kim, P.E.Jeon, J.C.Choi that is suitable near ultraviolet excitation, and H.L.Parka, S.I.Mho, G.C.Kim, Appl.Phys.Lett. Applied Physics wall bulletin, 84 volume (15) phases, 2931 pages, 2004), it consists of Ba 3MgSi 2O 8: Eu 2+, Mn 2+, but it is relatively low to constitute the red composition luminous efficiency of its white light.This year, the Japanology personnel have reported a kind of red fluorescence powder (Xianqing Piao that is suitable near ultraviolet excitation, Takashi Horikawa, Hiromasa Hanzawa, and Ken-ichi Machida, Appl.Phys.Lett. Applied Physics wall bulletin, 88 volumes, 161908 pages, 2006), it consists of Sr 2Si 5N 8: Eu 2+, but because the experiment condition harshness, the cost height also only rests on the laboratory development at present.
Summary of the invention
The present invention seeks to utilize of the orange photoemissive sensibilized of the royal purple light emission of Eu to Mn, provide a kind of can the 200nm-430nm wavelength light excite send down 500nm-700nm light be suitable for orange light phosphor powder for white light LED of near ultraviolet excitation and preparation method thereof.
Fluorescent material provided by the invention is a kind of alkaline earth pyrophosphate salt by rare earth element and magnesium-yttrium-transition metal Mn codoped, and general formula is M 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, wherein M represents a kind of or any two kinds of combinations among Ca, Sr, the Ba; X, y, z are mole number, and its span is: 0.001≤x≤0.05,0.04≤y≤0.16,0≤z≤0.05.
It is as follows that the present invention prepares the orange light phosphor powder for white light LED method:
1) by formula M 2-x-y-zP 2O 7: Eu x, Mn y, Dy zStoichiometric ratio takes by weighing oxide compound, DAP and Ca, a kind of or any two kinds of combination carbonate among Sr, the Ba or the hydrophosphate of Eu and Dy, the carbonate of Mn, and abundant porphyrize mixing;
2) mixture that step 1) is obtained is inserted crucible, put into High Temperature Furnaces Heating Apparatus, in High Temperature Furnaces Heating Apparatus, put into solid carbon, or feeding hydrogen and nitrogen, the volumetric molar concentration of hydrogen is less than 20%, and the volumetric molar concentration of nitrogen is greater than 80%, and hydrogen and nitrogen pressure are normal pressure, roast in 1200 ℃ of-1300 ℃ of temperature obtained sintered compact in roast 2-4 hour;
3) with step 2) sintered compact that obtains grinds becomes powder, promptly gets orange light phosphor powder.
Beneficial effect: adopt the inventive method synthetic fluorescent material can under the 200nm-430nm wavelength light excites, send 500nm-700nm light, thereby can be complementary with near-ultraviolet light photodiode commonly used at present, be applied to the three primary colours white light LEDs as the orange light phosphor powder composition, its preparation method is simple, pollution-free, cost is low.
Description of drawings
Fig. 1 is embodiment of the invention 6Ca 1.82P 2O 7: Eu 0.04, Mn 0.14Emmission spectrum (400nm excites) under the 200nm-430nm wavelength light excites.As can be seen from the figure, excite down Ca in the 400nm wavelength light 1.82P 2O 7: Eu 0.04, Mn 0.14The light of emission can reach more than 0.7 (a.u) near the light intensity 600nm wavelength.
Fig. 2 is embodiment of the invention 6Ca 1.82P 2O 7: Eu 0.04, Mn 0.14Excitation spectrum (monitoring 595nm).
Embodiment
Embodiment 1: preparation Ca 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, x=0.01 wherein, y=0.04, z=0 embody formula and are: Ca 1.95P 2O 7: Eu 0.01, Mn 0.04Take by weighing 212.16g CaHPO by stoichiometric ratio 4, 5.28g (NH 4) 2HPO 4, 3.68g MnCO 3, 1.41g Eu 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.Put into solid carbon in High Temperature Furnaces Heating Apparatus, solid carbon is 1: 1 with the weight ratio of the orange light phosphor powder that will prepare, and promptly obtains orange light phosphor powder Ca in 2 hours 1250 ℃ of heating 1.95P 2O 7: Eu 0.01, Mn 0.04
Embodiment 2: preparation Ca 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, x=0.01 wherein, y=0.08, z=0.01 embody formula and are: Ca 1.90P 2O 7: Eu 0.01, Mn 0.08, Dy 0.01Take by weighing 206.80g CaHPO by stoichiometric ratio 4, 10.56g (NH 4) 2HPO 4, 7.36g MnCO 3, 1.41g Eu 2O 3, 1.49g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 2 hours 1250 ℃ of heating 1.90P 2O 7: Eu 0.01, Mn 0.08, Dy 0.01
Embodiment 3: preparation Ca 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, x=0.02 wherein, y=0.04, z=0.02 embody formula and are: Ca 1.92P 2O 7: Eu 0.02, Mn 0.04Dy 0.02Take by weighing 208.90gCaHPO by stoichiometric ratio 4, 8.45g (NH 4) 2HPO 4, 3.68g MnCO 3, 2.82g Eu 2O 3, 2.98g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 2 hours 1250 ℃ of heating 1.92P 2O 7: Eu 0.02, Mn 0.04Dy 0.02
Embodiment 4: preparation Ca 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, x=0.03 wherein, y=0.10, z=0.04 embody formula and are: Ca 1.83P 2O 7: Eu 0.03, Mn 0.10Dy 0.04Take by weighing 199.10gCaHPO by stoichiometric ratio 4, 17.96g (NH 4) 2HPO 4, 9.20g MnCO 3, 4.23g Eu 2O 3, 5.96g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 2 hours 1250 ℃ of heating 1.83P 2O 7: Eu 0.03, Mn 0.10Dy 0.04
Embodiment 5: preparation Ca 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, x=0.04 wherein, y=0.12, z=0.04 embody formula and are: Ca 1.80P 2O 7: Eu 0.04, Mn 0.12Dy 0.04Take by weighing 195.84gCaHPO by stoichiometric ratio 4, 21.20g (NH 4) 2HPO 4, 11.04g MnCO 3, 5.64g Eu 2O 3, 5.96g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 4 hours 1200 ℃ of heating 1.80P 2O 7: Eu 0.04, Mn 0.12Dy 0.04
Embodiment 6: preparation Ca 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, x=0.04 wherein, y=0.14, z=0 embody formula and are: Ca 1.82P 2O 7: Eu 0.04, Mn 0.14Take by weighing 198.02g CaHPO by stoichiometric ratio 4, 19.01g (NH 4) 2HPO 4, 12.88g MnCO 3, 5.64g Eu 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 2 hours 1250 ℃ of heating 1.82P 2O 7: Eu 0.04, Mn 0.14
Embodiment 7: preparation Ca 2-x-yP 2O 7: Eu x, Mn y, Dy z, x=0.05 wherein, y=0.14, z=0.04 embody formula and are: Ca 1.77P 2O 7: Eu 0.04, Mn 0.16Dy 0.05Take by weighing 192.58gCaHPO by stoichiometric ratio 4, 24.29g (NH 4) 2HPO 4, 12.88g MnCO 3, 7.04g Eu 2O 3, 5.96g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 4 hours 1200 ℃ of heating 1.77P 2O 7: Eu 0.05, Mn 0.14Dy 0.04
Embodiment 8: preparation Ca 2-x-yP 2O 7: Eu x, Mn y, Dy z, x=0.05 wherein, y=0.16, z=0.05, the formula of embodying is: Ca 1.76P 2O 7: Eu 0.05, Mn 0.14, Dy 0.05Take by weighing 191.49g CaHPO by stoichiometric ratio 4, 25.35g (NH 4) 2HPO 4, 14.72g MnCO 3, 7.04g Eu 2O 3, 7.45g Dy 2O 3Behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ca in 4 hours 1200 ℃ of heating 1.76P 2O 7: Eu 0.05, Mn 0.14, Dy 0.05
Embodiment 9: preparation Ba 2-x-yP 2O 7: Eu x, Mn y, Dy z, x=0.05 wherein, y=0.14, z=0.04 embody formula and are: Ba 1.77P 2O 7: Eu 0.04, Mn 0.16Dy 0.05Take by weighing 279.42gBaCO by stoichiometric ratio 3, 211.2 (NH 4) 2HPO 4, 12.88g MnCO 3, 7.04g Eu 2O 3, 5.96g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Ba in 3 hours 1200 ℃ of heating 1.77P 2O 7: Eu 0.05, Mn 0.14Dy 0.04
Embodiment 10: preparation Sr 2-x-yP 2O 7: Eu x, Mn y, Dy z, x=0.05 wherein, y=0.14, z=0.04 embody formula and are: Sr 1.77P 2O 7: Eu 0.04, Mn 0.16Dy 0.05Take by weighing 209.05g SrCO by stoichiometric ratio 3, 211.2g (NH 4) 2HPO 4, 12.88g MnCO 3, 7.04g Eu 2O 3, 5.96g Dy 2O 3, behind the abundant porphyrize mixing of the raw material that takes by weighing, insert high-purity corundum crucible or platinum crucible, put into High Temperature Furnaces Heating Apparatus.At H 2And N 2(H under the reducing atmosphere condition 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%), reducing gas is under the normal pressure, promptly obtains orange light phosphor powder Sr in 3 hours 1200 ℃ of heating 1.77P 2O 7: Eu 0.05, Mn 0.14Dy 0.04

Claims (9)

1, a kind of orange light phosphor powder for white light LED of near ultraviolet excitation is characterized in that general formula is M 2-x-y-zP 2O 7: Eu x, Mn y, Dy z, wherein M is a kind of or any two kinds of combinations among Ca, Sr, the Ba; X, y, z are mole number, and its span is: 0.001≤x≤0.05,0.04≤y≤0.16,0≤z≤0.05.
2, the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 1 is characterized in that x=0.03; Y=0.10; Z=0.04.
3, the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 1 is characterized in that x=0.01; Y=0.08; Z=0.01.
4, the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 1 is characterized in that x=0.04; Y=0.12; Z=0.04.
5, the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 1 is characterized in that x=0.04; Y=0.14; Z=0.
6, the preparation method of the orange light phosphor powder for white light LED of the described near ultraviolet excitation of a kind of claim 1 is characterized in that following steps:
1) by formula M 2-x-y-zP 2O 7: Eu x, Mn y, Dy zStoichiometric ratio takes by weighing oxide compound, DAP and Ca, a kind of or any two kinds of combination carbonate among Sr, the Ba or the hydrophosphate of Eu and Dy, the carbonate of Mn, and abundant porphyrize mixing;
2) mixture that step 1) is obtained is inserted crucible, put into High Temperature Furnaces Heating Apparatus, in High Temperature Furnaces Heating Apparatus, put into solid carbon, or feeding hydrogen and nitrogen, the volumetric molar concentration of hydrogen is less than 20%, and the volumetric molar concentration of nitrogen is greater than 80%, and hydrogen and nitrogen gas pressure are normal pressure, roast in 1200 ℃ of-1300 ℃ of temperature obtained sintered compact in roast 2-4 hour;
3) with step 2) sintered compact that obtains grinds becomes powder.
7, the preparation method of the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 6 is characterized in that the roast temperature is 1250 ℃, H 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%, the roast time is 2 hours.
8, the preparation method of the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 6 is characterized in that the roast temperature is 1200 ℃, H 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%, the roast time is 3 hours.
9, the preparation method of the orange light phosphor powder for white light LED of near ultraviolet excitation according to claim 6 is characterized in that the roast temperature is 1200 ℃, H 2Volumetric molar concentration be 5%, N 2Volumetric molar concentration be 95%, the roast time is 4 hours.
CN200610131687A 2006-11-30 2006-11-30 A kind of orange light phosphor powder for white light LED and preparation method thereof Expired - Fee Related CN100575453C (en)

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CN101962543A (en) * 2009-09-29 2011-02-02 鹤壁佳多科工贸有限责任公司 Europium-excited strontium phosphate near-ultraviolet fluorescent powder
CN102097574A (en) * 2010-12-14 2011-06-15 山西乐百利特科技有限责任公司 Led
CN102250614B (en) * 2011-05-19 2013-11-27 中国科学院长春光学精密机械与物理研究所 High brightness mechanical luminescent material and preparation method thereof
CN102796984B (en) * 2011-05-23 2014-07-09 海洋王照明科技股份有限公司 Multielement-doped strontium phosphate luminescent film, and preparation method and applications thereof
CN115491202B (en) * 2022-10-17 2023-05-23 云南大学 Dysprosium-europium co-doped tellurium phosphate fluorescent powder for white light LED and microwave solid phase synthesis method thereof

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