CN1186103A - Green fluorescent powder and preparation thereof - Google Patents

Green fluorescent powder and preparation thereof Download PDF

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Publication number
CN1186103A
CN1186103A CN 96123003 CN96123003A CN1186103A CN 1186103 A CN1186103 A CN 1186103A CN 96123003 CN96123003 CN 96123003 CN 96123003 A CN96123003 A CN 96123003A CN 1186103 A CN1186103 A CN 1186103A
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China
Prior art keywords
fluorescent material
matrix
sio
preparation
fusing assistant
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Pending
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CN 96123003
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Chinese (zh)
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刘行仁
林海
张晓�
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CHANGCHUN PHYS INST CHINESE
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CHANGCHUN PHYS INST CHINESE
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Priority to CN 96123003 priority Critical patent/CN1186103A/en
Publication of CN1186103A publication Critical patent/CN1186103A/en
Pending legal-status Critical Current

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Abstract

A green fluorescent powder is rare-earth element activated magnesium zinc calcium chlorosilicate. It has a chemical expression : Ca8Mg1-aZna(SiO4)4Cl2 : xEu2+, yM, where M=Ce3+ and Mn2+; Ca can be replaced by less Sr or Ba; a is 0-1.0; x is 0-0.2; and y is 0-0.1 mol. Said green fluorescent powder has stable performance and high energy transformation efficiency.

Description

A kind of green emitting phosphor and preparation method thereof
The present invention relates to a kind of is green emitting phosphor of matrix and preparation method thereof with chlorine Magnesium Silicate q-agent zinc calcium.
Under long wave ultraviolet light excites, launched efficiently in the past and mainly contained in the green fluorescent material: zinc sulphide type and alkaline earth sulfide fluorescent material, as ZnS:Cu, ZnS:Cu, Al, CaS:Ce etc.But they are unsettled materials, easily decompose in air, the fluorescent material performance is descended greatly, even can decompose and emit deleterious hydrogen sulfide, harm environment and health.
The purpose of this invention is to provide a kind of stable performance, the green emitting phosphor that energy conversion rate is high.
Fluorescent material of the present invention is rare-earth activated chlorine Magnesium Silicate q-agent zinc calcium, and its chemical expression is as follows:
Ca 3Mg 1-aZn a(SiO 4) 4Cl 2：XEu 2+，yM
Wherein: M is Ce 3+And Mn 2+, a small amount of Sr, Ba can replace Ca; In the formula, 0≤a≤1,0≤x≤0.2,0≤y≤0.1 mole.
By stoichiometric ratio CaCO 3: MgO (ZnO): SiO 2: CaCl 2=7: 1: 4: 1 mol ratio is produced the matrix of fluorescent material, excessive CaCl 2Can play the fusing assistant effect, the amount of taking by weighing is 1.0-2.5 a times of calculated amount, and activator is Eu 2+, sensitizing agent is Ce 3+, fusing assistant is Li 2CO 3, above-mentioned raw materials fully grind be mixed even after, in the weakly reducing atmosphere under 1000-1200 ℃ calcination 1-3 hour, can obtain required fluorescent material, its body colour is a yellow-green colour, with Eu 2+Concentration increases and deepens, and concerning zinciferous compound, synthesizes zinciferous matrix, this matrix and adulterated activator Eu then earlier in air 2+, sensitizing agent Ce 3+, fusing assistant Li 2CO 3Deng mixing, synthetic required fluorescent material in high-temperature reductibility atmosphere, reducing atmosphere can be 95%N 2+ 5%H 2(volume ratio) mixed gas, the also gas of generation but carbon granules burns in air.
Providing embodiment below is described specifically the present invention.
Embodiment one, take by weighing CaCO 321.00g, MgO1.21g, SiO 27.21g, CaCl 25.01g, Eu 2O 30.528g and Li 2CO 31.03g.It is even that above-mentioned raw materials mill is mixed, and in the reducing atmosphere, 1100 ℃ of calcinations 3 hours are taken out, and use deionized water wash, sieve, and dry, and it is yellowish green obtaining body colour, consists of Ca 8Mg (SiO 4) 4Cl 2: 0.1Eu 2+Divalent europium activated calcium magnesium chloro-silicate fluorescent material.This fluorescent material excites down at 365nm, the green glow of emitting bright.
Embodiment two, take by weighing CeO 20.052g all the other conditions obtain Ca with embodiment one 8Mg (SiO 4) 4Cl 2: 0.1Eu 2+, 0.01Ce 3+Fluorescent material, its body colour are oyster, in UV-light and blue-light excited following, launch the green glow of very strong band indigo plant, and its luminance factor is not mixed Ce 3+The fluorescent material height.
Embodiment three, take by weighing Eu 2O 30.158g, CeO 20.155g other condition obtains the Ca that body colour is an oyster with embodiment one 3Mg (SiO 4) 4Cl 2: 0.03Eu 2+, 0.03Ce 3+Fluorescent material, exciting down at 365nm, its green emitting intensity is not mix Ce 3+1.5 times.
Embodiment four, take by weighing CaCO 321.00g, ZnO2.44g, SiO 27.21g, CaCl 210.00g mix grinding is even, in 1220 ℃ of constant temperature numbers minute, temperature was reduced to 1160 ℃ of constant temperature rapidly 3 hours, obtained Ca aZn (SiO 4) 4Cl 2White polycrystalline substrate material.Take by weighing Eu 2O 3Activator 0.158g, Li 2CO 3The chlorine zinc silicate calcium matrix mix grinding of fusing assistant 1.03g and above-mentioned acquisition is even, and calcination is 3 hours in 1000 ℃ of weakly reducing atmospheres, and all the other conditions are with embodiment one, and obtaining body colour is the divalent europium activated chlorine zinc silicate calcium Ca of oyster 8Zn (SiO 4) 4Cl 2: 0.03Eu 2+Fluorescent material.
Embodiment five, take by weighing CeO 20.052g all the other conditions obtain the coactivated Ca of divalent europium and trivalent cerium with embodiment four 8Zn (SiO 4) 4Cl 2: 0.03Eu 2+, 0.01Ce 3+Fluorescent material.
Embodiment six, take by weighing CaCO 321.00g, MgO0.61g, ZnO1.22g, CaCl 26.66g, Li 2CO 31.03g mill is mixed evenly, puts into High Temperature Furnaces Heating Apparatus, in 1220 ℃ of constant temperature numbers minute, constant temperature was 3 hours after temperature was reduced to 1160 ℃, and washing is sieved, and obtains Ca after the oven dry 8Mg 0.5Zn 0.5(SiO 4) 4Cl 2White matrix.Take by weighing Eu then 2O 30.158g, CeO 20.052g and above-mentioned matrix mix grinding is even, weakly reducing atmosphere calcination 3 hours, obtains light yellow Ca under 1100 ℃ 8Mg 0.5Zn 0.5(SiO 4) 4Cl 2: 0.03Eu 2+, 0.01Ce 3+Fluorescent material.

Claims (2)

1, a kind of green emitting phosphor is characterized in that fluorescent material is rare-earth activated chlorine Magnesium Silicate q-agent zinc calcium, and its chemical expression is as follows:
Ca 8Mg 1-aZn a(SiO 4) 4Cl 2：XEu 2+，yM
Wherein: M is Ce 3+And Mn 2+, a small amount of Sr, Ba can replace Ca; In the formula, 0≤a≤1,0≤x≤0.2,0≤y≤0.1 mole.
2, a kind of preparation method of green emitting phosphor is characterized in that by stoichiometric ratio CaCO 3: MgO (ZnO): SiO 2: CaCl 2=7: the matrix of 1: 4: 1 mol ratio preparation fluorescent material, excessive CaCl 2Can play the fusing assistant effect, the amount of taking by weighing is 1.0-2.5 a times of calculated amount, and activator is Eu 2+, sensitizing agent is Ce 3+, fusing assistant is Ll 2CO 3, above-mentioned raw materials fully grind be mixed even after, in the weakly reducing atmosphere 1000-1200 ℃ under calcination 1-3 hour, zinciferous compound is then synthesized zinciferous matrix, this matrix and adulterated activator Eu then earlier in air 2+, sensitizing agent Ce 3+, fusing assistant Li 2CO 3Deng mixing, synthetic required fluorescent material in high-temperature reductibility atmosphere, reducing atmosphere can be 95%N 2+ 5%H 2(volume ratio) mixed gas, the also gas of generation but carbon granules burns in air.
CN 96123003 1996-12-26 1996-12-26 Green fluorescent powder and preparation thereof Pending CN1186103A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 96123003 CN1186103A (en) 1996-12-26 1996-12-26 Green fluorescent powder and preparation thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 96123003 CN1186103A (en) 1996-12-26 1996-12-26 Green fluorescent powder and preparation thereof

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CN1186103A true CN1186103A (en) 1998-07-01

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CN 96123003 Pending CN1186103A (en) 1996-12-26 1996-12-26 Green fluorescent powder and preparation thereof

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1325603C (en) * 2003-11-27 2007-07-11 上海交通大学 Long-time afterglow luminescent silicate material and its producing method
CN100383988C (en) * 2003-08-20 2008-04-23 刘行仁 White light LED and light converting luminophore
CN101010413B (en) * 2004-09-07 2010-08-25 住友化学株式会社 Phosphor, phosphor paste and light-emitting device
WO2012000176A1 (en) * 2010-06-29 2012-01-05 海洋王照明科技股份有限公司 Fluorescent powder of halogen silicate containing nano-metal particles and preparaion method thereof
CN101307229B (en) * 2007-04-05 2012-07-04 株式会社小糸制作所 Phosphor
CN1729267B (en) * 2002-12-20 2012-12-19 丰田合成株式会社 Phosphor and optical device using same
CN102925153A (en) * 2012-11-23 2013-02-13 中国科学院长春光学精密机械与物理研究所 Color-adjustable single-phase fluorescent material and application thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1729267B (en) * 2002-12-20 2012-12-19 丰田合成株式会社 Phosphor and optical device using same
CN100383988C (en) * 2003-08-20 2008-04-23 刘行仁 White light LED and light converting luminophore
CN1325603C (en) * 2003-11-27 2007-07-11 上海交通大学 Long-time afterglow luminescent silicate material and its producing method
CN101010413B (en) * 2004-09-07 2010-08-25 住友化学株式会社 Phosphor, phosphor paste and light-emitting device
CN101307229B (en) * 2007-04-05 2012-07-04 株式会社小糸制作所 Phosphor
WO2012000176A1 (en) * 2010-06-29 2012-01-05 海洋王照明科技股份有限公司 Fluorescent powder of halogen silicate containing nano-metal particles and preparaion method thereof
CN102933685A (en) * 2010-06-29 2013-02-13 海洋王照明科技股份有限公司 Fluorescent powder of halogen silicate containing nano-metal particles and preparaion method thereof
US8956553B2 (en) 2010-06-29 2015-02-17 Ocean's King Lighting Science & Technology Co., Ltd. Fluorescent powder of halogen silicate containing nano-metal particles and preparation method thereof
CN102925153A (en) * 2012-11-23 2013-02-13 中国科学院长春光学精密机械与物理研究所 Color-adjustable single-phase fluorescent material and application thereof
CN102925153B (en) * 2012-11-23 2014-01-15 中国科学院长春光学精密机械与物理研究所 Color-adjustable single-phase fluorescent material and application thereof

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