CN101717633A - Preparation method of europium-activated aluminate blue fluorescent powder - Google Patents

Preparation method of europium-activated aluminate blue fluorescent powder Download PDF

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CN101717633A
CN101717633A CN200910309873A CN200910309873A CN101717633A CN 101717633 A CN101717633 A CN 101717633A CN 200910309873 A CN200910309873 A CN 200910309873A CN 200910309873 A CN200910309873 A CN 200910309873A CN 101717633 A CN101717633 A CN 101717633A
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preparation
fluorescent powder
europium
temperature
blue fluorescent
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CN101717633B (en
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陈伟
万国江
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JIANGMEN KEHENG INDUSTRY Co Ltd
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JIANGMEN KEHENG INDUSTRY Co Ltd
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Abstract

The invention discloses a preparation method of europium-activated aluminate blue fluorescent powder. The preparation method comprises the following steps of: weighing soluble salts of corresponding elements according to compositions of the fluorescent powder, and preparing into a mixed solution; adjusting the pH value of the mixed solution into 1 to 3 by using an alkaline solution, obtaining a precursor mixed solution, introducing into an ultrasonic sprayer, conveying into a reaction furnace by carrier gas, controlling the temperature of the reaction furnace to be 800-1100 DEG C, and reacting for 2-5min to obtain a precursor; putting the precursor into a microwave reaction furnace, reacting for 15-30min in the reducing atmosphere of 800-1200 DEG C, then reducing the temperature to room temperature in the reducing atmosphere, washing and drying to obtain a finished product. The method has simple steps, easy control of reaction conditions, short sintering time, low reaction temperature, less energy consumption, energy saving, environmental protection and prolonging of the service life of a device; and the prepared fluorescent powder is beneficial to coating, and has loose powder body, approximately spherical granules, even grain diameter distribution, no grinding, good brightness and heat stability.

Description

A kind of preparation method of europium-activated aluminate blue fluorescent powder
Technical field
The present invention relates to a kind of preparation method of blue colour fluorescent powder, particularly a kind of preparation method of europium-activated aluminate blue fluorescent powder.
Background technology
Plasma flat-plate shows that PDP has advantages such as ultra-thin, high-resolution, big picture, by universally acknowledged be the one preferred technique of wall-hanging high definition television HDTV, and fluorescent material plays decisive role to the PDP performance.
The general formula of europium-activated aluminate blue fluorescent powder is (Ba 1-x-z, Sr z) Mg yAl 10O 17: Eu x(wherein: 0.05≤x≤0.15; 0≤z≤0.25; 1.0≤y≤1.4), this kind is the excellent efficient blue fluorescent material of plasma display at vacuum ultraviolet-excited quantum yield height, high color purity down.
Produce this blue colour fluorescent powder at present both at home and abroad adopts high temperature solid-state method synthetic more, for example US3937998, US6096243, CN85100242, CN1091149, CN1129727, CN1189535, CN1203208 etc., adopt the high temperature solid-state method synthesis temperature up to 1500 ℃, the fluorescent material that obtains is reunited, particle diameter is thick, can't be directly used in and be coated with screen, must reduce particle diameter through ball mill pulverizing earlier.
Pulverize crystal morphology, introducing impurity that ball milling can destroy fluorescent material, reduce the thermostability and the luminosity of fluorescent material, light decay is bigger.
The light decay that the crystal grain deterioration that causes for the elimination ball mill pulverizing causes, people have explored some new europium-activated aluminate blue fluorescent powder synthetic methods, as sol-gel method (as CN1197831, CN1334309, CN1903977A etc.), coprecipitation method etc., though these methods can reduce synthesis temperature, but technology is complicated, can not get the little spheroidal particle that is evenly distributed of particle diameter equally.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of new europium-activated aluminate blue fluorescent powder.
The technical solution used in the present invention is:
A kind of preparation method of europium-activated aluminate blue fluorescent powder may further comprise the steps:
1) according to the composition of fluorescent material, take by weighing the water-soluble salt of respective element, be mixed with mixing solutions;
2) use basic solution to regulate mixing solutions pH value to 1～3, obtain precursor mixed solution;
3) precursor mixed solution is imported in the ultrasonic nebulizer, send in the Reaktionsofen by carrier gas, the temperature of control Reaktionsofen is 800 ℃～1100 ℃, and reaction 1～5min obtains presoma;
4) presoma is placed the microwave reaction stove, the microwave reaction furnace temperature is 800 ℃～1200 ℃, reacts 10～30min in the reducing atmosphere in the microwave reaction stove;
5) drop to room temperature in the reducing atmosphere, the gained powder is dismissed in deionized water naturally, with the salpeter solution washing, is washed till neutrality with deionized water at last, and oven dry promptly obtains finished product.
The invention has the beneficial effects as follows:
The inventive method step is simple, and reaction conditions is easy to control; Sintering time is short, and temperature of reaction is low, and the energy of consumption is few, energy-conserving and environment-protective, has prolonged work-ing life of equipment; The fluorescent material powder of preparation is loose, is roughly spheroidal particle, size distribution is even, need not to grind, and brightness and Heat stability is good are beneficial to and are coated with screen.
Description of drawings
Fig. 1 is the XRD figure of the embodiment of the invention 1;
Fig. 2 is the SEM figure of the embodiment of the invention 1;
Fig. 3 is the SEM figure of Comparative Examples 1;
Fig. 4 is exciting and emmission spectrum figure of the embodiment of the invention 1.
Embodiment
Below in conjunction with example, further specify the present invention.
Embodiment 1:Ba 0.9MgAl 10O 17: Eu 0.1
1) gets Ba (NO 3) 2Solution (0.4mol/L) 90ml, Al (NO 3) 3Solution (1mol/L) 400ml, Mg (NO 3) 2Solution (0.4mol/L) 100ml, Eu (NO 3) 3Solution (0.2mol/L) 20ml mixes, and obtains mixing solutions;
2) use ammoniacal liquor to regulate the pH=2 of mixing solutions, obtain precursor solution;
3) precursor mixed solution is imported in the ultrasonic nebulizer, send in the Reaktionsofen by carrier gas, the temperature of control Reaktionsofen is 800 ℃, and reaction 5min obtains presoma;
4) presoma is placed the microwave reaction stove, the microwave reaction furnace temperature is 1000 ℃, (N in the reducing atmosphere in the microwave reaction stove 2: H 2=9: 1) reaction 25min;
5) drop to room temperature in the reducing atmosphere, the gained powder is dismissed in deionized water naturally, with the salpeter solution washing, is washed till neutrality with deionized water at last, and oven dry promptly obtains finished product.
Embodiment 2:Ba 0.88MgAl 10O 17: Eu 0.12
1) gets Ba (NO 3) 2Solution (0.4mol/L) 88ml, Al (NO 3) 3Solution (1mol/L) 400ml, Mg (NO 3) 2Solution (0.4mol/L) 100ml, Eu (NO 3) 3Solution (0.2mol/L) 24ml mixes, and obtains mixing solutions;
2) use urea soln to regulate the pH=1 of mixing solutions, obtain precursor solution;
3) precursor mixed solution is imported in the ultrasonic nebulizer, send in the Reaktionsofen by carrier gas, the temperature of control Reaktionsofen is 900 ℃, and reaction 4min obtains presoma;
4) presoma is placed the microwave reaction stove, the microwave reaction furnace temperature is 1200 ℃, reducing atmosphere (N in the microwave reaction stove 2: H 2=1: reaction 15min 1);
5) drop to room temperature in the reducing atmosphere, the gained powder is dismissed in deionized water naturally, with the salpeter solution washing, is washed till neutrality with deionized water at last, and oven dry promptly obtains finished product.
Embodiment 3:Ba 0.9Mg 1.1Al 10O 17: Eu 0.1
1) gets Ba (NO 3) 2Solution (0.4mol/L) 90ml, Al (NO 3) 3Solution (1mol/L) 400ml, Mg (NO 3) 2Solution (0.4mol/L) 110ml, Eu (NO 3) 3Solution (0.2mol/L) 20ml mixes, and obtains mixing solutions;
2) use ammoniacal liquor to regulate the pH=3 of mixing solutions, obtain precursor solution;
3) precursor mixed solution is imported in the ultrasonic nebulizer, send in the Reaktionsofen by carrier gas, the temperature of control Reaktionsofen is 1100 ℃, and reaction 2min obtains presoma;
4) presoma is placed the microwave reaction stove, the microwave reaction furnace temperature is 1100 ℃, (N in the reducing atmosphere in the microwave reaction stove 2: H 2=1: 3) reaction 20min;
5) drop to room temperature in the reducing atmosphere, the gained powder is dismissed in deionized water naturally, with the salpeter solution washing, is washed till neutrality with deionized water at last, and oven dry promptly obtains finished product.
Embodiment 4:(Ba 0.7Sr 0.2) MgAl 10O 17: Eu 0.1
1) gets Ba (NO 3) 2Solution (0.4mol/L) 70ml, Sr (NO 3) 2Solution (0.4mol/L) 20ml, Al (NO 3) 3Solution (1mol/L) 400ml, Mg (NO 3) 2Solution (0.4mol/L) 100ml, Eu (NO 3) 3Solution (0.2mol/L) 20ml mixes, and obtains mixing solutions;
2) use ammoniacal liquor to regulate the pH=2 of mixing solutions, obtain precursor solution;
3) precursor mixed solution is imported in the ultrasonic nebulizer, send in the Reaktionsofen by carrier gas, the temperature of control Reaktionsofen is 1000 ℃, and reaction 3min obtains presoma;
4) presoma is placed the microwave reaction stove, the microwave reaction furnace temperature is 800 ℃, (CO) reaction 30min in the reducing atmosphere in the microwave reaction stove;
5) drop to room temperature in the reducing atmosphere, the gained powder is dismissed in deionized water naturally, with the salpeter solution washing, is washed till neutrality with deionized water at last, and oven dry promptly obtains finished product.
The chemical constitution of Comparative Examples is than identical with the chemical chemical constitution of corresponding embodiment, and is identical with the chemical constitution of embodiment 1 as Comparative Examples 1, different just its preparation methods.The preparation method of Comparative Examples is as follows:
1) takes by weighing corresponding raw material, add H 3BO 3As fusing assistant, 1450 ℃ of sintering 4h pulverize ball milling and obtain work in-process;
2) with work in-process in 1400 ℃, N 2: H 2Reduction 4h cool to room temperature in same reducing atmosphere in=9: 1 the atmosphere;
3) the sinter ball milling is arrived the about 6 μ m of median size, with the salpeter solution washing, be washed till neutrality with deionized water at last, oven dry promptly obtains finished product.
The performance perameter of each embodiment and Comparative Examples is as shown in table 1.
Table 1 fluorescent material performance perameter table
Numbering D 50(μm) λp(nm) Br％ ΔBr％(600℃，0.5h)
Embodiment 1 2 450 100.5 2.5
Embodiment 2 2 450 102.3 2.3
Embodiment 3 2 449 99.5 2.8
Embodiment 4 2 452 102.0 2.7
Comparative Examples 1 6 450 101.5 4.2
Comparative Examples 2 6 450 103.7 4.5
Comparative Examples 3 6 449 100.1 3.9
Comparative Examples 4 6 452 103.6 ?4.3
Fig. 1 is the XRD figure of the embodiment of the invention 1, and the spectral line of spectral line and standard substance matches.
Fig. 2 is the SEM figure of the embodiment of the invention 1, can be clearly seen that from figure fluorescent material of the present invention is spherical in shape or subsphaeroidal substantially, and particle is little, need not to grind, and granular size is comparatively even, is beneficial to very much to be coated with screen.
Fig. 3 is the SEM figure of Comparative Examples 1, and as can be seen from the figure, the powder after grinding is an irregular body, and size distribution is inhomogeneous, is unfavorable for being coated with screen.
Fig. 4 is exciting and emmission spectrum figure of the embodiment of the invention 1.
The inventive method step is simple, and reaction conditions is easy to control; Sintering time is short, and temperature of reaction is low, and the energy of consumption is few, energy-conserving and environment-protective, has prolonged work-ing life of equipment; The fluorescent material powder of preparation is loose, is roughly spheroidal particle, size distribution is even, need not to grind, and brightness and Heat stability is good are beneficial to and are coated with screen.

Claims (4)

1. the preparation method of an europium-activated aluminate blue fluorescent powder may further comprise the steps:
1) according to the composition of fluorescent material, take by weighing the water-soluble salt of respective element, be mixed with mixing solutions;
2) use basic solution to regulate mixing solutions pH value to 1～3, obtain precursor mixed solution;
3) precursor mixed solution is imported in the ultrasonic nebulizer, send in the Reaktionsofen by carrier gas, the temperature of control Reaktionsofen is 800 ℃～1100 ℃, and reaction 2～5min obtains presoma;
4) presoma is placed the microwave reaction stove, the microwave reaction furnace temperature is 800 ℃～1200 ℃, reacts 15～30min in the reducing atmosphere in the microwave reaction stove;
5) drop to room temperature in the reducing atmosphere, the gained powder is dismissed in deionized water naturally, with the salpeter solution washing, is washed till neutrality with deionized water at last, and oven dry promptly obtains finished product.
2. the preparation method of a kind of europium-activated aluminate blue fluorescent powder according to claim 1 is characterized in that described water-soluble salt is preferably nitrate.
3. the preparation method of a kind of europium-activated aluminate blue fluorescent powder according to claim 1 is characterized in that basic solution comprises ammoniacal liquor, urea soln.
4. the preparation method of a kind of europium-activated aluminate blue fluorescent powder according to claim 1 is characterized in that reducing atmosphere is preferably CO, N2: H2=9: 1～1: 3 gas mixture.
CN200910309873.XA 2009-11-17 2009-11-17 Preparation method of europium-activated aluminate blue fluorescent powder Expired - Fee Related CN101717633B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102031114A (en) * 2010-11-26 2011-04-27 中国科学院理化技术研究所 Preparation method of spherical fluorescent powder with nano structure
CN102822104A (en) * 2011-03-31 2012-12-12 安瀚视特控股株式会社 Glass plate production method
CN104498027A (en) * 2014-11-28 2015-04-08 广州珠江光电新材料有限公司 Fluorescent powder high in luminous efficacy and heat stability and preparation method of fluorescent powder
US9359242B2 (en) 2011-03-31 2016-06-07 Avanstrate Inc. Glass-plate manufacturing method
CN111139070A (en) * 2020-01-06 2020-05-12 南方科技大学 Preparation method of fluorescent powder, fluorescent powder and light source

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1861737A (en) * 2006-06-09 2006-11-15 江西财经大学 Preparation process of long afterglow luminescent powder superfine powder of alkaline earth aluminate by codeposition/microwave method
CN1974716A (en) * 2006-12-18 2007-06-06 天津理工大学 Red long-afterglow phosphor material and its prepn process

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
吕兴栋等: "Synthesis of Ultra-fine SrAl2O4:Eu,Dy Phosphor and Its Luminescent Properties", 《JOURNAL OF RARE EARTHS》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102031114A (en) * 2010-11-26 2011-04-27 中国科学院理化技术研究所 Preparation method of spherical fluorescent powder with nano structure
CN102822104A (en) * 2011-03-31 2012-12-12 安瀚视特控股株式会社 Glass plate production method
CN102822104B (en) * 2011-03-31 2015-08-26 安瀚视特控股株式会社 The manufacture method of sheet glass
US9359242B2 (en) 2011-03-31 2016-06-07 Avanstrate Inc. Glass-plate manufacturing method
CN104498027A (en) * 2014-11-28 2015-04-08 广州珠江光电新材料有限公司 Fluorescent powder high in luminous efficacy and heat stability and preparation method of fluorescent powder
CN111139070A (en) * 2020-01-06 2020-05-12 南方科技大学 Preparation method of fluorescent powder, fluorescent powder and light source
CN111139070B (en) * 2020-01-06 2022-08-05 南方科技大学 Preparation method of fluorescent powder, fluorescent powder and light source

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