CN102071016A - Aluminate blue fluorescent powder and preparation method thereof - Google Patents
Aluminate blue fluorescent powder and preparation method thereof Download PDFInfo
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- CN102071016A CN102071016A CN2011100283929A CN201110028392A CN102071016A CN 102071016 A CN102071016 A CN 102071016A CN 2011100283929 A CN2011100283929 A CN 2011100283929A CN 201110028392 A CN201110028392 A CN 201110028392A CN 102071016 A CN102071016 A CN 102071016A
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Abstract
The invention belongs to the field of luminous materials and discloses aluminate blue fluorescent powder used for a fluorescent lamp, a plasma display panel (PDP) display device and a white light-emitting diode (LED), and a preparation method thereof. The fluorescent powder has a molecular formula of SiO2 embedded BaMgAl10O17:Eu2+, and stoichiometric ratios (mol) of various raw materials are that: SiO2 is 1 to 10 mol, BaCO3 is 0.8 to 1.2mol, Mg(NO3)2 is 0.8 to 1.2mol, Al(NO)39H2O is 8 to 12 mol and Eu2O3 is 0.08 to 0.8mol. The prepared spherical aluminate blue fluorescent powder with controlled dimension and a core-shell structure is excited by 254nm ultraviolet light, emits high-efficiency blue light, and has a main peak at 450nm, high stability and high luminous intensity. The prepared fluorescent powder has a regular spherical structure, the dimension can be controlled by controlling the dimension of the SiO2, and the preparation process is simple and easy for industrialization; therefore, the preparation method can serve as a novel method for preparing the blue fluorescent powder.
Description
Technical field
The invention belongs to field of light emitting materials, the preparation method of the aluminate blue fluorescent powder of particularly a kind of sphere, controllable size, nucleocapsid structure.
Background technology
Blue colour fluorescent powder BaMgAl
10O
17: Eu
2+(BAM) be one of most important composition of three primary colors fluorescent powder, it not only can be applied to the preparation of luminescent lamp, in the demonstration field, as the manufacturing of plasm TV (PDP); High-end lighting field, as the manufacturing field of white light LEDs, blue colour fluorescent powder BAM is widely used.At present the BAM that uses adopts the high temperature solid-state method preparation, and it is more serious to reunite, and the later stage is to obtain reasonable size and pattern to adopt ball-milling technology that the crystal morphology of BAM is influenced bigger, has lost luminous efficiency when obtaining small particle size.Adopt the blue colour fluorescent powder (BAM) of this patent method preparation to have globosity, all be the nucleocapsid structure of size control, avoid the loss of light efficiency, be both and can obtain the product of ideal dimensions, in use coating efficiency is higher for the BAM of last globosity, helps reducing cost.
Summary of the invention
The aluminate blue fluorescent powder that the purpose of this invention is to provide a kind of sphere, controllable size, nucleocapsid structure;
Another object of the present invention provides its preparation method of the aluminate blue fluorescent powder of a kind of sphere, controllable size, nucleocapsid structure.
The molecular formula of the aluminate blue fluorescent powder of sphere of the present invention, controllable size, nucleocapsid structure is:
SiO
2@BaMgAl
10O
17:Eu
2+。
The preparation method of the aluminate blue fluorescent powder of sphere of the present invention, controllable size, nucleocapsid structure may further comprise the steps:
1SiO
2The preparation of nuclear
1.1 add an amount of alcohol, water and strong aqua in the mixing tank successively, stir, make solution mix; Slowly in above-mentioned solution, drip the mixed solution of tetraethoxy (TEOS), alcohol, continue to stir; The amount concentration ratio of each material is: TEOS: H
2O: NH
4OH=(0.1-1.0): (1.0-10.0): 1.0;
1.2 gained solution is water bath with thermostatic control 1-10h under 30-80 ℃ of condition, centrifuge washing, and 80-160 ℃ of following dry 12-24h promptly gets the SiO that size is about 100-1000nm after the grinding
2Microballoon (as shown in Figure 1);
2SiO
2@BaMgAl
10O
17: Eu
2+The preparation of nucleocapsid structure
2.1 take by weighing Eu
2O
3Be dissolved in the nitric acid and obtain, add BaCO more successively
3, Mg (NO
3)
2And Al (NO
3)
39H
2O, the addition of each species is equal to the stoichiometric ratio of BAM, adds citric acid (C at last
6H
8O
7H
2O), total metal ion in the control solution: the concentration ratio of citric acid is 1: (1-6);
2.2 add strong aqua behind above-mentioned mixing solutions heating, the magnetic agitation 3-12h, the adjusting pH value is 4-8, gets water white transparency colloidal sol, adds the SiO that has prepared in 1.2
2Microballoon stirred 1-12 hour; Solution is at 80-160 ℃, and constant temperature 1-4h gets xerogel, 80-160 ℃ of dry 6-12h, 800-1000 ℃ of preroasting 2-5h; Grind back 1200-1450 ℃ of reductase 12-5h in reducing atmosphere, obtain SiO
2@BaMgAl
10O
17: Eu
2+Nucleocapsid structure (as shown in Figure 2).
The aluminate blue fluorescent powder of the sphere of the present invention's preparation, controllable size, nucleocapsid structure is sent efficient blue light by the 254nm ultraviolet excitation, launches main peak at 450nm, good stability, luminous intensity height.The fluorescent material that obtains all is the globosity of rule, and size can be by control SiO
2Size realize that preparation technology is simple, be easy to industrialization, so the present invention can be used as a kind of preparation method of novel blue colour fluorescent powder.
Description of drawings
Fig. 1 is
SiO
2The field emission microscope photo of microballoon
Fig. 2 is SiO
2@BaMgAl
10O
17: Eu
2+The projection electron microscope photo
Embodiment
Below the present invention is elaborated: altogether for two embodiment, for saving space, two examples are narrated in the lump, and when having only data, two examples are identical, and when two data were arranged, previous was example 1 data, data instance 2 data in the parantheses.
Add an amount of alcohol, water and strong aqua in the mixing tank successively, stir, make solution mix.Slowly in above-mentioned solution, drip the mixed solution of tetraethoxy (TEOS), alcohol, continue to stir; The amount concentration ratio of each material is: TEOS: H
2O: NH
4OH=0.1 (1.0): 1.0 (10): 1.0; Gained solution is water bath with thermostatic control 1 (10) h under 80 ℃ of conditions, centrifuge washing, and 80 (160) ℃ of down dry 12 (24) h promptly get the SiO that size is about 100 (1000) nm after the grinding
2Microballoon.
Take by weighing 0.008 (0.12) mol Eu
2O
3Be dissolved in the nitric acid and obtain, add 0.8 (1.2) mol BaCO more successively
3, 0.8 (1.2) mol Mg (NO
3)
2With 8 (12) mol Al (NO)
39H
2O adds 0.1 (6.0) mol citric acid (C at last
6H
8O
7H
2O), total metal ion in the control solution: the concentration ratio of citric acid is 1: 6; Add strong aqua behind mixing solutions heating, magnetic agitation 3 (12) h, regulating pH value is 4 (8), gets water white transparency colloidal sol, adds the SiO that has prepared
2Microballoon stirred 1 (12) hour; Solution is at 80 (160) ℃, and constant temperature 1 (4) h gets xerogel, 80 (160) ℃ of drying 6 (12) h, 800 (1200) ℃ of preroasting 2 (5) h; Grind back (1200) 1450 ℃ of reductase 12s (5) h in reducing atmosphere, obtain SiO2@BaMgAl
10O
17: Eu
2+Nucleocapsid structure.
The aluminate BAM blue colour fluorescent powder of the present invention's preparation is spherical nucleocapsid structure, controllable size, at the 254nm ultraviolet excitation, sends efficient blue light, launches main peak at 450nm, good stability, luminous intensity height.
Claims (2)
1. aluminate blue fluorescent powder, it is characterized in that: the molecular formula of described aluminate blue fluorescent powder is: SiO
2@BaMgAl
10O
17: Eu
2+
2. the preparation method of aluminate blue fluorescent powder according to claim 1, it is characterized in that: described method steps comprises:
2.1 add an amount of alcohol, water and strong aqua in the mixing tank successively, stir, make solution mix; Slowly in above-mentioned solution, drip the mixed solution of tetraethoxy (TEOS), alcohol, continue to stir; The amount concentration ratio of each material is: TEOS: H
2O: NH
4OH=(0.1-1.0): (1.0-10.0): 1.0;
2.2 gained solution is water bath with thermostatic control 1-10h under 30-80 ℃ of condition, centrifuge washing, and 80-160 ℃ of following dry 12-24h promptly gets the SiO that size is about 100-1000nm after the grinding
2Microballoon;
2.3 take by weighing Eu
2O
3Be dissolved in the nitric acid and obtain, add BaCO more successively
3, Mg (NO
3)
2And Al (NO)
39H
2O, the mol ratio of each species equals BAM molecule metering ratio, adds citric acid (C at last
6H
8O
7H
2O), control total concentration of metal ions, the concentration of citric acid=1: (1-6);
2.4 add strong aqua behind above-mentioned mixing solutions heating, the magnetic agitation 3-12h, the adjusting pH value is 4-8, gets water white transparency colloidal sol, adds the SiO that has prepared in 2.2
2Microballoon stirred 1-12 hour; Solution is at 80-160 ℃, and constant temperature 1-4h gets xerogel, 80-160 ℃ of dry 6-12h, 800-1000 ℃ of preroasting 2-5h; Grind back 1200-1450 ℃ of reductase 12-5h in reducing atmosphere, obtain SiO
2@BaMgAl
10O
17: Eu
2+Nucleocapsid structure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100283929A CN102071016A (en) | 2011-01-11 | 2011-01-11 | Aluminate blue fluorescent powder and preparation method thereof |
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|---|---|---|---|
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Family
ID=44029777
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103789861A (en) * | 2011-12-31 | 2014-05-14 | 四川虹欧显示器件有限公司 | Blue fluorescence fiber used for plasma display panel and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049574A (en) * | 2007-04-26 | 2007-10-10 | 东北师范大学 | Photocatalysis material possessing hud structure of photoluminescent property, and preparation method |
-
2011
- 2011-01-11 CN CN2011100283929A patent/CN102071016A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101049574A (en) * | 2007-04-26 | 2007-10-10 | 东北师范大学 | Photocatalysis material possessing hud structure of photoluminescent property, and preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 肖林久等: "溶胶-凝胶法制备的BaMgAl10O17∶Eu2+ 荧光性能研究", 《稀土》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103789861A (en) * | 2011-12-31 | 2014-05-14 | 四川虹欧显示器件有限公司 | Blue fluorescence fiber used for plasma display panel and preparation method thereof |
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Application publication date: 20110525 |