CN1190115A - Preparation of blue fluorescent powder - Google Patents
Preparation of blue fluorescent powder Download PDFInfo
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- CN1190115A CN1190115A CN97101362A CN97101362A CN1190115A CN 1190115 A CN1190115 A CN 1190115A CN 97101362 A CN97101362 A CN 97101362A CN 97101362 A CN97101362 A CN 97101362A CN 1190115 A CN1190115 A CN 1190115A
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- fluorescent powder
- blue fluorescent
- crucible
- powder
- described preparation
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Abstract
The two-valent europium activated blue fluorescent barium aluminate powder is prepared through one-step high- temperature solid- phase synthesis. Substrate, activator, additive and other raw material are processed through material selection, mixing, low- temperature preheating, baking and post-treatment. The said fluorescent powder is used in producing color plasma disply plate.
Description
The invention belongs to a kind of manufacture method that is used for color plasma flat-panel monitor (PDP) fluorescent material.
Color PDP is a coating red, green, blue three primary colors fluorescent powder in the gas panel that is filled with mixed inert gas such as He+Xe or He+Ar, and the vacuum-ultraviolet light excitated fluorescent powder that produces when utilizing geseous discharge reaches demonstration video picture purpose.Therefore, directly affect the performance of indicating meter as the fluorescent material of one of PDP critical material.
The present invention provides a kind of manufacturing high performance BaMgAl for this purpose
14O
23: the method for Eu blue colour fluorescent powder.
Fluorescent material of the present invention is divalent europium activated barium aluminate, has β-Al
2O
3Crystalline structure, its chemical expression is as follows:
BaMgAl
14O
23：Eu
Eu
2+Can partly replace Ba
2+, by above-mentioned fluorescent material form stoichiometric ratio take by weighing the oxide compound that contains Ba, Mg, Al respectively, also can be corresponding salt and Eu
2O
3Raw material adds a spot of boric acid (boron oxide) and metal fluoride additive, and mill is mixed even, adopts high temperature solid state reaction, in weakly reducing atmosphere, and under 1300-1450 ℃ of temperature, calcination 2-3 hour synthetizing phosphor powder, the product that obtains is at 2%HNO
3Stir in the solution and soaked 2 hours, be washed till neutrality with hot deionized water, the powder slurry sieves, and 120 ℃ of oven dry obtain white powder.
Characteristics of the present invention are: (1) manufacturing process is simple, easy handling; (2) the satisfied concentration range of activator is proposed; (3) batch mixing is placed in the corundum crucible, can reduce or overcome crucible through 200-300 ℃ of low-temperature prewarming technology and burst; (4) use carbon granules in air, to burn and produce weak reducing gas, also available 1-5%H
2(volume ratio)+99-95%N
2(volume ratio) mixed gas is applicable in box-type furnace, cellar for storing things, tunnel or the tube furnace and makes fluorescent material as weak reducing gas; (5) selected a spot of boron oxide for use, boric acid and metal fluoride additive have not only reduced calcination temperature, and have improved the luminous intensity of fluorescent material.The fluorescent material that the present invention obtains is launched blue light under vacuum-ultraviolet light (VUV) or electron-beam excitation, can be used as the blue composition of color plasma flat-panel monitor (PDP).
Embodiment 1, take by weighing BaCO
320.00g, MgO4.60g Al
2O
382.20g, Eu
2O
32.43g, above-mentioned raw materials is packed in the ball grinder, put into agate ball, the weight ratio of ball and raw material is 1: 1, the ball milling time is more than 8 hours, the material of mixing is packed in the corundum crucible, on raw material, cover one deck carbon dust, build crucible cover, put into 200 ℃ of preheatings of preheating oven 1 hour, when another sintering oven is warming up to 1350 ℃, from preheating oven, takes out crucible and put into sintering oven immediately, constant temperature 2 hours, take out crucible cools to room temperature, remove carbon dust, white powder is packed in the ball grinder, add entry and Ф 3mm glass sphere, powder: water: ball ≈ 1: 1: 1, ball milling 2 hours is starched powder in the beaker of packing into, uses 2%HNO
3Solution soaking 2 hours, and often stirring then is washed till neutrality with hot deionized water, and the powder slurry is sieved with 400 orders, and 120 ℃ of oven dry in baking oven behind the suction filtration promptly obtain the BaMgAl of color PDP
14O
23: the Eu blue colour fluorescent powder, exciting down at 149.5nm, luminous intensity is 100.
Embodiment 2, take by weighing BaCO
320.00g, MgO4.60g, Al
2O
382.20g, Eu
2O
32.43g, H
3BO
30.50g all the other conditions are with embodiment 1, exciting down at 149.5nm, luminous intensity is 105.
Embodiment 3, take by weighing BaCO
320.00g, MgO4.2g, MgF
20.72g, Al
2O
382.20g, Eu
2O
32.43g, H
3BO
30.50g all the other conditions are with embodiment 1, exciting down at 149.5nm, luminous intensity is 109.
Embodiment 4, take by weighing BaCO
320.00g, MgO3.24g, Mg (OH)
2.4MgCO
3.6H
2O3.48g, AL
2O
382.20g, Eu
2O
32.43g, H
3BO
30.50g all the other conditions are with embodiment 1, exciting down at 149.5nm, luminous intensity is 106.
Embodiment 5, take by weighing BaCO
316.00g, BaCl
25.06g, MgO4.60g, Al
2O
382.20g, Eu
2O
32.43g, H
3BO
30.50g all the other conditions are with embodiment 1, exciting down at 149.5nm, luminous intensity is 107.
Embodiment 6, take by weighing BaCO
320.00g, MgO4.20g, MgF
20.70g, Al
2O
379.30g, AlF
34.80g, Eu
2O
32.43g, H
3BO
30.50g all the other conditions are with embodiment 1, exciting down at 149.5nm, luminous intensity is 113.
Embodiment 7, take by weighing BaCO
316.00g, BaCl
25.06g, MgO3.24g, Mg (OH)
2.4MgCO
3.6H
2O3.48g, Al
2O
382.20g, Eu
2O
32.43g, H
3BO
30.50g all the other conditions are with embodiment 1, exciting down at 149.5nm, luminous intensity is 107.
Claims (6)
1, a kind of preparation of blue fluorescent powder, its chemical expression is as follows:
BaMgAl
14O
23：Eu
It is characterized in that, comprise substrate material, activator concentration, additive, batch mixing and preheating, burn till and the aftertreatment several steps.
2, by the described preparation of blue fluorescent powder of claim 1, its substrate material be characterised in that by fluorescent material form stoichiometric ratio take by weighing the oxide compound that contains Ba, Mg, Al respectively, also can be corresponding salt.
3, by the described preparation of blue fluorescent powder of claim 1, the concentration that it is characterized in that the activator europium sesquioxide is in the 0.05-0.25 molar range, additive can be at least a in the following material: boron oxide, boric acid, Mg, Ba, the oxide compound of Al and fluorochemical, its add-on is the 0.1%-10% of fluorescent material weight.
4, by the described preparation of blue fluorescent powder of claim 1, it is characterized in that with substrate material activator and additive mixing and ball milling are even, be placed in the corundum crucible in 200-300 ℃ preheating 2-3 hour.
5, by the described preparation of blue fluorescent powder of claim 1, it is characterized in that the raw material crucible of preheating is put into 1300-1450 ℃ of firing furnace, in the weakly reducing atmosphere that in air, produces calcination 1-3 hour, also can contain 1-5%H by carbon burning
2(volume ratio)+99-95%N
2In (volume ratio) mixed gas calcination 1-3 hour, directly from high temperature, take out crucible then, be cooled to room temperature, in the time of also can not taking out crucible and reduce to 800 ℃ of left and right sides rapidly crucible is taken out with stove, be cooled to room temperature.
By claim 1 and 5 described preparation of blue fluorescent powder, it is characterized in that 6, earlier with Ф 2-5mm glass sphere, also available baton round is put into water in aftertreatment, ball milling 2 hours is to separate the fluorescent material that scatters.Powder wherein: water: ball ≈ 1:: 1: 1 (weight ratio), use rare nitric acid dousing fluorescent material 2 hours then, at last with deionized water wash to neutral.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB971013624A CN1137956C (en) | 1997-02-05 | 1997-02-05 | Preparation of blue fluorescent powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB971013624A CN1137956C (en) | 1997-02-05 | 1997-02-05 | Preparation of blue fluorescent powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1190115A true CN1190115A (en) | 1998-08-12 |
| CN1137956C CN1137956C (en) | 2004-02-11 |
Family
ID=5165680
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB971013624A Expired - Fee Related CN1137956C (en) | 1997-02-05 | 1997-02-05 | Preparation of blue fluorescent powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1137956C (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294231C (en) * | 2001-12-13 | 2007-01-10 | 奥斯兰姆施尔凡尼亚公司 | Illuminant paste composition |
| CN100396752C (en) * | 2002-05-17 | 2008-06-25 | 松下电器产业株式会社 | Plasma display device |
| CN100396754C (en) * | 2002-05-17 | 2008-06-25 | 松下电器产业株式会社 | Plasma display unit, phosphor and process for producing phosphor |
| CN101264932B (en) * | 2007-03-15 | 2010-12-22 | 南京工业大学 | Method for preparing mixed valence molybdenum-based oxide by triboelectric injection functional particles |
| CN101420004B (en) * | 2002-02-15 | 2012-07-04 | 三菱化学株式会社 | Light emitting device and illuminator using the same |
-
1997
- 1997-02-05 CN CNB971013624A patent/CN1137956C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1294231C (en) * | 2001-12-13 | 2007-01-10 | 奥斯兰姆施尔凡尼亚公司 | Illuminant paste composition |
| CN101420004B (en) * | 2002-02-15 | 2012-07-04 | 三菱化学株式会社 | Light emitting device and illuminator using the same |
| CN100396752C (en) * | 2002-05-17 | 2008-06-25 | 松下电器产业株式会社 | Plasma display device |
| CN100396754C (en) * | 2002-05-17 | 2008-06-25 | 松下电器产业株式会社 | Plasma display unit, phosphor and process for producing phosphor |
| CN101264932B (en) * | 2007-03-15 | 2010-12-22 | 南京工业大学 | Method for preparing mixed valence molybdenum-based oxide by triboelectric injection functional particles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1137956C (en) | 2004-02-11 |
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| CF01 | Termination of patent right due to non-payment of annual fee |