CN1137956C - Preparation of blue fluorescent powder - Google Patents
Preparation of blue fluorescent powder Download PDFInfo
- Publication number
- CN1137956C CN1137956C CNB971013624A CN97101362A CN1137956C CN 1137956 C CN1137956 C CN 1137956C CN B971013624 A CNB971013624 A CN B971013624A CN 97101362 A CN97101362 A CN 97101362A CN 1137956 C CN1137956 C CN 1137956C
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- crucible
- powder
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- activator
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Abstract
The present invention relates to a method for preparing blue barium aluminate fluorescent powder activated by bivalent europium, which adopts a synthesis method through high-temperature solid phase reaction in one step. The method comprises the steps of selection, material mixing, preheating at low temperature, sintering, post-treating, etc. of materials, such as substrates, activating agents, additives, etc. The preparation process is used for blue high-performance fluorescent powder used for colored plasma flat panel display (PDP) and has the advantages of simple method, no pollution and low cost.
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 mixing 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
Blue colour fluorescent powder BaMgAl of the present invention
14O
23: Eu, divalent europium is an activator.Activator can be an europium sesquioxide in the present invention, and the concentration of europium sesquioxide is in 0.05～0.25 molar range.Additive can be at least a in the following material; Boron oxide, boric acid, the oxide compound of Mg, Ba, Al and fluorochemical, add-on is 0.1～10% of a fluorescent material weight.Wherein, Eu
2+Can partly replace Ba
2+
Press BaMgAl
14O
23: the stoichiometric ratio that Eu forms is got the raw materials ready.Taking by weighing the oxide compound that contains Mg, Ba, Al respectively, also can be corresponding salt and Eu
2O
3Raw material adds a spot of boric acid (boron oxide) and metal fluoride additive.The oxide compound or the corresponding salt that contain Mg, Ba, Al are substrate material, Eu
2O
3Be activator.
Substrate material, activator, additive are packed in the ball grinder, put into agate ball, the weight ratio of ball and raw material is 1: 1, and the ball milling time is more than 8 hours.This process is a batch mixing of the present invention.
Preheating: substrate material, activator, additive mixing and ball milling evenly after, be placed in the corundum crucible, preheating is 2～3 hours in 200 ℃～300 ℃.
Burn till: after the crucible preheating of substrate material, activator, additive is housed, put into 1300 ℃～1450 ℃ firing furnaces, 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)+99～95N
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 be cooled to 800 ℃ of left and right sides rapidly crucible is taken out with stove, be cooled to room temperature.
Aftertreatment: at last the above-mentioned powder of calcination, with φ 2～5mm glass sphere or baton round, put into water, ball milling 2 hours is to separate the powder that scatters.In the mechanical milling process, powder: water: ball is 1: 1: 1, is weight ratio.Starched 2 hours with rare nitric acid dousing powder, extremely neutral with deionized water wash at last.The powder slurry is sieved through 400 orders, filter back 120 ℃ of oven dry in baking oven, and detect, promptly obtain blue colour fluorescent powder of the present invention.
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
2Go back gas a little less than the conduct of (volume ratio) mixed gas, be applicable in box-type furnace, cellar for storing things, tunnel or the tube furnace and make fluorescent material; (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 2 hours, 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 φ 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, MgO 4.60g 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, MgO 4.20g 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, MgO 3.24g, Mg (OH)
24MgCO
36H
2O 3.48g, 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, MgO 4.60g 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, MgO 4.20g 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, MgO 3.24g, Mg (OH)
24MgCO
3.6H
2O 3.48g, 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 (1)
1, a kind of preparation of blue fluorescent powder, its chemical expression is as follows: BaMgAl
14O
23: Eu, it is characterized in that it comprises batch mixing, preheating, burns till and the aftertreatment several steps, its raw material comprises substrate material, activator and additive; The stoichiometric ratio of forming by substrate material takes by weighing oxide compound or its corresponding salt that contains Mg, Ba, Al respectively, add the activator europium sesquioxide, volumetric molar concentration is in 0.05～0.25 scope, additive can be at least a in the following material: the oxide compound of boron oxide, boric acid, Mg, Ba, Al and fluorochemical, its add-on are 0.1～10% of fluorescent material weight; Substrate material, activator, additive mixing and ball milling is even; The uniform material of mixing and ball milling is placed in the corundum crucible, and preheating is 2～3 hours in 200 ℃～300 ℃; Then the material crucible of preheating is put into 1300 ℃～1450 ℃ firing furnaces, in the weakly reducing atmosphere that in air, produces calcination 1-3 hour, also can contained 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 be cooled to 800 ℃ of left and right sides rapidly crucible is taken out, be cooled to room temperature with stove; Earlier with φ 2～5mm glass sphere or baton round, put into water in aftertreatment, ball milling 2 hours is to dismiss powder, powder: water: ball=1: 1: 1 (weight ratio), with rare nitric acid dousing 2 hours, with deionized water wash to neutrality.
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 CN1190115A (en) | 1998-08-12 |
| CN1137956C true 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) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6660184B2 (en) * | 2001-12-13 | 2003-12-09 | Osram Sylvania Inc. | Phosphor paste compositions |
| CN100468789C (en) * | 2002-02-15 | 2009-03-11 | 三菱化学株式会社 | Light emitting device and illuminating device using it |
| JP4096618B2 (en) * | 2002-05-17 | 2008-06-04 | 松下電器産業株式会社 | Plasma display device |
| JP2003336052A (en) * | 2002-05-17 | 2003-11-28 | Matsushita Electric Ind Co Ltd | Plasma display device |
| CN101264932B (en) * | 2007-03-15 | 2010-12-22 | 南京工业大学 | Method for preparing mixed valence molybdenum-base oxide by triboelectricity injection functional particles |
-
1997
- 1997-02-05 CN CNB971013624A patent/CN1137956C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1190115A (en) | 1998-08-12 |
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