High-brightness small blue luminous particle and its preparation method

A fluorescent powder and small particle technology, applied in the direction of luminescent materials, chemical instruments and methods, etc., can solve the problems of reduced luminous efficiency, high equipment requirements, high reaction temperature, etc., and achieve short afterglow time, high luminous purity, and thermal stability good sex effect

Inactive Publication Date: 2006-04-19
袁曦明
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the other hand, since these phosphors are usually prepared by a high-temperature solid-phase method, the reaction temperature is relatively high, and the requirements for equipment are relatively high, and the crystal grain size of the prepared phosphor is about 5-10 microns. In order to obtain better Fluorescent powder with excellent luminous performance and high luminous efficiency, and in order to meet the needs of PDP coating and apply to compact energy-saving lamps, mercury-free neon lights, new background light sources for liquid crystal displays, etc., phosphors with fine particles are required, usually small particle size The phosphor is obtained by grinding or grinding large phosphor particles, so that the luminous efficiency is greatly reduced due to the destruction of the crystal morphology of the phosphor

Method used

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  • High-brightness small blue luminous particle and its preparation method
  • High-brightness small blue luminous particle and its preparation method
  • High-brightness small blue luminous particle and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] ①According to the stoichiometric ratio according to the molecular formula CaAl 2 o 4 :Eu 2+ 0.005 Weigh 2.804g CaO (98%, A.R), 0.044g Eu 2 o 3 (99.99%) was dissolved with hydrochloric acid, and 28.4035g AlCl was added 3 ·6H 2 O (85%, A.R), dubbed 160ml solution.

[0027] ② Stir the solution, add ammonia water to adjust the pH value to 4.5-6.5, add 20.9061 g of oxalic acid (the sum of oxalic acid: metal ions = 1.1-1.3: 1), add ammonia water to adjust the pH value to 4.5-6.5, and continue to stir the solution for 30 minutes.

[0028] ③Put the solution in a water bath and keep the temperature at 25-45°C for 12-24 hours to form a white precipitate.

[0029] ④ Wash and filter the white precipitate, and dry it in an oven at 75-95°C to obtain oxalate powder.

[0030] ⑤Put the oxalate into the crucible, under N 2 、H 2 (H 2 Accounting for 10-11%) under a reducing atmosphere, heat at 450-550°C and 850-950°C for 20-40 minutes respectively, and then calcinate at 1250-135...

Embodiment 2

[0032] ①According to the stoichiometric ratio according to the molecular formula CaAl 2.1 o 4.5148 :Eu 2+ 0.08 Weigh 2.804g CaO (98%, A.R), 0.704g Eu 2 o 3 (99.99%) was dissolved with hydrochloric acid, and 29.8237g AlCl was added 3 ·6H 2 O (85%, A.R), dubbed 160ml solution.

[0033] ② Stir the solution, add ammonia water to adjust the pH value to 4.5-6.5, add 21.3146 g of oxalic acid (the sum of oxalic acid: metal ions = 1.1-1.3: 1), add ammonia water to adjust the pH value to 4.5-6.5, and continue to stir the solution for 20-40 minutes.

[0034] ③Put the solution in a water bath and keep the temperature at 25-45°C for 12-24 hours to form a white precipitate.

[0035] ④ Wash and filter the white precipitate, and dry it in an oven at 75-95°C to obtain oxalate powder.

[0036] ⑤Put the oxalate into the crucible, under N 2 、H 2 (H 2 Accounting for 8-11%) in a reducing atmosphere, heat at 450-550°C and 850-950°C for 20-40 minutes respectively, and then calcinate at 125...

Embodiment 3

[0038] ①According to the stoichiometric ratio according to the molecular formula CaAl 2.4 o 4.6 :Eu 2+ 0.02 Weigh 2.804g CaO (98%, A.R), 0.176g Eu 2 o 3 (99.99%) dissolved with hydrochloric acid, added 34.0842g AlCl 3 ·6H 2 O (85%, A.R), dubbed 160ml solution.

[0039]② Stir the solution, add ammonia water to adjust the pH value to 4.5-6.5, add 24.5836 g of oxalic acid (the sum of oxalic acid: metal ions = 1.1-1.3: 1), add ammonia water to adjust the pH value to 4.5-6.5, and continue to stir the solution for 20-40 minutes.

[0040] ③Put the solution in a water bath and keep the temperature at 20-35°C for 12-24 hours to form a white precipitate.

[0041] ④ Wash and filter the white precipitate, and dry it in an oven at 75-95°C to obtain oxalate powder.

[0042] ⑤Put the oxalate into the crucible, under N 2 、H 2 (H 2 Accounting for 10-11%) in a reducing atmosphere, heat at 450-550°C and 850-950°C for 20-40 minutes respectively, and then calcined at 1250-1350°C for 4 h...

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Abstract

A high-brightness small blue-light fluorescent particle (300 nm) has a formular Ca1-xEuxAlyO4, where x=0.005-0.1 and y=2-2.4. It is prepared through adding oxalic acid as precipitant in an acidic solution of metallic ions, controlling pH value and water bath temp for depositing the metallic ions to become small particles and controlling sintering temp. Its advantages are high luminescent efficiency, long afterglow, and high stability.

Description

technical field [0001] The invention relates to the technical field of luminescent materials, i.e. phosphors required for applications such as color plasma display (PDP), compact energy-saving lamps, mercury-free neon lights, and new background light sources for liquid crystal displays, especially alkaline earth metal aluminum activated by europium Salt phosphor and its preparation method. Background technique [0002] There are many types of blue-emitting luminescent materials for alkaline earth metal aluminates activated by europium, such as the commercial blue-emitting phosphor BaMgAl that can be used for plasma flat panel displays (PDPs). 10 o 17 :Eu 2+ , BaMgAl 14 o 23 :Eu 2+ , the disadvantage of these two phosphors is low thermal stability. S.Tanaka from Tottori University in Japan used a high-temperature solid-phase method to convert the raw material CaCO 3 , α-Al 2 o 3 、Eu 2 o 3 Blue-emitting CaAl synthesized at 1500 °C after mixing 2 o 4 :Eu 2+ Phosph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/00
Inventor 袁曦明杨应国王永钱王红梅张继红
Owner 袁曦明
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