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Preparation method for regular particle-shaped aluminate green emitting phosphor

A green phosphor, aluminate technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of difficult to achieve industrialization, low brightness of phosphors, low output rate, etc., and achieve regular particle morphology and preparation. Simple process and uniform particle size

Inactive Publication Date: 2012-10-10
甘肃稀土新材料股份有限公司 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above method can avoid some problems caused by the high-temperature solid-phase method, the brightness of the prepared phosphor is lower than that of the high-temperature solid-phase method, and it is difficult to realize industrialization due to the need for special equipment and low output rate.

Method used

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  • Preparation method for regular particle-shaped aluminate green emitting phosphor
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  • Preparation method for regular particle-shaped aluminate green emitting phosphor

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Experimental program
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Effect test

Embodiment 1

[0020] According to (Ce 0.63 Tb 0.37 )MgAl 11 o 19 Molecular formula weighs 0.4874gCeO respectively 2 , 0.3118gTb 4 o 7 , 0.1814gMgO, 2.5235gAl 2 o 3 , Weigh flux 0.007gH 3 BO 3 , 0.0701gLi 2 CO 3 , 0.1402gAlF 3 , put all the raw materials into an agate mortar and add an appropriate amount of alcohol to grind for 1 h; put the mixed raw materials into a crucible in an air atmosphere at 1500 ° C for 5 h, and cool to room temperature with the furnace to obtain the primary calcined product; grind and pulverize the primary calcined product After being placed in the crucible again, H 2 / N 2 Insulate at 1500°C for 3~5h in reducing atmosphere (reducing atmosphere used is changed from 10%H 2 and 90%N 2 composition), cooled to room temperature with the furnace to obtain the final calcined product; the final calcined product was ground and pulverized, washed, filtered, dried, and sieved (100 mesh) to obtain CMAT green phosphor.

Embodiment 2

[0022] According to (Ce 0.63 Tb 0.37 )MgAl 11 o 19 Molecular formula weighs 0.4874gCeO respectively 2 , 0.3118gTb 4 o 7 , 0.1814gMgO, 2.5235gAl 2 o 3 , Weigh flux 0.021gH 3 BO 3 , 0.0701gLi 2 CO 3 , 0.2102gAlF 3 , put all the raw materials into an agate mortar and add an appropriate amount of alcohol to grind for 1 hour; put the mixed raw materials into a crucible in an air atmosphere at 1550 ° C for 5 hours, and cool to room temperature with the furnace to obtain the primary calcined product; grind and pulverize the primary calcined product Placed in the crucible again, H 2 / N 2 Insulate at 1550°C for 3~5h in a reducing atmosphere (the reducing atmosphere used is changed from 10%H 2 and 90%N 2 composition), cooled to room temperature with the furnace to obtain the final calcined product; the final calcined product was ground and pulverized, washed, filtered, dried, and sieved (100 mesh) to obtain CMAT green phosphor.

Embodiment 3

[0024] According to (Ce 0.63 Tb 0.37 )MgAl 11 o 19 Molecular formula weighs 0.4874gCeO respectively 2 , 0.3118gTb 4 o 7 , 0.1814gMgO, 2.5235gAl 2 o 3 , Weigh flux 0.007gH 3 BO 3 , 0.1402gLi 2 CO 3 , 0.2102gAlF 3 , put all the raw materials into an agate mortar and add an appropriate amount of alcohol to grind for 1 h; put the mixed raw materials into a crucible in an air atmosphere at 1600 ° C for 5 h, and cool to room temperature with the furnace to obtain the primary calcined product; grind and pulverize the primary calcined product Placed in the crucible again, H 2 / N 2 Keep warm at 1600°C for 3~5h in a reducing atmosphere (the reducing atmosphere used is changed from 10%H 2 and 90%N 2 composition), cooled to room temperature with the furnace to obtain the final calcined product; the final calcined product was ground and pulverized, washed, filtered, dried, and sieved (100 mesh) to obtain CMAT green phosphor.

[0025] Table 1, the effect of different flux r...

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Abstract

The invention discloses a preparation method for regular particle-shaped aluminate green emitting phosphor. The method comprises the following steps of: weighing raw materials according to the stoichiometric proportion of all chemical components in an expression (Ce0.63Tb0.37)MgAl11019; weighing a H3BO3 fluxing agent, a Li2CO3 fluxing agent and a AlF3 fluxing agent which are used as composite fluxing agents, and adding into raw materials and uniformly mixing; placing raw material powder in a crucible and calcining to obtain a primary calcined product; crushing the primary calcined product, placing in the crucible again, and calcining in the atmosphere of H2 / N2 to obtain a secondary calcined product; and crushing the secondary calcined product, washing, filtering, drying and screening to obtain a final product. According to the preparation method, (Ce,Tb)MgAl11O19 (CMAT) green emitting phosphor which is regular in particle shape, uniform in particle size and high in relative luminance is obtained on the basis of the conventional high-temperature solid phase method by mainly adjusting the proportion of all the fluxing agents in the composite fluxing agents; and the preparation process is simple, so that the green emitting phosphor can be industrially produced on large scale.

Description

technical field [0001] The invention belongs to the technical field of luminescent materials, and in particular relates to a method for preparing green fluorescent powder for energy-saving lamps with regular particle shape, uniform particle size and high relative luminous brightness. Background technique [0002] Rare earth aluminate (Ce,Tb)MgAl co-activated by cerium and terbium 11 o 19 (referred to as CMAT) is the green component of the rare earth three-color phosphor used in energy-saving lamps. The crystal structure of this fluorescent powder is magnetite-like, which has the characteristics of narrow emission spectrum band, high luminous efficiency, good color rendering index, high luminous efficiency, stable chemical properties, and long service life. Therefore, the phosphor is currently the most commonly used green commercial phosphor for energy-saving lamps at home and abroad. [0003] The method of preparing aluminate green powder in industrial production is mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64
Inventor 张尚虎王育华张加驰于化琴李树胜周美娇方中心徐玉君马彩红董小芳
Owner 甘肃稀土新材料股份有限公司
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