Preparation method of flaky aluminate green phosphor

A green phosphor, aluminate technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of uneven mixing, high temperature and long time of high-temperature solid-phase calcination, and achieve shortened calcination time and luminous performance. Excellent, the effect of reducing the phase temperature

Active Publication Date: 2013-06-05
江苏优氟防腐科技有限公司
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  • Claims
  • Application Information

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Problems solved by technology

The industrial preparation method is still the high-temperature solid-phase method, and other methods such as the sol-gel method and the hydrothermal method still have no industrial application prospects, while the high-temperature solid-phase method has a high calcination temperature (above 1500 ° C), a long time, and uses It takes a long time to mix the raw materials and co-solvent evenly, and the product particles are coarse and irregular in shape. It takes a long time for ball milling to meet the requirements of use. It is a synthetic method with high energy consumption, long cycle time and is not environmentally friendly.
[0003] The study of new methods for the preparation of phosphors with physical properties control has always been a research hotspot in the field of luminescent materials, because the particle size, morphology and crystallinity of phosphors have a crucial impact on their luminescent properties. High-temperature solid-phase synthesis of CMAT often adds co-solvent salts through solid-solid phase mixing to promote phase formation. Due to uneven mixing, the effect is not ideal, and high temperature and long-term calcination is still required.

Method used

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  • Preparation method of flaky aluminate green phosphor
  • Preparation method of flaky aluminate green phosphor
  • Preparation method of flaky aluminate green phosphor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 0.2305 g CeO 2, Place in 30 ml 1:1 nitric acid solution, add 5 ml 30% hydrogen peroxide dropwise, stir while heating until completely dissolved, then weigh 0.1234 g Tb 4 o 7 , 0.08g MgO and 8.28 g Al(NO 3 ) 3 9H 2 O was added to it, heated and dissolved to obtain a mixed solution of nitrates. Add 0.8658 g NH to the mixed solution obtained above 4 F and 5.32 g of urea, heated and stirred to dissolve them, and concentrated to a nearly viscous state, then put them into a microwave oven to heat and ignite, and the combustion products were put into a nitrogen-hydrogen mixed gas (H 2 : 5 V%) in a tube atmosphere furnace at 1100 °C for 2 h. The product after heat treatment is washed, dried, ground and sieved to obtain Ce 0.67 Tb 0.33 MgAl 11 o 19 Phosphor.

Embodiment 2

[0031] Weigh 0.2305 g CeO 2, Place in 30 ml 1:1 nitric acid solution, add 5 ml 30% hydrogen peroxide dropwise, stir while heating until completely dissolved, then weigh 0.1234 g Tb 4 o 7 , 0.08g MgO and 0.594 g Al powder were added, heated and dissolved to obtain a nitrate mixed solution. Add 0.6734 g NH to the mixed solution obtained above 4 F and 4.56 g urea, heated and stirred to make it dissolve, and condensed to close to viscous state, continue heating to trigger self-propagating combustion reaction, and the combustion product is put into nitrogen-hydrogen mixed gas (H 2 : 5 V%) in a tube atmosphere furnace at 1100 °C for 2 h. The product after heat treatment is washed, dried, ground and sieved to obtain Ce 0.67 Tb 0.33 MgAl 11 o 19 Phosphor.

Embodiment 3

[0033] Weigh 0.2305 g CeO 2, Place in 30 ml 1:1 nitric acid solution, add 5 ml 30% hydrogen peroxide dropwise, stir while heating until completely dissolved, then weigh 0.1234 g Tb 4 o 7 , 0.08g MgO and 1.716 g Al(OH) 3 , added to it, heated and dissolved to obtain a mixed solution of nitrates. Add 0.8658 g NH to the mixed solution obtained above 4 F and 4.56 g urea, heated and stirred to make it dissolve, and concentrated to a nearly viscous state, then put it into a microwave oven to heat and ignite, and the combustion product was put into a nitrogen-hydrogen mixed gas (H 2 : 5 V%) in a tube atmosphere furnace at 1100 °C for 2 h. The product after heat treatment is washed, dried, ground and sieved to obtain Ce 0.67 Tb 0.33 MgAl 11 o 19 Phosphor.

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Abstract

The invention relates to a preparation method of a flaky aluminate green phosphor. The preparation method comprises the following steps: 1, respectively weighing corresponding raw materials according to the amount of an object product to be prepared and the stoichiometric ratio of all metal elements in Ce1-xTbxMgAl11O19, and preparing a mixed nitrate solution of metals contained in the object product; 2, adding an organic fuel to the mixed nitrate solution obtained in step 1, and heating to dissolve; 3, adding ammonium fluoride to the mixed solution obtained in step 2, heating to dissolve, and continuously concentrating the mixed solution until that the mixed solution is in an approximately sticky state; 4, initiating the sticky solution obtained in step 3 to be subjected to self-propagating combustion; 5, post-treating self-propagating combusted products obtained in step 4; and 6, washing, drying, grinding, and sieving the product obtained in step 5 to obtain the object product. The preparation method of the invention, which has the advantages of phase forming temperature reduction, calcining time shortening, excellent luminescent performance, controllable particle size, uniform size, regular morphology, simple enforcement, low cost, rapidness, and energy saving, has a good industrialization application prospect.

Description

technical field [0001] The invention belongs to the technical field of material preparation, in particular to a preparation method of a rare earth luminescent material. technical background [0002] Rare earth tricolor phosphor green powder doped with Tb 4+ Phosphates, borates, aluminates, etc., among them, Ce 1-x Tb x MgAl 11 o 19 Aluminate phosphor (CMAT for short) has high temperature resistance and good stability, so that other phosphors cannot be replaced now, and it can also be used in new PDP flat panel displays. The industrial preparation method is still the high-temperature solid-phase method, and other methods such as the sol-gel method and the hydrothermal method still have no industrial application prospects, while the high-temperature solid-phase method has a high calcination temperature (above 1500 ° C), a long time, and uses It takes a long time to mix the raw materials and co-solvents evenly, and the product particles are coarse and irregular in shape. I...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/80
Inventor 陈伟凡柯于胜林玉翠刘铭
Owner 江苏优氟防腐科技有限公司
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