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Preparation method of fluorescent powder with controllable luminescent property and prepared fluorescent powder

A technology for luminescent properties and phosphors, applied in the directions of luminescent materials, chemical instruments and methods, etc., can solve the problems of uncontrollable luminescent properties of phosphors, difficult to achieve controllable modulation, and complicated preparation processes.

Inactive Publication Date: 2019-01-04
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, Eu 3+ Ions are easily reduced to Eu in a weak reducing atmosphere 2+ ions, making it difficult to achieve Eu 2+ with Eu 3+ Ions coexist, more difficult to achieve Eu 2+ with Eu 3+ Controllable modulation of ion doping ratio
[0004] Currently, reports involving Eu 2+ with Eu 3+ The control technology of ion doping ratio has disadvantages such as complex preparation process, small conditional adjustability, and uncontrollable luminescence characteristics of phosphor powder.
For example, in Document 1 (RSC Adv., 2017, 7, 1711), the phosphor was sintered three times in a weak reducing atmosphere to reach Eu 2+ with Eu 3+ In the state of ion coexistence, the preparation process is complicated and it is difficult to control the ion doping ratio; Document 2 (Angew. Chem. Int. Ed., 2015, 54, 11501-11503) in order to realize Eu 2+ with Eu 3+ The adjustment of ion doping ratio requires the use of special reducing agents under vacuum conditions and the need to control the temperature gradient

Method used

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  • Preparation method of fluorescent powder with controllable luminescent property and prepared fluorescent powder
  • Preparation method of fluorescent powder with controllable luminescent property and prepared fluorescent powder
  • Preparation method of fluorescent powder with controllable luminescent property and prepared fluorescent powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Preparation (Eu 2+ 0.005 Eu 3+ 0.045 A + 0.045 m 0.905 ) 2 SiO 4 Phosphor powder, the steps are as follows:

[0043] in Eu 2 o 3 , Li 2 CO 3 , CaCO 3 , Sr(NO 3 ) 2 and SiO 2 As the initial raw material, the molar ratio of Eu:Li:(Ca+Sr):Si was 0.1:0.09:1.81:1, and the raw materials were wet mixed with alcohol solution for 1 h, and dried in a fume hood at room temperature. Obtain a uniform mixed powder;

[0044] Press the mixed powder into a block at 40 MPa, put it into a corundum crucible, sinter at 1100 °C for 2 h in an air atmosphere, press it into a block after grinding, and then sinter at 1450 °C for 6 h in an air atmosphere, cool down to room temperature, and grind to an average particle size of 0.5-15 μm.

[0045] Put the above powder into a small corundum crucible, cover the small corundum crucible cover (not sealed), put the small corundum crucible into a large corundum crucible with carbon powder, cover the cover as a microwave double-layer rea...

Embodiment 2

[0048] Preparation (Eu 2+ 0.02 Eu 3+ 0.1 A + 0.1 m 0.78 ) 2 SiO 4 Phosphor powder, the steps are as follows:

[0049] in Eu 2 o 3 , Li 2 CO 3 , CaCO 3 、BaCO 3 and SiC 8 h 20 o 4 As the initial raw materials, the molar ratio of Eu:Li:(Ca+Ba):Si was 0.24:0.2:1.56:1, and the raw materials were wet mixed with alcohol solution for 1 h, and dried in a fume hood at room temperature. Obtain a uniform mixed powder;

[0050] Press the mixed powder into a block at 40 MPa, put it into a corundum crucible, sinter at 800 °C for 5 h in an air atmosphere, press it into a block after grinding, and then sinter at 1300 °C for 10 h in an air atmosphere, cool down to room temperature, and grind to an average particle size of 0.5-15 μm.

[0051] Put the above powder into a small corundum crucible, cover the small corundum crucible cover (not sealed), put the small corundum crucible into a large corundum crucible with silicon carbide powder, cover the cover as a microwave double-l...

Embodiment 3

[0054] Preparation (Eu 2+ 0.1 Eu 3+ 0.08 A + 0.08 m 0.74 ) 2 SiO 4 Phosphor powder, the steps are as follows:

[0055] in Eu 2 o 3 、K 2 CO 3 , CaCO 3 , SrCO 3 and SiO 2 As the initial raw material, the molar ratio of Eu:K:(Ca+Sr):Si was 0.36:0.16:1.48:1, and the raw materials were wet mixed with alcohol solution for 1 h, and dried in a fume hood at room temperature. Obtain a uniform mixed powder;

[0056] Press the mixed powder into a block at 40 MPa, put it into a corundum crucible, sinter at 1100 °C for 3 h in an air atmosphere, press it into a block after grinding, and then sinter at 1450 °C for 6 h in an air atmosphere, cool down to room temperature, and grind to an average particle size of 0.5-15 μm.

[0057] Put the above powder into a small corundum crucible, cover the small corundum crucible cover (not sealed), put the small corundum crucible into a large corundum crucible with carbon powder, cover the cover as a microwave double-layer reactor, and the...

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Abstract

The invention discloses a preparation method of fluorescent powder with controllable luminescent property and prepared fluorescent powder. The preparation method comprises the following steps: calcining to obtain (Eu3+x+yA+yM1-x-2y)2SiO4 fluorescent powder, and preparing Eu<2+>, Eu<3+> double-doped phosphor silicate, namely (Eu2+xEu3+yA+yM1-x-2y)2SiO4 from the fluorescent powder by utilizing a microwave reduction method. The preparation process is simple, rapid and low in energy consumption, process parameters are easy to control and regulate, the condition control is simple, the adjustable range is wide, controllable regulation of the output performance of the fluorescent powder can be realized, and different luminescent requirements are met. The fluorescent powder is short in productioncycle, high in production efficiency and low in requirements on equipment and conditions, and contributes to realizing material component integration and integrated design. Therefore, the fluorescentpowder has potential of industrialization and batch production.

Description

technical field [0001] The present invention relates to a preparation method of a series of fluorescent powders with different luminous characteristics, in particular to a preparation method with simple process and controllable luminous characteristics of fluorescent powders, and also relates to a preparation method with different luminous characteristics and continuous luminescence band from red light to green light A series of adjustable fluorescent powder belongs to the technical field of fluorescent powder and its preparation. Background technique [0002] Silicate-based luminescent materials have good chemical stability and thermal stability, high photoconversion efficiency, and wide excitation band spectrum, and the raw materials of silicate are abundant and the synthesis process is simple, so it has always been the design and development research hotspots. Europium ion doped silicate phosphor such as Eu 2+ The ionoluminescent 214 phase (M 2 SiO 4 , M=Ca, Sr or Ba)...

Claims

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Application Information

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IPC IPC(8): C09K11/59
CPCC09K11/7734
Inventor 王树贤叶正茂吴佳明卢晓磊
Owner UNIV OF JINAN
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