A preparation method of phosphor powder with controllable luminescence characteristics and the phosphor powder obtained

A technology of luminescent properties and phosphors, applied in luminescent materials, chemical instruments and methods, etc., can solve the problems of difficult to control the ion doping ratio, uncontrollable luminescent properties of phosphors, and difficult to achieve controllable modulation, etc., and achieve light output performance. Low requirements for controllable modulation, equipment and conditions, and high production efficiency

Inactive Publication Date: 2021-05-18
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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  • A preparation method of phosphor powder with controllable luminescence characteristics and the phosphor powder obtained
  • A preparation method of phosphor powder with controllable luminescence characteristics and the phosphor powder obtained
  • A preparation method of phosphor powder with controllable luminescence characteristics and the phosphor powder obtained

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 The average particle size is 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 re...

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 The average particle size is 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 th...

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Abstract

The invention discloses a method for preparing fluorescent powder with controllable luminescence characteristics and the obtained fluorescent powder. The preparation steps are: obtaining (Eu 3+ x+y A + y m 1‑x‑2y ) 2 SiO 4 Phosphor powder, the phosphor is obtained by microwave reduction method to obtain Eu 2+ , Eu 3+ Double-doped silicate phosphor——(Eu 2+ x Eu 3+ y A + y m 1‑x‑2y ) 2 SiO 4 . The preparation process of the present invention is simplified, fast, low energy consumption, process parameters are easy to control and adjust, condition control is simple and the adjustable range is large, and the controllable modulation of the light output performance of the fluorescent powder can be realized to meet different lighting requirements. Phosphor powder has a short production cycle, high production efficiency, and low requirements for equipment and conditions, which is conducive to the realization of material device integration and integrated design, so it has the potential for industrialization and mass 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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Patent Type & Authority Patents(China)
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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