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Method for preparing M2SiO4-based fluorescent powders at lower temperature

A low-temperature, fluorescent powder technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of high requirements for heating equipment configuration, easy generation of heterogeneous phases, large energy consumption, etc., and achieve low requirements for synthesis equipment, The effect of shortening the time and reducing energy consumption and equipment loss

Active Publication Date: 2013-04-03
江苏龙力泵阀制造有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method often requires multiple high-temperature firings, and it is easy to generate impurity phases during this process
The above-mentioned preparation process consumes a lot of energy in production, and has high requirements on the configuration of heating equipment. Synthetic products generally need to be post-processed such as crushing and grading, which consumes time and energy.

Method used

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  • Method for preparing M2SiO4-based fluorescent powders at lower temperature
  • Method for preparing M2SiO4-based fluorescent powders at lower temperature
  • Method for preparing M2SiO4-based fluorescent powders at lower temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Sr 1.93 Ba 0.05 SiO 4 :0.02Eu 2+ Preparation of yellow phosphor:

[0019] Weigh 0.0965 mole Sr(NO 3 ) 2 , 0.0025 mol Ba(NO 3 ) 2 , 0.167 mole CON 2 H 4 , 0.001 mole Eu(NO 3 ) 3 .6H 2 O and 0.05 mole SrCl 2 ·6H 2 O mix them and grind them in an agate mortar for 30 minutes to make them thoroughly mixed to obtain a paste mixture A; add 0.05 mole (C 2 H 5 O) 4 Si was added to the mixture A, and it was thoroughly ground and mixed in a mortar for 60 minutes until gel B was obtained; then the gel B was moved to a muffle furnace at 550° C., taken out and ground after 30 minutes, and powder C was obtained. Put powder C into a reducing atmosphere furnace, heat it to 850℃, keep it for 1h, and keep it at 20%H 2 -80% Ar reduced to 200℃ in a reducing atmosphere, take it out, grind in a mortar for 5 minutes to obtain product D; finally weigh an appropriate amount of product D, soak in 100ml, 80℃ deionized water and stir for 6 hours, filter and dry it at 100℃ Dry to high purity Sr 1.93 Ba ...

Embodiment 2

[0021] Sr 1.93 Ba 0.05 SiO 4 :0.02Eu 2+ Preparation of yellow phosphor:

[0022] Weigh 0.0965 mole Sr(NO 3 ) 2 , 0.0025 mol Ba(NO 3 ) 2 , 0.167 mole CON 2 H 4 , 0.001 mole Eu(NO 3 ) 3 .6H 2 O and 0.025 mole SrCl 2 ·6H 2 O mix them and grind them in an agate mortar for 30 minutes to make them thoroughly mixed to obtain a paste mixture A; add 0.05 mole (C 2 H 5 O) 4 Si was added to the mixture A, and it was thoroughly ground and mixed in a mortar for 60 minutes until gel B was obtained; the rest were the same as in Example 1. The product obtained is pure phase Sr 1.93 Ba 0.05 SiO 4 :0.02Eu 2+ Yellow phosphor.

Embodiment 3

[0024] Sr 1.93 Ba 0.05 SiO 4 :0.02Eu 2+ Preparation of yellow phosphor:

[0025] Weigh 0.0965 mole Sr(NO 3 ) 2 , 0.0025 mol Ba(NO 3 ) 2 , 0.167 mole CON 2 H 4 , 0.001 mole Eu(NO 3 ) 3 .6H 2 O and 0.0125 mole SrCl 2 ·6H 2 O mix them and grind them in an agate mortar for 30 minutes to make them thoroughly mixed to obtain a paste mixture A; add 0.05 mole (C 2 H 5 O) 4 Si was added to the mixture A, and it was thoroughly ground and mixed in a mortar for 60 minutes until a gel B was obtained; the rest were the same as in Example 1. The product obtained is high purity Sr 1.93 Ba 0.05 SiO 4 :0.02Eu 2+ Yellow phosphor.

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Abstract

The invention discloses a method for preparing M2SiO4-based fluorescent powders at lower temperature, comprising the following steps: firstly, weighing needed metal nitrate, urea and SrCl2 6H2O according to the stoichiometric ratio of M2SiO4, wherein M is one or more of Zn, Mg, Sr, Ca, Ba, Mn and Eu; adding needed (C2H5O)4Si after the metal nitrate, the urea and the SrCl2 6H2O are fully mixed, and then fully mixing for a second time to obtain gel; and secondly, moving the gel into a muffle furnace of 550 DEG C, taking out after 30 min, firing the gel in a reduction atmosphere furnace at 800-870 DEG C for 1h after grinding, taking out after cooling to 200 DEG C in the reduction atmosphere, and carrying out treatments of washing by deionized water, filtering and drying after a little grinding, so as to obtain the high-purity M2SiO4-based fluorescent powders. The method has low synthesis temperature (below 870 DEG C), short time (1h), simple process flow, easy operation and low requirements for synthesizing equipment and is beneficial to industrialization.

Description

Technical field [0001] The invention relates to a preparation of M at a lower temperature 2 SiO 4 The method of matrix phosphor belongs to the technical field of material synthesis. technical background [0002] M 2 SiO 4 Matrix silicate phosphors are widely used in various optical fields due to their stable physical and chemical properties, excellent aging resistance, high light conversion efficiency, high crystallinity, and good transparency of crystals. In M 2 SiO 4 Add a small amount of different luminescent ions (Mn 2+ , Eu 2+ Etc.) can make it have different luminous properties. Such as ZnSiO 4 :Mn 2+ Green phosphors are widely used in CRT, PDP, long-lasting display and other fields; (Ba, Sr, Ca, Mg) 2 SiO 4 :Eu 2+ Yellow phosphors are widely used in the field of white LED lighting. [0003] Currently, M 2 SiO 4 (M is selected from one or more element combinations among Zn, Mg, Sr, Ca and Ba) The preparation of matrix silicate phosphor mainly adopts the traditional high temp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/79
Inventor 强耀春张宝林
Owner 江苏龙力泵阀制造有限公司