Nitride red phosphor and process for producing the same

一种红色荧光、荧光材料的技术，应用在红色氮化物荧光材料领域，能够解决荧光材料数量少等问题

Inactive Publication Date: 2007-12-19
UBE IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, there are very few reports on fluorescent materials that absorb blue light and emit red photoluminescence

Method used

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  • Nitride red phosphor and process for producing the same
  • Nitride red phosphor and process for producing the same
  • Nitride red phosphor and process for producing the same

Examples

Experimental program
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Embodiment 1

[0114] In order to obtain Eu powder as a raw material, metal europium is directly nitrided. In a nitrogen box, metallic europium (manufactured by Soekawa Chemical Co., Ltd., 99.9%, block) was filed with a file to obtain fine-grained metallic europium of 350 μm or less. The obtained fine-grained metal europium was charged into a carbon crucible and the crucible was kept at 500° C. for 15 minutes in a nitrogen atmosphere, then kept at 750° C. for 2 hours, further kept at 900° C. for 1 hour, and then in a furnace cool down. After cooling, the crucible was placed in a nitrogen box and the EuN was removed in a nitrogen atmosphere. This powder was pulverized into a powder of 150 μm or less and used as a raw material.

[0115] Subsequently, in order to obtain Ca 3 N 2 Powder, directly nitrided calcium metal. In a nitrogen box, metallic calcium (manufactured by Wako Pure Chemical Co., Ltd., 99.0%, granular) was charged into a carbon crucible and the crucible was kept at 450° C. f...

Embodiment 2

[0132]Prepare the same raw material as in Example 1, and in a nitrogen box with Ca 3 N 2 :AlN:Si 3 N 4 = Ratio of 20.0:60.0:20.0 (mol %) These raw materials were weighed, and EuN was further added to 100 parts by weight of the raw materials obtained in the above ratio so that Eu was 1.5 parts by weight. The resulting mixture was fired by the same method as in Example 1 to obtain a red fluorescent material. Figure 8 shows the X-ray diffraction pattern of this powder. Similar to Example 1, FIG. 9 shows an enlarged view of a portion where 2θ is 30°-42°. Here, for comparison, this red fluorescent material was compared with Comparative Example 9 (orthogonal CaAlSiN 3 ) and Example 1 (monoclinic CaAlSiN 3 )Compare. According to the comparison, it was found that the red fluorescent material of this example was a crystal similar to Example 1 and was monoclinic. Fig. 10 similarly shows a comparison of parts with 2Θ of 45°-70°. Also in this section, it was confirmed that the cr...

Embodiment 3

[0135] Prepare the same raw material as in Example 1, and in a nitrogen box with Ca 3 N 2 :AlN:Si 3 N 4 = Ratio of 60.0:30.0:10.0 (mol %) These raw materials were weighed, and EuN was further added to 100 parts by weight of the raw materials obtained in the above ratio so that Eu was 1.5 parts by weight. The resulting mixture was fired by the same method as in Example 1 to obtain a red fluorescent material. Figure 11 shows the X-ray diffraction pattern of this powder. The residue of CaO is remarkable, but the X-ray diffraction pattern except for CaO is the same as that of Example 1 and this red fluorescent material is found to be monoclinic CaAlSiN 3 . Since the red fluorescent material contained CaO, pickling was performed in the same manner as in Example 1 to remove CaO. The photoluminescence spectrum and the excitation spectrum were measured by the same method as in Example 1, and it was found that the photoluminescence spectrum and the excitation spectrum were almost...

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Abstract

A red phosphor whose phosphor-constituting crystal phase consists of CaAlSiN3 activated by monoclinic Eu. In particular, there is provided a red phosphor characterized by consisting of powder of CaAlSiN3 activated by Eu having an average particle diameter, as in unpulverized form measured by the laser diffraction / scattering particle size distribution measuring method, of = 10 [mu]m. Further, there is provided a light emitting device comprising a blue light emitting element, the above red phosphor capable of converting blue light emitted by the blue light emitting element to red light and a yellow phosphor capable of converting the blue light to yellow light. Still further, there is provided a process for producing CaAlSiN3 activated by Eu, comprising firing in a nitrogenous atmosphere at 1400 to 2000 DEG C a raw material powder of Ca3N2, AlN and Si3N4 whose composition falls within the region as enclosed in the composition diagram of 1 by straight lines connecting four points A to D each represented by (Ca3N2 : AlN : Si3N4) wherein the Ca3N2, AlN and Si3N4 mean molar ratio thereof, as follows: Point A: (10:70:20), Point B: (10:65:25), Point C: (70:23:7), and Point D: (70:22:8), the raw material powder further containing EuN in an amount of 0.01 to 20 pts.wt. in terms of Eu per 100 pts.wt. of the sum of Ca3N2, AlN and Si3N4.

Description

technical field [0001] The invention relates to a red nitride fluorescent material used in displays, liquid crystal backlights, fluorescent lamps, white light-emitting diodes, etc., and a manufacturing method thereof. Background technique [0002] As the practical use of blue diodes has been realized recently, research is being actively conducted to develop white light emitting diodes by using blue diodes as light sources. Such white light-emitting diodes are lightweight, do not use mercury, and have a long life, so demand for them is expected to grow rapidly in the future. The commonly used white light-emitting diode is YAG (Y 3 Al 5 o 12 :Ce) powder and epoxy resin mixture paste coating blue light emitting device prepared (see Japanese Unexamined Patent Publication (Kokai) No. 2000-208815). [0003] However, the color of YAG:Ce photoluminescence is located near x=0.41 and y=0.56 in the CIE chromaticity coordinates, and when mixed with the color of blue excitation light...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/64C01B21/082C09K11/08
CPCC01P2002/84C01B21/0602C01P2002/72C01P2002/77C09K11/7728C09K11/0883C01P2006/60C01P2002/54
Inventor 坂田信一山尾猛山田哲夫
Owner UBE IND LTD
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