WO2016114481A1 - Procédé de production d'un matériau de conversion de couleur faisant appel à une nanopoudre de verre, et dispositif émettant de la lumière blanche - Google Patents

Procédé de production d'un matériau de conversion de couleur faisant appel à une nanopoudre de verre, et dispositif émettant de la lumière blanche Download PDF

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Publication number
WO2016114481A1
WO2016114481A1 PCT/KR2015/012177 KR2015012177W WO2016114481A1 WO 2016114481 A1 WO2016114481 A1 WO 2016114481A1 KR 2015012177 W KR2015012177 W KR 2015012177W WO 2016114481 A1 WO2016114481 A1 WO 2016114481A1
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WO
WIPO (PCT)
Prior art keywords
phosphor
color conversion
glass
conversion material
glass powder
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PCT/KR2015/012177
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English (en)
Korean (ko)
Inventor
박태호
황평하
임형석
김종성
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(주)베이스
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Publication of WO2016114481A1 publication Critical patent/WO2016114481A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/078—Glass compositions containing silica with 40% to 90% silica, by weight containing an oxide of a divalent metal, e.g. an oxide of zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/089—Glass compositions containing silica with 40% to 90% silica, by weight containing boron
    • C03C3/091—Glass compositions containing silica with 40% to 90% silica, by weight containing boron containing aluminium

Definitions

  • the present invention relates to a color conversion glass (Phosphor In Glass (PIG)) manufacturing technology for LEDs, and more particularly to a method for producing a color conversion material and a light emitting device having excellent color conversion efficiency and light transmittance using nano glass powder. will be.
  • POG Phosphor In Glass
  • Phosphors are required for white light emission from LEDs emitting monochromatic light such as blue light.
  • the following three methods are mainly used to implement the phosphor.
  • the first method is to mold silicon mixed with yellow phosphor on a blue LED chip.
  • the white LED package manufactured in such a form there is a problem in that yellowing occurs due to deterioration of the color conversion material at a high temperature, and also serves as a main factor in the deterioration of reliability due to gas and moisture penetration.
  • the second is a method of dispersing and molding a yellow phosphor in an organic material such as epoxy. In this case, too, there is a problem that the heat resistance is weak by using an organic material.
  • the third method is to mount a color conversion glass (Phosphor In Glass (PIG)) in which a yellow phosphor is dispersed in the glass in a cover form.
  • POG Phosphor In Glass
  • the high temperature deterioration problem can be solved as described above, and the resistance to gas and moisture penetration is also excellent.
  • firing should be performed at a sufficiently high temperature to increase the light transmittance.
  • the problem of phosphor degradation often occurs.
  • One object of the present invention is to provide a method for producing a color conversion material that can reduce the firing temperature using the nano glass powder to suppress the reaction with the phosphor, and also excellent light transmittance.
  • Another object of the present invention is to provide a white light emitting device having excellent color conversion efficiency and light transmittance even when the temperature of the light emitting device is increased to 200 ° C. or more.
  • Color conversion material manufacturing method for achieving the above object is a method of manufacturing a color conversion material (Phosphor In Glass (PIG)) is disposed on the front of the LED to convert the color, the average particle diameter of 100nm Forming a nano glass powder which is less than or equal to; Mixing the nano glass powder and the phosphor to form a mixture; Molding the mixture to form a molded body; And firing the molded body.
  • POG Phosphor In Glass
  • Color conversion material manufacturing method for achieving the above object is a method for manufacturing a color conversion material to convert the color is disposed on the front surface of the LED, forming a nano glass powder having an average particle diameter of 100nm or less Making; Preparing a paste including the nano glass powder and the phosphor; And baking the paste on the substrate glass and then firing the paste.
  • the phosphor may be (Lu x Ce 1-x ) 3 Al 5 O 12 (0.75 ⁇ x ⁇ 0.95).
  • a white light emitting device for achieving the other object includes an LED and a color conversion material (Phosphor In Glass (PIG)) disposed on the front of the LED, the LED emits blue light, the color
  • POG Phosphor In Glass
  • the conversion material is a yellow phosphor is dispersed in the glass, the yellow phosphor is characterized in that (Lu x Ce 1-x ) 3 Al 5 O 12 (0.75 ⁇ x ⁇ 0.95).
  • the glass in weight%, SiO 2 55-70%, Al 2 O 3 10-22%, B 2 O 3 1-15%, CaO 10% or less and SrO 2-10%, R 2 O (R Li, Na, K, Rb and Cs), Sb 2 O 3 , F, Cl, SO 3 , P 2 O 5 , V 2 O 5 , PbO, ZnO and Bi 2 O 3 are not intentionally added It may not be.
  • the glass by weight SiO 2 55-70%, Al 2 O 3 10-22%, B 2 O 3 1-15%, CaO 10% or less, SrO 2-10%, MgO 5% by weight or less
  • the firing temperature can be lowered without lowering the light transmittance, and thus the phosphor reaction. By suppressing this, the fall of the color conversion efficiency can be prevented.
  • Figure 1 (Lu 0. 9 Ce 0. 1) shows the characteristics change according to the temperature of 3 Al 5 O 12 phosphor.
  • FIG. 2 schematically shows an example of a white light emitting device according to the present invention.
  • the method for producing a color conversion material (Phosphor In Glass; PIG) according to the present invention uses a nano glass powder having an average particle diameter of 100 nm or less.
  • the glass firing temperature In the case of a glass-based color conversion material, the glass firing temperature must be high enough to suppress the generation of bubbles, thereby obtaining a high light transmittance. However, at such high firing temperatures, color conversion efficiency decreases often due to phosphor deterioration.
  • the present invention provides a method for producing a color conversion material having excellent light transmittance and excellent color conversion efficiency by applying such characteristics.
  • the color conversion material manufacturing method according to an embodiment of the present invention may use a bulk baking method or a paste baking method.
  • a nano glass powder having an average particle diameter of 100 nm or less is formed, and mixed with a phosphor to form a mixture, and then molding, and then firing the molded body.
  • the phosphor may be included in an amount of about 3 to 70 wt% based on the total weight of the nano glass powder and the phosphor.
  • the content of the phosphor may be adjusted by the thickness of the color conversion material, the LED size, the number of LEDs, and the like.
  • a process may include forming a nano glass powder having an average particle diameter of 100 nm or less, preparing a paste including the nano glass powder and the phosphor, applying the paste to the substrate glass, and then firing the paste.
  • the paste may include an organic solvent, an organic binder, and the like, and these components are removed in a drying process and a firing process after applying the paste.
  • Phosphors can be degraded not only at high temperatures but also by the glass itself.
  • SiO 2 contributes to improving the glass stability by forming a three-dimensional network structure.
  • the SiO 2 is preferably added at 55 to 70% by weight of the total weight of the glass. When the addition amount of SiO 2 is less than 55% by weight, the addition effect is insufficient. In contrast, if SiO 2 exceeds 70% by weight, there is a problem in the glass softening temperature is too high.
  • Al 2 O 3 contributes to glass stabilization.
  • the Al 2 O 3 is preferably added at 10 to 22% by weight of the total weight of the glass.
  • the addition amount of Al 2 O 3 is less than 10% by weight, the addition effect is insufficient.
  • the addition amount of Al 2 O 3 exceeds 22% by weight, the glass fluidity may be greatly reduced.
  • B 2 O 3 contributes to the formation of mesh, and contributes to lowering the firing temperature through viscosity reduction.
  • the B 2 O 3 is preferably added in 1 to 15% by weight of the total weight of the glass. When the amount of B 2 O 3 added is less than 1% by weight, the effect of addition is insufficient. In contrast, when the amount of B 2 O 3 added exceeds 15% by weight, crystallization of the glass may proceed rapidly.
  • CaO and SrO lower the softening temperature of the glass, contributing to lowering the firing temperature for producing color converted glass.
  • These components are preferably added in CaO: 10% by weight or less, SrO: 2-10% by weight, and may further include one or more of 5% by weight or less of MgO and 5% by weight or less of BaO.
  • the total content of CaO, SrO, MgO, BaO is more preferably 10 to 25% by weight of the total weight of the glass.
  • the softening temperature may be lowered without reducing the light transmittance, and when any component exceeds the above range, problems such as reduced fluidity and promotion of crystallization may occur.
  • the glass having the composition has a micro size of about 100 ⁇ m
  • the glass may be manufactured by baking at about 800 ° C. or more corresponding to a softening temperature or more.
  • the firing temperature may be lowered to about 750 °C or more.
  • the firing temperature is too high exceeding 980 °C, phosphor discoloration may occur.
  • the phosphors were mixed in the same amount and molded in a plate form, and then baked at the firing temperature shown in Table 3 for 30 minutes to prepare a color conversion material.
  • a unit is a weight part, and when a total is 100 weight part, it is the same value as weight%.
  • the phosphor discoloration did not occur as a whole, although firing was performed at 800 ° C. or higher. However, in case of specimen 42, the phosphor was slightly discolored when firing was performed at an excessively high temperature of 1000 ° C.
  • the glass powder having an average particle diameter of 100 ⁇ m is used.
  • the firing temperature may be lowered, and thus the effect of preventing phosphor degradation during firing may be further improved.
  • the phosphor may be a (Lu x Ce 1-x ) 3 Al 5 O 12 (0.75 ⁇ x ⁇ 0.95) phosphor.
  • yellow and blue light emitting phosphor is a YAG phosphor
  • SiO 4 phosphor a nitride phosphor is used.
  • these phosphors have a characteristic in that when the temperature of the light emitting device rises above 200 ° C by driving the LED, the characteristics thereof deteriorate rapidly.
  • FIG. 2 schematically shows an example of a white light emitting device according to the present invention.
  • the white light emitting device includes an LED chip 102 and a color conversion material 103.
  • the LED chip 102 is mounted on the package body 101 and outputs blue light.
  • the color conversion material 103 is disposed in front of the LED, the color conversion material is a yellow phosphor dispersed in the glass, the yellow phosphor as described above (Lu x Ce 1 -x ) 3 Al 5 O 12 (0.75 ⁇ x ⁇ 0.95).
  • the firing temperature can be lowered without lowering the light transmittance. Therefore, the fall of color conversion efficiency can be prevented by suppressing fluorescent reaction.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Led Device Packages (AREA)
  • Luminescent Compositions (AREA)
  • Glass Compositions (AREA)

Abstract

Cette invention concerne un procédé de production d'un matériau de conversion de couleur faisant appel à une nanopoudre de verre, et un dispositif émettant de la lumière blanche. Le procédé de production d'un matériau de conversion de couleur faisant appel à une nanopoudre de verre selon l'invention est un procédé de production d'un matériau de conversion de couleur (phosphore dans verre (PIG)) qui est agencé sur la face avant d'une LED et convertit les couleurs, le procédé comprenant les étapes consistant à : broyer du verre parent pour former une nanopoudre de verre ayant une taille moyenne de grain égale ou inférieure à 100 nm ; mélanger le nanopoudre de verre et des phosphores pour former un mélange ; mettre le mélange en forme pour obtenir un corps compact ; et fritter le corps compact.
PCT/KR2015/012177 2015-01-13 2015-11-12 Procédé de production d'un matériau de conversion de couleur faisant appel à une nanopoudre de verre, et dispositif émettant de la lumière blanche WO2016114481A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR1020150006430A KR101631829B1 (ko) 2015-01-13 2015-01-13 나노 유리 파우더를 이용한 색변환 소재 제조 방법 및 백색 발광 장치
KR10-2015-0006430 2015-01-13

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WO2016114481A1 true WO2016114481A1 (fr) 2016-07-21

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11920072B2 (en) * 2019-04-11 2024-03-05 Nichia Corporation Method for producing rare earth aluminate sintered body

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102166026B1 (ko) * 2019-12-16 2020-10-15 한국세라믹기술원 고강도 색변환 소재용 유리 조성물 및 색변환 소재의 제조방법

Citations (5)

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Publication number Priority date Publication date Assignee Title
KR20090026308A (ko) * 2006-07-18 2009-03-12 쇼와 덴코 가부시키가이샤 형광체, 그 제조 방법 및 발광 장치
KR20100040442A (ko) * 2008-10-10 2010-04-20 삼성에스디아이 주식회사 플라즈마 디스플레이 패널용 녹색 형광체, 이를 포함하는 녹색 형광체 조성물 및 이를 채용한 플라즈마 디스플레이 패널
JP2011108599A (ja) * 2009-11-20 2011-06-02 Toshiba Lighting & Technology Corp 照明装置
KR101253381B1 (ko) * 2005-05-11 2013-04-11 니폰 덴키 가라스 가부시키가이샤 형광체 복합 유리, 형광체 복합 유리 그린 시트 및 형광체 복합 유리의 제조 방법
JP2014221706A (ja) * 2013-05-14 2014-11-27 株式会社オハラ 複合材料及びその製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101253381B1 (ko) * 2005-05-11 2013-04-11 니폰 덴키 가라스 가부시키가이샤 형광체 복합 유리, 형광체 복합 유리 그린 시트 및 형광체 복합 유리의 제조 방법
KR20090026308A (ko) * 2006-07-18 2009-03-12 쇼와 덴코 가부시키가이샤 형광체, 그 제조 방법 및 발광 장치
KR20100040442A (ko) * 2008-10-10 2010-04-20 삼성에스디아이 주식회사 플라즈마 디스플레이 패널용 녹색 형광체, 이를 포함하는 녹색 형광체 조성물 및 이를 채용한 플라즈마 디스플레이 패널
JP2011108599A (ja) * 2009-11-20 2011-06-02 Toshiba Lighting & Technology Corp 照明装置
JP2014221706A (ja) * 2013-05-14 2014-11-27 株式会社オハラ 複合材料及びその製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US11920072B2 (en) * 2019-04-11 2024-03-05 Nichia Corporation Method for producing rare earth aluminate sintered body

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