KR101403755B1 - Green Phosphor - Google Patents
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Abstract
본 발명은 녹색 형광체에 관한 것으로, 소결온도 T의 합성 반응 분위기로부터 작성되며, 녹색 형광체의 일반식은 (Gd, Sr)3-x-yMxAl2O7: Ry，0≤ｘ≤１，0<ｙ≤0.3 (식 1) 이다. 그 중, M은 2가의 칼슘, 바륨 또는 이들의 혼합 원자가 화합물이고, R은 란탄계 금속의 원소이다. 또 (Gd, Sr)3-x-y는 GdzSr3-x-y-z, 0 < z < 3-x-y (식 2)의 표식이다. 이 종의 형광체는 자외광에 의해 여기되며, 광출사의 영역은 녹색광이다. (Gd, Sr) 3-xy M x Al 2 O 7 : R y , 0? X? 1, 0, < y? 0.3 (Equation 1). Among them, M is a divalent calcium, barium or a mixed atom compound thereof, and R is an element of a lanthanide metal. Further, (Gd, Sr) 3-xy is a mark of Gd z Sr 3-xyz and 0 <z < 3-xy (formula 2). The phosphor of this species is excited by ultraviolet light, and the region of light emission is green light.
Description
본 발명은 녹색 형광체에 관한 것이고, 특히 일반식이 (Gd, Sr)3-x- yMxAl2O7: Ry，0≤ｘ≤１，0<ｙ≤0.3 (식 1)이다. (Gd, Sr) 3-x- y M x Al 2 O 7 : R y , 0? X? 1, 0 < y ? 0.3 (Formula 1).
그 중, M은 2가의 칼슘, 바륨 또는 이들의 혼합 원자가 화합물이고, R은 란탄계 금속의 원소이다. Among them, M is a divalent calcium, barium or a mixed atom compound thereof, and R is an element of a lanthanide metal.
또 (Gd, Sr)3-x-y는 GdzSr3 -x-y-z, 0 < z < 3-x-y (식 2)의 표식이다. Further, (Gd, Sr) 3-xy is a label of Gd z Sr 3 -xyz and 0 <z < 3-xy (formula 2).
에너지 절약과 탄소경감이라고 하는 환경보호 의식의 태두로부터, 세계 각국 모두 백광의 발광 다이오드(Light emitting diode, LED)의 발전에 따라서 점점 중시되는 것과 함께, 종래의 조명 설비도 점차로 바뀌고 있다. 백광의 발광 다이오드는 체적이 작고, 전기소비가 적으며 (종래의 백열 전구의 십분의 일), 수명이 길고, 발광 효율이 높으며, 반응속도가 빠른 등, 많은 장점을 지니며, 현재는 표시장치, 신호등, 조명 등 폭넓게 응용되고 있다. 한편, 세계적인 에너지 부족 및 에너지 절약과 탄소경감이 점점 중시되고 있는 점에서, 발광 다이오드는 종래의 조명이 극복하지 못했던 문제를 해결할 수 있기 때문에, 장래는 더욱 중요한 조명 설비로 되는 것이 확실시된다. From the beginning of environmental conservation consciousness called energy saving and carbon abatement, all the countries around the world are increasingly emphasized by the development of white light emitting diode (LED), and the conventional lighting equipment is gradually changing. The light emitting diode of the white light has many advantages such as a small volume, low electric consumption (one tenth of a conventional incandescent lamp), a long life, a high luminous efficiency and a fast reaction speed. , Traffic lights, and lighting. On the other hand, since global energy shortage, energy saving, and carbon reduction are increasingly emphasized, light emitting diodes can solve the problems that conventional lighting can not overcome, and it is certain that the future will become more important lighting equipment.
니치아 가가꾸 고교 가부시끼가이샤는 1996년에 청색광의 LED를 가지고, 이트륨 알루미늄 가넷(Cerium-doped yttrium aluminum garnet; YAG: Ce) 도핑된 형광체를 여기시켜, 황색 형광체를 형성하고, 이 황색 형광체를 청색과 혼합한 것이 밸색광(미국특허 U.S. 5,998,925호 (특허문헌 1))의 발광을 성공하였다. 그러나, 이 종의 백색광 다이오드의 출사광은 차가운 색의 백광이고, 발광 영역에 적색광을 결여하고 있어 연색성도 낮다. 이 때문에, 현재의 백색광 다이오드는 청색의 다이오드에 황색의 형광체와의 조합 이외에, 청색의 다이오드에 녹색, 적색의 형광체 및 자외광 발광 다이오드 자외선 발광 다이오드(Ultraviolet light emitting diode, 이하 UV-LED라 칭함)를 청색과 녹색과 적색 3색의 형광체와의 조합에 의해 백색광을 형성하는 방식이 사용되고 있다. 그 중, UV-LED와 3색의 형광체와 조합한 것이 좋은 연색성을 얻을 수 있기 때문에, 자외광의 여기에 적절한 청색, 녹색 및 적색의 형광체의 개발은 현재 중요한 연구 과제이다. Nichia Kagaku Kogaku Co., Ltd., in 1996, excited a phosphor doped with cerium-doped aluminum garnet (YAG: Ce) with an LED of blue light to form a yellow phosphor, (US Pat. No. 5,998,925 (Patent Document 1)) successfully emitted light. However, the outgoing light of the white light diode of this species is white light of a cold color, and lacks red light in the light emitting region, and the color rendering property is also low. For this reason, in addition to the combination of a blue diode and a yellow phosphor, current white light diodes can be replaced by blue, green, red phosphors, and ultraviolet light emitting diodes (UV-LEDs) A combination of blue, green, and red phosphors is used to form white light. Among them, development of blue, green and red phosphors suitable for the excitation of ultraviolet light is an important research task because good color rendering property can be obtained by combining UV-LED and three-color phosphors.
1975년 Fava씨와 Flem씨가 Materials Research Bulltin (Vol. 10, p.75) Journal(비특허문헌 1)에서, Gd2SrAl2O7 의 구조를 발표하였다. 그것은 일종의 Sr3Ti2O7의 구조결에 속하고, 공간군은 I4/mmm이며, 결정구조는 [AlO4] 사면체를 구성하며, 일종의 층상 구조이다. 이 외에, Zvereva 등은 1994년, Russian Journal of General Chemistry (vol. 74, p.655) (비특허문헌 2)에서 Gd3＋ 와 Sr2＋는 결정에 있어서, 2개의 동일한 배위 격자를 갖고, 2개의 상이한 격자점 위치(lattice position)를 동시에 점하여 있고, 배위수는 각각 12 배위와 9 배위, 배위 원자는 양자 모두 산소 원자이다. 이 종의 결정 화합물은 간단하게 작성될 수 있지만, 녹색광을 여기하는 특성을 갖고 있지 않다. In 1975, Fava and Flem published the structure of Gd 2 SrAl 2 O 7 in Materials Research Bulletin (Vol. 10, p. 75) Journal (non-patent document 1). It belongs to a structure of Sr 3 Ti 2 O 7 , the space group is I4 / mmm, and the crystal structure constitutes [AlO 4 ] tetrahedron, and it is a layered structure. In addition, Zvereva et al. Have reported that Gd 3 + and Sr 2 + in crystals have two identical coordination lattices in the Russian Journal of General Chemistry (vol. 74, p.655) (non-patent document 2) Two different lattice positions are pointed at the same time, and the coordination number is 12 and 9, respectively. The coordination atoms are both oxygen atoms. The crystal compound of this species can be simply prepared, but does not have the property of exciting green light.
발명자는 형광체 분야에 있어서의 다년간의 연구 개발 경험을 기초로 하여, (Gd, Sr)3-xMxAl2O7 계통 중, 0 ≤ x ≤ 1, M을 2가의 칼슘 또는 바륨 또는 이들의 혼합 원자가 화합물을 사용하여, (Gd, Sr)3-xMx의 격자점 위치에 활성제로서 란탄계 원소 R을 도핑하는 것에 의해, (Gd, Sr)3-x-yMxAl2O7 : Ry (식 3)이 형성된다. 그 중, 혹시, R이 유로퓸 이온일 때, 당 화합물을 자외광에 의해 여기하면, 녹색의 형광을 발광한다. Based on the experience of many years of research and development in the field of phosphors, the inventors have found that among the (Gd, Sr) 3- xMxAl 2 O 7 system, 0 ≤ x ≤ 1, M is bivalent calcium or barium, use, (Gd, Sr) 3- x as an active agent to a grid point location of the M x by doping a lanthanide element R, (Gd, Sr) 3 -xy M x Al 2 O 7: R y ( formula 3 are formed. Among them, when R is a europium ion, if the compound is excited by ultraviolet light, green fluorescence is emitted.
본 발명의 일개 목적은, 자외광의 여기에 의해, 녹색광을 발광할 수 있는 녹색 형광체를 제공한다. An object of the present invention is to provide a green phosphor capable of emitting green light by excitation of ultraviolet light.
상기 목적을 달성하기 위하여, 본 발명의 녹색 형광체는 소결 온도 T의 합성 반응 분위기로 이루어지고, 녹색 형광체의 일반식은 (Gd, Sr)3-x-yMxAl2O7 : Ry, 0 ≤ x ≤ 1, 0 < y ≤ 0.3 (식 1)이다. 그 중, M은 2가의 칼슘, 바륨 또는 이들의 혼합 원자가 화합물이고, R은 란탄계 금속의 원소이다. 또 (Gd, Sr)3-x-y는 GdzSr3-x-y-z, 0 < z < 3-x-y (식 2)의 표식이다. 상기 녹색 형광체는 파장 300~450 nm의 광에 의해 여기된다. 또, 녹색 형광체는 출사하는 파장의 영역은 400 ~ 700 nm이다. 그 중, 소결 온도 T는 1500 ~ 1700℃이다. 또, 합성반응의 분위기는 H2 및 N2를 포함한다. In order to achieve the above object, the green phosphor of the present invention is in a synthesis reaction atmosphere of sintering temperature T, and the general formula of the green phosphor is (Gd, Sr) 3-xy M x Al 2 O 7 : R y , 1, 0 < y? 0.3 (Equation 1). Among them, M is a divalent calcium, barium or a mixed atom compound thereof, and R is an element of a lanthanide metal. Further, (Gd, Sr) 3-xy is a mark of Gd z Sr 3-xyz and 0 <z < 3-xy (formula 2). The green phosphor is excited by light having a wavelength of 300 to 450 nm. The green phosphor has a wavelength of 400 to 700 nm. Among them, the sintering temperature T is 1500 to 1700 ° C. The atmosphere of the synthesis reaction includes H 2 and N 2 .
일실시예에 있어서, 소결온도 T는 1600℃이다. 또, 합성 반응 분위기의 H2 와 N2의 비례는 H2 ≒ 10%, N2 ≒ 90%이다. In one embodiment, the sintering temperature T is 1600 占 폚. The proportions of H 2 and N 2 in the synthesis reaction atmosphere are H 2 ≒ 10% and N 2 ≒ 90%.
상기 배합 설계를 기초로, 본 발명에 의해 참신한 알루민산염 화합물을 제공하고, 자외광 영역의 광파를 유효하게 흡수하여, 녹색광 영역의 광파를 여기할 수 있다. Based on the above blending design, the inventive novel aluminate compound can be provided, the light wave in the ultraviolet light region can be effectively absorbed, and the light wave in the green light region can be excited.
도 1은 본 발명의 바람직한 실시예에 있어서의 Gd2Sr0 .977Al2O7 : Eu0 .03의 X선 분말 회절 스펙트럼도이다.
도 2는 본 발명의 바람직한 실시예 Gd2Sr0 .97Al2O7 : Eu0 .03의 X선 여기광 스펙트럼도이다.
도 3은 본 발명의 바람직한 실시예 Gd2SrO .97Al2O7 : Eu0 .03의 방사 스펙트럼
도 4는 본 발명의 바람직한 실시예 Gd2Sr0 .97Al2O7 : Eu0 .03의 색도 좌표도이다. 1 is an X-ray powder diffraction spectrum of Gd 2 Sr 0 .97 7Al 2 O 7 : Eu 0 .03 in a preferred embodiment of the present invention.
2 is an X-ray excitation light spectrum diagram of a preferred embodiment Gd 2 Sr 0 .97 Al 2 O 7 : Eu 0 .03 of the present invention.
3 is a graph showing the emission spectrum of a preferred embodiment of the present invention Gd 2 Sr O .97 Al 2 O 7 : Eu 0 .03
4 is a chromaticity coordinate diagram of a preferred embodiment Gd 2 Sr 0 .97 Al 2 O 7 : Eu 0 .03 of the present invention.
본 발명의 내용의 더 나은 이해를 도모하기 위하여, 이하에 의해 도면과 함께 설명한다. BRIEF DESCRIPTION OF THE DRAWINGS For a better understanding of the subject matter of the present invention, reference is made to the following description, taken in conjunction with the drawings, in which: Fig.
실시예Example
본 발명의 녹색 형광체의 일반식은 (Gd, Sr)3-x-yMxAl2O7 : Ry，0 ≤ ｘ ≤１，0 < y ≤ 0.3 (식１)이다. 그 중, M은 2가의 칼슘, 바륨 또는 이들의 혼합 원자가 화합물이고, R은 란탄계 금속의 원소다. Ce, Eu, Pr, Nd, Sm, Tb, Er, Yb, Dy의 어느 하나 또는 2개 이상의 혼합 원자가 화합물로부터 선택할 수 있다. 예컨대, 란탄계 금속이 2개 이상의 혼합 원자가 화합물일 때, R1y1R2y2R3y3…으로 나타낼 수 있다. 그 중, 0 < y1 ≤ 0.3, 0 < y2 ≤ 0.3, 0 < y3 ≤ 0.3,...이다. 또한, (Gd, Sr)3-x-y는 GdzSr3-x-y-z, 0 < z < 3-x-y 의 표식이다. 녹색 형광체의 제조는, 소결온도 T가 1500~1700℃, H2 및 N2를 포함하는 합성 반응 분위기에서, 히트 세트에 의해 합성한다. The general formula of the green phosphor of the present invention is (Gd, Sr) 3-xy M x Al 2 O 7 : R y , 0 ≦ x ≦ 1, 0 <y ≦ 0.3. Wherein M is a divalent calcium, barium or mixed atom compound thereof, and R is a member of a lanthanum-based metal. Any one or two or more mixed atoms of Ce, Eu, Pr, Nd, Sm, Tb, Er, Yb and Dy can be selected from the compounds. For example, when the lanthanide metal is a compound having two or more mixed atoms, R1 y1 R2 y2 R3 y3 ... . Among them, 0 < y1 0.3, 0 < y2 0.3, 0 < y3 0.3, .... Further, (Gd, Sr) 3-xy is a designation of Gd z Sr 3-xyz and 0 <z < 3-xy . The green phosphor is synthesized by heat setting in a synthesis reaction atmosphere containing sintering temperature T of 1,500 to 1,700 ° C, H 2 and N 2 .
바람직한 실시예에 있어서, 본 발명의 알루민산염 화합물의 화학식은 (Gd, Sr)3-x-yMxAl2O7 : Ry 이다. 그 중, M은 칼슘과 바륨의 혼합 원자가 화합물이고, R은 란탄계 원소 유로퓸 이온(Eu), 또 ｘ＝０, ｙ＝0.03이다. 본 실시예에 있어서, 제조에 사용된 출발원료는 Gd2O3, SrCO3, CaCO3, BaCO3, Al2O3와 Eu2O3을 그의 비례를 기초로 하여 적량을 취하고, 막자사발에 의해 균일하게 부수어 혼합한 후, 관상로에 넣어 1600℃, 수소(10%)/질소(90%) 환원 분위기에서 10시간을 소결한 후에 생성물을 획득할 수 있다. 정산 프로세스가 간단하고, 또 대량 생산에 적합하다. In a preferred embodiment, the formula of the aluminate compound of the present invention is (Gd, Sr) 3-xy M x Al 2 O 7 : R y . Among them, M is a mixed atom compound of calcium and barium, R is lanthanide element europium ion (Eu), and x = 0, y = 0.03. In this example, the starting materials used in the preparation were an appropriate amount based on the proportions of Gd 2 O 3 , SrCO 3 , CaCO 3 , BaCO 3 , Al 2 O 3 and Eu 2 O 3 , (10%) / nitrogen (90%) reducing atmosphere at 1600 ° C for 10 hours, and then the product can be obtained. The settlement process is simple and suitable for mass production.
도 1의 본 발명의 바람직한 실시예 Gd2Sr0 .97Al2O7 : Eu0 .03의 X선 분말 회절 스펙트럼도를 참조한다. 도시한 바와 같이, 본 발명의 바람직한 실시예에 있어서의 (Gd, Sr)3-x- yMxAl2O7 : Ry (x = 0, y = 0.03) (식 3)의 샘플은 X선 분말 회절 스펙트럼도에 의해, 결정상의 순도를 관찰한 결과는 기지 구조의 Gd2Sr0 .97Al2O7 표준 스펙트럼에 일치한다(JCPDS file NO: 00-076-0075). 따라서, 합성된 샘플은 순상(pure phase)을 입증할 수 있다. In the preferred embodiment Gd of the present invention of Figure 12Sr0 .97Al2O7 : Eu0 .03X-ray powder diffraction spectrum diagram of < RTI ID = 0.0 > As shown in the figure, in the preferred embodiment of the present invention, (Gd, Sr)3-x- yMxAl2O7 : Ry (x = 0, y = 0.03) The X-ray powder diffraction spectrum of the sample of the formula (3)2Sr0 .97Al2O7 It corresponds to the standard spectrum (JCPDS file NO: 00-076-0075). Thus, the synthesized sample can demonstrate a pure phase.
도 2의 본 발명의 바람직한 실시예 Gd2Sr0 .97Al2O7 : Eu0 .03의 X 여기광 스펙트럼도를 참조한다. 도시한 바와 같이, 본 실시예에 있어서, 샘플에 일정한 파장 513 nm의 광파를 출사시키는 것에 의해, 본 실시예는 300 nm로부터 450 nm의 광원에 의한 여기에 적합한 것을 알며, 자외선 발광 다이오드의 여기 파장 범위에 일치하는 것을 안다. The preferred embodiment Gd of the present invention in Figure 22Sr0 .97Al2O7 : Eu0 .03Quot; X < / RTI > excitation light spectrum diagram of FIG. As shown in the drawing, in this embodiment, by emitting a light wave having a constant wavelength of 513 nm to the sample, it is found that this embodiment is suitable for excitation by a light source of 300 nm to 450 nm, and the excitation wavelength of the ultraviolet light- I know that it matches the range.
이어서 도 3의 본 발명의 바람직한 실시예 Gd2Sr0 .97Al2O7 : Eu0 .03의 방사 스펙트럼도를 참조한다. 도시한 바와 같이, 본 실시예에 있어서, 알루민산염 화합물의 녹색 형광체는 365 nm의 여기 파장에 있어서, 출사광 스펙트럼이 513 nm에 파의 고점을 관찰할 수 있는 것과 함께 녹색 형광체의 출사 파장의 범위는 400~700 nm이다. Next preferred embodiment of the invention of Figure 3 Gd 2 Sr 0 .97 Al 2 O 7 : Refer to the emission spectrum of Eu 0 .03. As shown in the figure, in the present embodiment, the green phosphor of the aluminate compound can observe the peak of the wave at the excitation light spectrum at 513 nm at the excitation wavelength of 365 nm, and the emission wavelength of the green phosphor The range is 400 to 700 nm.
도 4의 본 발명의 바람직한 실시예 Gd2Sr0 .97Al2O7 : Eu0 .03의 색도 좌표도를 참조한다. 본 발명의 바람직한 실시예에 있어서, (Gd, Sr)3-x- yMxAl2O7 : Ry (x = 0, y = 0.03) (식 3)은 여기 파장 365 nm에서의 출사광 스펙트럼의 수치를 국제 조명 위원회가 제정한 색도좌표도에 기초로 하여 공식 환산을 실시한 결과, 출사광의 색도 좌표(0.2466, 0.4476)를 산출하여, 색도좌표도에 표시하면, 도 4에 나타내는 본 발명의 바람직한 실시예의 출사광은 녹색광의 영역인 것을 안다. A preferred embodiment of the invention of Figure 4 for example, Gd 2 Sr 0 .97 Al 2 O 7 : Eu 0 .03 . In a preferred embodiment of the present invention, (Gd, Sr) 3-x- y M x Al 2 O 7 : R y (x = 0, y = 0.03) (Equation 3) is a result of performing a formal conversion based on the chromaticity coordinate diagram established by the International Lighting Commission at the excitation light spectrum at the excitation wavelength of 365 nm. 0.2466, 0.4476) are calculated and expressed in the chromaticity coordinate diagram, it is known that the emitted light of the preferred embodiment of the present invention shown in Fig. 4 is a region of green light.
전술한 바와 같이, 본 발명의 녹색 형광체는 참신한 알루민산염 화합물을 사용하고, 300~450 nm 파장의 광파를 유효하게 흡수하여, 400~700 nm 파장의 광파를 출사할 수 있다. As described above, the green phosphor of the present invention can absorb light waves having a wavelength of 300 to 450 nm and emit light waves having a wavelength of 400 to 700 nm by using a novel aluminate compound.
(Gd, Sr)3-x- yMxAl2O7 : Ry (0≤ x ≤ 1, 0 < y ≤ 0.3 (Gd, Sr) 3-x- y M x Al 2 O 7 : R y (0? X? 1, 0 < y? 0.3
(Gd, Sr)3-x-y는 GdzSr3 -x-y-z, 0 < z < 3-x-y (Gd, Sr) 3-xy is Gd z Sr 3 -xyz , 0 <z < 3-xy
(Gd, Sr)3-x- yMxAl2O7 : Ry (x = 0, y = 0.03) (Gd, Sr) 3-x- y M x Al 2 O 7 : R y (x = 0, y = 0.03)
Claims (8)
상기 식 중에서,
M은 2가의 칼슘, 바륨 또는 이들의 혼합 원자가 화합물이고,
R은 란탄계 금속의 원소이며,
(Gd, Sr)3-x-y는 GdzSr3-x-y-z, 0 < z < 3-x-y (식 2)의 표식이다. A green phosphor comprising the following formula (Gd, Sr) 3-xy M x Al 2 O 7 : R y , 0? X? 1, 0 <
In the formula,
M is a divalent calcium, barium or mixed atom compound thereof,
R is an element of the lanthanide metal,
(Gd, Sr) 3-xy is a label of Gd z Sr 3-xyz , 0 <z < 3-xy (Formula 2).
The green phosphor according to claim 7, wherein the volume ratio of H 2 and N 2 in the synthesis reaction atmosphere is 10:90.
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