KR101525317B1 - Phosphor and light emitting device comprising the same - Google Patents
Phosphor and light emitting device comprising the same Download PDFInfo
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- KR101525317B1 KR101525317B1 KR1020130132126A KR20130132126A KR101525317B1 KR 101525317 B1 KR101525317 B1 KR 101525317B1 KR 1020130132126 A KR1020130132126 A KR 1020130132126A KR 20130132126 A KR20130132126 A KR 20130132126A KR 101525317 B1 KR101525317 B1 KR 101525317B1
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 229910052788 barium Inorganic materials 0.000 claims abstract description 20
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 11
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 11
- 229910052777 Praseodymium Inorganic materials 0.000 claims abstract description 11
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 11
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 11
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 11
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 10
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 9
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 9
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 7
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 7
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 7
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 7
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 6
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 5
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 5
- 229910052732 germanium Inorganic materials 0.000 claims abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 4
- 238000000634 powder X-ray diffraction Methods 0.000 claims abstract description 4
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 3
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 3
- 229910052718 tin Inorganic materials 0.000 claims abstract description 3
- 230000001747 exhibiting effect Effects 0.000 claims abstract 2
- 239000013078 crystal Substances 0.000 claims description 14
- 230000005284 excitation Effects 0.000 claims description 12
- 239000011159 matrix material Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 229910052693 Europium Inorganic materials 0.000 claims description 7
- 238000002441 X-ray diffraction Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 229910000789 Aluminium-silicon alloy Inorganic materials 0.000 claims 1
- 229910052748 manganese Inorganic materials 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 82
- 239000002994 raw material Substances 0.000 description 45
- 239000000843 powder Substances 0.000 description 44
- 238000001354 calcination Methods 0.000 description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 21
- 229910001873 dinitrogen Inorganic materials 0.000 description 19
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 17
- 238000002156 mixing Methods 0.000 description 15
- 238000010298 pulverizing process Methods 0.000 description 15
- 238000005303 weighing Methods 0.000 description 8
- 229910052765 Lutetium Inorganic materials 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000004767 nitrides Chemical group 0.000 description 2
- 229910016569 AlF 3 Inorganic materials 0.000 description 1
- 101100496858 Mus musculus Colec12 gene Proteins 0.000 description 1
- 229910002795 Si–Al–O–N Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
본 발명은 일반식 (A)1-xREx(B)a(X)b (여기서, A는 Ba, Sr, Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu 및 Zn 중에서 선택된 원소를 1종 이상 포함하고, B는 Al, Si, P, Ga, Ge, Sn 및 Bi 중에서 선택된 1종 이상 포함하고, X는 O, N, Cl, F, C , S 및 Se 중에서 선택된 1종 이상 포함하고, RE는 Eu를 필수원소로 하고, Mn, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm 및 Yb 중에서 선택된 원소를 1종 이상 포함함)로 나타내는 형광체로서, 분말 X선 회절 패턴에 있어서 가장 강도가 있는 회절 피크의 상대 강도를 100%로 했을 때, 상기 X선 회절 패턴의 브래그 각도(2θ)가 15.7°~16.5°, 24.6°~25.8°, 31.1°~32.2°, 36.1°~37.1°인 범위에서 상대강도 10% 이상의 회절피크를 나타내는 상을 주상으로 포함하고, 상기 a 및 b는 4≤a≤6, 6≤b≤12 인 형광체를 제공한다.(A) 1-x RE x (B) a (X) b wherein A is at least one element selected from the group consisting of Ba, Sr, Ca, Mg, Sc, Y, La, Ce, Pr, At least one element selected from the group consisting of Al, Si, P, Ga, Ge, Sn and Bi, and at least one element selected from the group consisting of Gd, Tb, Dy, Ho, Er, Tm, Yb, X is at least one element selected from the group consisting of O, N, Cl, F, C, S and Se; RE is at least one element selected from the group consisting of Mn, Ce, Pr, Nd, Sm, Gd, Tb, Er, Tm, and Yb), wherein, assuming that the relative intensity of the diffraction peak having the highest intensity in the powder X-ray diffraction pattern is 100%, the phosphor represented by Bragg And a phase exhibiting a diffraction peak of 10% or more in relative intensity in the range of angles (2?) Of 15.7 to 16.5, 24.6 to 25.8, 31.1 to 32.2, and 36.1 to 37.1, b is 4? a? 6, and 6? b? 12.
Description
본 발명은 새로운 결정구조를 갖는 형광체와 이 형광체를 포함하는 발광장치에 관한 것으로, 보다 상세하게는 내구성이 우수한 산질화물로 이루어지고 자외선 발광 다이오드를 여기원으로 할 때 하늘색 발광이 가능하며 특히 사이알론(SIALON) 형광체의 대체 또는 보완용으로 적합하게 사용될 수 있는 새로운 산질화물계 형광체와 이 형광체를 포함하는 발광장치에 관한 것이다.The present invention relates to a phosphor having a novel crystal structure and a light emitting device including the phosphor. More particularly, the present invention relates to a light emitting device comprising an oxynitride excellent in durability and capable of emitting blue light when an ultraviolet light emitting diode is used as an excitation source, (SIALON) phosphors, and a light emitting device including the phosphor.
최근 조명, LCD 백라이트, 자동차 조명용 등으로 각광을 받고 있는 백색 LED발광장치는, 통상 청색 또는 근자외선을 방출하는 LED 발광소자와, 이 발광소자에서 방출하는 광을 여기원으로 하여 파장을 가시광선으로 변환시키는 형광체를 포함하여 이루어진다.BACKGROUND ART [0002] A white LED light emitting device, which has recently been spotlighted for illumination, LCD backlighting, automobile lighting, and the like, has an LED light emitting device that emits blue or near ultraviolet light and a light source that emits light from the light emitting device, And a phosphor for converting the phosphor.
이러한 백색 LED를 구현하는 방법으로 종래, 발광 소자로서 파장이 450~550nm인 InGaN계 재료를 사용한 청색 발광 다이오드를 사용하고 형광체로는 (Y,Gd)3(Al,Ga)5O12의 조성식으로 표현되는 황색발광의 YAG계 형광체를 사용한 것이 대표적인데, 이 백색 LED는 발광 소자로부터 방출된 청색광을 형광체층으로 입사시켜 형광체층 내에서 수회의 흡수와 산란을 반복하며 이 과정에서 형광체에 흡수된 청색광은 황색으로 파장변환이 이루어진 황색광과 입사된 청색광의 일부가 혼합되어 인간의 눈에는 백색으로 보이게 하는 것이다.These white as how to implement the LED using a conventional blue light emitting diode with an InGaN-based material having a wavelength of 450 ~ 550nm as a light emitting element and phosphor is (Y, Gd) as the 3 (Al, Ga) 5 O 12 composition formula In this white LED, the blue light emitted from the light emitting device is incident on the phosphor layer, and absorption and scattering are repeated several times in the phosphor layer. In this process, the blue light absorbed by the phosphor A part of the yellow light whose wavelength is converted into yellow and the blue light which is incident is mixed to make the white light appear to the human eye.
그러나 이러한 구조의 백색 LED는 빛에 적색 성분이 적고, 색 온도가 높으며, 적색 및 녹색 성분이 부족하여 연색성이 떨어지는 조명광 밖에 얻지 못한다는 문제점이 있다.However, the white LED of such a structure has a problem that only a red light component is less in color, a color temperature is high, and only red light and green component are lacking, so that only an illumination light with poor color rendering is obtained.
또한, 산화물계 형광체의 경우, 일반적으로 여기원의 파장이 400nm를 넘어서면 발광강도가 저하하는 경향을 보이기 때문에, 청색광을 이용하여 고휘도의 백색광을 만들기에 적합하지 않은 점도 있다.In addition, in the case of the oxide-base phosphor, in general, when the wavelength of the excitation source exceeds 400 nm, the emission intensity tends to be lowered, and therefore, it is not suitable for producing white light of high luminance by using blue light.
이에 따라, 산화물계 형광체에 비해 동등 이상의 안정성을 가지면서도 400nm를 넘어서는 여기원에서의 발광효율도 우수한 산질화물 형광체가 최근 백색 LED 분야에서 관심을 받고 있다. 그리고 산질화물 형광체는 원래 엔지니어링 세라믹스로 개발된 소재여서 습기나 발열에 의한 효율 감소와 색 변환이 적다는 강점도 있다.Accordingly, oxynitride phosphors, which have an equal or better stability than oxide-based phosphors and have excellent luminescence efficiency in an excitation source exceeding 400 nm, have recently received attention in the white LED field. The oxynitride phosphors are originally developed as engineering ceramics, and have the advantage of less efficiency and less color conversion due to moisture and heat generation.
그러나 형 또는 형 사이알론(Si-Al-O-N)을 벗어난 조성 영역에서의 산질화물 형광체의 존재는 거의 연구되거나 알려져 있지 않다.However, the presence of oxynitride phosphors in the compositional range outside the mold or intermetallic (Si-Al-O-N) is scarcely studied or known.
본 발명은 기존의 사이알론 형광체의 조성 영역을 벗어나고 산질화물로 이루어져 있어 구조 안정성이 우수하고 특히 하늘색에서 발광휘도가 우수하며, 하늘색 발광이 필요한 조명이나, 다양한 형광체의 조합을 통한 백색 발광 조명, 또는 기존 조명의 발광특성을 향상시키는 튜닝용 형광체로 적합하게 사용될 수 있는 새로운 결정구조의 형광체 및 이 형광체를 적용한 발광장치를 제공하는 것을 목적으로 한다.The present invention relates to a sialon phosphor which is excellent in structural stability because it is composed of an oxynitride and is out of the composition range of a conventional sialon phosphor and has excellent luminescence brightness especially in light blue, It is another object of the present invention to provide a phosphor having a novel crystal structure which can be suitably used as a phosphor for tuning which improves the emission characteristics of existing lights and a light emitting device using this phosphor.
상기 과제를 해결하기 위한 본 발명의 제1측면은, 일반식 (A)1-xREx(B)a(X)b (여기서, A는 Ba, Sr, Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu 및 Zn 중에서 선택된 원소를 1종 이상을 포함하고, B는 Al, Si, P, Ga, Ge, Sn 및 Bi 중에서 선택된 1종 이상을 포함하고, X는 O, N, Cl, F, C , S 및 Se 중에서 선택된 1종 이상을 포함하고, RE는 Eu를 필수원소로 하고, Mn, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm 및 Yb 중에서 선택된 원소를 1종 이상을 포함함)로 나타내는 형광체로서, 분말 X선 회절 패턴에 있어서 가장 강도가 있는 회절 피크의 상대 강도를 100%로 했을 때, 상기 X선 회절 패턴의 브래그 각도(2θ)가 15.7°~16.5°, 24.6°~25.8°, 31.1°~32.2°, 36.1°~37.1°인 범위에서 상대강도 10% 이상의 회절피크를 나타내는 상을 주상으로 포함하고, 상기 a 및 b는 4≤a≤6, 6≤b≤12인 형광체를 제공한다.(A) 1-x RE x (B) a (X) b wherein A is at least one element selected from the group consisting of Ba, Sr, Ca, Mg, Sc, Y, La B, at least one element selected from the group consisting of Al, Si, P, Ga, and Ge, and at least one element selected from Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, , Sn, and Bi, wherein X includes at least one selected from O, N, Cl, F, C, S, and Se, RE includes Eu as an essential element, at least one selected from Mn, Ce, And at least one element selected from the group consisting of Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm and Yb) And a relative intensity of 10% in the range of Bragg angles (2?) Of 15.7 to 16.5, 24.6 to 25.8, 31.1 to 32.2, and 36.1 to 37.1 of the X-ray diffraction pattern, Or more of the diffraction peak, and a and b each represent a phosphor with 4? A? 6 and 6? B? 12 The.
또한, 상기 형광체의 모체는 사방정계(orthorombic) 결정구조일 수 있다.The matrix of the phosphor may be an orthoromic crystal structure.
또한, 상기 형광체의 모체의 격자상수는 a = 9.48461Å, b = 13.47194Å, c = 5.77323Å 이며, 상기 격자상수는 10%의 변동이 가능하다.In addition, the lattice constants of the matrix of the phosphor are a = 9.48461 Å, b = 13.47194 Å, c = 5.77323 Å, and the lattice constant can be varied by 10%.
또한, 상기 형광체에 있어서, 상기 A는 Sr 또는 Ba을 포함할 수 있다.Further, in the above-mentioned phosphor, A may include Sr or Ba.
또한, 상기 형광체에 있어서, 상기 A가 Sr 또는 Ba을 포함할 경우, 상기 Sr Ba은 그 일부가 Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu 및 Zn 중에서 선택된 1종 이상으로 몰비율로 20% 이하로 대체될 수 있다.In the above-mentioned phosphor, when the A contains Sr or Ba, the Sr Ba partially contains Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy , Ho, Er, Tm, Yb, Lu and Zn in a mole ratio of 20% or less.
또한, 상기 형광체에 있어서, 상기 X는 O 및 N을 포함할 수 있다.Further, in the above-mentioned phosphor, X may include O and N. [
또한, 상기 형광체에 있어서, 상기 X가 O 및 N을 포함할 경우, 상기 O 및 N은 Cl, F, C , S 및 Se 중에서 선택된 1종 이상으로 대체될 수 있다.In the above-mentioned phosphor, when X includes O and N, the O and N may be replaced by at least one selected from Cl, F, C, S and Se.
상기 형광체는 300~400nm 여기광에 대하여 450~500nm의 발광 피크 파장을 나타낼 수 있다.The phosphor may exhibit an emission peak wavelength of 450 to 500 nm with respect to excitation light of 300 to 400 nm.
상기 형광체의 모체에 함유된 Sr 또는 Ba과 (Al,Si) 및 (O,N)의 비율((Sr 또는 Ba):(Al, Si):(O,N))을 x:y:z라 할 때, 상기 비율은 바람직하게 1:5:8 일 수 있다.The ratio (Sr or Ba): (Al, Si): (O, N)) of Sr or Ba and (Al, Si) and (O, N) contained in the matrix of the phosphor is set to x: y: , The ratio may preferably be 1: 5: 8.
본 발명의 과제를 해결하기 위한 본 발명의 제2측면은, 여기광을 방출하는 발광소자 및 상기 여기광을 흡수하여 가시광을 방출하는 파장변환부를 포함하며, 상기 파장변환부는 상기한 형광체를 포함하는 발광장치를 제공한다.According to a second aspect of the present invention, there is provided a light emitting device comprising: a light emitting device that emits excitation light; and a wavelength converter that absorbs the excitation light to emit visible light, wherein the wavelength converter includes: A light emitting device is provided.
상기 발광장치에 있어서, 상기 발광소자는 자외선 발광다이오드일 수 있다.In the light emitting device, the light emitting device may be an ultraviolet light emitting diode.
본 발명과 같이 Ba, Sr, Al, Si, O, N을 기반으로 하는 새로운 결정구조를 갖는 형광체 조성물은 이제까지 보고된 바가 없으며, 이 조성물은 Eu 도핑시 하늘색 형광체로 사용될 수 있으며, 광 효율이 우수하여 LED용 형광체로 적합하게 사용될 수 있다.As described above, a phosphor composition having a new crystal structure based on Ba, Sr, Al, Si, O, or N has not been reported so far, and the composition can be used as a blue phosphor when Eu doping is used. So that it can be suitably used as a phosphor for LED.
또한, 본 발명의 형광체는 구성 원소의 몰비 조절을 통해, Ba 또는 Sr 자리에 산화수가 같는 물질을 치환하였을 시 발광 파장의 변화가 가능하며, 발광 효율 또한 변화시킬 수 있고, Eu 도핑 농도에 따라서도 발광 파장 변화 및 광 효율 변화가 가능하여, 튜닝용 형광체로도 유용하게 사용될 수 있다.In addition, in the phosphor of the present invention, by changing the molar ratio of constituent elements, it is possible to change the emission wavelength when a substance having the same oxidation number is substituted for Ba or Sr sites, and also to change the luminous efficiency, It is possible to change the light emission wavelength and the light efficiency, and thus can be usefully used as a phosphor for tuning.
도 1은 본 발명의 실시예 1 및 2에 따라 제조된 형광체의 선 회절 패턴의 브래그 각도(θ)가 15.7°~16.5°, 24.6°~25.8°, 31.1°~32.2°, 36.1°~37.1°인 부분을 표시한 것이다.
도 2는 본 발명의 실시예 1 및 2에 따라 제조된 형광체의 PL 특성을 나타낸 것이다.
도 3은 본 발명의 실시예 3~8에 따라 제조된 형광체의 선 회절 패턴을 표시한 것이다.
도 4은 본 발명의 실시예 9~14에 따라 제조된 형광체의 선 회절 패턴을 표시한 것이다.
도 5은 본 발명의 실시예 3~8에 따라 제조된 형광체의 PL 특성을 나타낸 것이다.
도 6은 본 발명의 실시예 9~14에 따라 제조된 형광체의 PL 특성을 나타낸 것이다.FIG. 1 is a graph showing the results of a Bragg angle (?) Of a ray diffraction pattern of a phosphor prepared according to Examples 1 and 2 of the present invention of 15.7 ° to 16.5 °, 24.6 ° to 25.8 °, 31.1 ° to 32.2 °, 36.1 ° to 37.1 ° Quot ;.
2 shows the PL characteristics of the phosphors prepared according to Examples 1 and 2 of the present invention.
Fig. 3 shows the ray diffraction patterns of the phosphors prepared according to Examples 3 to 8 of the present invention.
Fig. 4 shows a ray diffraction pattern of a phosphor prepared according to Examples 9 to 14 of the present invention.
5 shows the PL characteristics of the phosphors prepared according to Examples 3 to 8 of the present invention.
6 shows the PL characteristics of the phosphors prepared according to Examples 9 to 14 of the present invention.
본 발명자들은 사이알론 형광체와 같이 산질화물로 이루어져 있어 구조적으로 안정하여 내구성이 우수하며, 특정한 컬러를 가져 특수 조명이나 백색 LED의 튜닝용으로 사용할 수 있는 새로운 형광체 조성물을 연구한 결과, Ba나 Sr과 같은 알카리토금속과 Al 및 Si로 이루어진 특정 조성의 산질화물이 종래에 알려져 있지 않은 무기 결정구조를 형성하며, 이 무기 결정구조를 모체로 한 형광체가 높은 휘도로 하늘색 발광을 할 수 있음을 밝혀내고 본 발명에 이르게 되었다.The present inventors have studied a novel phosphor composition which is structurally stable and has excellent durability because it is composed of an oxynitride such as a sialon phosphor and has a specific color and can be used for special illumination or tuning of a white LED. As a result, It has been found out that the same alkaline earth metal, oxynitride of a specific composition of Al and Si forms an inorganic crystal structure not known in the past, and that the phosphor having the inorganic crystal structure as a matrix can emit blue light with high luminance. It came to the invention.
이하 본 발명을 실시하기 위한 구체적인 내용에 대해 상세하게 설명한다.Hereinafter, the present invention will be described in detail.
형광체Phosphor
본 발명에 따른 형광체는 일반식 (A)1-xREx(B)a(X)b (여기서, A는 Ba, Sr, Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu 및 Zn 중에서 선택된 원소를 1종 또는 이상 포함하고, B는 Al, Si, P, Ga, Ge, Sn 및 Bi 중에서 선택된 1종 또는 이상 포함하고, X는 O, N, Cl, F, C , S 및 Se 중에서 선택된 1종 또는 이상 포함하고, RE는 Eu를 필수원소로 하고, Mn, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm 및 Yb 중에서 선택된 원소를 1종 이상 포함함)로 나타내는 형광체로서, 분말 X선 회절 패턴에 있어서 가장 강도가 있는 회절 피크의 상대 강도를 100%로 했을 때, 상기 X선 회절 패턴의 브래그 각도(2θ)가 15.7°~16.5°, 24.6°~25.8°, 31.1°~32.2°, 36.1°~37.1°인 범위에서 상대강도 10% 이상의 회절피크를 나타내는 상을 주상으로 포함하고, 상기 a 및 b는 4≤a≤6, 6≤b≤12 인 형광체를 제공한다.(A) 1-x RE x (B) a (X) b wherein A is at least one element selected from the group consisting of Ba, Sr, Ca, Mg, Sc, And one or more elements selected from the group consisting of Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Zn; B is at least one element selected from Al, Si, P, Ga, Ge, Ce, Pr, Nd, Sm, Gd, Cr, and Sb, wherein X is at least one element selected from the group consisting of O, N, Cl, F, Tb, Dy, Ho, Er, Tm and Yb), wherein the relative intensity of the diffraction peak having the highest intensity in the powder X-ray diffraction pattern is 100% An image showing a diffraction peak having a relative intensity of 10% or more in the range of Bragg angles (2?) Of 15.7 to 16.5, 24.6 to 25.8, 31.1 to 32.2, and 36.1 to 37.1 of the X- Wherein a and b are 4? A? 6 and 6? B? 12, respectively.
이러한 형광체는 300~400nm 파장의 자외선 여기광에 대하여 450~500nm의 발광 피크 파장을 나타낼 수 있다.Such a phosphor may exhibit an emission peak wavelength of 450 to 500 nm with respect to ultraviolet excitation light having a wavelength of 300 to 400 nm.
또한, 상기 형광체의 모체는 사방정계(orthorombic) 결정구조를 가지는 것을 특징으로 한다.Further, the matrix of the phosphor has an orthoromic crystal structure.
또한, 상기 형광체의 모체의 격자상수는 a = 9.48461Å, b = 13.47194Å, c = 5.77323Å 이며, 상기 격자상수는 10% 이하로, 바람직하게는 5% 이하의 변할 수 있으며, 이 경우에도 본 발명에 따른 형광체의 특성을 나타낼 수 있다.Further, the lattice constants of the matrix of the phosphor are a = 9.48461 Å, b = 13.47194 Å, c = 5.77323 Å, and the lattice constant can be changed to 10% or less, preferably 5% or less. The characteristics of the phosphor according to the invention can be shown.
또한, 상기 형광체의 모체에 있어서, 상기 A가 Sr 또는 Ba을 포함할 경우, 상기 Sr 또는 Ba은 그 일부가 Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu 및 Zn 중에서 선택된 1종 이상으로 대체되더라도 동일한 결정구조를 가지며, 발광중심 금속원소로 Eu 등을 고용시킬 경우, 자외선 여기원으로 조사되었을 때 하늘색 발광을 할 수 있다. 이때 Sr 또는 Ba를 대체하는 타 원소들이 20%를 초과하여 포함될 경우 본 발명에 따른 결정구조를 갖는 상(phase)이 형성되지 않을 수 있으므로 20% 이하로 대체되는 것이 바람직하고, 10% 이하로 대체되는 것이 보다 바람직하다.In the matrix of the phosphor, when the A contains Sr or Ba, the Sr or Ba may be at least one selected from the group consisting of Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb, Lu, and Zn. When Eu or the like is incorporated into the luminescent center metal element, can do. At this time, when the elements containing Sr or Ba are included in an amount of more than 20%, phases having a crystal structure according to the present invention may not be formed. Therefore, they are preferably replaced by 20% or less, .
또한, 상기 형광체의 모체에 있어서 원료에 SrF2, SrCl2, AlF3, NHCl,NHF, C등의 강화제를 넣음으로써 음이온 자리에 Cl, F, C 등이 치환될 수 있다.Further, by adding a strengthening agent such as SrF 2 , SrCl 2 , AlF 3 , NHCl, NHF, C or the like to the raw material in the matrix of the phosphor, Cl, F, C and the like can be substituted in the anion site.
또한, 상기 형광체의 모체에 있어서, 상기 모체에 함유된 Sr 또는 Ba과 (Al, Si) 및 (O,N)의 비율((Sr 또는 Ba):(Al, Si):(O,N))을 x:y:z라 할 때, 상기 비율은 바람직하게 1:5:8 일 수 있다.(Sr or Ba): (Al, Si): (O, N)) of Sr or Ba and (Al, Si) and (O, N) contained in the matrix of the phosphor, Is x: y: z, the ratio may preferably be 1: 5: 8.
또한, 본 발명에 따른 형광체에 있어서, 상기 부활제(RE)의 고용량(x)은 몰비로 0.001보다 작을 경우 발광 원소의 부족으로 휘도가 충분하지 않고, 0.2를 초과할 경우 이른바 농도 소광(消光)의 효과로 인해 오히려 휘도가 감소하므로, 0.001~0.2의 범위에서 높은 휘도를 얻을 수 있어 바람직하고, 몰비로 0.04~0.08 범위로 고용되는 것이 보다 바람직하다. 또한, 부활제로는 유로퓸(Eu)이 가장 바람직하며, 유로퓸(Eu)에 Mn, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm 및 Yb 중에서 선택된 1종 이상의 원소를 코도핑(co-doping)할 수 있다.In the phosphor according to the present invention, when the molar ratio (x) of the activator (RE) is less than 0.001, the brightness is insufficient due to the shortage of luminescent elements. , It is preferable that the luminance is in the range of 0.001 to 0.2 and preferably in the range of 0.04 to 0.08 in terms of the molar ratio. As the activating agent, europium (Eu) is the most preferable and at least one element selected from Mn, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm and Yb is added to the europium It can be co-doped.
또한, 본 발명에 따른 조성의 형광체는 단상(single phase)으로 이루어지는 것이 이상적이지만, 제조 과정에서 소량의 불가피한 비정질상이나 사방정계(orthorombic)가 아닌 기타 결정상이 포함될 수 있으며, 이러한 비정질상이나 기타 결정상을 포함하는 혼합물이라도 특성에 영향이 없는 한 일부 포함될 수 있다.The phosphor of the composition according to the present invention is ideally composed of a single phase. However, a small amount of unavoidable amorphous phase or other crystal phase other than orthorombic may be included in the production process, and such an amorphous phase or other crystal phase May be included as long as they do not affect the properties.
또한, 본 발명에 따른 형광체의 평균 입도는 1㎛~20㎛의 범위가 바람직한데, 평균입도가 1㎛보다 작으면 산란에 의한 광 흡수율이 저하되고, LED를 밀봉하는 수지로의 균일한 분산이 용이하지 않을 수도 있고, 평균 입도가 20㎛를 초과하면 발광 강도 및 색조의 불균일이 발생할 경우가 있기 때문이다.
The average particle size of the phosphor according to the present invention is preferably in the range of 1 탆 to 20 탆. If the average particle size is smaller than 1 탆, the light absorptance due to scattering decreases and the uniform dispersion of the resin sealing the LED If the average particle size exceeds 20 mu m, the light emission intensity and color tone may be uneven.
형광체의 제조방법Method of manufacturing phosphor
이하, 본 발명에 따른 형광체의 제조방법을 상세하게 설명한다.Hereinafter, a method for producing a phosphor according to the present invention will be described in detail.
형광체 제조 원료로는 주요 성분인 Si, Sr, Ba, Al, Eu의 경우, 규소질화물(Si3N4), 탄산스트론튬 (SrCO3), 탄산바륨(BaCO3), 산화알루미늄(Al2O3) 및 유로퓸산화물(Eu2O3) 분말을 사용하였다.(Si 3 N 4 ), strontium carbonate (SrCO 3 ), barium carbonate (BaCO 3 ), aluminum oxide (Al 2 O 3 ), and the like are used as raw materials for producing phosphors, Si, Sr, Ba, ) And europium oxide (Eu 2 O 3 ) powder were used.
상기 원료물질들은 소정의 조성이 되도록 SrCO3, Al2O3, BaCO3, α-Si3N4, Eu2O3을 칭량하여 혼합하였는데, 이때 샘플당 혼합물의 양은 1g이 되도록 하였다. 이상과 같은 원료물질의 혼합작업은 대기 분위기에서 수작업으로 10분 동안 혼합하였다.SrCO 3 , Al 2 O 3 , BaCO 3 , α-Si 3 N 4 , and Eu 2 O 3 were weighed and mixed to obtain a predetermined composition. The amount of the mixture per sample was 1 g. The mixing of the raw materials as described above was performed by hand for 10 minutes in the atmosphere.
이와 같이 얻어진 혼합물 샘플들을 대기압 이상 20기압 이하의 질소 가스를 주성분으로 하여 H2가스가 0~25% 이루어지는 질소 가스 분위기에서 수행하는데, 이와 같이 질소 가스 분위기에서 소성을 하게 되면 고온 소성 중에 합성되는 질화물의 분해를 방지 또는 억제할 수 있고, 생성되는 질화물의 조성 편차를 줄일 수 있어 성능이 우수한 형광체 조성물을 제조할 수 있게 된다.The thus obtained mixture samples are carried out in a nitrogen gas atmosphere containing 0 to 25% of H 2 gas as a main component and a nitrogen gas having a pressure of not less than 20 atm and not more than 20 atm. When the calcination is performed in a nitrogen gas atmosphere, It is possible to prevent or suppress the decomposition of the nitride, and to reduce the compositional deviation of the nitride to be produced, thereby making it possible to produce a phosphor composition excellent in performance.
한편, 질소가스를 주성분으로 한다는 것은, 전체 가스대비 질소 가스가 75% 이상으로 포함된 것을 의미한다. 또한, 소성온도는 1500℃가~1700℃가 바람직하며 고품질의 형광체를 얻기 위해서는 1550℃가 이상이 보다 바람직하다. 또한, 소성시간은 30분~100시간의 범위 내로 할 수 있는데, 품질과 생산성 등을 고려할 때 2시간~24시간이 바람직하다. 본 실시 형태에서는 상압 초고순도 질소(99.999%) 가스 분위기 하에서 1600℃가의 소성 온도로 8시간 동안 소성을 실시한 후 파쇄하여 형광체를 제조하였다.On the other hand, when nitrogen gas is used as the main component, it means that the nitrogen gas is contained in an amount of 75% or more relative to the total gas. The baking temperature is preferably 1500 ° C to 1700 ° C, and more preferably 1550 ° C or more to obtain a high-quality phosphor. The firing time may be in the range of 30 minutes to 100 hours, preferably 2 hours to 24 hours, considering the quality and productivity. In this embodiment, firing was performed at a firing temperature of 1600 DEG C for 8 hours in an atmospheric ultra-high purity nitrogen (99.999%) gas atmosphere, followed by pulverization, thereby preparing phosphors.
이하, 보다 구체적인 실시예를 참조하여 본 발명의 산질화물계 형광체를 상세하게 설명한다.
Hereinafter, the oxynitride-based fluorescent material of the present invention will be described in detail with reference to more specific examples.
[실시예 1][Example 1]
실시예 1의 형광체 조성물의 원료분말은, BaCO3 0.3831g, Al2O3 0.2483g, α-Si3N4 0.3392g, Eu2O3 0.0294g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.0.3831 g of BaCO 3, 0.2483 g of Al 2 O 3, 0.3392 g of? -Si 3 N 4 and 0.0294 g of Eu 2 O 3 were weighed out respectively as raw material powders of the phosphor composition of Example 1 and then pulverized 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 2][Example 2]
실시예 2의 형광체 조성물의 원료분말은, SrO3 0.3199g, Al2O3 0.2392g, α-Si3N4 0.4127g, Eu2O3 0.0282g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 2 was obtained by weighing 0.3199 g of SrO 3, 0.2392 g of Al 2 O 3, 0.4127 g of α-Si 3 N 4 and 0.0282 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 3][Example 3]
실시예 3의 형광체 조성물의 원료분말은, BaCO3 0.3802g, Al2O3 0.2498g, α-Si3N4 0.3416g, Eu2O3 0.0284g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 3 was obtained by weighing 0.3802 g of BaCO 3, 0.2498 g of Al 2 O 3, 0.3416 g of α-Si 3 N 4 and 0.0284 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 4][Example 4]
실시예 4의 형광체 조성물의 원료분말은, BaCO3 0.3909g, Al2O3 0.2371g, α-Si3N4 0.3416g, Eu2O3 0.0387g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 4 was obtained by weighing 0.3909 g of BaCO 3, 0.2371 g of Al 2 O 3, 0.3416 g of α-Si 3 N 4 and 0.0387 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 5][Example 5]
실시예 5의 형광체 조성물의 원료분말은, BaCO3 0.3843g, Al2O3 0.2475g, α-Si3N4 0.3375g, Eu2O3 0.0307g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 5 was obtained by weighing 0.3843 g of BaCO 3, 0.2475 g of Al 2 O 3, 0.3375 g of α-Si 3 N 4 and 0.0307 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 6][Example 6]
실시예 6의 형광체 조성물의 원료분말은, BaCO3 0.3485g, Al2O3 0.1825g, α-Si3N4 0.4444g, Eu2O3 0.0245g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.0.3485 g of BaCO 3, 0.1825 g of Al 2 O 3, 0.4444 g of? -Si 3 N 4 and 0.0245 g of Eu 2 O 3 were weighed out respectively as raw material powders of the phosphor composition of Example 6, 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 7][Example 7]
실시예 7의 형광체 조성물의 원료분말은, BaCO3 0.3696g, Al2O3 0.2532g, α-Si3N4 0.3461g, Eu2O3 0.0311g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.0.3696 g of BaCO 3, 0.2532 g of Al 2 O 3, 0.3461 g of? -Si 3 N 4, and 0.0311 g of Eu 2 O 3 were weighed out, respectively, and the resultant powders of the phosphor compositions of Example 7 were used 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 8][Example 8]
실시예 8의 형광체 조성물의 원료분말은, BaCO3 0.3695g, Al2O3 0.2479g, α-Si3N4 0.3459g, Eu2O3 0.0366g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 8 was obtained by weighing 0.3695 g of BaCO 3, 0.2479 g of Al 2 O 3, 0.3459 g of α-Si 3 N 4 and 0.0366 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 9][Example 9]
실시예 9의 형광체 조성물의 원료분말은, SrO3 0.3214g, Al2O3 0.2365g, α-Si3N4 0.4137g, Eu2O3 0.0.284g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.0.3214 g of SrO 3, 0.2365 g of Al 2 O 3, 0.4137 g of? -Si 3 N 4 and 0.0284 g of Eu 2 O 3 were weighed out, respectively, in the raw material powder of the phosphor composition of Example 9, 1 g of a raw material powder mixture was obtained. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 10][Example 10]
실시예 10의 형광체 조성물의 원료분말은, SrO3 0.3221g, Al2O3 0.2324g, α-Si3N4 0.4176g, Eu2O3 0.0279g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 10 was obtained by weighing 0.3221 g of SrO 3, 0.2324 g of Al 2 O 3, 0.4176 g of α-Si 3 N 4 and 0.0279 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 11][Example 11]
실시예 11의 형광체 조성물의 원료분말은, SrO3 0.3360g, Al2O3 0.2277g, α-Si3N4 0.4074g, Eu2O3 0.0290g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.0.3360 g of SrO 3, 0.2277 g of Al 2 O 3, 0.4074 g of? -Si 3 N 4 and 0.0290 g of Eu 2 O 3 were weighed out respectively as raw material powders of the phosphor composition of Example 11, 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 12][Example 12]
실시예 12의 형광체 조성물의 원료분말은, SrO3 0.3354g, Al2O3 0.2313g, α-Si3N4 0.4035g, Eu2O3 0.0298g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 12 was obtained by weighing 0.3354 g of SrO 3, 0.2313 g of Al 2 O 3, 0.4035 g of α-Si 3 N 4 and 0.0298 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 13][Example 13]
실시예 13의 형광체 조성물의 원료분말은, SrO3 0.3284g, Al2O3 0.2370g, α-Si3N4 0.4094g, Eu2O3 0.0253g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.0.3284 g of SrO 3, 0.2370 g of Al 2 O 3, 0.4094 g of? -Si 3 N 4 and 0.0253 g of Eu 2 O 3 were weighed out respectively as raw material powders of the phosphor composition of Example 13, 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
[실시예 14][Example 14]
실시예 14의 형광체 조성물의 원료분말은, SrO3 0.2997g, Al2O3 0.2486g, α-Si3N4 0.4252g, Eu2O3 0.0265g을 각각 칭량한 후, 대기 분위기에서 유발을 사용하여 수작업으로 혼합하는 방식으로 1g의 원료 분말 혼합물을 얻었다. 이와 같이 혼합된 원료분말 혼합물 1g을 도가니에 충전하고, 소성로의 내부에 질소 가스를 분당 500cc 흘려주어 1600℃에서 8시간 동안 가열하는 소성처리를 한 후 분쇄함으로써, 형광체 조성물을 얻었다. 이 형광체 조성물을 390nm 광원으로 여기시켰을 때 하늘색 발광이 되는 것으로 확인되었다.The raw material powder of the phosphor composition of Example 14 was obtained by weighing 0.2997 g of SrO 3, 0.2486 g of Al 2 O 3, 0.4252 g of α-Si 3 N 4 and 0.0265 g of Eu 2 O 3 , 1 g of raw material powder mixture was obtained by mixing by hand. 1 g of the raw material powder mixture thus mixed was charged into a crucible, and nitrogen gas was flowed into the calcining furnace at a rate of 500 cc / minute, followed by calcination treatment at 1600 占 폚 for 8 hours, followed by pulverization to obtain a phosphor composition. When this phosphor composition was excited by a light source at 390 nm, it was confirmed to emit blue light.
(nm)Luminescence peak wavelength
(nm)
이상과 같이 제조된 형광체 조성물들의 결정구조를 XRD를 사용하여 분석(실시예 1 및 2는 synchrotron XRD 분석결과이고, 실시예 3~14는 XRD 분석결과임)하였으며, 도 1, 3, 4는 실시예 1~14에 따라 제조한 형광체 분말의 X선 회절 결과를 나타낸 것이다.The crystal structures of the phosphor compositions prepared as described above were analyzed using XRD (Examples 1 and 2 are results of XRD analysis of synchrotron, and Examples 3 to 14 are XRD analysis results). FIGS. 1, 3 and 4 X-ray diffraction results of the phosphor powders prepared according to Examples 1 to 14 are shown.
도 1에 나타난 바와 같이, 본 발명의 실시예 1 및 2에 따른 형광체는, 분말 X선 회절 패턴에 있어서 가장 강도가 있는 회절 피크의 상대 강도를 100%로 했을 때, 상기 X선 회절 패턴의 브래그 각도(2θ)가 15.7°~16.5°, 24.6°~25.8°, 31.1°~32.2°, 36.1°~37.1°인 범위에서 상대강도 10% 이상의 회절피크를 나타낸다.As shown in Fig. 1, the phosphors according to Examples 1 and 2 of the present invention are characterized in that when the relative intensity of the diffraction peak having the highest intensity in the powder X-ray diffraction pattern is taken as 100% Shows a diffraction peak of 10% or more in relative intensity in the range of angles (2?) Of 15.7 ° to 16.5 °, 24.6 ° to 25.8 °, 31.1 ° to 32.2 °, and 36.1 ° to 37.1 °.
그런데, 기존의 Si, Al, O, N을 주성분으로 하는 형광체에서 본 발명의 실시예 1 및 2와 같은 결정구조를 나타내는 형광체는 알려진 바가 없다. 즉, 본 발명의 실시예 1 및 2에 따른 형광체는 종래에 알려져 있지 않은 새로운 결정구조를 갖는 것이다.However, there are no known phosphors having crystal structures similar to those of Examples 1 and 2 of the present invention in conventional phosphors containing Si, Al, O, and N as main components. That is, the phosphors according to Examples 1 and 2 of the present invention have a novel crystal structure not known in the art.
도 2, 5, 6은 본 발명의 실시예 1~14에 따라 제조된 형광체의 PL 특성을 나타낸 것이다.FIGS. 2, 5 and 6 show PL characteristics of the phosphors prepared according to Examples 1 to 14 of the present invention.
도 2에 나타난 바와 같이, 본 발명의 실시예 1에 따라 제조된 형광체는 390nm 여기원으로 조사되었을 때, 발광피크파장이 475nm인 하늘색 발광을 하였다. 또한 본 발명의 실시예 2에 따라 제조된 형광체는 390nm 여기원으로 조사되었을 때, 발광피크파장이 485nm인 하늘색 발광을 하였다.
As shown in FIG. 2, when the phosphor prepared according to Example 1 of the present invention was irradiated with a excitation source of 390 nm, it emits blue light having an emission peak wavelength of 475 nm. When the phosphor prepared according to Example 2 of the present invention was irradiated with a excitation source having a wavelength of 390 nm, the phosphor emits blue light having a peak emission wavelength of 485 nm.
Claims (11)
상기 형광체의 모체는 사방정계(orthorombic) 결정구조를 갖는 것을 특징으로 하는 형광체.The method according to claim 1,
Wherein the matrix of the phosphor has an orthoromic crystal structure.
상기 형광체의 모체의 격자상수는 a = 9.48461Å, b = 13.47194Å, c = 5.77323Å 이며, 상기 격자상수는 10% 이내의 변동이 가능한 것을 특징으로 하는 형광체.3. The method of claim 2,
Wherein the lattice constants of the matrix of the phosphor are a = 9.48461 Å, b = 13.47194 Å and c = 5.77323 Å, and the lattice constant is variable within 10%.
상기 A는 Sr 또는 Ba를 포함하는 것을 특징으로 하는 형광체.The method according to claim 1,
Wherein A comprises Sr or Ba.
상기 Sr 또는 Ba는 그 일부가 Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu 및 Zn 중에서 선택된 1종 이상으로 20mol% 이하로 대체되는 것을 특징으로 하는 형광체.5. The method of claim 4,
The Sr or Ba is at least one selected from Ca, Mg, Sc, Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, To 20 mol% or less.
상기 X는 O 및 N을 포함하는 것을 특징으로 하는 형광체.The method according to claim 1,
Wherein X represents O and N. < RTI ID = 0.0 > 11. < / RTI >
상기 O 또는 N은, Cl, F, C, S 및 Se 중에서 선택된 1종 이상으로 대체되는 것을 특징으로 하는 형광체.The method according to claim 6,
Wherein the O or N is replaced with at least one selected from Cl, F, C, S and Se.
상기 형광체는 300~400nm 여기광에 대하여 450~500nm의 발광 피크 파장을 나타내는 것을 특징으로 하는 형광체.The method according to claim 1,
Wherein the phosphor has an emission peak wavelength of 450 to 500 nm with respect to 300 to 400 nm excitation light.
상기 형광체에 함유된 Sr 또는 Ba과 (Al,Si) 및 (O,N)의 비율(Sr 또는 Ba):(AlSi):(O,N))이 1:5:8인 것을 특징으로 하는 형광체.The method according to claim 1,
Wherein a ratio of Sr or Ba and (Al, Si) and (O, N) (Sr or Ba) :( AlSi) :( O, N) contained in the phosphor is 1: 5: .
상기 여기광을 흡수하여 가시광을 방출하는 파장변환부;를 포함하며,
상기 파장변환부는 제1항 내지 제9항 중 어느 한 항에 기재된 형광체를 포함하는 발광장치.A light emitting element that emits excitation light; And
And a wavelength converter for absorbing the excitation light to emit visible light,
Wherein the wavelength conversion section comprises the phosphor according to any one of claims 1 to 9.
상기 발광소자는 자외선 발광다이오드인 것을 특징으로 하는 발광장치.
11. The method of claim 10,
Wherein the light emitting element is an ultraviolet light emitting diode.
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