CN1596478A - 发光材料,可特别用于led用途 - Google Patents
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- 239000000463 material Substances 0.000 title claims abstract description 24
- 229910052788 barium Inorganic materials 0.000 claims abstract description 8
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 6
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract 2
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 23
- 230000005855 radiation Effects 0.000 claims description 15
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 150000002739 metals Chemical class 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical group [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims 1
- 229910015811 MSi2 Inorganic materials 0.000 claims 1
- 230000005284 excitation Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 150000001768 cations Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000295 emission spectrum Methods 0.000 description 4
- 238000000695 excitation spectrum Methods 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 3
- 239000000049 pigment Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 229910016064 BaSi2 Inorganic materials 0.000 description 2
- 229910004706 CaSi2 Inorganic materials 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052681 coesite Inorganic materials 0.000 description 2
- 229910052906 cristobalite Inorganic materials 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052682 stishovite Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910052905 tridymite Inorganic materials 0.000 description 2
- 229910002020 Aerosil® OX 50 Inorganic materials 0.000 description 1
- 229910016010 BaAl2 Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910002795 Si–Al–O–N Inorganic materials 0.000 description 1
- 229910003669 SrAl2O4 Inorganic materials 0.000 description 1
- 229910004412 SrSi2 Inorganic materials 0.000 description 1
- 239000005084 Strontium aluminate Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 229940125898 compound 5 Drugs 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- -1 nitride silicate Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229910000018 strontium carbonate Inorganic materials 0.000 description 1
- LEDMRZGFZIAGGB-UHFFFAOYSA-L strontium carbonate Chemical compound [Sr+2].[O-]C([O-])=O LEDMRZGFZIAGGB-UHFFFAOYSA-L 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910003158 γ-Al2O3 Inorganic materials 0.000 description 1
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- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
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- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
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Abstract
公开了由Eu掺杂的、一般组成为MSi2O2N2的氧氮化物主体晶格组成的紫外-蓝光激发的绿光发光材料,其中M是选自Ca、Sr、Ba的至少一种碱土金属。
Description
技术领域
本发明涉及发光材料,其可在光谱区的紫外-蓝色部分受激发光,更具体而言,但不只限于,涉及光源用磷光体,特别是9用于发光二极管(LED)的磷光体。所述磷光体属于稀土活化的硅氧氮化物类。
背景技术
迄今为止,通过将发蓝光的二极管与发黄光的磷光体组合实现了白光LEDs。这种组合的色泽稳定性差,但是,可以通过采用红-绿-蓝体系(RGB)将其显著改进。这种体系采用例如红和蓝发射体,与发射绿光的铝酸盐磷光体如SrAl2O4:Eu或BaAl2O4:Eu组合起来,可能要向Eu中加入Mn,其发射最大值在约520nm处,参见US-A 6 278 135。然而,这些铝酸盐的激发和发射谱带的位置不是最佳的。必须用330-400nm的短波紫外线来激发它们。
另一方面,已知一些从MSiON类衍生而来的磷光体,参见例如VanKrevel的“On new rare-earth doped M-Si-Al-O-N materials”,TU Eindhoven 2000,ISBN 90-386-2711-4,Chapter 6。它们掺杂了Tb。在365nm或254nm激发实现了发射。
发明内容
本发明的一个目的是提供一种新型的发光材料。另一个目的是提供一种具有精细调制的发射绿光的磷光体,其可以由紫外/蓝色辐射高效率地激发。另一个目的是提供一种磷光体,其用于具有至少一个LED作为光源的照明装置中,该LED发出380-470nm的一级辐射,通过暴露于该LED的一级辐射的此类磷光体将该辐射部分或全部地转变为较长波长的辐射。另一个目的是提供一种照明装置,该装置发出白光,而且特别是具有高色泽稳定性。另一个目的是提供一种高效率的照明装置如LED装置,其在380-470nm内具有良好的吸收并且易于制造。
这些目的通过权利要求1和8表明的特征而分别获得了实现。在从属权利要求中提供了特别有优势的构型。
至少借助于源自Eu-或Eu、Mn-共活化的硅氧烷氧氮化物类材料实现了所述转变。更具体而言,通过用Eu离子掺杂MSi2O2N2(M=Ca,Sr,Ba)主体晶格产生了一种新型磷光体材料。得到的磷光体表现出高度的化学和热稳定性。
所有相关性能的更大范围的精细调制可以通过用(AlO)部分地替换(SiN)来实现,特定的百分比用x表示,最高为40%,得到了由MSi2-xAlxO2+xN2-x表示的通式组合物,优选范围是1-15%(x=0.01-0.15)。
对于可在蓝光辐射下被高效率地激发的绿光发射材料而言,金属M优选是Ca或至少主要是Ca,添加少量的Ba和/或Sr。氮的引入提高了共价键合的程度和配位场的***。结果是与氧化物晶格相比,这导致了激发和发射谱带向较长波长发生位移。得到的磷光体表现出高度的化学和热稳定性。
所有相关性能的更大范围的精细调制可以通过采用阳离子M来实现,通过组合几种所述的M金属并包含Zn作为部分阳离子M,优选高达5-40mol%的M,和/或用Ge至少部分替换Si来获得阳离子M。掺杂到阳离子M中的Eu的量为M的0.1-25%的部分替换,优选2-15%的M。此外,在假设Eu量给定的情况下,进一步掺杂Mn可以精细调制相关性能,优选为所述给定Eu掺杂量的至多50%。
由于这些材料有低能量激发谱带而能将紫外-蓝光辐射转变为绿光,可以将它们用于例如白光源(例如灯)中,特别是基于主要发蓝光的LEDs(一般是基于在约430-470nm发射的GaN或InGaN)与红光发射磷光体组合的光源。合用的红光发射磷光体是掺杂了Eu的氮化硅材料,如M2Si5N8(M=Ca,Sr,Ba),参见例如WO 01/40403。也可以应用于彩色光源。
附图简述
在下文中,参考多个示范性实施方案更详细地说明本发明。在附图中:
图1显示了一个半导体组件(LED),其用作白光光源,其含有铸模树脂(图1a)和不含有铸模树脂(图1b);
图2显示了具有本发明磷光体的照明装置;
图3-5显示了本发明磷光体的发射光谱和反射光谱。
具体实施方式
以举例的方式,描述了与用于WO 01/40403中的相似结构,该结构与InGaN晶片一起用于白光LED中。此类白光光源的结构具体地示于图1a中。该光源基于最大发射波长为400nm的InGaN型半导体组件(晶片1),具有第一和第二电连接2、3,其包埋在不透明基底罩8的凹穴9区域中。其中一个电连接3经由连接导线4与晶片1相连。凹穴具有一个用作晶片1的蓝光一级辐射反射器的壁7。凹穴9填充了电器内封胶5,其含有作为主要成分(优选至少80重量%)的聚硅氧烷铸模树脂(或环氧铸模树脂),还含有磷光体颜料6(优选少于15重量%)。还特别含有少量的甲基醚和高分散硅胶。磷光体颜料是发出蓝、绿和红光的三种颜料与本发明的绿色磷光体的混合物。
图1b显示了具有半导体组件10的光源的实施方案,其中,向白光的转化是通过直接施用在单独的晶片上的磷光体转化层16实现的。在基底11的顶部有接触层12、镜层13、LED晶片14、滤光片15和磷光体层16,该磷光体层受到LED的一级辐射的激发并将其转化为可见的长波辐射。该结构单元被塑料透镜17所包围。只显示了两个欧姆接触中的上部接触18。LED的一级紫外辐射在400nm附近,二级辐射由采用BaSi2O2N2:Eu的本发明第一磷光体(在500nm附近发射)来发射并由采用氮化物硅氧酸盐的第二磷光体(发射出橙红色光)来发射。
图2显示了照明装置20。其包含一个通用支持体21,一个立方体形的外罩22与其粘合。其顶部一侧装有通用盖板23。该立方体形外罩上有多个切槽,其中安放着单个的半导体组件24。它们是最大发射在450-470nm附近的发蓝光的发光二极管。向白光的转化借助于转化层25进行,转化层25安置在可接受到蓝光辐射的所有表面上。这包括所述外罩侧壁、盖板和支持体的内表面。转化层25由在红光光谱区域发射的磷光体、本发明的在绿光光谱区域发射的磷光体组成,与未被吸收的一级蓝光辐射混合在一起成为白光。
采用Eu2O3(纯度99.99%)、BaCO3(纯度>99.0%)、SrCO3(纯度>99.0%)、CaCO3(纯度>99.0%)、SiO2和Si3N4作为制造本发明新型磷光体的商购原料。通过行星式球磨机,在异丙醇中,将原料以适当的量均质地湿法混合4-5小时。混合后,将混合物在炉中干燥并在玛瑙研钵中研磨,接着在水平管式炉中,在还原性氮气/氢气气氛下,将粉末在钼坩锅中于1100-1400℃下煅烧。煅烧后用粉末X-光散射法(铜K-α线)测定材料。
在紫外-蓝光激发下,所有样品都显示出高效率发光效应,最大发射在蓝绿区域(M=Ba的情况下)、绿色区域(M=Ca)或黄绿区域(M=Sr)。发射和激发光谱的典型实例可见于图3(M=Ca)、图4(M=Sr)和图5(M=Ba)。对于CaSi2O2N2:Eu来说,获得了一种绿光发射磷光体(560nm有最大发射),其可以在光谱的蓝色部分(激发最大值在约440nm处)被高效率地激发。通过采用M=(Ba,Sr)的混合复合物并变化Ba和Sr的比例,发射可以在500nm-570nm内移动,激发谱带的顶部可以从400nm移至高达430nm。观测到的向较长波长的移动可归因于Eu 5d波段在较低能量下的重心和Eu 5d谱带较强的配位场***。通过用(AlO)至少部分地替换(例如高达15mol%)(SiN),可以实现另外的操作,得到优选结构MSi2-xO2+xAlxN2-x:Eu(例如x=0.15)。
由于这些材料有低能激发谱带而能将紫外-蓝光转化成绿光,可以将它们用于白光源,例如基于主要发射蓝光的LEDs(一般为GaN或InGaN)并结合红光发射磷光体的白光源。
通过引入Zn作为阳离子M的补充,优选不超过30%,并用Ge至少部分替换Si,优选不超过25%可以实现其它的精细调制。
表1
原料 | 级别 |
MCO3(M=Ca,Sr,Ba) | 99.0% |
SiO2 | Aerosil OX50 |
γ-Al2O3 | >99.995 |
Si3N4 | β含量:23.3%,O~0.7% |
Eu2CO3 | 99.99% |
以下给出了合成方法。可能的原料示于表1中。
按照以下反应方程可以合成所有的氧氮化物磷光体:
在水平管式炉中,在主要为N2辅以少量H2(10%)的还原性气氛下,将粉末混合物在Mo坩锅中于1100-1400℃煅烧几个小时。
随着原子半径由Ba减小至Ca,发现通过该反应用(AlO)+替换(SiN)+变得更为容易。
图3显示了CaSi2O2N2:Eu的典型发射/激发光谱。
图4显示了SrSi2O2N2:Eu的典型发射/激发光谱。
图5显示了BaSi2O2N2:Eu的典型发射/激发光谱。
在所有实施方案中,所掺杂的Eu为阳离子M的10%。
M=Ca时的最大发射在560nm附近,M=Sr时在570nm附近,M=Ba时在500nm附近。
Claims (11)
1、发光材料,特别是一种LED用磷光体,其可在380-470nm的紫外-蓝光区域被激发,其特征在于掺杂Eu的一般组成为MSi2O2N2的主体晶格,其中M是选自Ca、Sr、Ba的至少一种碱土金属,Eu占M的比例为0.1-30%。
2、权利要求1的紫外-蓝光激发的发光材料,其中M是钙以获得绿光发射。
3、权利要求1的紫外-蓝光激发的发光材料,其中M是至少两种这些金属的混合物。
4、权利要求1的紫外-蓝光激发的发光材料,其中M还包含Zn,优选最高为40mol%。
5、权利要求1的紫外-蓝光激发的发光材料,其中Si被Ge全部或部分地替换,优选最高为25mol%。
6、权利要求1的紫外-蓝光激发的发光材料,其中的主体材料进一步用Mn掺杂,Mn的量优选为至多高达Eu掺杂量的50%。
7、权利要求1的紫外-蓝光激发的发光材料,其中的SiN部分地被AlO替换,得到由MSi2-xAlxO2+xN2-x表示的通式组合物。
8、含有前述权利要求之一的紫外-蓝光激发的发光材料的光源(20)。
9、权利要求8的光源,其中一级发射光是蓝色的,并且将权利要求1-7的紫外-蓝光激发的发光材料与其它磷光体,特别是红光发射磷光体组合,将部分一级发射光转化为较长波长的二级发射光,从而发射出白光。
10、权利要求8的光源,其中一级发射辐射是紫外的,并且将权利要求1-7的紫外-蓝光激发的发光材料与其它磷光体,特别是红光发射磷光体组合,将部分一级发射光转化为较长波长的二级发射光,从而发射出白光。
11、权利要求8的光源,其中该光源是包含至少一个LED的照明装置。
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2003
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- 2003-09-23 TW TW092126179A patent/TWI283078B/zh not_active IP Right Cessation
- 2003-09-23 WO PCT/EP2003/010599 patent/WO2004030109A1/en active IP Right Grant
- 2003-09-23 AT AT03750612T patent/ATE335800T1/de not_active IP Right Cessation
- 2003-09-23 EP EP03750612A patent/EP1449264B1/en not_active Expired - Lifetime
- 2003-09-23 DE DE60307415T patent/DE60307415T2/de not_active Expired - Lifetime
- 2003-09-23 JP JP2004539002A patent/JP3851331B2/ja not_active Expired - Lifetime
- 2003-09-23 US US10/496,707 patent/US7351356B2/en not_active Expired - Lifetime
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CN101045860B (zh) * | 2002-10-16 | 2010-06-09 | 日亚化学工业株式会社 | 氧氮化物荧光体及其制造方法以及使用该氧氮化物荧光体的发光装置 |
CN101253814B (zh) * | 2005-08-30 | 2010-09-01 | 发光物质工厂布赖通根有限责任公司 | 碳氮化硅酸盐发光物质 |
WO2008011782A1 (en) | 2006-05-26 | 2008-01-31 | Dalian Luminglight Science And Technology Co., Ltd. | Silicate-containing luminescent material,its making method and the light-emitting device using the same |
WO2008022552A1 (fr) | 2006-08-15 | 2008-02-28 | Luming Science And Technology Group Co., Ltd. | Matériau luminescent à base de silicate avec pic multi-émission, son procédé de fabrication et son utilisation dans un dispositif d'éclairage |
US8664847B2 (en) | 2007-02-02 | 2014-03-04 | Osram Opto Semiconductors Gmbh | Arrangement and method for generating mixed light |
CN101760190B (zh) * | 2009-10-30 | 2013-07-03 | 彩虹集团公司 | 一种合成稀土掺杂氮氧化物荧光粉及其制备方法 |
CN101775292A (zh) * | 2010-02-23 | 2010-07-14 | 厦门大学 | 一种Eu掺杂氮氧化物荧光粉的制备方法 |
CN102585823A (zh) * | 2012-01-31 | 2012-07-18 | 厦门大学 | 一种紫外led激发三基色氮氧化物荧光粉及其合成方法 |
CN104371710A (zh) * | 2014-11-14 | 2015-02-25 | 广东华科新材料研究院有限公司 | 一种新型绿色氮硅氧荧光粉及其制备方法 |
CN105838371A (zh) * | 2016-04-27 | 2016-08-10 | 山东盈光新材料有限公司 | 一种led用氮氧化物荧光粉及制备方法 |
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US7351356B2 (en) | 2008-04-01 |
DE60307415D1 (de) | 2006-09-21 |
ATE335800T1 (de) | 2006-09-15 |
EP1413618A1 (en) | 2004-04-28 |
WO2004030109A1 (en) | 2004-04-08 |
TW200408149A (en) | 2004-05-16 |
DE60307415T2 (de) | 2007-03-29 |
US20050205845A1 (en) | 2005-09-22 |
EP1449264A1 (en) | 2004-08-25 |
WO2004030109A8 (en) | 2004-06-10 |
CN100592537C (zh) | 2010-02-24 |
TWI283078B (en) | 2007-06-21 |
JP3851331B2 (ja) | 2006-11-29 |
EP1449264B1 (en) | 2006-08-09 |
JP2005530917A (ja) | 2005-10-13 |
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