CN1337989A - 使用发射黄－红光的磷光体的光源 - Google Patents
使用发射黄－红光的磷光体的光源 Download PDFInfo
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- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 12
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 10
- 229910052788 barium Inorganic materials 0.000 claims abstract description 8
- 229910052784 alkaline earth metal Inorganic materials 0.000 claims abstract description 7
- 150000001342 alkaline earth metals Chemical class 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims description 41
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 230000005855 radiation Effects 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 7
- 125000002648 azanetriyl group Chemical group *N(*)* 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- 150000002739 metals Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 description 12
- 229910016066 BaSi Inorganic materials 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 8
- 229910052693 Europium Inorganic materials 0.000 description 7
- 238000000295 emission spectrum Methods 0.000 description 7
- 238000006862 quantum yield reaction Methods 0.000 description 7
- 229910052761 rare earth metal Inorganic materials 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
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- 229910052581 Si3N4 Inorganic materials 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 4
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000000985 reflectance spectrum Methods 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- -1 rare earth-activated silicon nitride class Chemical class 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
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- 235000004515 gallic acid Nutrition 0.000 description 2
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- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
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- 238000002360 preparation method Methods 0.000 description 2
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- 229910052727 yttrium Inorganic materials 0.000 description 2
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 2
- PLXMOAALOJOTIY-FPTXNFDTSA-N Aesculin Natural products OC[C@@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](O)[C@H]1Oc2cc3C=CC(=O)Oc3cc2O PLXMOAALOJOTIY-FPTXNFDTSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 229910006360 Si—O—N Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910003668 SrAl Inorganic materials 0.000 description 1
- 239000005084 Strontium aluminate Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QKYBEKAEVQPNIN-UHFFFAOYSA-N barium(2+);oxido(oxo)alumane Chemical compound [Ba+2].[O-][Al]=O.[O-][Al]=O QKYBEKAEVQPNIN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001642 boronic acid derivatives Chemical class 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- GTDCAOYDHVNFCP-UHFFFAOYSA-N chloro(trihydroxy)silane Chemical compound O[Si](O)(O)Cl GTDCAOYDHVNFCP-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005401 electroluminescence Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
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- 238000004020 luminiscence type Methods 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
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- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
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- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000002639 sodium chloride Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- FZBINJZWWDBGGB-UHFFFAOYSA-L strontium 3,4,5-trihydroxythiobenzate Chemical compound [Sr++].Oc1cc(cc(O)c1O)C([O-])=S.Oc1cc(cc(O)c1O)C([O-])=S FZBINJZWWDBGGB-UHFFFAOYSA-L 0.000 description 1
- FNWBQFMGIFLWII-UHFFFAOYSA-N strontium aluminate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Sr+2].[Sr+2] FNWBQFMGIFLWII-UHFFFAOYSA-N 0.000 description 1
- 208000011117 substance-related disease Diseases 0.000 description 1
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- 230000007704 transition Effects 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
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Abstract
一种使用发射黄－红光的光源,它具有MxSiyNz:Eu型的次氮基硅酸盐的主晶格,其中M是选自Ca、Sr、Ba组中的至少一种碱土金属,而且z=(2/3)x+(4/3)y。
Description
发明领域
本发明涉及使用发射黄-红光的磷光体的光源，更具体地说，不仅仅涉及发光二极管(LED)。磷光体属于稀土活化的氮化硅类。其它应用领域是电灯，特别是高强度放电灯或荧光灯。
技术背景
以Eu2+掺杂的物质通常发射UV-蓝光(Blasse和Grabmeier：发光材料，Springer出版社，海德堡，1994)。一些研究表明，还可发射可见光谱的绿光和黄光(Blasse：二价镧系元素发射的特别情况，欧洲固态无机化学杂志，33(1996)，p.175；Poort，Blokpoel和Blasse：Eu2+在铝酸钡和铝酸锶以及镓酸钡和镓酸锶中的发光，化学物质7(1995)，p.1547；Poort，Reijnhoudt，van der Kuip，和Blasse：Eu2+在含成行的碱土金属的硅酸盐主晶格中的发光，合金和组合物杂志，241(1996)，p.75)。至今，仅在某些例外的情况下，如在碱土金属硫化物和岩盐的相关晶格中的Eu2+发射红光(Nakao，Eu2+离子活化的MgS、CaS和CaSe磷光体的发光中心，日本物理学会杂志，48(1980)，p.534)，在碱土金属的硫代镓酸盐中的Eu2+发射红光(Davolos，Garcia，Fouassier，和Hagenmuller，在硫代镓酸锶和硫代镓酸钡中的Eu2+的发光，固态化学杂志，83(1989)，p.316)和在一些硼酸盐中的Eu2+发射红光(Diaz和Keszler：在固态硼酸盐中Eu2+的发射红光、绿光和蓝光：结构特性关系，材料评述专刊，31(1996)，p.147)。至今仅报导碱土金属氮化硅MgSiN2：Eu中的Eu2+的发光(Gaido，Dubrovskii和Zykov：铕活化的MgSiN2的光致发光，Izv.苏联科学院，无机材料，10(1974)，p.564；Dubrovskii，Zykov和Chernovets：稀土活化的MgSiN2的发光，Izv.苏联科学院，无机材料，17(1981)，p.1421)和Mg1-xZnxSiN2：En中的Eu2+的发光(Lim，Lee，Chang：Mg1-xZnxSiN2：Tb的光致发光特性在薄膜电致发光装置中的应用，无机和有机电致发光，柏林，科技出版社，(1996)，p.363)。曾发现Eu2+在光谱的绿光和绿/蓝光部分的发光。
次氮基硅酸盐类型的新的主晶格是基于其中结合有碱土金属离子(M＝Ca、Sr和Ba)的交联SiN2四面体的三维网络。这类晶格例如是Ca2Si5N8(Schlieper和Schlick：次氮基硅酸盐I，Ca2Si5N8的高温合成和晶体结构，普通无机化学杂志，621(1995)，p.1037)、Sr2Si5N8和Ba2Si5N8(Schlieper、Millus和Schlick：次氮基硅酸盐II，Sr2Si5N8和Ba2Si5N8的高温合成晶体结构，普通无机化学杂志，621，(1995)，p.1380)，以及BaSi7N10(Huppertz和Schnick：高凝聚的次氮基硅酸盐BaSi7N10中的边缘共享SiN4四面体，欧洲化学杂志，3(1997)，p.249)。该晶格类型示于表1。
基于硫化物的磷光体(如碱土金属硫化物)不太适用于照明应用，特别是对LED的应用，因为它们与包封的树脂系统相互作用，并且部分受到水解浸蚀。发红光的Eu2+活化的硼酸盐已表明在LED的工作温度下有一定程度的温度猝灭。
发明内容
本发明的目的是避免现有技术的缺点。另一目的是提供一种有改进型红光再现R9的光源。再一目的是提供一种有改进型全彩色再现Ra的光源。还一目的是提供一种有强彩色再现的LED。
对于LED的应用，希望直到至少100℃都是特别稳定的。其典型的工作温度为约80℃。
这些目的均兼有权利要求1的特征。在附属权利要求中可找到其有利的实施方案。
本光源采用一种新的发射浅黄-红光的磷光体。其吸收至少在蓝-绿的光谱范围内。此外，在吸收时有荧光发射。以Eu2+掺杂的发光物质在黄-红的光谱范围内有发射，特别是红、橙或黄光的发射。这些磷光体都以碱土金属的氮化硅材料作为主晶格。特别是它们极有希望用于采用磷光体的LED中。至今，通过发蓝光的二极管和发荧光的磷光体的组合实现了发白光的LED。这种组合仅有差的色彩再现。采用多色(如红-绿-蓝)体系可达好得多的性能。通常该新材料可与发射绿光(或发射黄光)的磷光体，如其发射最大波长为520nm的SrAl2O4：Eu2+一起使用。
具体而言，采用发射黄-红光的磷光体的新光源使用MxSiyNz：En型次氮基硅酸盐作为主晶格，其中M是选自Ca、Sr、Ba的碱土金属中的至少一种，z＝2/3x＋4/3y。氮的掺入增加共价键和配位场分裂的比例。结果，与氧化物晶格相比，导致激发和发射带明显移向较长波长。
优选的是磷光体的类型为x＝2，y＝5。在另一优选实施方案中，磷光体的类型为x＝1，y＝7。
优选在磷光体中的金属M是锶，因为这样的磷光体以较短的黄-红的波长发射。因此，与大部分其它选定的金属M相比，有更高的效率。
在另一实施方案中，磷光体使用不同金属的混合物，如Ca(10％(原子))和Ba(其余量)作为组分M。
这些材料在UN和蓝色可见光谱(直到大于450nm)中有高的吸收和好的激发、并有高的量子效率和达100℃的低温猝灭。
它可用于有蓝光发射主源与一种和多种磷光体(红和绿)的发光转换LED。另一应用领域是小型荧光灯和高强度放电灯中的钒酸钇的替代物。
附图简述
图1为未掺杂的Ba2Si5N8和Ba2Si5N8：Eu的漫反射谱；
图2为未掺杂的BaSi7N10和BaSi7N10：Eu的漫反射谱；
图3为Ba2Si5N8：Eu的发射谱；
图4为BaSi7N10：Eu的发射谱；
图5-7为Sr2Si5N8：Eu的一些实施方案的发射谱；
图8为Ca2Si5N8：Eu的发射谱；
图9为白光LED的发射谱；
图10为用作白光光源的半导体元件。
实施方案详述
Eu2O3(纯度99.99％)、或Eu金属(99.99％)、Ba金属(＞99％)；Sr金属(99％)、Ca3N2(98％)、或Ca粉末(99.5％)和Si3N4(99.9％)以市售原料使用。Ba和Sr在550-800℃的氮气气氛中焙烧氮化。接着，Ca3N2或氮化的Ba、Ca和Sr在氮气气氛下于研钵中研磨，并以化学计算量与Si3N4混合。Eu浓度为10％(原子)，与碱土金属离子相似。该粉末混合物在钼坩埚中于约1300-1400℃的卧式管炉中于氮/氢气氛下焙烧。焙烧后该粉末由粉末X-射线衍射(CuKα-线)表明其特征，结果表明形成所有的化合物。
未掺杂的Ba2Si5N8、Ca2Si5N8和BaSi7N10的浅灰-白色粉末。这些未掺杂的经稀土元素活化的氮化硅在可见光范围(400-650nm)有强反射，并在250-300nm其反射大大下降(图1和2)。反射比的下降是由于主晶格的吸收。Eu掺杂的样品是橙-红色，但BaSi7N10：Eu是橙-黄色(表1)。只有Eu2+掺杂的以稀土元素活化的氮化硅是深着色的，并使其成为有利的橙-红磷光体。Ba2Si5N8：Eu的反射谱的典型实例表明，由于Eu的吸收与主晶格吸收相重叠，并延伸至500-550nm(图1)。这说明这些化合物的红-橙色。对Sr2Si5N8：Eu和Ca2Si5N8：Eu发现有类似的反射谱。
对于BaSi7N10：Eu，在可见光部分的Eu的吸收要小得多(图2)，它说明该化合物的橙-黄色。
所有样品在UV激发下者能有效发光，并在可见光谱的橙-红部分有发射最大值(见表1)。图3和4给出两种典型的发射光谱的实例。其表明，发射是在特别长的波长处(Eu2+发射)，对BaSi7N10：Eu(图4)其最大值达660nm。在低能处发现激发带，这是Eu2+5d带在低能处的重心及Eu2+5d带的强配位场分裂的结果，如对含N3-的晶格所预计的(Van Krevel，Hintzen，Metselaar，和Meijerink：在Y-Si-O-N材料中长波长Ce3+发光，J.Alloys和Comp(合金和化合物杂志)168(1998)272)。
由于低能激发带，这些材料要将蓝光转换成红光，因此可用于白光源中，例如基于与发射红光、黄光和/或绿光的磷光体相结合的主要发射蓝光的LED(典型为GaN或InGaN)。
表1
| 化合物 | 晶体结构 | 颜色 | 发射最大值(nm)* |
| Ca2Si5N8：Eu | 单斜晶系 | 橙-红 | 600至630 |
| Sr2Si5N8：Eu | 斜方晶系 | 橙-红 | 610至650 |
| Ba2Si5N8：Eu | 斜方晶系 | 橙-红 | 620至660 |
| BaSi7N10：Eu | 单斜晶系 | 橙-黄 | 640至680 |
*取决于制备条件和活化体浓度；Eu-浓度的典型值可在1-10％变化，相似于碱土金属离子M
其发射最大值远在长波侧。一个具体的例子是Sr1.8Eu0.2Si5N8型的磷光体。其发射谱示于图5。
另一个实现M实施方案是使用Zn。它可部分或完全由Ba、Sr或Ca替换。
完全或部分替换Si的另一实施方案是Ge，具体的实例为Sr1.8Eu0.2Ge5N8。
还研究了另一些具体实施例。
研究了发射红光的磷光体Sr2Si5N8：Eu2+的制备条件和光学特性。最佳时其量子效率约为70％。根据Eu2+在样品中的浓度和加热条件，该发射在610-650nm之间是可调的。在400nm和460nm处的吸收是高的(反射仅15-40％)，并且在80℃的发光猝灭是低的(仅4％)。未研磨的磷光体的粒度低于5μm。这些特性使该磷光体特别适于在UV光和蓝光LED中应用。
合成氮化物的原料是Si3N4(99.9％(主α-相)，Alfa Aesar)、Sr金属(枝状物99.9％，Alfa Aesar)和Eu2O3(4N)。Sr金属必须经氮化，并且在使用Eu金属代替Eu2O3时，Eu金属也必须经氮化。该Sr金属在氩气气氛的手套箱中的玛瑙研钵中经手工研磨，并在800℃的N2气中氮化。其氮化达80％以上。
再研磨后，该氮化过的金属与Si3N4和Eu2O3一起研磨，并在手套箱中再次手工混合。该混合物的加热参数通常如下：
以18℃/分升温达800℃
在800℃下保持5小时
以18℃/分升温达T终(1300-1575℃)
在T终下保持5小时
H2(3.75％)/N2为400升/时
以Ca3N2作原料制备了Ca2Si5N8：Eu2+。
所有样品的一览表示于表1.通常这些样品首先在800℃下加热，然后以同样循环在高温(1300-1600℃)下第二次加热。样品再经研磨(在空气中研磨)、过筛和测定。
表1：(Ca，Sr)2Si5N8：Eu2+样品的加热循环参数
| 代码 | Ca/Sr | Eu2+(％) | 时间1(h) | 温度1(℃) | 时间2(h) | 温度2(℃) |
| EC/HU 31/00 | Ca | 10 | 5 | 800 | 5 | 1400 |
| EC/HU 42/00 | Ca | 1 | 5 | 800 | 5 | 1565 |
| EC/HU 41/00 | Ca0.4Sr1.4 | 10 | 5 | 800 | 5 | 1565 |
| EC/HU 62/00 | Sr | 1 | 5 | 800 | 5 | 1400 |
| EC/HU 63/00 | Sr | 2 | 5 | 800 | 5 | 1400 |
| EC/HU 64/00 | Sr | 3 | 5 | 800 | 5 | 1400 |
| EC/HU 65/00 | Sr | 5 | 5 | 800 | 5 | 1400 |
| EC/HU 66/00 | Sr | 8 | 5 | 800 | 5 | 1400 |
| EC/HU 67/00 | Sr | 10 | 5 | 800 | 5 | 1400 |
由此加热所得的样品表明含10％Eu2+的Sr2Si5N8样品的深橙色。随Eu2+较少，其颜色变淡。Ca样品为黄-橙色。
还有另一特征，即粉末颗粒非常小，其平均粒度d50为约0.5-5μm，通常d50＝1.3μm。对于用发光材料加工LED，小粒度是有利的。例如材料在树脂中能有均匀分布。
表2：(Ca，Sr)2Si5N8：Eu2+样品的光学数据
| 代码 | Ca/Sr | Eu2+(％) | 发射最大(nm) | 反射400(％) | 反射460(％) | 量子效率(％) | x | y |
| EC/HU 31/00 | Ca | 10 | 619 | 12 | 19 | 26 | 0.600 | 0.396 |
| EC/HU 42/00 | Ca | 1 | 603 | 47 | 58 | 37 | 0.555 | 0.435 |
| EC/HU 41/00 | Ca0.4Sr1.4 | 10 | 660 | 17 | 22 | 59 | 0.636 | 0.354 |
| EC/HU 62/00 | Sr | 1 | 609 | 53 | 58 | 70 | 0.602 | 0.393 |
| EC/Hu 63/00 | Sr | 2 | 618 | 43 | 48 | 73 | 0.615 | 0.381 |
| EC/Hu 64/00 | Sr | 3 | 621 | 36 | 41 | 72 | 0.622 | 0.374 |
| EC/Hu 65/00 | Sr | 5 | 624 | 26 | 32 | 67 | 0.632 | 0.365 |
| EC/HU 66/00 | Sr | 8 | 636 | 21 | 26 | 67 | 0.641 | 0.356 |
| EC/HU 67/00 | Sr | 10 | 644 | 17 | 22 | 64 | 0.642 | 0.354 |
表2中的样品通常按第一循环(例如800℃下5小时)首次加热，如上述。
包含在表2中的是发射最大值的位置、平均波长、在400和460nm处的反射、量子效率和x和y的颜色坐标。
由表2可看出，纯Ca样品并不如Sr样品有利。惊奇的是，Sr-Ca化合物的发射波长比纯Sr化合物的发射波长更长。
具体实例示于图6-8。图6给出含3％Eu和量子效率为72％的样品HU64/00(Sr2Si5N8：Eu2+)的能量分布(任意单位)和反射(百分数)。图7给出含5％Eu和量子效率为67％的样品HU65/00(Sr2Si5N8：Eu2+)的能量分布(任意单位)和反射(百分数)。图8给出含1％Eu和量子效率为37％的样品HU42/00(Ca2Si5N8：Eu2+)的能量分布(任意单位)和反射(百分数)。
光源的具体实例是已知其原理的白光LED，例如参见US-5998925或US-A6066861。它使用发射蓝光的主光源(发射峰约在380-470nm)，优选是(In)GaN-芯片，其辐射被基于树脂和至少一种磷光体的转换材料部分吸收。使用用于主光源的蓝光的两种或三种转换磷光体，对白光LED可得到改进的彩色再现。一些实施方案可同时包含第一磷光体和本发明的第二磷光体，第一磷光体的主发射在480-600nm，例如基于钇的石榴子石、硫代棓酸盐和/或氯硅酸盐，本发明的第二磷光体为新型稀土元素活化的氮化硅，其主发射在600nm以上，优选在650nm以上。不同磷光体在发射之间的某些重叠可在600-650nm间存在。特别是在使用基于420-470nm之间主发射的白光LED，并同时有第一磷光体YAG：Ce(黄光)和第二磷光体M2Si5N8：Eu2+(红光)时，彩色再现Ra达85和甚至约90，这取决于混合物和M的选择情况。
在第一磷光体有更绿的发射(最大在约490nm)时可得到更进一步的改进。
另一概念是用于激发三个磷光体(RGB-概念)的发射UV-辐射的主光源，其中红光组分是本发明的以稀土元素活化的氮化硅的新型磷光体，绿光和蓝光组分是上述已知的磷光体。
此外，可用本发明的新型磷光体产生高稳定红光或橙光或黄光的LED，该LED可基于发射峰在约380-480nm的主光源(优选InGaN-芯片)，其光由本发明的以稀土元素活化的由Eu掺杂的氮化硅的氮化物磷光体完全转换。这些LED与已知的有黄-红色直接激发的市售LED相比有较高的效率和改进的稳定性。
图9给出一些白光LED的发射谱。它们基于InGaN-芯片发射主辐射，其发射峰在460nm，它在覆盖芯片的环氧树脂中被部分转换。
一种用于白光的光源的图式结构示于图10。光源有InGaN半导体元件(芯片1)，其发射峰波长为460nm；第一和第二电接线端2、3，它包括连接线14；该半导体元件埋在不透光的基壳8的凹穴9的区域中。基壳8和凹穴9之间的边界是作为发射自芯片1的主蓝光的反射器的壁，凹穴9填有浇注物5，它含作为主要组分的环氧浇注树脂和磷光体颜料6(小于浇注物5的15％)。其它还包括少量甲基醚和一种高度分散的硅胶。
一些实施方案的树脂包含不同的磷光体组合物。具体而言，以基于仅由YAG：Ce磷光体转换发射的主蓝光的标准白光LED提供参比。磷光体比例为树脂的3.6％(重量)(曲线1)。除YAG：Ce外，还研究三个含Sr2Si5N8：Eu2+的实施方案。在保持转换磷光体的总比例为恒定(3.6％)的条件下，由Sr2Si5N8：Eu2+替换0.25％的YAG：Ce，见曲线2。Sr2Si5N8：Eu2+的量再增加到0.5％(曲线3)和7.5％(曲线4)。其彩色再现Ra有明显改进：相对参比(曲线1)改进6％(曲线2)，改进10％(曲线3)和改进12％(曲线4)。
Claims (10)
1.一种使用发射黄-红光的光源，其中磷光体转换至少部分来自主光源的辐射，其特征在于该磷光体有MxSiyNz：Eu型次氮基型硅酸盐的主晶格，其中M是选自Ca、Sr、Ba、Zn组中的至少一种碱土金属，而且z＝2/3x＋4/3y。
2.权利要求1的光源，其中x＝2，y＝5。
3.权利要求1的光源，其中x＝1，y＝7。
4.权利要求1的光源，其中M是锶。
5.权利要求1的光源，其中M是至少该组的两种金属的混合物。
6.权利要求1的光源，其中Si由Ge全部或部分替换。
7.权利要求1的光源，其中磷光体的平均粒度为0.5-5μm。
8.权利要求1的光源，其中光源发射主辐射，在主辐射的激发下磷光体发射第二辐射。
9.权利要求8的光源，其中主辐射是蓝光，优选在420-470nm范围(峰波长)，并且与第二辐射，优选与至少另一磷光体的第二辐射组合，以获得白光。
10.权利要求9的光源，其彩色再现Ra至少为85，优选为90。
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| CN101353576B (zh) * | 2004-07-14 | 2011-12-07 | 株式会社东芝 | 含氮荧光物质、其制造方法以及发光器件 |
| US8053798B2 (en) | 2006-06-30 | 2011-11-08 | Seoul Semiconductor Co., Ltd. | Light emitting device |
| CN101438428B (zh) * | 2006-06-30 | 2012-01-25 | 首尔半导体株式会社 | 发光装置 |
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