CN1596292A - 发光材料和使用它的发光二极管 - Google Patents

发光材料和使用它的发光二极管 Download PDF

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CN1596292A
CN1596292A CN03801605.2A CN03801605A CN1596292A CN 1596292 A CN1596292 A CN 1596292A CN 03801605 A CN03801605 A CN 03801605A CN 1596292 A CN1596292 A CN 1596292A
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luminescent material
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H·T·辛岑
李元强
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Ams Osram International GmbH
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Abstract

一种UV－蓝可激发的发光材料，其由具有共同组成为MAl2－xSixO4－xNx的掺杂Eu的氧氮化物主体晶格，其中M为选自Ca，Sr，Ba的至少一种碱土金属。

Description

发光材料和使用它的发光二极管
                        技术领域
本发明涉及一种发光材料，其可以在光谱区的紫外-蓝光部分激发，更具体涉及，但不局限于用于光源，优选发光二极管(LED)的磷光体。磷光体属于一类稀土活性氧氮化硅。
                        技术背景
迄今为止，通过发蓝光的二极管和发黄光的磷光体联合就可实现白光LED。这种联合的色彩还原性很差，然而通过使用红-绿-蓝系统(RGB)就能够得到大大改进。例如，这种系统使用红色和蓝色发光体，联合发绿光的铝酸盐磷光体，比如SrAl2O4:Eu或BaAl2O4:Eu，并可能把Mn添加到Eu中，其最大发射约在520nm，见US-A6 278 135。然而，这些铝酸盐的激发位置和发射带并不是最优的。其不得不通过330～400nm范围内的短紫外激发。
令人感兴趣的发光新材料是用Eu2+掺杂的α-硅铝氧氮陶瓷(sialon)，其结构为MtSi12-(m+n)Al(m+n)N(16-n)，其中M为Ca或Y或稀土金属。t值为m/val+，其中val+是离子M的价电荷。例如，M＝Sr+的val+值为2。这样，整个结构的电荷完全被补偿。更进一步的细节见例如J.Van Krevel等在2002年四月的J.Sol.St.Chem.，19-24页的“Tb，Ce，或Eu-掺杂的α-硅铝氧氮陶瓷材料”，和R.-J.Xie等在200年五月J.A.Ceram.Soc.1229-1234页的“Preparation andLuminescence Spectra of Ca and rare Earth co-doped α-SiAlONCeramics”，并且进一步出现在US-Pub 2002/0043926之上，其参考文献都涉及α-硅铝氧氮陶瓷类型的Ca-硅铝氧氮陶瓷。硅铝氧氮陶瓷的其他类型到现在还不得而知。
                        发明内容
本发明的一个目的是提供一种如权利要求1前述部分所述的新型发光材料。另一个目的是提供一种具有微调发射的磷光体，其能够通过UV/蓝辐射有效激发。另一个目的是提供一种磷光体，用于具有至少一个LED作为光源的照明装置，这种LED发射的初级辐射为360～470nm，这种辐射通过暴露于LED发出的初级辐射的磷光体而被部分或全部转化为波长更长的长波辐射。另一个目的是提供一种照明装置，能够发射白光，特别是具有高色彩还原性。另一个目标是提供一种像LED设备一样在360～470nm有很好的吸收并且易于生产的高效照明装置。
这些目的通过权利要求1和10表征的性质得以分别达成。在从属权利要求中给出了具体的优势结构。
这种转化至少通过衍生于Eu活化或Eu、Mn-共活化铝酸盐的氧氮化物磷光体而实现。更详细地讲，现有技术的缺点通过以下方式克服：在MAl2O4:Eu(M＝Ca，Sr，Ba)中引入氮，形成氧氮化物磷光体，通常并优选维持鳞石英结构。然而，并不排斥其他结构。更具体说，(AlO)+部分地被(SiN)+取代，生成通式组合物：MAl2-xSixO4-xNx:(Eu或Eu，Mn)。x设定为x≥0.002而且至多x＝1.5。对比前面提及的现有技术的衍生自氮化物Si3N4的α-硅铝氧氮陶瓷类型的结构，此处结构更类似于氧化物，是衍生于SiO2的改性，特别优选衍生自鳞石英结构。
相对照，α-硅铝氧氮陶瓷材料表现为氮化物结构，换句话说，他们是基于Si3N4的，其中Si-N部分被Al-O和/或Al-N取代。因为在α-硅铝氧氮陶瓷和鳞石英中可能的激发部位与周围离子的局部相互作用有很大不同，这些不同结构就会导致不同的发光行为。
就以Ca作为M的主成分的情况而言，优选的值是0.01≤x≤0.1。就以Ba或Sr作为M的主成分的情况而言，优选的值是0.1≤x≤0.7。氮的结合增加了共价键合和配位场分裂的程度。因此，与氧化物晶格相比，导致激发带向更长波长迁移。获得的磷光体表现出高化学或热稳定性。通过使用正离子M就能够获得所有相关性能的更广的微调，这可以通过组合几种所述M金属(特别是Sr和Ba)，并进一步包含Zn作为部分正离子M(优选10～40mol％)，和/或至少部分用Ge取代Si(优选5～25mol％)和/或用Ga取代Al(优选5～25mol％)就可以实现。对于发绿光的材料优选金属M主要是Ba和/或Sr，对于发蓝光主要是Ca。掺杂到正离子M中的Eu量为M的0.1～25％，优选2～15％。另外进一步用Mn掺杂来获得相关性能的微调时，优选用量为Eu掺杂量的至多50％。
由于这些材料具有低能激发带，能够把UV-蓝辐射转化为蓝-绿光，因此例如他们能够应用于白色光源(例如灯)，特别是基于组合使用红光发射磷光体的基发射为蓝光的LEDs(典型为具有约430～470nm的GaN或InGaN)。一种合适的发射红光的磷光体是掺杂Eu的氮化硅材料，如M2Si5N8(M＝Ca，Sr，Ba)，例如参见WO 01/40403。而且应用于彩色光源也是可能的。
                        附图简述
在接下来的上下文中，参考多个典型实施方案更详细解释本发明。在附图中：
图1显示了一个半导体组件(LED)，其用作白光光源，其含有浇注树脂(图1a)和没有浇注树脂(图1b)；
图2显示了本发明的一个具有磷光体的发光装置；
图3显示了本发明磷光体的发射光谱和反射光谱；
图4～8显示了本发明另一个磷光体的发射光谱和反射光谱；
图9显示了单位晶胞体积与x值的关系。
                     实施本发明的最佳模式
通过举例的方式来描述在WO 01/40403中使用的相似结构，其被用于与InGaN晶片在一起的白光LED。这种白光光源的结构具体见图1a。这种光源是基于具有400nm波长发射峰的InGaN型半导体组件(晶片1)，具有第一和第二电路连接2、3，其包埋在不透明基罩8的凹槽区域9中。连接之一3经一连接导线4连接到晶片1。凹槽具有一个壁7，作为晶片1的蓝光初级辐射的反射器。凹槽9用含有硅酮浇注树脂(或环氧浇注树脂)作为其主要组成(优选超过80wt％)，并进一步含有磷光体颜料6(优选低于15wt％)的灌注混合物来填充。而且也可以还存在少量的，尤其是甲基醚和氧相二氧化硅。磷光体颜料是本发明的绿色磷光体与发射蓝光、绿光和红光的三种颜料的混合物。
图1b显示了具有半导体组件10的光源的实施方案，在该半导体组件10中向白光的转化是通过磷光体转化层16实施的，该磷光体转化层16可直接应用于单个晶片。在基底11的顶部，存在一个接触层12、一面镜层13、一个LED晶片14、一个滤光器15和磷光体层16，其通过LED初级辐射激发，并将其转化为可见光波长辐射。这种结构单元用塑料透镜17围住。仅仅图示了两个欧姆接触器的上接触器18。LED的初级UV辐射约为400nm，次级辐射是通过本发明的第一磷光体(M(1-c)Al2-xSixO4-xNx:Dc，D为Eu或Eu，Mn)发射。特别优选使用BaAl2-xSixO4-xNx:(10％)Eu2+，其发射约525nm(或以调谐的一般式语言，c＝0.1和D＝Eu)，和通过使用发射橙红光的次氮基硅酸盐的第二磷光体。
图2显示了一个照明设备20，其含有一个共同支架21，方形外罩22黏结其上。其上侧面提供一共同罩子23。方形外罩具有一个保险装置，其中装上单独的半导体组件24。他们是具有约450～470nm发射峰的发蓝光的二极管。通过转化层25实现向白光的转化，这些转化层排列在所有可以让蓝色辐射照射的表面上。这些包括外罩，支架和罩子的侧壁的内表面。转化层25包括发射在红光光谱区的磷光体和使用本发明的绿光光谱区的磷光体，并与不吸收初级辐射的蓝光部分混合在一起主要转化为白光。
Eu2O3(纯度为99.99％)、BaCO3(纯度＞99.0％)、SrCO3(纯度＞99.0％)、CaCO3(纯度为99.0％)、Al2O3(纯度为99.9％)、SiO2和Si3N4可用于商业用原材料，用于生产新发明的磷光体。这些原材料通过行星式球磨机在异丙醇中以合适的量均相湿混4-5小时。经混合的混合物在炉中干燥并在玛瑙研钵中磨细。随后，在平管炉中，在钼坩锅中，在还原性的氮气/氢气气氛存在下，于1100-1400℃下锻烧粉末。锻烧后，通过粉末X-衍射(铜K-α线)表征。
所有的样品在UV-蓝激发下都表现出有效发光最大发射，在蓝光区(即M＝Ca的情况)尤其是435～445nm，或在绿光区(如M＝Sr或Ba的情况)尤其是Ba情况下波长为495～530nm和Sr情况下波长为515～575nm。发射和激发光谱的两个典型实例见图3和图4。图3显示的是带有不同x值的SrAl2-xSixO4-xNx:Eu的发射和激发光谱。图4显示的是带有不同x值的BaAl2-xSixO4-xNx:Eu的发射/激发光谱。
通过使用不同量的氮，各种发射可以在495～575nm范围内迁移。特别是Sr对迁移是敏感的(图3)，同时激发带的顶部能够从低于400nm迁移到430～465nm，优选至440nm，见M＝Ba(图4)。所观察到向更高波长的迁移是Eu 5d在低能量处的重心和Eu 5d带更强的配位场分裂作用的结果。
附加的微调通过以下方法实现：用优选不超过30％的Zn添加到正离子M，和优选不超过25％的Ga部分取代Al，和/或优选不超过25％的Ge取代Si。
表1
原材料  等级
MCO3(M＝Ca，Sr，Ba) 99.0％
SiO2  Aerosil OX50
γ-Al2O3  ＞99.995
Si3N4  β含量23.3％，O～0.7％
Eu2O3  99.99％
接下来是MAl2-xSixO4-xNx:(10％)Eu2+(M＝Ca，Sr，Ba)的合成步骤，可能的起始原料见表1。
包含鳞石英的所有氧氮化物磷光体根据以下反应方程合成(忽略气相)，
其中M为Ca，Sr，Ba单独或组合使用，一个实例是y＝0.1。
例如，Ba0.9Eu0.1Al2-xSixO4-xNx的组成如下表2所示：
表2(单位：克)
    x值     BaCO3     Al2O3     Si3N4     SiO2     Eu2O3
    0.3     3.497     1.689     0.205     0.088     0.343
    0.5     3.500     1.492     0.342     0.146     0.343
详细的实验结果显示，磷光体的发光性能几乎与精确的SiO2含量无关。然而把SiO2的含量降低到某个合适的值(例如，至多降至SiO2含量计算值的1/60)会大大增强相纯度和效率。
在平管炉中用钼坩锅于1100～1400℃下在含少量H2(10％)的N2还原性气氛下锻烧粉末混合物几小时。
图5～8进一步显示了解释了SiO2含量减少的作用的样品激发和发射光谱。
图5的实施方案：Ba0.9Eu0.1Al2-xSixO4-xNx，其中x＝0.3，SiO2含量没有减少。对于发射光谱用λ激发＝440nm对磷光体进行激发，对于激发光谱在λ监控＝530nm处进行监控。其主相具有BaAl2O4结构。
图6的实施方案：Ba0.9Eu0.1Al2-xSixO4-xNx，其中x＝0.3，SiO2含量减少到SiO2含量计算值的1/4。(λ激发＝440nm，λ监控＝530nm)。其主相具有BaAl2O4结构。
图7的实施方案：Ba0.9Eu0.1Al2-xSixO4-xNx，其中x＝0.5，SiO2含量减少到SiO2含量计算值的1/16。(λ激发＝440nm，λ监控＝530nm)。其主相具有BaAl2O4结构。
Si3N4用作以下方程式〔1〕的(SiN)+源：
(M＝Ca，Sr，Ba)。
随着原子半径由Ba到Ca的降低，发现通过该反应用(SiN)+替换(AlO)+变得更加困难。晶格参数结果显示，N在具有鳞石英结构的BaA12O4中的最大溶解度约为x≈0.6。图9显示了单位晶胞体积和具有鳞石英结构的BaAl2-xSixO4-xNx中x值之间的关系。正如所预期那样，同Al-O距离相比，由于Si-N距离变得更小，随着x值的增大，单位晶胞体积降低，如图9所示。对于x值大大超过0.6时，单位晶胞体积几乎维持成常数，并能够观察到第二相。
因此，用铝酸钡和x值高达0.6而无需调节SiO2的含量就能获得良好的结果。
而且使用铝酸Sr也能获得良好的结果。SiO2含量的减少(以y表示)导致MAl2-xSix-yO4-x-2yNx:Eu型的非化学计量的铝酸盐，优选y≤0.25x。调节SiO2含量可以达到最佳性能，x值高至0.5。对于铝酸Ca而言情况相同，然而有更小的x值，优选低于0.05。
现在更详细地讨论MAl2-xSixO4-xNx:10％Eu2+的发光性能。图8显示了MAl2-xSixO4-xNx:Eu2+(M＝Sr，Ca)的激发和发射光谱。SiO2的含量没有减少。更详细地，各自具有不同的x值，图8a显示了SrAl2-xSixO4-xNx:Eu2+(10％)的激发和发射光谱，图8b显示了CaAl2-xSixO4-xNx:10％Eu2+(10％)的激发和发射光谱。
与单位晶胞体积和MAl2-xSixO4-xNx的x值之间的关系结果相对应，根据正离子的不同，发射带或多或少地向更长波长方向迁移。以Ba而言，典型的迁移为495迁移至530nm，对于Sr，典型迁移为515迁移至575nm，对于Ca，典型迁移为440迁移至445nm。对于BaAl2-xSixO4-xNx:(10％)Eu2+，随着结合的N含量x值的增加，发射带迁移为约497迁移至527nm。激发带相应地从385迁移至425nm。
对于MAl2-xSixO4-xNx:(10％)Eu2+，M至少为Sr或Ca的至少一种，(SiN)+的含量基本上不会增加发射波长和激发波长，因为在晶格参数中几乎没有观察到迁移。就M＝Ca而言，相应于少量N的引入，Eu的发射带最大迁移低于10nm。因此，少量(SiN)+的引入仅仅能够对Eu2+离子的局部配位产生微弱影响。该讨论通过加入标准化学计量的SiO2量加以理解。
然而，令人非常吃惊的是，已经证实在几种情况下使用低于化学计量的SiO2量是有利的。就SrAl2-xSixO4-xNx:Eu2+(10％)而言，最明显的是在反应(1)中降低SiO2的含量会影响N的引入和发光性能。其理由还不能够完全知晓。当用于反应(1)的SiO2含量为较低的因子60时，就会发现，引入到具有填塞的鳞石英结构的SrAl2O4晶格的(SiN)+含量就增加。最大溶解度为x≈0.5(表1)。由于N的引入，Eu的发射带迁移到更长的波长，高达575nm(图3)。在N的最大溶解度(x＝0.3...0.5)处出现了430nm明显的激发肩峰，如图3所示。
除了衍生自鳞石英结构，衍生自SrAl2O3N2结构也是可能的。这种化合物在1998年被Schnick发现。其与LnSi3N5(Ln＝La，Ce，Pr，Nd)型硅酸盐氮化物是同位素的。

Claims (13)

1.一种发光材料，优选为用于LED用途的磷光体，其在360～470nm的UV-蓝光区可激发，其特征在于用Eu掺杂具有共同组成的MAl2-xSixO4-xNx主体晶格，其中M为选自Ca，Sr，Ba的至少一种碱土金属，0.002≤x且x≤1.5，优选x低于0.7，Eu含量为M的0.1～25％。
2.权利要求1的UV-蓝可激发的发光材料，其中主体晶格衍生自鳞石英结构。
3.权利要求1的UV-蓝可激发的发光材料，其中为了获得绿光发射，M是锶和/或钡。
4.权利要求1的UV-蓝可激发的发光材料，其中为了获得蓝光发射，M是钙。
5.权利要求1的UV-蓝可激发的发光材料，其中M是这些金属中至少两种的混合物。
6.权利要求1的UV-蓝可激发的发光材料，其中M另外含有Zn，优选至多40mol％。
7.权利要求1的UV-蓝可激发的发光材料，其中Al全部或部分被Ga取代。
8.权利要求1的UV-蓝可激发的发光材料，其中Si全部或部分被Ge取代，优选不超过25％。
9.权利要求1的UV-蓝可激发的发光材料，其中主体材料进一步用Mn掺杂，共掺杂的Mn含量优选最多为Eu掺杂的50％。
10.具有前述权利要求任一项的UV-蓝可激发的发光材料的光源(20)。
11.权利要求10的光源，其中初级发射光是蓝光，并且权利要求1～9的UV-蓝可激发的发光材料与其他磷光体，特别是红光发射磷光体组合使用，以便把初级发射光转化成波长更长的次级发射光以获得白光发射。
12.权利要求10的光源，其中初级发射辐射是UV，并且权利要求1～9的UV-蓝可激发的发光材料与其他磷光体，特别是红光和蓝光发射磷光体组合使用，以便把初级发射辐射转化成波长更长的次级发射光以获得白光发射。
13.权利要求10的光源，其中光源是具有至少一种LED的照明设备。
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