CN113056540A - 用于制造陶瓷转换器元件的方法、陶瓷转换器元件和光电组件 - Google Patents
用于制造陶瓷转换器元件的方法、陶瓷转换器元件和光电组件 Download PDFInfo
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- CN113056540A CN113056540A CN201980076268.4A CN201980076268A CN113056540A CN 113056540 A CN113056540 A CN 113056540A CN 201980076268 A CN201980076268 A CN 201980076268A CN 113056540 A CN113056540 A CN 113056540A
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Abstract
提供了用于制造陶瓷转换器元件的方法。所述方法包括以下步骤:提供磷光体作为起始材料,将所述磷光体与至少一种金属氧化物粉末混合以形成混合物,对所述混合物进行加工以形成其中所述磷光体嵌入陶瓷基体中的陶瓷转换器材料。此外,提供了具有陶瓷转换器元件的光电组件和陶瓷转换器元件。
Description
本发明涉及用于制造陶瓷转换器元件的方法、陶瓷转换器元件、和光电组件。
辐射发光组件如,例如,发光二极管(LED)发射可见或不可见的辐射。根据LED的材料,LED发射第一辐射的光,例如在InGaN的情况下,发射蓝光。这样的LED可以与包含磷光体的转换器层组合,所述磷光体将第一辐射至少部分地转换成不同波长的第二辐射。例如,发射蓝光的LED可以与发射黄光的氧化物转换器如YAG:Ce组合,例如以产生白光。包括LED和转换器层的照明装置单独发射第二辐射的光或与未转换的第一辐射组合发射第二辐射的光。
目前,陶瓷磷光体转换器YAG:Ce(掺杂有Ce的钇铝石榴石)可以通过不同的方法来合成。例如,存在用不同氧化物(例如Y2O3、Al2O3、CeO2和Gd2O3)开始并通过数个步骤进行加工的混合氧化物方法。通常,取决于起始氧化物的颗粒尺寸和烧结期间的晶粒生长,该方法导致或粗或细的陶瓷的磷光体颗粒尺寸或晶粒尺寸。混合氧化物方法的缺点是,有时氧化物之间的反应不完全,从而导致非化学计量的YAG:Ce磷光体颗粒以及其他不期望的相例如(含Ce或含Gd的)YAG(Y3Al5O12)、YAM(Y4Al2O9)、YAP(YAlO3)、Y2O3或Al2O3。这种混合物导致材料的较低的量子效率(QE)并因此产生低的光通量。
用于制造陶瓷磷光体转换器YAG:Ce的另一种方法是共沉淀磷光体前体合成方法,所述方法使用湿化学工艺来产生起始混合物,在所述起始混合物中包含Y、Al、Ce、Gd等的不同有机盐或无机盐在水性溶剂或有机溶剂中彼此反应,并且包含这些元素的化合物共沉淀。用这种方法,所得的磷光体表现出细颗粒尺寸,然而,当对细粉末进行加工时,有时观察到未反应的相例如YAM、YAP等。这导致最终陶瓷转换器的第二相或第三相,从而导致色移和低的QE。
一个目的是提供改善的用于制造陶瓷转换器元件的方法。另一个目的是提供改善的包括陶瓷转换器元件的光电组件和陶瓷转换器元件。这些目的用根据独立权利要求的方法以及光电组件和陶瓷转换器元件来解决。方法和光电组件的另外的实施方案是从属权利要求、说明书和示例性实施方案的主题。
根据一个方面,提供了用于制造陶瓷转换器元件的方法。
陶瓷转换器元件应理解为能够将第一辐射的波长至少部分地转换成第二辐射的波长。为了这个目的,其包含能够通过光致发光转换辐射的磷光体作为活性材料。期望在转换辐射时具有高的QE。在下文中,表述“陶瓷转换器元件”和“转换器元件”可互换使用。
根据一个实施方案,提供了磷光体作为起始材料。换言之,该方法使用用作起始材料的具有期望晶体结构的预合成的磷光体粉末。因此,陶瓷转换器元件中的磷光体的光学性能和显微组织可以根据其中要实施转换器元件的装置的需求来定制。例如,磷光体的期望颗粒尺寸可以以具备具有受控的散射、吸收、孔尺寸、孔密度和其他显微组织特性的陶瓷转换器元件的方式来确定。
根据另一个实施方案,将磷光体和至少一种金属氧化物粉末混合以形成混合物。由于磷光体还可以以粉末的形式提供,因此根据一个实施方案,混合物为粉末混合物。
根据另一个实施方案,可以对混合物进行加工以形成其中磷光体嵌入陶瓷基体材料中的陶瓷转换器材料。基体材料为主要由金属氧化物粉末形成的陶瓷基体,所述金属氧化物粉末包括某些期望的性能并且被添加到预合成的磷光体中或者与预合成的磷光体混合,其中磷光体包括期望或特定的性能。
根据一个方面,提供了用于制造陶瓷转换器元件的方法。该方法包括以下步骤:提供磷光体作为起始材料,将磷光体与至少一种金属氧化物粉末混合以形成混合物,以及对混合物进行加工以形成其中磷光体嵌入陶瓷基体材料中的陶瓷转换器材料。
这样的方法易于实施且成本低。由于将预合成的磷光体用作起始材料中的一者,因此可以将进一步的方法仅视为混合氧化物法。
可以选择用作起始材料的磷光体使得其具有非常高的QE,从而导致当将转换器元件应用于光电装置时,陶瓷转换器元件也具有高的QE和封装转换效率(CQE)。为了这个目的,选择具有非常高的QE的磷光体作为起始材料。由于受控的加工,磷光体及其QE不被损坏,并且可以至少在很大程度上在最终的陶瓷转换器元件中和封装中保持并实现高的QE和/或高的CQE。
例如,对通过混合氧化物方法或共沉淀方法制造的陶瓷转换器元件观察到的最大QE为约90%至95%。在通过如上所述的方法制造的陶瓷转换器元件的情况下,可以获得QE和/或CQE比通过常规方法制造的相应转换器高2%至3%的陶瓷转换器元件。
根据另一个实施方案,磷光体选自掺杂的石榴石、基于氧化物的磷光体、基于氮化物的磷光体、基于氧氮化物的磷光体及其组合。例如,掺杂的石榴石选自用Ce和/或Gd掺杂的YAG或LuAG。用于磷光体的另一些实例为Eu2+掺杂的258-氮化物或Eu3+掺杂的YAG。根据另一个实施方案,磷光体包括掺杂的石榴石。
石榴石应理解为包含选自各种化学元素的特定化学组成的晶体结构类型。在当前情况下,这样的元素可以为例如Y、Gd、Al和O,Ce作为掺杂剂。
本领域技术人员可理解,可以在混合物中同时使用多于一种类型的不同化学组成的磷光体,从而产生多个波长带的转换光用于定制的颜色,例如以特定比例混合的如绿色、黄色、橙色和/或红色的成分。为了产生不同的组合,必须使用不同的磷光体组分材料。
根据另一个实施方案,至少一种金属氧化物粉末选自未掺杂的石榴石、稀土元素(特别地从La至Lu)的氧化物、过渡金属的氧化物、碱金属元素(alkaline elements)的氧化物、碱土金属元素(alkaline earth elements)的氧化物及其组合。例如,金属氧化物粉末包括未掺杂的石榴石或Al2O3。例如,如果将YAG用作被掺杂以形成磷光体的石榴石,则金属氧化物可以选自例如未掺杂的YAG和/或Al2O3。
根据另一个实施方案,磷光体和金属氧化物粉末不含第二相和/或杂质。例如,在YAG作为石榴石的情况下,没有形成不期望的相例如YAM、YAP或Y2O3作为残留的第二相或第三相,使得转换器元件的QE保持为高的。
根据另一个实施方案,掺杂的石榴石包含YAG以及金属氧化物粉末包含YAG和/或Al2O3,或者其中掺杂的石榴石包含LuAG以及金属氧化物粉末包含LuAG和/或Al2O3。在这些材料组合的情况下,可以制造具有高亮度和高QE的陶瓷转换器元件。
根据另一个实施方案,磷光体包含选自镧系元素,特别地选自Ce和/或Gd的掺杂剂。其他镧系元素如Pr、Eu等也是可能的掺杂剂。
根据另一个实施方案,磷光体包括以下晶粒尺寸:d50选自0.5μm≤d50≤40μm的范围以及d90≤45μm。特别地,d50可以选自1μm≤d50≤20μm的范围,以及d90可以选自≤25μm。因此,在该方法中可以使用大晶粒尺寸的磷光体。由于大的晶粒尺寸,例如,磷光体的结晶度和化学组成使得可以实现与细颗粒的情况相比更低的与金属氧化物的反应性以及转换器元件在应用于LED封装时更有利的光学散射性能。
相比之下,用作金属氧化物的YAG或LuAG粉末或者用作金属氧化物的Al2O3粉末可以具有在0.1μm≤d50≤10μm的范围内的d50以及d90≤15μm,优选地0.1μm≤d50≤5μm以及d90≤8μm。
全部起始材料,即掺杂的磷光体和金属氧化物,可以为高活性且可烧结的。磷光体例如YAG:Ce的掺杂水平可以在0.05原子%至6原子%,优选0.1原子%至4原子%,例如0.5原子%至4原子%的范围内。金属氧化物例如YAG或Al2O3的掺杂水平可以在0.0原子%至1原子%,优选0.0原子%至0.02原子%的范围内。用作基体的YAG粉末可以为没有第二相并且纯度超过99.5%的立方晶体。用作基体的Al2O3粉末可以为没有第二相并且纯度超过99.5%的α-Al2O3晶体。预合成的YAG:Ce磷光体可以具有没有第二相的立方晶相。
根据另一个实施方案,磷光体包括至少90%的量子效率QE。优选地,磷光体的量子效率>95%或者甚至等于或大于99%。
根据另一个实施方案,所述方法包括混合的步骤,混合进而可以包括研磨。研磨进行足够长的时间长度以促进良好地混合并包含期望的尺寸范围的良好地堆积的粉末颗粒的良好的生坯显微组织。在研磨之后,浆料和/或粉末颗粒基本上不包含任何团聚体,并且与起始材料(即磷光体和金属氧化物)的颗粒具有相同或相似的尺寸。此外,经研磨的粉末颗粒包括颗粒之间的细且窄分布的空隙尺寸,其中空隙尺寸可以等于或低于晶粒尺寸的水平。
根据另一个实施方案,加工包括向混合物中添加至少一种添加剂以形成浆料,对浆料进行流延成型以形成生坯部例如生坯板,对生坯部进行预烧和/或脱黏(debinding,脱脂)以及烧结以形成陶瓷转换器材料。转换器材料可以形成为任何期望的形状,例如小片或试样块。
根据另一个实施方案,至少一种添加剂可以选自水、粘结剂、消泡剂、分散剂、增塑剂、及其混合物。优选地向混合物中添加水、粘结剂、消泡剂、分散剂和增塑剂。这些添加剂中的一些还是成孔添加剂并混合至混合物足够长的时间以使添加剂散布。例如,根据起始粉末的性能,混合进行6小时至72小时。
根据另一个实施方案,烧结在湿或干氢气气氛中或者在干或湿氢气-氮气气氛中进行。
根据另一个方面,提供了光电组件。组件包括有源层序列和陶瓷转换器元件,所述有源层序列发射第一波长的电磁辐射,所述陶瓷转换器元件施加在有源层序列的光束路径中并将第一波长至少部分地转换成第二波长,其中陶瓷转换器元件包括至少90%,特别地至少95%,特别地至少99%的量子效率。
根据一个实施方案,光电组件包括用根据上述实施方案中的一者的方法制造的陶瓷转换器元件。因此,关于所述方法所公开的所有特征和特性对于光电组件也是有效的,反之亦然。由于陶瓷转换器元件用如上所述的方法制造,光电组件具有高的CQE。
根据另一个实施方案,陶瓷转换器元件包含选自以下的磷光体:Ce和/或Gd掺杂的YAG、Ce和/或Gd掺杂的LuAG、及其混合物。根据另一个实施方案,陶瓷转换器元件包含嵌入选自YAG和Al2O3及其组合的基体中的Ce和/或Gd掺杂的YAG,或者其中陶瓷转换器元件包含嵌入选自LuAG和Al2O3及其组合的基体中的Ce和/或Gd掺杂的LuAG。这样的转换器元件可以为发射黄光的转换器元件或发射绿光的转换器元件。有源层序列可以例如包含InGaN并发射蓝光。
另一个方面是指用根据上述实施方案中的一者的方法制造的陶瓷转换器元件。因此,关于所述方法所公开的所有特征和性能对于陶瓷转换器元件也是有效的,反之亦然。
通过以上方法适当地制备的陶瓷转换器元件可以包括透射率(如总透射率或在线透射率)和QE值的组合使得当封装至LED时其得到更高的CQE值。这还可以通过其散射性能(双向散射分布函数,BSDF;相对于入射光传播从-90度至90度的散射强度的高积分总图)的详细测量来证明。
下面参照附图和示例性实施方案描述另外的实施方案和实施例。
图1示出了光电组件的示意性截面;
图2示出了根据一个示例性实施方案的方法中使用的磷光体的SEM图像;
图3示出了流延带的照片;
图4示出了经烧结的小片的照片;
图5示出了透射率值和反射率值;
图6示出了经烧结的材料的SEM图像;
图7示出了经烧结的材料的光谱;
图8示出了经烧结的材料的转换线;
图9示出了LPWo-B值;
图10示出了转换器元件的示例性实施方案和参照例的光谱;
图11示出了示例性实施方案和参照例的CQE;以及
图12示出了示例性实施方案和参照例的吸收和转换光子测量。
图1示出了光电组件的示意性截面。其包括其上施加有有源层序列10的基底30。在有源层序列10的光束路径中施加陶瓷转换器元件20。有源层序列10和陶瓷转换器元件20可以施加在壳体40中,其中可以在壳体40与有源层序列10之间施加体积铸件50。为了清晰起见,未示出光电组件另外的元件如,例如,电连接件。
陶瓷转换器元件20可以包含例如YAG基体或Al2O3基体中的YAG:(Gd/Ce)磷光体。
陶瓷转换器元件20可以如下制造。
使用高活性并且可烧结的具有没有第二相的立方晶相的预合成的YAG:Ce磷光体作为起始材料,Ce掺杂水平为0.05原子%至6原子%,优选为0.1原子%至4原子%,例如0.5原子%至4原子%;颗粒尺寸分别为:d50为0.5μm至40μm,优选为1μm至20μm,以及d90≤45μm,优选地≤25μm。另外的起始材料为高活性并且可烧结的具有没有第二相的立方晶相并且纯度>99.5%的YAG粉末,Ce掺杂水平为0原子%至1原子%,优选为0原子%至0.02原子%;颗粒尺寸分别为:d50为0.1μm至10μm,优选为0.1μm至5μm,以及d90≤15μm,优选地≤8μm。可替代地,或者除此之外,可以将Al2O3粉末用作具有没有第二相的α-Al2O3晶体的基体并且可以利用如YAG粉末相对应的特性。
表1示出了包含YAG基体中的磷光体(Y0.796Gd0.2Ce0.004)3Al5O12和添加剂的用于流延成型的示例性批料。
表1
WB4101为丙烯酸类粘结剂,DF002为非有机硅消泡剂,PL005为高pH增塑剂。
当将添加剂混合至混合物中时,然后将批料流延、干燥并切割或冲压成期望的尺寸和形状。经烧结的陶瓷转换器元件的期望形状可以包括例如1mm×1mm的尺寸以及70μm至300μm的厚度。根据芯片设计,可以切割掉或者可以不切割掉转换器元件的一个角以提供用于将线接合至LED芯片的顶表面的空间。对于较小的LED芯片,尺寸还可以小至0.5mm2。
可以将生坯板或生坯部放置在氧化铝板上,然后将氧化铝板放置在空气气氛炉中并使用例如以下的时间-温度周期进行加热:25℃至400℃持续4小时,400℃至1150℃持续4小时,在1150℃下保持0.5小时至2小时的时间,以及在3小时内冷却至25℃。
在这样的热处理期间,可以除去含有机碳的物质,包括用于保持粉末的有机粘结剂以及成孔添加剂材料(如果有的话)一起除去。1150℃的保持温度足够高以允许粉末颗粒颈缩在一起,从而赋予部件足够的强度以进行操作。成孔添加剂可以被烧尽,从而根据烧结温度成比例地留下复制其尺寸和形状的空隙。
例如,将预烧的陶瓷小片转移到钼板上,然后例如在湿氢气气氛中在1500℃至1825℃下在峰温度下烧结1分钟至2小时的时间。可替代地,可以在干条件或湿条件下选择氢气-氮气气氛。
在氢烧结期间,随着陶瓷粉末烧结,小片收缩,并且孔隙被除去。如果初始粉末颗粒尺寸适当并采用适当的混合和研磨条件,并且没有向批料中添加成孔添加剂,则基体孔隙将在升高的烧结温度下减小至使最终转换器元件表现出高透明度和半透明的水平。
根据实施例1,以约11.5体积%的含量将Gd/Ce比为0/100以及代替YAG晶体中的Y的约2.2原子%的Ce含量的YAG:(Gd/Ce)磷光体(P)的批料引入到未掺杂的YAG基体(Ml)中。在研磨、添加成孔添加剂(如果是必要的)、流延、干燥并冲压成期望的部件尺寸之后,将部件加热并在热处理之后在从1680℃至1760℃的不同温度下进行烧结。使用激光系统测量由此获得的样品(PM1)的QE。
根据实施例2,以约11.5体积%的含量将Gd/Ce比为0/100以及代替YAG中的Y的约2.2原子%的Ce含量的YAG:(Gd/Ce)磷光体(P)的批料引入到未掺杂的Al2O3基体(M2)中。在如关于实施例1的上述过程并在从1620℃至1760℃的不同温度下进行烧结之后,测量由此获得的样品(PM2)的QE值。
然而,PM1显示出98%的QE以及PM2显示出92%的QE,参照例R2(单相YAG:Ce标准转换器)显示出91%的QE,以及参照例R1(第二相转换器-通过混合氧化物方法制造的Al2O3基体中的YAG:Ce)显示出90%的QE。
根据实施例3,以约7.2体积%的含量将Gd/Ce比为0/100以及代替YAG中的Y的约3原子%的Ce含量的YAG:(Gd/Ce)磷光体(P2)引入到未掺杂的YAG基体(Ml)中。按照如上所述的过程,但是对磷光体进行预研磨并在湿合成气体N2-H2(约3.6体积%)中在从1620℃至1760℃的不同温度下进行烧结,在积分球中在Oslon Black Flat(OBF)封装中测量由此获得的样品P2M1-N2-H2的CQE。典型的CQE数据列于表2中。为了比较,表2中还包括使用通过共沉淀方法制备的磷光体粉末的标准产品作为在相似的Cx值下的参照例。参照例为具有15原子%的Gd和0.2原子%的Ce的掺杂YAG的单相YAG:Ce标准转换器。
根据实施例4,以7.2体积%的含量将Gd/Ce比为0/100以及代替YAG中的Y的约3原子%的Ce含量的YAG:(Gd/Ce)磷光体(P2)的批料引入到未掺杂的YAG基体(Ml)中。按照如上所述的过程,但是对磷光体进行预研磨并在湿H2中在从1620℃至1760℃的不同温度下进行烧结,在球中使用OBF封装测量由此获得的样品P2M1-H2的CQE值。典型的CQE数据列于表2中。表2中还列出了使用来自发射光谱的流明(Lm)除以蓝色芯片光功率(Wo-b)计算的Lm/Wo-b值,以及使用由发射光谱积分的流明(Lm)除以其发射光谱积分的功率(Wvis)计算的LER值。
表2
在下文中,P表示Ce含量为约3原子%以及晶粒尺寸d50为约17μm的YAG:Ce粉末。该磷光体具有大晶粒,良好地结晶并预合成以具有高的QE。P1表示经流延和烧结的磷光体。PM1表示YAG基体中的磷光体,该磷光体的含量为11.5体积%。PM2表示Al2O3基体中的磷光体,其中磷光体的含量为11.5体积%。M1表示经流延和烧结的基体YAG。M2表示经流延和烧结的基体Al2O3。此外,P2M1-H2表示YAG基体中的Ce含量为约3原子%以及d50为约7μm的YAG:Ce磷光体,该磷光体的含量为7.2体积%并在湿氢气气氛中经烧结。相应地,P2M1-N2-H2表示YAG基体中的Ce含量为约3原子%以及d50为约7μm的YAG:Ce磷光体,该磷光体的含量为7.2体积%并在湿氢气氮气气氛中经烧结。
图2示出了未经表面处理且具有约99%的QE和约17μm的d50的磷光体P的SEM图像。该磷光体的色点适用于例如照明灯颜色盒。在本基体方法中,粒径d50对于陶瓷加工不理想。图2b是图2a的放大。
虽然难以控制磷光体P的浆料流变性,但即使大晶粒的标准粘结剂水平太高并且胶体分散困难,也仍然能够流延成型。样品PM2更好地进行流延成型。纯磷光体样品P1,尤其是尺寸为约25mm×25mm且厚度为约120μm时,经常翘曲,这归因于在流延过程期间的颗粒沉降,但样品PM1和PM2显示出较低的翘曲。流延成型样品P1和PM2通过照片示于图3a(P1)、图3b(P1)和图3c(PM2)中。
图4示出了样品PM1、PM2、P1、M1和M2的经烧结的部分的照片。可以看出YAG样品PM1和M1分别表现出比Al2O3样品PM2和M2更高的透明度。
图5a示出了经烧结的样品PM1、PM2、P1、M1和M2的取决于波长λ(nm)的透射率值T(%),图5b示出了相同样品在300nm至800nm的波长范围内的取决于波长λ(nm)的反射率值Ref(%)。
表3总结了样品P、P1、PM1、PM2、Ml和M2(其全部均在1720℃下经烧结)、以及参照样品R1(通过常规的第二相方法(即用额外的Al2O3作为基体的混合氧化物法)制造的第二相样品)和R2(如上下文中用表2描述的单相样品)的吸收ABS和透射率T的值,通过激光球测量QE和吸收。
表3
图6a至6e示出了样品PM1(图6a)、PM2(图6b)、P1(图6c)、M1(图6d)和M2(图6e)的显微组织的SEM图像,其全部均在1720℃下经烧结。在图6a中,可以观察到具有一些BaAl2O4相的开始扩大的晶粒生长(EGG)。同样,在样品PM2中,可以在表面(图6b,左)处和裂纹(图6b,右)中观察到晶粒中具有孔的氧化铝的大晶粒和BaAl2O4。样品P1烧结不良,并在其表面(图6c,右)上和遍及整个块体(图6c中的裂纹,左)中具有含BaAl2O4和CeO2相的大晶粒尺寸。如在图6d中可以看出,基体M1具有较小的晶粒尺寸,图6e中所示的基体M2具有扩大的晶粒生长和晶粒内部的孔。
图7a和图7b示出了与蓝色LED相比基体M1、M2、样品PM1、PM2以及磷光体P1和P的光谱(图7a示出了取决于波长λ(nm)的强度I(mw/nm)以及图7b示出了取决于波长λ(nm)的归一化强度Inorm)。在球中使用LED上的1mm×1mm×0.1mm陶瓷磷光体元件进行测量。可以看出PM1的强度高于PM2的强度,PM2的强度高于P1的强度。P1显示出非常低的蓝色透射率,并且可以在纯基体M1中观察到一些Ce污染。此外,在样品M1中可以看到相当高的蓝色透射率,可以在样品M2中看到稍低的蓝色透射率。与蓝色LED相比,可以识别出没有光谱偏移。此外,如图7b中可以看出,由于烧结不良,在具有高散射的样品P1中,作为Ce再吸收的红移最大。
可以表明样品P(因此为YAG:Ce粉末)具有在激光球(Lab 30)中测量的99%的非常高的QE。但是仅用P制成的陶瓷不能保持其高的QE值,而是显示出88%的降低的值,可能是由于不良烧结行为和/或BaAl2O4相和CeO2相的出现。样品PM1在LED上显示出98%的高QE和高流明。样品PM2具有92%的QE和降低的流明,但仍然比通过氧化物方法的常规的Al2O3中的YAG:Ce(即,由Y2O3、Al2O3、CeO2等的混合物形成的YAG:Ce磷光体)和标准产品单相陶瓷转换器的QE(90%和91%)更高。Ml的透射率高于M2中的透射率,因此样品PM1显示出比样品PM2更高的透射率。未掺杂的YAG陶瓷Ml表现出弱发射,这归因于来自浆料加工或来自烧结炉的Ce污染。
在下文中,检验气氛对材料烧结的影响。在此,磷光体为掺杂有Ce(约3%)的YAG磷光体,其具有高QE和约7μm的d50,具有团聚体并指定为P2。基体为YAG基体,并且磷光体在基体中的含量为7.2体积%。烧结在两种气氛中进行。标准为5lpm(升/分钟)湿H2(0℃露点)。将由此烧结的样品指定为P2M1-H2。另一个气氛为8lpm N2,和<0.3lpm湿H2(0℃露点),其中H2的量为约1.5%至3%。将这些样品指定为P2M1-N2-H2。
图8示出了参照样品Rl、R2以及样品P2M1-N2-H2和P2M1-H2的转换线(坐标Cy取决于坐标Cx)。图8a示出了在OT(内部设计的针孔球测量系统)上的测量结果,图8b示出了在干LED(内部设计系统但在球系统中在LED芯片上放置有陶瓷转换器)上的测量结果。经烧结的小片的转换线接近参照例,具有轻微的绿移。
图9示出了样品P2M1-H2和P2M1-N2-H2在相似的色点Cx下,具有比参照样品R1更高的LPWo-b,Lm/Wo-b使用发射光谱的流明(Lumens)除以蓝色芯片光功率(Wo-b)来定义和计算。
图10示出了在球中在LED(没有胶)上记录的光谱。测量样品P2M1-H2和P2M1-N2-H2,并将取决于波长λ(nm)的其强度I与适光曲线(PC)进行比较,该适光曲线是在CIE 1931色空间中使用的CIE标准曲线。光源中的光通量(或可见光功率)由适光的光度函数定义。可以表明,在N2-H2中烧结的样品相对于H2中烧结的样品仅存在微小的光谱偏移。适光曲线仅提供参照。
样品P2M1-H2和P2M1-N2-H2的数据分析表明P2M1-N2-H2的CQE比参照例R2高1%,以及比样品P2M1-H2中的高0.7%。
这也显示在图11中,其中样品P2M1-N2-H2的取决于Cx的CQE最高,其比参照例R2高1%,并且合成气体的情况比标准湿氢烧结的情况的CQE高。通常,可以表明合成气体的情况的CQE比仅在湿氢中的情况的CQE在统计学上更高,并且具有YAG基体的材料的CQE也比参照例R2的CQE在统计学上更高。
图12示出了在H2和N2-H2中烧结的不同样品以及参照样品R2的取决于Cx的蓝色吸收(蓝色abs)和转换光子(conv)的测量(图12a)。可以表明,由于较高的发射与蓝色透射比率,因此辐射的发光效率(LER)随着Cx线性增加(图12b)。在N2-H2中烧结的基体材料显示出更大的蓝色吸收和更多的转换光子,从而导致更低的泵通过(pump-through)百分比和更高的转换百分比。观察到的更高的CQE不是由色移引起的。
本发明的保护范围不限于上文中给出的实施例。本发明体现在各个新颖的特征和该特征的各个组合中,其特别地包括权利要求中所述的任何特征的每种组合,即使该特征或特征的组合没有在权利要求或实施例中明确指出。
本专利申请要求美国专利申请16/198,108的优先权,其公开内容通过引用并入本文。
附图标记
10 有源层序列
20 陶瓷转换器元件
30 基底
40 壳体
50 体积铸件
P YAG:Ce磷光体粉末
P1 YAG:Ce磷光体粉末,经流延和烧结
P2 YAG:Ce磷光体粉末
PM1 YAG基体中的YAG:Ce
PM2 Al2O3基体中的YAG:Ce
Ml YAG基体
M2 Al2O3基体
P2M1-H2 YAG基体中的YAG:Ce,在湿氢中烧结
P2M1-N2-H2 YAG基体中的YAG:Ce,在氮和湿氢中烧结
R1至R2 参照样品
PC 适光曲线
Claims (18)
1.一种用于制造陶瓷转换器元件(20)的方法,包括以下步骤:
-提供磷光体作为起始材料,
-将所述磷光体与至少一种金属氧化物粉末混合以形成混合物,
-对所述混合物进行加工以形成其中所述磷光体嵌入陶瓷基体材料中的陶瓷转换器材料。
2.根据权利要求1所述的方法,其中所述磷光体选自掺杂的石榴石、基于氧化物的磷光体、基于氮化物的磷光体、基于氧氮化物的磷光体及其组合。
3.根据权利要求1所述的方法,其中所述磷光体包括掺杂的石榴石。
4.根据前述权利要求中的一项所述的方法,其中所述至少一种金属氧化物粉末选自未掺杂的石榴石、稀土元素的氧化物、过渡金属的氧化物、碱金属元素的氧化物、碱土金属元素的氧化物及其组合。
5.根据前述权利要求中的一项所述的方法,其中所述磷光体和所述金属氧化物粉末不含第二相和/或杂质。
6.根据权利要求3所述的方法,其中所述掺杂的石榴石包含YAG以及所述金属氧化物粉末包含YAG和/或Al2O3,或者其中所述掺杂的石榴石包含LuAG以及所述金属氧化物粉末包含LuAG和/或Al2O3。
7.根据前述权利要求中的一项所述的方法,其中所述磷光体包含选自镧系元素,特别地选自Ce和/或Gd的掺杂剂。
8.根据前述权利要求中的一项所述的方法,其中所述磷光体包括以下晶粒尺寸:d50选自0.5μm≤d50≤40μm的范围以及d90≤45μm。
9.根据前述权利要求中的一项所述的方法,其中所述磷光体包括至少90%的量子效率QE。
10.根据前述权利要求中的一项所述的方法,其中所述混合包括研磨。
11.根据前述权利要求中的一项所述的方法,其中所述加工包括向所述混合物中添加至少一种添加剂以形成浆料,对所述浆料进行流延成型以形成生坯部,对所述生坯部进行预烧和/或脱黏以及烧结以形成所述陶瓷转换器材料。
12.根据权利要求11所述的方法,其中所述烧结在湿或干氢气气氛中或者在干或湿氢气-氮气气氛中进行。
13.根据权利要求11和12中的一项所述的方法,其中所述至少一种添加剂选自水、粘结剂、消泡剂、分散剂、增塑剂、及其混合物。
14.一种光电组件,包括
有源层序列(10),所述有源层序列(10)发射第一波长的电磁辐射,以及
陶瓷转换器元件(20),所述陶瓷转换器元件(20)施加在所述有源层序列(10)的光束路径中并将所述第一波长至少部分地转换成第二波长,
其中,
所述陶瓷转换器元件(20)包括至少90%的量子效率。
15.根据权利要求14所述的光电组件,其中所述陶瓷转换器元件(20)用根据前述权利要求1至13中的一项所述的方法来制造。
16.根据权利要求14和15中的一项所述的光电组件,其中所述陶瓷转换器元件(20)包含选自以下的磷光体:Ce和/或Gd掺杂的YAG、Ce和/或Gd掺杂的LuAG、及其混合物。
17.根据权利要求14至16中的一项所述的光电组件,其中所述陶瓷转换器元件(20)包含嵌入选自YAG和Al2O3及其组合的基体中的Ce和/或Gd掺杂的YAG,或者其中所述陶瓷转换器元件包含嵌入选自LuAG和Al2O3及其组合的基体中的Ce和/或Gd掺杂的LuAG。
18.一种用根据权利要求1至13中的一项所述的方法制造的陶瓷转换器元件(20)。
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