CN113024252A - 白光激光照明用多级孔结构陶瓷荧光体及其制备方法 - Google Patents
白光激光照明用多级孔结构陶瓷荧光体及其制备方法 Download PDFInfo
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Abstract
本发明公开白光激光照明用多级孔结构陶瓷荧光体及制备方法，所述陶瓷荧光体的化学组成为(CexReyY1‑x‑y)3Al5O12，其中，Re为Lu、Tb、Gd中的一种或多种，x、y的取值范围为：0.001≤x≤0.05，0≤y≤0.5；所述陶瓷荧光体的内部分布有一级孔和二级孔，所述一级孔为球形气孔，孔径≤3μm，所述二级孔为多面体气孔，孔径≤5μm。本发明的有益效果在于：具有显著提高的光通量和良好的均匀出光。
Description
技术领域
本发明涉及白光激光照明用多级孔结构陶瓷荧光体及其制备方法。
背景技术
激光照明的技术主流是以半导体激光器为核心光源，采用蓝色激光激发荧光体转换成其他波长的光，进而得到高亮白光照明。白光激光照明除了需要具备白光LED照明光源的发光效率和光生物安全等一般要求以外，还要能够充分实现激光照明的高亮高光效的优势。因此，激光照明对荧光体具有特殊性能指标要求，在多颗激光器（LD）共同汇聚的高辐照功率密度下，荧光体需具备优异的耐蓝光辐照能力、猝灭特性和热稳定性，在光转换过程中保持稳定的高光效。目前，YAG基荧光陶瓷以其优异的机械性能、高光效及热稳定性，成为激光照明优选的荧光体材料。对于给定化学组成的YAG基荧光陶瓷来说，其荧光性能很大程度上取决于其微观结构，尤其是气孔的存在，会直接影响光在其中的散射和传播，进而影响荧光性能。
在荧光陶瓷烧结过程中，由于粉体的团聚作用、粒径分布以及烧结制度的共同影响，在陶瓷中会残留一部分气孔。在激光照明过程中，陶瓷气孔通过散射来自激光器的入射蓝光和陶瓷转换的黄光可以有效的调节陶瓷内部光的散射和吸收过程，对于增强陶瓷荧光体的光吸收、光提取以及均匀混光具有重要意义。这类似于传统LED灯具中“粉+胶”模式，利用荧光粉颗粒和有机材料的折射率不同实现光的散射。然而气孔率过高会导致蓝光在陶瓷内部不断地被散射和再吸收而无法实现光出射，导致蓝光成分的缺失，引起整体光效的降低。
中国发明专利申请CN109467453A的专利中采用造孔剂制备了含不规则微孔结构的荧光陶瓷，但是由于造孔剂参与高温烧结过程，不可避免的在陶瓷荧光体内部形成杂质缺陷，对转换效率造成负面影响。此外，不规则微孔结构虽然能够调节陶瓷荧光体内部光的散射和吸收，但是在高辐照功率密度下，容易聚集局部热应力，导致荧光体在使用过程中发生猝灭或损坏，在实际应用中受到限制。
发明内容
本发明目的是解决现有技术中的问题，而提供新型的白光激光照明用多级孔结构陶瓷荧光体及其制备方法。
为了实现这一目的，本发明的技术方案如下：白光激光照明用多级孔结构陶瓷荧光体，所述陶瓷荧光体的化学组成为(CexReyY1-x-y)3Al5O12，其中，Re为Lu、Tb、Gd中的一种或多种，x、y的取值范围为：0.001≤x≤0.05，0≤y≤0.5；所述陶瓷荧光体的内部分布有一级孔和二级孔，所述一级孔为球形气孔，孔径≤3μm，所述二级孔为多面体气孔，孔径≤5μm。
作为白光激光照明用多级孔结构陶瓷荧光体的优选方案，所述陶瓷荧光体的激发光的波长范围为420-500nm，在所述激发光的激发下形成的发射光的波长范围为450-750nm。
作为白光激光照明用多级孔结构陶瓷荧光体的优选方案，所述陶瓷荧光体的上表面附着BLUE PASS增透膜，下表面附着金属反射层，并焊接在铜质散热基座中；优选的金属反射层是铝膜、银膜中的一种。
本发明还提供白光激光照明用多级孔结构陶瓷荧光体的制备方法，用于制备陶瓷荧光体，包含有以下步骤，
步骤S1，制备浆料：根据化学组成为(CexReyY1-x-y)3Al5O12计量比采用水热法制备YAG基荧光粉体，其中，Re为Lu、Tb、Gd、Ga中的一种或多种，x、y的取值范围为：0.001≤x≤0.05，0≤y≤0.5；将所述YAG基荧光粉体、材料A以及材料B混合，制得均匀分散的浆料，其中，所述材料A选自聚苯乙烯、聚丙烯中至少一种材质的有机微球，颗粒尺寸≤5μm，质量占比为0-20%；所述材料B选自去离子水、有机溶液中的至少一种；
步骤S2，浆料注入模具，在-5至-100℃温度范围内凝固成型，待所述浆料完全冷冻后进行冷冻干燥，得到块体原片；
步骤S3，将所述块体原片经冷等静压，制得荧光体素坯；以及，
步骤S4，将所述荧光体素坯经阶梯法烧结制备得到所述陶瓷荧光体。
作为白光激光照明用多级孔结构陶瓷荧光体的制备方法的优选方案，步骤S4中，阶梯烧结法包含两个烧结阶段：第一阶段，在600℃-1300℃的条件下煅烧4-10小时进行脱脂和预烧处理；第二阶段，在1000℃-1800℃进行热等静压烧结，进行致密化处理。
与现有技术相比，本发明的有益效果至少在于：具有显著提高的光通量和良好的均匀出光，经表面增透膜和底部散热基座组成的发光装置可以满足高功率白光激光照明应用领域。
附图说明
图1为本发明的多级孔结构陶瓷荧光体断面的扫描电镜照片，大孔-介孔级球形气孔在陶瓷晶界处分散均匀，尺寸范围为0.1-3μm。
图2为本发明的多级孔结构陶瓷荧光体的内部结构及其激光转换发光示意图，4颗蓝光激光器激发下光通量≥1.5klm。
具体实施方式
下面通过具体的实施方式连接附图对本发明作进一步详细说明。在此需要说明的是，对于这些实施方式的说明用于帮助理解本发明，但不构成对本发明的限定。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。
实施例1：
以Y2O3、Tb7O4、CeO2和Al(NO3)3•9H2O为原料配成硝酸盐溶液，根据(Ce0.01Tb0.20Y0.79)3Al5O12化学计量比混合相应硝酸盐溶液，采用水热法经120℃保温10h合成粒径在50-200nm范围的YAG基荧光粉体。将YAG基荧光粉体、商用聚苯乙烯微球（粒径≤5μm）以及无水乙醇按质量占比45%：5%：50%进行配比，然后添加一定量的分散剂作为添加剂，在三维混料机中制备混合均匀的浆料。将所述浆料注入模具，在-5至-100℃温度场范围内低温凝固成型，待浆料完全冷冻后进行冷冻干燥，得到YAG基荧光粉体与聚苯乙烯微球均匀分布的块体原片；将所述原片经冷等静压制得素坯；将所述素坯经阶梯法烧结制得多级孔陶瓷荧光体，其中一级孔为球形气孔，孔径小于等于0.5μm-3μm；所述二级孔为多面体气孔，孔径为1μm-5μm；其中陶瓷晶粒尺寸为15μm-35μm。
将多级孔陶瓷荧光体的上下表面分别镀蓝光增透膜和反射膜，并焊接在铜质散热基座中。利用4颗激光二极管（单颗额定功率4W，发射波长455nm）作为蓝光激发光源，蓝光激发陶瓷荧光体发射黄光，可获得1.87 klm以上的稳定光通量，满足高流明白光激光照明应用。
实施例2：
以Y2O3、Tb7O4、CeO2和Al(NO3)3•9H2O为原料配成硝酸盐溶液，根据(Ce0.02Tb0.30Y0.68)3Al5O12化学计量比混合相应硝酸盐溶液，采用水热法经120℃保温10h合成粒径在50-200nm范围的YAG基荧光粉体。将YAG基荧光粉体、商用聚苯乙烯微球（粒径≤5μm）以及无水乙醇按质量占比40%：10%：50%进行配比，然后添加一定量的分散剂作为添加剂，在三维混料机中制备混合均匀的浆料。将所述浆料注入模具，在-5至-100℃温度场范围内低温凝固成型，待浆料完全冷冻后进行冷冻干燥，得到YAG基荧光粉体与聚苯乙烯微球均匀分布的块体原片；将所述原片经冷等静压制得素坯；将所述素坯经阶梯法烧结制得多级孔陶瓷荧光体，其中一级孔为球形气孔，孔径小于等于0.5μm-3μm；所述二级孔为多面体气孔，孔径为1μm-5μm；其中陶瓷晶粒尺寸为15μm-35μm。
将多级孔陶瓷荧光体的上下表面分别镀蓝光增透膜和反射膜，并焊接在铜质散热基座中。利用4颗激光二极管（单颗额定功率4W，发射波长455nm）作为蓝光激发光源，蓝光激发陶瓷荧光体发射黄光，可获得1.91 klm以上的稳定光通量，满足高流明白光激光照明应用。
以上仅表达了本发明的实施方式，其描述较为具体和详细，但且不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。
Claims (5)
1.白光激光照明用多级孔结构陶瓷荧光体，其特征在于，所述陶瓷荧光体的化学组成为(CexReyY1-x-y)3Al5O12，其中，Re为Lu、Tb、Gd中的一种或多种，x、y的取值范围为：0.001≤x≤0.05，0≤y≤0.5；所述陶瓷荧光体的内部分布有一级孔和二级孔，所述一级孔为球形气孔，孔径≤3μm，所述二级孔为多面体气孔，孔径≤5μm。
2.根据权利要求1所述的白光激光照明用多级孔结构陶瓷荧光体，其特征在于，所述陶瓷荧光体的激发光的波长范围为420-500nm，在所述激发光的激发下形成的发射光的波长范围为450-750nm。
3.根据权利要求1或2所述的白光激光照明用多级孔结构陶瓷荧光体，其特征在于，所述陶瓷荧光体的上表面附着BLUE PASS增透膜，所述陶瓷荧光体的下表面附着金属反射层，并焊接在铜质散热基座中；优选的金属反射层是铝膜、银膜中的一种。
4.白光激光照明用多级孔结构陶瓷荧光体的制备方法，其用于制备权利要求1至3中任意一项的陶瓷荧光体，其特征在于，包含有以下步骤，
步骤S1，制备浆料：根据化学组成为(CexReyY1-x-y)3Al5O12计量比采用水热法制备YAG基荧光粉体，其中，Re为Lu、Tb、Gd、Ga中的一种或多种，x、y的取值范围为：0.001≤x≤0.05，0≤y≤0.5；将所述YAG基荧光粉体、材料A以及材料B混合，制得均匀分散的浆料，其中，所述材料A选自聚苯乙烯、聚丙烯中至少一种材质的有机微球，颗粒尺寸≤5μm，质量占比为0-20%；所述材料B选自去离子水、有机溶液中的至少一种；
步骤S2，浆料注入模具，在-5至-100℃温度范围内凝固成型，待所述浆料完全冷冻后进行冷冻干燥，得到块体原片；
步骤S3，将所述块体原片经冷等静压，制得荧光体素坯；以及，
步骤S4，将所述荧光体素坯经阶梯法烧结制备得到所述陶瓷荧光体。
5.根据权利要求4所述的白光激光照明用多级孔结构陶瓷荧光体的制备方法，其特征在于，步骤S4中，阶梯烧结法包含两个烧结阶段：第一阶段，在600℃-1300℃的条件下煅烧4-10小时进行脱脂和预烧处理；第二阶段，在1000℃-1800℃进行热等静压烧结，进行致密化处理。
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