CN112624752A - 一种复合荧光陶瓷及高亮度led照明光源 - Google Patents
一种复合荧光陶瓷及高亮度led照明光源 Download PDFInfo
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- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 claims abstract description 9
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Abstract
本发明提供一种复合荧光陶瓷器件及高亮度LED照明光源，所述复合荧光陶瓷由荧光陶瓷片和无发光陶瓷片组成，所述荧光陶瓷片的化学式为(Y1‑xCex)3Al5O12，x=0.001~0.01；所述无发光陶瓷片为YAG透明陶瓷，化学式为Y3Al5O12。本发明的有益效果在于：采用体系匹配的YAG材料来封装荧光陶瓷，并通过控制烧结温度来实现两者之间的完美烧结，有效实现荧光陶瓷的热量向无发光陶瓷进行传导，运行温度低，发光效率高。
Description
技术领域
本发明涉及LED照明领域，尤其涉及一种复合荧光陶瓷及高亮度LED照明光源设计。
背景技术
当前，LED芯片集成技术越来越成熟，蓝光功率密度超过1~2W/mm2已成必然趋势。然而，光转换材料吸收的能量产生的越多，随之产生的热量也增多，对于光转换材料提出了更高的标准。
一般，光转换材料的热量产生途径有两种：1) 光转换材料斯托克斯损失：发光离子吸收能量从基态跃迁到激发态后，内转换和振动弛豫到激发态的最低能级产生无辐射跃迁，发光光子能量降低，光谱向长波方向移动；2) 光转换材料温度猝灭的“恶性循环效应”：蓝光能量密度过高，光转换材料内部产生热量较快，温度急速上升，导致其量子效率（光转换效率）会急剧下降，当温度超过一定阈值后（约300℃）将下降至30%；这意味着产生的更多热量，反过来引起器件温度继续升高，进而带来永久性破坏。例如，在采用荧光粉作为光转换材料时，超过0.2 W/mm2的蓝光激发下，温度瞬间由198℃升高到549℃，远远超过荧光粉正常运行温度(<200℃)，发光严重猝灭并伴随碳化现象。因此，良好的散热设计和相关装置对保障光转换材料的正常运行（运行温度<150℃）尤其重要。
在光转换材料中，荧光陶瓷具有极高的热导率，导热性好，且发光性能优异，被认为是最佳的高亮度照明材料。一般的，荧光陶瓷散热的方式有两种方案：一种是将小尺寸荧光陶瓷直接贴合在芯片表面，通过芯片来导热；另一种方式是采用大尺寸荧光陶瓷片，通过自身和基底导热。两者均存在一定的问题。前者在高功率密度时，热累积太大，仅靠向芯片导热效率很低（芯片自身也会产生热量），会达到荧光陶瓷的热猝灭温度，瞬间死灯；后者不利于获得高的光学拓展量，提高光束整形难度，高亮度光源。一种新的技术方案，即多个荧光陶瓷组合方案，有利于陶瓷的散热和发光。例如，专利CN111285680A提出了一种包边结构的荧光陶瓷器件：将荧光陶瓷与非发光陶瓷分别烧结，随后组合在一起，应用在激光照明系统。但要维持荧光陶瓷稳定运行，仍需要给补充额外的散热装置；另一方面，两步烧结工艺复杂，且实现包边圆弧与圆片紧密贴合存在一定的困难，导致荧光陶瓷热量很难传导和辐射出去。因此，综合来看，需要新的组合和烧结方案，既可实现小尺寸、高亮度荧光陶瓷器件，又可实现其稳定运行。
发明内容
本发明针对现有技术存在的问题，提出一种发光陶瓷与非发光陶瓷叠层的荧光陶瓷器件及其照明光源。
为实现上述目的，本发明采用的技术方案如下：
一种复合荧光陶瓷器件，由荧光陶瓷片和无发光陶瓷片组成，上表层为荧光陶瓷片，下表层为无发光陶瓷片。
优选的，所述荧光陶瓷片的化学式为(Y1-xCex)3Al5O12，x=0.001~0.01；所述无发光陶瓷片为YAG透明陶瓷，化学式为Y3Al5O12。
优选的，所述荧光陶瓷片的尺寸为3*3 mm，厚度为0.5~1.0 mm；所述无发光陶瓷的尺寸为20*20 mm，厚度为0.5~1.0 mm。
本发明提供一种复合荧光陶瓷器件的制备方法，实现荧光陶瓷与无发光陶瓷的组合，包含有以下步骤：
步骤1: 按照荧光陶瓷片和无发光陶瓷片的化学计量比，并分别加入0.1~1.0wt.%的TEOS，分别配出两种混合粉体，即荧光陶瓷和无发光陶瓷粉体；
步骤2：以无水乙醇作为溶剂，氧化铝球作为球磨介质，分别进行球磨；球磨时间为20~24h；球磨转速为150~170 r/min；
步骤3：将两组浆料进行烘干，烘干条件为40~60℃，时间6 h；
步骤4：将粉体过筛，过筛目数为100~200；
步骤5：压片，模具大小为24*24 mm；首先将荧光陶瓷粉体进行压片处理，压力4~20Mpa，保压1 min；其次将无发光陶瓷粉体进行压片, 压力4~20Mpa，保压1 min；最终将两个方片组合压片，压力4~20 Mpa，保压2 min，获得陶瓷素坯。
步骤6：将压片后的素坯进行冷等静压，压强为200~250 MPa，保压时间为5 min。
步骤7：预烧，烧结温度为800~1000℃，保温12h；
步骤8：真空烧结，烧结制温度为1700~1780℃，保温12h，自然冷却。
步骤9：退火，烧结温度为1350~1450℃，保温12h；
步骤10：裁剪，将荧光陶瓷层切割成3*3 mm。
步骤11：抛光，将无发光陶瓷表面抛光，得所述复合荧光陶瓷器件。
本发明还提供一种基于复合荧光陶瓷器件的高亮度LED照明光源，包含发光透镜、荧光陶瓷片、无发光陶瓷片、硅胶、LED芯片、散热基底；其中，所述散热基底上设有无发光陶瓷片，所述无发光陶瓷片与散热基底紧密贴合并形成第一容置空间；所述第一容置空间内设有LED芯片，所述LED芯片与无发光陶瓷片之间还设有硅胶；所述无发光陶瓷片上设有发光透镜，与所述发光透镜形成第二容置空间，所述荧光陶瓷片位于所述第二容置空间内。
优选的，所述荧光陶瓷的发光效率为200~300 lm/W，色温为3500~7000 K。
优选的，所述硅胶在400~800nm的透明度为80%~95%，折射率为1.45~1.56。
优选的，所述LED芯片的尺寸为2.5*2.5 mm，发射波长为435~460 nm，最大蓝光输出功率为9~12 W。
优选的，所述散热基底的材质为紫铜或铝。
与现有技术相比，本发明具有以下有益效果：
1. 本发明的荧光陶瓷的尺寸仅有3*3 mm，相比目前的大尺寸荧光陶瓷器件（φ>10 mm）具有更小的发光面积，亮度更高，光整形难度更低。同时，3*3 mm的尺寸极好的匹配蓝光LED芯片尺寸（2.5*2.5 mm），混光和照明效果更加优异。
2. 包边结构的复合陶瓷器件，在素坯阶段，荧光陶瓷与无发光陶瓷之间的结合性有待考验，预计烧结后会出现开裂现象；而叠层的复合陶瓷器件通过三次压片处理后，可实现两者紧密贴合，烧结后未存在开裂和脱落现象。
3. 上下叠层的复合荧光陶瓷器件一般为了获得高显色指数（>80）照明光源而进行不同体系陶瓷的组合；本发明创新性的采用体系匹配的YAG材料来封装荧光陶瓷，并通过控制烧结温度来实现两者之间的完美烧结，有效实现荧光陶瓷的热量向无发光陶瓷进行传导。
4. 本发明的无发光荧光陶瓷的尺寸为20*20 mm，相比包边结构的复合荧光陶瓷器件，与散热基底的基础面积更大，散热速率更快，更好的适应10W以上蓝光LED芯片的激发，使其运行在较低温度下（<100℃），并能够获得较高发光效率（维持200lm/W以上）。
5. 优化了荧光陶瓷抛光方案，即陶瓷单面抛光，相比目前荧光陶瓷采用双面抛光的方案，出光效果更加均匀，出光效率更高。
附图说明：
图1 一种基于复合荧光陶瓷器件的高亮度LED照明光源示意图；
图中：10发光透镜、20荧光陶瓷片、30无发光陶瓷片、40硅胶、50 LED芯片、60散热基底。
具体实施方式
下面通过具体的实施方式并结合附图作进一步说明。
实施例1
一种复合荧光陶瓷器件，如图1所示，上表层为荧光陶瓷片20，下表层为无发光陶瓷片30。
按照Ce掺杂浓度为0.1 at.% 和Ce掺杂浓度为0.0 at.%（无掺杂）的YAG荧光陶瓷进行配料，均加入1.0 wt.%的TEOS，配出两种混合粉体。
以无水乙醇作为溶剂，氧化铝球作为球磨介质，分别进行球磨；球磨时间为20 h；球磨转速为150 r/min。
球磨后，将两组浆料进行烘干，烘干条件为40℃，时间6 h。
将粉体过筛，过筛目数为100。
用大小为24*24 mm模具对粉体进行成型：首先将荧光陶瓷粉体进行压片处理，压力4 Mpa，保压1 min；其次将无发光陶瓷粉体进行压片，压力4 Mpa，保压1 min；最终将两个方片组合压片，压力4 Mpa，保压2 min。
通过真空塑封机进行真空包装，在200Mpa的压强下保压5min进行二次成型，得到复合陶瓷素坯。
将素坯进行预烧，烧结温度为1000℃，保温12h，去除有机物。
将素坯进行真空烧结，烧结制温度为1700℃，保温12h，随后自然冷却。
对复合陶瓷进行退火处理，烧结温度为1350℃，保温12h。
退火后，荧光陶瓷器件的尺寸为20*20 mm。将荧光陶瓷层切割为尺寸3*3 mm，厚度打磨为0.5mm；对无发光陶瓷进行抛光，最终厚度为0.5mm。
对复合荧光陶瓷器件进行封装，如图1所示，包含发光透镜10、荧光陶瓷片20、无发光陶瓷片30、硅胶40、LED芯片50、散热基底60；其中，所述散热基底60上设有无发光陶瓷片30，所述无发光陶瓷片30与散热基底60紧密贴合并形成第一容置空间；所述第一容置空间内设有LED芯50片，所述LED芯片50与无发光陶瓷片30之间还设有硅胶40；所述无发光陶瓷片30上设有发光透镜10，与所述发光透镜10形成第二容置空间，所述荧光陶瓷片20位于所述第二容置空间内。
其中，发光透镜10底部放置荧光陶瓷片20，荧光陶瓷片20与无发光陶瓷片30通过烧结贴合在一起，无发光陶瓷片30与散热基底60紧密贴合，散热基底60内部放置LED芯片50，LED芯片50与无发光陶瓷片30中间设有硅胶40。
采用的硅胶40在400~800nm的透明度为80%，折射率为1.45；LED芯片50的尺寸为2.5*2.5mm，发射波长为435nm；散热基底60的材质为紫铜。当LED芯片50的输出功率为9 W时，荧光陶瓷片20稳定发光：其运行温度为80℃；发光效率为200 lm/W；光通量高达1800lm；色温为7000 K。
实施例2
一种复合荧光陶瓷器件，上表层为荧光陶瓷片20，下表层为无发光陶瓷片30。
按照Ce掺杂浓度为1.0 at.% 和Ce掺杂浓度为0.0 at.%（无掺杂）的YAG荧光陶瓷进行配料，均加入0.1 wt.%的TEOS，配出两种混合粉体。
以无水乙醇作为溶剂，氧化铝球作为球磨介质，分别进行球磨；球磨时间为24 h；球磨转速为170 r/min。
球磨后，将两组浆料进行烘干，烘干条件为60℃，时间6 h。
将粉体过筛，过筛目数为200。
用大小为24*24 mm模具对粉体进行成型：首先将荧光陶瓷粉体进行压片处理，压力20 Mpa，保压1 min；其次将无发光陶瓷粉体进行压片，压力20 Mpa，保压1 min；最终将两个方片组合压片，压力20 Mpa，保压2 min。
通过真空塑封机进行真空包装，在250 Mpa的压强下保压5 min进行二次成型，得到复合陶瓷素坯。
将素坯进行预烧，烧结温度为800℃，保温12h，去除有机物。
将素坯进行真空烧结，烧结制温度为1780℃，保温12h，随后自然冷却。
对复合陶瓷进行退火处理，烧结温度为1450℃，保温12h。
退火后，荧光陶瓷器件的尺寸为20*20 mm。将荧光陶瓷层切割为尺寸3*3 mm，厚度打磨为1.0 mm；对无发光陶瓷进行抛光，最终厚度为1.0 mm。
对复合荧光陶瓷器件进行封装，包含发光透镜10、荧光陶瓷片20、无发光陶瓷片30、硅胶40、LED芯片50、散热基底60；其中，所述散热基底60上设有无发光陶瓷片30，所述无发光陶瓷片30与散热基底60紧密贴合并形成第一容置空间；所述第一容置空间内设有LED芯50片，所述LED芯片50与无发光陶瓷片30之间还设有硅胶40；所述无发光陶瓷片30上设有发光透镜10，与所述发光透镜10形成第二容置空间，所述荧光陶瓷片20位于所述第二容置空间内。
采用的硅胶40在400~800nm的透明度为95%，折射率为1.56；LED芯片50的尺寸为2.5*2.5mm，发射波长为460 nm；散热基底60的材质为铝。当LED芯片50的输出功率为12 W时，荧光陶瓷片20稳定发光：其运行温度为79℃；发光效率为300 lm/W；光通量高达3600lm；色温为3500 K。
实施例3
一种复合荧光陶瓷器件，上表层为荧光陶瓷片20，下表层为无发光陶瓷片30。
按照Ce掺杂浓度为0.5 at.% 和Ce掺杂浓度为0.0 at.%（无掺杂）的YAG荧光陶瓷进行配料，均加入0.1 wt.%的TEOS，配出两种混合粉体。
以无水乙醇作为溶剂，氧化铝球作为球磨介质，分别进行球磨；球磨时间为24 h；球磨转速为155 r/min。
球磨后，将两组浆料进行烘干，烘干条件为50℃，时间6 h。
将粉体过筛，过筛目数为200。
用大小为24*24 mm模具对粉体进行成型：首先将荧光陶瓷粉体进行压片处理，压力20 Mpa，保压1 min；其次将无发光陶瓷粉体进行压片，压力20 Mpa，保压1 min；最终将两个方片组合压片，压力20 Mpa，保压2 min。
通过真空塑封机进行真空包装，在250 Mpa的压强下保压5 min进行二次成型，得到复合陶瓷素坯。
将素坯进行预烧，烧结温度为800℃，保温12h，去除有机物。
将素坯进行真空烧结，烧结制温度为1780℃，保温12h，随后自然冷却。
对复合陶瓷进行退火处理，烧结温度为1350℃，保温12h。
退火后，荧光陶瓷器件的尺寸为20*20 mm。将荧光陶瓷层切割为尺寸3*3 mm，厚度打磨为0.8mm；对无发光陶瓷进行抛光，最终厚度为0.8 mm。
对复合荧光陶瓷器件进行封装，包含发光透镜10、荧光陶瓷片20、无发光陶瓷片30、硅胶40、LED芯片50、散热基底60；其中，所述散热基底60上设有无发光陶瓷片30，所述无发光陶瓷片30与散热基底60紧密贴合并形成第一容置空间；所述第一容置空间内设有LED芯50片，所述LED芯片50与无发光陶瓷片30之间还设有硅胶40；所述无发光陶瓷片30上设有发光透镜10，与所述发光透镜10形成第二容置空间，所述荧光陶瓷片20位于所述第二容置空间内。
采用的硅胶40在400~800nm的透明度为95%，折射率为1.5；LED芯片50的尺寸为2.5*2.5mm，发射波长为460 nm；散热基底60的材质为紫铜。当LED芯片50的输出功率为12 W时，荧光陶瓷片20稳定发光：其运行温度为84℃；发光效率为284 lm/W；光通量高达3408lm；色温为5552 K。
实施例4
一种复合荧光陶瓷器件，上表层为荧光陶瓷片20，下表层为无发光陶瓷片30。
按照Ce掺杂浓度为1.0 at.% 和Ce掺杂浓度为0.0 at.%（无掺杂）的YAG荧光陶瓷进行配料，均加入0.1 wt.%的TEOS，配出两种混合粉体。
以无水乙醇作为溶剂，氧化铝球作为球磨介质，分别进行球磨；球磨时间为24 h；球磨转速为170 r/min。
球磨后，将两组浆料进行烘干，烘干条件为60℃，时间6 h。
将粉体过筛，过筛目数为200。
用大小为24*24 mm模具对粉体进行成型：首先将荧光陶瓷粉体进行压片处理，压力20 Mpa，保压1 min；其次将无发光陶瓷粉体进行压片，压力20 Mpa，保压1 min；最终将两个方片组合压片，压力20 Mpa，保压2 min。
通过真空塑封机进行真空包装，在250 Mpa的压强下保压5 min进行二次成型，得到复合陶瓷素坯。
将素坯进行预烧，烧结温度为800℃，保温12h，去除有机物。
将素坯进行真空烧结，烧结制温度为1790℃，保温12h，随后自然冷却。
对复合陶瓷进行退火处理，烧结温度为1450℃，保温12h。
退火后，荧光陶瓷器件的尺寸为20*20 mm。将荧光陶瓷层切割为尺寸3*3 mm，厚度打磨为1.0 mm；对无发光陶瓷进行抛光，最终厚度为1.0 mm。
对复合荧光陶瓷器件进行封装，包含发光透镜10、荧光陶瓷片20、无发光陶瓷片30、硅胶40、LED芯片50、散热基底60；其中，所述散热基底60上设有无发光陶瓷片30，所述无发光陶瓷片30与散热基底60紧密贴合并形成第一容置空间；所述第一容置空间内设有LED芯50片，所述LED芯片50与无发光陶瓷片30之间还设有硅胶40；所述无发光陶瓷片30上设有发光透镜10，与所述发光透镜10形成第二容置空间，所述荧光陶瓷片20位于所述第二容置空间内。
采用的硅胶40在400~800nm的透明度为95%，折射率为1.56；LED芯片50的尺寸为2.5*2.5mm，发射波长为460 nm；散热基底60的材质为铝。当LED芯片50的输出功率为12 W时，荧光陶瓷片20发光严重猝灭，发光效率为90 lm/W；光通量仅1080 lm；色温20456 K；其运行温度近220℃。由于陶瓷烧结温度超过1780℃，荧光陶瓷20中Ce的发光猝灭，且与无发光陶瓷30之间的接触不紧密，热量不能及时导出，最终导致LED照明器件的照明参数极不理想。
最后需要说明的是，以上实施例仅用以说明本发明的技术方案而非限制。尽管参照上述实施例对本发明进行了详细说明，本领域的普通技术人员应当理解，可以对发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的范围，其均应涵盖在本发明的权利要求范围中。
Claims (10)
1.一种复合荧光陶瓷器件，其特征在于，由荧光陶瓷片（20）和无发光陶瓷片（30）组成，上表层为荧光陶瓷片（20），下表层为无发光陶瓷片（30）。
2.如权利要求1所述的一种复合荧光陶瓷器件，其特征在于，所述荧光陶瓷片（20）的化学式为(Y1-xCex)3Al5O12，x=0.001~0.01；所述无发光陶瓷片（30）为YAG透明陶瓷，化学式为Y3Al5O12。
3.如权利要求1所述的一种复合荧光陶瓷器件，其特征在于，所述荧光陶瓷片（20）的尺寸为3*3 mm，厚度为0.5~1.0 mm；所述无发光陶瓷片（30）的尺寸为20*20 mm，厚度为0.5~1.0 mm。
4.一种如权利要求2所述的复合荧光陶瓷器件的制备方法，其特征在于，包含有以下步骤：
步骤1: 按照荧光陶瓷片（20）和无发光陶瓷片（30）的化学计量比进行配料，并分别加入0.1~1.0 wt.%的TEOS，分别配出荧光陶瓷粉体和无发光陶瓷粉体；
步骤2：以无水乙醇作为溶剂，氧化铝球作为球磨介质，分别进行球磨；球磨时间为20~24h；球磨转速为150~170r/min；
步骤3：将两组浆料进行烘干，烘干条件为40~60℃，时间6 h；
步骤4：将粉体过筛，过筛目数为100~200；
步骤5：压片，模具大小为24*24 mm；首先将荧光陶瓷粉体进行压片处理，压力4~20Mpa，保压1 min；其次将无发光陶瓷粉体进行压片, 压力4~20Mpa，保压1 min；最终将两个方片上下堆叠，进行压片，压力4~20Mpa，保压2 min；
步骤6：将压片后的素坯进行冷等静压，压强为200~250 MPa，保压时间为5 min；
步骤7：预烧，烧结温度为800~1000℃，保温12h；
步骤8：真空烧结，烧结制温度为1700~1780℃，保温12h，自然冷却；
步骤9：退火，烧结温度为1350~1450℃，保温12h；
步骤10：裁剪，将荧光陶瓷片切割成3*3 mm；
步骤11：抛光，将无发光陶瓷片表面抛光，得所述复合荧光陶瓷器件。
5.一种基于复合荧光陶瓷器件的高亮度LED照明光源，包括如权利要求1-4任一项所述的复合荧光陶瓷器件，其特征在于，还包括发光透镜（10）、硅胶（40）、LED芯片（50）、散热基底（60）；其中，所述散热基底（60）上设有无发光陶瓷片（30），所述无发光陶瓷片（30）与散热基底（60）紧密贴合并形成第一容置空间；所述第一容置空间内设有LED芯片（50），所述LED芯片（50）与无发光陶瓷片（30）之间还设有硅胶（40）；所述无发光陶瓷片（30）上设有发光透镜（10），与所述发光透镜（10）形成第二容置空间，所述荧光陶瓷片（20）位于所述第二容置空间内。
6.如权利要求5所述的一种基于复合荧光陶瓷器件的高亮度LED照明光源，其特征在于，所述荧光陶瓷片（20）的发光效率为200~300 lm/W，色温为3500~7000 K。
7.如权利要求5所述的一种基于复合荧光陶瓷器件的高亮度LED照明光源，其特征在于，所述硅胶（40）在400~800nm的透明度为80%~95%，折射率为1.45~1.56。
8.如权利要求5所述的一种基于复合荧光陶瓷器件的高亮度LED照明光源，其特征在于，所述LED芯片（50）的尺寸为2.5*2.5 mm，发射波长为435~460 nm，最大蓝光输出功率为9~12 W。
9.如权利要求5所述的一种基于复合荧光陶瓷器件的高亮度LED照明光源，其特征在于，所述散热基底（60）的材质为紫铜或铝。
10.如权利要求5所述的一种基于复合荧光陶瓷器件的高亮度LED照明光源，其特征在于，所述荧光陶瓷片（20）与无发光陶瓷片（30）通过烧结贴合在一起。
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