CN117353146A - 一种具有高反射层的激光照明用荧光器件及其制备方法 - Google Patents
一种具有高反射层的激光照明用荧光器件及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种具有高反射层的激光照明用荧光器件及其制备方法，采用流延成型结合真空烧结制备了荧光层‑高反射层‑衬底层的复合荧光器件，所述荧光层以YAG陶瓷作为基质材料，Ce3+离子作为发光离子，其分子式为nAl2O3‑(Ce0.002Y0.998)3Al5O12，0≤n≤0.8，所述高反射层采用Al2O3，所述衬底层采用紫铜片。其制备方法：将流延得到的复相素坯与干压的Al2O3素坯塑封并采用等静压成型结合起来，通过真空烧结得到发光材料，最后将抛光后的陶瓷与紫铜片进行焊接，即得荧光器件。本发明的荧光器件整体导热性能优异，同时具有高亮度和高发光效率。
Description
技术领域
本发明涉及激光照明用荧光材料领域，具体涉及一种具有高反射层的激光照明用荧光器件及其制备方法。
背景技术
蓝色激光二极管(LD)和远程颜色转换器通常用于实现激光驱动的白色照明。蓝光LD可以通过简单地增加输入功率密度来实现高亮度照明，但高功率密度激光激发产生的大量热量积累和光转换损失为颜色转换器的热管理带来了新的挑战。传统的树脂磷(PiS)颜色转换器由于其热稳定性差，导热性有限，在高功率密度激光激发下存在严重的热侵蚀和碳化问题，无法满足激光照明的实际应用。因此，开发具有多种结构配置和材料设计的新型颜色转换器是迫切需要的。
此外，激光照明的颜色转换器架构根据基板的透明度分为反射模式和透射模式。在提高荧光材料的散热能力和发光饱和阈值方面，反射式转换器优于透射式转换器。Al2O3陶瓷由于其低成本、出色的热稳定性、优异的耐腐蚀性和高反射率而成为反射式颜色转换器的替代基板。同时由于Al2O3的良好的导热系数(～30W·m-1·K-1)和Al2O3颗粒优异的散射效应而适合作为反射界面。紫铜因其高导热系数(～380W·m-1·K-1)、优异的热稳定性和低膨胀系数而被指定为导热基板。在此，提出的这种热鲁棒性和高反射性的复相荧光层-Al2O3层-紫铜片荧光器件，可以在高功率密度激光激发下，维持颜色转换器的有效散热，同时实现高光通量和超高效率的激光驱动白光照明。
CN108527960A公开了一种荧光陶瓷与蓝宝石复合陶瓷材料，复合陶瓷材料包括荧光陶瓷层、蓝宝石层及连接层，连接层为石英玻璃、铝酸盐玻璃或硼酸盐玻璃。此方案中高导热基底(蓝宝石)与发光材料中间的连接层仍为玻璃材料，导热性能太差，不能有效解决热效应问题。CN217361618U公开了一种高反射率的陶瓷荧光片，将陶瓷荧光片、高反射层、复合材料层、粘连层、蓝宝石片和增透膜等粘接在一起形成荧光材料。虽然可以发挥各功能层的作用，然而，该方法所需的工艺是十分苛刻的，精度高，成本较高，不适合大规模生产。
发明内容
本发明的目的是提供一种具有高反射层的激光照明用荧光器件，导热性能和发光性能优异。
本发明的另一目的是提供上述具有高反射层的激光照明用荧光器件的制备方法，
为实现上述目的，本发明采用的技术方案如下：
一方面，本发明提供一种具有高反射层的激光照明用荧光器件，该荧光器件是荧光层-高反射层-衬底层的三明治层设计，所述荧光层以YAG陶瓷作为基质材料，Ce3+离子作为发光离子，其分子式为nAl2O3-(Ce0.002Y0.998)3Al5O12，0≤n≤0.8，所述高反射层采用Al2O3，所述衬底层采用紫铜片。
优选的，所述荧光层的厚度为0.2～1.2mm，所述高反射层的厚度为0.5～3mm。
另一方面，本发明还提供上述具有高反射层的激光照明用荧光器件的制备方法，包括下列步骤：
(1)按照化学式nAl2O3-(Ce0.002Y0.998)3Al5O12，0≤n≤0.8中各元素的化学计量比分别称量原料粉体，依次进行球磨、干燥、过筛、煅烧；
(2)将步骤(1)中的混合粉体与分散剂、无水乙醇混合，球磨后加入粘结剂和增塑剂，继续球磨、除泡；
(3)将步骤(2)除泡的浆料进行流延，得到不同厚度的的陶瓷流延膜片；通过塑封将流延膜片与干压的Al2O3素坯组合起来，再将整个素坯进行等静压成型，得到陶瓷素坯；
(4)将步骤(3)的得到的陶瓷素坯置于马弗炉中进行排胶处理，之后放入真空炉进行烧结，最后将陶瓷置于马弗炉中在空气气氛下退火并将发光材料表面进行抛光；
(5)将步骤(4)的抛光后的陶瓷与紫铜片进行焊接，即得荧光材料。
优选的，步骤(2)中，所述分散剂为鲱鱼油、油酸、柠檬酸钠、聚丙烯酸或NP-10中的任意一种或几种，所述分散剂的添加量为混合粉体总质量的3～10％。
优选的，步骤(2)中，所述粘结剂为聚乙烯醇缩丁醛酯(PVB)，所述粘结剂的添加量为混合粉体总质量的2～8％。
优选的，步骤(2)中，所述增塑剂为邻苯二甲酸丁基苄酯(BPP)、聚乙烯醇、过氧化特戊酸特丁酯、甘油中的任意一种或几种，所述增塑剂的添加量为混合粉体总质量的2～7％。
优选的，步骤(3)中，所述流延层的总厚度为0.2～1.2mm。
优选的，步骤(3)中，所述干压的Al2O3素坯的厚度为0.5～3mm。
优选的，步骤(4)中，所述烧结温度为1500～1740℃，烧结时间为5～12h。
与现有技术相比，本发明具有如下有益效果：
1.本发明通过设置Al2O3高反射层，增强了荧光层的反射效果，可以获得更高的光通量和发光效率。
2.本发明与先前的复合陶瓷制备技术相比，本发明中材料各标准粉体通过流延成型得到的素坯，再与干压的Al2O3素坯通过等静压成型结合牢固起来，烧结后的陶瓷再焊接在紫铜片基底上，进一步提升荧光陶瓷导热性能。
3.本发明所述荧光器件在25W/mm2激光激发下，发光效率200～300lm/W，光通量2000～3000lm；运行温度70～120℃，成品率高，适合批量生产，能够满足激光照明技术迅猛发展的市场需求，具有良好的经济效益。
附图说明
图1为本发明荧光器件的结构示意图；
附图中：1.nAl2O3-Ce:YAG陶瓷层，2.Al2O3陶瓷层，3.紫铜片。
图2为本发明荧光器件工作示意图。
图3为实施例3制备的荧光器件的光通量图。
具体实施方式
下面结合附图和具体实施例对本发明作进一步详细说明。
实施例1：
(1)按照化学式(Ce0.002Y0.998)3Al5O12称量Al2O3、Y2O3、CeO2原料粉体，即能得到0.2at.％Ce:YAG荧光陶瓷；其中，Al2O3为25.751g、Y2O3为34.149g、CeO2为0.104g，共60.004g。以无水乙醇作为溶剂、氧化铝球作为球磨介质，将准确称量的原料粉体置于球磨罐内以180r/min球磨15h，得到混合均匀的浆料；将球磨后的浆料干燥后过200目筛，过筛后的粉体置于马弗炉内在600℃下煅烧；
(2)将煅烧后的混合粉体置于无水乙醇中，加入0.6g鲱鱼油和0.6g NP-10，球磨6h后加入1.8g PVB和1.2g BPP再球磨6h，随后将浆料放在真空压力为1Torr的真空除泡机内真空除泡10min，制备出0.2at.％Ce:YAG的浆料；
(3)将除泡后的浆料流延得到厚度为0.2mm的Ce:YAG流延膜片，通过塑封将流延膜片与干压厚度为0.5mm的Al2O3素坯组合起来，再将整个素坯在150MPa下等静压得到陶瓷素坯。
(4)将陶瓷素坯置于马弗炉在600℃下排胶，之后将素坯置于真空炉中在下烧结；烧结温度为1500℃，烧结时间为5h；最后将陶瓷置于马弗炉在1200℃下退火并抛光。
(5)最后将抛光后的陶瓷与紫铜片进行焊接，即得0.2at.％Ce:YAG-Al2O3-紫铜片的荧光器件。
本实施例所制备得到的荧光器件的结构示意图如图1所示，从上到下依次排列nAl2O3-Ce:YAG陶瓷层1，Al2O3陶瓷层2，紫铜片3。其工作示意图如图2所示。
将该荧光器件放在25W/mm2激光激发下，其发光效率为200lm/W，光通量2000lm；运行温度120℃。
实施例2：
(1)按照化学式0.6Al2O3-(Ce0.002Y0.998)3Al5O12称量Al2O3、Y2O3、CeO2原料粉体，Al2O3/Ce:YAG质量之比为60wt.％，即0.6Al2O3-Ce:YAG荧光陶瓷；其中，Al2O3的为38.594g、Y2O3为21.343g、CeO2为0.065g，共60.002g。以无水乙醇作为溶剂、氧化铝球作为球磨介质，将准确称量的原料粉体置于球磨罐内以180r/min球磨15h，得到混合均匀的浆料；将球磨后的浆料干燥后过200目筛，过筛后的粉体置于马弗炉内在600℃下煅烧；
(2)将煅烧后的粉体置于无水乙醇中加入2g柠檬酸钠和1.5g NP-10，球磨6h后加入3g PVB和3g BPP再球磨6h，随后将浆料放在真空压力为1Torr的真空除泡机内真空除泡10min，分别制备出0.6Al2O3-Ce:YAG的浆料；
(3)将除泡后的浆料流延得到厚度为0.8mm的0.6Al2O3-Ce:YAG流延膜片，通过塑封将流延膜片与干压厚度为1.5mm的Al2O3素坯组合起来，再将整个素坯在150MPa下等静压得到陶瓷素坯。
(4)将陶瓷素坯置于马弗炉在600℃下排胶，之后将素坯置于真空炉中在下烧结；烧结温度为1650℃，烧结时间为8h；最后将陶瓷置于马弗炉在1200℃下退火并抛光。
(5)最后将抛光后的陶瓷与紫铜片进行焊接，即得(0.6Al2O3-Ce:YAG)-Al2O3-紫铜片的荧光器件。
本实施例所制备得到的荧光器件的结构示意图如图1所示，从上到下依次排列nAl2O3-Ce:YAG陶瓷层1，Al2O3陶瓷层2，紫铜片3。其工作示意图如图2所示。
将该荧光器件放在25W/mm2激光激发下，其发光效率为240lm/W，光通量2600lm；运行温度95℃。
实施例3：
(1)按照化学式0.8Al2O3-(Ce0.002Y0.998)3Al5O12称量Al2O3、Y2O3、CeO2原料粉体，Al2O3/Ce:YAG质量之比为80wt.％，即0.8Al2O3-Ce:YAG荧光陶瓷；其中，Al2O3的为40.976g、Y2O3为18.972g、CeO2为0.058g，共60.006g。以无水乙醇作为溶剂、氧化铝球作为球磨介质，将准确称量的原料粉体置于球磨罐内以180r/min球磨15h，得到混合均匀的浆料；将球磨后的浆料干燥后过200目筛，过筛后的粉体置于马弗炉内在600℃下煅烧；
(2)将煅烧后的粉体置于无水乙醇中加入4g聚丙烯酸和2g油酸，球磨6h后加入6gPVB和2.4g BPP再球磨6h，随后将浆料放在真空压力为1Torr的真空除泡机内真空除泡10min，分别制备出0.8Al2O3-Ce:YAG的浆料；
(3)将除泡后的浆料流延得到厚度为1.2mm的Ce:YAG流延膜片，通过塑封将流延膜片与干压厚度为3mm的Al2O3素坯组合起来，再将整个素坯在150MPa下等静压得到陶瓷素坯。
(4)将陶瓷素坯置于马弗炉在600℃下排胶，之后将素坯置于真空炉中在下烧结；烧结温度为1740℃，烧结时间为12h；最后将陶瓷置于马弗炉在1200℃下退火并抛光。
(5)最后将抛光后的陶瓷与紫铜片进行焊接，即得(0.8Al2O3-Ce:YAG)-Al2O3-紫铜片的荧光器件。
本实施例所制备得到的荧光器件的结构示意图如图1所示，从上到下依次排列nAl2O3-Ce:YAG陶瓷层1，Al2O3陶瓷层2，紫铜片3。其工作示意图如图2所示。
将该荧光器件放在25W/mm2激光激发下，其发光效率为300lm/W，光通量3000lm(如图3所示)；运行温度70℃。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种具有高反射层的激光照明用荧光器件，其特征在于，该荧光器件是荧光层-高反射层-衬底层的三明治层设计，所述荧光层以YAG陶瓷作为基质材料，Ce3+离子作为发光离子，其分子式为nAl2O3-(Ce0.002Y0.998)3Al5O12，0≤n≤0.8，所述高反射层采用Al2O3，所述衬底层采用紫铜片。
2.根据权利要求1所述的一种具有高反射层的激光照明用荧光器件，其特征在于，所述荧光层的厚度为0.2～1.2mm，所述高反射层的厚度为0.5～3mm。
3.一种权利要求1或2所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，包括下列步骤：
(1)按照化学式nAl2O3-(Ce0.002Y0.998)3Al5O12，0≤n≤0.8中各元素的化学计量比分别称量原料粉体，依次进行球磨、干燥、过筛、煅烧；
(2)将步骤(1)中的混合粉体与分散剂、无水乙醇混合，球磨后加入粘结剂和增塑剂，继续球磨、除泡；
(3)将步骤(2)除泡的浆料进行流延，得到不同厚度的的陶瓷流延膜片；通过塑封将流延膜片与干压的Al2O3素坯组合起来，再将整个素坯进行等静压成型，得到陶瓷素坯；
(4)将步骤(3)的得到的陶瓷素坯置于马弗炉中进行排胶处理，之后放入真空炉进行烧结，最后将陶瓷置于马弗炉中在空气气氛下退火并将发光材料表面进行抛光；
(5)将步骤(4)的抛光后的陶瓷与紫铜片进行焊接，即得荧光材料。
4.根据权利要求3所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，步骤(2)中，所述分散剂为鲱鱼油、油酸、柠檬酸钠、聚丙烯酸或NP-10中的任意一种或几种，所述分散剂的添加量为混合粉体总质量的3～10％。
5.根据权利要求3所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，步骤(2)中，所述粘结剂为聚乙烯醇缩丁醛酯，所述粘结剂的添加量为混合粉体总质量的2～8％。
6.根据权利要求3所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，步骤(2)中，所述增塑剂为邻苯二甲酸丁基苄酯、聚乙烯醇、过氧化特戊酸特丁酯、甘油中的任意一种或几种，所述增塑剂的添加量为混合粉体总质量的2～7％。
7.根据权利要求3所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，步骤(3)中，所述流延层的总厚度为0.2～1.2mm。
8.根据权利要求3所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，步骤(3)中，所述干压的Al2O3素坯的厚度为0.5～3mm。
9.根据权利要求3所述的具有高反射层的激光照明用荧光器件的制备方法，其特征在于，步骤(4)中，所述烧结温度为1500～1740℃，烧结时间为5～12h。
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