CN112552038A - 一种绿色荧光复合陶瓷及其制备方法和应用 - Google Patents
一种绿色荧光复合陶瓷及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种绿色荧光复合陶瓷及其制备方法和应用。绿色荧光复合陶瓷主要由稀土铝酸盐石榴石和氧化铝两种晶体组成，按化学组成Lu3‑x‑zCezRexAlyO12的元素计量比制备而成，其中，Re为Y、Gd中的至少一种，x、y、z的取值范围分别为：0≤x≤2，6＜y≤20，0＜z≤0.3，且公开了绿色荧光复合陶瓷的制备方法及绿色荧光复合陶瓷在基于大功率蓝光LED或LD的固态照明与显示的应用。本发明制备的绿色荧光复合陶瓷，其量子效率高、热稳定性优异，且制备方法简单，在常压下通过玻璃晶化的方式即可得到致密度高、透过率可调的绿色荧光透明陶瓷，并且制备的绿色荧光透明陶瓷可以通过与大功率蓝光LED或LD等固态激发光源组合封装出高功率发光器件。
Description
技术领域
本发明属于固体发光材料的一种复合陶瓷，具体涉及一种绿色荧光复合陶瓷及其制备方法和应用。
背景技术
白光LED因具有高效、环保、长寿命、体积小等许多优点而应用广泛，并已经逐渐取代传统照明光源。半导体固态照明光源正朝着高稳定性、高光学品质和高激发密度的方向发展，有望应用于汽车大灯、隧道灯、强力探照灯等特殊照明领域。以大功率LED或者激光二极管(LD)等作为激发光源的高功率荧光转换型固态照明光源在运行时会产生巨大的热量，使得器件的运行温度大于150℃。然而，由于有机封装材料物理化学稳定性差且热导率低，传统的“荧光粉+硅胶”型有机-无机复合荧光转换体，无法应用于高功率固态照明，特别是激光照明领域。
作为一种块体材料，荧光陶瓷是一种全无机荧光转换体。它不但能够拥有荧光晶体的高荧光量子效率和高热导率，还能通过组分调控、烧结过程的控制实现对透明度的调控，进而优化其对光的散射、透过和吸收。
绿色荧光陶瓷能够被应用于高品质绿色照明或者宽色域显示等领域，如专利文献《一种绿色荧光透明陶瓷的制备方法和应用》(CN 110204324A)就公开了一种绿色硅酸盐石榴石荧光透明陶瓷及其应用。铝酸盐石榴石相比于硅酸盐石榴石，具有更高的热导率和光谱可调性，但是目前稀土铝酸盐(Re3Al5O12)石榴石荧光陶瓷的制备方法均采用高压、高真空烧结技术。如专利文献《一种用于高光效LED的绿光透明陶瓷荧光体的制备方法》(CN104891967A)公开了一种绿色透明陶瓷(Cex％Lu100％-x％)3Al5O12的制备方法其制备时采用了冷等静压(150～300Mpa)和高真空烧结，其工艺复杂，重复性差。又如，专利文献《一种石榴石型铝酸盐荧光陶瓷的制备方法及所制成的荧光陶瓷》(CN 104909741 A)公开了一种石榴石型荧光陶瓷的制备方法，其制备时采用了真空电子束熔炼技术，并且在0.01-100Pa的高真空下进行热处理，制备成本极高。高压、高真空等致密化烧结的工艺复杂、成本高昂极大地限制了荧光陶瓷在高功率照明领域的广泛应用。
发明内容
为了解决背景技术中存在的问题，本发明的目的在于提供一种绿色荧光复合陶瓷；本发明的另一目的在于提供上述绿色荧光复合陶瓷的无需高压和高真空的制备方法及其应用。
为实现上述目的，本发明的技术方案是：
一、一种绿色荧光复合陶瓷：
绿色荧光复合陶瓷主要由稀土铝酸盐石榴石和氧化铝两种晶体组成，按化学组成Lu3-x-zRexAlyO12：zCe的元素计量比制备而成，其中，Re为Y、Gd中的至少一种，x、y、z的取值范围分别为：0≤x≤2，6＜y≤20，0＜z≤0.3。
二、一种绿色荧光复合陶瓷的制备方法，包括以下具体步骤：
(1)按化学组成Lu3-x-zRexAlyO12：zCe中的元素计量比，其中，Re为Y、Gd中的至少一种，x、y、z的取值范围分别为：0≤x≤2，6＜y≤20，0＜z≤0.3，称取含有Lu、Al、Re、Ce的氧化物、碳酸盐或者硝酸盐为原料，然后通过研磨、搅拌等方式将其充分混合；
(2)将步骤(1)所得的原料，在高温熔化设备中进行熔融操作，然后经冷却后得到透明玻璃样品。
(3)将步骤(2)所得的透明玻璃样品放入箱式炉中进行析晶处理，在常压下，首先在800～1000℃下进行保温，随后升温至1100～1600℃进行致密化烧结，并在气氛下进行析晶，经冷却后得到致密化的绿色荧光复合陶瓷。
(4)将步骤(3)所得的致密化的绿色荧光复合陶瓷依次进行打磨成片状、表面抛光处理后得量子效率高、热稳定好及透过率能调的最终的绿色荧光复合陶瓷。
所述步骤(3)中，保温的时间和致密化烧结的时间均为1-40h。
所述步骤(3)中的气氛为空气、氧气、氮气和氢气混合气、氩气、一氧化碳气体中的至少一种。
三、绿色荧光复合陶瓷的应用
所述的绿色荧光复合陶瓷在基于大功率蓝光LED或LD的固态照明与显示的应用。
所述绿色荧光复合陶瓷制备荧光转换型固态光源，所述的荧光转换型固态光源应用于照明与显示。
所述的荧光转换型固态光源采用发射波长为420～480nm的LED或者LD作为固态激发光源。
本发明无需高压、高真空就可以制备出致密度高、透过率可调的绿色荧光复合陶瓷，且其常温下内量子效率高达98％、且在150℃下也几乎不发生热猝灭。
本发明的有益效果：
本发明涉及一种量子效率高、热稳定性优异的绿色荧光复合陶瓷；其制备方法不需要复杂的制备工艺，也不需要高压、高真空等极端条件，在常压下通过玻璃晶化的方式即可得到致密度高、透过率可调的绿色荧光透明陶瓷，并且可以通过与大功率蓝光LED或LD等固态激发光源组合封装出高功率发光器件。
附图说明
图1是实施例1制备的样品的XRD图谱；
图2是实施例1-3制备的样品的激发和发射光谱；
图3是实施例1制备的样品的总透过率；
图4是实施例1制备的样品的热稳定性测试；
图5是实施例1和实施例3制备的样品结合450nm蓝光LED封装的LED器件的光谱。
具体实施方式
下面结合附图和实施例对本发明作进一步说明。
实施例1
按以下分子式Lu2.99Ce0.01Al10O12的计量比分别称取氧化镥、氧化铝和氧化铈原料，放入玛瑙研钵中，加入3ml酒精，搅拌、研磨20min使原料充分混合后得到混合粉体，使用压片机将混合粉体压制成薄片，然后截取该薄片的二十分之一，放入配备有双光束二氧化碳激光器的气悬浮炉中，使用高纯氧气作为载气，对样品进行悬浮熔炼，使样品保持熔融状态约30s，通过切断激光使熔体快速冷却，获得具有相应组分的玻璃球。接着将所获得的玻璃球放入高温箱式炉中，在空气氛围下以10℃/min的速度升至900℃并保温2h，最后以5℃/min的速度升至1300℃，常压下进行致密化烧结5h，自然冷却后，得到致密化的球形荧光透明陶瓷。将球形荧光透明陶瓷打磨成片状，对荧光透明陶瓷片进行表面抛光处理后，即获得在420-480nm激发下发射峰值在511nm左右的绿光荧光复合陶瓷。
如图1所示，是实施例1制备的样品的XRD图谱，从图中可知，制备的绿色荧光复合陶瓷属于石榴石结构的立方晶相。
如图2所示，实施例1制备的绿色荧光复合陶瓷在420-480nm的蓝光激发下，发射出峰值的511nm的宽带绿光，内量子效率为98％。
如图3所示，是实施例1制备的样品的总透过率，其中此实施例在样品的厚度为0.5mm时发射峰值在511nm处的总透过率为50％。
如图4所示，是实施例1制备的样品的热稳定性测试，从图中可知，制备的样品的热稳定好，其在150℃下积分强度未发生改变。
如图5所示，实施例1制备的样品结合450nm蓝光LED封装的LED器件的光谱，其光谱覆盖蓝光到绿光区域，可以应用于基于LED的照明与显示领域。
实施例2
除了将致密化烧结温度(致密化温度)改为1100℃，烧结时间(致密化时间)改为2h，其他制备步骤和工艺条件与实施例1相同。本实施例激发和发射光谱、热稳定性与实施例1相似，内量子效率为90％，在样品的厚度为0.5mm时发射峰值在511nm处的总透过率为80％。
实施例3
除了将致密化烧结温度(致密化温度)改为1600℃，其他制备步骤和工艺条件与实施例1相同。本实施例激发和发射光谱、热稳定性与实施例1相似，内量子效率为95％，在样品的厚度为0.5mm时发射峰值在511nm处的总透过率为20％，结合450nm蓝光LED封装的LED器件的光谱见图5。
实施例4至实施例20：
按表1中的实施例化学式组成及其化学计量比称取相应原料，其致密化温度、致密化时间和气氛见表1，其他步骤与上述实施例皆相同。表1中透过率值均为0.5mm厚的样品在波长511nm处的总透过率。
表1实施例1-20
由此可见，本发明通过不同的元素配比、保温条件、烧结条件等工艺条件能调节光透过率，适当延长烧结保温时间能实现更高的透过率。本发明的光透过率最高可达到80％，实现了极高的致密性。显然，上述实施例仅仅是为了清楚的说明所作的举例，在上述说明的基础上还可以做出其他形式的变动或变化，由此所引申出的显而易见的变化或变动仍属于本发明的保护范围之内。本发明实施例中玻璃的制备采用了气悬浮炉法，然而，其制备方法并不局限于此，其他能够将原料充分熔化且快速冷却的方法均可以获得本发明所述的玻璃。本发明实施例中所采用的原料也可以使用含有相应元素但不引入外来杂质的其他化合物。
Claims (6)
1.一种绿色荧光复合陶瓷，其特征在于：所述的绿色荧光复合陶瓷主要由稀土铝酸盐石榴石和氧化铝两种晶体组成，按化学组成Lu3-x-zCezRexAlyO12的元素计量比制备而成，其中，Re为Y、Gd中的至少一种，x、y、z的取值范围分别为：0≤x≤2，6＜y≤20，0＜z≤0.3。
2.一种权利要求1所述的绿色荧光复合陶瓷的制备方法，其特征在于：方法包括以下步骤：
(1)按照权利要求1所述的化学组成及计量比，称取含有Lu、Al、Re、Ce的氧化物、碳酸盐或者硝酸盐为原料，Re为Y、Gd中的至少一种，然后通过研磨、搅拌方式将原料充分混合；
(2)将步骤(1)中的原料，在熔化设备中进行熔融操作，然后经冷却后得到透明玻璃样品；
(3)将步骤(2)所得的透明玻璃样品放入箱式炉中进行析晶处理，在常压下，首先在800～1000℃下进行保温，随后升温至1100～1600℃进行致密化烧结，并在气氛下进行析晶，经冷却后得到致密化的绿色荧光复合陶瓷；
(4)将步骤(3)所得的致密化的绿色荧光复合陶瓷依次进行打磨成片状、表面抛光处理后得最终的绿色荧光复合陶瓷。
3.根据权利要求2所述的一种绿色荧光复合陶瓷的制备方法，其特征在于：所述步骤(3)中，保温的时间和致密化烧结的时间均为1-40h。
4.根据权利要求2所述的一种绿色荧光复合陶瓷的制备方法，其特征在于：所述步骤(3)中的气氛为空气、氧气、氮气和氢气混合气、氩气、一氧化碳气体中的至少一种。
5.根据权利要求2-4任一所述的制备方法制成的绿色荧光复合陶瓷的应用，其特征在于：所述的绿色荧光复合陶瓷在基于大功率蓝光LED或LD的固态照明与显示的应用。
6.根据权利要求5的绿色荧光复合陶瓷的应用，其特征在于：所述绿色荧光复合陶瓷制备荧光转换型固态光源，所述的荧光转换型固态光源应用于照明与显示。
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