CN109437860A - 一种白光led用黄色复相荧光陶瓷及其制备方法 - Google Patents

一种白光led用黄色复相荧光陶瓷及其制备方法 Download PDF

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CN109437860A
CN109437860A CN201811504212.8A CN201811504212A CN109437860A CN 109437860 A CN109437860 A CN 109437860A CN 201811504212 A CN201811504212 A CN 201811504212A CN 109437860 A CN109437860 A CN 109437860A
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fluorescence ceramics
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王晓君
李会利
谷池
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Jiangsu Normal University
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Abstract

本发明公开了一种白光LED用黄色复相荧光陶瓷及其制备方法，该黄色复相荧光陶瓷是由98～99.5％CaF2陶瓷粉体和0.5～2％YAG:Ce荧光粉粉体球磨混合后采用热压法烧结得到。本发明制得的荧光陶瓷由CaF2、YAG:Ce两相构成，结晶度好，晶粒粒径范围在5～10μm，在蓝光激发下发射出～565纳米的黄光，发光效率高，热稳定性好。本发明的复相荧光陶瓷材料采用热压法在较低温度下(～700℃)制备得到，制备工艺简单，生产成本低。

Description

一种白光LED用黄色复相荧光陶瓷及其制备方法
技术领域
本发明属于无机发光材料领域，涉及一种荧光陶瓷，特别涉及一种白光LED用黄色复相荧光陶瓷及其制备方法。
背景技术
白光发光二极管(Light Emitting Diode，简称LED)具有能耗低、效率高、无污染、寿命长等特点，在固态照明、液晶背光源、汽车前照灯等领域具有十分广阔的应用前景。目前，市场上应用最广泛、最成熟的白光LED技术是荧光粉转换型，封装时将YAG:Ce(Y3Al5O12:Ce3+)荧光粉分散于环氧树脂、硅胶等有机材料中，蓝光LED芯片激发YAG:Ce荧光粉发出黄光，适当比例的黄光与蓝光混合形成白光。但是，随着白光LED亮度和功率的不断提高，环氧树脂、硅胶自身存在的耐热性差、易老化、吸湿性、高温和短波光照射下易变色等缺陷暴露了出来，严重影响了器件的寿命。荧光陶瓷具有热导率高、耐高温、抗热冲击性好等优势，能够有效解决上述问题。因此，研发高效廉价的荧光陶瓷和简单低能耗的合成方法对LED的发展具有重要意义。
发明内容
本发明的目的是提供一种白光LED用黄色复相荧光陶瓷，发光效率高，化学性质稳定。
本发明的另一目的是提供上述白光LED用黄色复相荧光陶瓷的制备方法，原料成本低，制备工艺简单，能耗低。
为实现上述目的，本发明采用的技术方案如下：一种白光LED用黄色复相荧光陶瓷，包括CaF2陶瓷粉体和YAG:Ce荧光粉体，其化学通式为：CaF2-YAG:Ce，其中YAG:Ce粉体与CaF2陶瓷粉体的质量比为0.5～2：98～99.5。
上述荧光陶瓷在460nm的蓝光激发下，发射出主波长565nm的黄色荧光。
本发明还提供上述白光LED用黄色复相荧光陶瓷的制备方法，具体包括以下步骤：
(1)称取原料：按质量比为0.5～2：98～99.5分别称取YAG:Ce粉体、CaF2粉体；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入球磨罐中，加入磨球，以无水乙醇为介质，所述磨球与原料粉体总量的球料比为1～2：1，球磨4～8小时，得到前驱体浆料；将得到的前驱体浆料真空干燥，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
优选的，步骤(3)中热压法烧结的工艺参数为：升温速率5～20℃/min，保温温度600～800℃，保温时间4～20h，热压压力40～60MPa。
优选的，步骤(2)中所述球磨罐的材质为聚四氟乙烯，所述磨球为氧化铝球。
优选的，步骤(2)中所述球磨的转速为180r/min。
优选的，步骤(2)中所述无水乙醇与原料粉体总量的质量比为2～4：1。
优选的，步骤(2)中真空干燥的条件为：温度60～80℃，保温10～24小时。
本发明提供的黄色CaF2-YAG:Ce复相荧光陶瓷由CaF2、YAG:Ce两相构成，结晶度好，晶粒粒径范围在5～10μm，在460nm的蓝光激发下，发射出主波长565nm的黄色荧光，具有发光效率高、热稳定性好、易成型等优点。此外，本发明开发的荧光陶瓷制备工艺简单、烧结温度低，极大的降低了能耗和成本，具有重要的应用前景。
附图说明
图1为本发明中实施例1制备的黄色CaF2-YAG:Ce复相荧光陶瓷的X射线衍射图谱。
图2为本发明中实施例1制备的黄色CaF2-YAG:Ce复相荧光陶瓷的扫描电镜照片。
图3为本发明中实施例1制备的黄色CaF2-YAG:Ce复相荧光陶瓷的激发光谱和发射光谱。
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)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为1：99分别称取YAG:Ce粉体0.2g、CaF2粉体19.8g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入1倍原料粉体重量的氧化铝球磨珠和3倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨8小时，得到前驱体浆料；将得到的前驱体浆料放到80℃的真空干燥箱中保温24小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率20℃/min，保温温度700℃，保温时间10h，热压压力60MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
图1为实施例1制备的黄色CaF2-YAG:Ce复相荧光陶瓷的X射线衍射图谱。由图可见，制备的荧光陶瓷由CaF2、YAG:Ce两相构成，表明在陶瓷烧结过程中无新的杂质相产生，制备的陶瓷材料相纯度高，结晶度好。
图2为实施例1制备的黄色CaF2-YAG:Ce复相荧光陶瓷的扫描电镜照片。由图可见，该方法合成的复相荧光陶瓷的晶粒粒径范围在5～10μm。
图3为实施例1制备的黄色CaF2-YAG:Ce复相荧光陶瓷的激发光谱和发射光谱。由图可见，制备的复相荧光陶瓷在460nm激发下发射出～565nm的黄光，与YAG:Ce粉体的光谱一致，可被蓝光LED芯片有效激发；此外，烧结前后，样品的激发光谱和发射光谱的形状基本没有发生改变，并且没有新的激发峰或发射峰出现，表现出较好的发光性能。
实施例2
(1)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为0.5：99.5分别称取YAG:Ce粉体0.1g、CaF2粉体19.9g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入1倍原料粉体重量的氧化铝球磨珠和3倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨8小时，得到前驱体浆料；将得到的前驱体浆料放到80℃的真空干燥箱中保温24小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率20℃/min，保温温度700℃，保温时间10h，热压压力60MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
本实施例制备的黄色CaF2-YAG:Ce复相荧光陶瓷的XRD图、激发光谱和发射光谱与实施例1的荧光陶瓷样品相似。
实施例3
(1)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为1.5：98.5分别称取YAG:Ce粉体0.3g、CaF2粉体19.7g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入1倍原料粉体重量的氧化铝球磨珠和3倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨8小时，得到前驱体浆料；将得到的前驱体浆料放到80℃的真空干燥箱中保温24小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率20℃/min，保温温度700℃，保温时间10h，热压压力60MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
本实施例制备的黄色CaF2-YAG:Ce复相荧光陶瓷的XRD图、激发光谱和发射光谱与实施例1的荧光陶瓷样品相似。
实施例4
(1)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为1：49分别称取YAG:Ce粉体0.4g、CaF2粉体19.6g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入1倍原料粉体重量的氧化铝球磨珠和3倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨8小时，得到前驱体浆料；将得到的前驱体浆料放到80℃的真空干燥箱中保温24小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率20℃/min，保温温度700℃，保温时间10h，热压压力60MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
本实施例制备的黄色CaF2-YAG:Ce复相荧光陶瓷的XRD图、激发光谱和发射光谱与实施例1的荧光陶瓷样品相似。
实施例5
(1)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为1：99分别称取YAG:Ce粉体0.2g、CaF2粉体19.8g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入2倍原料粉体重量的氧化铝球磨珠和4倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨4小时，得到前驱体浆料；将得到的前驱体浆料放到60℃的真空干燥箱中保温24小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率5℃/min，保温温度700℃，保温时间10h，热压压力60MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
本实施例制备的黄色CaF2-YAG:Ce复相荧光陶瓷的XRD图、激发光谱和发射光谱与实施例1的荧光陶瓷样品相似。
实施例6
(1)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为1：99分别称取YAG:Ce粉体0.2g、CaF2粉体19.8g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入1倍原料粉体重量的氧化铝球磨珠和2倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨8小时，得到前驱体浆料；将得到的前驱体浆料放到80℃的真空干燥箱中保温10小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率10℃/min，保温温度600℃，保温时间20h，热压压力60MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
本实施例制备的黄色CaF2-YAG:Ce复相荧光陶瓷的XRD图、激发光谱和发射光谱与实施例1的荧光陶瓷样品相似。
实施例7
(1)称取原料：设定YAG:Ce、CaF2原料粉体的总重量为20g，按质量比为1：99分别称取YAG:Ce粉体0.2g、CaF2粉体19.8g；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入聚四氟乙烯球磨罐中，加入2倍原料粉体重量的氧化铝球磨珠和4倍原料粉体重量的无水乙醇，球磨转速180r/min，球磨5小时，得到前驱体浆料；将得到的前驱体浆料放到70℃的真空干燥箱中保温18小时，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型，升温速率20℃/min，保温温度800℃，保温时间4h，热压压力40MPa；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
本实施例制备的黄色CaF2-YAG:Ce复相荧光陶瓷的XRD图、激发光谱和发射光谱与实施例1的荧光陶瓷样品相似。

Claims (8)

1.一种白光LED用黄色复相荧光陶瓷，其特征在于，包括CaF2陶瓷粉体和YAG:Ce荧光粉体，其化学通式为：CaF2-YAG:Ce，其中YAG:Ce粉体与CaF2陶瓷粉体的质量比为0.5～2：98～99.5。
2.根据权利要求1所述的白光LED用黄色复相荧光陶瓷，其特征在于，所述荧光陶瓷在460nm的蓝光激发下，发射出主波长565nm的黄色荧光。
3.一种权利要求1或2所述的白光LED用黄色复相荧光陶瓷的制备方法，其特征在于，具体包括以下步骤：
(1)称取原料：按质量比为0.5～2：98～99.5分别称取YAG:Ce粉体、CaF2粉体；
(2)原料粉体的混合：采用球磨法混合原料粉体，将初始原料放入球磨罐中，加入磨球，以无水乙醇为介质，所述磨球与原料粉体总量的球料比为1～2：1，球磨4～8小时，得到前驱体浆料；将得到的前驱体浆料真空干燥，得到干燥、混合均匀的原料粉体混合物；再将所述原料粉体混合物放在玛瑙研钵中研磨、粉碎、过200目筛网，取筛下物得到分散性较好的原料粉体混合物；
(3)将步骤(2)得到的原料粉体混合物填入石墨磨具中，采用热压法烧结，在热压炉中压模烧结成型；
(4)撤去压力后自然冷却至室温，得到黄色CaF2-YAG:Ce复相荧光陶瓷。
4.根据权利要求3所述的白光LED用黄色复相荧光陶瓷的制备方法，其特征在于，步骤(3)中热压法烧结的工艺参数为：升温速率5～20℃/min，保温温度600～800℃，保温时间4～20h，热压压力40～60MPa。
5.根据权利要求3所述的白光LED用黄色复相荧光陶瓷的制备方法，其特征在于，步骤(2)中所述球磨罐的材质为聚四氟乙烯，所述磨球为氧化铝球。
6.根据权利要求3所述的白光LED用黄色复相荧光陶瓷的制备方法，其特征在于，步骤(2)中所述球磨的转速为180r/min。
7.根据权利要求3所述的白光LED用黄色复相荧光陶瓷的制备方法，其特征在于，步骤(2)中所述无水乙醇与原料粉体总量的质量比为2～4：1。
8.根据权利要求3所述的白光LED用黄色复相荧光陶瓷的制备方法，其特征在于，步骤(2)中真空干燥的条件为：温度60～80℃，保温10～24小时。
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