CN106866132A - 一种用于照明或显示的荧光陶瓷及其制备方法 - Google Patents

一种用于照明或显示的荧光陶瓷及其制备方法 Download PDF

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CN106866132A
CN106866132A CN201710033395.9A CN201710033395A CN106866132A CN 106866132 A CN106866132 A CN 106866132A CN 201710033395 A CN201710033395 A CN 201710033395A CN 106866132 A CN106866132 A CN 106866132A
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fluorescence ceramics
ball milling
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卓宁泽
王海波
刘光熙
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Nanjing Tech University
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Abstract

本发明公开了一种用于照明或显示的荧光陶瓷及其制备方法，所述的荧光陶瓷包括陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉。所述铝硅酸盐荧光粉化学式为(Ca1‑xMx)1‑y‑zAl2Si2O8：yEu2+，zR，元素M为Mg，Sr，Ba中的一种，R为Ce3+，Mn4+，Dy3+，Tb3+中的一种，其中x，y，z为摩尔系数，范围0.01＜x＜1，0.2≤y≤0.7，0≤z≤0.6，y+z＜1，制备荧光陶瓷主要通过高温煅烧工艺，具体步骤包括：球磨，球磨结束后，进行干压成型、冷等静压成型、真空煅烧、热等静压煅烧和退火处理。本发明制备的荧光陶瓷，具有高的激发与发射效率，物化性质稳定，适合高能量密度光连续激发使用，在照明或显示领域有较好的应用前景。

Description

一种用于照明或显示的荧光陶瓷及其制备方法
技术领域
本发明涉及一种用于照明或显示的荧光陶瓷，并提供了该荧光陶瓷的制备方法，属于发光材料领域。
背景技术
白光LED由于具有光效高、寿命长、节能环保、安全可靠等优点，目前在照明、显示等领域逐渐逐渐占据市场份额。实现白光LED的主要形式是半导体芯片激发荧光粉材料，具体的工艺为将荧光粉材料与有机树脂材料(如有机硅树脂、环氧树脂等)混合脱泡后，点涂到半导体芯片的表面，再经过固化成型后，即可制得白光LED。这种形式工艺简单，成本低，但是也存在诸多不可解决的问题，随着半导体芯片功率能量密度的增加，单位面积出射光能量升高，如激光的激射时，传统这种形式中的荧光粉的光衰减非常严重，同时有机树脂材料作为一种高分子材料，在长期的高能量、高温环境下分子链将会发生解聚，产生黄化现象，导致发光效率的下降，因此制备出物化性质稳定，耐高能量密度光连续激发使用的荧光材料，是实现超大功率白光LED照明或显示的关键环节。
发明内容
为解决上述技术问题，本发明提供一种用于照明或显示的荧光陶瓷，该荧光陶瓷由陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉通过高温烧结工艺制备而成；制备的荧光陶瓷，具有高的激发与发射效率，物化性质稳定，适合高能量密度光连续激发使用，在照明或显示领域有较好的应用前景。
所述的铝硅酸盐荧光粉化学式为(Ca1-xMx)1-y-zAl2Si2O8：yEu2+，zR，元素M为Mg，Sr，Ba中的一种，R为Ce3+，Mn4+，Dy3+，Tb3+中的一种，其中x，y，z为摩尔系数，范围0.01＜x＜1，0.2≤y≤0.7，0≤z≤0.6，y+z＜1，激发光谱范围250-480nm，发射光谱范围400-700nm；
所述的陶瓷原料粉体为MgAl2O4、Y2O3、MgAlON和AlN中的至少一种；
所述的烧结助剂为MgO、SiO2、TiO2和CaO中的至少一种；
所述的荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别为：70-90％、0.5-8％和2-29.5％；
本发明还提供上述荧光陶瓷的制备方法，具体步骤为：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca1-xMx)1-y-zAl2Si2O8：yEu2+，zR中各元素的比例，称取元素M的碳酸盐、CaCO3、Al2O3、SiO2、Eu2O3和元素R的氧化物作为原料，将称取的原料混合均匀，进行球磨，球磨时间为3-4小时，球磨速度100-130转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉还原气氛中进行高温煅烧，温度为1050-1450℃，时间为8-12小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别称取材料，加入球磨罐中进行球磨，球磨时间为5-20小时，球磨速度200-300转/分钟，球磨结束后，将材料进行干压成型，压力为80-150MPa，保压时间5-15分钟，干压结束后进行冷等静压成型，压力为200-400MPa，保压时间5-10分钟，冷等静压结束后，将材料进行真空煅烧，温度为1500-1750℃，时间为7-13小时，真空度10-1-10-4Pa，真空煅烧结束后进行热等静压煅烧，温度为1600-1700℃，时间为2-8小时，压力为150-200MPa，最后进行退火处理，温度为700-1000℃，时间为8-12小时，随后冷却至室温，即可制备所需的荧光陶瓷；
在上述方法中，所述的还原气氛由活性炭或者N2/H2提供。
有益效果：
1、本发明涉及的荧光陶瓷具有宽谱激发与发射，激发光谱范围250-480nm，发射光谱范围400-700nm；
2、本发明涉及的荧光陶瓷物化性质稳定，适合高能量密度光连续激发使用。
附图说明
图1是具体实施例1中制备的荧光陶瓷样品的激发和发射光谱
具体实施方式
结合实施案例对本发明做进一步详细说明，但本发明保护范围不限于所述内容。
实施例1：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca0.3Mg0.7)0.8Al2Si2O8：0.2Eu2+中各元素的比例，称取MgCO3、CaCO3、Al2O3、SiO2和Eu2O3作为原料，将称取的原料混合均匀，进行球磨，球磨时间为3小时，球磨速度120转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉活性炭所形成的还原气氛中进行高温煅烧，温度为1250℃，时间为8.5小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别为75％、3％和22％称取材料，加入球磨罐中进行球磨，球磨时间为13小时，球磨速度240转/分钟，球磨结束后，将材料进行干压成型，压力为100MPa，保压时间10分钟，干压结束后进行冷等静压成型，压力为270MPa，保压时间8分钟，冷等静压结束后，将材料进行真空煅烧，温度为1600℃，时间为8小时，真空度10-3Pa，真空煅烧结束后进行热等静压煅烧，温度为1690℃，时间为3小时，压力为180MPa，最后进行退火处理，温度为850℃，时间为9小时，随后冷却至室温，即可制备所需的荧光陶瓷；
实施例2：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca0.4Sr0.6)0.5Al2Si2O8：0.4Eu2+，0.1Ce3+中各元素的比例，称取SrCO3、CaCO3、Al2O3、SiO2、Eu2O3和CeO2作为原料，将称取的原料混合均匀，进行球磨，球磨时间为3.5小时，球磨速度120转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉活性炭所形成的还原气氛中进行高温煅烧，温度为1150℃，时间为9.5小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别为80％、2％和18％称取材料，加入球磨罐中进行球磨，球磨时间为12小时，球磨速度245转/分钟，球磨结束后，将材料进行干压成型，压力为110MPa，保压时间6分钟，干压结束后进行冷等静压成型，压力为300MPa，保压时间8分钟，冷等静压结束后，将材料进行真空煅烧，温度为1650℃，时间为8.5小时，真空度10-1Pa，真空煅烧结束后进行热等静压煅烧，温度为1650℃，时间为5小时，压力为150MPa，最后进行退火处理，温度为7900℃，时间为10小时，随后冷却至室温，即可制备所需的荧光陶瓷；
实施例3：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca0.9Sr0.1)0.3Al2Si2O8：0.25Eu2+，0.45Ce3+中各元素的比例，称取SrCO3、CaCO3、Al2O3、SiO2、Eu2O3和CeO2作为原料，将称取的原料混合均匀，进行球磨，球磨时间为3.5小时，球磨速度120转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉炉N2/H2所形成的还原气氛中进行高温煅烧，温度为1350℃，时间为8小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别为90％、0.5％和9.5％称取材料，加入球磨罐中进行球磨，球磨时间为5小时，球磨速度300转/分钟，球磨结束后，将材料进行干压成型，压力为80MPa，保压时间13分钟，干压结束后进行冷等静压成型，压力为280MPa，保压时间7分钟，冷等静压结束后，将材料进行真空煅烧，温度为1700℃，时间为8小时，真空度10-4Pa，真空煅烧结束后进行热等静压煅烧，温度为1680℃，时间为3小时，压力为180MPa，最后进行退火处理，温度为900℃，时间为10小时，随后冷却至室温，即可制备所需的荧光陶瓷；
实施例4：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca0.6Ba0.4)0.1Al2Si2O8：0.6Eu2+，0.3Dy3+)中各元素的比例，称取BaCO3、CaCO3、Al2O3、SiO2、Eu2O3和Dy2O3作为原料，将称取的原料混合均匀，进行球磨，球磨时间为4小时，球磨速度120转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉活性炭所形成的还原气氛中进行高温煅烧，温度为1400℃，时间为11小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别为70％、1％和29％称取材料，加入球磨罐中进行球磨，球磨时间为9小时，球磨速度300转/分钟，球磨结束后，将材料进行干压成型，压力为120MPa，保压时间13分钟，干压结束后进行冷等静压成型，压力为300MPa，保压时间8分钟，冷等静压结束后，将材料进行真空煅烧，温度为1500℃，时间为13小时，真空度10-4Pa，真空煅烧结束后进行热等静压煅烧，温度为1650℃，时间为5小时，压力为150MPa，最后进行退火处理，温度为950℃，时间为11小时，随后冷却至室温，即可制备所需的荧光陶瓷；
实施例5：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca0.5Ba0.5)0.3Al2Si2O8：0.5Eu2+，0.2Tb3+)中各元素的比例，称取BaCO3、CaCO3、Al2O3、SiO2、Eu2O3和Tb2O3作为原料，将称取的原料混合均匀，进行球磨，球磨时间为3.5小时，球磨速度120转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉N2/H2所形成的还原气氛中进行高温煅烧，温度为1050℃，时间为11小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别称取材料，加入球磨罐中进行球磨，球磨时间为10小时，球磨速度250转/分钟，球磨结束后，将材料进行干压成型，压力为140MPa，保压时间12分钟，干压结束后进行冷等静压成型，压力为300MPa，保压时间6分钟，冷等静压结束后，将材料进行真空煅烧，温度为1650℃，时间为11小时，真空度10-2Pa，真空煅烧结束后进行热等静压煅烧，温度为1600℃，时间为6.5小时，压力为200MPa，最后进行退火处理，温度为950℃，时间为8.5小时，随后冷却至室温，即可制备所需的荧光陶瓷。

Claims (6)

1.一种用于照明或显示的荧光陶瓷，其特征在于：所述的荧光陶瓷由陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉通过高温烧结工艺制备而成；所述的铝硅酸盐荧光粉化学式为(Ca1-xMx)1-y-zAl2Si2O8：yEu2+，zR，元素M为Mg，Sr，Ba中的一种，R为Ce3+，Mn4+，Dy3+，Tb3+中的一种，其中x，y，z为摩尔系数，范围0.01＜x＜1，0.2≤y≤0.7，0≤z≤0.6，y+z＜1，激发光谱范围250-480nm，发射光谱范围400-700nm。
2.根据权利要求1所述的用于照明或显示的荧光陶瓷，其特征在于：所述的陶瓷原料粉体为MgAl2O4、Y2O3、MgAlON和AlN中的至少一种。
3.根据权利要求1所述的用于照明或显示的荧光陶瓷，其特征在于：所述的烧结助剂为MgO、SiO2、TiO2和CaO中的至少一种。
4.根据权利要求1所述的用于照明或显示的荧光陶瓷，其特征在于：所述的荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别为：70-90％、0.5-8％和2-29.5％。
5.根据权利要求1所述的用于照明或显示的荧光陶瓷，包括以下实现步骤：
A.硅铝酸盐荧光粉的制备：按照化学式(Ca1-xMx)1-y-zAl2Si2O8：yEu2+，zR中各元素的比例，称取元素M的碳酸盐、CaCO3、Al2O3、SiO2、Eu2O3和元素R的氧化物作为原料，将称取的原料混合均匀，进行球磨，球磨时间为3-4小时，球磨速度100-130转/分钟；球磨结束后，将原料装入坩埚中，在高温固相炉还原气氛中进行高温煅烧，温度为1050-1450℃，时间为8-12小时，煅烧结束后，将高温固相炉温度降至室温时，打开炉膛，取出材料，粉碎过筛，即可制备所需的铝硅酸盐荧光粉；
B.荧光陶瓷的制备：按照荧光陶瓷中的陶瓷原料粉体、烧结助剂和铝硅酸盐荧光粉的质量配比分别称取材料，加入球磨罐中进行球磨，球磨时间为5-20小时，球磨速度200-300转/分钟，球磨结束后，将材料进行干压成型，压力为80-150MPa，保压时间5-15分钟，干压结束后进行冷等静压成型，压力为200-400MPa，保压时间5-10分钟，冷等静压结束后，将材料进行真空煅烧，温度为1500-1750℃，时间为7-13小时，真空度10-1-10-4Pa，真空煅烧结束后进行热等静压煅烧，温度为1600-1700℃，时间为2-8小时，压力为150-200MPa，最后进行退火处理，温度为700-1000℃，时间为8-12小时，随后冷却至室温，即可制备所需的荧光陶瓷。
6.根据权利要求5所述的用于照明或显示的荧光陶瓷的实现步骤，其特征在于：所述的还原气氛由活性炭或者N2/H2提供。
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107739153A (zh) * 2017-11-06 2018-02-27 南昌大学 一种具有高效绿光发射的透明玻璃及制备方法
CN110056838A (zh) * 2019-05-27 2019-07-26 轻工业部南京电光源材料科学研究所 一种紫外上转换植物保护灯及其制备方法
CN111517804A (zh) * 2020-04-27 2020-08-11 中国科学院上海硅酸盐研究所 一种氮化物红色复相荧光陶瓷及其制备方法
CN114921244A (zh) * 2022-05-24 2022-08-19 营口理工学院 一种纺锤棒状MgAl2O4:Tb3+荧光粉及制备方法
CN115784717A (zh) * 2022-12-08 2023-03-14 中国科学院上海硅酸盐研究所 一种铝酸锶长余辉发光陶瓷及其制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006316200A (ja) * 2005-05-13 2006-11-24 Pioneer Electronic Corp 蛍光体およびガス放電表示装置
CN101735807A (zh) * 2009-12-11 2010-06-16 四川大学 一种近紫外激发的led用铝硅酸盐蓝色荧光粉及其制备方法
CN101935204A (zh) * 2009-10-23 2011-01-05 郑子山 一种超长余辉蓝色蓄光陶瓷材料及其制备方法
CN102071015A (zh) * 2011-01-21 2011-05-25 中国计量学院 一种铕、锰共掺激活的白光荧光粉及其制备方法
CN104291796A (zh) * 2014-09-23 2015-01-21 上海三思电子工程有限公司 一种led用透明荧光陶瓷的制备方法
CN106010516A (zh) * 2016-06-28 2016-10-12 东台市天源荧光材料有限公司 一种锰激发的铝硅酸盐荧光粉及其制备方法
CN106281315A (zh) * 2016-01-27 2017-01-04 轻工业部南京电光源材料科学研究所 微弧光传感器用深红/近红外下转换荧光材料及其制备方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006316200A (ja) * 2005-05-13 2006-11-24 Pioneer Electronic Corp 蛍光体およびガス放電表示装置
CN101935204A (zh) * 2009-10-23 2011-01-05 郑子山 一种超长余辉蓝色蓄光陶瓷材料及其制备方法
CN101735807A (zh) * 2009-12-11 2010-06-16 四川大学 一种近紫外激发的led用铝硅酸盐蓝色荧光粉及其制备方法
CN102071015A (zh) * 2011-01-21 2011-05-25 中国计量学院 一种铕、锰共掺激活的白光荧光粉及其制备方法
CN104291796A (zh) * 2014-09-23 2015-01-21 上海三思电子工程有限公司 一种led用透明荧光陶瓷的制备方法
CN106281315A (zh) * 2016-01-27 2017-01-04 轻工业部南京电光源材料科学研究所 微弧光传感器用深红/近红外下转换荧光材料及其制备方法
CN106010516A (zh) * 2016-06-28 2016-10-12 东台市天源荧光材料有限公司 一种锰激发的铝硅酸盐荧光粉及其制备方法

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107739153A (zh) * 2017-11-06 2018-02-27 南昌大学 一种具有高效绿光发射的透明玻璃及制备方法
CN110056838A (zh) * 2019-05-27 2019-07-26 轻工业部南京电光源材料科学研究所 一种紫外上转换植物保护灯及其制备方法
CN111517804A (zh) * 2020-04-27 2020-08-11 中国科学院上海硅酸盐研究所 一种氮化物红色复相荧光陶瓷及其制备方法
CN111517804B (zh) * 2020-04-27 2021-08-31 中国科学院上海硅酸盐研究所 一种氮化物红色复相荧光陶瓷及其制备方法
CN114921244A (zh) * 2022-05-24 2022-08-19 营口理工学院 一种纺锤棒状MgAl2O4:Tb3+荧光粉及制备方法
CN115784717A (zh) * 2022-12-08 2023-03-14 中国科学院上海硅酸盐研究所 一种铝酸锶长余辉发光陶瓷及其制备方法

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