CN106398688B - 一种应用于新生儿黄疸病治疗led器件中的蓝光荧光粉及其合成方法 - Google Patents
一种应用于新生儿黄疸病治疗led器件中的蓝光荧光粉及其合成方法 Download PDFInfo
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Abstract
一种应用于新生儿黄疸病治疗LED器件中的蓝光荧光粉及其合成方法，其化学组成式为：SiO2‑Mg1‑xCl2:Eu2+ x；其中0.001≤x≤0.90。上述蓝色荧光粉的合成方法，包括如下步骤：将MgO、SiO2和Eu2O3在500~1000℃，空气气氛中煅烧1~5h，形成荧光粉A；再次将荧光粉A研磨后，将荧光粉A在500~1000℃的还原气氛中煅烧1~5h，形成最终的蓝光荧光粉。所述反应是在陶瓷坩埚和管式还原炉中进行。（1）本发明所得的荧光粉为石英型结构，所用原料无毒、价廉易得；合成方法采用高温固相反应，具有合成方法简单，合成时间短等优点。（2）本发明产品所含紫外线含量占整体荧光发射量的千分之一不到，且较完美地覆盖了光照治疗黄疸病所需的辐射范围，提高了能量利用率与安全性。
Description
技术领域
本发明属于无机材料的稀土掺杂荧光粉，具体地说，涉及一种应用于新生儿黄疸病治疗LED器件中的蓝光荧光粉及其合成方法。
背景技术
光照治疗是新生儿黄疸病治疗中的一种方法。由于光照治疗不像药物治疗对新生儿产生毒性，也不像换血疗法一样对新生儿产生过重的身体负担，所以它是新生儿黄疸病治疗中最常用的方法。光照疗法中使用蓝光，作为蓝光光源，最常用的为蓝色荧光粉与激发芯片组合而成的LED器件。所以蓝光荧光粉的开发有着广阔的应用前景。
患黄疸病的新生儿皮肤首先吸收蓝光，然后蓝光将皮肤中的胆红素氧化掉，使之产生一种极性较强、可随尿液排出的氧化物而从身体中代谢出去。400-520nm范围内的蓝光对此治疗都有效，特别是460±10nm的蓝光与胆红素的吸收光谱更加匹配。目前用于此光照治疗的蓝光荧光粉都存在既发射蓝光，也发射一定紫外光的问题。首先，这浪费了一定的能量，不环保。其次，紫外线辐射对于新生儿的伤害较大，不利于健康。所以开发新型紫外线含量低的、高效的蓝光荧光粉是目前急需解决的问题。
发明内容
本发明的目的在于克服现有技术的缺点，提供一种紫外线含量低，用于新生儿黄疸病治疗LED器件中的蓝光荧光粉及其合成方法。
为了实现上述目的，本发明采用如下技术方案：
一种蓝光荧光粉，其化学组成式为：SiO2-Mg1-xCl2:Eu2+ x；其中0.001≤x≤0.90。
上述蓝色荧光粉的合成方法，包括如下步骤：将MgO、SiO2和Eu2O3在500～1000℃，空气气氛中煅烧1～5h，形成荧光粉A；再次将荧光粉A研磨后，将荧光粉A在500～1000℃的还原气氛中煅烧1～5h，形成最终的蓝光荧光粉。所述反应是在陶瓷坩埚和管式还原炉中进行。
与现有的荧光粉相比，本发明具有如下有益效果：
(1)本发明所得的荧光粉为α-石英型结构，所用原料无毒、价廉易得；合成方法采用高温固相反应，具有合成方法简单，合成时间短等优点。
(2)本发明产品所含紫外线含量占整体荧光发射量的千分之一不到，且较完美地覆盖了光照治疗黄疸病所需的辐射范围，提高了能量利用率与安全性。
附图说明
图1为本发明实验例1～3所制备的蓝色荧光粉的XRD图。
图2为本发明实施例1所制备的蓝色荧光粉的荧光激发光谱图。
图3为本发明实施例1所制备的蓝色荧光粉的荧光发射光谱图。
图4为本发明实施例1所制备的蓝色荧光粉的荧光发射变温光谱图。其中，图4中，是荧光粉的升温曲线，曲线从上到下，温度升高，荧光强度降低。
图5为本发明实施例1所制备的蓝色荧光粉的漫反射谱图。
具体实施方式
为更好理解本发明，下面结合实施例对本发明做进一步地详细说明，但是本发明要求保护的范围并不局限于实例表示的范围。
实施例1：蓝色荧光粉的制备
将0.01mol的MgO、0.02mol的NH4Cl、0.03mol的SiO2和1.2×10—4mol(0.3mol％)的Eu2O3放入玛瑙研钵中研磨1小时至混合均匀。放入陶瓷坩埚中，然后在高温炉中，加热至1000℃，保温2小时，然后自然冷却。取出样品后放入玛瑙研钵，再加入0.02mol的NH4Cl，研磨至充分混匀。然后放入陶瓷坩埚中，装入管式还原炉中，在H2：N2体积比例为1:9的还原气氛中，加热至1000℃，保温2小时，然后自然冷却，取出后研磨再进行后续测试。产品的XRD衍射峰如图1所示；荧光激发光谱如图2所示；荧光发射光谱如图3所示；荧光发射变温光谱图如图4；蓝色荧光粉的漫反射谱图如图5。如图1中谱线1所示，所有衍射峰都能与底部的α-石英型结构的标准峰(JCPDS No.46-1045)相对应，由此可知所得产物为纯的α-石英型结构。将此荧光粉紫外光部分与整体荧光发射部分分别作积分，然后相除得到紫外光部分占整个荧光发射部分的比例，该比例不足0.1％，证明本荧光粉紫外辐射极少，安全性高。
实施例2：蓝色荧光粉的制备
将0.01mol的MgO、0.02mol的NH4Cl、0.03mol的SiO2和2.4×10—4mol(0.6mol％)的Eu2O3放入玛瑙研钵中研磨1小时至混合均匀。放入陶瓷坩埚中，然后在高温炉中，加热至1000℃，保温2小时，然后自然冷却。取出样品后放入玛瑙研钵，再加入0.02mol的NH4Cl，研磨至充分混匀。然后放入陶瓷坩埚中，装入管式还原炉中，在H2：N2体积比例为1:9的还原气氛中，加热至1000℃，保温2小时，然后自然冷却，取出后研磨再进行后续测试。产品的XRD衍射峰如图1所示。如图1中谱线2所示，所有衍射峰都能与底部的α-石英型结构的标准峰(JCPDS No.46-1045)相对应，由此可知所得产物为纯的α-石英型结构。实施例2的荧光激发光谱图，荧光发射光谱图，荧光发射变温光谱图，蓝色荧光粉的漫反射谱图均与实施例1一致。
实施例3：蓝色荧光粉的制备
将0.01mol的MgO、0.02mol的NH4Cl、0.03mol的SiO2和1.2×10—4mol(0.3mol％)的Eu2O3放入玛瑙研钵中研磨1小时至混合均匀。放入陶瓷坩埚中，然后在高温炉中，加热至900℃，保温2小时，然后自然冷却。取出样品后放入玛瑙研钵，再加入0.02mol的NH4Cl，研磨至充分混匀。然后放入陶瓷坩埚中，装入管式还原炉中，在H2：N2体积比例为2:8的还原气氛中，加热至900℃，保温1.5小时，然后自然冷却，取出后研磨再进行后续测试。产品的XRD衍射峰如图1所示。如图1中谱线3所示，所有衍射峰都能与底部的α-石英型结构的标准峰(JCPDSNo.46-1045)相对应，由此可知所得产物为纯的α-石英型结构。实施例3的荧光激发光谱图，荧光发射光谱图，荧光发射变温光谱图，蓝色荧光粉的漫反射谱图均与实施例1一致。
Claims (1)
1.一种蓝光荧光粉，其特征在于由如下方法制成：
将0.01mol的MgO、0.02mol的NH4Cl、0.03mol的SiO2和1.2×10—4mol的Eu2O3放入玛瑙研钵中研磨1小时至混合均匀；放入陶瓷坩埚中，然后在高温炉中，加热至1000℃，保温2小时，然后自然冷却；取出样品后放入玛瑙研钵，再加入0.02mol的NH4Cl，研磨至充分混匀；然后放入陶瓷坩埚中，装入管式还原炉中，在H2：N2体积比例为1:9的还原气氛中，加热至1000℃，保温2小时，然后自然冷却，取出后研磨再进行后续测试。
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| CN1677695A (zh) * | 2004-03-29 | 2005-10-05 | 宏齐科技股份有限公司 | 白光发光二极管单元 |
| CN101517035A (zh) * | 2006-09-27 | 2009-08-26 | 奥斯兰姆奥普托半导体有限责任公司 | 发射辐射装置 |
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| CN1640985A (zh) * | 2004-01-06 | 2005-07-20 | 孙家跃 | 365nm紫外线激活的颜色可调蓝色荧光材料 |
| CN1677695A (zh) * | 2004-03-29 | 2005-10-05 | 宏齐科技股份有限公司 | 白光发光二极管单元 |
| CN101517035A (zh) * | 2006-09-27 | 2009-08-26 | 奥斯兰姆奥普托半导体有限责任公司 | 发射辐射装置 |
| CN102226086A (zh) * | 2011-04-23 | 2011-10-26 | 龙南县顺德明辉荧光材料有限责任公司 | 一种稀土卤硅酸盐红色长余辉荧光粉及其制备方法 |
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