CN101386784B - 一种微波激励低温液相燃烧合成纳米荧光粉的制备方法 - Google Patents
一种微波激励低温液相燃烧合成纳米荧光粉的制备方法 Download PDFInfo
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Abstract
本发明涉及一种PDP用EuxBa1-xMgAl10O17纳米荧光粉的微波激励液相燃烧合成方法，属发光材料领域。本发明是由含Ba2+、Mg2+、Al3+的硝酸盐与尿素(或甘氨酸，卡巴胺)以摩尔比1∶1.5的比例组合，并加入相应的改性剂，将混合均匀的溶液置于2.45GHz的微波装置中进行微波激励液相燃烧合成反应，得到纳米级的六方晶系EuxBa1-xMgAl10O17荧光粉。本发明的特点是：工艺简单，反应迅速，点燃温度低，不需要还原性气氛保护，燃烧合成反应在几分钟内即可完成，所制得的荧光粉晶粒尺寸为30-40nm；本发明合成的荧光粉产物纯净、结晶优良、发光效率高，不需要球磨粉碎和后处理即可直接应用。而且本发明具有节能、环保、高效、可靠等优势，适合工业化生产。
Description
技术领域
本发明涉及一种PDP用EuxBa1-xMgAl10O17纳米荧光粉的微波激励低温液相燃烧合成方法，属发光材料领域。
背景技术
等离子体显示(Plasma Display Panel，简称PDP)具有显示面积大、高清晰、超薄、超轻、视角宽(超过160°)、响应快、不受磁场干扰、可显示1670万种以上色彩等一系列突出优点，在高清晰平面显示器领域占有绝对优势，被世界公认是实现壁挂式高清晰平板显示的首选技术。
对于PDP而言，荧光粉是决定其显示质量的关键材料，它关系着显示器件的亮度、色度、分辨率和图像质量等重要性能指标。
目前商用荧光粉一般采用传统的高温固相法合成，需要1600℃以上的高温长时间反应，不但能耗大、成本高，而且在此高温下产物易烧结且颗粒粗大，需球磨粉碎，从而导致晶形破坏而严重损害荧光粉的发光性能。因此，为了解决现有问题，低温合成工艺的研究与开发已成为迫切需要。
由于纳米微粒具有小尺寸效应、表面效应、量子尺寸效应和宏观量子隧道效应等使得它在光、电、磁等方面呈现常规材料不具备的光学和电学特性。当荧光粉基质的颗粒尺寸小到纳米级范围内，其中掺杂的激活离子的发光和动力学性质就会发生改变，从而影响其光吸收、激发寿命、能量传递、光量子效率和浓度猝灭等性质而提高荧光粉的性能。
湿化学法作为一种制备超细纳米粉的方法正成为各国材料科学家研究的热点。该法由于原料在溶液中反应，因而组分能达到分子、离子级别上的均匀混合，且合成温度低，成分容易精确控制。
常见的湿化学法包括共沉淀法、Sol-gel法(溶胶—凝胶法)、水热合成法、液相燃烧法等。共沉淀法和Sol-gel法工艺复杂、生产周期长、过程影响因素多。近年来，微波激励液相燃烧法作为一种快速、高效的制备纳米粉体方法，可用来合成结晶优良、粒径分布窄、形貌可控且纯度高的纳米粉体。
本发明目的在于提出一种制备PDP纳米蓝色荧光粉(通式为EuxBa1-xMgAl10O17，简称BAM)的方法，从而开发出低成本、易于产业化、且产物性能优良的制备BAM的方法。该方法最主要特点是采用微波激励低温液相燃烧合成BAM纳米蓝色荧光粉。
微波作为一种迅速而有效的加热方式，在加速化学反应、提高产品质量等方面发挥了巨大的作用，并且日益广泛用于新材料的合成领域。与常规加热相比，微波加热不需热的传导和对流，在极短时间内使介质分子达到活化状态，加剧分子的运动与碰撞，大大加快反应速度，缩短反应周期，并因内外同时加热，体系受热均匀，在合成反应过程中不存在温度梯度，从而保证合成产品的均一性。
为达到上述目的，本发明采用如下技术方案：
本发明的微波激励的液相介质为金属硝酸盐、尿素(或甘氨酸)与适量添加剂所组成的混合溶液。金属硝酸盐、尿素(或甘氨酸，卡巴胺)、添加剂(适量)等所组成的反应物在水溶液中达到原子级的均匀混合，保证了稀土离子激活剂均匀分布在基质晶格中，从而可获得高效荧光材料。
将均匀混合的溶液装入反应装置并置入微波设备中进行微波激励低温燃烧合成反应。微波激励设备采用单模微波辐射设计，其微波强度恒定，能够产生持续的微波场，使样品受到均衡的微波辐射强度，通过调节持续波的输出功率来改变能量强度。
按化学式EuxBa1-xMgAl10O17的成分比例，称取摩尔比为1：1.2金属离子的硝酸盐和有机燃料放入微波装置，通过红外控温于550-600℃，燃烧合成反应5-10min，得到晶粒尺寸为30-40nm的纳米EuxBa1-xMgAl10O17荧光粉。微波反应条件为：微波频率为2.45-3.5GHz，微波功率为800-1200W，反应时间为5-10分钟，且用红外控温仪精确控温于550-600℃。荧光粉的基质晶相组成纯净，且其晶粒尺寸为30-60纳米。
具体包括如下步骤：
(1)，按化学式EuxBa1-xMgAl10O17称取摩尔比为1-3％光谱纯级的稀土氧化物，摩尔比为97-99％分析纯级的金属硝酸盐；
(2)，将稀土氧化物用30-60％的硝酸溶解，然后将称取的其余样品放入其中，最后加入适量的去离子水并不断搅拌，直至原料充分溶解；
(3)，加入甘氨酸，卡巴胺有机燃料尿素；有机燃料与硝酸盐的摩尔比为1.2-1.5；
(4)，加入0.5-1％的添加剂、助熔剂、形貌控制剂；
(5)，将混合均匀的溶液置入微波设备中进行微波激励低温燃烧合成反应，通过控制设定的温度及微波激励的时间获得目标荧光粉产物。
本发明与现有技术相比，具有如下优点：
(1)微波为整体、内部加热，反应物受热均匀，而且升温速度快，大大缩短反应时间，具有高效、节能的优势；
(2)合成的产物纯净、结晶优良、发光效率高，产物的激发光谱、发射光谱完全符合使用要求；
(3)产物颗粒为球形、尺寸大小为30-40nm，不需要球磨粉碎和后处理即可直接应用；
(4)生产工艺简单，生产效率高，易于实现产业化。因为反应一旦点燃，则不需要外部再提供任何能量，整个燃烧过程完全依靠自身放出的热量自动、快速地完全。
因此，采用微波激励低温燃烧合成技术，可以实现高度纯净、结晶优良、发光效率高的EuxBa1-xMgAl10O17荧光粉的低成本制备。
本发明制备的纳米荧光粉既可用于等离子显示(PDP)，亦可用于场发射显示(EED)、高分辨投影电视(PTVs)、发光二极管(LED)和无汞荧光灯。
附图说明
图1为制备的Eu0.15Ba0.85MgAl10O17荧光粉的XRD图谱，表明产物为纯相；
图2为制备的荧光粉的SEM像，可见颗粒为球形，尺寸大小25-40nm；
图3为制备的Eu0.1Ba0.9MgAl10O17荧光粉的激发光谱，可见其在真空紫外至紫外区均有良好的吸收；
图4为制备的Eu0.1Ba0.9MgAl10O17荧光粉的发射光谱，发射峰为450nm，为标准的蓝光发射。
具体实施方式
下面以实施例的方式进一步阐明本发明，而非仅局限于实施例。
实施例1
初始原料Eu2O3为光谱纯，Ba(NO3)2、Mg(NO3)2·6H2O、Al(NO3)3·9H2O及CO(NH2)2为分析纯。按Ba0.85MgAl10O17∶0.15Eu化学计量配比，用分析天平精确称取上述试剂。
在烧杯中，首先用浓硝酸(AR)将Eu2O3充分溶解，然后按摩尔比为0.9：1：10称取Ba(NO3)2、Mg(NO3)2·6H2O、Al(NO3)3·9H2O放入其中。最后加入适量的去离子水并不断搅拌，直至原料充分溶解，获得均匀混合的澄清透明溶液。
将溶液置入微波设备中进行微波激励低温燃烧合成反应。通过红外控温仪精确控温于550℃。微波激励频率为2.45GHz，微波功率为800W，反应时间为10分钟。反应完毕后，即得泡沫状白色粉体产物。产物经X射线粉末衍射分析，结果表明产物为纯相，如图1所示。产物的场发射扫描电镜像如图2所示，表明颗粒为球形，且尺寸为30nm左右。
实施例2
初始原料Eu2O3为光谱纯，Ba(NO3)2、Mg(NO3)2·6H2O、Al(NO3)3·9H2O及CO(NH2)2为分析纯，并称取一定量的AlF3作助熔剂。
按Ba0.9MgAl10O17∶0.1Eu化学计量配比，用分析天平精确称取上述试剂。
在烧杯中，首先用浓硝酸(AR)将Eu2O3充分溶解，然后将按摩尔比为0.9：1：10称取Ba(NO3)2、Mg(NO3)2·6H2O、Al(NO3)3·9H2O放入其中。最后加入适量的去离子水并不断搅拌，直至原料充分溶解，获得均匀混合的澄清透明溶液。
将溶液置入微波设备中进行微波激励低温燃烧合成反应。通过红外控温仪精确控温于600℃。微波激励频率为2.45GHz，微波功率为800W，反应时间为10分钟。反应完毕后，即得泡沫状白色粉体产物。获得的产物经过国家同步辐射实验室的真空紫外光谱性能测试，其激发光谱如图3所示，可见其在真空紫外至紫外区均有良好的吸收；其发射光谱如图4所示，其发射峰为450nm，为标准的蓝光发射。
Claims (1)
1.一种微波激励低温液相燃烧合成纳米EuxBa1-xMgAl10O17荧光粉的制备方法，其特征在于：按化学式EuxBa1-xMgAl10O17的成分比例，称取摩尔比为1∶1.2金属离子的硝酸盐和有机燃料放入微波装置，通过红外控温于550-600℃，燃烧合成反应5-10min，得到晶粒尺寸为30-40nm的纳米EuxBa1-xMgAl10O17荧光粉；
其中X的取值为0.1和0.15。
微波反应条件为：微波频率为2.45-3.5GHz，微波功率为800-1200W，反应时间为5-10分钟，且用红外控温仪精确控温于550-600℃。
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Patent Citations (4)
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| CN1294170A (zh) * | 1999-10-29 | 2001-05-09 | 重庆建筑大学 | 长余辉磷光粉燃烧制备法 |
| CN1396234A (zh) * | 2002-06-14 | 2003-02-12 | 中国地质大学（武汉） | 一种制备铝酸盐长余辉发光粉的方法 |
| CN1654424A (zh) * | 2004-12-31 | 2005-08-17 | 济南大学 | 钇铝石榴石粉体的制备方法 |
| CN1940012A (zh) * | 2005-09-28 | 2007-04-04 | 北京工商大学 | 微波燃烧－发泡法制备不球磨长余辉粉体材料 |
Non-Patent Citations (2)
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| 孙彦彬等."稀土发光材料的合成方法".《稀土》.2003,第24卷(第1期),43-47. |
| 陈哲."Ba/Mg比值对(BaxMg)2/(x+1)Al10O17:Eu2+晶体结构和发光特性的影响".《发光学报》.2007,第27卷(第1期),111-115. |
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| CN101386784A (zh) | 2009-03-18 |
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