CN1121471C - 对潮湿不敏感的电致发光荧光物质 - Google Patents

对潮湿不敏感的电致发光荧光物质 Download PDF

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CN1121471C
CN1121471C CN99101071A CN99101071A CN1121471C CN 1121471 C CN1121471 C CN 1121471C CN 99101071 A CN99101071 A CN 99101071A CN 99101071 A CN99101071 A CN 99101071A CN 1121471 C CN1121471 C CN 1121471C
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K·A·克利内丁斯特
R·F·克拉克
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Abstract

本发明涉及一种其上涂有氮化铝共形涂层的荧光物质颗粒。共形涂层意指沿单个颗粒表面外形所形成的涂层。形成这种荧光物质的方法包含的步骤有：将惰性气体引入反应容器；将荧光物质颗粒引入反应容器；将反应容器加热到反应温度；将氮化物涂覆用前体引入反应容器；将一种共反应剂引入反应容器；维持惰性气体流、共反应剂流和前体供应一段时间，足以涂覆荧光物质颗粒。利用这种方法产生的用氮化物涂覆的荧光物质颗粒在高湿度(即大于95%)条件下使用100小时之后仍具有优异的效率标称值和强亮度值。

Description

对潮湿不敏感的电致发光
荧光物质
本申请对于1998.1.12申请的第60/072510号临时专利申请的权益提出权利要求。
本发明涉及一些涂覆的颗粒，特别是涉及其上有共形涂覆的颗粒。更具体说本发明涉及荧光物质，特别涉及其上具有涂覆层的电致发光的荧光物质，该涂覆层保护荧光物质免于吸收湿气和大力增加寿命和效率。
由4585673、4825124、5080928、5118529、5156885、5220243、5244750和5418062号美国专利公知一些带涂覆层的荧光物质。由上面提到的某些专利可知，一种涂料前体和氧可以用于涂覆保护性的涂层。例如参阅5244750和4585673号关国专利。在这些专利的几个其它专利中的涂覆方法是采用化学蒸汽沉积，利用水解来涂覆保护性的涂覆层。另据报道，在大气压下可采用化学蒸汽沉积在硅、琉态碳和玻璃基片上由六(二甲基酰胺)二铝和氨来沉积氮化铝涂层薄膜。例如参阅在“材料资源杂志”(Journal Material Resources)的第6卷第1期(1991.1)由Gordon等人所著“在200℃～250℃下氮化铝薄膜的大气压化学蒸汽沉积”；以及在“Journal Material Resources”第7卷第7期(1992.7)由Gordon等人所著“氮化铝薄膜的化学蒸汽沉积”，如果能研制一种在无水或水蒸汽存在进行的涂覆方法，则在本技术领域中被认为是一种进展。能增加这样涂覆的荧光物质的效率和寿命是本技术领域的又一进展。能提供不依赖氧的涂覆层和方法是本技术领域的更进一步的进展。提供一种具有氮化铝涂覆层的电致发光荧光物质又是本领域的更进一步的进展。
因此，本发明的一个目的是消除现有技术存在的缺点。
本发明的另一目的是改进涂覆荧光物质的操作。
本发明的再一目的是提供一种不使用水或水蒸汽或氧的荧光物质涂覆方法。
根据本发明通过提供一种其上涂覆有氮化铝共形涂层的荧光物质颗粒来实现这些目的。共形涂层是指沿单个颗粒的表面外形所形成的涂层。
通过提供一种制备这种荧光物质的方法来进一步实现这些目的，该方法包含的步骤是：向装有荧光物质颗粒的反应容器中引入惰性气体；将所述反应容器加热到反应温度；向所述反应容器中引入氮化物涂覆用前体六(二甲基酰胺)二铝；向所述反应容器引入一种共反应剂无水氨；维持所述惰性气体流、共反应剂流和前体供应一段时间，足以用所述耐潮湿氮化物涂覆所述荧光物质颗粒。
利用这种方法产生的用氮化物涂覆的荧光物质颗粒在高湿度(＞95％)下使用100小时之后，在灯具中仍具有优异的效率标称值和很强的亮度值，亮度大于58.2坎/米2。
图1是前体输送速率与温度倒数的关系图；
图2是按照蒸汽压曲线表示的相同数据的关系图；以及
图3是前体输送速率与载气流量的关系图；
为了更好地理解本发明以及其它和另外的目的-优点和能力，结合上面介绍的附图，参阅如下的说明和肝提出的权利要求。
在本发明的一优选实施例中，在一气体流化床反应容器中进行涂覆反应，该反应容器包含一个1英寸外径(2.54厘米)玻璃管，其具有一粗孔率的烧结玻璃板作为气体分配板。肝使用的荧光物质是由Osram SylvanlaInc.，Towanda PA可购得的723型电致发光荧光物质(ZnS∶Cu)，通过惰性气体例如氮的注入使荧光物质流化。通过氨与六(二甲基酰胺)二铝(Al2(N(CH3)2)6)与氨反应形成氮化物涂覆层(其可包含一定量的氢以及氮化铝)。由Strem Chemicals，Newburyport，MA得到氮化铝前体，并装在不锈钢鼓泡器中。将该鼓泡器维持在100℃下，利用纯化的氮气作载体将前体输送到反应容器中。夹带前体的氮通过维持在超过鼓泡器温度20℃～30℃温度为130-140℃的管道向上穿过烧结玻璃分配板。由MathesonChemicals，Gloucester，MA得到的无水氨共反应剂在经由具有烧结玻璃板的中心玻璃管进入流化床之前通过一Unit(单位)质量流量控制器。氨在进入该流化床之前由纯化氮稀释。此外，氮载气通过Centorr纯化器纯化，接着Matheson Nanochem气体纯化器纯化。氨也通过Nanochem纯化器。
由不锈钢管道和附属装置构成气体操纵系统。在玻璃反应器部件和气体管道之间采用玻璃-金属密封件。
在良好密封的系统上进行四次涂覆试验。在每一试验中荧光物质重40克，鼓泡器温度为110℃。涂覆温度(即反应容器温度)、时间和气体流量表示在表I中。
                                      表I
试验编号 温度(℃) 时间(小时) N2(载气)流量(标准立方厘米/分)   NH3流量(标准立方厘米/分) N2(稀释剂)流量(标准立方厘米/分)
L2503-12   200   4.5     1000     200     300
L2503-13   150   5.0     500     100     150
L2503-14   150   20.0     250     200     100
L2503-16   225   12     500     100     150
在涂覆试验之前，通过利用作为载气的以1000标准立方厘米/分流动的高纯氮的输送测量，在95℃～120℃的温度下测定氮化物前体的蒸汽压力。然后按100℃的鼓泡器温度，以10到1000标准立方厘米/分的载气流量测定输送速率。结果表示在图1中。图2包含按照蒸汽压力表示的相同数据。以100℃的鼓泡器温度的载气流为函数得到的输送数据表示在图3中。这些图表明，蒸汽压力是足够高到可利用鼓泡器作为将化学试剂输送到流化床反应容器的实用装置。在两个数量级(10-1000标准立方厘米/分N2)的范围内输送数据对于流量曲线的线性关系表明，这种方式适合于前体输送。
在表II中表示了：以总试样重量的百分值表示的铝含量(％Al)、B.E.T表面面积(S.A.(米2/克)、根据用化学分析电子光谱(ESCA)测定的百分覆盖率(％覆盖率)、根据以中性粒子溅射质谱(SNMS)及以SiO2为参考材料测量得出的还似涂层厚度。
                         表II
试验编号     ％Al     S.A.(米2/克)   ％覆盖率 厚度(埃)
L2503-12     2.9     0.07     99     2700
L2503-13     1.5     0.05     98     800
L2503-14     2.5     0.06     99     2200
L2503-16     3.3     0.05     100     4300
将表1和表2及图1中的数据进行比较，可以看出，在流化床内基本上所有的前体反应形成实际上覆盖所有荧光物质颗粒的涂覆层。X射线光电子光谱(XPS)表面分析表明有相当高的表面氧浓度，该结果与CVD沉积的氮化铝的公知的表面反应性相一致。然而，涂覆的荧光物质的SNMS分析已经表明，在相对低的氧信号电平和Zn、S、Al和N的信号电平之间没有明显的相互关系，这表明与氮化铝涂覆层没有特别关联的相对恒定的氧本底。此外，如在表III中所示，EDS分析表明，相对的氧浓度与在纯AlN试样中发现的氧浓度是可比的。
                           表III
                       根据EDS的原子成分(％)
试验编号     Al     N     O     Zn     S
L2503-12     16     71     5.1     4.3     2.6
L2503-14     18     70     3.6     4.5     3.3
L2503-16     20     70     2.8     4.1     1.8
纯AlN     28     67     4.8     …     …
制作包含未涂覆的荧光物质以及由每次试验得到的经涂覆的荧光物质的电致照明灯具。将灯具封装在一种透水材料Mylar中，使得可以测定和比较各种材料对于湿度的灵敏度。在两种环境下即相对湿度小于10％和相对湿度大于95％的条件下使相同的灯具在100伏和400赫下运行。还测定效率(流明/瓦)。这些结果概括在表IV中。
                                     表IV
试验编号   效率(流明/瓦)         相对湿度＜10％的亮度(坎/m2)0小时           24小时          100小时       相对湿度＞95％的亮度(坎/m2)0小时           24小时          100小时
L2503-12     5.26   77.4   75.4   68.5   78.8   80.9   60.3
L2503-13     4.23   89.1   85.3   75.4   89.8   90.5   20.9
L2503-14     4.26   77.4   75.7   66.5   76.7   75.0   60.0
L2503-16     5.90   78.1   74.3   66.8   78.5   80.5   75.0
未涂覆的     1.75   102.4   108.3   85.3   104.5   34.3   12.7
灯具性能数据清楚地表明，当适当涂覆有氮化铝涂覆层时有各种优点。与未经涂覆的荧光物质比较，该未经涂覆的荧光物质的灯具在潮湿环境下持续100小时之后性能急剧下降，而经涂覆厚度大于2000埃的涂层的材料，例如L2503-12、L2503-14和L2503-16的性能就很显然。例如，一种其中包含有所述的带氮化铝涂层的电致发光荧光物质的电致发光灯，在相对湿度大于95％的环境中运行100小时之后的亮度，比采用未涂覆氮化物涂层的相同荧光物质的相似的灯的亮度高4倍。甚至未经充分覆盖的经涂覆的材料(L2503-13)(由表II看出，后一种材料仅有98％的覆盖率和厚度为800埃)在苛刻的环境下，情况也不好。
因此，这里提供的电致发光荧光物质具有很好的效率、长的寿命和适用于潮湿环境。
虽然这里指出的和描述的是目前认为是本发明的优选实施例，但很明显，对本技术领域的技术人员来说，在不偏离由所提出的权利要求限定的本发明的范围的前提下，可以进行各种变化和修改。

Claims (9)

1.一种电致发光荧光物质，它由颗粒组成，基本上在每一颗粒上均涂有氮化铝的共形涂层。
2.一种包含耐潮湿光源的电致发光灯，所述光源包含如权利要求1所述的电致发光荧光物质。
3.如权利要求2所述的灯，其中所述灯在暴露于相对湿度大于95％的环境中100小时之后，具有的亮度大于58.2坎/米2。
4.如权利要求3所述的灯，其中所述荧光物质的颗粒具有的涂层厚度大于2000埃。
5.一种将耐潮湿氮化铝涂层涂覆到电致发光荧光物质颗粒上的方法，它包含的步骤有：向装有荧光物质颗粒的反应容器中引入惰性气体；将所述反应容器加热到反应温度；向所述反应容器中引入氮化物涂覆用前体六(二甲基酰胺)二铝；向所述反应容器引入一种共反应剂无水氨；维持所述惰性气体流、共反应剂流和前体供应一段时间，足以用所述耐潮湿氮化物涂覆所述荧光物质颗粒。
6.如权利要求5所述的方法，其中所述的前体是从维持在约100℃下的供料源载送的。
7.如权利要求6所述的方法，其中所述的前体是利用纯氮气通过维持在约130℃～140℃温度下的管道由所述料原载送到所述反应容器的。
8.如权利要求7所述的方法，其中所述无水氨在进入反应容器前利用纯氮稀释。
9.一种电致发光灯，其中包含有权利要求1所述的带氮化铝涂层的电致发光荧光物质，所述灯在相对湿度大于95％的环境中运行100小时之后的亮度，比采用未涂覆氮化物涂层的相同荧光物质的相似的灯的亮度高4倍。
CN99101071A 1998-01-12 1999-01-12 对潮湿不敏感的电致发光荧光物质 Expired - Fee Related CN1121471C (zh)

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US09/175,787 US6064150A (en) 1998-01-12 1998-10-20 Nitride coated particle and composition of matter comprised of such particles
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US6509058B2 (en) 2003-01-21
DE69904246D1 (de) 2003-01-16
US6064150A (en) 2000-05-16
KR100306356B1 (ko) 2001-09-24
US20020011781A1 (en) 2002-01-31
EP0928826A1 (en) 1999-07-14
CA2255871C (en) 2003-10-07
US6456002B1 (en) 2002-09-24
DE69904246T2 (de) 2003-04-17
KR19990067828A (ko) 1999-08-25
CA2255871A1 (en) 1999-07-12
CN1227862A (zh) 1999-09-08
EP0928826B1 (en) 2002-12-04
JPH11260557A (ja) 1999-09-24

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