CN101360803A - 具有高初始亮度的防潮电致发光磷光体及其制造方法 - Google Patents
具有高初始亮度的防潮电致发光磷光体及其制造方法 Download PDFInfo
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Abstract
本发明是电致发光磷光体，其中各个独立的磷光体颗粒包封在通过原子层沉积(ALD)涂覆法施加的无机涂层中。在优选实施方案中，该涂层是羟基氧化铝。包封的磷光体表现出对大气湿度的极端不敏感性并且在灯中仅经受极小的初始亮度损失。
Description
相关申请的交叉引用
本申请要求2006年1月26日提交的美国临时申请No.60/766,543的权益。
技术领域
本发明涉及电致发光(electroluminescent)磷光体(phosphors)，更特别涉及已经处理为防潮的电致发光磷光体。本发明再更特别涉及具有极大降低的潮湿引发劣化和高初始亮度的电致发光磷光体。
发明背景
电致发光(EL)灯可以大致分成两类：(1)通常通过气相沉积技术(如CVD)或溅射法在刚性玻璃基底上沉积磷光体与介电材料的交替薄膜而制成的薄膜EL灯；和(2)用分散在树脂中并以交替层形式涂在塑料片上的微粒材料制成的厚膜EL灯。在后一情况下，厚膜电致发光灯可以构造成薄的挠性发光设备，从而使它们适于更广泛的用途。
图1中显示了传统厚膜EL灯的截面示意图。灯2具有两个介电层20和22。涂在塑料膜12b上的第一导电材料4(如石墨)形成灯2的第一电极(该电极还可以包含金属箔)；而涂在第二塑料膜12a上的透明导电材料6(如氧化铟锡)的薄层形成第二电极。夹在两个导电电极4和6之间的是介电材料14的两层20和22，所述介电材料可以是例如氰乙基纤维素、氰乙基淀粉、聚-(甲基丙烯酸甲酯/丙烯酸乙酯)和/或氟烃聚合物。与第一电极4相邻的是其中嵌有铁电材料10(优选钛酸钡)颗粒的介电材料14的层。与第二电极6相邻的是其中嵌有电致发光磷光体8颗粒的介电材料14的层。当向电极施加交变电压时，由磷光体发出可见光。
可用于厚膜EL灯的电致发光磷光体主要由已被各种活化剂，例如Cu、Au、Ag、Mn、Br、I和Cl掺杂的硫化锌构成。在美国专利Nos.5,009,808、5,702,643、6,090,311和5,643,496中描述了硫化锌基EL磷光体的实例。优选的EL磷光体包括可以被Cl和/或Mn共掺杂的ZnS:Cu磷光体。
电致发光磷光体，特别是ZnS:Cu磷光体的亮度由于在电场施加过程中存在湿气而明显降低。已经报道，硫化锌基磷光体的亮度降低是由硫空位的增加造成的，所述硫空位通过下列反应产生：
ZnS+2H2O-->SO2+Zn+2H2
硫以SO2形式从磷光体中选出；结果，在磷光体中留下硫空位和锌。
因此，重要的是加入防潮保护措施以延长EL灯的光发射。通常，独立的EL磷光体颗粒被无机涂层包封以改进它们对潮湿引发的劣化的耐受性。在美国专利Nos.5,220,243、5,244,750、6,309,700和6,064,150中描述了此类涂层的实例。在磷光体颗粒悬浮在气体流化床中的同时经化学气相沉积(CVD)反应形成这些无机涂层。通常，在磷光体颗粒表面上沉积薄而连续的涂层，由此保护它们免受大气湿度的影响。
用于EL磷光体的优选涂层由三甲基铝(TMA)的水解产生。在经此引用并入本文的美国专利Nos.5,080,928和5,220,243中描述了水解的TMA涂层和CVD法。水解的TMA涂层的组成被认为主要为羟基氧化铝(AlOOH)，但是在组成上可以随反应条件在氧化铝和氢氧化铝之间变化。为方便起见，水解的TMA涂层的组成在本文中被称作羟基氧化铝(AlOOH)，但是要理解的是，这也包括从氧化铝(Al2O3)到氢氧化铝(Al(OH)3)的整个组成范围。TMA与水的反应可以如下描述：
Al(CH3)3+(3+n)/2H2O-->AlO(3-n)/2(OH)n+3CH4(0≤n≤3)
图2是对于在50℃，90％相对湿度下在EL灯中工作的传统AlOOHCVD涂覆的EL磷光体，随铝含量(涂层厚度)而变的100小时维持率(保持)的图。可以看出，与大约3.8重量％铝(作为总涂覆的磷光体重量的百分比)对应的涂层厚度在传统CVD法的情况下代表产生残留初始亮度与高防潮性的最佳组合的涂层厚度。本文所用的100小时维持率是指100小时光输出除以0小时光输出并乘以100％，(100小时/0小时)×100％。与未涂覆的磷光体相比，CVD包封的EL磷光体总是由于涂覆过程而经受初始亮度的显著损失。据猜测，这种降低可能由外涂层的存在造成的磷光体颗粒内部的电场降低引起。
发明概述
本文所用的术语初始亮度(IB)是指在灯初次工作时在电致发光灯中的磷光体亮度。为了进行测量并使灯的光输出稳定化，可能经过数分钟的简短期间。这也被称作0小时亮度。由于潮湿引发的劣化造成的亮度迅速降低，优选将含有未涂覆磷光体的EL灯层压在防潮包装中以进行初始亮度测量。对于涂覆的EL磷光体，残留的初始亮度(RIB)表示为百分比并相对于相同EL磷光体在其未涂覆状态下在EL灯中在相同条件下工作时的初始亮度测定；RIB＝(IB(涂覆的)/IB(未涂覆))×100％。优选地，本发明的涂覆的EL磷光体的残留初始亮度为至少95％。
已经发现，原子层沉积(ALD)能够在EL磷光体颗粒上提供比传统CVD法更薄的涂层，同时保持相当的防潮保护水平和更高的初始亮度水平。ALD是有吸引力的薄膜沉积技术，因为其允许对沉积法进行原子级控制。ALD涂层具有许多优异的特征，例如共形性(conformality)、均匀性、可再现性和精确的厚度控制。实际上，ALD是使用两种化学蒸气前体的特殊类型的CVD，这两种前体以两者不会同时以气相存在于反应器中的方式周期性注入沉积系统。这样做的目的是迫使前体在ALD沉积过程中在基底上而非在气相中反应。在经此引用并入本文的美国专利Nos.6,913,827和6,613,383中描述了ALD涂覆法的实例。
在ALD沉积法中，一种前体作为单层吸附在表面上；随后吹扫该系统以除去过量前体；注入第二前体以便与吸附的材料反应；然后再吹扫该系统。在每一前体脉冲后使用载气流(通常N2)和真空泵送吹扫该系统。重复ALD沉积周期，每一前体的定量供料时间为大约10至20秒，直至获得所需薄膜厚度。这导致在非常复杂的表面，例如半导体器件上的高纵横比形貌上的非常均匀的沉积。该反应是自限制的且生长速率通常为每周期大约0.1至
产生非常无缺陷的薄膜。由于基本每次一个单层地形成涂层，ALD比现有CVD法更可能获得更致密的涂层。
对于ALD施加的羟基氧化铝涂层，已经证实，需要至少大约更优选大约
的涂层厚度以有效保护EL磷光体免受潮湿引发的劣化。花费大约800个ALD沉积周期以获得大约
厚度。优选地，当在50℃和90％相对湿度下在EL灯中工作时，ALD涂覆的磷光体的残留初始亮度为至少95％且100小时维持率为至少60％。更优选地，在50℃和90％相对湿度下在EL灯中工作时，残留初始亮度为至少95％且100小时维持率为至少75％。尽管AlOOH是优选涂层，预计可以通过ALD以类似益处在电致发光磷光体上施加其它无机涂层。这类其它无机涂层包括但不限于，氮化铝、二氧化硅和二氧化钛。
附图简述
图1是传统厚膜EL灯的截面示意图。
图2是对于在50℃，90％相对湿度下工作的传统CVD涂覆EL磷光体，随铝含量而变的100小时维持率的图。
图3是对于通过本发明的ALD法制成的涂覆的磷光体，100小时维持率相对于涂层厚度的图。
发明详述
为了更好理解本发明以及本发明的其它和进一步目的、优点和能力，参考联系上述附图给出的下列公开内容和所附权利要求。
本发明是电致发光磷光体，其中各个独立的磷光体颗粒包封在通过原子层沉积(ALD)涂覆法施加的无机涂层中。在一个优选实施方案中，该涂层是羟基氧化铝。包封的磷光体对大气湿度表现出极端不敏感性并在灯中仅经受极小的初始亮度损失。
特别地，本发明的方法包括在流化床中使用ALD法使EL磷光体颗粒被无机薄膜涂覆。在一种优选方法中，通过向磷光体颗粒流化床中以ABAB....次序引入一系列交替剂量的气化三甲基铝(TMA)和水蒸汽，以便在磷光体颗粒表面上基本一次一个单层地沉积羟基氧化铝薄膜，形成ALD涂层。这两种前体相继在惰性载气中脉冲到涂覆反应器中，在脉冲之间进行吹扫以防止气相反应。流化床反应器保持在450K和1Torr压力下。由于每对前体脉冲(一个周期)产生几乎一个单层薄膜，可以通过沉积周期数精确控制所得薄膜的厚度。
涂层厚度可以与沉积在磷光体上的铝的量相关联。使用溅射中性质谱学(SNMS)测量法和作为参比材料的标准Ta2O5薄膜评估涂层厚度。为了满足在50％/90％相对湿度条件下对EL灯的100小时维持率要求，ALD法优选持续大约800个周期直至沉积的铝总量达到至少1.6重量％。
参照下列实施例更详细描述本发明。但是，应该理解的是，本发明无论如何不受这类具体实施例的限制。
厚膜电致发光试验灯以下列通用方式构造。将磷光体与粘合剂(DuPont Microcircuit Materials Luxprint 8155粘合剂)混合。液体粘合剂中磷光体的百分比为60重量％。将磷光体悬浮液筛网印刷到具有透明的导电氧化铟锡层的0.0065-0.0075英寸厚的PET薄膜，例如可获自CPFilms的OC-200上。聚酯筛网具有每英寸137或140根线。在干燥后，通过两次施加钛酸钡填充的介电油墨(DuPont Microcircuit MaterialsLuxprint
8153电致发光介电绝缘体)，形成介电层，其施加在磷光体层上并在施加之间干燥。在将介电层干燥后，在介电层上施加背面碳电极(DuPont Microcircuit Materials Luxprint
7144 Carbon Conductor)。在电致发光灯上施加层的优选方法是筛网印刷，也称作“丝网(silk-screening)”。但是，也可以成功地使用其它涂覆技术，例如拖拉(draw)刮刀涂覆和辊到辊(roll-to-roll)涂覆。在干燥后，该电致发光灯准备好进行亮度和维持率试验。在湿度箱中测试的灯要求背面碳电极被覆盖以防止液态水进入灯。在这种情况下，在碳电极上施加薄压敏胶带(3M Scotch 821带)。
实施例1
将大约200克发绿光的ZnS:Cu电致发光磷光体(类型728，OSRAM SYLVANIA Products Inc.，Towanda，PA)装入用于ALD涂覆的振动流化床反应器。流化床反应器是具有多孔金属盘作为气体分配器的不锈钢塔。使用高纯氮气作为流化气体。整个反应器被蛤壳型炉围绕且反应器温度保持在450K。使用三甲基铝(TMA)和去离子水作为前体且反应被分成两个自限制的半反应以沉积羟基氧化铝涂层。一系列气动活化阀控制前体在涂覆周期中的自动和相继定量供料。这两种前体均经由其蒸气压输送并将该系统排空并始终保持在1.0Torr的压力下。在每一前体剂量后，用氮气吹扫该系统以去除未反应的物类以及在反应过程中形成的任何甲烷。由于在反应器顶部设置了过滤器以减少淘析，在每一周期后使用反吹步骤将收集的粉末吹出过滤器。磷光体被涂覆100个涂覆周期。
实施例2
如实施例1中那样制备此实施例中的磷光体，只是涂覆周期数增至300。
实施例3
如实施例1中那样制备此实施例中的磷光体，只是涂覆周期数增至600。
制备用实施例1-3中所用的相同未涂覆磷光体制成的传统CVD涂覆的磷光体作为与ALD涂覆的样品比较的对照物。通过将气化的TMA和水蒸汽前体同时引入保持在大气压和450K下的流化床反应器，施加CVD涂层。
制造含有未涂覆磷光体以及包封磷光体的厚膜电致发光试验灯。含有未涂覆磷光体的对照灯专门包装在ACLAR(Honeywell Inc.供应的水不可透的透明薄膜)中，从而使未涂覆磷光体的湿度敏感性最小化。含有包封磷光体的相同的灯在100V和400Hz下在两种环境中工作100小时。在灯试验#1中，条件为21℃和50％相对湿度。对于灯试验#2，在湿度室中在50℃和90％相对湿度下进行加速环境测试。这些灯的试验结果列在表1中。也提供以总涂覆的磷光体重量的百分比(重量％Al)表示的ALD涂覆的磷光体的铝含量和以埃表示的近似涂层厚度。
如表1中所示，ALD涂覆的EL磷光体的100小时维持率随着通过增加涂覆周期数而实现的涂层厚度的增加而增加。但是，在加速环境试验(50℃，90％相对湿度)中，600周期ALD涂覆的磷光体的100小时维持率仍然比标准CVD涂覆的磷光体低大约10％。通过如图3中那样绘制涂层厚度相对于100小时维持率，据估计，涂层厚度为
的ALD涂覆的磷光体可以实现与CVD涂覆的对照物类似的100小时维持率性能。
表1
实施例4
如实施例1中那样制备此实施例中的磷光体，只是涂覆周期数增至800且磷光体是不同的发绿光的ZnS:Cu电致发光磷光体(类型729，OSRAM SYLVANIA Products Inc.，Towanda，PA)。在表2中显示和比较这种ALD涂覆的磷光体和由相同磷光体制成的CVD涂覆的对照物的灯数据和分析。CVD涂覆的对照物(3.8重量％Al)的涂层厚度被认为是在高维持率和残留初始亮度方面对这种磷光体而言最佳的厚度。
通过将涂覆周期数增至800，ALD涂覆的磷光体上的铝涂覆重量增至1.6重量％。基于SNMS测量法，在800周期磷光体上的AlOOH涂层厚度估计为
其约为标准CVD涂覆的EL磷光体厚度的一半。这种ALD涂覆的磷光体和CVD涂覆的磷光体在灯中具有几乎相同的100小时维持率。但是，ALD涂覆的EL磷光体保持大约96％的初始亮度，而CVD涂覆的磷光体仅保持80％的初始亮度。
表2
尽管已经显示和描述了在本发明的优选实施方案中目前考虑的内容，但本领域技术人员显而易见的是，可以在不背离由所附权利要求确定的本发明的范围的情况下对其作出各种变动和修改。
Claims (18)
1.电致发光磷光体，包含：硫化锌基电致发光磷光体的独立颗粒，其中各个颗粒被包封在无机涂层中，该磷光体在并入在50℃，90％相对湿度环境中在100V和400Hz下工作的电致发光灯中时表现出至少95％的残留初始亮度和至少60％的100小时维持率。
2.权利要求1的磷光体，其中100小时维持率为至少75％。
3.权利要求1的磷光体，其中电致发光磷光体为ZnS:Cu。
4.权利要求1的磷光体，其中无机涂层为羟基氧化铝。
5.权利要求4的磷光体，其中100小时维持率为至少75％。
6.权利要求4的磷光体，其中电致发光磷光体为ZnS:Cu。
7.包封电致发光磷光体的方法，包括：
(a)形成电致发光磷光体颗粒的流化床；
(b)将第一气相前体引入流化床；
(c)吹扫流化床；
(d)将第二气相前体引入流化床以便与第一前体反应并在磷光体颗粒上形成无机涂层；
(e)吹扫流化床；和
(f)重复步骤(a)至(e)直至达到至少大约
涂层厚度。
8.权利要求7的方法，其中第一或第二气相前体是气化的三甲基铝或水蒸汽且涂层是羟基氧化铝。
9.权利要求7的方法，其中最终涂层厚度为至少大约
10.权利要求9的方法，其中在重复步骤(a)至(e)大约800个周期后达到步骤(f)中的最终涂层厚度。
11.包封电致发光磷光体的方法，包括：
(a)形成ZnS:Cu电致发光磷光体颗粒的流化床；
(b)将气化的三甲基铝引入流化床；
(c)吹扫流化床；
(d)将水蒸汽引入流化床以便与三甲基铝反应并在磷光体颗粒上形成羟基氧化铝涂层；
(e)吹扫流化床；和
(f)重复步骤(a)至(e)直至达到至少大约
的最终涂层厚度。
12.权利要求11的方法，其中最终涂层厚度为至少大约
13.权利要求12的方法，其中在重复步骤(a)至(e)大约800个周期后达到步骤(f)中的最终涂层厚度。
14.权利要求11的方法，其中气化的三甲基铝在步骤(d)中引入，且水蒸汽在步骤(b)中引入。
15.权利要求14的方法，其中最终涂层厚度为至少大约
16.权利要求15的方法，其中在重复步骤(a)至(e)大约800个周期后达到步骤(f)中的最终涂层厚度。
17.涂覆的电致发光磷光体，包含：硫化锌基电致发光磷光体的独立颗粒，其中各个颗粒被包封在羟基氧化铝涂层中，该磷光体表现出至少95％的残留初始亮度并具有与CVD涂覆的含羟基氧化铝涂层的磷光体相当的防潮性，其中CVD涂覆的磷光体的铝含量为3.8重量％。
18.权利要求17的涂覆的磷光体，其中涂覆的电致发光磷光体的铝含量为1.6重量％。
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2007
- 2007-01-12 US US11/622,523 patent/US7833437B2/en not_active Expired - Fee Related
- 2007-01-15 CN CN200780001473.1A patent/CN101360803B/zh not_active Expired - Fee Related
- 2007-01-15 EP EP07710127A patent/EP1976648A4/en not_active Withdrawn
- 2007-01-15 CA CA002631729A patent/CA2631729A1/en not_active Abandoned
- 2007-01-15 KR KR1020087013045A patent/KR101385780B1/ko not_active IP Right Cessation
- 2007-01-15 JP JP2008552524A patent/JP5384945B2/ja not_active Expired - Fee Related
- 2007-01-15 WO PCT/US2007/060539 patent/WO2007087480A2/en active Application Filing
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8298666B2 (en) | 2006-01-26 | 2012-10-30 | Global Tungsten & Powders Corp. | Moisture resistant electroluminescent phosphor with high initial brightness and method of making |
| CN101805602B (zh) * | 2009-02-18 | 2014-03-26 | 深圳市绎立锐光科技开发有限公司 | 光波长转换材料的封装方法及结构 |
| CN105683335A (zh) * | 2013-11-01 | 2016-06-15 | 默克专利有限公司 | 硅酸盐无机发光材料 |
| CN107532080A (zh) * | 2015-04-27 | 2018-01-02 | 默克专利股份有限公司 | 硅酸盐磷光体 |
| US10689570B2 (en) | 2015-04-27 | 2020-06-23 | Merck Patent Gmbh | Silicate phosphors |
| CN105838351A (zh) * | 2016-04-21 | 2016-08-10 | 湖南农业大学 | 一种改善发光材料热稳定性的方法 |
| CN105885823A (zh) * | 2016-04-21 | 2016-08-24 | 湖南农业大学 | 一种改善发光材料化学稳定性的方法 |
| CN105838351B (zh) * | 2016-04-21 | 2018-04-20 | 湖南农业大学 | 一种改善发光材料热稳定性的方法 |
| CN105885823B (zh) * | 2016-04-21 | 2018-07-31 | 湖南农业大学 | 一种改善发光材料化学稳定性的方法 |
| CN109328223A (zh) * | 2016-06-27 | 2019-02-12 | 通用电气公司 | 经涂布的锰掺杂的磷光体 |
| CN110062800A (zh) * | 2016-10-31 | 2019-07-26 | 英特曼帝克司公司 | 经涂覆的窄带绿色磷光体 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1976648A2 (en) | 2008-10-08 |
| KR20080089337A (ko) | 2008-10-06 |
| US20070172580A1 (en) | 2007-07-26 |
| CN101360803B (zh) | 2014-05-28 |
| JP5384945B2 (ja) | 2014-01-08 |
| EP1976648A4 (en) | 2012-01-25 |
| US7833437B2 (en) | 2010-11-16 |
| WO2007087480A3 (en) | 2008-05-15 |
| CA2631729A1 (en) | 2007-08-02 |
| JP2009524736A (ja) | 2009-07-02 |
| WO2007087480A2 (en) | 2007-08-02 |
| KR101385780B1 (ko) | 2014-04-24 |
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