CN1121509C - 高效和长寿命的场致发光磷光体的制备方法 - Google Patents
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Abstract
一种通过化学气相沉积涂覆磷光体颗粒的方法。步骤如下：向反应容器中输入惰性气体；向所述反应容器中加入磷光体颗粒；加热所述反应容器至反应温度；向所述反应容器中加入包括碳的涂膜母体；连续地向所述反应容器中加入母体料流；向所述反应容器中输入氧/臭氧混合物，所述氧/臭氧混合物含有低于4.4%(重量)的臭氧；以及保持所述的惰性气流、氧/臭氧混合物料流并进一步提供母体。该方法制备的磷光体在涂膜中含有2200-6300ppm的碳，并使灯的效率大于6.1流明/瓦特。
Description
本发明涉及包膜颗粒，尤其是具有敷形涂膜的颗粒。更具体地说，本发明涉及磷光体，尤其是涉及在其表面上具有涂膜的场致发光磷光体，其涂膜保护磷光体免于吸湿并大幅度延长寿命和提高效率。
包膜磷光体是众所周知的，参见US4585673；4828124；5080928；5118529；5156885；5220243；5244750和5418062。由刚刚提到的一些专利已知，涂膜母体和氧气可用以涂覆保护涂膜。例如，参见US5244750和4585673。这些专利中的其它几个专利中的涂膜方法采用化学气相沉积法，提供水解来涂覆保护涂膜。另外，上述1998年9月16日提交的美国专利申请09/153978公开了一种采用化学气相沉积涂覆磷光体颗粒的方法，并使用了氧/臭氧反应试剂。后一种方法是在没有水或水蒸气的情况下进行的。上述1998年10月22日提交的美国专利申请09/177226公开了一种氧/臭氧改进方法，通过在开始进行沉积前，首先用母体使磷光体饱和，而进一步延长其寿命和提高效率。进一步提高这类包膜磷光体的效率并延长其寿命将是本领域的一大进展。
因此，本发明的一个目的是克服现有技术的缺点。
本发明的另一个目的是提高包膜磷光体的操作性。
本发明的再一个目的是提供磷光体涂覆法的装置，所述方法不使用水或水蒸气。
在本发明的一个方面中，这些目的是通过一种涂覆磷光体颗粒的方法实现的，其步骤包括：向反应容器中输入惰性气体；向所述反应容器中加入磷光体颗粒；加热所述反应容器至反应温度；向所述反应容器中加入含有碳的涂膜母体，其时间足以用所述母体饱和所述磷光体颗粒；连续地向所述反应容器中加入母体料流；向所述反应容器中输入氧/臭氧混合物，所述氧/臭氧混合物含有低于4.4％(重量)的臭氧；并且保持所述的惰性气体流、氧/臭氧混合物料流并进一步提供母体，其时间足以涂覆所述磷光体颗粒。在一个实施方案中，在输入所述氧/臭氧混合物料时保持搅拌并且所需要的涂膜时间为约40-70小时。
已经发现：在上述方法中，当臭氧发生器在大大低于最高效率的情况下操作并且涂膜母体含有碳时，所产生的磷光体颗粒将具有一层涂膜，所述涂膜含有约2200-6300ppm的碳。当将这些磷光体颗粒用于制备场致发光灯时，使得灯的效率达6.1-7.7流明/瓦特，远超过对照值的3.3流明/瓦特。
为了更好地理解本发明，以及本发明的一些或其它目的、优点和性能，参见下面公开的内容。
现在更详细地描述本发明，本发明提供了一种制备高效和长寿命的场致发光(EL)磷光体的方法，该方法通过用有机、含金属的母体，例如三甲基铝(TMA)来涂覆这类磷光体。该方法采用化学气相沉积，在单个磷光体颗粒上沉积涂膜，尤其是以这种方式涂覆磷光体，使得涂膜中含有大量的碳。
首先使环绕TMA鼓泡管的惰性氮气流(流速为5.0升/分钟)流入空的、直径为4英寸、作流化床使用的石英管的底部。向长度为36英寸的石英管中装入10.0kg铜掺杂的硫化锌(ZnS：Cu)场致发光磷光体，例如由Osram Sylvania制造公司，Towanda，PA销售的Sylvania型728。在床高为约18英寸的流化床反应器中，用氮气流悬浮磷光体颗粒。接通振动混合器，并以60转/分钟的速度运行，通过外部炉使床温加热到约180℃。在涂覆过程中，用置于粉末中部的热电偶控制反应器的温度在±3℃范围内。当温度接近180℃时，用通过TMA鼓泡管的氮气流引发TMA预处理步骤，流速为2.0升/分钟。使TMA鼓泡管保持在34℃的温度下，并保持TMA汽压恒定。将含有汽化TMA涂膜母体的第二股氮气流与流速为5.0升/分钟、通过TMA鼓泡管流入流化床反应器底部的氮气流混合。该稀释的TMA母体蒸汽流过置于管反应器下并用来支承磷光体颗粒床的金属熔体。在用TMA母体饱和磷光体颗粒表面10分钟后，使流速为16.5升/分钟的氧气通过由PCI臭氧和控制体系公司制造的GL-1型臭氧发生器。通过改变流过变压器的直流电流来控制发生器的臭氧产生速率。通过设定各种臭氧输出速率，从臭氧发生器中产生不同量的臭氧。通过一系列呈圆周状分布于振动混合器管轴上的孔，使氧/臭氧混合物流入反应器中，开始涂覆过程，所述振动混合器置于振动盘上。在涂覆实验结束(约70小时)时，收集最终产品，用于进行化学分析和灯评估。
实施例
进行四种涂膜实验，研究包膜EL磷光体的碳浓度对灯性能的影响。掺入到涂膜中的碳浓度受涂覆环境下臭氧浓度的影响。如上所述，通过改变流过变压器的直流电流来控制臭氧浓度。通过用PCI制造的系列#400臭氧监测器测定该浓度。在整个实验中，向臭氧发生器中通入恒定流速为16.5升/分钟的氧气。实验结果列于表1中。
表1
| 试样 | ％O3 | 碳ppm | ％Al | 灯性能光输出(Ft.L) 差效率 | ||||
| 24小时 | 100小时 | 500小时 | 寿命小时 | Lm/w | ||||
| 基础试样 | 150 | 3.3 | ||||||
| TH9 | 4.3 | 2200 | 4.4 | 22.2 | 21.7 | 18.0 | 2276 | 6.1 |
| TH13 | 4.3 | 2300 | 4.3 | 22.0 | 21.4 | 17.5 | 2118 | 6.2 |
| TH14 | 3.0 | 4400 | 4.4 | 19.8 | 19.5 | 16.5 | 2283 | 6.4 |
| TH15 | 2.0 | 6300 | 4.0 | 19.0 | 18.8 | 15.8 | 2348 | 7.7 |
基础试样为未涂覆的硫化锌:铜EL磷光体。所示的碳量是残余的杂质。下面的两个试样TH9和TH13代表对照组，其中臭氧发生器是在现有技术的最好状态下运行的。该状态代表容量为约100％。臭氧的平均浓度为约4.3％。在本发明的一个方面中，即下一个试样TH14，臭氧输出被控制在65％，其结果是产生的臭氧量为3.0％(重量)。最后一个测试TH15保持臭氧浓度恒定在2％(重量)，臭氧输出控制在38％。对涂膜磷光体的总碳量、铝、BET、颗粒大小进行了分析和灯测试，结果示于表1中。
在灯中，所有的涂膜试样都运行的很好，其效率超过6.1流明/瓦特，24小时光输出为约19呎朗伯。基于化学分析和灯测试，两个对照组试样TH9和TH13很好地重复。两个试样在涂膜中均含有约2200ppm的碳并且该薄膜使EL灯的效率从3.3流明/瓦特提高到6.2流明/瓦特。通过使臭氧浓度从4.3％(重量)降低到3.0％(重量)，TH14的碳浓度明显地增加到4400ppm。较高的碳浓度使效率和寿命稍有增加。当TH15的臭氧浓度降低到2.0％(重量)时，最终涂膜的碳含量为6300ppm。TH15的半衰期要稍好于TH14，但效率提高到7.7流明/瓦特。从而得到了明显的改进。
因此，显而易见，通过向含金属的涂膜中掺入大量的碳类物质，提高了EL灯的效率和延长了寿命。
尽管我们已经说明和描述了本发明优选的实施方式，但是，很显然，对于本领域熟练的技术人员来说，各种改变和改进都不脱离由所附权利要求书限定的本
发明的范围。
Claims (9)
1.涂覆磷光体颗粒的方法，所涂的膜包括碳，涂覆以下述方式进行：向反应容器中输入惰性气体；向所述反应容器中加入磷光体颗粒；加热所述反应容器至反应温度；向所述反应容器中加入包括碳的涂膜母体，以用所述母体饱和所述磷光体颗粒；以及连续地向所述反应容器中加入母体料流；
其改进包括：向所述反应容器中输入氧/臭氧混合物，所述氧/氧混合物含有约2-4.3重量％的臭氧；以及保持所述的惰性气流、氧/臭氧混合物料流并进一步提供母体，以涂覆所述磷光体颗粒。
2.根据权利要求1的方法，其中所述母体是三甲基铝。
3.根据权利要求1的方法，其中所述惰性气体是氮气。
4.根据权利要求1的方法，其中所述反应温度为约180℃，所述饱和所需要的时间为约10分钟。
5.根据权利要求1的方法，其中涂膜所述磷光体的所需要的时间为约40-70小时。
6.根据权利要求1的方法，其中在输入所述氧/臭氧混合物期间保持搅拌。
7.一种根据权利要求1方法制备的包膜磷光体，其中所述涂膜含有约2200-6300ppm的碳。
8.根据权利要求7的包膜磷光体，其中所述磷光体是包膜场致发光磷光体。
9.根据权利要求7的包膜磷光体，其中所述磷光体是包膜颗粒。
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| Application Number | Priority Date | Filing Date | Title |
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| US8773998P | 1998-06-02 | 1998-06-02 | |
| US60/087739 | 1998-06-02 | ||
| US09/243674 | 1999-02-02 | ||
| US09/243,674 US6361864B1 (en) | 1998-06-02 | 1999-02-02 | Method for making high-efficacy and long life electroluminescent phophor |
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| CN1121509C true CN1121509C (zh) | 2003-09-17 |
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| CA2268602C (en) * | 1998-06-02 | 2004-06-22 | Osram Sylvania Inc. | Method for making long-life electroluminescent phosphor |
| KR20020014480A (ko) * | 2000-08-18 | 2002-02-25 | 구자홍 | 탄소나노튜브를 미량 혼합한 형광체 |
| US6733826B2 (en) * | 2000-12-18 | 2004-05-11 | Osram Sylvania Inc. | Method and apparatus for coating electroluminescent phosphors |
| KR100455401B1 (ko) * | 2001-12-12 | 2004-11-06 | 유재수 | 유동층을 이용한 형광체 표면처리 방법 |
| AU2002358277A1 (en) * | 2001-12-27 | 2003-07-24 | Aerogel Composite, Llc | Aerogel and metallic compositions |
| TWI307505B (en) * | 2006-03-08 | 2009-03-11 | Ind Tech Res Inst | Apparatus for fabricating coverlayer of optical information storage media and operating method of the same |
| WO2012146064A1 (zh) * | 2011-04-27 | 2012-11-01 | Mii Jenn-Wei | 光学薄膜灯可见光涂布区出光结构的改善装置 |
| KR101696733B1 (ko) | 2015-06-04 | 2017-01-17 | 주식회사 포스코 | 표면품질이 우수한 페라이트계 스테인리스 냉간압연강판 및 이의 제조 방법 |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4363998A (en) * | 1981-05-19 | 1982-12-14 | Westinghouse Electric Corp. | Fluorescent lamp processing which improves performance of zinc silicate phosphor used therein |
| US4585673A (en) * | 1984-05-07 | 1986-04-29 | Gte Laboratories Incorporated | Method for coating phosphor particles |
| US5188763A (en) * | 1986-08-29 | 1993-02-23 | Gte Products Corporation | Method for preparing zinc orthosilicate phosphor |
| US5156885A (en) | 1990-04-25 | 1992-10-20 | Minnesota Mining And Manufacturing Company | Method for encapsulating electroluminescent phosphor particles |
| US5080928A (en) | 1990-10-05 | 1992-01-14 | Gte Laboratories Incorporated | Method for making moisture insensitive zinc sulfide based luminescent materials |
| US5294867A (en) * | 1992-03-13 | 1994-03-15 | Gte Products Corporation | Low pressure mercury vapor discharge lamp containing an amalgam |
| EP0560617A3 (en) * | 1992-03-13 | 1993-11-24 | Kawasaki Steel Co | Method of manufacturing insulating film on semiconductor device and apparatus for carrying out the same |
| JPH06251874A (ja) * | 1993-02-24 | 1994-09-09 | Nec Kansai Ltd | 電界発光灯及びその製造方法 |
| US5666031A (en) * | 1994-03-16 | 1997-09-09 | Osram Sylvania Inc. | Neon gas discharge lamp and method of pulsed operation |
| DE19849581B4 (de) * | 1997-10-27 | 2005-05-12 | Osram Sylvania Inc., Danvers | Verfahren zur Herstellung eines elektrolumineszenten Phosphors mit langer Lebensdauer |
-
1999
- 1999-02-02 US US09/243,674 patent/US6361864B1/en not_active Expired - Lifetime
- 1999-05-14 CA CA002271908A patent/CA2271908C/en not_active Expired - Fee Related
- 1999-06-01 KR KR1019990019991A patent/KR100541630B1/ko not_active IP Right Cessation
- 1999-06-02 DE DE69912531T patent/DE69912531T2/de not_active Expired - Lifetime
- 1999-06-02 JP JP15509399A patent/JP4054136B2/ja not_active Expired - Fee Related
- 1999-06-02 EP EP99110661A patent/EP0969070B1/en not_active Expired - Lifetime
- 1999-06-02 CN CN99107692A patent/CN1121509C/zh not_active Expired - Fee Related
-
2000
- 2000-05-15 US US09/570,965 patent/US6426115B1/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| KR20000005801A (ko) | 2000-01-25 |
| DE69912531T2 (de) | 2004-05-13 |
| EP0969070B1 (en) | 2003-11-05 |
| JP4054136B2 (ja) | 2008-02-27 |
| DE69912531D1 (de) | 2003-12-11 |
| US6426115B1 (en) | 2002-07-30 |
| JP2000053958A (ja) | 2000-02-22 |
| CN1254768A (zh) | 2000-05-31 |
| KR100541630B1 (ko) | 2006-01-10 |
| CA2271908C (en) | 2009-04-07 |
| EP0969070A1 (en) | 2000-01-05 |
| US6361864B1 (en) | 2002-03-26 |
| CA2271908A1 (en) | 1999-12-02 |
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