CN1771127A - 挠性高温超阻挡物 - Google Patents
挠性高温超阻挡物 Download PDFInfo
- Publication number
- CN1771127A CN1771127A CNA2004800092597A CN200480009259A CN1771127A CN 1771127 A CN1771127 A CN 1771127A CN A2004800092597 A CNA2004800092597 A CN A2004800092597A CN 200480009259 A CN200480009259 A CN 200480009259A CN 1771127 A CN1771127 A CN 1771127A
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- Prior art keywords
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- gas barrier
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- substrate
- polymer
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Abstract
本发明提供一种挠性阻透组件,包括Tg大于或等于热稳定的聚对苯二甲酸乙二醇酯(“HSPET”)的Tg的挠性可见光透过的基底,该基底用Tg大于或等于HSPET的Tg的第一聚合物层覆盖,进一步用至少两个可见光透过的无机阻挡层覆盖,该无机阻挡层通过至少一个Tg大于或等于HSPET的Tg的第二聚合物层隔开,可用于安装、覆盖、封装或形成水汽或氧气敏感性制品,如有机发光器件和光阀。
Description
本发明涉及阻挡膜和电子装置。
背景
当与水蒸汽或氧气接触时,有机发光器件(OLED)产量会降低或过早失效。金属和玻璃被用于包封和延长OLED装置的寿命,但是金属通常缺少透明性,而玻璃缺少挠性。为找到OLED和其他电子装置用的可选择包封材料已经进行了广泛的努力。挠性聚合阻挡膜对水蒸汽和氧气有较低渗透性,因此特别适用,然而尽管在工业上进行了广泛努力,但仅取得了有限的成功。涉及挠性阻挡膜的文献包括美国专利5,440,446(Shaw等人)、5,530,581(Cogan)、5,681,666(Treger等人)、5,686,360(Harvey,III等人)、5,736,207(Walther等人)、6,004,660(Topolski等人)、6,083,628(Yializis)、6,146,225(Sheats等人)、6,214,422(Yializis)、6,268,695(Affinito)、6,358,570(Affinito)、6,413,645(Graff等人)、6,492,026(Graff等人)和6,497,598(Affinito);美国专利申请US2001/0015620 A1(Affinito)、US 2002/0125822 A1(Graff等人)、US2002/0150745 A1(Martin等人)和US 2002/0176993 A1(Graff等人)、欧洲专利申请EP 0 777 280 A2(Motorola、Inc.)和PCT公布申请WO97/16053(Robert Bosch GmbH)。Walther等人的专利公开了一种塑料容器用的阻透组件,报道的最低氧气透过速率是0.375cc/m2/天/bar。
发明概述
在一个方面中,本发明提供一种阻透组件(下文有时称为″阻挡膜″),包括玻璃态转变温度(″Tg″)大于或等于热稳定的聚对苯二甲酸乙二醇酯(″HSPET″)的挠性可见光透过的基底,该基底用Tg大于或等于HSPET的Tg的第一聚合物层覆盖,进一步用至少两个可见光透过的无机阻挡层覆盖,该无机阻挡层通过至少一个Tg大于或等于HSPET的Tg的第二聚合物层隔开,在23℃和90%RH下该阻透组件的氧气透过速率小于0.005cc/m2/天。
在另一方面中,本发明提供一种制造阻透组件的方法,包括:
a)提供Tg大于或等于HSPET的Tg的挠性光-透射基底;
b)在该基底上形成Tg大于或等于HSPET的Tg的第一聚合物层;
c)在该第一聚合物层上形成可见光透过的第一无机阻挡层;
d)在该第一无机阻挡层上形成Tg大于或等于HSPET的Tg的第二聚合物层;及
e)在该第二聚合物层上形成可见光透过的第二无机阻挡层,
其中在23℃和90%RH下该阻透组件的氧气透过速率小于0.005cc/m2/天。
在另一个方面中,本发明提供一种显示或照明装置,包括至少部分用阻透组件覆盖的水汽或氧气敏感性光源或光阀,该阻透组件包括Tg大于或等于HSPET的Tg的挠性可见光透过的基底,该基底用Tg大于或等于HSPET的Tg的第一聚合物层覆盖,进一步用至少两个可见光透过的无机阻挡层覆盖,该无机阻挡层通过至少一个Tg大于或等于HSPET的Tg的第二聚合物层隔开。
从下面详细说明,可以清楚本发明的这些和其他方面。然而,决不能将上述概述解释为对要求保护的主题的限制,主题仅由所附的权利要求书来限定,而权利要求书在审查中可以修改。
附图简要说明
图1是所公开的阻透组件的示意性剖面图;
图2是所公开的层压阻透组件的示意性剖面图;
图3是用于实施所公开方法的装置的示意图;
图4是所公开的OLED装置的示意性剖面图;及
图5是所公开的阻透组件的显微照片;
在各附图中相同的附图标记代表相同元件。附图中的元件不是按比例绘制的。
详细说明
使用方向术语如″在...上面″、″在...上″、″在...最上″等描述各层在本发明的阻透组件或装置中的位置,表明一层或多层相对于水平基底层的位置。不用于指在制造过程中或之后阻透组件或装置在空间上有任何特定方向。
术语″覆盖″指层相对于本发明阻透组件的基底或其他元件的位置,表明该层在基底或其他元件之上,但与基底或其他元件不必须相邻。术语″用...隔开″指聚合物层相对于两个无机阻挡层的位置,表明聚合物层在两个无机阻挡层之间,但与任一无机阻挡层不必须相邻。
术语″聚合物″指均聚物和共聚物,及可以形成为共混物的均聚物或共聚物,例如通过共挤压或反应形成,包括例如酯交换反应。术语″共聚物″包括无规和嵌段共聚物。术语″固化的聚合物″包括交联和未交联的聚合物。术语″交联″聚合物指聚合物链通过共价化学价连接在一起的聚合物,通常通过交联分子或基团连接,以形成网络聚合物。交联聚合物其一般特征是不可溶的,但是在适合溶剂中会溶胀。
术语″Tg″指当分析大量而不是薄膜形式的固化聚合物时的玻璃态转变温度。当仅能以薄膜形式检测聚合物的情况下,通常可以在合理精度内分析大量形式固化聚合物的Tg。通常通过分析热量流速vs.温度来测定大量形式的Tg值,使用扫描差示量热法(DSC)测定聚合物部分移动的开始和变形点(通常第二次转变),在变形点时聚合物从下班态转变成橡胶态。使用动态机械热分析(DMTA)技术也可以分析大量形式固化聚合物的Tg值,其测量聚合物模数随温度和振动频率的变化。
术语″可见光透过的″基底、层、组件或装置指基底、层、组件或装置沿法向轴测量的光谱可见部分平均透射率至少约为20%,Tvis。
参考图1,阻透组件通常用110表示。组件110包括由Tg大于或等于HSPET的Tg(Tg=约78℃)的可见光透过的挠性塑料薄膜制成的基底112。基底112用Tg大于或等于HSPET的Tg的聚合物层114覆盖,再用两个或多个可见光透过的无机阻挡层覆盖,如用聚合物层如层118和122隔开的层116、120和124。组件110优选也包括在最上的可见光透过的无机阻挡层124之上的保护性聚合物上层126。
图2表明使用一层可见光透过的粘合剂132面对面地将两块组件110层压在一起得到的层压阻透组件130。
优选的挠性光-透射基底112其可见光透射在550nm时至少约70%。优选通过使用热固化、拉伸下退火、或其他技术使基底是热稳定的,这样当基底未受强制时至少到加热稳定温度下防止收缩。如果基底不是热稳定的,那么优选其Tg大于聚甲基丙烯酸甲酯(″PMMA″,Tg=105℃)。更优选地,基底Tg至少约110℃,再更优选至少约120℃,最优选至少约128℃。除了HSPET外,特别优选的基底包括其他热稳定的高Tg聚酯,PMMA,苯乙烯/丙烯腈(″SAN″,Tg=110℃),苯乙烯/马来酸酐(″SMA″,Tg=115℃),聚萘二甲酸乙二酯(″PEN″,Tg=约120℃),聚甲醛(″POM″,Tg=约125℃),聚乙烯基萘(″PVN″,Tg=约135℃),聚醚醚酮(″PEEK″,Tg=约145℃),聚芳基醚酮(″PAEK″,Tg=145℃),高Tg含氟聚合物(例如,DYNEONTMTHE,六氟丙烯、四氟乙烯、乙烯的三聚物,Tg=约149℃),聚碳酸酯(″PC″,Tg=约150℃),聚α-甲基苯乙烯(Tg=约175℃),多芳基化合物(″PAR″,Tg=190℃),聚砜(″PSul″,Tg=约195℃),聚苯醚(″PPO″,Tg=约200℃),聚醚酰亚胺(″PEI″,Tg=约218℃),聚芳基砜(″PAS″,Tg=220℃),聚醚砜(″PES″,Tg=约225℃),聚酰胺酰亚胺(PAI″,Tg=约275℃),聚酰亚胺(Tg=约300℃)和聚酞酰胺(热变形温度120℃)。对于材料成本是重要的那些应用而言,由HSPET和PEN制成的基底是特别优选的。对于阻挡性能是最重要的那些应用而言,可以使用由更昂贵材料制成的基底。优选基底厚度约0.01~约1mm,更优选约0.05~约0.25mm。
Tg大于或等于HSPET的Tg的第一聚合物层置于基底上。可以使用各种聚合物材料。形成适度高Tg聚合物的挥发性单体是特别优选的。优选第一聚合物层其Tg大于PMMA,更优选Tg至少约110℃,更优选至少约150℃,最优选至少约200℃。可用于形成第一层的特别优选单体包括聚氨酯丙烯酸酯(例如,CN-968,Tg=约84℃,CN-983,Tg=约90℃,这两种商业上可从Sartomer Co.得到),丙烯酸异冰片酯(例如,SR-506,商业上可从Sartomer Co.得到,Tg=约88℃),二季戊四醇五丙烯酸酯(例如,SR-399,商业上可从Sartomer Co.得到,Tg=约90℃),用苯乙烯掺混的环氧丙烯酸酯(例如,CN-120S80,商业上可从Sartomer Co.得到,Tg=约95℃),四丙烯酸二-三羟甲基丙酯(例如,SR-355,商业上可从Sartomer Co.得到,Tg=约98℃),二甘醇二丙烯酸酯(例如,SR-230,商业上可从Sartomer Co.得到,Tg=约100℃),1,3-丁二醇二丙烯酸酯(例如,SR-212,商业上可从Sartomer Co.得到,Tg=约101℃),五丙烯酸酯(例如,SR-9041,商业上可从Sartomer Co.得到,Tg=约102℃),季戊四醇四丙烯酸酯(例如,SR-295,商业上可从Sartomer Co.得到,Tg=约103℃),季戊四醇三丙烯酸酯(例如,SR-444,商业上可从Sartomer Co.得到,Tg=约103℃),乙氧基化的(3)三羟甲基丙烷三丙烯酸酯(例如,SR-454,商业上可从Sartomer Co.得到,Tg=约103℃),乙氧基化的(3)三羟甲基丙烷三丙烯酸酯(例如,SR-454HP,商业上可从Sartomer Co.得到,Tg=约103℃),烷氧基化的三官能丙烯酸酯(例如,SR-9008,商业上可从Sartomer Co.得到,Tg=约103℃),二丙二醇二丙烯酸酯(例如,SR-508,商业上可从Sartomer Co.得到,Tg=约104℃),新戊二醇二丙烯酸酯(例如,SR-247,商业上可从SartomerCo.得到,Tg=约107℃),乙氧基化的(4)双酚A二甲基丙烯酸酯(例如,CD-450,商业上可从Sartomer Co.得到,Tg=约108℃),环己烷二甲醇二丙烯酸酯(例如,CD-406,商业上可从Sartomer Co.得到,Tg=约110℃),甲基丙烯酸异冰片酯(例如,SR-423,商业上可从Sartomer Co.得到,Tg=约110℃),环二丙烯酸酯(例如,IRR-214,商业上可从UCBChemicals得到,Tg=约208℃),三(2-羟乙基)异氰脲酸酯三丙烯酸酯(例如,SR-368,商业上可从Sartomer Co.得到,Tg=约272℃),上述甲基丙烯酸酯的丙烯酸酯和上述丙烯酸酯的甲基丙烯酸酯。
通过将一层单体或低聚物涂覆到基底上并原位交联层形成聚合物,而形成第一聚合物层,例如闪蒸和气相沉积照射可交联的单体,然后使用例如电子束装置、UV光源、放电装置或其他适合装置交联。通过冷却基底可以提高涂覆效率。也可以使用常规涂覆方法如辊涂(例如,凹版式辊涂)或旋涂(例如,静电旋涂)将单体或低聚物涂覆到基底上,然后按上述进行交联。也可以通过涂覆一层含有低聚物或聚合物的溶剂并干燥涂覆层来除去溶剂,来形成第一聚合物层。如果在高温下提供玻璃态转变温度大于或等于HSPET的玻璃态转变温度的玻璃态聚合层,那么也可以使用等离子体聚合。最优选地,通过闪蒸和气相沉积、然后原位交联形成第一聚合物层,例如,美国专利4,696,719(Bischoff),4,722,515(Ham),4,842,893(Yializis等人),4,954,371(Yializis),5,018,048(Shaw等人),5,032,461(Shaw等人),5,097,800(Shaw等人),5,125,138(Shaw等人),5,440,446(Shaw等人),5,547,908(Furuzawa等人),6,045,864(Lyons等人),6,231,939(Shaw等人)和6,214,422(Yializis);公布的PCT申请WO 00/26973(Delta VTechnologies,Inc.);D.G.Shaw和M.G.Langlois,″A New VaporDeposition Process for Coating Paper and Polymer Webs″,6thInternational Vacuum Coating Conference(1992);D.G.Shaw和M.G.Langlois,″A New High Speed Process for Vapor Depositing Acrylate ThinFilms:An Update″,Society of Vacuum Coaters 36th Annual TechnicalConference Proceedings(1993);D.G.Shaw和M.G.Langlois,″Use ofVapor Deposited Acrylate Coatings to Improve the Barrier Properties ofMetallized Film″,Society of Vacuum Coators 37th Annual TechnicalConference Proceedings(1994);D.G.Shaw,M.Roelirig,M.G.Langlois和C.Sheehan,″Use of Evaporated Acrylate Coatings to Smooth theSurface of Polyester and Polypropylene Film Substrates″,RadTech(1996);J.Affinito,P.Martin,M.Gross,C.Coronado和E.Greenwell,″Vacuum deposited polymer/metal multiplayer films for opticalapplication″,Thin Solid Films 270,43-48(1995);J.D.Affinito,M.E.Gross,C.A.Coronado,G.L.Graff,E.N.Greenwell和P.M.Martin,″Polymer-Oxide Transparent Barrier Layers″,Society of Vacuum Coaters39th Annual Technical Conference Proceedings(1996)。
每个聚合物层的平滑度、连续性及其对下层的粘合性优选通过适当预处理来增强。优选的预处理方法是在适合的反应性或非反应性气氛中利用放电处理(例如,等离子,辉光放电,电晕放电,介质阻挡放电或大气压放电);化学预处理或火焰预处理。这些预处理使下层表面更易于接受以后涂覆的聚合层。等离子预处理是特别优选的。在下层上也可以使用与高Tg聚合物层相比具有不同成分的单独粘合促进层,以改进中间层粘合。粘合促进层可以是单独聚合层或含金属层,如金属、金属氧化物、金属氮化物或金属氧氮化物层。粘合促进层其厚度为几nm(例如,1或2nm)至约50nm,而且在需要时可以更厚。
第一聚合物层所需的化学成分和厚度部分地取决于基底性质和表面形状。优选厚度足以提供一种平滑无缺陷的表面,其上随后可以涂覆第一无机阻挡层。例如,第一聚合物层其厚度为几nm(例如,2或3nm)到约5微米,而且在需要时可以更厚。
用Tg大于或等于HSPET的Tg的聚合物层隔开的至少两个可见光透过的无机阻挡层置于第一聚合物层之上。这些层分别称为″第一无机阻挡层″、″第二无机阻挡层″和″第二聚合物层″。如果需要还可存在额外的无机阻挡层和聚合物层,包括Tg不大于或等于HSPET的Tg的聚合物层。然而,优选相邻每对无机阻挡层仅由Tg大于或等于HSPET的Tg的聚合物层隔开,更优选仅由Tg大于PMMA的Tg的聚合物层隔开。
各无机阻挡层不必须相同。可以使用各种无机阻挡材料。优选的无机阻挡材料包括金属氧化物、金属氮化物、金属碳化物、金属氧氮化物、金属氧硼化物及其组合,例如,硅氧化物如二氧化硅,铝氧化物如氧化铝,钛氧化物如氧化钛,铟氧化物,锡氧化物,铟锡氧化物(″ITO″),钽氧化物,锆氧化物,铌氧化物,碳化硼,碳化钨,碳化硅,氮化铝,氮化硅,氮化硼,铝氧氮化物,硅氧氮化物,硼氧氮化物,锆氧硼化物,钛氧硼化物,及其组合。铟锡氧化物,硅氧化物,铝氧化物和其组合是特别优选的无机阻挡材料。ITO是通过适当选择相对比例的构成成分而具有导电性的陶瓷材料实例。优选使用薄膜金属化领域中所用的技术来形成无机阻挡层,如溅射(例如,阴极或平面磁控溅射),蒸发(例如,电阻或电子束蒸发),化学气相沉积,电镀等。最优选使用溅射形成无机阻挡层,例如反应性溅射。与低能量技术如常规化学气相沉积方法相比,通过高能量沉积技术如溅射形成的无机层具有增强的阻挡性能。尽管不限于理论,但是可以认为,性能增强是由于较大动能的物质在基底上冷凝,从而因压实使无效部分较低。每个无机阻挡层的平滑度、连续性及其对下层的粘合性可通过预处理来增强(例如,等离子体预处理),这些与对第一聚合物层所述的相似。
无机阻挡层不必须具有相同厚度。每个无机阻挡层所需的化学成分和厚度部分地取决于下层性质和表面形状,也取决于阻透组件所需的光学性能。优选无机阻挡层足够厚从而连续,也优选足够薄以确保阻透组件和包括该组件的制品具有所需程度的可见光透射性和柔软性。优选每个无机阻挡层的物理厚度(与光学厚度相对)约3~约150nm,更优选约4~约75nm。
除了阻挡作用外,一个或多个可见光透过的无机阻挡层的所有或部分可用作例如电极(适当时导电)或接触敏感表面。这可通过使部分层暴露或将层与导线、电路或其他电子元件相连来实现。
用于隔开第一、第二和任何额外无机阻挡层的第二聚合物层不必须相同,也不必须具有相同厚度。可以使用各种第二聚合物层材料。优选的第二聚合物层材料包括上述针对第一聚合物层所述的那些。优选按上面针对第一聚合物层所述的,通过闪蒸和气相沉积、然后原位交联来涂覆第二聚合物层。在形成第二聚合物层之前,也优选使用上面那些预处理(例如,等离子体预处理)。第二聚合物层所需的化学成分和厚度部分地取决于下层性质和表面形状。第二聚合物层厚度优选足以提供一种平滑无缺陷的表面,其上随后可以涂覆无机阻挡层。通常与第一聚合物层相比,第二聚合物层厚度较小。例如,第二聚合物层其厚度约5nm~约10微米,而且在需要时可以更厚。
优选阻透组件具有保护性聚合物上层。上层可以称作″第三聚合物层″。挥发性(甲基)丙烯酸酯单体优选用作第三聚合物层,Tg大于或等于HSPET的Tg的挥发性丙烯酸酯单体是特别优选的(例如,上面针对第一和第二聚合物层所述的那些),Tg大于PMMA的Tg的挥发性丙烯酸酯单体是最优选的。需要时,可以使用常规涂覆方法如辊涂(例如,凹版式辊涂)或旋涂(例如,静电旋涂)涂覆第三聚合物层,然后使用例如UV照射进行交联。最优选地,最优选地,通过上面针对第一和第二聚合物层所述的闪蒸、气相沉积、然后交联单体形成第三聚合物层。在形成第三聚合物层之前,也优选使用上面那些预处理(例如,等离子体预处理)。第三聚合物层所需的化学成分和厚度部分地取决于下层性质和表面形状,也取决于阻透组件可能受到损害,及可应用的装置需求。第三聚合物层厚度优选足以提供一种平滑无缺陷的表面,其会防止下层受到普通损害。通常与第一聚合物层相比,第三聚合物层厚度较小,与第二聚合物层相比厚度较大。例如,第三聚合物层其厚度约5nm~约10微米,而且在需要时可以更厚。
优选的阻透组件具有足量的无机阻挡层,并且基底、第一和第二聚合物层优选具有足够高Tg,从而阻透组件是可见光透过的,并且在38℃和100%相对湿度下水蒸汽透过速率(WVTR)小于约0.005g/m2/天,更优选在50℃和100%相对湿度下小于约0.005g/m2/天,最优选在85℃和100%相对湿度下小于约0.005g/m2/天。优选透明值(Tvis,通过平均400nm~700nm间的透射百分数T来测定)至少约20%,更优选至少约60%。
图3表明用于连续辊至辊制造本发明阻透组件的优选装置180。动力辊181a和181b使基底织物182前后移动通过装置180。可控制温度的旋转滚筒183a和183b、空转辊184a、184b、184c、184d和184e传输织物182通过金属溅射涂覆器185,等离子体预处理器186,单体蒸发器187和E-束交联装置188。液体单体189从储存器190供应至蒸发器187。通过装置180使用多通道将连续层或成双层涂覆到织物182。额外的涂覆器、预处理器、蒸发器和交联装置也可加到装置180中,例如,沿滚筒183a和183b外围设置,以连续沉积几对层。装置180也可装置在适合室中(图3未示),并保持真空或供应适合惰性气氛,以防止氧气、水蒸汽、灰尘和其他大气污染物干扰各种预处理、单体涂覆、交联和溅射步骤。
各种功能层或涂层可加到本发明的阻透组件中,以改变或提高其物理或化学性能,尤其是在阻挡膜的表面。这种层或涂层可以包括例如可见光透过的导电层或电极(例如,铟锡氧化物);抗静电涂层或薄膜;阻燃剂;UV稳定剂;耐磨剂或硬膜材料;光学涂层;防雾材料;磁性或磁光涂层或薄膜;照相乳液;棱镜薄膜;全息薄膜或图像;粘合剂,如压敏粘合剂或热熔粘合剂;促进与相邻层粘合的漆;及当以粘合辊形式使用阻透组件时的低粘性衬底材料。这些功能性成分可以加到阻透组件的一个或多个最外层,或者也可以涂覆成单独薄膜或涂层。
对某些应用而言,可能需要改变阻透组件的外观或性能,如通过将染色的薄膜层层压到阻透组件,将着色的涂层涂覆至阻透组件的表面,或在用于制造阻透组件的一种或多种材料中包括染料或颜料。染料或颜料可以在一个或多个选定的光谱区域吸收,包括部分红外、紫外或可见光谱。染料或颜料可用于补充阻透组件的性能,尤其是阻透组件可以透过一些频率而反射另一些频率。
阻透组件例如可用油墨或其他印刷标记处理,如用于显示产品识别、方向信息、广告、警告、装饰或其他信息的标记。各种技术可用于在阻透组件上印刷,例如丝印、喷印、热转印、凸版印刷、胶印、苯胺印刷、点刻印刷、激光印刷等,并且可以使用各类油墨,包括一种和两种成分的油墨、氧化性干燥和UV-干燥油墨、溶解油墨、分散油墨、100%油墨体系。
本发明的阻透组件可用于在各种应用中防止水蒸汽、氧气或其他气体透过。本发明的阻透组件特别适用于封装OLED、光阀如液晶显示器(LCDs)和其他电子装置。本发明代表性的封装OLED装置200表明在图4中。装置200的前侧或发光侧在图4中朝下。装置200包括本发明的可见光透过的阻透组件210,其外部ITO层(在图4中未示,但方向朝上)作为阳极。发光结构220形成在阻透组件210上,与外部ITO层接触。结构220包括多个层(图4中没有分开显示),当供给适合电能时,互相配合通过阻透组件210朝下发光。装置200也包括导电阴极230和金属箔包层250。箔包层250通过粘合剂240与装置220的后面、侧面和部分前面粘合。在粘合剂240中形成的开口260使箔250的一部分270变形与阴极230接触。箔250的另一开口(图4中未显示)与由阻透组件210的外部ITO层形成的阳极接触。金属箔250和阻透组件210很大程度上防止水蒸汽和氧气到达发光结构220。
现在结合下面的非限制性实施例说明本发明,其中除非另有所指所有的份数和百分数都按重量计。
实施例1
用丙烯酸酯和铟锡氧化物(″ITO″)层覆盖聚萘二甲酸乙二酯(″PEN″)基底薄膜,以七层交替的丙烯酸酯/ITO/丙烯酸酯/ITO/丙烯酸酯/ITO/丙烯酸酯的结构排列。各层形成如下:
(层1)将91米长、0.127mm厚×508mm宽的KALADEXTM1020PEN薄膜(商业上可从Dupont-Teijin Films得到,Tg=120℃)放到连续辊至辊真空处理室中。抽空室使压力降到8×10-6torr。用600W氮等离子体处理薄膜,使用钛阴极,使用织物速率9.1米/min,并保持薄膜背面与与冷至0℃的涂覆滚筒接触。在等离子体处理后,同时薄膜仍与滚筒接触时,用通过混合97%IRR-214环二丙烯酸酯(商业上可从UCB Chemicals得到,Tg=208℃)和3%EBECRYLTM170丙烯酸酯化的酸性粘合促进剂(商业上可从UCB Chemicals得到)制得的丙烯酸酯混合物涂覆等离子体处理的薄膜表面。在涂覆前使丙烯酸酯混合物真空脱气,并通过在60kHz频率下操作的超声喷雾器(商业上可从SonotekCorp.得到)以流速3.0ml/min抽吸进保持在275℃的加热汽化室。得到的单体蒸汽流冷凝在等离子体处理的薄膜表面上,使用在8kV和2.5毫安下工作的单灯丝进行电子束-交联,以形成426nm厚的丙烯酸酯层。
(层2)反转室内的织物方向,使用90% In2O3/10% SnO2靶(商业上可从Umicore铟Products得到)将ITO无机氧化物层喷溅沉积在20米长的丙烯酸酯涂覆的织物表面上。使用1500瓦的功率,含有134sccm氩气和3.0sccm氧气且压力为3毫乇的气体混合物,织物速率为0.55米/分钟,来喷溅ITO,得到沉积在层1丙烯酸酯上的48nm厚ITO层。
(层3)再次反转织物方向。使用与层1相同的一般条件,在同一20米织物长度上涂覆和交联第二丙烯酸酯层,但下面条件除外。在3000W下使用钛阴极和层2的氩气/氧气气体混合物进行等离子体处理,单体流速为1.1ml/min。在层2上得到104nm厚的丙烯酸酯层。
(层4)再次反转织物方向。使用与层2相同的条件,在层3上沉积48nm厚的ITO层。
(层5)再次反转织物方向。使用与层3相同的条件,在层4上涂覆104nm厚的丙烯酸酯层。
(层6)再次反转织物方向。使用与层2相同的条件,在层5上沉积48nm厚的ITO层。
(层7)再次反转织物方向。使用与层3相同的条件,在层6上涂覆104nm厚的丙烯酸酯层。
得到的七层叠层(未计基底)在30°入射角下其平均光谱透射率Tvis=50%(通过平均400nm~700nm间的透射百分数T来测定),水蒸汽透过速率(在85℃和100%RH下根据ASTM F-129测定)小于0.005g/m2/天,这低于MOCON PERMATRAN-WTM3/31 WVTR测试系统(商业上可从MOCON Inc.得到)的检测限制速率。当在38℃和90% RH下分析时,薄膜的氧气透过速率(根据ASTM D-3985测定,并分析薄膜面对测试气体的任一侧)小于0.005cc/m2/天,这低于MOCONOXTRANTM2/20氧气透过速率测试系统(商业上可从MOCON Inc.得到)的检测限制速率,且当在50℃和90%RH下分析时,低于平均值0.030cc/m2/天。
实施例1的阻透组件浸在液氮中,分成两半,并使用扫描电子显微镜进行剖面分析。图5表明得到显微照片。在图5中可以清楚地看到基底312、第一聚合物层314、可见光透过的无机阻挡层316、320和324、第二聚合物层318和322、第三聚合物层326。
实施例2
按与实施例1相同的方式制备七层叠层,但是使用SR-368D混合的丙烯酸酯混合物(商业上可从Sartomer Co.得到,为SR-351三羟甲基丙烷三丙烯酸酯和SR-368三(2-羟乙基)异氰脲酸酯三丙烯酸酯的50∶50混合物),在形成层3、5和7时未使用等离子体处理。基于SR-351的62℃ Tg和SR-368的272℃ Tg的算术平均值,分析SR-368D的Tg是167℃。
得到的七层叠层在30°入射角下其平均光谱透射率Tvis=68%,WVTR(在50℃和100% RH下测定)小于0.005g/m2/天,这低于WVTR测试系统的检测限制速率。
实施例3
按与实施例1相同的方式制备七层叠层,但使用MELINEXTM617聚对苯二甲酸乙二醇酯(″PET″)薄膜基底(商业上可从DuPont-TeijinFilms得到,Tg=70℃)和不同的丙烯酸酯。三丙二醇二丙烯酸酯(″TRPGDA″,商业上可从UCB Chemicals得到,Tg=62℃)用作层1的丙烯酸酯。含有97% TRPGDA和3% EBECRYL 170丙烯酸酯化的酸性粘合促进剂并且分析Tg=62℃的混合物用于形成层3、5和7。
得到的七层叠层在30°入射角下其平均光谱透射率Tvis=71%,WVTR(在50℃和100% RH下测定)为0.036g/m2/天。
实施例4
热稳定的PET基底
按与实施例1相同的方式制备七层叠层,但使用MELINEXTMST725热稳定的PET薄膜基底(商业上可从DuPont-Teijin Films得到,Tg=78℃),100% IRR-214丙烯酸酯但没有EBECRYL 170丙烯酸酯化的酸性粘合促进剂形成层1、3、5和7,在2000W下使用硅阴极和层2的氩气/氧气气体混合物进行等离子体处理,同时沉积层3、5和7。
得到的七层叠层在30°入射角下其平均光谱透射率Tvis=77%,WVTR(在60℃和100%RH下测定)为0.006g/m2/天。
实施例5
基底Tg对WVTR的影响
用三层叠层的SiAlO无机氧化物和商业可得到的阻挡聚合物(SARANTMF-278,商业上可从Dow Chemical Company得到)覆盖具有不同玻璃态转变温度的几个基底,以无机氧化物/阻挡聚合物/无机氧化物的结构排列。初始步骤后,部分聚甲基戊烯、聚丙烯、PET和聚醚砜薄膜基底首尾连接在一起,形成一个卷状物。各无机氧化物和阻挡聚合物层在这些基底上形成如下:
(层1)将连接的卷状物加到连续辊至辊喷溅涂覆机上。沉积室抽吸至压力为2×10-6Torr。使用2kW和600V,含有51sccm氩气和30sccm氧气且压力为1毫乇的气体混合物,织物速率为0.43米/分钟,通过反应性溅射Si-Al(95/5)靶(商业上可从Academy Precision Materials得到)在基底薄膜上沉积60nm厚SiAlO无机氧化物层。
(层2)从真空涂覆机上除下氧化物涂覆的织物。使用Model CAG-150微凹版式涂覆机(商业上可从Yasui-Seiki Co.得到),将Saran F278聚合物在四氢呋喃和甲苯的65/35v/v混合物中的10%溶液连续涂覆到上层1,该涂覆机安装有150R压花辊,在6.1m/min织物速率下工作。在80℃温度下在涂覆机的干燥部分中蒸发溶剂。
(层3)将聚合物涂覆的织物加到真空涂覆机中。使用与层1相同的条件,在层2上沉积第二SiAlO无机氧化物层。
然后在38℃和100%RH下测定每段涂覆的阻透组件的WVTR。结果列于下面表1中:
表1
基底 | Tg,℃ | WVTR@38℃/100%RH,g/m2/天 |
PMP(聚甲基戊烯)1 | 29 | 4.76 |
PP(聚丙烯)2 | -30~+20 | 2.35 |
PET3 | 70 | 0.281 |
PES(聚醚砜)4 | 225 | 0.0825 |
1 TPX薄膜,商业上可从Westlake Plastics得到。
2 商业上可从Copol International得到。
3 商业上可从Teijin Corp得到。
4 商业上可从Westlake Plastics得到。
如表1中PET和PES基底所示,WVTR值随基底Tg增大而降低。PMP和PP基底其Tg值低于WVTR测试温度,因此它们的WVTR值所受影响与高Tg基底的不同。
实施例6
聚合物层Tg对WVTR的影响
HSPE 100 0.1mm PET薄膜(商业上可从Teijin Films得到,Tg=70℃)用一系列四层聚合物/无机氧化物/聚合物/无机氧化物叠层覆盖,其中使用不同玻璃态转变温度的聚合物层。无机氧化物是ITO,聚合物从下面表2所列的成分形成,在制剂中每一种成分经重量份表示:
表2
制剂 | |||||
成分 | 1 | 2 | 3 | 4 | 5 |
SR-2381 | 17 | - | 5 | - | - |
CD-4062 | - | 17 | - | - | - |
SR-5063 | - | - | 13 | - | - |
B-CEA4 | 3 | 3 | 2 | 10 | |
LC2425 | - | - | - | 20 | - |
EBECRYLTM6296 | - | - | - | - | 85 |
1-四氧基-2-丙醇 | 75.6 | 75.6 | 75.6 | 75.6 | 360 |
甲基乙基酮 | 113.4 | 113.4 | 113.4 | 113.4 | 540 |
IRGACURE 1847 | 1 | 1 | 1 | 1 | 5 |
1 1,6-己二醇二丙烯酸酯(商业上可从Sartomer Co.得到,Tg=43℃)。
2 环己烷二甲醇二丙烯酸酯(商业上可从Sartomer Co.得到,Tg=110℃)。
3 丙烯酸异冰片酯(商业上可从Sartomer Co.得到,Tg=88℃)。
4 β-羧乙基丙烯酸酯(商业上可从UCB Chemicals Corp.得到)。
5 液晶聚合物(PALIOCOLORTM LC 242,商业上可从BASF Corp.得到,Tg不适用)。
6 用30%三羟甲基丙烷三丙烯酸酯和5%羟乙基甲基丙烯酸酯稀释的环氧酚醛二丙烯酸酯(商业上可从UCB Chemicals Corp.得到)。
7 1-羟基环己基苯基酮光引发剂(商业上可从得到Ciba SpecialtyChemicals)。
(层1)使用Model CAG-150微凹版式涂覆机和150R压花辊以线速率6.1m/min将表2所示的五种制剂涂覆在连续PET薄膜基底上。使用在100%功率下工作的6kW Fusion H灯泡(商业上可从Fusion WSystems得到)固化涂层。
(层2)将涂覆的薄膜基底装到溅射涂覆机上,并抽吸至压力为2×10-6Torr。使用300W和420V,90/10锡氧化物/铟氧化物靶(商业上可从Arconium Specialty Alloys得到),含有30sccm氩气和8sccm氧气且压力为4毫乇的气体混合物,织物速率为0.127米/分钟,在层1的制剂上沉积40nm厚ITO无机氧化物层。
(层3和层4)分别使用与层1和层2相同的条件,在层2上涂覆第二聚合物层形成层3,在层3上沉积第二ITO层形成层4。
然后在50℃和100%RH下测定每段涂覆的阻透组件的WVTR。结果列于下面表3中:
表3
聚合物层 | Tg,℃ | WVTR@50℃/100%RH,g/m2/天 |
制剂11 | 43 | 1.08 |
制剂22 | 110 | 0.63 |
制剂33 | 93.5 | 1.47 |
制剂44 | -- | 0.1 |
制剂55 | 122 | 0.09 |
1 1,6-己二醇二丙烯酸酯和β-羧乙基丙烯酸酯的聚合物。
2 环己烷二甲醇二丙烯酸酯和β-羧乙基丙烯酸酯的聚合物。
3 丙烯酸异冰片酯和β-羧乙基丙烯酸酯的聚合物。
4 PALIOCOLORTMLC 242的聚合物。
5 环氧酚醛二丙烯酸酯和β-羧乙基丙烯酸酯的聚合物。
如表3中制剂1、2和5所示,WVTR值随聚合物Tg增大而降低。制剂1、2和5的聚合物从大量多功能单体或低聚物制得。制剂3和4观察到不同行为。制剂3含有75%单功能单体,因此没有与制剂1、2和5相同的方式交联。制剂4基于从UV固化液晶二丙烯酸酯单体得到的液晶聚合物,因此没有与制剂1、2和5表现出相同行为。
实施例7
层压阻挡结构
使用光学粘合剂以相对方式将在PET基底上具有六层叠层的两个阻透组件粘合在一起组装成层压阻透组件。得到的层压阻透组件具有PET/聚合物1/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO/光学粘合剂/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO/聚合物1/PET结构。阻透组件的形成及层压如下:
使用Model CAG-150微凹版式涂覆机和110R压花辊以速率6.1m/min用制剂6(下表4所示)涂覆HSPE 50 0.05mm PET薄膜(商业上可从Teijin得到,Tg=70℃)。使用在100%功率下工作的Fusion F600H灯泡固化涂层,得到的层称为″聚合物1″。使用光扫描差示量热法(″photo DSC″)测定聚合物1具有122.8℃ Tg。
(层2)使用针对实施例5中SiAlO无机氧化物层的条件,在层1上沉积60nm厚SiAlO无机氧化物层。
(层3)使用层1的条件,但4.6m/min的涂覆速率,用制剂7(下表4所示)涂覆层2并固化,得到的层称为″聚合物2″。聚合物2具有90℃ Tg。
(层4,层5和层6)。分别使用与层2和层3相同的条件,在层3上沉积第二SiAlO层以形成层4,在层4上涂覆第二层聚合物2以形成层5,在层5上沉积第三层SiAlO以形成层6,从而提供具有PET/聚合物1/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO结构的阻透组件。
表4
制剂 | ||
成分 | 1 | 2 |
EBECRYLTM 629 | 145.5 | - |
β-CEA | 37.5 | - |
IRGACURE 184 | 9.03 | - |
UVI-69741 | - | 2.25 |
EHPE31502 | - | 42.75 |
MEK | 972 | 405 |
1 CYRACURETM UVI-6974三芳基磺酸六氟锑酸盐(商业上可从Ciba Specialty Chemicals得到)。
2 聚酯EHPE3150固体脂环族环氧树脂(商业上可从DaicelChemical Industries得到,Tg=90℃)。
得到的涂覆阻透组件卷状物分成两卷,并使用3MTM 8141光学透明层压粘合剂(商业上可从3M Co.得到)和连续辊至辊层合机以相对方式层压在一起。检测非层压阻透组件在38℃和100%RH下的WVTR值,及层压阻透组件在38℃/100%RH和50℃/100%RH下的WVTR值。结果列于下面表5中:
表3
阻透组件结构 | WVTR g/m2/天@100%RH和38℃或50℃ |
PET/聚合物1/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO | 0.041(38℃) |
PET/聚合物1/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO/光学粘合剂/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO/聚合物1/PET | <0.005(38℃) |
PET/聚合物1/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO/光学粘合剂/SiAlO/聚合物2/SiAlO/聚合物2/SiAlO/聚合物1/PET | <0.005(50℃) |
如表5结果所示,相对层压步骤使WVTR降低。WVTR小于0.005g/m2/天,在38℃和50℃的测量温度下,低于MOCON PERMATRAN-W3/3l WVTR测试系统的检测限制速率。
实施例8
OLED装置
实施例1的阻透组件样品再次装到连续辊至辊真空处理室中,按如下沉积上表面ITO导电层:
(层8)使用与层6相同的条件溅射沉积ITO,但使用0.19米/分钟织物速率,以提供沉积在层7的丙烯酸酯上的138nm厚ITO层。
使用X-ACTOTM刀(商业上可从Hunt Corporation得到)将得到的上表面导电阻挡物切成22×22mm的正方形。用丙酮漂洗和空气干燥后,使用MICRO-RIE Series 80等离子体系统(商业上可从Technics,Inc.得到)并在50瓦功率和200毫乇氧气压力下接触4分钟,从而在氧气等离子体中清洗正方形。BAYTRONTMP 4083聚噻吩(商业上可从得到Bayer Corporation)的1%固体水溶液以2500rpm速率于30秒内旋涂在清洁的正方形上。将正方形固持在旋涂机真空卡盘上,首先将22×22×1mm载玻片放在真空卡盘上,应用真空以固定载玻片,在载玻片上面加入一滴甲醇,在甲醇上面放置清洁的正方形,将正方形边缘与载玻片边缘对齐。甲醇充在载玻片和正方形间的空间中,并且在旋涂操作中固定正方形。在氮气氛中,在70℃热平板上干燥涂覆的正方形。
将涂覆的正方形转移至钟形蒸发室中,并抽空至约10-6torr。通过带有19.5mm正方开口的遮光板在涂覆的正方形上依序热气相沉积下面的层:
(层1)2245厚的4,4′,4″-三(N-(3-甲基苯基)-N-苯基氨基)三苯基胺层(″MTDATA″,商业上可从H.W.Sands Corp.得到),用7%四氟四氰基苯醌二甲烷(″FTCNQ″,商业上可从Tokyo Kasei Kogyo Co.,Tokyo,Japan得到)掺杂。
(层2)300厚的N,N′-二(萘基-1)-N,N′-二苯基联苯胺(″α-NPB″,商业可以OPD7534从H.W.Sands Corp.得到)。
(层3)300厚的三(8-羟基喹啉基)铝(″AlQ3″,商业上可从H.W.Sands Corp得到),用1%(10-(2-苯并噻唑基)-2,3,6,7-四氢-1,1,7,7-四甲基1-1H,5H,11H-[1]苯并吡喃基[6,7,8-ij]喹啉-11-酮(″C545T″染料,商业上可从Eastman Kodak Co.得到)。
(层4)200厚的AlQ3层。
蒸汽涂覆的正方形转移至带有薄膜蒸发室的手套箱中(″Edwards500″,商业上可从BOC Edwards得到),热沉积阴极。将1000厚钙层(使用商业上可从Alfa-Aesar Co.得到的靶)和2000厚银层(使用商业上可从Alfa-Aesar Co.得到的靶)在约10-7torr下通过带有1cm2圆孔的金属遮光板相继沉积在正方形上,使得阴极大致沉积在正方形的中心。使带有鳄鱼夹的ITO阳极与带有细金线的Ca/Ag阴极接触,当使约4~9伏DC通过得到的OLED装置时,发出绿光。
按2002年12月19日提交的未决美国专利申请10/324,585中所述,用铜箔封装装置。将约50×100mm的3MTM Thermo-Bond薄膜845EG热层压薄膜(0.06mm粘合剂厚度)标记在带有25mm2的2×8栅格的释放衬垫侧。使用手持打孔机在每个25mm2中心打出6mm圆孔。将带孔的热层压薄膜放在约125×75mm的0.05mm厚Cu箔上(商业上可从McMaster-Carr Supply Co.得到),其中粘合剂侧接触箔,然后放在76×229×0.64mm铝板上(商业上可从Q-panel Company得到),其中释放衬垫侧接触铝板。得到的组件连续三次通过TDE Systems ModelHL-4062-辊热层合机(商业上可从Kmart Corp.得到),在约102℃下操作,将粘合剂薄膜层压到Cu箔上,使箔在粘合剂中形成6mm孔。从铝载体板上除去层压Cu箔,用剪刀切成25mm2,放入装有发绿光OLED装置的手套箱中。25mm2层压Cu箔用剪刀切成约20mm2,使得粘合剂层中的6mm孔大约保持在正方形的中心。然后除去释放衬垫,暴露的粘合剂层靠着22mm2OLED装置的阴极侧,粘合剂层中6mm孔大约在OLED装置的阴极中心,层压Cu箔正方形相对于OLED基底旋转45°,使得层压Cu箔正方形的角落对齐并超出OLED基底边缘的中点。得到的组件用摄子固定在一起,放在100℃烤盘上约20秒,使层压Cu箔与OLED基底粘合。然后,在氮气气氛的手套箱中,通过使组件穿过在约100℃下工作的BESTECHTM Model 29622辊式热层合机(商业上可从Rose Art Industries得到),将Cu箔角落折叠在OLED装置前面,并层压。冷却后,通过接触装置角落上的暴露ITO部分使阳极与封装的OLED连接,通过接触Cu箔使阴极连接。当施加电流时,从装置发出绿光。
本领域所属技术人员在本发明范围内可以对本发明做出各种修改和变化。本发明不限于用于上面所说明的那些。
Claims (42)
1.一种阻透组件,包括Tg大于或等于HSPET的Tg的挠性可见光透过的基底,该基底用Tg大于或等于HSPET的Tg的第一聚合物层覆盖,进一步用至少两个可见光透过的无机阻挡层覆盖,该无机阻挡层通过至少一个Tg大于或等于HSPET的Tg的第二聚合物层隔开,在23℃和90%RH下该阻透组件的氧气透过速率小于0.005cc/m2/天。
2.如权利要求1所述的阻透组件,其中该基底的Tg大于PMMA的Tg。
3.如权利要求1所述的阻透组件,其中该基底的Tg至少约120℃。
4.如权利要求1所述的阻透组件,其中该基底包括热稳定的PET或聚萘二甲酸乙二酯。
5.如权利要求1所述的阻透组件,其中该基底包括聚甲醛、聚乙烯基萘、聚醚醚酮、含氟聚合物、聚碳酸酯、聚α-甲基苯乙烯、聚砜、聚苯醚、聚醚酰亚胺、聚醚砜、聚酰胺酰亚胺、聚酰亚胺或聚酞酰胺。
6.如权利要求1所述的阻透组件,其中该第一或第二聚合物层的Tg大于PMMA的Tg。
7.如权利要求1所述的阻透组件,其中该第一和第二聚合物层的Tg至少约150℃。
8.如权利要求1所述的阻透组件,其中该第一或第二聚合物层包括环己烷二甲醇二丙烯酸酯、甲基丙烯酸异冰片酯、环二丙烯酸酯或三(2-羟乙基)异氰脲酸酯三丙烯酸酯的聚合物。
9.如权利要求1所述的阻透组件,其中该阻透组件中的该第一、第二和任何其他聚合物层的Tg大于或等于PMMA的Tg。
10.如权利要求1所述的阻透组件,其中至少一个无机阻挡层包括金属氧化物。
11.如权利要求1所述的阻透组件,其中至少一个无机阻挡层包括铟锡氧化物。
12.如权利要求1所述的阻透组件,其中至少一个无机阻挡层包括硅氧化物或铝氧化物。
13.如权利要求1所述的阻透组件,其中至少一个无机阻挡层包括铝和硅的混合氧化物。
14.如权利要求1所述的阻透组件,在50℃和100%相对湿度下水蒸汽透过速率小于0.005g/m2/天。
15.如权利要求1所述的阻透组件,在85℃和100%相对湿度下水蒸汽透过速率小于0.005g/m2/天。
16.如权利要求1所述的阻透组件,Tvis至少约60%。
17.如权利要求1所述的阻透组件,其中该组件的至少一部分用导电层或电极覆盖。
18.如权利要求17所述的阻透组件,其中该导电层或电极是可见光透过的。
19.如权利要求1所述的阻透组件,其中该阻透组件中的所有聚合物层是交联的。
20.如权利要求1所述的阻透组件,具有至少三个用Tg至少约150℃的第二聚合物层隔开的可见光透过的无机阻挡层。
21.一种制造阻透组件的方法,包括:
a)提供Tg大于或等于HSPET的Tg的挠性可见光透过的基底;
b)在该基底上形成Tg大于或等于HSPET的Tg的第一聚合物层;
c)在该第一聚合物层上形成可见光透过的第一无机阻挡层;
d)在该第一无机阻挡层上形成Tg大于或等于HSPET的Tg的第二聚合物层;及
e)在该第二聚合物层上形成可见光透过的第二无机阻挡层,
其中在23℃和90%RH下该阻透组件的氧气透过速率小于0.005cc/m2/天。
22.如权利要求21所述的方法,其中该第一或第二聚合物层的Tg大于PMMA的Tg。
23.如权利要求21所述的方法,其中该第一和第二聚合物层的Tg至少约150℃。
24.如权利要求21所述的方法,其中该基底包括热稳定的PET、聚萘二甲酸乙二酯、聚甲醛、聚乙烯基萘、聚醚醚酮、含氟聚合物、聚碳酸酯、聚α-甲基苯乙烯、聚砜、聚苯醚、聚醚酰亚胺、聚醚砜、聚酰胺酰亚胺、聚酰亚胺或聚酞酰胺。
25.如权利要求21所述的方法,其中该第一或第二聚合物层包括环己烷二甲醇二丙烯酸酯、甲基丙烯酸异冰片酯、环二丙烯酸酯或三(2-羟乙基)异氰脲酸酯三丙烯酸酯的聚合物。
26.如权利要求21所述的方法,其中至少一个无机阻挡层包括金属氧化物。
27.如权利要求21所述的方法,其中至少一个无机阻挡层包括铟锡氧化物、硅氧化物、铝氧化物或铝和硅的混合氧化物。
28.如权利要求21所述的方法,其中使用足够数量的无机阻挡层,其中该基底、第一和第二聚合物层具有足够高的Tg,从而该阻透组件是可见光透过的,并且在50℃和100%相对湿度下水蒸汽透过速率小于约0.005g/m2/天。
29.如权利要求21所述的方法,其中使用足够数量的无机阻挡层,其中该基底、第一和第二聚合物层具有足够高的Tg,从而该阻透组件是可见光透过的,并且在85℃和100%相对湿度下水蒸汽透过速率小于约0.005g/m2/天。
30.一种显示或照明装置,包括至少部分用阻透组件覆盖的水汽或氧气敏感性光源或光阀,该阻透组件包括Tg大于或等于HSPET的Tg的挠性可见光透过的基底,该基底用Tg大于或等于HSPET的Tg的聚合物层覆盖,进一步用至少两个可见光透过的无机阻挡层覆盖,该无机阻挡层通过至少一个Tg大于或等于HSPET的Tg的聚合物层隔开。
31.如权利要求30所述的显示装置,其中该第一或第二聚合物层的Tg大于PMMA的Tg。
32.如权利要求30所述的显示装置,其中该第一和第二聚合物层的Tg至少约150℃。
33.如权利要求30所述的显示装置,其中该基底包括热稳定的PET、聚萘二甲酸乙二酯、聚甲醛、聚乙烯基萘、聚醚醚酮、含氟聚合物、聚碳酸酯、聚α-甲基苯乙烯、聚砜、聚苯醚、聚醚酰亚胺、聚醚砜、聚酰胺酰亚胺、聚酰亚胺或聚酞酰胺。
34.如权利要求30所述的显示装置,其中该第一或第二聚合物层包括环己烷二甲醇二丙烯酸酯、甲基丙烯酸异冰片酯、环二丙烯酸酯或三(2-羟乙基)异氰脲酸酯三丙烯酸酯的聚合物。
35.如权利要求30所述的显示装置,其中至少一个无机阻挡层包括金属氧化物。
36.如权利要求30所述的显示装置,其中至少一个无机阻挡层包括铟锡氧化物、硅氧化物、铝氧化物或铝和硅的混合氧化物。
37.如权利要求30所述的显示装置,其具有足够数量的无机阻挡层,并且具有足够高Tg的基底、第一和第二聚合物层,从而该阻透组件是可见光透过的,并且在50℃和100%相对湿度下水蒸汽透过速率小于约0.005g/m2/天,在23℃和90%RH下氧气透过速率小于0.005cc/m2/天。
38.如权利要求30所述的显示装置,其具有足够数量的无机阻挡层,并且具有足够高Tg的基底、第一和第二聚合物层,从而该阻透组件是可见光透过的,并且在85℃和100%相对湿度下水蒸汽透过速率小于约0.005g/m2/天。
39.如权利要求30所述的显示装置,其中该阻透组件具有至少三个用Tg至少约150℃的聚合物层隔开的可见光透过的无机阻挡层。
40.如权利要求30所述的显示装置,在该阻透组件和该光源或光阀之间还包括导电层。
41.如权利要求30所述的显示装置,其中该光源或光阀包括有机发光器件。
42.如权利要求30所述的显示装置,其中该光源或光阀包括液晶显示器。
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- 2003-04-02 US US10/405,284 patent/US7018713B2/en not_active Expired - Lifetime
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2004
- 2004-03-31 EP EP10182971.1A patent/EP2277698B1/en not_active Expired - Lifetime
- 2004-03-31 WO PCT/US2004/009956 patent/WO2004089620A2/en active Application Filing
- 2004-03-31 KR KR1020057018768A patent/KR101119702B1/ko active IP Right Grant
- 2004-03-31 CN CN2004800092597A patent/CN1771127B/zh not_active Expired - Lifetime
- 2004-03-31 JP JP2006509551A patent/JP5117717B2/ja not_active Expired - Lifetime
- 2004-03-31 EP EP16175849.5A patent/EP3121003A1/en not_active Withdrawn
- 2004-03-31 EP EP04749603.9A patent/EP1613468B1/en not_active Expired - Lifetime
- 2004-04-01 TW TW093109106A patent/TWI357915B/zh not_active IP Right Cessation
- 2004-04-01 MY MYPI20041201A patent/MY135796A/en unknown
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2005
- 2005-11-14 US US11/272,929 patent/US7486019B2/en not_active Expired - Lifetime
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2009
- 2009-01-30 US US12/363,457 patent/US7980910B2/en not_active Expired - Lifetime
- 2009-11-13 US US12/617,818 patent/US7940004B2/en not_active Expired - Lifetime
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2010
- 2010-01-13 US US12/686,801 patent/US20100119840A1/en not_active Abandoned
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2011
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Also Published As
Publication number | Publication date |
---|---|
KR101119702B1 (ko) | 2012-03-19 |
US20040195967A1 (en) | 2004-10-07 |
TW200508296A (en) | 2005-03-01 |
EP2277698B1 (en) | 2020-07-15 |
JP2006525152A (ja) | 2006-11-09 |
CN1771127B (zh) | 2010-12-15 |
JP2011131601A (ja) | 2011-07-07 |
WO2004089620A3 (en) | 2005-02-17 |
US20090142476A1 (en) | 2009-06-04 |
EP1613468A2 (en) | 2006-01-11 |
US20100073936A1 (en) | 2010-03-25 |
JP5117717B2 (ja) | 2013-01-16 |
US20100119840A1 (en) | 2010-05-13 |
JP5702188B2 (ja) | 2015-04-15 |
EP1613468B1 (en) | 2019-10-09 |
US20060062937A1 (en) | 2006-03-23 |
US7940004B2 (en) | 2011-05-10 |
US7018713B2 (en) | 2006-03-28 |
KR20060010737A (ko) | 2006-02-02 |
MY135796A (en) | 2008-06-30 |
EP2277698A1 (en) | 2011-01-26 |
US7980910B2 (en) | 2011-07-19 |
WO2004089620A2 (en) | 2004-10-21 |
TWI357915B (en) | 2012-02-11 |
US7486019B2 (en) | 2009-02-03 |
EP3121003A1 (en) | 2017-01-25 |
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