CN100530756C - 具有梯度组成的扩散阻挡涂层以及结合了该涂层的器件 - Google Patents
具有梯度组成的扩散阻挡涂层以及结合了该涂层的器件 Download PDFInfo
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- CN100530756C CN100530756C CNB038250721A CN03825072A CN100530756C CN 100530756 C CN100530756 C CN 100530756C CN B038250721 A CNB038250721 A CN B038250721A CN 03825072 A CN03825072 A CN 03825072A CN 100530756 C CN100530756 C CN 100530756C
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Abstract
一种复合制品,其包括基片(340),该基片具有至少一个表面和布置在基片表面上的梯度组成的涂层(350)。该涂层材料的组成沿所述涂层的厚度基本连续地变化。该涂层(350)降低了氧气、水蒸气和其它化学物质通过基片(340)的透过率,使得该复合制品可以有效地用作扩散阻挡物,以保护化学敏感器件(320)或材料。一种有机发光器件(310)结合了此复合制品以向其提供延长的寿命。
Description
技术领域
本发明一般性地涉及具有改善的耐化学物质扩散的复合膜,并涉及结合了该复合膜的器件。具体地,本发明涉及具有至少一种有机电致发光材料的发光器件,其结合了该复合膜并具有改善的环境稳定性。
背景技术
电致发光(″EL″)器件,其可以划分为有机的或无机的,在图形显示器(graphic display)和成像领域中是公知的。已经为了多种应用以不同形状制造了EL器件。然而,无机EL器件一般有需要高激活电势和低亮度的问题。另一方面,更最近开发的有机EL器件(“OELDs”)除制造简单外,还提供了更低激活电势和更高亮度的优势,并且因此提供了更为广泛的应用的前景。
OELD通常是形成在基片上的薄膜结构,基片例如玻璃或透明塑料。有机EL材料的发光层和任选的邻近半导体层夹在负极和正极(anode)之间。半导体层可以是空穴(正电荷)-注入或电子(负电荷)-注入层,并且还包括有机材料。发光层的材料可以选自许多有机EL材料。发光有机层本身可以由多个亚层组成,各亚层包括不同的有机EL材料。现有技术的有机EL材料可以发出电磁(″EM″)辐射,该辐射具有可见光谱中的窄范围波长。除非特别说明,术语″EM辐射″和″光″在本申请中互换使用,以一般地表示具有紫外(″UV″)至中红外(″mid-IR″)范围内的波长的辐射,换句话说,具有约300nm~约10微米范围内的波长。为了获得白光,现有技术的器件结合了紧密排列的OELDs,发射蓝、绿和红光。这些颜色混合在一起产生白光。
常规OELDs建造在玻璃基片上,这是因为玻璃的透明性和对氧气与水蒸气的低渗透性的组合。这些和其它反应性物质的高渗透性会导致器件的腐蚀或其它劣化。然而,玻璃基片不适用于需要柔韧性的某些应用。此外,涉及大玻璃基片的制造工艺固有地较慢,因此导致高制造成本。已经使用了柔韧的塑料基片建造OLED。然而,这些基片对于氧气和水蒸气不是不可透的,因此它们本身不适于制造长效(long-lasting)OELDs。为了改善这些基片对氧气和水蒸气的耐性,已经将交替的聚合物层和陶瓷材料层施用于基片的表面上。已经认为在这种多层阻挡层中,聚合物层起作用,以掩盖在相邻的陶瓷层中的任何缺陷,来降低通过由陶瓷层中的缺陷可能造成的通道对氧气和/或水蒸气的扩散率。然而,在聚合物层和陶瓷层之间的界面通常由于邻近材料的不相容性而较弱,因此这些层易于分层。
因此,仍然需要具有耐用的膜,其具有降低的对环境反应性材料的扩散率。还非常需要提供这些膜以制备柔韧的OELDs,其对环境因素造成的劣化非常耐用。
发明内容
本发明提供一种基片,其具有布置在其表面上的至少一种涂层,该涂层能够降低化学物质通过的扩散率。该涂层包括一种材料,该材料的组成沿其厚度方向变化。这种涂层将被定义成下面的可互换的术语:“具有梯度(graded)组成的扩散阻挡涂层”、“梯度组成的扩散阻挡涂层”、“梯度组成的阻挡涂层”、“扩散阻挡涂层”或简单的“梯度组成涂层”。
在本发明的一方面,基片包括聚合物材料。
在本发明的另一方面,基片和涂层之间的区域是扩散的,使得从主体(bulk)基片的组成到邻近基片的涂层部分的组成存在逐步的变化。在该实施方式中,邻近基片的涂层的材料渗入基片中。
在本发明的另一方面,装配体中含有至少具有梯度组成的扩散阻挡涂层的基片,该装配体包括对化学物质敏感的器件,以防止这种装配体受到这些化学物质的损害。
在本发明的另一方面,这种器件是OELD,其包括一对电极和夹在电极间的有机发光层。
本发明的另一方面,OELD夹在两层膜之间,各层膜带有具有梯度组成的扩散阻挡涂层。
本发明还提供制造涂覆有扩散阻挡涂层的基片的方法,该涂层具有梯度组成。该方法包括以下步骤:(a)提供具有基片表面的基片;(b)在基片表面上沉积具有第一组成的涂层材料;和(c)基本上连续地改变涂层材料的组成,使得涂层的组成沿涂层的厚度方向从第一组成变化到第二组成。
在本发明的另一方面,提供制造装配体的方法,该装配体包括对化学物质敏感的器件,该方法包括以下步骤:(a)提供至少涂覆有扩散阻挡涂层的基片,该涂层具有梯度组成;和(b)在基片上布置该器件。
在本发明的另一方面,该器件为OELD,并且该方法包括以下步骤:(a)提供至少涂覆有扩散阻挡涂层的基片,该涂层具有梯度组成;(b)在基片上形成第一电极;(c)在第一电极上形成有机发光层;和(d)有机发光层上形成第二电极。
本发明的另一方面,将OLED和涂覆有扩散阻挡涂层的基片层压在一起以形成光源,该OLED包括一对电极和布置在该电极对之间的有机发光层,该扩散阻挡涂层具有梯度组成。
从精读本发明下面的详细描述和附图,本发明的其它特征和优势是很明显的,附图中相同的标号表示相同的元件。
附图说明
图1是使用膨胀热等离子体化学气相沉积(expanding thermal-plasmachemical-vapor deposition)的沉积装置的示意图。
图2是用于连续沉积的图1装置的示意图。
图3是使用射频等离子体增强的化学气相沉积(radio-frequencyplasma-enhanced chemical-vapor deposjtion)的沉积装置示意图。
图4显示本发明的梯度组成的阻挡涂层在各种深度中的元素组成。
图5比较了通过未涂覆的基片和涂覆有梯度组成的阻挡涂层的基片的氧气透过率。
图6比较了通过未涂覆的基片和涂覆有梯度组成的阻挡涂层的基片的水透过率。
图7显示通过具有梯度组成的阻挡涂层的基片的相对透光率,与通过未涂覆的基片的相对透光率进行比较。
图8示意性地显示了使用带有具有梯度组成的阻挡涂层的基片的器件。
图9示意性地显示了OELD的构造。
图10显示了包括空穴注入增强层的OELD的另一实施方式。
图11显示了包括空穴注入增强层和空穴传输层的OELD的另一实施方式。
图12显示了包括电子注入和传输层的OELD的另一实施方式。
图13显示了在具有梯度组成的阻挡涂层的基片和反射层之间密封的OELD。
图14显示了在两个基片之间密封的OELD,每个基片都具有梯度组成的阻挡涂层。
图15显示了具有光转化层的密封的OELD。
发明详述
本发明一方面提供具有至少布置在其表面上的涂层的基片,该涂层能够降低化学物质通过基片的扩散率。涂层包括一种材料,该材料的组成沿其厚度方向变化。该涂覆的基片可用于对多种器件或部件如电子器件提供保护,该器件或部件容易受到环境中通常存在的反应性化学物质的影响。在另一实例中,该基片或膜带有具有梯度组成的扩散阻挡涂层,能够有利地用于诸如食品等材料的包装,该材料易于被通常存在于环境中的化学或生物试剂损坏。
OELDs中的有机发光材料和/或负极(cathode)材料易于受环境中存在的反应性物质的侵害,该物质例如氧气、水蒸气、硫化氢、SOx、NOx、溶剂等。具有梯度组成的扩散阻挡涂层的膜特别适用于延长这些器件的寿,并使它们更经济可行。本发明的阻挡涂层可以通过将反应物质的反应或重组的产物沉积到基片或膜上而制备。改变相对供应率或改变反应物质的本性导致沿其厚度方向具有梯度组成的涂层。因此,本发明的涂层不具有明显的界面,在该界面处涂层的组成急剧变化。这种组成的急剧变化倾向于在涂层结构中导入弱化点(weak spots),在这些弱化点处可能易于发生分层。受益于具有梯度组成的扩散阻挡涂层的基片材料为有机聚合物材料,例如聚对苯二甲酸乙二醇酯(″PET″)、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂;聚酯,例如Mylar(E.I.du Pont de Nemours&Co.制造);聚酰亚胺,例如Kapton H或Kapton E(du Pont制造)、ApicalAV(Kanegafugi Chemical Industry Company制造)、Upilex(UBE Industries,Ltd.制造);聚醚砜(“PES”,Sumitomo制造);聚醚酰亚胺,例如Ultem(GeneralElectric Company制造);和聚乙烯萘(polyethylenenaphthalene)(″PEN″)。
沿厚度方向区域的合适的涂层组合物是有机的、无机的或陶瓷材料。这些材料通常是反应等离子体物质的反应或重组产物,并沉积在基片表面上。有机涂层材料通常包括碳、氢、氧和任选的其它微量元素,例如硫、氮、硅等,取决于反应物的类型。导致涂层中的有机组成的合适的反应物是具有高达15个碳原子的直链或支链烷烃、烯烃、炔烃、醇、醛、醚、烯化氧、芳族化合物(aromatics)等。无机和陶瓷涂层材料通常包括下面元素的氧化物、氮化物、碳化物、硼化物或其组合:IIA、IIIA、IVA、VA、VIA、VIIA、IB和IIB族元素;IIIB、IVB和VB族的金属;和稀土金属。例如,可以通过重组产生自硅烷(SiH4)和诸如甲烷或二甲苯的有机材料的等离子体,将碳化硅沉积在基片上。可以通过从产生自硅烷、甲烷和氧气或硅烷和环氧丙烷的等离子体来沉积碳氧化硅(silicon oxycarbide)。也可以通过从产生自有机硅氧烷前体的等离子体来沉积碳氧化硅,该有机硅前体例如四乙氧基硅烷(TEOS)、六甲基二硅氧烷(HMDSO)、六甲基二硅氮烷(HMDSN)或八甲基环四硅氧烷(D4)。可以从产生自硅烷和氨的等离子体来沉积氮化硅。可以通过产生自酒石酸铝和氨的混合物的等离子体来沉积碳氮氧化铝(Aluminum oxycarbonitride)。可以选择反应物的其它组合以获得所需的涂层组成。特定反应物的选择是本领域技术人员已知的。通过在反应产物沉积的过程中,改变引入到反应器室的反应物的组成,以形成涂层来获得涂层的梯度组成。
涂层厚度通常为约10nm~约10000nm,优选为约10nm~约1000nm,和更优选为约10nm~约200nm。可能需要选择不阻碍光通过基片的透射的涂层厚度,例如透光率的降低小于约20%,优选小于约10%和更优选小于约5%。涂层可以通过许多沉积技术之一形成,沉积技术例如等离子体增强的化学气相沉积(″PECVD″)、射频等离子体增强的化学气相沉积(″RFPECVD″)、膨胀热等离子体化学气相沉积(″ETPCVD″),包括反应溅射的溅射、电子回旋加速器共振等离子体增强的化学气相沉积(electron-cyclotron-resonance plasma-enhanced chemical-vapordeposition)(ECRPECVD″)、电感耦合等离子体增强的化学气相沉积(″ICPECVD″)或其组合。
图1示意性地显示了用于ETPCVD技术的反应器10和相关设备。至少一个通常由钨制成的负极20布置在负极套30中。正极板40布置在负极套30的一端。任选地,至少负极套是电未接地的(electrically floating)。在负极20和正极40之间施加的电压产生用于等离子体产生的电弧。载气,例如氩气通过管线50供应到电弧中。产生等离子体并从在正极40中心的喷嘴或喷孔70离去。可以通过管线60将第一反应物气体在负极20和正极40之间的某点供入载气管线。第二反应物气体通过供应管线80供应到喷孔70下游处的某点。供应管线80也可以用布置在用于更好混合的膨胀等离子体束84中的开孔环终止。可以配备其它反应物供应管线用于不同的反应物质。从反应物气体产生的自由基合并,并运载到基片90,在其上沉积,该基片在基片支撑物100上被支撑。基片支撑物100布置在与喷嘴70有一定距离并与其相对处,并且通过基片支撑物轴110,相对于喷嘴70可移动。反应器10经真空线路112保持在真空下。例如,当希望在基片上的涂层包括氮化硅时,第一反应物气体可以为氨气,和第二反应物气体可以为硅烷。第一和第二反应物气体的相对供应速率在沉积过程中变化,以改变当建立涂层时沉积材料的组成。虽然图1示意性地显示了作为单片的基片90,涂层可以在相似的设备中沉积在连续基片上。例如,图2显示了薄聚合物基片115的供应辊120,该供应辊120布置在基片支撑物100的一侧,并且卷绕辊122布置在基片支撑物100的另一侧。当辊120连续展开和辊122连续缠绕时,未涂覆的基片膜115在涂层材料通过基片支撑物100上方时连续接收涂层材料。在本发明的另一实施方式中,基片膜115经过与许多重叠的等离子体束相对的区域,各个等离子体束产生有不同或变化的组成以接受涂层,涂层的组成沿其厚度方向连续变化。
在ETPCVD技术中,相对于常规的PECVD技术,等离子体在高压下产生。电弧通道65中的等离子体的速度为声速的数量级。等离子体经过喷嘴70超声速地膨胀到反应器室10中,并亚声速地(subsonically)向基片90移动。
图3示意性地显示RFPECVD技术的反应器200和相关设备。射频(″RF″)能量通过RF发生器和放大器204和匹配网络208施加到布置在反应器200中的负极210,该网络包括用于产生全系统的适当阻抗或其它电气性能的多个电气和/或电子部件,以将来自RF发生器和放大器204的能量转移最大化。基片90布置在与负极210相对的基片支撑物100上,以接受等离子体沉积。基片支撑物可以为接地的或电耦合到另一RF发生器和匹配网络,如果需要不同的电势。反应物气体或气体的混合物通过气体供应214引入气体分配器212。气体分配器212可以具有促进气体的分配基本均匀的任何形状。例如其可以为具有穿孔的环,该穿孔直接朝向基片支撑物100。或者,负极210本身可以为中空和多孔的并接受反应物气体。产生等离子体,并通过RF场保持,流向基片90。等离子体中的前体物质结合并沉积在基片90上。在涂层建立的同时,通过改变供入分配器212的反应物气体混合物的组成,可以改变涂层的组成。如上所述,通过配备未卷绕的供应辊和卷绕辊,连续基片,例如聚合物膜可以涂覆有梯度组成的涂层。基片同样可以向多个沉积站(deposition stations)的相反向移动,该沉积站供应不同的气体组合物,以产生具有梯度组成涂层的连续膜。
ECRPECVD是另一种合适的沉积技术。该方法在低压下操作,通常小于约0.5mm Hg,并通常无需电极。通过微波产生放电。使用磁场以形成电子气体的共振条件,由于电子在距基片一定距离处加速,这导致非常高度的电离。低压保持了高数密度的游离自由基,直至等离子体到达基片,并防止了其通常不理想的剧烈轰击。
ICPECVD是另一种无电极沉积技术,其可以在低压下产生高密度等离子体。通过电磁场形成等离子体,该电磁场由布置在沉积室一端的外部的同心感应线圈产生。
基片在相对端布置在沉积室中。通常在远小于0.5mm Hg的压力下进行沉积。
在本发明的另一实施方式中,可以控制等离子体中离子的能量,以使它们穿入基片的表面层,以在主体基片的组成和涂层的组成之间产生扩散过渡区域(diffuse transition region)。这种过渡防止了组成的急剧变化,并降低了涂层分层的任何可能性。
使用RFPECVD技术将厚度为约500nm的梯度组成的涂层形成在聚碳酸酯基片上,该基片的尺寸为约10cmx10cm和厚度为约0.2mm,并测量水蒸气和氧气透过率(transmission)。使用硅烷(最大流量为约500标准cm3/分钟),氨气(最大流量为约60标准cm3/分钟)和环氧丙烷(最大流量为约500标准cm3/分钟)来制备梯度涂层,该涂层包括硅、碳、氧和氮。改变沉积过程中反应物气体的流量,以使涂层的组成沿其厚度方向连续变化。当从环氧丙烷产生等离子体时,施加到RF电极的能量为约100W,和当硅烷和氨气的混合物供入反应器中时,所述能量为约200W。反应器中的真空水平为约0.2mm Hg并且平均温度为约55℃。图4显示通过动态XPS测量作为溅射时间函数的涂层的元素组成,以在动态XPS测试过程中除去涂层的部分厚度,这直接与涂层的厚度相关。氧气和水蒸气透过率测试结果显示在图5和6中。与未涂覆的基片相比,通过涂覆的塑料基片的氧气透过率被降低了三个数量级以上,而且水蒸气透过率降低了两个数量级以上。在可见光谱的不同波长下,通过涂覆的基片的透光率显示于图7中。在蓝色~红色区域(约430nm~约700nm)中透光率的下降通常小于7%。
可有利地使用涂覆有梯度组成涂层的塑料基片以制备基于有机发光材料的柔韧的光源,该涂层通过上述任何方法形成。其它可得益于梯度组成涂层所提供的保护的电子器件为例如包括液晶显示器的显示器、光电器件、柔韧的集成电路或医用诊断系统的部件。术语″柔韧″指能够弯曲成曲率半径小于约100cm的形状。术语″基本透明的″指使在可见光范围(即在约400nm~约700nm的波长范围),光的总透过率为至少约50%,优选至少约80%,更优选为至少90%。应该理解梯度组成的阻挡涂层的组成不必从其一个表面向另一表面单调变化。单调变化的组成仅仅是本发明的用于阻挡的梯度组成的一种情况。
图8是本发明实施方式的示意图。应该理解本申请的附图不是按照比例绘制的。OELD或发光器件310包括有机EL组件320,其布置在上述的具有梯度组成的阻挡涂层350的基本透明的基片340上。梯度组成的阻挡涂层350可以布置或以其它方式形成在基片340邻近有机EL组件320的一个或两个表面上。优选,梯度组成的阻挡涂层350布置或形成在基片340邻近有机EL组件320的表面上,或者其可以完全覆盖基片340。虽然图8示意性地显示了在基片340和涂层350之间的明显界面,如上所述可以形成该涂层以使在其间没有急剧的界面。
基片340可以为单片或包括多个不同材料的相邻片的结构,并且其折射率(或折射指数)为约1.05~约2.5,优选为约1.1~约1.6。优选地,基片340由基本透明的聚合物材料制成。合适的聚合物材料的实例为聚对苯二甲酸乙二醇酯(″PET″)、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂、聚酯、聚酰亚胺、聚醚酰亚胺、PES、PEN、聚降冰片烯或聚环状烯烃。
如图9所示,发光组件320包括至少一种有机EL材料的至少一层330,其夹在电极对322和338之间。如下面描述的,在电极和有机EL材料的层330之间,发光组件可包括一个或多个附加层。当通过电源326供应电压,并施加到电极322和338时,从有机EL材料发光。在优选的实施方式中,电极322为负极,注入负电荷载流子(电子)到有机EL层330中,并由具有低功函,例如小于约4eV的材料制成。适用于作为负极的低功函材料为K、Li、Na、Mg、La、Ce、Ca、Sr、Ba、Al、Ag、In、Sn、Zn、Zr、Sm、Eu、其合金或其混合物。优选的制造负极层322的材料为Ag-Mg、Al-Li、In-Mg、和Al-Ca合金。也可以为分层的非合金结构,例如薄层的金属,例如Ca(厚度为约1~约10nm)或非金属,例如LiF,被某些其它金属的较厚层覆盖,例如铝或银。在该实施方式中,电极338为正极,注入正电荷载流子(或空穴)至有机层330,并由具有高功函的材料制成,功函例如大于约4.5eV,优选为约5eV~约5.5eV。氧化铟锡(″ITO″)通常用于该目的。ITO对于光透射是基本透明的,并允许至少80%的光穿过其中。因此,从有机电致发光层330发射的光可以容易地通过ITO正极层逃离,而没有被严重地削弱。其它适用作正极层的材料为氧化锡、氧化铟、氧化锌、氧化铟锌、氧化镉锡及其混合物。此外,用于正极的材料可以掺杂有铝或氟以改善电荷注入性能。电极层322和338可以通过物理气相沉积、化学气相沉积、离子束辅助沉积、或溅射沉积在下层的元素上。薄的基本透明的金属层也是合适的。
虽然负极和正极层322和338的优选顺序如上所述,电极层也可以是相反的。电极层322和338可以分别作为正极和负极。通常此时负极层的厚度为约200nm。
有机EL层330作为空穴和电子二者的传输介质。在该层中,这些激发的物质结合,并降低到较低的能级,同时在可见光范围发射EM辐射。选择有机EL材料以在所需的波长范围内电致发光。有机EL层330的厚度优选保持在约100~约300nm的范围内。有机EL材料可以为聚合物、共聚物、聚合物的混合物或具有不饱和键的较低分子量的有机分子。这些材料具有离域的JI电子体系,该体系赋予聚合物链或有机分子支持具有高迁移率的正和负电荷载流子的能力。合适的EL聚合物为聚(N-乙烯基咔唑)(″PVK″,在约380-500nm波长发射紫~蓝光),聚(烷基芴),例如聚(9,9-二己基芴)(410-550nm)、聚(二辛基芴)(在最大EL发射处波长为436nm)、或聚{9,9-双(3,6-二氧杂庚基)-芴-2,7-二基}(400-550nm);聚(对亚苯基)衍生物,例如聚(2-癸氧基-1,4-亚苯基)(400-550nm)。可以使用这些聚合物的混合物或基于这些聚合物的一种或多种的共聚物,以调节发出的光的颜色。
另一类合适的EL聚合物是聚硅烷。聚硅烷是直链硅氧烷主链的聚合物,该主链被多种烷基和/或芳基侧基取代。它们是沿聚合物主链具有离域σ共轭电子的准一维材料。聚硅烷的实例为聚(二正丁基硅烷)、聚(二正戊基硅烷)、聚(二正己基硅烷)、聚(甲基苯基硅烷)和聚{双(对丁基苯基)硅烷},这些公开于H.Suzuki等人的″Near-Ultraviolet Electroluminescence FromPolysilaness,″331 Thin Solid Films 64-70(1998)。这些聚硅烷发射波长在320nm~约420nm的光。
也可以应用分子量小于约5000的有机材料,其由大量芳族单元构成。这种材料的实例为1,3,5-三{N-(4-二苯基氨基苯基)苯基氨基}苯,其发射波长在380-500nm的光。有机EL层也可以从较低分子量有机分子制备,例如苯基蒽、四芳基乙烯、香豆素、红荧烯、四苯基丁二烯、蒽、二萘嵌苯、蔻或其衍生物。这些材料通常发射最大波长为约520nm的光。其它合适的材料为低分子量金属有机复合物,例如铝-、镓-和铟-乙酰丙酮化物,其发射波长范围为415-457nm的光,铝-(皮考基甲基酮)-双{2,6-二(叔丁基)苯氧化物}或钪-(4-甲氧基-皮考基甲基酮)-双(乙酰丙酮化物),其发射波长范围为420-433nm的光。对于白光应用,优选的有机EL材料是发射蓝-绿波长的光的那些。
多于一层的有机EL层可以相继形成在另一层的顶部,各层包括不同的有机EL材料,该有机EL材料在不同波长范围发光。该结构可以有助于调节从整个发光器件310发出的光的颜色。
此外,发光组件320中可以包括一层或更多的附加层,以便提供整个器件310的效率。例如,这些附加层可以用于改善电荷注入(电子或空穴注入增强层)或传输(电子或空穴传输层)到有机EL层。这些层各自的厚度保持在小于500nm,优选小于100nm。这些附加层的材料通常为低到中等分子量(小于约2000)的有机分子。它们可以在制造器件310的期间,通过常规方法,例如喷涂、浸涂、或物理或化学气相沉积而涂布。在本发明的一个实施方式中,如图10所示,空穴注入增强层336形成在正极层338和有机EL层330之间,以在该器件破坏前,在给定的正向偏压下提供更高的注入电流和/或更高的最大电流。因此,空穴注入增强层促进了空穴从正极的注入。空穴注入增强层的合适的材料为公开于美国专利5,998,803中的亚芳基类化合物,例如3,4,9,10-苝四羧酸二酐或双(1,2,5-噻二唑基(thiadiazolo))-对-喹啉并(quino)双(1,3-二硫杂环戊二烯)。
在本发明的另一实施方式中,如图11所示,发光组件320还包括空穴传输层334,其布置在空穴注入增强层336和有机EL层330之间。空穴传输层334的功能是传输空穴并阻挡电子的传输以便空穴和电子最佳地在有机EL层330中结合。适于空穴传输层的材料为三芳基二胺、四苯基二胺、芳族叔胺、腙衍生物、咔唑衍生物、三唑衍生物、咪唑衍生物、具有氨基的噁二唑衍生物和公开于美国专利6,023,371中的聚噻酚(polythiophenes),将其在此引入作为参考。
在本发明的另一实施方式中,如图12所示,发光组件320包括附加层324,其布置在负极层322和有机EL层330之间。层324具有注入和传输电子至有机EL层330的结合功能。适用于电子注入和传输层的材料为金属有机复合物,例如三(8-喹啉醇化(quinolinolato))铝、噁二唑衍生物、苝衍生物、吡啶衍生物、嘧啶衍生物、喹啉衍生物、喹喔啉衍生物、二苯基醌衍生物和硝基取代的芴衍生物,如公开于美国专利6,023,371,在此将其引入作为参考。
反射金属层360可以布置在有机EL组件320上,以反射发射自基本透明的基片340的任何辐射,并将该辐射定向到基片340,使得增加该方向上发射的总的辐射量。反射金属层360还具有防止反应性环境物质,例如氧气和水蒸气扩散到有机EL组件320的附加功能。否则,此种扩散可能会降低OELD的长期性能。用于反射层360的合适的金属为银、铝及其合金。提供足以基本上防止氧气和水蒸气的扩散的厚度是有利的,只要该厚度基本上不降低整个器件的柔韧性。在本发明的一个实施方式中,可以在该反射层上形成至少一种不同材料的一层或多层附加层,所述不同材料例如不同的金属或金属化合物,以进一步降低氧气和水蒸气扩散到有机EL元件的扩散率。此时,用于这些附加层(或多层)的材料不需要是反射材料。化合物,例如金属化合物、金属氮化物、金属碳化物、金属氧氮化物或金属氧碳化物可以用于此目的。
在本发明的另一实施方式中,如图13所示,在反射金属层360布置在有机EL组件320上之前,可以将基本透明的有机聚合物材料的粘合层358布置在有机EL组件320上。适用于形成该有机聚合物层的材料的实例为聚丙烯酸酯,例如丙烯酸、甲基丙烯酸、这些酸的酯或丙烯腈的均聚物或共聚物;聚氟乙烯、聚偏二氯乙烯、聚乙烯醇、乙烯醇和乙二醛(也称作乙烷二醛(ethanedial)或氧杂醛(oxaaldehyde))的共聚物、聚对苯二甲酸乙二醇酯、聚对亚苯基二甲基(perylene)(基于对-二甲苯的热塑性聚合物)和衍生自环烯烃及其衍生物的聚合物(例如聚(芳基环丁烯),公开于美国专利4,540,763和5,185,391,在此将其引入作为参考)。优选,该粘合层材料是电绝缘的和基本透明的聚合物材料。合适的材料为聚丙烯酸酯。
在本发明的另一实施方式中,如图14所示,具有梯度组成的阻挡涂层372的第二聚合物基片370布置在与基片340相对的有机EL组件320上,以形成围绕有机EL组件320的完全密封。梯度组成的阻挡涂层372可以布置在基片370的任一侧上。可以优选布置梯度组成的阻挡涂层372与有机EL组件320相邻。具有梯度组成的阻挡涂层372的第二聚合物基片370也可以布置在反射金属层360上,以提供对有机EL组件320的进一步保护。可替换地,梯度组成的阻挡层372可以直接沉积在有机EL组件320上,而不是布置在第二聚合物基片(例如370)上。此时,可以消除第二基片(例如370)。
可选择地,具有梯度组成的阻挡涂层372的第二基片370可以布置在有机EL组件320和反射层360之间。当其可以提供某些制造或成本优势时,特别是当涂覆的基片370的透明性也重要时,这种结构可能是理想的。
在本发明的另一实施方式中,发光器件310还包括光散射材料,其布置在从发光器件310发射的光的光路上,以提供来自它的更均匀的光。例如,图15解释了包括布置在基片340上的散射材料的层390的实施方式。通过选择其尺寸在约10纳米~约100微米的颗粒提供该光散射材料。优选的实施方式包括尺寸为约4微米的颗粒。例如,对于发射白光的器件,粒度优选为50-65nm的数量级。光散射材料的颗粒可以有利地分散在基本透明的聚合物成膜材料中,例如上述的那些材料,并且将该混合物成型为可以布置在基片340上的膜。合适的光散射材料是折射率高于成膜材料的固体。因为通常的成膜材料的折射率为约1.3~约1.6,颗粒状散射材料的折射率应该高于约1.6,并且应该在目标波长范围内是光学透明的。此外,优选光散射材料是无毒的,并且充分抵挡暴露在正常周围环境下的降解。对于设计来提供可见照明(波长在约400-700nm)的器件,合适的光散射材料的实例为金红石(TiO2)、二氧化铪(HfO2)、氧化锆(ZrO2)、锆石(ZrO2·SiO2)、钆镓石榴子石(Gd3Ga5O12)、硫酸钡、氧化钇(Y2O3)、钇铝石榴子石(″YAG″,Y3Al5O12)、方解石(CaCO3)、蓝宝石(Al2O3)、金刚石、氧化镁和氧化锗。有必要制备具有高度光学纯度的这些化合物,即在所关心的波长范围吸收光的杂质必须严格最小化。这些化合物不需要是化学计量纯、相纯的,并且可以含有适当的原子取代,例如YAG中Gd可以代替高达60%的钇。锆折射率玻璃的颗粒,例如可以获自Schott Glass Technologies或Corning,Inc.也可以使用,条件是它们对暴露于来自由OELD或其磷光体发射的光的暗花。光的散射也可以用具有粗糙或纹理表面(″漫射膜″)的塑料或玻璃膜获得,其粗糙特征通常在散射光波长的部分(fraction)的数量级上。在本发明的一个实施方式中,基片的一个表面可以是带纹理或粗糙的以便促进光散射。
根据本发明的另一方面,层390中的光散射颗粒可以包括光致发光(″PL″)材料(或者此处也称作″磷光体″),其能够吸收部分由有机EL元件发出的具有第一波长范围的EM辐射,并发射具有第二波长范围的EM辐射。因此,含有这类PL材料能够提供对OELD发出的光的颜色的调节。粒度和颗粒表面与聚合物介质之间的相互作用决定了颗粒在聚合物材料中分散以形成膜或层390的好坏。许多微米尺寸的氧化物材料颗粒,例如氧化锆、钇和稀土石榴子石和卤代磷酸盐通过简单搅拌在标准硅氧烷聚合物中分散良好,该聚合物例如聚(二甲基硅氧烷)。如果有必要,可以加入其它分散剂材料(例如表面活性剂或聚合物材料,如聚(乙烯醇)),例如用于使许多标准磷光体悬浮在溶液中。磷光体颗粒可以通过任何研磨或粉碎方法,例如使用氧化锆-增韧的球的球磨或喷射研磨,由较大片的磷光体材料制备。它们也可以通过从溶液中生长晶体而制备,并且它们的尺寸可以通过在适当时候终止晶体生长而控制。优选的磷光体材料有效吸收有机EL材料发射的EM辐射,并在另一个光谱区域再发射光。此种有机EL材料和磷光体的结合使得在调节发光器件310发射的光的颜色时,具有灵活性。可以选择特定的磷光体材料或磷光体的混合物,以便发射所需颜色或一定范围的颜色,以补充由有机EL材料和有机PL材料发出的颜色。示例性的磷光体是铈掺杂的钇铝氧化物Y3Al5O12石榴子石(“YAG:Ce”)。其它合适的磷光体基于用多于一种的稀土离子掺杂的YAG,例如(Y1-x-yGdxCey)3Al5O12(“YAG:Gd,Ce”)、(Y1-xCex)3(Al1-yGay)O12(“YAG:Ga,Ce”)、(Y1-x-yGdxCey)(Al5-zGaz)O12(“YAG:Gd,Ga,Ce”)和(Gd1-xCex)Sc2Al3O12(“GSAG”),其中0≤x≤1,0≤y≤1,0≤z≤5和x+y≤1。例如YAG:Gd,Ce磷光体显示在约390nm~约530nm的波长范围(即,蓝-绿光谱区域)吸收光,并且在约490nm~约700nm的波长范围(即,绿-红光谱区域)发射光。相关的磷光体包括Lu3Al5O12和Tb2Al5O12,二者都用铈掺杂。此外,这些铈掺杂的石榴子石磷光体也可以用少量的Pr(例如,约0.1-2mol%)附加掺杂,以提供发红光的进一步增强。下面是被EM辐射有效激发的磷光体的实例,该辐射在300nm~约500nm的波长区域由聚硅烷及其衍生物发射。
发绿光的磷光体:Ca8Mg(SiO4)4Cl2:Eu2+,Mn2+;GdBO3:Ce3+,Tb3+;CeMgAl11O19:Tb3+;Y2SiO5:Ce3+,Tb3+;和BaMg2Al16O27:Eu2+,Mn2+。
发红光的磷光体:Y2O3:Bi3+,Eu3+;Sr2P2O7:Eu2+,Mn2+;SrMgP2O7:Eu2+,Mn2+;(Y,Gd)(V,B)O4:Eu3+;和3.5MgO.0.5MgF2.GeO2:Mn4+(氟代锗酸镁)。
发蓝光的磷光体:BaMg2Al16O27:Eu2+;Sr5(PO4)10Cl2:Eu2+;和(Ba,Ca,Sr)5(PO4)10(Cl,F)2:Eu2+,(Ca,Ba,Sr)(Al,Ga)2S4:Eu2+。
发黄光的磷光体:(Ba,Ca,Sr)5(PO4)10(Cl,F)2:Eu2+,Mn2+。
其它离子也可以引入磷光体中,以将能量从有机材料发出的光转移到磷光体主晶格中的其它活化剂离子,作为增加能量利用的途径。例如,当Sb3+和Mn2+离子存在于相同的磷光体晶格中时,Sb3+有效地吸收在蓝光区的光,该光不被Mn2+很有效吸收,并将能量转移至Mn2+离子。因此,有机EL材料发射的更大总量的光被两种离子吸收,导致整个器件的更高量子效率。
光致发光材料也可以为有机染料,其能够吸收由有机EL材料发射的辐射并在可见光光谱发射电磁辐射。
磷光体颗粒分散在成膜聚合物材料,例如聚丙烯酸酯类、基本透明的聚硅氧烷或环氧树脂中。使用磷光体组合物,其为聚合物材料和磷光体的混合物的小于约30%体积,优选小于约10%体积。可以将溶剂加入到混合物中,以将成膜材料的粘度调节至所需水平。通过在基片上喷涂、浸涂、印刷或流延,将成膜材料和磷光体颗粒的混合物成型为层。之后,将膜从基片上除去,并布置到发光组件320上。膜或层390的厚度优选小于1mm,更优选为小于500微米。优选地,成膜聚合物材料的折射率接近基片40和有机EL材料的折射率,即在约1.4~约1.6的范围。
根据本发明的一方面,散射材料和磷光体的颗粒分散在相同的膜或层390中。在另一实施方式中,散射膜390可以是扩散膜,其为具有粗糙表面的塑料膜。
现在描述制备本发明的OELD的方法。首先提供清洁过的柔韧基片,例如塑料。然后通过上述多种沉积技术的一种,在柔韧的基片的至少一个表面上形成梯度组成的阻挡涂层。
在梯度组成阻挡涂层上沉积第一导电材料,以形成有机EL组件320的第一电极。可选择地,可以在未涂覆有梯度组成的阻挡涂层的基片340的表面上沉积第一电极。第一电极可以是正极或负极,并且在上述用于电极的材料中选择一种或多种适宜材料。优选地,第一电极是包括透明金属氧化物的正极,氧化物例如ITO。第一电极材料优选溅射沉积在基片上。而且,第一电极可以通过例如蚀刻图案化成所需的构造。通过物理或化学气相沉积、旋涂、浸涂、印刷或流延,接着聚合,如果有必要,或者固化该材料,将至少一种有机EL材料沉积在第一电极上。有机EL材料可以稀释在溶剂中以调节其粘度或者与作为成膜载体的其它聚合物材料混合。第二导电材料沉积在至少一种有机EL材料上,以形成第二电极。优选,第二电极是负极。第二电极可以沉积在有机EL材料的整个面积上,或图案化成所需形状或构造。第二电极的厚度保持到最小,例如小于或等于约200nm。电极和有机EL材料包括有机EL组件320。
任选地将反射金属沉积在有机EL组件320与基片340相对的表面上。反射金属可以通过例如溅射或物理气相沉积而沉积。在本发明的一个实施方式中,在反射金属层沉积在有机EL组件320上之前,基本透明材料的粘合层沉积在其上。优选地,粘合层包含电绝缘和基本透明的聚合物材料。粘合层可以通过上述用于沉积有机层的方法之一沉积。形成反射金属层以完全包围有机EL组件320。优选地,反射金属层与梯度组成的阻挡涂层一起形成围绕有机EL组件320的气密密封。此外,其它无机材料的一个或多个附加层可以沉积在反射金属层上。
将散射颗粒或PL材料和透明聚合物材料的混合物沉积在基片340的与有机EL元件相对的表面上。或者,该混合物可以通过带铸法(tape castingmethod),例如刮刀法(doctor blade method)流延成胶带(tape)。然后将该胶带固化并附着到基片340上。
在另一种实施方式中,用于操作本发明的OELD所必需或需要的子集(subsets)层形成在单独的组件中,然后将该组件层压或附着在一起以制备工作器件。例如,具有第一梯度组成的阻挡涂层的第一基片、有机EL元件的装配体和具有第二梯度组成的阻挡涂层的第二基片层压在一起以提供具有改善的耐环境中化学物质侵袭的光源。
在本发明的另一方面,大面积的柔韧的显示器或照明体系引入了本发明的OELD。
虽然前面已经描述了本发明特别优选的实施方式,对本领域普通技术人员应该理解的是,可以对其进行许多改进、替换或变化而不脱离所附权利要求书限定的精神和范围。
Claims (48)
1.一种复合制品,包括柔韧的透明基片(340),该基片具有至少一个基片表面和布置在所述至少一个基片表面上的梯度组成的阻挡涂层(350),所述梯度组成的阻挡涂层(350)包括涂层材料,所述涂层材料包含有机和无机材料,该涂层材料的组成沿所述梯度组成的阻挡涂层(350)的厚度连续地变化。
2.权利要求1的复合制品,其中所述基片(340)包括聚合物材料。
3.权利要求2的复合制品,其中所述聚合物材料选自聚对苯二甲酸乙二醇酯、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂、聚酯、聚酰亚胺、聚醚酰亚胺、聚醚砜、聚乙烯萘、聚降冰片烯、聚环烯烃。
4.权利要求1的复合制品,其中所述无机材料选自下面元素的氧化物、氮化物、碳化物、硼化物或其组合:IIA、IIIA、IVA、VA、VIA、VIIA、IB和IIB族元素;IIIB、IVB和VB族的金属;和稀土金属。
5.权利要求1的复合制品,其中通过选自下面的方法形成所述涂层材料:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积,溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积或其组合。
6.权利要求1的复合制品,其中通过膨胀热等离子体化学气相沉积形成所述涂层材料。
7.权利要求1的复合制品,其中通过射频等离子体增强的化学气相沉积形成所述涂层材料。
8.权利要求1的复合制品,其中氧气通过具有沉积在其上的所述涂层(350)的所述基片的透过率小于0.1cm3/(m2天),在25℃下并且用含有21体积%氧气的气体测量。
9.权利要求1的复合制品,其中水蒸气通过具有沉积在其上的所述涂层(350)的所述基片的透过率小于1g/(m2天),在25℃下并用具有100%相对湿度的气体测量。
10.权利要求1的复合制品,还包括在所述基片(340)和所述涂层(350)之间的扩散区域,所述扩散区域包括所述基片和所述涂层的材料。
11.一种包括柔韧的透明基片(340)的复合制品,该基片具有至少一个基片表面和布置在所述至少一个基片表面上的梯度组成的阻挡涂层(350);所述涂层(350)包括涂层材料,该材料的组成沿所述梯度组成的阻挡涂层的厚度连续变化;所述基片包括聚合物材料;所述涂层材料包括有机材料和无机材料;其中氧气通过具有沉积在其上的所述涂层(350)的所述基片的透过率小于0.1cm3/(m2天),在25℃下并且用含有21体积%氧气的气体测量,水蒸气通过涂覆有所述涂层的所述基片的透过率小于1g/(m2天),在25℃下并用具有100%相对湿度的气体测量,且通过选自下面的方法将所述涂层沉积在所述基片上:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积,溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积或其组合。
12.一种制备复合制品的方法,所述方法包括:
提供具有至少一个基片表面的柔韧的透明基片(340);
在所述基片表面上沉积具有组成的梯度组成的阻挡涂层(350)材料,所述涂层材料包括有机材料和无机材料;和
连续地改变所述涂层材料的所述组成,同时形成所述涂层(350)使得所述组成沿所述梯度组成的阻挡涂层(350)的厚度连续变化。
13.权利要求12的方法,其中所述沉积选自:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积,溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积或其组合。
14.权利要求12的方法,其中所述基片(340)包括聚合物材料,所述聚合物材料选自聚对苯二甲酸乙二醇酯、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂、聚酯、聚酰亚胺、聚醚酰亚胺、聚醚砜、聚乙烯萘、聚降冰片烯、聚环烯烃。
15.权利要求12的方法,其中所述无机材料选自下面元素的氧化物、氮化物、碳化物、硼化物或其组合:IIA、IIIA、IVA、VA、VIA、VIIA、IB和IIB族元素;IIIB、IVB和VB族的金属;和稀土金属。
16.权利要求12的方法,还包括将至少一部分所述涂层材料渗透进入所述基片(340)中,以便在所述基片和所述涂层之间产生扩散区域。
17.权利要求16的方法,其中所述扩散区域的产生是通过高能离子轰击所述基片(340)的表面以溅射所述基片的一部分材料,并沉积包括溅射的基片材料和另一种材料的混合材料。
18.权利要求12的方法,其中通过改变由等离子体产生的反应性物质的组成进行所述涂层(350)的所述组成的改变,该等离子体定向在所述基片上。
19.发光器件(310),包括:
柔韧的透明基片(340),该基片具有第一基片表面和第二基片表面,至少一个所述基片表面涂覆有梯度组成的阻挡涂层(350),该涂层的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料;和
有机电致发光(″EL″)组件(320),其包括有机EL层(330),该有机EL层(330)布置在两电极(322,338)之间,并布置在所述柔韧的透明基片(340)上。
20.权利要求19的发光器件(310),还包括具有布置在其上的第二梯度组成的阻挡涂层的透明的膜(370),所述透明的膜(370)布置在与所述柔韧的透明基片(340)相对的所述有机EL组件(320)上。
21.权利要求19的发光器件(310),其中所述柔韧的透明基片(340)包括选自以下材料的聚合物材料:聚对苯二甲酸乙二醇酯、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂、聚酯、聚酰亚胺、聚醚酰亚胺、聚醚砜、聚乙烯萘、聚降冰片烯、聚环烯烃。
22.权利要求19的发光器件(310),其中所述无机材料选自选自下面元素的氧化物、氮化物、碳化物、硼化物或其组合:IIA、IIIA、IVA、VA、VIA、VIIA、IB和IIB族元素;IIIB、IVB和VB族的金属;和稀土金属。
23.权利要求19的发光器件(310),还包括布置在所述有机EL层上的反射层(360),所述反射层包括选自金属、金属氧化物、金属氮化物、金属碳化物、金属氧氮化物、金属氧碳化物及其组合中的材料。
24.权利要求19的发光器件(310),其中所述有机EL层(330)包括选自聚(N-乙烯基咔唑)、聚(烷基芴)、聚(对亚苯基)、聚硅烷、它们的衍生物、它们的混合物和它们的共聚物中的材料。
25.权利要求的19发光器件(310),其中所述有机EL层(330)包括选自1,3,5-三{N-(4-二苯基氨基苯基)苯基氨基}苯,苯基蒽、四芳基乙烯、香豆素、红荧烯、四苯基丁二烯、蒽、二萘嵌苯、蔻、铝-(皮考基甲基酮)-双{2,6-二(叔丁基)苯氧化物}、钪-(4-甲氧基-皮考基甲基酮)-双(乙酰丙酮化物),铝-乙酰丙酮化物、镓-乙酰丙酮化物和铟-乙酰丙酮化物中的材料。
26.权利要求19的发光器件(310),还包括光-散射层(390),所述层(390)包括分散在透明的基体中的散射颗粒,所述层(390)布置在与所述有机EL组件(320)相对的所述基片(340)的表面上。
27.权利要求26的发光器件(310),还包括光致发光(″PL″)材料的颗粒,该光致发光(″PL″)材料混合有所述光-散射层(390)中的散射颗粒,其中所述PL材料选自(Y1-xCex)3Al5O12、(Y1-x-yGdxCey)3Al5O12、(Y1-xCex)3(Al1-yGay)O12、(Y1-x-yGdxCey)(Al5-zGaz)O12、(Gd1-xCex)Sc2Al3O12、Ca8Mg(SiO4)4Cl2:Eu2+,Mn2+、GdBO3:Ce3+,Tb3+、CeMgAl11O19:Tb3+、Y2SiO5:Ce3+,Tb3+、BaMg2Al16O27:Eu2+,Mn2+、Y2O3:Bi3+,Eu3+、Sr2P2O7:Eu2+,Mn2+、SrMgP2O7:Eu2+,Mn2+、(Y,Gd)(V,B)O4:Eu3+、3.5MgO.0.5MgF2.GeO2:Mn4+(氟代锗酸镁)、BaMg2Al16O27:Eu2+、Sr5(PO4)10Cl2:Eu2+、(Ca,Ba,Sr)(Al,Ga)2S4:Eu2+、(Ba,Ca,Sr)5(PO4)10(Cl,F)2:Eu2+,Mn2+、Lu3Al5O12:Ce3+、Tb3Al5O12:Ce3+、及其混合物,其中0≤x≤1,0≤y≤1,0≤z≤5和x+y≤1。
28.权利要求26的发光器件(310),还包括分散在所述散射层(390)中的至少一种有机PL材料,所述有机PL材料能够吸收所述有机EL材料发射的至少一部分电磁(″EM″)辐射,并能在可见光光谱中发射EM辐射。
29.权利要求19的发光器件(310),其中所述有机EL组件(320)还包括至少一个附加层(324,334,336),该附加层布置在所述电极(322,338)之一和所述有机EL层(330)之间,所述附加层(324,334,336)履行选自以下的至少一种功能:电子注入增强、电子传输增强、空穴注入增强和空穴传输增强。
30.一种发光器件(310),包括:
柔韧的透明基片(340),其具有第一基片表面和第二基片表面,至少一个所述基片表面涂覆有梯度组成的阻挡涂层(350),该涂层的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料;和
有机电致发光(″EL″)组件(320),其包括有机EL层(330),该层布置在两电极(322,338)之间并布置在所述柔韧的透明基片(340)上;
其中所述柔韧的透明基片(340)包括选自聚对苯二甲酸乙二醇酯、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂、聚酯、聚酰亚胺、聚醚酰亚胺、聚醚砜、聚乙烯萘、聚降冰片烯、聚环烯烃中的聚合物材料;和所述有机EL层包括选自聚(N-乙烯基咔唑)、聚(烷基芴)、聚(对亚苯基)、聚硅烷、其衍生物、其混合物、其共聚物、1,2,3-三{N-(4-二苯基氨基苯基)苯基氨基}苯、苯基蒽、四芳基乙烯、香豆素、红荧烯、四苯基丁二烯、蒽、二萘嵌苯、蔻、铝-(皮考基甲基酮)-双{2,6-二(叔丁基)苯氧化物}、钪-(4-甲氧基-皮考基甲基酮)-双(乙酰丙酮化物)、铝-乙酰丙酮化物、镓-乙酰丙酮化物和铟-乙酰丙酮化物中的材料。
31.一种发光器件(310),包括:
柔韧的透明基片(340),其具有第一基片表面和第二基片表面,至少一个所述基片表面涂覆有第一梯度组成的阻挡涂层(350),该涂层的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料;
有机电致发光(″EL″)组件(320),其包括有机EL层(330),该层布置在两电极(322,338)之间并布置在所述柔韧的透明基片(340)上;
反射层(360),其布置在与所述基片相对的所述有机EL组件(320)上;和
具有第二梯度组成的阻挡涂层(372)的透明的膜(370),该膜布置在与所述有机EL组件(320)相对的所述反射层(360)上;
其中所述柔韧的透明基片(340)和所述透明的膜(370)包含选自聚对苯二甲酸乙二醇酯、聚丙烯酸酯、聚碳酸酯、聚硅氧烷、环氧树脂、聚硅氧烷官能化的环氧树脂、聚酯、聚酰亚胺、聚醚酰亚胺、聚醚砜、聚乙烯萘、聚降冰片烯、聚环烯烃中的聚合物材料;所述第二梯度组成的阻挡涂层材料包括选自有机材料和无机材料及其组合中的材料;和所述有机EL层包括选自聚(N-乙烯基咔唑)、聚(烷基芴)、聚(对亚苯基)、聚硅烷、其衍生物、其混合物、其共聚物、1,2,3-三{N-(4-二苯基氨基苯基)苯基氨基}苯、苯基蒽、四芳基乙烯、香豆素、红荧烯、四苯基丁二烯、蒽、二萘嵌苯、蔻、铝-(皮考基甲基酮)-双{2,6-二(叔丁基)苯氧化物}、钪-(4-甲氧基-皮考基甲基酮)-双(乙酰丙酮化物)、铝-乙酰丙酮化物、镓-乙酰丙酮化物和铟-乙酰丙酮化物中的材料。
32.权利要求31的发光器件(310),还包括散射层(390),其布置在与所述有机EL组件(320)相对的所述透明的基片上,所述散射层(390)包括散射颗粒和分散在透明的基体中的PL材料的颗粒。
33.一种器件装配体(310),包括布置在柔韧的透明基片(340)上的器件(320),所述基片具有第一基片表面和第二基片表面,至少一个所述基片表面涂覆有梯度组成的阻挡涂层(350),该涂层的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料。
34.权利要求33的器件装配体(310),其中所述器件(320)选自液晶显示器、光电电池、集成电路和医用诊断系统的部件。
35.一种制造发光器件的方法,所述方法包括:
提供柔韧的透明基片(340),其具有第一基片表面和第二基片表面,至少一个所述基片表面涂覆有第一梯度组成的阻挡涂层(350),该涂层的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料;和
沉积有机EL组件(320),该组件包括有机EL层(330),该层布置在所述柔韧的透明的基片上的两电极(322,338)之间。
36.权利要求35的制造发光器件(310)的方法,其中所述沉积所述有机EL组件(320)包括通过在所述梯度组成的阻挡涂层(340)上沉积第一导电材料而形成第一电极(338);在所述第一电极上沉积所述有机EL层(330);和通过在所述有机EL层(330)上沉积第二导电材料而形成第二电极(322)。
37.权利要求35的制造发光器件(310)的方法,进一步包括在与所述透明的基片(340)相对的所述有机EL组件(320)上布置反射层(360)。
38.权利要求37的制造发光器件(310)的方法,进一步包括在所述反射层42上布置透明的膜(370),该膜涂覆有第二梯度组成的阻挡涂层(372)。
39.权利要求35的制造发光器件(310)的方法,进一步包括在所述基片(340)的表面上布置散射层(390),所述散射层包括分散在透明的基体中的PL材料颗粒。
40.权利要求35的制造发光器件(310)的方法,进一步包括在与所述透明的基片(340)相对的所述有机EL组件(320)上布置第二梯度的阻挡涂层(372)。
41.权利要求35的制造发光器件(310)的方法,进一步包括在所述有机EL组件(320)上布置第二柔韧的基片(370),所述第二基片上具有第二梯度组成的阻挡涂层(372)。
42.一种制造发光器件(310)的方法,所述方法包括:
提供柔韧的透明基片(340),该基片具有第一基片表面和第二基片表面;
在至少一个所述基片表面上沉积第一梯度组成的阻挡涂层(350),所述阻挡涂层包括有机材料和无机材料,该第一阻挡涂层(350)的组成沿其厚度连续改变,所述沉积通过选自以下的方法进行:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积,溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积;
在所述柔韧的透明基片(340)上布置有机EL组件(320),该组件包括布置在两电极(322,338)之间的有机EL层(330);和
在所述有机EL组件(320)上布置透明的膜(370),该膜涂覆有第二梯度组成的阻挡涂层(372),所述第二梯度组成的阻挡涂层的组成沿其厚度连续变化,并且所述第二梯度组成的阻挡涂层通过选自下面的方法沉积到所述膜(370)上:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积,溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积或其组合。
43.权利要求42的制造发光器件(310)的方法,进一步包括在所述有机EL组件(320)和所述涂覆的透明的膜(370)之间布置反射层(360)。
44.权利要求42的制造发光器件(310)的方法,其中进行在至少一个所述基片表面上沉积第一梯度组成的阻挡涂层(350),以使至少一部分所述涂层的材料渗透进入所述基片(340)中。
45.一种制造包含器件(310)的装配体的方法,所述方法包括:
提供柔韧的透明基片(340),其具有第一基片表面和第二基片表面,至少一个所述基片表面涂覆有第一梯度组成的阻挡涂层(350),该涂层的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料;和
在所述柔韧的透明基片(340)上布置所述器件。
46.权利要求45的方法,其中所述器件(310)选自液晶显示器、光电电池、集成电路和医用诊断系统的部件。
47.一种制造器件(320)的方法,所述方法包括:
提供柔韧的透明基片(340),其具有第一基片表面和第二基片表面;
在至少一个所述基片表面上沉积第一梯度组成的阻挡涂层(350),所述第一阻挡涂层(350)的组成沿其厚度连续变化,所述阻挡涂层包括有机材料和无机材料,所述沉积通过选自下面的方法进行:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积、溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积;
在柔韧的透明基片(340)上布置器件(320);和
在所述器件(320)上布置透明的膜(370),该膜涂覆有第二梯度组成的阻挡涂层(372),所述第二梯度组成的阻挡涂层的组成沿其厚度连续变化,并且所述第二梯度组成的阻挡涂层通过选自下面的方法沉积到所述膜(370)上:等离子体增强的化学气相沉积、射频等离子体增强的化学气相沉积、膨胀热等离子体化学气相沉积,溅射、反应溅射、电子回旋加速器共振等离子体增强的化学气相沉积、电感耦合等离子体增强的化学气相沉积和其组合。
48.权利要求47的方法,其中所述器件(320)选自液晶显示器、光电电池、集成电路和医用诊断系统的部件。
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Cited By (2)
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CN107587120A (zh) * | 2017-08-23 | 2018-01-16 | 无锡荣坚五金工具有限公司 | 一种具有调制结构的高绝缘纳米防护涂层的制备方法 |
CN107587120B (zh) * | 2017-08-23 | 2018-12-18 | 江苏菲沃泰纳米科技有限公司 | 一种具有调制结构的高绝缘纳米防护涂层的制备方法 |
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