CN1791989A - 通过原子层沉积形成的塑料基材阻挡层膜 - Google Patents

通过原子层沉积形成的塑料基材阻挡层膜 Download PDF

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CN1791989A
CN1791989A CNA2004800134392A CN200480013439A CN1791989A CN 1791989 A CN1791989 A CN 1791989A CN A2004800134392 A CNA2004800134392 A CN A2004800134392A CN 200480013439 A CN200480013439 A CN 200480013439A CN 1791989 A CN1791989 A CN 1791989A
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P·F·卡西亚
R·S·麦克莱恩
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Abstract

气体渗透阻挡层可通过原子层沉积法(ALD)沉积在塑料或玻璃基材上。ALD涂层的使用可在低浓度的涂层缺陷下，以数十纳米厚度降低许多量级的渗透率。这些薄涂层保护了塑料基材的柔韧性和透明性。这种制品可用于容器、电力和电子应用。

Description

通过原子层沉积形成的塑料基材阻挡层膜
发明领域
本发明涉及包含塑料或玻璃基材以及通过原子层沉积形成的环境气体渗透阻挡层的制品。该制品可以是诸如有机发光二极管的电力或电子器件的部件。该制品也可用于气体渗透很重要的应用中的容器。
背景技本
Featherby和Dehaven(WO 2001067504)公开了一种密封涂层器件。这种器件的形成包括提供集成半导体电路型板、施加包封该电路型板的含有无机材料的第一层，以及施加包封该电路型板的第二层步骤。
Aintila(WO 9715070A2)公开了在基材表面的金属接触盘区域上形成接触***块，包括用原子层外延生长在基材上形成氧化物层，该层在后续加工步骤中要求的点处有开口。
Aftergut和Ackerman(US 5641984)公开了包含水分阻挡层的密封辐照成像器。在原子层外延生长技术中沉积了介电材料层作为该密封结构的一部分。
Aftergut和Ackerman(US 5707880)公开了包含水分阻挡层的密封辐照成像器，该阻挡层包含通过原子层外延生长沉积的介电材料层。
以上文献都没有公开包含聚合物或玻璃基材的渗透阻挡层。
发明概述
本发明描述了一种制品，该制品包含：
a)由选自塑料和玻璃的材料制成的基材，和
b)通过原子层沉积法沉积在所述基材上的膜。
本发明还是一种制品，该制品包含：
a)由选自塑料和玻璃的材料制成的基材；
b)涂覆的粘合层；和
c)通过原子层沉积法沉积的气体渗透阻挡层。
本发明的另一种实施方案是一种制品，该制品包含：
a)由选自塑料和玻璃的材料制成的基材；
b)有机半导体，和
c)通过原子层沉积法沉积的气体渗透阻挡层。
本发明的又一种实施方案是一种制品，该制品包含：
a)选自塑料和玻璃的材料制成的基材；
b)液晶聚合物，和
c)通过原子层沉积法沉积的气体渗透阻挡层。
本发明还描述了作为封闭容器的实施方案。
本发明的另一个实施方案是电力或电子器件。
本发明的又一个实施方案是发光聚合物器件。
本发明的又一个实施方案是液晶聚合物器件。
本发明还描述了有机发光二极管。
本发明的另一个实施方案是晶体管。
本发明又一个实施方案是包含发光聚合物器件的电路。
又一种器件是有机光电池。
本发明提出的第二种器件包含许多层，每层都包含一个上述制品，其中这些制品互相接触。在这样的一种实施方案中，这种上述制品的第二种制品通过层叠手段相互接触。
附图简述
图1表示具有阻挡层基材和阻挡层外涂层的发光聚合物器件。
图2表示具有阻挡层基材和阻挡层封口层的发光聚合物器件。
图3表示具有阻挡层基材和阻挡层封口层的有机晶体管。
图4表示具有阻挡层基材和阻挡层封口层的有机晶体管。
图5表示通过涂有25nm的Al2O3阻挡层膜的0.002英寸厚聚萘二甲酸乙二醇酯(PEN)测量的光透射。
详细描述
O2和H2O蒸汽很容易透过聚合物膜。为了降低封装应用中的渗透率，往往在聚合物上涂覆薄层无机膜。常用铝涂层聚酯。通过物理气相沉积(PVD)或化学气相沉积(CVD)形成的光学透明阻挡层，主要是SiOx或AlOy，也可用于封装。后一种膜可商购，在工业上称为“玻璃涂层”阻挡层膜。它们使环境气体渗透改善了约10倍，使通过聚酯膜的透过率降低到约1.0cc O2/m2/天和1.0ml H2O/m2/天(M.Izu，B.Dotter，和S.R.Ovshinsky，J.Photopolymer Science and Technology，Vol.8，1995，pp195-204)。尽管这种适度改进是许多大体积封装应用中性能与造价之间合理的折中，但该性能远远不能满足电子领域的封装要求。电子封装通常要求其期望寿命比例如饮料封装要长至少一个数量级。作为实例，在柔性聚酯基材上构建的基于有机发光聚合物(OLED)的柔性显示器对于隔离环境气体所需要的阻挡层改善估计要达到105-106倍，因为气体既会使发光聚合物，也会使通常为Ca或Ba的水敏感性金属阴极严重降解。
由于聚合物的固有自由体积分数，其内在渗透率通常高104-106倍，不能实现诸如柔性OLED显示器的电子应用中所需的保护水平。只有基本上为零渗透率的无机材料才能提供适当的阻挡层保护。理论上，无缺陷的连续薄膜无机涂层对环境气体应该是不渗透的。然而，实际情况是不管从涂覆方法，还是从损害阻挡层性能的基材缺陷看，薄膜都存在诸如针孔的缺陷。甚至膜中的颗粒边界都会存在容易渗透的路径。为了实现最好的阻挡层性能，膜应该在洁净环境中沉积在清洁、无缺陷的基材上。膜的结构应该是非结晶的。沉积方法应该是非定向的(即CVD优于PVD)，且实现没有特征的微结构的生长机理理想的是一层接一层的，以避免具有粒状微观结构的柱状生长。
原子层沉积(ALD)是一种满足低渗透的许多准则的膜生长方法。原子层沉积方法的描述可在“Atomic Layer Epitaxy”，Tuomo Suntola，Thin Solid Films，Vol.216(1992)，pp.84-89中找到。正如其名称所暗示的，通过ALD的膜生长通过一层接一层的方法形成。通常情况下，膜前体蒸汽在真空室中被吸收在基材上。然后从真空室抽出该蒸汽，在基材上留下通常主要是单层的被吸收前体的薄层。然后在加热条件下将反应剂引入真空室中，以促进与所吸收前体的反应，形成期望的材料层。从真空室中抽出反应产物。通过再次将基材暴露在前体蒸汽下，并重复该沉积方法，可形成后续的材料层。ALD在生长方面与常规CVD和PVD方法相反的是，CVD和PVD的生长是在基材表面上有限数量的成核位置处开始和进行。后一种技术会导致形成其中圆柱体之间具有边界的圆柱形微结构，气体很容易沿这些边界渗透。ALD能制备非常薄的膜，这种膜具有极其低的透气率，使得这种膜作为阻挡层用于封装布置在塑料基材上的敏感性电子器件和元件极具吸引力。
本发明描述了通过ALD在塑料基材上形成的阻挡层，该阻挡层可用于避免环境气体穿越。本发明的基材包括常用类型的聚合物材料，例如Christopher Hall的Polymer Materials，(Wiley，纽约，1989)或J.Comyn的Polymer Permeability，(Elsevier，伦敦，1985)中所描述的聚合物，但并不限于这些。常用实例包括聚对苯二甲酸乙二醇酯(PET)和聚萘二甲酸乙二醇酯(PEN)，它们可以成卷购买用作膜基。通过ALD形成的适合用作阻挡层的材料包括元素周期表中IVB、VB、VIB、IIIA和IVA族的氧化物和氮化物以及它们的结合。其中特别感兴趣的是SiO2、Al2O3和Si3N4。这些族元素的氧化物的一个优点是其透光性，这一点对于可见光必须离开或进入器件的电子显示器和光电池特别有吸引力。Si和Al的氮化物在可见光谱范围也是透明的。
在ALD方法中用于形成这些阻挡层材料的前体可选自本领域普通技术人员公知的，在诸如M.Leskela和M.Ritala的“ALD precursorchemistry：Evolution and future challenges”，Journal de Physique IV，Vol.9，pp837-852(1999)以及该文引用的参考文献的公开出版物中列举的前体。
通过ALD合成这些阻挡层涂层的基材温度范围优选50-250℃。温度太高(＞250℃)就与温度敏感性塑料基材的加工不相容，这或者是因为塑料基材的化学降解，或者是由于基材较大的尺寸变化会损坏ALD涂层。
阻挡层膜的优选厚度范围是2-100nm。更优选2-50nm。层厚越薄，就越能承受弯曲而不导致膜撕裂。这一点对于视柔韧性为理想性能的聚合物基材极其重要。膜的撕裂会损害阻挡层的性能。薄的阻挡层膜在光的输入或输出很重要的电子器件的情况下还能提高透明度。存在一个与连续膜覆盖对应的最小厚度，此时基材的所有缺陷都被阻挡层膜覆盖。对于几乎无缺陷的基材，对于良好阻挡层性能的临界厚度估计至少为2nm，但可达10nm厚。
通过ALD涂覆的某些氧化物和氮化物阻挡层可要求一个“起始层”或“粘合层”，以促进与塑料基材或需要保护的制品间的粘合。粘合层的优选厚度为1-100nm。粘合层材料的选择可来自与阻挡层材料相同的族。氧化铝和氧化硅是优选的粘合层，它们也可通过ALD沉积，但诸如化学和物理气相沉积或本领域公知的其它沉积方法也是合适的。
阻挡层结构的基本结构单元是：(A)通过ALD涂覆在塑料或玻璃基材上的带有或不带有粘合层的单个阻挡层，或(B)通过ALD涂覆在塑料基材每一面上的带有或不带有粘合层的阻挡层。然后可按任何数量将这种基本结构组合，方法是通过将这种结构单元与其本身层叠，形成多个独立的阻挡层。阻挡层涂层领域公知的是，物理上分开的多个层对总体阻挡层性能的改善程度远远大于与层数对应的简单的倍增因子倍数。这一点在例如Y.G.Tropsha和N.G.Harvey的J.Phys.Chem.B 1997，Vol.101，pp2259-2266，“Activated rate theory treatmentof oxygen and water transport through silicon oxide/poly(ethyleneterephthalate)composite barrier structures(通过氧化硅/聚对苯二甲酸乙二醇酯复合阻挡层结构输送氧和水的活化率理论处理)”中有说明。这是由于气体分子的扩散路径通过分开的多个阻挡层迂回。有效的扩散路径远大于单个层厚度之和。
另一种阻挡层结构涉及直接涂覆需要保护的电子或电光学器件。在这方面ALD特别有吸引力，因为它形成了高度保形的涂层。从而使具有复杂形状的器件能完全涂覆和保护。
实施例
实施例1
图1表示发光聚合物器件的示意图。为简化起见，将该发光聚合物器件表示成夹在两个电极之间的发光聚合物(LEP)。在实践中，可将空穴传导和/或电子传导层***合适电极与LEP层之间，以提高器件效率。阳极是铟-锡氧化物层，而阴极是Ca/Al层复合材料。通过在电极间施加电压，注入阳极的空穴与注入阴极的电子结合形成放射性衰变的激发子，从LEP发射光。LEP通常是诸如聚苯乙烯(PPV)或其衍生物的光敏聚合物。阳极往往是Ba或Ca，它们对环境气体，特别是水蒸汽具有相当的活性。由于这些敏感材料的使用，器件封装就必须排斥环境气体，以便实现合理的器件寿命。在图1中，封装由阻挡层-基材和外涂阻挡层膜构成，基材可以是沉积了LEP器件的塑料或玻璃。基材由0.004英寸厚的聚萘二甲酸乙二醇酯(PEN)的聚酯膜组成。PEN膜的每一面上都涂有50nm厚的Al2O3膜，该膜通过原子层沉积法沉积，用三甲基铝作为铝的前体和臭氧(O3)作为氧化剂。沉积期间的基材温度为150℃。在ALD方法中，将PEN基材置于装有机械泵的真空室中。抽空真空室。将三甲基铝前体注入500毫托压力的室中约2秒。然后用氩气清洗真空室约2秒。然后将氧化剂臭氧注入500毫托压力的室中约2秒。最后用氩气清洗氧化剂约2秒。重复该沉积方法50次，获得约100nm厚的涂层。Al2O3层对可见光光学透明。该涂覆基材可弯曲而不损坏涂层。其中一个Al2O3阻挡层通过射频磁控管溅射由10％(重量)锡搀杂的铟氧化物钯涂覆铟-锡氧化物透明导体。该ITO膜的厚度为150nm。将LEP旋涂在ITO电极上，然后分别由Ca和Al金属源热蒸镀带有约1μm Al的5nm Ca的阳极。然后再用三甲基铝作铝的前体和臭氧(O3)作氧化剂，通过原子层沉积法在该LEP器件上涂覆50nm厚的Al2O3外阻挡层膜。所得结构现在不透过环境气体。
实施例2
另一种式样的封装示意图如图2。外涂阻挡层被没有上述实施例1中所述ITO电极的相同基材阻挡层结构(Al2O3/PEN/Al2O3)代替。该覆盖阻挡层结构用一层环氧树脂密封基材阻挡层。
实施例3
图3说明一种带有ALD阻挡层涂层的有机晶体管的保护对策。所示晶体管是用有机半导体作为最终层或外层的底栅结构。因为大部分有机半导体是对空气敏感的，长时间暴露在空气中会破坏它们的性能，因此需要保护对策。图3中的封装包括阻挡层-基材，在该阻挡层-基材上沉积晶体管，然后密封成相同的封盖阻挡层结构。该基材由0.004英寸厚的聚萘二甲酸乙二醇酯(PEN)聚酯膜组成。PEN膜的每一面上都涂有50nm厚的Al2O3膜，该膜通过原子层沉积方法，用三甲基铝作为铝的前体，用臭氧(O3)作为氧化剂沉积形成。沉积期间的基材温度为150℃。在ALD方法中，将PEN基材置于装有机械泵的真空室中。将真空室抽空。将三甲基铝前体注入500毫托压力真空室约2秒。然后用氩气清洗真空室约2秒。然后将氧化剂臭氧注入500毫托压力真空室约2秒。最后用氩气清洗氧化剂约2秒。重复该沉积方法约50次，获得约100nm厚的涂层。将100nm厚的Pd金属栅电极通过遮光板用离子束溅射到Al2O3阻挡层膜上。然后通过等离子增强的化学气相沉积方法沉积250nm Si3N4的栅电介质，同样通过遮光板使其与金属栅接触。随后制成100nm厚Pd源和漏电极的布线图，离子束溅射到栅电介质上。最后通过允许与源-漏电极接触的遮光板热蒸发外层有机半导体，例如并五苯。整个晶体管用Al2O3/PEN/Al2O3阻挡层结构覆盖，用环氧密封胶封装到基材阻挡层上。
实施例4
在图4中，实施例3的封装阻挡层可用三甲基铝作铝的前体、臭氧(O3)作氧化剂的原子层沉积方法沉积形成的单层50nm厚Al2O3代替。有机晶体管器件的两种封装结构对环境气体都不渗透。带有阻挡层涂层的塑料基材也可用不渗透的玻璃基材代替。阻挡层封装层由通过等离子增强的化学气相沉积方法在室温下沉积的氮化硅的起始粘合剂层，和实施例3中所述通过原子层沉积法沉积的50nm厚Al2O3阻挡层构成。
实施例5
通过原子层沉积法在120℃下涂覆0.002英寸厚的聚对苯二甲酸乙二醇酯(PEN)基材膜，在该PEN基材的一面上涂有约25nm厚的Al2O3。在评价其透气性性能前，将该带涂层PEN基材至少一次弯曲到至少1.5英寸半径，从刚性硅载体晶片上除去涂覆Al2O3-涂覆PEN基材，该基材在ALD沉积期间用Kapton胶带粘附在晶片上。用商用仪器(MOCON Ox-Tran 2/20)测量50％相对湿度下通过带有ALD法沉积的Al2O3的膜的氧输送率。测量80小时厚，在测量灵敏度(0.005cc-O2/m2/天)范围内，尽管严重地预先弯曲，都没有检测到有氧输送通过阻挡层膜(＜0.005cc/m2/天)。为了比较，我们测量出氧通过未涂覆的PEN基材的输送为约10cc-O2/m2/天。图5表示该涂有Al2O3的PEN阻挡层和未涂覆的PEN的光透射相同(400nm以上的透射率＞80％)，证明了薄Al2O3阻挡层涂层的透明性。

Claims (16)

1.一种制品，包含：
a)由选自塑料和玻璃的材料制成的基材，和
b)在所述基材上通过原子层沉积法沉积的气体渗透阻挡层。
2.一种制品，包含：
a)由选自塑料和玻璃的材料制成的基材，
b)涂覆的粘合层，和
c)在所述基材上通过原子层沉积法沉积的气体渗透阻挡层。
3.一种制品，包含：
a)由选自塑料和玻璃的材料制成的基材，
b)有机半导体，和
c)通过原子层沉积法沉积的气体渗透阻挡层。
4.一种制品，包含：
a)由选自塑料和玻璃的材料制成的基材，
b)液晶聚合物，和
c)通过原子层沉积法沉积的气体渗透阻挡层。
5.权利要求1、2、3或4中任何一项的制品，其中该制品是封闭容器。
6.权利要求1、2、3或4中任何一项的制品，其中该制品是电力或电子器件。
7.权利要求1、2、3或4中任何一项的制品，其中该制品是发光聚合物器件。
8.权利要求1、2、3或4中任何一项的制品，其中该制品是有机发光二极管。
9.权利要求1、2、3或4中任何一项的制品，其中该制品是晶体管。
10.权利要求1、2、3或4中任何一项的制品，其中该制品是包含发光聚合物器件的电路。
11.权利要求1、2、3或4中任何一项的制品，其中该制品是包含晶体管的电路。
12.权利要求1、2、3或4中任何一项的制品，其中该制品是有机光电池。
13.权利要求1、2、3或4中任何一项的制品，其中通过原子层沉积法沉积的气体渗透阻挡层沉积在聚合物的表面侧和底面侧。
14.包含许多层的第二种制品，每层包含一个权利要求1、2、3或4任何一项中描述的制品，其中制品相互接触。
15.权利要求11的第二种制品，其中权利要求1、2、3或4任何一项的制品通过层叠手段相互接触。
16.权利要求1、2、3或4中任何一项的制品，其中该制品是液晶显示器。
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