CN117062481A - 用作柔性显示器件的水汽阻隔膜 - Google Patents

用作柔性显示器件的水汽阻隔膜 Download PDF

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CN117062481A
CN117062481A CN202311039451.1A CN202311039451A CN117062481A CN 117062481 A CN117062481 A CN 117062481A CN 202311039451 A CN202311039451 A CN 202311039451A CN 117062481 A CN117062481 A CN 117062481A
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layer
water vapor
magnetron sputtering
vapor barrier
barrier film
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金闯
张礼勋
蒋晓明
孙交锴
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Taicang Sidike New Material Science and Technology Co Ltd
Jiangsu Sidike New Materials Science and Technology Co Ltd
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Taicang Sidike New Material Science and Technology Co Ltd
Jiangsu Sidike New Materials Science and Technology Co Ltd
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Abstract

本发明公开了一种用作柔性显示器件的水汽阻隔膜，包括基底层和位于基底层外侧的水汽阻隔层，水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式中的任意一种被布置：(S‑D)m‑S‑P顺序、(D‑S)m‑D‑P顺序、(S‑D)m‑P顺序或(D‑S)m‑P顺序，其中m是交替的S和D的数量。本发明将磁控溅射工艺和ALD(原子层沉积)工艺相结合，利用ALD工艺具有良好的缺陷覆盖率的特点，可以覆盖磁控溅射溅射层的缺陷，能够实现10–5g/m2·day级别水汽阻隔膜制备。

Description

用作柔性显示器件的水汽阻隔膜
技术领域
本发明涉及阻隔膜材料领域，特别涉及一种用作柔性显示器件的水汽阻隔膜。
背景技术
柔性有机电子技术，如OLED(有机发光二极管)、OPV(有机光伏)、OTFT(有机薄膜晶体管)等，将在显示器以及照明、可穿戴等应用中引发巨大的变化。特别的是，柔性OLED显示器正在成为显示行业中的常见的显示器之一，而柔性基板作为OLED电子器件中的关键部件，需要匹配高水汽阻隔性能的水汽阻隔膜(水汽透过率10–5g/m2·day级别)。实现高阻隔水汽性能最常见的方法主要是PECVD(等离子体化学气相沉积)等工艺，但PECVD沉积速率慢。而磁控溅射法作为是一种沉积速率很高的替代方法，但通过磁控溅射制造的薄膜存在晶点、针孔等形貌缺陷，形貌上的缺陷导致其不能达到10–5g/m2·day级别的水汽透过率。
发明内容
本发明所要解决的技术问题在于针对上述现有技术中的不足，提供一种用作柔性显示器件的水汽阻隔膜。
为解决上述技术问题，本发明采用的技术方案是：一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于所述基底层外侧的水汽阻隔层，所述水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，所述水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式中的任意一种被布置：(S-D)m-S-P顺序、(D-S)m-D-P顺序、(S-D)m-P顺序或(D-S)m-P顺序，其中m是交替的S和D的数量。
优选的是，所述磁控溅射层采用卷对卷磁控溅射工艺沉积得到。
优选的是，所述磁控溅射层的材料为二氧化硅(SiO2)、三氧化二铝(Al2O3)、一氧化硅(SiO)、氮化硅(Si3N4)、氮氧化硅(SiOxNy)、氮化钛(TiN)中的一种或多种的组合。
优选的是，所述原子沉积层采用卷对卷原子层沉积工艺沉积得到。
优选的是，所述原子沉积层的材料为二氧化硅(SiO2)、三氧化二铝(Al2O3)、一氧化硅(SiO)、氮化硅(Si3N4)、氮氧化硅(SiOxNy)、氮化钛(TiN)中的一种或多种的组合。
优选的是，所述磁控溅射层的材料为氮化硅，所述原子沉积层的材料为三氧化二铝。
优选的是，制备所述磁控溅射层的卷对卷磁控溅射工艺条件为：使用纯硅靶材，功率为6000W，气体流量位70sccm的氮气和80sccm的氩气；
所述磁控溅射层的厚度为50nm。
优选的是，制备所述原子沉积层的卷对卷原子层沉积工艺条件为：气源前驱体为三甲基铝和臭氧，卷绕镀膜鼓温度为100℃；
所述原子沉积层的厚度为45nm。
优选的是，所述水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式中的任意一种被布置：D-S-P顺序、S-D-S-P顺序、D-S-D-S-P顺序或D-S-D-S-D-S--P顺序。
优选的是，所述基底层为以下材料中的一种或多种形成的卷材：聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸乙二醇酯(PET)、三醋酸纤维素(TAC)、环烯烃共聚物(COP)、环烯烃聚合物(COC)、聚碳酸酯(PC)、聚醚醚酮(PEEK)。更优选为聚醚醚酮(PEEK)卷材。
本发明的有益效果是：
本发明提供的用作柔性显示器件的水汽阻隔膜是通过磁控溅射工艺和ALD(原子层沉积)工艺相结合制备得到，利用ALD工艺具有良好的缺陷覆盖率的特点，可以覆盖磁控溅射溅射层的缺陷；以磁控溅射层为主，ALD技术为辅助进行缺陷调整，能够实现10–5g/m2·day级别水汽阻隔膜制备。
附图说明
图1为本发明的实施例1中的用作柔性显示器件的水汽阻隔膜的结构示意图；
图2为本发明的实施例2中的用作柔性显示器件的水汽阻隔膜的结构示意图；
图3为本发明的实施例3中的用作柔性显示器件的水汽阻隔膜的结构示意图；
图4为本发明的实施例4中的用作柔性显示器件的水汽阻隔膜的结构示意图；
图5为本发明的对比例1中的用作柔性显示器件的水汽阻隔膜的结构示意图；
图6为本发明的对比例2中的用作柔性显示器件的水汽阻隔膜的结构示意图。
具体实施方式
下面结合实施例对本发明做进一步的详细说明，以令本领域技术人员参照说明书文字能够据以实施。
应当理解，本文所使用的诸如“具有”、“包含”以及“包括”术语并不排除一个或多个其它元件或其组合的存在或添加。
下列实施例中所使用的试验方法如无特殊说明，均为常规方法。下列实施例中所用的材料试剂等，如无特殊说明，均可从商业途径得到。下列实施例中未注明具体条件者，按照常规条件或者制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。
实施例1
参照图1，一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于基底层外侧的水汽阻隔层，水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式被布置：D-S-P顺序；即(D-S)m-P顺序，m＝1。
其中，磁控溅射层(S)材料为氮化硅(Si3N4)，使用纯硅靶材，在恒定功率为6000W下，通过气体流量控制器注入70sccm的氮气与80sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Si3N4，厚度为50nm。
其中，原子层沉积层(D)为三氧化二铝(Al2O3)，反应气源前驱体为三甲基铝(TMA)和臭氧，卷绕镀膜鼓温度为100℃，通过调控气场、等离子体强度、走速等参数控制三甲基铝与臭氧反应，即可在表面形成原子层沉积层Al2O3，厚度为45nm。
实施例2
参照图2，一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于基底层外侧的水汽阻隔层，水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式被布置：S-D-S-P顺序；即(S-D)m-S-P顺序，m＝1。
其中，基底层为50微米的聚醚醚酮卷材薄膜(PEEK)。
其中，磁控溅射层(S)材料为氮化硅(Si3N4)，使用纯硅靶材，在恒定功率为6000W下，通过气体流量控制器注入70sccm的氮气与80sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Si3N4，2个氮化硅层的厚度均为50nm。
其中，原子层沉积层(D)为三氧化二铝(Al2O3)，反应气源前驱体为三甲基铝(TMA)和臭氧，卷绕镀膜鼓温度为100℃，通过调控气场、等离子体强度、走速等参数控制三甲基铝与臭氧反应，即可在表面形成原子层沉积层Al2O3，厚度为45nm。
实施例3
参照图3，一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于基底层外侧的水汽阻隔层，水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式被布置：D-S-D-S-P顺序；即(D-S)m-P顺序，m＝2。
其中，基底层为50微米的聚醚醚酮卷材薄膜(PEEK)。
其中，磁控溅射层(S)材料为氮化硅(Si3N4)，使用纯硅靶材，在恒定功率为6000W下，通过气体流量控制器注入70sccm的氮气与80sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Si3N4，2个磁控溅射层Si3N4的厚度均为50nm。
其中，原子层沉积层(D)为三氧化二铝(Al2O3)，反应气源前驱体为三甲基铝(TMA)和臭氧，卷绕镀膜鼓温度为100℃，通过调控气场、等离子体强度、走速等参数控制三甲基铝与臭氧反应，即可在表面形成原子层沉积层Al2O3，2个原子层沉积层Al2O3厚度均为45nm。
实施例4
参照图4，一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于基底层外侧的水汽阻隔层，水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式被布置：D-S-D-S-D-S--P顺序；即(D-S)m-P顺序，m＝3。
其中，基底层为50微米的聚醚醚酮卷材薄膜(PEEK)。
其中，磁控溅射层(S)材料为氮化硅(Si3N4)，使用纯硅靶材，在恒定功率为6000W下，通过气体流量控制器注入70sccm的氮气与80sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Si3N4，3个磁控溅射层Si3N4的厚度均为50nm。
其中，原子层沉积层(D)为三氧化二铝(Al2O3)，反应气源前驱体为三甲基铝(TMA)和臭氧，卷绕镀膜鼓温度为100℃，通过调控气场、等离子体强度、走速等参数控制三甲基铝与臭氧反应，即可在表面形成原子层沉积层Al2O3，3个原子层沉积层Al2O3厚度均为45nm。
对比例1
参照图5，一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于基底层外侧的水汽阻隔层，水汽阻隔层为磁控溅射层Si3N4。
其中，基底层为50微米的聚醚醚酮卷材薄膜(PEEK)。
其中，磁控溅射层Si3N4工艺条件为：使用纯硅靶材，在恒定功率为10000W，通过气体流量控制器注入100sccm的氮气与120sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Si3N4，厚度为100nm。
对比例2
参照图6，一种用作柔性显示器件的水汽阻隔膜，包括：基底层和位于基底层外侧的水汽阻隔层，基底层为50微米的聚醚醚酮卷材薄膜(PEEK)。
水汽阻隔层包括从基底层侧依次向外设置的磁控溅射层Si3N4和磁控溅射层Al2O3。磁控溅射层Si3N4工艺条件为：使用纯硅靶材，在恒定功率为10000W，通过气体流量控制器注入100sccm的氮气与120sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Si3N4，厚度为100nm。磁控溅射层Al2O3工艺条件为：使用纯铝靶材，在恒定功率为20000W下，通过气体流量控制器注入120sccm的氧气与150sccm的氩气进入卷对卷溅射系统，在表面形成磁控溅射层Al2O3，厚度为50nm。
以下对实施例1-4和对比例1-2制备的水汽阻隔膜进行水汽透过率测试：
水汽透过率(以下简称：WVTR)测试采用MOCON Permatran-W 3/34G，连续模式测试，测试面积0.005平方米，温度38℃，湿度90％(相对100％湿度)，WVTR值越小，该样品的水汽阻隔性能越高。
测试结果如下表1所示：
表1
将对比例1和对比例2对比可以发现，磁控溅射的氧化铝不能有效改善氮化硅表面的缺陷，提升水汽阻隔率；
实施例1和对比例2对比可以发现：ALD沉积的的氧化铝相对于磁控溅射的氧化铝而言，ALD沉积的氧化铝可以起到改善氮化硅表面形貌，从而有效提升水汽阻隔率的作用；
实施例3和实施例4作为本发明的较优实施例，分别已经达到10–5g/m2·day和10– 6g/m2·day级别的水汽透过率，可以作为高性能水汽阻隔膜应用于柔性OLED、有机薄膜晶体管等电子器件。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。

Claims (10)

1.一种用作柔性显示器件的水汽阻隔膜，其特征在于，包括：基底层和位于所述基底层外侧的水汽阻隔层，所述水汽阻隔层由多层交替层叠的磁控溅射层和原子沉积层构成，将磁控溅射层记为S、原子沉积层记为D、基底层记为P，所述水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式中的任意一种被布置：(S-D)m-S-P顺序、(D-S)m-D-P顺序、(S-D)m-P顺序或(D-S)m-P顺序，其中m是交替的S和D的数量。
2.根据权利要求1所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述磁控溅射层采用卷对卷磁控溅射工艺沉积得到。
3.根据权利要求2所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述磁控溅射层的材料为二氧化硅(SiO2)、三氧化二铝(Al2O3)、一氧化硅(SiO)、氮化硅(Si3N4)、氮氧化硅(SiOxNy)、氮化钛(TiN)中的一种或多种的组合。
4.根据权利要求1所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述原子沉积层采用卷对卷原子层沉积工艺沉积得到。
5.根据权利要求4所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述原子沉积层的材料为二氧化硅(SiO2)、三氧化二铝(Al2O3)、一氧化硅(SiO)、氮化硅(Si3N4)、氮氧化硅(SiOxNy)、氮化钛(TiN)中的一种或多种的组合。
6.根据权利要求1所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述磁控溅射层的材料为氮化硅，所述原子沉积层的材料为三氧化二铝。
7.根据权利要求6所述的用作柔性显示器件的水汽阻隔膜，其特征在于，制备所述磁控溅射层的卷对卷磁控溅射工艺条件为：使用纯硅靶材，功率为6000W，气体流量位70sccm的氮气和80sccm的氩气；
所述磁控溅射层的厚度为50nm。
8.根据权利要求6所述的用作柔性显示器件的水汽阻隔膜，其特征在于，制备所述原子沉积层的卷对卷原子层沉积工艺条件为：气源前驱体为三甲基铝和臭氧，卷绕镀膜鼓温度为100℃；
所述原子沉积层的厚度为45nm。
9.根据权利要求1-8中任意一项所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述水汽阻隔层中的磁控溅射层和原子沉积层按照以下层叠方式中的任意一种被布置：D-S-P顺序、S-D-S-P顺序、D-S-D-S-P顺序或D-S-D-S-D-S--P顺序。
10.根据权利要求1所述的用作柔性显示器件的水汽阻隔膜，其特征在于，所述基底层的材料为聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸乙二醇酯(PET)、三醋酸纤维素(TAC)、环烯烃共聚物(COP)、环烯烃聚合物(COC)、聚碳酸酯(PC)、聚醚醚酮(PEEK)中的一种或多种。
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