CN114805889B - 一种用于柔性显示屏的罩层胶膜及其制备方法 - Google Patents

一种用于柔性显示屏的罩层胶膜及其制备方法 Download PDF

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CN114805889B
CN114805889B CN202210386149.2A CN202210386149A CN114805889B CN 114805889 B CN114805889 B CN 114805889B CN 202210386149 A CN202210386149 A CN 202210386149A CN 114805889 B CN114805889 B CN 114805889B
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王景泉
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Abstract

本发明公开了一种用于柔性显示屏的罩层胶膜及其制备方法，包括基层，在基层表面上依次层叠有硬涂层、粘结剂层、功能涂层，所述粘结剂层采用气溶胶材料。所述粘结剂层采用柔韧性二氧化硅气凝胶，粘结剂层密度值为30～60kg/m3，杨氏模量为1×105～1.5×105N/m2。本发明提供的柔性显示屏罩层胶膜，发挥多涂层协同作用，硬涂层具有高硬度、高韧性、高透光率，粘结剂层具有高透光率和柔韧性，同时对硬涂层及功能涂层具有良好的层间附着力，功能涂层具有高柔韧性、高透光率，同时起到防指纹、防眩光、防起雾的作用，在不影响通透性的同时使透过的光线柔和、美观，另外柔性显示屏的罩层胶膜具有较高的耐反复折弯性能，尤其适用于柔性显示屏以及投屏显示。

Description

一种用于柔性显示屏的罩层胶膜及其制备方法
技术领域
发明涉及胶膜技术领域，尤其涉及一种柔性显示屏罩层胶膜及其制备。
背景技术
透明聚合物薄膜作为核心材料在光学和柔性显示行业得到了广泛的应用，并因其重量轻、易于加工等优点在显示器行业中替代玻璃应用。
随着国际、国内柔性屏不断研发及改进，包括柔屏材质厚度的不断突破，当前国内最薄的屏厚度为0.03mm，可折叠次数普遍在20～30万次以内，针对越发超薄的突破，其柔性屏体系中相对应的高硬度的硬质涂层的配套研发正在积极进行，其中涉及了可折叠、柔性显示器的薄膜包括AF涂层。为了满足超薄材质要求下使用透明聚合物薄膜作为可折叠显示器及柔性显示器的窗盖，其柔韧性是一个非常重要的问题，同时它需要满足高硬度和耐磨性等表面性能。然而，由于应用了SiO2作为AF涂层的粘结剂后薄膜的柔韧性明显变差，无法达到百万次级别的折叠性能寿命加速测试的要求，因此使用传统方法制造透明聚合物薄膜难以作为超薄化可折叠显示器及柔性显示器的窗盖应用。
发明内容
本发明的目的是提供一种具有高柔韧性、高硬度、耐划伤、耐指纹、防雾、耐反复折弯的柔性显示屏罩层胶膜，同时具有高透光性及使光线柔和的效果。
一种用于柔性显示屏的罩层胶膜，包括基层，以及在基层表面依次层叠的硬涂层、粘结剂层和功能涂层，所述粘结剂层采用气溶胶材料。
其中所述硬涂层由包含一下质量分的组分：聚甲基丙烯酸甲酯80～100份、交联剂20～150份、助剂1～10份，其中交联剂为三羟甲基丙烷三丙烯酸酯，助剂为附着力促进剂、分散剂、消泡剂中的一种或多种。
用于硬涂层的组合物中包含(甲基)丙烯酸酯可以进一步提高硬涂层的硬度和柔韧性以及透光性；硬涂层厚度为1μm至30μm；
除此之外，为了获得一个适当的硬涂层与外涂层的柔韧性比例，硬涂层也可以包含高柔韧改性聚氨酯丙烯酸酯10～20份。
为了保证硬涂层同时具有较高的柔韧性，交联剂用量优选为50～100份；
本发明硬涂层的制备方法包括：先将聚甲基丙烯酸甲酯高速搅拌均匀分散，然后加入交联剂和助剂继续进行低速搅拌分散，再使用三辊机进行多次研磨至细度≤3μm。
基层可包括选自由聚对苯二甲酸乙二醇酯(PET)基树脂、聚醚砜(PES)基树脂、聚萘二甲酸乙二醇酯(PEN)基树脂、聚丙烯酸酯(PAR)基树脂组成的组中的至少一种。优选地，基层包括由聚酰亚胺树脂形成的膜。基层厚度为10μm至200μm，优选地厚度为30μm至100μm。
功能涂层包含以下质量份的组分：氟硅树脂80～100份、稀土磷酸盐微粒0.1～50份、硅烷偶联剂1～30份、季戊四醇三丙烯酸酯10～15份。
功能涂层的厚度为100～500μm，优选为300～400μm，有利于保证水接触角和保证表面质量。
本发明功能涂层的制备方法包括：先将稀土磷酸盐微粒、氟硅树脂高速搅拌均匀分散，然后加入硅烷偶联剂、季戊四醇三丙烯酸酯继续进行低速搅拌分散即得。
本发明粘结剂层厚度为100～200μm，优选地厚度为120～150μm，采用柔韧性二氧化硅气凝胶，粘结剂层密度值为30～60kg/m3，杨氏模量为4×104～1×105N/m2。
本发明采用柔韧性二氧化硅气凝胶作为硬涂层与功能涂层之间的粘结剂层，具有高应力和恢复性，能够提高柔性显示屏罩层胶膜整体的柔韧性，防止出现膜层滑移、膜层断裂等现象。在一种优选方案中，本发明采用以甲基三乙氧基硅烷和正甲基硅烷为硅源、在乙醇和水中与氨水反应得到的溶胶，经静置老化保温后制得的柔韧性二氧化硅气凝胶。相较于采用单一硅源所制备的柔韧性二氧化硅气凝胶，本发明选用的柔韧性二氧化硅气凝胶可以大幅提高胶膜的光扩散率和反复折弯性能。
本发明制得的柔性显示屏罩层胶膜可以用于制造柔性显示屏，所述柔性显示屏从上到下依次层叠有柔性显示屏罩层胶膜、彩色滤光层、液晶层、透明电极层、下偏光片、柔性背光模组，所述柔性显示屏罩层胶膜与彩色滤光层之间、柔性背光模组与下偏光片之间采用光学胶粘结在一起，所述下偏光片贴附在透明电极层下，所述彩色滤光层与透明电极层通过框胶固定连接在一起，从而在所述彩色滤光层与透明电极层之间形成用来填充液晶层的容置空间，采用本发明柔性显示屏罩层胶膜制得的柔性显示屏具有优异的表面耐磨性、透光性、视觉效果，尤其具备达到百万次级别的耐反复折弯性能。
稀土磷酸盐微粒是稀土钪或钇的磷酸盐微粒，具有高折射率和高阿贝数。当涂层中的稀土磷酸盐微粒比例逐渐增加，胶膜的光扩散度升高，逐渐拥有较高的图像显示性，因此本发明的柔性显示屏罩层胶膜也可以在玻璃窗类透明介质上用于投屏广告或投影显示视频内容。本发明中选用平均粒径在5-20微米的稀土磷酸盐微粒。
本发明用于柔性显示屏的罩层胶膜的制备方法包括：将硬涂层辊涂在基材上，然后在90℃下干燥15～20分钟；将粘结剂层辊涂在硬涂层上，然后在90℃下干燥20～30分钟；最后将功能涂层辊涂于粘结剂层上，在氮气环境下采用EB固化装置完全固化。
电子束固化辐射电压为380～420KeV，辐射剂量50～80kGy。
本发明的有益效果：
本发明提供的柔性显示屏的罩层胶膜，发挥多涂层协同作用，硬涂层具有高硬度、高韧性、高透光率，粘结剂层具有高透光率和柔韧性，同时对硬涂层及功能涂层具有良好的层间附着力，功能涂层具有高柔韧性、高透光率，同时起到防指纹、防眩光、防起雾的作用，在不影响通透性的同时使透过的光线柔和、美观，达到透光不透明的舒适效果，另外柔性显示屏的罩层胶膜具有较高的耐反复折弯性能，反复折弯后无折痕、断裂、褶皱、蠕变现象，使用寿命长，尤其适用于柔性显示屏以及投屏显示。
附图说明
图1是本发明实施例4的结构示意图；
其中，1-柔性显示屏罩层胶膜、2-彩色滤光层、3-液晶层、4-透明电极层、5-下偏光片、6-柔性背光模组。
具体实施方式
通过以下实施例对本发明的检测方法作进一步的说明，但这些实施例不对本发明构成任何限制。
柔韧性二氧化硅气凝胶的制备：将145mL甲基三乙氧基硅烷、15mL正甲基硅烷、450mL乙醇和60mL水混合均匀后，加入盐酸溶液调节混合溶液的pH值至2～3，再加入3.5mL氨水溶液，得到溶胶，将溶胶静置凝胶，然后置于无水乙醇中进行老化，老化温度为50℃，老化后凝胶样品在82℃下保温4.5h，以1℃/min的速率升温至120℃，保温8h。
以下各实施例硬涂层的制备方法包括：本发明的硬涂层的制备方法包括先将聚甲基丙烯酸甲酯高速搅拌均匀分散，然后加入交联剂和助剂继续进行低速搅拌分散，再使用三辊机进行多次研磨至细度≤3μm。
以下各实施例用于柔性显示屏的罩层胶膜的制备方法包括：将硬涂层辊涂在基材上，然后在90℃下干燥15～20分钟；将柔韧性二氧化硅气凝胶辊涂在硬涂层上形成粘结剂层，然后在90℃下干燥20～30分钟；最后将功能涂层辊涂于粘结剂层上，在氮气环境下采用EB固化装置完全固化，获得柔性显示屏罩层胶膜1成品。
电子束固化条件：电子束固化辐射电压为380～420KeV，辐射剂量50～80kGy，每层固化时间为3～5s。
实施例1～3、对比例1～3的各原料及用量如表1所示。
表1
Figure BDA0003593786820000041
对比例4
将氟硅树脂替换为环氧丙烯酸酯，其余同实施例1。
对比例5
粘结剂层采用SiO2，其余同实施例1。
实施例4
对实施例1～3和对比例1～3所制备的柔性显示屏罩层胶膜1成品分别进行透光率、雾度、水接触角和光扩散率测试，结果见表2。
表2
Figure BDA0003593786820000042
Figure BDA0003593786820000051
透光率：根据GB/T 2410-2008测量标准用DR81透光率仪测量。
雾度：根据GB/T 2410-2008测量标准用雾度计TH-100设备测量。
水接触角：使用Model 590,p/n 590-F1设备测量去离子水的接触角。
光扩散率：使用分布光度计GC5000L测量透射率和反射率，通过分布光度计中内置的程序计算扩散率。
实施例5
用实施例1～3、对比例1～5完全固化制得的柔性显示屏罩层胶膜1制备一种柔性显示屏，从上到下依次层叠有柔性显示屏罩层胶膜1、彩色滤光层2、液晶层3、透明电极层4、下偏光片5、柔性背光模组6，所述柔性显示屏罩层胶膜1与彩色滤光层2之间、柔性背光模组6与下偏光片5之间采用光学胶粘结在一起，所述下偏光片5贴附在透明电极层4下，所述彩色滤光层2与透明电极层4通过框胶固定连接在一起，从而在所述彩色滤光层2与透明电极层4之间形成用来填充液晶层3的容置空间。对上述制成的柔性显示屏表面进行测试，结果见表3。
表3
实施例 硬度 耐磨性 反向R(mm) 反复折弯
1 H 88 1.1 OK
2 H 87 1.2 OK
3 H 87 1.4 OK
对比例1 H 86 2.3 NG
对比例2 H 86 1.7 NG
对比例3 H 87 1.1 OK
对比例4 F 80 1.7 NG
对比例5 H 87 3.3 NG
硬度：推车式铅笔硬度计，载荷750g。
耐磨性：用LER902K砂质橡皮，施加500g的载荷，以40～60次/分钟的速度，20mm左右的行程，在样本表面来回摩擦。
反向R：使用弯曲测试仪设备JIRBT-620测量开裂时的半径R。
反复折弯：采用日本TCDMLH-C4BR柔性屏弯曲耐久试验机，开合角度为0-180°、外折半径为R5、拉伸负重为1kg的测试条件下，按照60r/min的速度测试100万次后点亮屏幕观察是否有分层、断裂、老化，显色是否正常。
以上实施例仅用以说明本发明的技术方案，而非对其限制；尽管参照前述实施例对本发明进行了详细的说明，本领域的普通技术人员应当理解：其依然可能对前述各实施例所记载的技术方案进行修改，或者对其中部分技术特征进行等同替换；而这些修改或者替换，并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。

Claims (9)

1.一种用于柔性显示屏的罩层胶膜，其特征在于，包括基层，以及在基层表面依次层叠的硬涂层、粘结剂层和功能涂层，所述粘结剂层采用气凝胶材料；所述硬涂层包含以下质量份的组分：聚甲基丙烯酸甲酯80~100份、交联剂20~150份和助剂1~10份；功能涂层包含以下重量份的组分：氟硅树脂80~100份、稀土磷酸盐微粒0.1～50份、硅烷偶联剂1～30份和季戊四醇三丙烯酸酯10~15份。
2.根据权利要求1所述用于柔性显示屏的罩层胶膜，其特征在于，所述粘结剂层采用柔韧性二氧化硅气凝胶。
3.根据权利要求2所述用于柔性显示屏的罩层胶膜，其特征在于，粘结剂层密度值为30～60kg/m³，杨氏模量为4×104～1×105N/m2。
4.根据权利要求1所述用于柔性显示屏的罩层胶膜，其特征在于，所述交联剂为三羟甲基丙烷三丙烯酸酯。
5.根据权利要求3所述用于柔性显示屏的罩层胶膜，其特征在于，基层厚度为10μm至200μm；硬涂层厚度为1μm至30μm；功能涂层厚度为100至500μm；粘结剂层厚度为100至200μm。
6.一种权利要求1所述用于柔性显示屏的罩层胶膜的制备方法，其特征在于，包括：将硬涂层辊涂在基材上，然后在90℃下干燥15～20分钟；将粘结剂层辊涂在硬涂层上，然后在90℃下干燥20～30分钟；最后将功能涂层辊涂于粘结剂层上，在氮气环境下采用EB固化装置完全固化。
7.根据权利要求6所述用于柔性显示屏的罩层胶膜的制备方法，其特征在于，所述硬涂层的制备方法包括：先将聚甲基丙烯酸甲酯高速搅拌均匀分散，然后加入交联剂和助剂继续进行低速搅拌分散，再使用三辊机进行多次研磨至细度≤3μm。
8.根据权利要求6所述用于柔性显示屏的罩层胶膜的制备方法，其特征在于，所述功能涂层的制备方法包括：先将稀土磷酸盐微粒、氟硅树脂高速搅拌均匀分散，然后加入硅烷偶联剂、季戊四醇三丙烯酸酯继续进行低速搅拌分散即得。
9.根据权利要求6所述柔性显示屏罩层胶膜的制备方法，其特征在于，电子束固化辐射电压为380~420KeV，辐射剂量50~80kGy。
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