CN111925727B - 一种偏光片用离型剂、离型膜及其制备方法 - Google Patents
一种偏光片用离型剂、离型膜及其制备方法 Download PDFInfo
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Abstract
本发明涉及电子材料领域，具体公开了一种用于偏光片PSA层成型和保护的离型剂、离型膜及其制备方法，该离型剂的组分包括2‑10wt%烯基硅油、0.03‑2wt%固化剂、不超过3wt%剥离调节剂、0.03‑3wt%硅烷偶联剂、0.03‑2wt%铂金催化剂、0.03‑2wt%纳米硅微粉、76‑97.88%wt%溶剂；剥离调节剂为羟基硅油或甲基硅氧烷，所述溶剂为甲苯、庚烷、丁酮的混合物。本发明使用固化剂、剥离调节剂以及包含甲苯、庚烷、丁酮的混合溶剂有效降低离型层的表面自由能和表面张力，实现残余接着率≥92%和低配向角≤11°，以获得以流平成膜性好、剥离力小且稳定、无彩虹纹、无眩光、低配向角的离型膜。
Description
技术领域
本发明涉及电子材料领域，特别是涉及一种用于偏光片PSA层的成型、保护的离型剂、离型膜及其制备方法。
背景技术
偏光片的结构包括最中间的PVA层、PVA两侧的TAC层、一侧TAC层上的PSA 层、位于PSA层侧的离型膜和位于另一TAC层侧的保护膜。PSA层是一层由主要由丙烯酸酯构成的压敏粘合剂，通常是由树脂溶液涂布于离型膜表面经高温加热干燥后成型，再转移贴合至TAC层上。
离型膜包括基材层和离型剂层，将离型剂涂布在基材层上形成离型膜。离型剂的组分、粘度等性质都对形成的离型膜及偏光片性能产生影响。
离型膜不仅在PSA涂布时发挥承载作用，而且在转移贴合到TAC层后起保护作用；后续在使用偏光片时，需剥离离型膜露出PSA层实现贴片。因此，离型膜需保证PSA层涂布的均匀性以及成型表面的光滑度，稳定且低的剥离力以实现与PSA层的可剥离性。
然而，现有的偏光片的PSA层仍然存在在离型膜无法均匀涂布成型或涂布后局部收缩产生麻点和空洞的问题；在与离型膜剥离时，存在着剥离力不稳定或经时变化大的问题。另外，离型膜的配向角没有得到足够的优化，离型膜还存在外观表现如雾度、彩虹纹、炫光的问题，影响偏光片的缺陷检出率，最终影响偏光片的性能质量。
如CN201710736953.8公开了末端含羟基的乙烯基硅油作为离型力调节剂在制备离型剂中的应用及其离型剂和离型膜，提高了离型膜的离型力以及离型力的稳定性，但尚未对离型膜的配向角和流平成膜性进行优化，所得到的离型膜仍存在外观表现如雾度、彩虹纹、炫光等问题，影响偏光片的性能质量。
发明内容
本发明的目的是针对现有技术的不足，提供一流平成膜性好、剥离力小且稳定、无彩虹纹、无眩光、低配向角的离型剂，以解决现有技术中离型膜的流平成膜性（PSA成型）、离型力、配向角及外观性能上仍存在的问题。
为解决上述技术问题，本发明采用的一个技术方案是：提供一种偏光片用离型剂，所述离型剂的组分包括2-10wt%烯基硅油、0.03-2wt%炔二醇、不超过3wt%剥离调节剂、0.03-3wt%硅烷偶联剂、0.03-2wt%铂金催化剂、0.03-2wt%纳米硅微粉、76-97.88wt%混合溶剂。
上述技术方案中，选用烯基硅氧烷树酯作为有机硅树脂，含量为2-10wt%。若含量小于2wt%，离型膜的离型力过低，易于PSA层脱；若含量大于10wt%，浓度过大，固体成分增多，涂布效果会变差。
发明人利用固化剂炔二醇含有的碳碳双键，使其与烯基硅油的碳碳双键键合，达到交联固化的效果。同时，若固化剂的分子量太小，固化反应快，会影响涂层的柔韧性；若固化剂的分子量太大，固化效率则低，而炔二醇的分子量为66-500之间，分子量合适，故发明人选用炔二醇对烯基硅油进行固化。
偶联剂的含量为0.03-3wt%，可增加离型膜表面附着力，降低表面自由能，调节表面接触角。
铂金催化剂的含量为0.03-2wt%，可增加固化速度和程度，铂金添加量会影响溶液的浴槽寿命、生产成本等，同时影响最终产品的离型力、附着力、残余接着率等。
纳米硅微粉的含量为0.03-2wt%，可改善离型膜的雾度和涂层微观结构，降低彩虹纹、炫光问题，同时改善涂层摩擦系数、减少离型膜与PSA贴合后裁切时产生位移而产生裁切纹异常。
作为优选，所述剥离调节剂为羟基硅油，其组分含量为3wt%以下；所述剥离调节剂为甲基硅氧烷，其组分含量为2wt%以下。
发明人发现使用含量为3wt%以下的羟基硅油，可控制离型力达5-40g/inch，故可将羟基硅油作为重剥离调节剂使用；使用含量为2wt%以下的甲基硅氧烷，可控制离型力达1-5g/inch，故可将甲基硅氧烷作为轻剥离调节剂使用。
作为优选，所述溶剂为甲苯、庚烷、丁酮的混合溶液。
进一步优选，所述混合溶液中甲苯、庚烷、丁酮的重量比为1:0.5-1:1-1.3。
溶剂为甲苯、庚烷和丁酮，甲苯的沸点为110℃，庚烷的沸点为98℃，丁酮的沸点为80℃，且三者对上述硅油树脂的溶解度不一样，通过三者的混合，便于控制涂布时离型剂层的流平性，可避免离型剂层橘皮纹、涂布线条等厚度不均现象。
发明人通过调节三者的比例，调整离型剂至合适的粘度。若离型剂溶液的粘度太低，涂布时容易出现涂层流挂、厚度不均的现象；若溶液粘度太高，涂布时涂层流平性差，容易出现涂层橘皮纹、涂布线条等厚度不均现象。而且，这种混合溶剂在固化时会随着温度的变化逐步挥发，使干燥后的离型面平整、光滑。
作为优选，所述离型剂的粘度为1.4-10cps。
作为优选，所述离型剂中还包括添加剂，所述添加剂包括流平剂、消泡剂等。
所述离型膜，所述离型膜包含基材层和离型剂层，所述离型剂层使用上述离型剂涂布于基材层所得。
作为优选，所得的离型膜的低表面接触角≤118°、低配向角≤11°、离型力1-40g/in、残余接着率≥92%、外观无彩虹纹和炫光。
作为优选，所述基材层为聚对苯二甲酸乙二醇酯薄膜（PET），厚度为19-100μm（厚度公差为±2μm），透光率≥88%，雾度≤10%，配向角≤11°。
所述离型膜的制备方法，具体如下：
步骤一：在甲苯、庚烷和丁酮的混合溶剂中，加入有机硅树脂、固化剂、剥离调节剂羟基硅油或甲基硅氧烷、偶联剂、铂金催化剂、纳米硅微粉搅拌均匀后形成离型剂悬浮液。
步骤二：将所述离型剂采用普通凹版转印式涂布、微凹涂布、狭缝挤出式涂布等涂布方式涂布到所述基材层上，得到离型膜。
作为优选，所述步骤二中，在离型剂涂布后进行烘烤，烘烤温度为70℃-150℃，烘烤时间为15秒－4分钟，离型层干燥后厚度为50-400nm。
通过实施上述技术方案，本发明具有如下的有益效果：
本发明通过调节离型剂的组分及其配比，所获得的离型剂涂布性好，其形成的离型层离型力稳定可控、表面接触角≤118°、残余接着率≥92%，从而实现PSA层在其离型面上优异的流平成膜性，不产生任何麻点和空洞。
使用所述离型剂所制得的离型膜透明度高、无彩虹、无炫光，配向角小于11°（对基材膜的配向角不产生影响），便于后续偏光片的缺陷观测。
具体实施方式
本发明公开了一种偏光片用离型膜及其制备方法，以下更详细地描述本发明。
本发明的特征在于所述离型膜的离型剂层所用的离型剂包含有2-10wt%烯基硅油、0.03-2wt%炔二醇、0-3wt%剥离调节剂羟基硅油或甲基硅氧烷、0.03-3wt%硅烷偶联剂、0.03-2wt%铂金催化剂、0.03-2wt%纳米硅微粉、76-97.88%wt%溶剂。
采用如此配比的离型剂可以有效降低离型层的表面自由能和表面张力，使得离型面的表面接触角≤118°，从而实现PSA层在其离型面上优异的流平成膜性，不产生任何麻点和空洞；同时，添加剥离调节剂使其获得可控的离型力，范围为1-40g/inch，可实现稳定且低的离型力，也可实现客户定制化的需求，并且残余接着率≥92%，另外可实现涂布性的提高，PSA胶涂布成膜性的提高，外观无彩虹纹和炫光，低配向角≤11°。
以下是对本发明的较佳实施例及比较例进行说明，对本发明的技术方案作进一步的描述，但下述实施例只是本发明中的较佳实施实例而非限制本发明。
设置组分不同配比的离型剂形成的离型膜具体如表一：
测试实施例与比较例：
【离型力的测定】：取25.4mm宽、200mm长的NITTO 31B胶带贴于膜的测试面，即离型面，并用标准碾压辊往复滚压3次（注意：贴合胶带是要一边贴一边辊压，避免胶带与离型之间有气泡而影响测试准确性）；贴好胶带后静置20分钟，实验室的温湿度分别控制在25±3℃及50±10RH%；然后用双面胶贴于样片的非测试面并固定在标准钢板上，待测试。将材料安装上夹具，用拉力机以180度角拉伸测试胶带的方法测试，拉力机电脑显示的数据即为试片的离型力（g/in）,取5个数值的平均值为测试结果。
【残余接着率】：将NITTO 31B胶带与离型膜的离型面贴合一定时间后，将NITTO31B胶带从离型膜的离型面剥离下来，再去测试NITTO31B胶带的粘力值,设为B；而NITTO31B胶带未经过与离型膜的离型面贴合，直接测试其粘力值，设为A，则残余接着率=（B/A）*100%。
【表面接触角】：使用光学水滴角测试仪，通过静滴法并依据JIS R3257测定接触角。
【成膜性】：将生产偏光片用的PSA胶水均匀涂布于离型膜的表面，观察胶水涂层是否有收缩产生麻点、局部破孔现象；没有收缩产生麻点、局部破孔现象，说明可成膜性优异。
【评价结果】
实施例与比较例的评价结果如表二所示。
分析表一和表二数据，对比实施例1与比较例1，本申请组方配比下得到的离型膜物性明显优异；对比实施例1与对比例2，对比实施例2与比较例2，本申请中使用剥离调节剂以及确定的重量份等使其具有高稳定性，以及PSA转贴和剥离容易。
本文中所描述的具体实施例仅仅是对本发明作举例说明，而非对本发明的限制，凡是利用本发明说明书内容所作的等效结构或等效流程变换，或直接或间接运用在其他相关的技术水平，均同理包括在本发明的专利保护范围内。
Claims (9)
1.一种用于形成偏光片的离型剂，其特征在于，所述离型剂的组分包括2-10wt%烯基硅油、0.03-2wt%炔二醇、不超过3wt%剥离调节剂、0.03-3wt%硅烷偶联剂、0.03-2wt%铂金催化剂、0.03-2wt%纳米硅微粉、76-97.88wt%溶剂，所述溶剂为甲苯、庚烷、丁酮的混合溶液。
2.根据权利要求1所述的用于形成偏光片的离型剂，其特征在于，所述剥离调节剂为羟基硅油，其组分含量为3wt%以下。
3.根据权利要求1所述的用于形成偏光片的离型剂，其特征在于，所述剥离调节剂为甲基硅氧烷，其组分含量为2wt%以下。
4.根据权利要求1所述的用于形成偏光片的离型剂，其特征在于，所述混合溶液中，甲苯、庚烷、丁酮的重量比为1:0.5-1:1-1.3。
5.根据权利要求1所述的用于形成偏光片的离型剂，其特征在于，所述离型剂的粘度为1.4-10cps。
6.一种用于形成偏光片的离型膜，包含基材层和形成于基材层上的离型剂层，其特征在于，所述离型剂层采用权利要求1-5任一项所述的离型剂所形成。
7.根据权利要求6所述的用于形成偏光片的离型膜，其特征在于，所述离型剂层的厚度为50-400nm。
8.根据权利要求6所述的用于形成偏光片的离型膜，其特征在于，所述离型膜的低表面接触角≤118°、低配向角≤11°、离型力1-40g/in、残余接着率≥92%。
9.根据权利要求6所述的用于形成偏光片的离型膜，其特征在于，在形成离型剂层时，采用的烘烤温度为70℃-150℃，烘烤时间为15秒－4分钟。
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