CN111171630A - 一种喷墨打印图案化透明导电膜的制备方法 - Google Patents
一种喷墨打印图案化透明导电膜的制备方法 Download PDFInfo
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- CN111171630A CN111171630A CN202010059264.XA CN202010059264A CN111171630A CN 111171630 A CN111171630 A CN 111171630A CN 202010059264 A CN202010059264 A CN 202010059264A CN 111171630 A CN111171630 A CN 111171630A
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- ink
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- nano silver
- silver rod
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Abstract
本发明属于导电膜准备技术领域，具体地说，涉及一种喷墨打印图案化透明导电膜的制备方法。所述的制备方法包括：S1、分别配制纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水；S2、分别将纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水加至供墨系统中；S3、将预先设计出的设计图纸输入至打印机中；S4、根据设计图纸在基材上依次喷墨打印纳米银棒导电墨水I和纳米银棒导电墨水II，固化，形成导电图案区与导电通道区；S5、在导电图案区与导电通道区表面喷墨打印功能墨水，固化，形成导电线路，再进行处理，即得图案化透明导电膜。本发明提供的喷墨打印图案化透明导电膜的制备方法成本低，且制得的图案化透明导电膜全透明。
Description
技术领域
本发明属于导电膜准备技术领域，具体地说，涉及一种喷墨打印图案化透明导电膜的制备方法。
背景技术
随着物质水平的日益提高，消费者对电子产品的要求正往轻薄化和柔性化、可视化、触控化的方面快速发展。目前全世界触摸屏及相关产业链正以极快的速度融入到人们的日常生活中。
透明导电膜是具有良好导电性和在可见光波段具有高透光率的一种薄膜。目前透明导电膜已广泛应用于平板显示、光伏器件、触控面板和电磁屏蔽等领域，具有极其广阔的市场空间。而随着上述器件朝轻薄化方向的快速发展，柔性透明导电膜因其具有轻薄、柔软性好等优点而成为研究的重点。
柔性透明导电膜一般可以分为非图形化的和图形化的两类。前者在诸如触摸屏等大多数实际应用中，往往需要曝光、显像、刻蚀及清洗等多道工序对透明导电膜进行图形化，方可应用。而后者无疑具有更好的生产效率，省去了后续复杂且易污染环境的图形化工艺，是透明导电膜的主要发展方向。
ITO一直主导着透明导电膜的市场。图形化ITO膜的制备方法主要有丝印、喷墨打印法和半导体制程中的lift-off工艺。但由于铟矿资源的有限性和ITO极差的抗绕折性，以纳米金属材料为基础的图形化透明导电膜成为了上述背景下的最佳解决方案。
其制作方法多为印刷法：将粒径在纳米量级的金属材料制备成导电墨水，使用改进后印刷工艺，将导电墨水印刷在柔性透明基底表面，经烧结后形成所需的导电网格。网格线条宽度在一定范围内控制透明导电膜的表面方阻和透光率。日本公司大日本印刷、富士胶片和郡士，以及德国公司Poly IC都分别使用印刷方法获得了性能优异的图形化柔性透明导电薄膜。其中Poly IC所获得的图形分辨率为15μm，表面方阻0.4-1Ω/sq，透光率大于80％。
但是印刷技术制作的透明导电膜，其导电网络时裸露在透明基底表面凸起结构，防划抗刮特性极差。此外这些结果的图形分辨率均受到印刷工艺的制约，难以进一步提高。为了满足高分辨的应用需求，必须进一步减小图形分辨率。最后同样由于印刷工艺的限制，烧结前固定线宽下导电墨水的量也很难以进一步提高，即在选定线宽和导电墨水的前提下，很难以提高导电材料的量，进而改善薄膜的导电性。
发明内容
为解决上述技术问题，本发明的目的在于提供喷墨打印图案化透明导电膜的制备方法。
为实现上述目的，本发明采用如下技术方案：
一种喷墨打印图案化透明导电膜的制备方法，其中，所述的制备方法包括如下步骤：
S1、分别配制纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水；
S2、分别将纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水加至供墨系统中；
S3、将预先设计出的设计图纸输入至打印机中；
S4、根据设计图纸在基材上依次喷墨打印纳米银棒导电墨水I和纳米银棒导电墨水II，固化，形成导电图案区与导电通道区；
S5、在导电图案区与导电通道区表面喷墨打印功能墨水，固化，形成导电线路，再进行处理，即得喷墨打印图案化透明导电膜。
进一步的，步骤S5中，功能墨水的打印范围为覆盖导电图案区与导电通道区或基材整个表面。
进一步的，步骤S4中喷墨打印纳米银棒导电墨水I至少一次，喷墨打印纳米银棒导电墨水II至少一次；步骤S5中喷墨打印功能墨水至少一次，且整个过程中最后一次喷墨打印的是功能墨水。
进一步的，所述喷墨打印的方式为连续喷墨打印、热泡式喷墨打印或压电式喷墨打印。
进一步的，步骤S4和步骤S5中，所述的固化在温度60℃-160℃下进行。
本发明中，导电图案区的透过率大于80％，方阻为5-100Ω；导电通道区的透过率大于50％，方阻小于导电图案区的方阻。
本发明中，所述的纳米银棒导电墨水I和纳米银棒导电墨水II的组成可以相同，也可以不同。
作为一种优选实施方案，本发明所述的纳米银棒导电墨水I和纳米银棒导电墨水II的组成相同。
具体地说，所述的纳米银棒导电墨水I和纳米银棒导电墨水II的组成如下：
进一步的，所述的单体为水溶性或醇溶性有机小分子化合物；优选相对分子质量小于500的水溶性或醇溶性有机小分子化合物；更优选聚乙二醇二丙烯酸酯、丙烯酸丁酯、甘油丙烯酸酯、季戊四醇三丙酸酯、三羟甲基丙烷三丙烯酸酯、乙氧基化三羟甲基丙烷三丙烯酸酯、N-乙烯基吡咯烷酮或丙烯酰吗啉中的至少一种。
所述的树脂A为水溶性或醇溶性树脂；优选脂肪族聚氨酯丙烯酸酯齐聚物、环氧丙烯酸酯齐聚物或聚酯(甲基)丙烯酸酯中的至少一种。
具体地，所述的脂肪族聚氨酯丙烯酸酯齐聚物可以为沙多玛CN9006NS或长兴化学DR-U026等；所述的环氧丙烯酸酯齐聚物可以为长兴化学6210G等；所述的聚酯(甲基)丙烯酸酯可以为东亚合成M-7100等。
本发明中，本发明中，所述的助剂可以选自润湿分散剂、消泡剂、流平剂或成膜助剂中的一种或多种。
本发明中，润湿分散剂主要用于降低墨水的表面张力，改善墨水的流平性；例如毕克DISPERBYK-199、DISPERBYK-2015、DISPERBYK-2012、BYK3410、DISPERBYK-180；迪高TEGOERBYK-1802tps、740、750、755、
Wet 280、Wet KL 245、Dispers 650；特别是，润湿分散剂还可以参与光固化反应，从而使打印制品呈现透明的外观。具体地，润湿分散剂可以为能够辐射交联的有机硅丙烯酸酯和改性聚硅氧烷类聚合物中的一种或多种。其中，能够辐射交联的有机硅丙烯酸酯可以为迪高公司的TEGO RAD 2010、2011、2100、2200N、2250等，能够辐射交联的有机硅丙烯酸酯能参与光固化反应并发生交联反应，从而有利于抑制打印制品的发朦等现象；改性聚硅氧烷聚合物可以为毕克公司的BYK-333、BYK-371、BYK-377，迪高公司的Tego wet 270、Tego Glide 450等。
消泡剂主要用于消除过滤及打印过程中所产生的气泡，避免产生的气泡影响打印流畅性；消泡剂可以为不含有机硅类的聚合物，例如迪高的不含有机硅消泡剂TEGO Airex920、TEGO Airex 921等。
成膜助剂用于防止墨水组合物发生沉积，从而保证墨水组合物储存过程中的稳定性；本发明对成膜助剂的种类不作严格限制，只要能满足前述要求即可。成膜助剂为淀粉、阿拉伯胶、果胶、琼脂、明胶、海藻胶、角叉胶、糊精等，通用明胶、可溶性淀粉、多糖衍生物等；合成品有羧甲基纤维素、丙二醇藻蛋白酸酯、甲基纤维素、淀粉磷酸钠、羧甲基纤维素钠、藻蛋白酸钠、酪蛋白、聚丙烯酸钠、聚氧乙烯、聚乙烯吡咯烷酮中的至少一种。
本发明中，纳米银棒导电墨水I和纳米银棒导电墨水II、功能墨水中所采用的引发剂可以为水性引发剂或醇溶性引发剂。
具体地说，所述的水性引发剂可以为芳酮类，包括二苯酮衍生物、硫杂蒽酮衍生物、烷基芳酮衍生物或苯偶酰衍生物中的至少一种。所述的水性引发剂还可以为光引发剂2959、陶氏AMP-95、IRGACURE 819或IRGACURE 500中的至少一种。
所述的醇溶性引发剂可以为2-羟基-2-甲基-苯基丙酮-1(光引发剂1173)、TPO或BDK中的至少一种。
所述的溶剂为水、乙醇或异丙醇中的一种或几种。
进一步的，所述的功能墨水的组成如下：
进一步的，所述的树脂B为聚乙烯、聚氯乙烯、环氧树脂、聚氨酯、聚丙烯酸酯、聚甲基丙烯酸甲酯、氟聚合物、聚酰胺、聚酰亚胺、聚硅氧烷、聚碳酸酯、聚砜、聚乙烯醇、聚酯、丙烯腈-丁二烯-苯丙烯的共聚物或其掺合物。
所述的功能材料为紫外线吸收剂、抗氧剂或高折射高硬度添加剂中的至少一种。具体地说，所述的紫外吸收剂为水杨酸酯类、苯酮类、苯并三唑类、取代丙烯腈类、三嗪类和受阻胺类的一种或几种组合；所述的抗氧剂为自由基清除型抗氧剂，如N-苯基-α-萘胺和烷基吩噻嗪等；金属减活型抗氧剂，如苯并三氮唑衍生物和巯基苯并噻唑衍生物的一种或几种组合；所述的高折射高硬度添加剂为硅微粉、滑石粉、陶土、云母、二氧化硅、粉煤灰、硅酸盐等矿物、玻璃纤维、碳纤维、晶须等。
本发明中，功能墨水中所采用的引发剂也可以为非水溶性引发剂，包括苯偶姻及衍生物(安息香、安息香双甲醚等)；苯偶酰类(二苯基乙酮等)；烷基苯酮类(二乙氧基苯乙酮等)；酰基磷氧化物(芳酰基膦氧化物、双苯甲酰基苯基氧化膦等)；二苯甲酮类(二苯甲酮等)。
所述的助剂同上。
所述的溶剂为丙酮、丁酮、甲乙酮、乙酸乙酯、甲苯、二甲苯、重芳烃、醋酸丁酯中的一种或几种。
与现有技术相比，本发明具有如下优点：
本发明提供的喷墨打印图案化透明导电膜的制备方法成本低，且制得的图案化透明导电膜全透明。
具体实施方式
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明实施例中，所述的纳米银棒分散液的制备方法如下：
1、将50ml乙二醇加入单口烧瓶中，加入10ml摩尔浓度为5mM的硝酸银乙二醇溶液、10ml摩尔浓度为0.006mM氯化钠、30ml摩尔浓度为2mM的PVP乙二醇溶液和增稠剂羧甲基纤维素混合，搅拌30分钟，得反应液；
2、将反应液加入烧瓶中，放置于真空干燥箱，通入惰性气体，置换气体三次，调节真空度-0.1Mpa，转速1000r/min，升温到120℃，保温24h，得到纳米银棒原液；
3、将纳米银棒表面处理后得到所述的纳米银棒分散液，所述的表面处理包括如下步骤：
①将纳米银棒原液100ml分散到500ml水中，缓慢加入2.5g磷酸二氢铝，搅拌，离心，待纳米银棒沉降到底部，去除上层液体；
②再将沉降到底部的纳米银棒分散到500ml水中，缓慢加入0.5g磷酸二氢铝，搅拌，离心，待纳米银棒沉降到底部，去除上层液体，重复3次；
③最后将沉降到底部的纳米银棒分散到200ml水中，即得纳米银棒分散液。
实施例1
S1、将纳米银棒分散液0.2％、单体丙烯酰吗啉0.1％、助剂流平剂BYK-3330.001％、润湿分散剂DISPERBYK-2012 0.001％、光引发剂IRGACURE 500 0.005％和水余量搅拌混合均匀后，过滤得到纳米银棒导电墨水I；
将纳米银棒分散液1％、单体丙烯酰吗啉0.5％、助剂流平剂BYK-380N 0.05％、润湿分散剂DISPERBYK-2012 0.005％、光引发剂IRGACURE 500 0.025％和水余量搅拌混合均匀后，过滤得到纳米银棒导电墨水II；将沙多玛CN9006NS2％、功能材料紫外线吸收剂9440.02％、光引发剂29590.02％、BYK3410 0.0001％和溶剂余量搅拌混合均匀后，过滤得到功能墨水；
S2、分别将纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水加至供墨系统中；
S3、将预先设计出的设计图纸输入至打印机中；
S4、根据设计图纸在基材上依次喷墨打印纳米银棒导电墨水I和纳米银棒导电墨水II，120℃下将溶剂挥发，再进行紫外固化，形成导电图案区与导电通道区；
S5、在导电图案区与导电通道区表面喷墨打印功能墨水，120℃下将溶剂挥发，再进行紫外固化，形成导电线路，再在丙烯酰吗啉的玻璃化温度145℃下处理，即得喷墨打印图案化透明导电膜；
其中步骤S5中，功能墨水的打印范围为覆盖导电图案区与导电通道区。
实施例2
S1、将纳米银棒分散液10wt％、脂肪族聚氨酯丙烯酸酯齐聚物沙多玛CN9006NS1％、助剂流平剂BYK-380N 0.01％、润湿分散剂DISPERBYK-20120.01％、光引发剂IRGACURE 500 0.01％和乙醇余量搅拌混合均匀后，过滤得到喷墨打印墨水；
按照上述配方和制备方法配制纳米银棒导电墨水II；
将沙多玛CN9006NS2％、功能材料紫外线吸收剂944 0.02％、光引发剂11730.01％、305T0.0001％和溶剂余量搅拌混合均匀后，过滤得到功能墨水；
S2、分别将纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水加至供墨系统中；
S3、将预先设计出的设计图纸输入至打印机中；
S4、根据设计图纸在基材上依次喷墨打印纳米银棒导电墨水I和纳米银棒导电墨水II，120℃下将溶剂挥发，再进行紫外固化，形成导电图案区与导电通道区；
S5、在导电图案区与导电通道区表面喷墨打印功能墨水，120℃下将溶剂挥发，再进行紫外固化，形成导电线路，即得喷墨打印图案化透明导电膜；
其中步骤S5中，功能墨水的打印范围为覆盖导电图案区与导电通道区。
最后应说明的是：以上所述仅为本发明的优选实施例而已，并不用于限制本发明，尽管参照前述实施例对本发明进行了详细的说明，对于本领域的技术人员来说，其依然可以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。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种喷墨打印图案化透明导电膜的制备方法，其特征在于，所述的制备方法包括如下步骤：
S1、分别配制纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水；
S2、分别将纳米银棒导电墨水I、纳米银棒导电墨水II和功能墨水加至供墨系统中；
S3、将预先设计出的设计图纸输入至打印机中；
S4、根据设计图纸在基材上依次喷墨打印纳米银棒导电墨水I和纳米银棒导电墨水II，固化，形成导电图案区与导电通道区；
S5、在导电图案区与导电通道区表面喷墨打印功能墨水，固化，形成导电线路，再进行处理，即得喷墨打印图案化透明导电膜。
2.根据权利要求1所述的制备方法，其特征在于，步骤S5中，功能墨水的打印范围为覆盖导电图案区与导电通道区或基材整个表面。
3.根据权利要求2所述的制备方法，其特征在于，步骤S4中喷墨打印纳米银棒导电墨水I至少一次，喷墨打印纳米银棒导电墨水II至少一次；步骤S5中喷墨打印功能墨水至少一次；且整个过程中最后一次喷墨打印的是功能墨水。
4.根据权利要求3所述的制备方法，其特征在于，所述喷墨打印的方式为连续喷墨打印、热泡式喷墨打印或压电式喷墨打印。
5.根据权利要求1-4任意一项所述的制备方法，其特征在于，步骤S4和步骤S5中，所述的固化在温度60℃-160℃下进行。
6.根据权利要求5所述的制备方法，其特征在于，所述的纳米银棒导电墨水I和纳米银棒导电墨水II的组成如下：
7.根据权利要求5所述的制备方法，其特征在于，所述的功能墨水的组成如下：
8.根据权利要求6所述的制备方法，其特征在于，
所述的单体为水溶性或醇溶性有机小分子化合物，优选相对分子质量小于500的水溶性或醇溶性有机小分子化合物，更优选聚乙二醇二丙烯酸酯、丙烯酸丁酯、甘油丙烯酸酯、季戊四醇三丙酸酯、三羟甲基丙烷三丙烯酸酯、乙氧基化三羟甲基丙烷三丙烯酸酯、N-乙烯基吡咯烷酮或丙烯酰吗啉中的至少一种；
所述的树脂A为水溶性或醇溶性树脂；优选脂肪族聚氨酯丙烯酸酯齐聚物、环氧丙烯酸酯齐聚物或聚酯(甲基)丙烯酸酯中的至少一种。
9.根据权利要求7所述的制备方法，其特征在于，所述的树脂B为聚乙烯、聚氯乙烯、环氧树脂、聚氨酯、聚丙烯酸酯、聚甲基丙烯酸甲酯、氟聚合物、聚酰胺、聚酰亚胺、聚硅氧烷、聚碳酸酯、聚砜、聚乙烯醇、聚酯、丙烯腈-丁二烯-苯丙烯的共聚物或其掺合物；所述的功能材料为紫外线吸收剂、抗氧剂或高折射高硬度添加剂中的至少一种。
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