CN104530832A - 在其表面上具有促进油墨粘附的塑料施釉体系 - Google Patents

在其表面上具有促进油墨粘附的塑料施釉体系 Download PDF

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CN104530832A
CN104530832A CN201410601762.7A CN201410601762A CN104530832A CN 104530832 A CN104530832 A CN 104530832A CN 201410601762 A CN201410601762 A CN 201410601762A CN 104530832 A CN104530832 A CN 104530832A
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luffer boards
adhesion promotor
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S·戈兰蒂
K·D·韦斯
J·纳
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Abstract

本发明涉及在其表面上具有促进油墨粘附的塑料施釉体系。本发明公开了包括基本上透明的基材的汽车窗板，该基材具有布置在其上的保护性涂层体系和涂覆到该保护性涂层体系上的导电性油墨。该导电性油墨的配方包括粘合促进剂并且适合于在该粘合促进剂的存在下附着于该保护性涂层的表面。

Description

在其表面上具有促进油墨粘附的塑料施釉体系
本申请是于2006年6月16日提交的PCT申请PCT/US2006/023626的中国国家阶段申请，申请号为200680021775.0、题目为“在其表面上具有促进油墨粘附的塑料施釉体系”的分案申请。
发明背景
用来为塑料汽车窗体提供装饰性功能(黑内障、渐隐、徽标等)或导电性功能(除霜器、天线等)的油墨通常直接地涂覆到窗体表面上并随后用保护性(耐候、耐磨)涂层外涂覆。然而，这可能导致在印刷图像的边缘产生光学扭曲。例如，沿着构成除霜器栅极图案的每一栅极线，这种光学扭曲可能影响驾驶员的视野。
如图1的部件10所示，这种光学扭曲的起因认为与部件10的整个基材12上和印刷图像14和部件10的其余表面之间的界面处产生的涂层厚度差异有关。如图1所示，接近图像部分界面的涂层体系(称为层1-3)的厚度(A厚度)可能显著地大于其余部分上方的涂层厚度(B厚度)。不同涂层之间的折射指数差异引起图1中标记为光路A和光路B的两个区域中光被不同地折射。因此，人眼将发觉印刷图像附近的光学扭曲。
考虑到现有技术中的上述缺陷及其它限制，认为仍需要印刷塑料窗板，该窗板在整个窗体范围内不显示，或至少最小化光学扭曲。
发明概要
为了克服现有技术中的不足，本发明提供如下消除光学扭曲的构造：将图像印刷到涂层体系的表面上而不是直接印刷到部件上。然而，涂层的表面性质不同于塑料的表面性质，因此引起遇到所涂覆的油墨对涂覆部件的表面的粘附性问题。在本发明的另一个方面中，为了增强油墨对涂覆到塑料基材上的施釉体系的表面的粘附性，对油墨配方作出改进。
当结合附图考虑以下描述和所附权利要求书时，本发明的其它目的、特征和优点将变得显而易见。
附图简述
图1是现有技术镶板的示意图，描述在它们之上涂覆了保护性涂层体系之后的塑料基材(B)和具有印刷图像的塑料基材(A)之间的光路差异；
图2是根据本发明一个实施方案的塑料施釉体系的示意图；和
图3是所测量的薄片电阻率(毫欧姆/平方)对在印刷之前添加到导电性油墨中的粘合促进剂(A)的量的曲线图。
发明详述
如下面进一步论述的那样，已经发现，将一类粘合促进剂添加到装饰性或导电性油墨配方中可以提供粘附性增强，允许此类油墨沉积到塑料施釉体系的表面上。在一个实施方案中，如图2所示，镶板110包括透明塑料基材114，在该基材114上按顺序涂覆了涂层体系113和印刷图像112。将粘合促进剂与限定印刷油墨图像112的油墨混合。在将印刷油墨图像112涂覆在塑料基材114的涂层体系113上之前，进行粘合促进剂与油墨的混合。该粘合促进剂充当涂釉基材115的表面和油墨中的聚合物树脂或存在于油墨内的颜料上的有机表面处理剂之间的偶联剂。
为了充当不同界面表面之间的偶联剂，粘合促进剂的第一端能够将涂釉基材115的表面的分子结构偶联。涂釉基材115具有耐磨表面，该耐磨表面通常是来自硅酮硬涂层的硅氧烷结构或来自SiwOxCyHz层的沉积的玻璃状结构。对这类表面的粘附可能经由离子、共价或氢键机理，以及经由范德华力建立。各种含羟基、甲氧基或乙氧基的硅烷已知有效地附着于含较高氧度的无机表面。
除了附着于基材114的涂层113之外，粘合促进剂还与油墨的固体结构发挥类似的作用。在这个实施方案中，粘合促进剂包括第二端，该第二端能够附着于油墨配方中的颜料或聚合物树脂。导电性油墨中的主要颜料可能性质上是金属的，如银、铜或氧化银。通常存在于装饰性油墨中的颜料可以是石墨或炭黑，以及二氧化钛的形式。既存在于导电性油墨又存在于装饰性油墨配方中的聚合物树脂可以是聚碳酸酯基、聚酯基、丙烯酸系树脂基或聚氨酯基的。
评价了与导电性油墨一起使用的十四种粘合促进剂(A至N)，如下表1所示。将每种粘合促进剂添加到导电性银油墨配方，如从ParelecInc.获得的油墨(EXA-101，New Jersey)中。在数分钟的期间内添加每种粘合促进剂，且对整个混合物进行搅拌处理以获得均匀性。添加到银油墨中的粘合促进剂的量为3wt％(在筛分试验中)至16wt％(在一些优化试验中)。使用常规丝网印刷技术和设备将油墨沉积到涂釉基材115的表面上。然而，其它技术，如通用丝网印刷、膜图像转印、机器人分配和掩模和喷雾将是适合的沉积方法，并没有脱离本发明的范围和精神。
表1
其上沉积有油墨涂釉基材115包括透明的聚碳酸酯基材114，该基材具有由硅酮硬涂层(Exatec LLC，SHP-9X丙烯酸底漆&SHX硅酮硬涂层)组成的保护性涂层113，有或没有通过等离子增强化学气相沉积(PECVD)沉积的玻璃状层。(该玻璃状层/PECVD体系可从Exatec LLC以900施釉体系商购。)在印刷到除霜器栅极图案中的涂釉基材的表面上之后，根据制造商的优选程序在129℃下将该银油墨固化大约60分钟。
使用本领域中已知的标准十字划线胶带剥离试验(ASTMD3359-95)进行印刷银栅极图案的粘附试验。尽管这一试验的实际的通过和失败标准通常与最终顾客的意见一致，但是在胶带扯下之后其余的银糊剂的百分率理论上将大于95％。对于试验目的，假定大于80％粘附将是可接受的(通过)，其中大于大约95％粘附是优选的。对于含3％各种粘合促进剂(A-N)的银油墨的初始粘附保留获得的结果在表2中显示出。
表2
如表2所示，具有八种粘合促进剂(A-E、J&M-N)的油墨配制通过了该试验，而其余六种粘合促进剂(F-I、K-L)失败。比较地，不含粘合促进剂油墨配方“O”的印刷图像发现在这一试验过程中完全地剥离，具有0％粘附和保留。通过该试验的所有粘合促进剂发现既通过了对SHX涂层的硅氧烷表面的粘附试验又通过了对900施釉体系的玻璃状表面的粘附试验。通过了该试验的每种粘合促进剂除油墨配方“B”之外发现满足大于大约95％保留的优选标准。通过该试验的粘合促进剂的一般家族包括异氰酸基、氰基、巯基和氨基官能团。粘合促进剂中的烃链的长度可以有不同并且可以提供一些对于克服空间阻碍而言的优点，所述空间阻碍阻碍偶联剂的两端与它们的目标官能团连接。发明人已经发现含异氰酸基和氰基的粘合促进剂与含巯基和氨基的粘合促进剂相比显示更坚固的粘附性能，因此是优选的。
由各种粘合促进剂显示的粘附性能的坚固度通过将印刷基材浸没在65℃水中数天来评价。使用此前描述的粘附试验在热水浴中1天后和在热水浴中4天后研究印刷图像112对涂釉基材115的表面的粘附。将6wt％粘合促进剂(A)添入银油墨中获得的试验数据的实例在表3中示出。由四个独立试验中的四种试验结果表示的所有印刷银图像被发现即使在热水中浸没四天之后仍通过了粘附交叉划线、带拉扯试验。因此，在使用这种粘合促进剂(A)后观察到的粘附改进显著大于不含任何粘合促进剂(O)的印刷图像在表2中观察到在0天(初始粘附)的粘附损失。
表3
发明人进一步发现添加到导电性油墨配方中的粘合促进剂的量不会影响由该印刷油墨显示的薄片电阻率水平，只要它在该油墨配方中维持少于大约6wt％。添加多于大约6wt％粘合促进剂到油墨配方中将引起由该印刷油墨显示的薄片电阻率的增加。薄片电阻率的这种增加与导电性的下降有关并因此如果印刷图像将用作除霜器栅极或天线的话则是不希望的。为含各种水平的粘合促进剂(A)的印刷图像测量的粘附数据以及相应的薄片电阻率数据在表4中给出。表4
粘合促进剂A
直接涂覆到聚碳酸酯上的没有粘合促进剂的银油墨获得的标准薄片电阻率值约为5毫欧姆/平方，由表4中的油墨(0)表示。试验#5和试验#6都发现提供类似的结果。涂覆到涂釉基材(PECVD)上的含粘合促进剂(A)的银油墨的薄片电阻率发现保持大约5-6毫欧姆/平方直到存在于该油墨中的粘合促进剂的百分率增加到大约8％。图3提供了薄片电阻率对粘合促进剂(A)的百分率的曲线图。如图3所示，大约6％的含量是可以使用而不引起印刷图像的薄片电阻率开始显著增加的最大粘合促进剂含量。
在另一个实施方案中，将不同量的粘合促进剂(A)如表5B所示以小于100:1且大于大约50:50的重量比添加到具有以下组成的装饰性油墨中：大约5-34wt％由聚酯油墨(8452，Nazdar，Kansas)获得的聚酯树脂和大约1-13wt％由聚碳酸酯油墨(HTR-952，Proell，Germany)获得的聚碳酸酯树酯。该装饰性油墨还包括大约0.1-5wt％芳族异氰酸酯催化剂，其余的部分是溶剂混合物(阻滞剂)。
表5B
用来制备表5B中所示的每一个试验的配方的程序可以描述如下：(1)将油墨称出加入其中混合和搅拌了阻滞剂和粘合促进剂(A)10分钟的容器，接着添加催化剂。(2)将该油墨混合物充分地搅拌另外15分钟，然后经由丝网印刷涂覆到涂釉基材上。小心防止产生大量或许多气泡，它们可能导致泡沫的形成。以制剂的总重量计，所添加的粘合促进剂的水平为大约5-25％。各个试验中的每个固化油墨层的厚度在表6中给出。
表6
对在65℃的水中10天后的用装饰性油墨印刷的涂釉基材(900体系)进行的交叉划线粘附试验的结果在表7中给出。对于装饰性油墨，添加粘合促进剂允许印刷图像能经受住暴露在浸水试验下大于3天，如由试验7-9所示。比较地，不包含粘合促进剂的印刷图像(对照)和含大于大约25％粘合促进剂的图像(试验10)发现在3天水浸之后没有通过粘附试验。
本发明的装饰性油墨可以是丙烯酸系树脂油墨、丙烯酸系树脂/硝化纤维素树脂油墨、硝化纤维素/聚酰胺树脂油墨、乙烯树脂/丙烯酸系树脂油墨、醇酸树脂油墨、乙烯树脂/聚酯树脂油墨、乙烯树脂油墨、聚碳酸酯树酯油墨、聚酯树脂油墨或含另一种有机树脂的油墨，以及它们的树脂的混合物、共聚物或共混物。含聚酯、聚碳酸酯或丙烯酸系树脂或它们的混合物、共混物或共聚物的油墨是优选的。油墨可以在性质上分为单组分或双组分油墨。
表7
试验7 Center 通过 通过 通过 通过 通过 通过
Edge 通过 通过 通过 通过 通过 通过
试验8 Center 通过 通过 通过 通过 通过 通过
Edge 通过 通过 通过 通过 通过 通过
试验9 Center 通过 通过 通过 通过 通过 通过
Edge 通过 通过 通过 通过 通过 通过
试验10 Center 通过 通过 通过 通过 失败 失败
Edge 通过 通过 通过 通过 失败 失败
装饰性油墨中的着色剂颜料优选是炭黑，但是也可以使用其它的无机和有机着色颜料。这些着色剂颜料可以包括但不局限于炭黑、铜酞菁蓝、二嗪紫、喹吖啶酮品红、偶氮二芳基化物黄、金红石二氧化钛(白色)、二萘嵌苯红、钼橙、黄色氧化铁、铬绿色氧化物或镉橙。特殊效应颜料，如珠光颜料和金属薄片可以引入配方中。
异氰酸酯催化剂(如果使用)优选是芳族多异氰酸酯，如NB-70催化剂(Nazdar Inc.,Kansas)。将这种特定的异氰酸酯分散在丙二醇甲醚乙酸酯(40％，还称作PM乙酸酯)中，但是也可以使用其它溶剂。异氰酸酯也可以是其它芳族或脂族二异氰酸酯，如聚合物六亚甲基二异氰酸酯(HMDI)、异佛尔酮二异氰酸酯(IPDI)、2,6-甲苯基二异氰酸酯(TDI)、二苯甲烷二异氰酸酯(MDI)或二甲苯二异氰酸酯(XDI)等。
任选的分散剂可用来确保颜料充分地分散。这一任选的分散剂可以是离子或非离子分散剂。这些表面活性剂包括，但不限于金属皂、磺酸酯、磷酸酯、脂肪酸酯、氟代脂族聚合物酯、钛酸酯或锆酸酯或铝酸酯偶联剂、有机改性的聚硅氧烷、聚(氧化烯)的嵌段共聚物和商业专利性表面活性剂，如和hyperdispersants(ICI美国,Inc.)。任选的表面活性剂优选是有机改性的聚硅氧烷，还称作聚醚硅氧烷共聚物，如Wet KL 245(Goldshmidt Chemical Corp.,Virginia)。
为了确保印刷图像的不透明性，可以将任选的不透明性增强填料用于装饰性油墨。这些任选的填料可以是性质上无机的填料，如氧化铝、二氧化硅、二氧化钛、硅酸镁(滑石)、硫酸钡、碳酸钙、硅酸铝(粘土)、硅酸钙(硅灰石)、硅酸铝钾(云母)、金属薄片等，或性质上有机的填料，如炉黑、槽黑和灯黑等。高度折射性填料，如二氧化钛优选用于增加不透明性，由于它们小于1.0微米的小平均颗粒尺寸。例如，平均颗粒尺寸为0.36微米的二氧化钛可作为R-706(DuPont Titanium Technologies，Delaware)获得。
导电性油墨可以由分散在聚合物基体中的导电性颗粒、薄片、粉末或它们的混合物和共混物组成。聚合物基体优选是环氧树脂、聚酯树脂、聚乙酸乙烯酯树脂、聚氯乙烯树脂、聚氨酯树脂或和它们的混合物和共聚物。存在于油墨、糊剂或油漆中的导电性颗粒、薄片或粉末可以由金属组成，所述金属包括但不限于银、铜、锌、铝、镁、镍、锡或它们的混合物和合金，以及任何金属化合物，如金属二硫属化物。这些导电性颗粒、薄片或粉末也可以是本领域技术人员已知的任何导电性有机材料，如聚苯胺、无定形碳和碳-石墨。
充当导电性油墨、糊剂或油漆中的载色剂的任何溶剂可以是为有机树脂提供溶解性的任何有机载体的混合物。金属油墨、糊剂或油漆的实例包括可从DuPont Electronic Materials,Research TrianglePark,NC(5000Membrane Switch,5029Conductor Composition,5021Silver Conductor和5096Silver Conductor)，AchesonColloids,Port Huron,MI(PF-007和Electrodag SP-405)，MethodeEngineering,Chicago,IL(31-1A Silver Composition、31-3A SilverComposition)，Creative Materials Inc.,Tyngsboro,MA(118-0292k Silver)和Advanced Conductive Materials,Atascadero,CA(PTF-12)商购的银-填充的组合物。
其上整体形成了涂层113和印刷图像112的基材114可以是任何透明的由热塑性聚合物树脂组成的镶板。本发明的热塑性树脂包括但不限于聚碳酸酯树酯、丙烯酸系树脂、聚芳酯树脂、聚酯树脂和聚砜树脂，以及它们的共聚物和混合物。透明的镶板可以通过使用本领域技术人员已知的任何技术，如模塑、热成形或挤出形成窗体形状。
涂覆到基材114上的并且其上印刷了导电性或装饰性油墨112的保护性涂层113包括但不限于硅酮硬涂层、聚氨酯涂层、丙烯酸树脂涂层和"玻璃状"涂层等。还可以使用由丙烯酸底漆&硅酮中间层或外涂有"玻璃状"或玻璃薄膜面漆的聚氨酯中间层组成的层状涂层体系。保护性涂层的实例包括丙烯酸底漆(SHP401，GE Silicones,Waterford,NY)和硅酮硬涂层(AS4000,GE Silicones)以及通过等离子增强化学气相沉积(PECVD)沉积的SiOxCyHz“玻璃状”薄膜的组合。层状涂层体系的实例是由Exatec LLC(Wixom,Michigan)作为用于塑料施釉的500&900提供的丙烯酸系树脂/硅酮“玻璃状”涂层体系。保护性涂层113可以通过浸涂、流涂、喷涂、等离子增强化学气相沉积(PECVD)或本领域技术人员已知的其它技术施涂。
虽然已经根据优选的实施方案描述了本发明，但是当然应当理解，本发明不限于此，因为本领域技术人员可以作出修改，尤其是根据上述教导作出修改。

Claims (8)

1.汽车窗板，该窗板包括：
基本上透明的塑料基材；
布置在该基材表面上的保护性涂层体系；和
涂覆到该保护性涂层体系上的导电性油墨，该导电性油墨包括粘合促进剂，该导电性油墨适合于在该粘合促进剂存在时附着于该保护性涂层的表面而在没有该粘合促进剂时不附着于该保护性涂层的表面；其中该导电性油墨由具有导电性颗粒、薄片、粉末或其混合物中的一种的聚合物基体组成；
其中该粘合促进剂以小于6wt％的量存在于导电性油墨中；和
其中该粘合促进剂是具有第一和第二端的分子，每一端具有含反应性官能团的硅烷偶联剂。
2.权利要求1的窗板，其中所述偶联剂的反应性官能团由以下基团组成：在该分子的一端，为羟基和烷氧基官能团之一，在该分子的另一端，为巯基、异氰酸基、氰基和氨基官能团之一。
3.权利要求2的窗板，其中所述偶联剂的反应性官能团由以下基团组成：在该分子的一端，为羟基和烷氧基官能团之一，在该分子的另一端，为异氰酸基和氰基官能团之一。
4.权利要求1的窗板，其中所述聚合物基体是环氧树脂、聚酯树脂、聚乙酸乙烯酯树脂、聚氯乙烯树脂、聚氨酯树脂或它们的混合物中的一种。
5.权利要求1的窗板，其中所述导电性油墨包含以下组分中的至少一种：银、铜、锌、铝、镁、镍、锡、金属二硫属化物、聚苯胺、无定形碳和石墨。
6.权利要求1的窗板，其中所述保护性涂层体系包含以下物质之一：硅酮硬涂层、聚氨酯涂层、丙烯酸树脂涂层、聚氨酯-丙烯酸酯共聚物玻璃薄膜涂层或它们的混合物。
7.权利要求1的窗板，其中所述保护性涂层体系包括丙烯酸系树脂/硅酮/玻璃-薄膜涂层体系。
8.权利要求1的窗板，其中所述保护性涂层体系包括丙烯酸底漆、硅酮硬涂层和通过等离子增强化学气相沉积而沉积的SiOxCyHz玻璃薄膜。
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US7811656B2 (en) 2010-10-12
KR101321262B1 (ko) 2013-10-30
KR20080025737A (ko) 2008-03-21
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