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CN1074006C - 涂覆的塑料基材 - Google Patents

涂覆的塑料基材 Download PDF

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CN1074006C
CN1074006C CN96197584A CN96197584A CN1074006C CN 1074006 C CN1074006 C CN 1074006C CN 96197584 A CN96197584 A CN 96197584A CN 96197584 A CN96197584 A CN 96197584A CN 1074006 C CN1074006 C CN 1074006C
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oxygen
protective coating
plasma polymerization
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CN1199410A (zh
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I－F·胡
P·J·奥科诺
J·C·图
J·H·瑟顿
S·E·巴勒斯
D·J·皮里迪
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Abstract

本发明涉及一种层压材料，包含：a)具有一个表面的基材；b)粘合促进层，该层通过将淀积在基材表面上的有机硅化合物在基本不存在氧的条件下进行第一次等离子体聚合而得到；和c)保护性涂层，该层通过将淀积在粘合层表面上的有机硅化合物在106J/kg至108J/kg的能量密度下且在足以超过化学计算量的氧存在下进行第二次等离子体聚合而得到，从而形成式SiO1.8-2.4C0.3-1.0和H0.7-4.0的硅聚合物。该涂层为基材提供耐磨性和耐溶剂性，且粘合促进层防止涂层与基材剥离。涂覆的塑料基材可用于液晶显示装置中代替玻璃。

Description

涂覆的塑料基材
本发明涉及涂覆的塑料基材，其一个实施方案可用于液晶显示装置中。该涂层保护基材不受磨蚀和溶剂降解。
目前，需要具有改进强度的更薄且重量更轻的液晶显示器。这一需要由以下事实表明：昂贵的便携式装置因值10分的玻璃的破裂而遭到毁灭性破坏。此外，某些装置中发生的所有场破坏半数以上是由这种破裂引起的。由于具有优异的柔韧性和抗冲击性，塑料基材为在液晶显示装置(LCD)中用作基材的玻璃的替代品。塑料基材也可通过改进制造方法中的产量而提供比玻璃基材更为经济的优点。
然而，不能因改进强度而牺牲玻璃基材所固有的优点。若选择塑料作为基材，理想的是将其设计成具有一定的物理性能，包括a)光学透明度；b)在加工该显示器所需的温度，通常至少160℃下的稳定性；c)低的双折射；d)对显示器生产中所用化学试剂的耐性；e)光稳定性；f)耐划伤性；g)硬度和h)电阻率。
因此，需要发现一种对用于LCD和其他用途的玻璃的替代品，它克服了玻璃基材的上述缺陷。
图1为9,9-双(4-羟苯基)芴和双酚A的共聚碳酸酯的应力光学系数(SOC)与玻璃化转变温度(Tg)的图。
在第一方面，本发明为一种层压材料，包括：
a)具有一个表面的塑料基材；
b)粘合促进层，该层通过将淀积在基材表面上的有机硅化合物在足以产生用于粘合的界面化学反应的能量水平下且在基本不存在氧的条件下进行第一次等离子体聚合而得到；和
c)保护性涂层，该层通过将淀积在粘合层表面上的有机硅化合物在106J/kg至108J/kg的能量密度下且在比步骤(b)中氧浓度高的氧存在下进行第二次等离子体聚合而得到。
在第二方面，本发明为一种层压材料，包括：
a)具有一个表面且厚度为0.1-10mm的塑料基材；
b)粘合促进层，该层通过将淀积在基材表面上的四甲基二硅氧烷在基本不存在氧的条件下进行等离子体聚合得到且厚度为1000-2000A；
c)保护性涂层，该层通过将淀积在粘合促进层表面上的四甲基二硅氧烷在106J/kg至108J/kg的能量密度且在足以超过化学计算量的氧存在下进行等离子体聚合而得到，从而形成式SiO1.8-2.4C0.3-1.0和H0.7-4.0的有机硅化合物，该化合物含有滞留的水和至少一种下列官能基团：Si-O-Si-,-Si-CH2-,-Si-H或-Si-OH；其中该保护性涂层厚度不低于0.1μm且不超过2μm；和
d)SiOx层，该层为淀积在保护性涂层表面上的四甲基二硅氧烷在超过化学计算量的氧存在下且在至少4倍于用于形成保护性涂层的能量密度的能量密度下等离子体聚合得到的层，其中SiOx层的厚度不低于0.1μm且不大于1μm。
本发明的层压材料能耐磨和耐溶剂，这是因为存在层状涂层。此外，该涂层因存在粘合促进层而耐剥离。
用于本发明层压材料的基材可以是热塑性或热固性材料。合适的热塑性材料实例包括聚乙烯，聚丙烯，聚苯乙烯，聚乙酸乙烯酯，聚乙烯醇，聚乙烯醇缩醛，聚甲基丙烯酸酯，聚丙烯酸，聚醚，聚酯，聚碳酸酯，纤维素树脂，聚丙烯腈，聚酰胺，聚酰亚胺，聚氯乙烯，含氟树脂和聚砜。热固性材料的实例为环氧树脂和脲三聚氰胺树脂。
基材的厚度与应用有关，但优选不低于0.1mm，更优选不低于0.3mm，最优选不低于0.5mm，且优选不超过10mm，更优选不超过5mm，最优选不超过2mm。
基材的表面首先用粘合促进层涂覆，该层通过将淀积在基材表面上的有机硅化合物进行等离子体聚合而形成。有机硅化合物等离子体聚合以生产粘合促进层在足以产生用于粘合的界面化学反应的能量水平下进行，优选在5×107J/kg至5×109J/kg的能量水平下。粘合促进层在不存在或基本不存在载气如氧的条件下制备。术语“基本不存在氧”在本文中用来表示等离子体聚合方法中氧的存在量不足以氧化有机硅化合物中的所有硅和碳。类似地，术语“超过化学计算量的氧”在本文中用来表示所存在的氧的总摩尔数大于有机硅化合物中硅和碳的总摩尔数。
粘合促进层的厚度与应用有关，优选不低于50，更优选不低于500，最优选不低于1000，且优选不超过10000，更优选不超过5000，最优选不超过2000。
然后用保护性涂层涂敷粘合促进层，该保护性涂层通过将淀积在粘合促进层表面上的有机硅化合物在106J/kg至108J/kg的能量密度且在高于形成粘合促进层所用的氧浓度下等离子体聚合而得到。优选保护性涂层在超过化学计算量的氧存在下形成。
基材的保护性涂层厚度主要取决于涂层以及基材的性能，但通常足够厚以赋予基材耐溶剂性。优选涂层厚度不低于0.1μm，更优选不低于0.4μm，最优选不低于0.8μm，且不大于10μm，更优选不大于5μm，最优选不大于2μm。
层压材料可非必要地包含SiOx层，该层通过将淀积在保护性涂层表面上的有机硅化合物在超过化学计算量的氧存在下且在至少两倍，更优选至少4倍，最优选6倍于用来形成保护性涂层的能量密度的能量密度下进行等离子体聚合得到。该层方便地称作SiOx层。然而，该SiOx层也可含有氢和碳原子。该SiOx层的厚度通常低于保护性涂层的厚度，且优选不低于0.01μm，更优选不低于0.02μm，最优选不低于0.05μm，且优选不大于5μm，更优选不大于2μm，最优选不大于1μm。
理想的是用交替的保护性涂层和SiOx层涂覆粘合促进层。保护性涂层与SiOx层的厚度比优选不低于1∶1，更优选不低于2∶1，且优选不大于10∶1，更优选不大于5∶1。
有机硅聚合物涂层由有机硅化合物如硅烷，硅氧烷或硅氮烷制备。硅烷的实例包括二甲氧基二甲基硅烷，甲基三甲氧基硅烷，四甲氧基硅烷，甲基三乙氧基硅烷，二乙氧基二甲基硅烷，甲基三乙氧基硅烷，三乙氧基乙烯基硅烷，四乙氧基硅烷，二甲氧基甲基苯基硅烷，苯基三甲氧基硅烷；3-缩水甘油氧丙基三甲氧基硅烷，3-甲基丙烯酰氧丙基三甲氧基硅烷，二乙氧基甲基苯基硅烷，三(2-甲氧基乙氧基)乙烯基硅烷，苯基三乙氧基硅烷和二甲氧基二苯基硅烷。硅氧烷的实例包括四甲基二硅氧烷(TMDSO)和六甲基二硅氧烷。硅氮烷的实例包括六甲基硅氮烷和四甲基硅氮烷。
有机硅聚合物涂层优选通过US 5,298,587中所公开的等离子体增强的化学蒸汽淀积(PECVD)技术施加。
在本发明的一个方面，层压材料呈光学透明且包含一种应力光学系数(SOC)为-2000至+2500 Brewsters和Tg(由差示扫描量热法测定)优选为160-270℃的基材。优选基材的SOC不低于-1000，更优选不低于-500，最优选不低于-100，且不大于1000，更优选不大于500，最优选不大于100 Brewsters。基材的Tg优选不低于180℃，更优选不低于190℃，最优选不低于200℃，至不大于250℃，更优选不大于240℃，最优选不大于230℃。术语“光学透明”在本文中用来表示根据ASTMD-1003测得基材的总透光率为至少80％，优选至少85％。
对于液晶显示应用，基材优选包含碳酸酯聚合物，该聚合物可以为均聚物或共聚物或具有所需SOC和Tg的共混物。优选基材包含碳酸酯聚合物，它为芳族多醇，更优选芳族二醇与碳酸酯前体的反应产物。芳族二醇的代表性实例包括邻苯二酚，间苯二酚，氢醌，二羟基萘，二羟基蒽，双(羟芳基)芴，二羟基菲，二羟基联苯和双(羟苯基)丙烷。优选芳族二醇包括9,9-双(4-羟苯基)芴和双酚A。
适用于制备这些碳酸酯聚合物的碳酸酯前体在本领域是众所周知的且包括碳酸衍生物，光气，卤代甲酸酯，或碳酸酯如碳酸二甲酯或碳酸二苯酯。碳酸酯聚合物可以由多种聚合方法制备，如界面方法，溶液方法或熔融方法，所有这些在本领域是众所周知的。
优选基材包含的碳酸酯聚合物含有二羟基芳基芴单体和双酚单体，更优选9,9’-二羟基芳基芴和双酚A的重复单元。9,9’-二羟基芳基芴与双酚A的单元比优选不低于30∶70，更优选不低于40∶60，且优选不大于90∶10，更优选不大于70∶30。
图1图示说明多种9,9-二羟苯基芴(BHPF)和双酚A(BPA)的共聚碳酸酯的SOC和Tg变化。该图表明BHPF/BPA为30∶70至90∶10mol％的共聚碳酸酯的SOC和Tg尤其适于液晶显示器应用中。最佳SOC(SOC等于0)发生在BHPF/BPA比为70∶30，而最佳Tg发生在稍低的比率下。幸运的是，Tg的调整可以在不显著改变SOC的情况下进行，例如通过将酯单元掺入碳酸酯聚合物中以制备碳酸酯/酯共聚物，或通过将聚酯和/或碳酸酯/酯共聚物与碳酸酯聚合物共混。掺入碳酸酯聚合物中的酯单元浓度或与碳酸酯聚合物共混的聚酯和/或碳酸酯/酯共聚物量足以达到所需的Tg，而不显著降低其他物理性能。
优选酯单元为脂族或芳族二酸或二酰氯的反应产物。脂族二酸或二酰氯优选为C3-12二酸或二(酰氯)，更优选C4-8二酸或二(酰氯)，最优选己二酸，己二酰氯，丁二酸或丁二酰氯。芳族二酸优选为对苯二甲酸，对苯二甲酰氯，间苯二甲酸，间苯二甲酰氯，2,6-萘二甲酸，或2,6-萘二酰氯。优选基材中酯单元的浓度基于碳酸酯单元和酯单元总摩尔数为10-50mol％。
以下实施例仅用于说明，而不是用来限制本发明范围。除非另有说明，所有百分比均为重量∶重量。
实施例1-SiOxCyHz涂覆的碳酸酯聚合物的制备
A．制备60∶40(摩尔比)的BHPF/BPA共聚碳酸酯
按如下制备60mol％9,9-双(4-羟苯基)芴(BHPF)和40mol％双酚A(BPA)的共聚碳酸酯。向100ml高压反应器(装有活塞)中加入BPA(0.913g,4.0mmol),BHPF(2.102g,6.0mmol)，叔丁酚(0.045g,0.30mmol)，50％NaOH水溶液(2.0g,25.0mmol)和水(16.14g)。用氮气吹扫反应器。将氮气吹过反应器内部空间10分钟，然后盖紧活塞。将密封的反应器放入水浴(69-71℃)中并搅拌溶液。单体溶解后将光气在二氯甲烷中的溶液(20.08g,6.65％溶液，13mmol)使用一个25ml气密注射器加到搅拌的混合物中。取出注射器并振摇反应混合物30秒。通过隔膜由注射器加入第二份50％NaOH(2.0g,25mmol)。
振摇混合物1分钟，然后用注射器加入额外的二氯甲烷(11.17g)，再加入4-二甲氨基吡啶(0.6ml1％水溶液)。振摇该混合物1分钟，然后将反应器在冰浴中振荡。打开反应器，吸移水相。有机相用1N HCl洗1次并用水洗两次，然后通过蒸发除去溶剂。所得共聚碳酸酯的Tg为230℃(PC-230)。该通用程序用于制备额外量的共聚碳酸酯，并将它们注塑成127×127×1.6mm的板。
B．制备BHPF/BPA共聚碳酸酯共混物
通过干混以A部分所述方式制备的共聚碳酸酯(56重量份)与双酚A聚碳酸酯(44重量份)制备Tg为190℃的BHPF/BPA共聚碳酸酯共混物(PC-190)。将所得混合物使用30mmWerner-Pfleiderer挤出机(进料区设在200℃，剩下4个区设在310℃)挤塑并造粒。
C．PECVD涂层在碳酸酯聚合物基材上的淀积
高度交联的有机硅涂层(通式SiOxCyHz)的淀积在装有US5,320,875的图1、2和3中所示喷淋头平面磁控管阴极的PECVD不锈钢箱中进行。将A或B部分制备的板(PC-230或PC-190)放入阴极上方3.2cm处，并围绕该阴极的中心。首先用1000-1500厚的等离子体聚合的TMDSO粘合层涂敷该板。将TMDSO(4sccm)通过喷淋头阴极供入室中。该喷淋头的气体入口孔均匀分布在磁控管阴极的等离子体环上。气体入口的这种构型通过使分子流过最强的等离子体区域而达到最大程度的四甲基二硅氧烷分解。用MKS Inc.的Model 1152蒸气流控制器控制TMDSO蒸气流，并用ENI电源(Model PlasmaLoc2)提供等离子体能量。在粘合促进层淀积过程中加于等离子体上的能量为500瓦(W),40Khz，相当于6.3×108J/kg的能量密度。室内基础压力低于1m Torr。加工压力大约为27mTorr。
通过将40sccmO2(流速由Model 1160MKS气流控制器控制)和4sccm TMDSO混合物供入室中而将高度交联的有机硅涂层淀积到粘合层上。在淀积过程中加于等离子体上的能量为40W,40Khz，对应于2.9×107J/kg的能量密度。
涂敷板对N-甲基吡咯烷酮(NMP)的耐性通过将1滴NMP加到涂敷表面上，然后使其在用水漂洗前保留5分钟而测定。目测无浑浊表明对NMP具有耐性。对于PC-230,1.0,1,2,1.4和1.6μm厚的涂层赋予耐溶剂性。对于PC-190,1.2,1.4和1.6μm厚的涂层赋予耐溶剂性。
实施例2-SiOxCyHz/SiOx涂敷的碳酸酯聚合物的制备
将实施例1中制得的具有粘合促进层的板(PC-190或PC-230)用SiOx和有机硅涂层交替涂敷。各SiOx涂层厚0.072μm，各高度交联的有机硅涂层厚0.262μm。第一层SiOx涂层通过将40sccmO2(流速由Model1160MKS气流控制器控制)和4sccm TMDSO混合物供入室中而施于板上。在淀积过程中加于等离子体上的能量为250W,40Khz，对应于1.8×108J/kg的能量密度。然后使用实施例1中所述条件施加第一层有机硅涂层。施加第二层SiOx涂层，然后是第二层有机硅涂层，再后是第三层SiOx涂层，最后是第三层有机硅涂层。涂层总厚度为1.0μm。PC-190和PC-230样品用这种交替涂敷技术都能耐NMP。

Claims (9)

1．一种层压材料，包含：
a)具有一个表面的塑料基材；
b)粘合促进层，该层通过将淀积在基材表面上的有机硅化合物在5×107J/kg至5×109J/kg的能量水平下且在基本不存在氧的条件下进行第一次等离子体聚合而得到；和
c)保护性涂层，该层通过将淀积在粘合层表面上的有机硅化合物在106J/kg至108J/kg的能量密度下且在比步骤(b)中氧浓度高的氧存在下进行第二次等离子体聚合而得到。
2．权利要求1的层压材料，还包含SiOx层，该层通过将淀积在保护性涂层表面上的第三种有机硅化合物在超过化学计算量的氧存在下且在至少两倍于用于形成保护性涂层的能量密度的能量密度下进行等离子体聚合得到。
3．权利要求2的层压材料，还包含交替的保护性涂层和SiOx层。
4．权利要求1-3中任一项的层压材料，其中等离子体聚合的有机硅聚合物各自独立地选自包括二甲氧基二甲基硅烷，甲基三甲氧基硅烷，四甲氧基硅烷，甲基三乙氧基硅烷，二乙氧基二甲基硅烷，甲基三乙氧基硅烷，三乙氧基乙烯基硅烷，四乙氧基硅烷，二甲氧基甲基苯基硅烷，苯基三甲氧基硅烷，3-缩水甘油氧丙基三甲氧基硅烷，3-甲基丙烯酰氧丙基三甲氧基硅烷，二乙氧基甲基苯基硅烷，三(2-甲氧基乙氧基)乙烯基硅烷，苯基三乙氧基硅烷，二甲氧基二苯基硅烷，四甲基二硅氧烷，六甲基二硅氧烷，六甲基硅氮烷和四甲基硅氮烷。
5．权利要求1-3中任一项的层压材料，其中等离子体聚合的有机硅聚合物各自为四甲基二硅氧烷。
6．权利要求1-3中任一项的层压材料，其中基材为包含碳酸酯前体与芳族二醇的反应产物的重复单元的碳酸酯聚合物。
7．权利要求6的层压材料，其中芳族二醇包括邻苯二酚，间苯二酚，氢醌，二羟基萘，二羟基蒽，双(羟芳基)芴，二羟基菲，二羟基联苯，或双(羟苯基)丙烷。
8．权利要求7的层压材料，其中芳族二醇包括9,9-双(4-羟苯基)芴和双酚A且9,9-双(4-羟苯基)芴与双酚A的重复单元比为40∶60-70∶30。
9．一种层压材料，包含：
a)具有一个表面且厚度不低于0.1mm且不大于10mm的塑料基材；
b)粘合促进层，该层通过将淀积在基材表面上的四甲基二硅氧烷在5×107J/kg至5×109J/kg的能量水平下、且在基本不存在氧的条件下进行等离子体聚合得到且厚度为1000-2000；
c)保护性涂层，该层通过将淀积在粘合促进层表面上的四甲基二硅氧烷在106J/kg至108J/kg的能量密度且在相对于四甲基二硅氧烷足以超过化学计算量的氧存在下进行等离子体聚合而得到，从而形成式SiO1.8-2.4C0.3-1.0和H0.7-4.0的有机硅化合物，该化合物含有滞留的水和至少一种下列官能基团：Si-O-Si-,-Si-CH2-,-Si-H或-Si-OH；其中该保护性涂层厚度不低于0.1μm且不超过2μm；和
d)SiOx层，该层为淀积在保护性涂层表面上的四甲基二硅氧烷在超过化学计算量的氧存在下且在至少4倍于用于形成保护性涂层的能量密度的能量密度下等离子体聚合得到的层，其中SiOx层的厚度不低于0.1μm且不大于1μm。
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