CN101909873B - 用于阳光控制及其它用途的红外线反射膜 - Google Patents
用于阳光控制及其它用途的红外线反射膜 Download PDFInfo
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- CN101909873B CN101909873B CN200880122804.1A CN200880122804A CN101909873B CN 101909873 B CN101909873 B CN 101909873B CN 200880122804 A CN200880122804 A CN 200880122804A CN 101909873 B CN101909873 B CN 101909873B
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Abstract
本发明提供的阳光控制膜包括能透射可见光的柔性载体、第一成核氧化物晶种层、第一金属层、有机间隔层、第二成核氧化物晶种层、第二金属层和聚合物型保护层。金属层和有机间隔层的厚度为使得阳光控制膜为能透射可见光并且能反射红外线。阳光控制膜的可见光透射率高、反射能量高并且总太阳热透射率低。
Description
相关专利申请的交叉引用
本专利申请要求提交于2007年12月28日的临时专利申请No.61/017477的优先权,该专利的公开内容以引用方式并入本文中。
技术领域
本发明涉及阳光控制膜和玻璃窗,包括车辆玻璃窗。
背景技术
阳光控制膜用于汽车风窗玻璃及其它车辆玻璃窗,以降低热量增益、内部温度和空调负载。市售的阳光控制膜包括得自SouthwallCorporation的XIRTM-70、XIR-75、V-KOOLTM和Hüper OptikTM膜,得自Bekaert Specialty Film,LLC的ULTRA PERFORMANCETM75膜,得自Sekisui Chemical Co.,Ltd.的S-LECTTM的隔音膜和太阳膜以及得自CPFilms Inc.的各种膜。具有阳光控制特征的被涂覆的玻璃产品包括得自PPG Industries,Inc.的SUNGATETM挡风玻璃和得自AFG Industries,Inc.的SOLARSHIELDTM玻璃。这些膜和被涂覆的玻璃产品旨在阻隔或吸收红外线(或在一些情况下为紫外线)能量,而透射可见光。遗憾的是,良好的红外线阻隔率和良好的可见光透射率是逆相关的。在获得所需的阳光控制水平的同时仍然满足适用的可见光透射率(Tvis)会是很难的。例如,欧洲标准ECE R-43要求挡风玻璃的Tvis至少为75%并且侧灯和后照灯的Tvis至少为70%。U.S.Federal Motor Vehicle SafetyStandard 205(美国联邦机动车辆安全标准205)(49C.F.R Part571.205)、SAE ANSI Z26.1-1996以及Japanese Standard JIS SafetyRegulations for Road Vehicles(日本工业标准道路车辆安全规则第29条)要求机动车辆的玻璃窗的Tvis至少为70%。
仍然存在具有高可见光透射率和良好阳光控制特性的阳光控制膜的需求。
发明内容
在一个方面,本发明提供阳光控制膜,该膜至少依次包括能透射可见光的柔性载体、第一成核氧化物晶种层、第一金属层、有机间隔层、第二成核氧化物晶种层、第二金属层和聚合物型保护层,其中金属层和有机间隔层的厚度为使得该膜能透射可见光并且能反射红外线。
在另一方面,本发明提供了一种层合的玻璃窗制品,该制品至少依次包括第一玻璃窗材料层、第一机械能量吸收层、本发明所公开的阳光控制膜、第二机械能量吸收层和第二玻璃窗材料层。
在另一方面,本发明提供用于形成阳光控制膜的方法,该方法包括:
a)提供能透射可见光的柔性载体,
b)在载体的顶上形成第一成核氧化物晶种层,
c)在第一晶种层的顶上形成第一金属层,
d)在第一金属层的顶上形成有机间隔层,
e)在有机间隔层的顶上形成第二成核氧化物晶种层,
f)在第二晶种层的顶上形成第二金属层,以及
g)在第二金属层的顶上形成聚合物型保护层,
其中金属层和有机间隔层的厚度为使得阳光控制膜能透射可见光并且能反射红外线。
本发明的这些方面以及其它方面在下面的具体实施方式中将显而易见。然而,在任何情况下,不应将上述发明内容理解为是对要求保护的主题的限制,该主题仅受所附权利要求书的限定,并且在审查期间可以进行修改。
附图说明
图1和图2为阳光控制膜的示意性剖视图;
图3为用于制备阳光控制膜的设备的示意图;
图4为层合的玻璃窗制品的示意性剖视图;和
图5和图6为示出用于若干阳光控制膜的反射能量(Re)与总太阳热透射率(TSHT)的关系的坐标图。
附图中多张图中相同的基准符号表示相同的元件。附图中的元件未按比例绘制。
具体实施方式
词语“一个”和“所述”与“至少一个”可互换使用,意指一个或多个所述元件。通过使用例如“在…的顶上”、“在…上”、“最上”、“下面的”等等用于本发明所公开的被涂覆的制品中各种元件位置的取向词,我们是指元件相对于水平朝上布置载体的相对位置。这并不意味着膜或制品在制造期间或之后在空间上应该具有任何特定的取向。
当相对于表面或制品使用时,术语“空间弯曲”意指表面或制品在两个不同的、非线性方向从单个点弯曲。
术语“共聚物”包括无规聚合物和嵌段共聚物两者。
当相对于聚合物使用时,术语“交联”意指聚合物具有通过共价化学键接合在一起的聚合物链(通常通过交联分子或基团),以形成网状聚合物。交联聚合物通常的特征在于其不溶性,但在存在适当溶剂的情况下可以是溶胀性的。
当相对于阳光控制膜使用时,术语“可延展的”意指在面内的方向能将膜拉伸至少约3%,并且在约0.25米的距离处用肉眼检查时膜中没有形成可见的不连续性。
当相对于载体、层、膜或制品使用时,术语“能反射红外线”意指在近正常角面处(如在约6°的入射角处)测量时,载体、层、膜或制品反射从约700nm至约4,000nm的波长区域中的至少100nm宽的谱带内的光的至少约50%。
术语“光”意指阳光辐射。
术语“金属”包括纯金属和金属合金。
当相对于表面或制品(如玻璃的或其它窗材料)使用时,术语“非平面”意指表面或制品具有连续的、间歇的、单向的或空间弯曲。
当相对于层使用时,术语“光学厚度”意指层的物理厚度乘以其面内折射率。
当相对于阳光控制膜或层合的玻璃窗制品使用时,术语“光学透明的”意指在约1米的距离处用肉眼检测时,在膜或制品中不存在可见的明显的失真、雾度或瑕疵。
术语“聚合物”包括均聚物和共聚物,以及(如通过共挤出或通过(如)酯交换反应在内的反应)可以在可混溶的共混物中形成的均聚物和共聚物。
术语“反射的能量”(“Re”)是指在从250nm至2500nm的波长范围内反射的能量。
当相对于载体、层、膜或制品使用时,术语“可见光透射率”或“能透射可见光”意指载体、层、膜或制品在550nm处的可见光透射率大于50%。
当相对于在层合的玻璃窗制品中的阳光控制膜使用时,术语“无显著的缝隙或褶皱”意指在约1米(优选约0.5米)的距离处用肉眼检测时,膜中不存在可见的不连续性。
当相对于层合的玻璃窗制品中的阳光控制膜使用时,术语“无明显褶皱”意指在约1米(优选约0.5米)的距离处用肉眼检测时,不存在由于光滑膜表面的收缩导致的小脊或皱纹。
参见图1,在100中总地示出了示例性的阳光控制膜。膜100包括能透射可见光的塑料膜(由(例如)聚对苯二甲酸乙二醇酯(“PET”)制成)形式的柔性载体102和在载体102的顶上的层的叠堆104。叠堆104包括第一成核氧化物晶种层106(由(例如)氧化锌制成)、第一金属层108(由(例如)银制成)、有机间隔层110(由(例如)交联丙烯酸酯制成)、第二成核氧化物晶种层112(也由(例如)氧化锌制成)和第二金属层114(也由(例如)银制成)。保护性聚合物层116(由(例如)交联的丙烯酸酯制成)位于第二金属层114的顶上。保护性聚合物层116限制对叠堆104的损坏,并且也可以改变叠堆的光学性质。载体102、第一晶种层106、第一金属层108、有机间隔层110、第二晶种层112、第二金属层114和保护性聚合物层116可以彼此相邻,或可以由图1中未示出的一个或多个额外的层隔开。晶种层106和112、金属层108和114以及有机间隔层110各能透射可见光(正如作为整体的膜100),并且至少第一金属层108、有机间隔层110和第二金属层114是连续的层。晶种层106和112不需要是连续的层,并且可以是比金属层108和114或有机间隔层110薄很多的层。例如,晶种层106和112各可以是一系列小的岛状物,该岛状物起到有助于上覆金属层更均一或更致密沉积的成核位点的作用。选择金属层108和114、居间的有机间隔层110和叠堆104的厚度,从而金属层108和114充分地薄,以部分反射并部分透射;并且通过层110充分地间隔开,从而膜100能透射可见光并且能反射红外线。例如,间隔层110的光学厚度可以为约透射光所需通带的中心波长的1/4至1/2,并且叠堆104可以表示Fabry-Perot干涉叠堆。波长在通带范围内的光将主要透射通过金属层108和114。
波长高于或低于通带的光将主要被金属层108和114反射。在图2中,在200处总地示出了另一个示例性的阳光控制膜。膜200与膜100类似,但在载体102和第一晶种层106之间包括有机基部涂层202(由(例如)交联的丙烯酸酯制成)。基部涂层202有助于消除载体102中的表面粗糙性和其它缺陷,并且有助于最终获得更平滑的金属层108和114的沉积。基部涂层202也可以改变叠堆104的光学性质。如果需要,基部涂层202可以是包含填料粒子(图2中未示出,但由(例如为)氧化锌纳米粒子的高折射率粒子制成)的硬质涂层,与不包含这类填料粒子的基部涂层相比,该硬质涂层可以增加硬度(对暴露的硬质涂层使用(例如)铅笔硬度测试来确定此硬度)。当选择适当时,与没有这类粒子而制成的制品相比,填料粒子也可以增加穿过制品200的可见光的透射率。尽管硬质涂层掩盖在叠堆104和保护性聚合物层116的下面,与将叠堆涂覆在较软的基部涂层或直接涂覆在载体102上相比,该硬质涂层令人惊讶地可以赋予叠堆104改善的耐久性(正如(例如)通过改善的耐磨性或对制品200进行的铅笔硬度测试所证实的那样)。如果需要,可以采用较软的基部涂层和硬质涂层两者,并且可以颠倒它们的顺序。
图3示出可以方便地用于制造本发明所公开的阳光控制膜的示例性设备300。机动卷轴302和304使载体306来回移动通过设备300。温控旋转筒308及惰轮310和312带着载体306经过等离子体预处理器314、晶种金属或晶种金属氧化物溅射涂敷器316、反射性金属溅射涂敷器318、蒸发器320和电子束交联设备322。从贮存器326向蒸发器320供应液态单体或低聚物324。在第一次经过设备300的过程中,可以在载体306上涂覆或形成第一成核氧化物晶种层(例如层106)、第一金属层(例如层108)和有机间隔层(例如层110)。有机间隔层可以用作临时保护层,当刚被涂覆的载体306从卷轴304重绕到卷轴302上时,有机间隔层减少对第一金属层的损坏。可以利用第二次通过设备300来涂覆或形成第二成核氧化物晶种层(例如层112)、第二金属层(例如层114)和聚合物型保护层(例如层116)。可将设备300封闭在合适的室内(在图3中未示出),并且保持在真空状态下或供有合适的惰性气体,以便阻止氧气、水蒸汽、粉尘和其它大气污染物干扰各种预处理、涂覆、交联和溅射步骤。也可以将反应性的气体(如氧气或水蒸汽)引入设备300中(或可以从载体或从室本身中脱气),以故意地形成干扰,如将金属层转化成氧化物层。
图4示出层合的安全挡风玻璃400的剖视图。挡风玻璃400具有连续的曲面,其曲率半径在挡风玻璃400中心区域(图4中仅用虚线示出)附近可以相对大,但它在挡风玻璃400的更急剧弯曲的末端区域402、404附近可以减小到相对小的值。挡风玻璃400至少依次包括外玻璃层406、第一机械能吸收层408(由(例如)增塑聚乙烯醇缩丁醛(“PVB”)制成)、太阳能控制膜200(其包括载体102、有机基部涂层202、第一成核氧化物晶种层106、第一金属层108、有机间隔层110、第二成核氧化物晶种层112、第二金属层114和保护性聚合物层116)、第二机械能吸收层410(也由(例如)PVB制成)以及内玻璃层412。如图4所示,将轧辊414和416用于去除空气并将玻璃层406和412、能量吸收层408和410以及膜200粘合在一起。如果需要,可以将阳光控制膜在挡风玻璃400内取向,从而载体被布置得离第二机械能吸收层410(而非第一机械能吸收层410)较近(如相邻)。然而,当载体是多层光学膜(“MOF”)时,例如美国专利No.7,215,473 B2中所述,阳光控制膜被有利地取向,从而载体离第一机械能吸收层410较近。
可以采用多种能透射可见光的载体。示例性的载体包括(但不限于)柔性塑料材料,柔性塑料材料包括热塑性膜,例如聚酯(如聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯)、聚丙烯酸酯(如聚甲基丙烯酸甲酯)、聚碳酸酯、聚丙烯、高密度聚乙烯或低密度聚乙烯、聚砜、聚醚砜、聚氨酯、聚酰胺、聚乙烯醇缩丁醛、聚氯乙烯、聚偏二氟乙烯、聚乙烯硫化物和环烯烃聚合物(如得自Topas AdvancedPolymers的TOPASTM和得自Zeon Chemicals,L.P.的ZEONORTM);以及热固性膜,例如纤维素衍生物、聚酰亚胺、聚酰亚胺苯并噁唑和聚苯并噁唑。优选的是由聚对苯二甲酸乙二醇酯和MOF(金属有机骨架材料)制成的载体。载体可以具有多种厚度,如约0.01mm至约1mm的厚度。然而,例如当需要自支承阳光控制制品时,载体可以相当厚。也可以通过在薄的、柔性载体上形成本发明所公开的阳光控制膜并且将柔性载体层合或者说是接合到较厚的、不可挠曲的或柔性较低的补充载体(例如玻璃或塑料面板)来制造这种自支承制品。
通过适当地预处理载体,可以增强各种阳光控制膜层的光滑度、连续性或粘附力中的一者或多者。在一个实施例中,预处理摄生法涉及在存在反应性或非反应性大气(如空气、氮气、氧气或惰性气体(例如氩气))的情况下的对载体的放电预处理(如等离子体、辉光放电、电晕放电、电介质屏蔽放电或大气压放电)、化学预处理或火焰预处理。这些预处理可以有助于确保载体或上覆层表面将易于接受随后涂覆的层。在另一个实施例中,使用有机基部涂层(例如图2中作为层202示出的有机基部涂层)涂覆载体,然后可任选地是使用等离子体或上述其它预处理中的一种进一步进行预处理。当采用时,有机基部涂层优选地基于一个或多个交联丙烯酸酯聚合物。如果有机基部涂层是硬质涂层或包括硬质涂层,则硬质涂层优选地基于包含无机氧化物粒子的分散体的涂层组合物,例如美国专利No.5,104,929(Bilkadi)中所述的组合物。3M 906 Abrasion Resistant Coating(3M 906耐磨涂层)(得自3M公司)是优选的硬质涂层组合物。可以使用多种技术(包括溶液涂覆、辊涂(如凹版辊涂)或喷涂(如静电喷涂))涂覆有机基部涂层,然后使用(例如)紫外线辐射使其交联。优选地通过可辐射交联的单体或低聚物(如丙烯酸酯单体或低聚物)的闪蒸和气相沉积,然后原位交联(使用(例如)电子束设备、UV光源、放电设备或其它合适的装置)来涂覆有机基部涂层(并且另外有利地有机间隔层和聚合物型保护层),如上述美国专利No.7,215,473 B2、美国专利No.6,929,864 B2、美国专利No.7,018,713 B2及其中引用的文件所述。有机基部涂层所需的化学组成和厚度将部分取决于载体的性质。对于聚对苯二甲酸乙二醇酯和MOF(金属有机骨架材料)载体,基部涂层可以(例如)由丙烯酸酯单体或低聚物形成,并且可以(例如)具有足以提供连续层的厚度(如几纳米至高达约2微米)。也可以调节基部涂层的厚度以增强膜的光学性质,如增加穿过叠堆的透射率并使叠堆的反射率最小化。可以通过在有机基部涂层中包括助粘添加剂或抗腐蚀添加剂,进一步改善第一成核氧化物晶种层对载体的粘附力。合适的助粘添加剂或抗腐蚀添加剂包括硫醇、酸(例如羧酸或有机磷酸)、三唑、染料和润湿剂。美国专利No.4,645,714中描述了具体的助粘添加剂(乙二醇双硫基乙醇酸酯)。有利地,所存在的添加剂的量足以使晶种层粘附力增加而不会导致晶种层的过度氧化或其它降解。
在成核氧化物晶种层中可以采用多种氧化物。晶种层可以是相同的或不同的,并且有利地是相同的。晶种层氧化物有利地以更均一或更致密的方式促进随后涂覆的金属层的沉积,或促使更早地形成(即以较薄的涂覆厚度)连续的金属层。可以根据所选择的载体和相邻的金属层来选择合适的氧化物,并且通常将根据经验进行选择。代表性的晶种层氧化物包括氧化镓、氧化铟、氧化镁、氧化锌、氧化锡及其混合物(包括混合型氧化物或掺杂型氧化物)。例如,晶种层可以包含氧化锌或掺杂有铝或氧化铝的氧化锌。可以使用在膜金属化领域中采用的技术形成晶种层,例如溅射(如平面溅射或旋转磁控管溅射);蒸镀(如热阻元件或电子束蒸镀);化学气相沉积;金属有机CVD(MOCVD);等离子体增强的、辅助的或激活的CVD(PECVD);离子溅射等等。可以(例如)便利地通过溅射晶种层氧化物直接形成晶种层,或通过在氧化气氛中溅射前体金属原位形成晶种层。溅射靶也可以包括金属(如铝、铟、锡或锌)或氧化物(如氧化铝、氧化铟、氧化铟锡、氧化锡或氧化锌),以使溅射靶具有更好的导电性。示例性的溅射靶包括氧化锌∶氧化铝、氧化锌∶氧化镓、氧化锌∶氧化锡、氧化铟∶氧化锌、氧化铟∶氧化锡、氧化铟∶氧化锡∶氧化锌、铟∶锌、铟∶锡、铟∶锡∶锌、氧化铟镓锌或Zn(1-x)MgxO:Al、MgIn2O(4-x)。其具体的实例包括99∶1和98∶2的氧化锌∶氧化铝、95∶5的氧化锌∶氧化镓、93∶7的氧化锌∶氧化镓、90∶10的氧化铟∶氧化锌、90∶10和95∶5的氧化铟∶氧化锌、从约76∶24至约57∶43的铟∶锌和90∶10的铟∶锡。晶种层可以具有相同或不同的厚度,并且优选地各充分地厚,从而随后涂覆的金属层将会均匀地吸收最少的光。晶种层优选地充分地薄,以便确保所得的阳光控制膜和采用该阳光控制膜的制品将具有所需程度的可见光透射率和近IR反射率或IR反射率。例如,晶种层的物理厚度(相对于光学厚度)可以为小于约20nm、小于约10nm、小于约8nm、小于约5nm、小于约4nm或小于约3nm。晶种层的物理厚度也可以为大于0nm、至少0.5nm或至少1nm。在一个实施例中,晶种层的物理厚度大于0并且小于约5nm。在第二实施例中,晶种层的物理厚度大于0并且小于约4nm。在第三实施例中,晶种层的物理厚度大于0并且小于约3nm。
在金属层中可以采用多种金属。金属层可以是相同或不同的,并且有利地是相同的。示例性的金属包括银、铜、镍、铬、贵金属(如金、铂或钯)及其合金。可对晶种层使用类似于上述技术的膜金属化领域的技术,并对非贵金属使用非氧化气氛,来形成金属层。金属层充分地厚以便具有连续性,并且充分地薄以便确保阳光控制膜或采用该阳光控制膜的制品将具有所需程度的可见光透射率以及近IR反射率或IR反射率。金属层通常将比晶种层厚。在一个实施例中,金属层的物理厚度将为约5nm至约50nm。在另一个实施例中,金属层的厚度为约5nm至约15nm。在第三实施例中,金属层的厚度为约5nm至约12nm。
有机间隔层位于第一金属层和第二成核晶种层之间,并且可以由多种有机材料形成。如果需要,可使用例如辊涂(如凹版辊涂)或喷涂(如静电喷涂)之类的常规涂覆方法来涂覆有机间隔层。优选地,使用(如)类似于当使用交联的有机基部涂层时采用的技术来交联有机间隔层。交联的有机间隔层具有若干优于非交联的有机间隔层的优点。不像非交联的有机间隔层那样,交联的有机间隔层在稍微加热时既不会熔融、又不会软化,并且因此在形成或层合的过程中,在温度和压力的同时影响下,交联的有机间隔层不太可能明显地流动、变形或变薄。交联的有机间隔层为高度耐溶剂的,而非交联的有机间隔层可以被溶剂(包括存在于车用流体(例如汽油、石油、传动液和车窗清洁剂)的那些)溶解或略微软化。与由类似的聚合物加工而成的非交联的有机间隔层相比,交联的有机间隔层也可以具有理想的物理特性,例如较高的模数和硬度、较好的应变弹性恢复性能或较好的弹性。优选地,有机间隔层在第一金属层或合金层的顶上原位交联。优选地,通过涉及上述美国专利No.6,929,864 B2、No.7,018,713 B2和No.7,215,473 B2及其中引用的文件所述的闪蒸、气相沉积和单体交联的方法形成间隔层。在这类方法中,优选地使用易挥发的(甲基)丙烯酸酯,尤其优选地使用易挥发的丙烯酸酯。可通过冷却载体来提高涂覆效率。尤其优选的单体包括:单独使用或结合其它多官能或单官能(甲基)丙烯酸酯使用的多官能(甲基)丙烯酸酯,例如二丙烯酸己二醇酯、乙氧基乙基丙烯酸酯、丙烯酸苯氧乙酯、氰乙基(单)丙烯酸酯、丙烯酸异冰片酯、异冰片基甲基丙烯酸酯、丙烯酸十八烷基酯、异癸基丙烯酸酯、丙烯酸月桂酯、β-羧乙基丙烯酸酯、丙烯酸四氢糠基酯、二腈丙烯酸酯、五氟苯基丙烯酸酯、硝基苯基丙烯酸酯、2-丙烯酸苯氧乙酯、2-苯氧基乙基甲基丙烯酸酯、2,2,2-三氟甲基(甲基)丙烯酸酯、二乙二醇二丙烯酸酯、二丙烯酸三乙二醇酯、三亚乙基乙二醇二甲基丙烯酸酯、三丙二醇二丙烯酸酯、二丙烯酸四乙二醇酯、新戊乙二醇二丙烯酸酯、丙氧化新戊乙二醇二丙烯酸酯、聚乙烯乙二醇二丙烯酸酯、二丙烯酸四乙二醇酯、双酚A环氧丙烯酸酯、1,6-己二醇二甲基丙烯酸酯、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、丙氧基化三羟甲基丙烷三丙烯酸酯、三(2-羟乙基)-异氰脲酸三丙烯酸酯、季戊四醇三丙烯酸酯、苯硫基乙醇丙烯酸酯、萘甲酰基丙烯酸乙酯、IRR-214环丙烯酸酯(得自UCB Chemicals)、环氧丙烯酸酯RDX80095(得自Rad-Cure Corporation)及其混合物。间隔层中可以包括多种其它固化性材料,如丙烯酰胺、乙烯基醚、乙烯基萘、丙烯腈以及它们的混合物。间隔层的物理厚度将部分取决于其折射率,并且部分取决于所需的阳光控制膜的光学特性。优选的光学厚度为所需透射光通带中心波长的约1/4至1/2。为了在红外线阻隔干扰叠堆中使用,交联的有机间隔层的折射率可以(例如)为约1.3至约1.7、光学厚度为约75nm至约275nm(如约100nm至约150nm)以及对应的物理厚度为约50nm至约210nm(如约65nm至约100nm)。可以采用光学建模来选择合适的层厚度。
可以使用多种有机材料来形成聚合物型保护层。如果需要,可以使用例如辊涂(如凹版辊涂)或喷涂(如静电喷涂)的常规涂覆方法来涂覆保护层。优选地,使用例如类似于当使用交联的有机基部涂层时采用的技术来交联保护层。也可以单独形成保护层并使用层合来涂覆保护层。优选地,使用如上所述的闪蒸、气相沉积和单体或低聚物的交联来形成保护层。在此类保护层中使用的示例性的单体或低聚物包括易挥发的(甲基)丙烯酸酯。保护层也可以包含助粘添加剂。示例性的添加剂包括上述间隔层的添加剂。当在例如PVB的机械能吸收材料的片材之间层合阳光控制膜时,可以选择保护层的折射率,使由于机械能吸收材料和阳光控制膜之间折射率的任何不同引起的界面处的反射最小化。也可以对保护层进行后处理,以增强保护层对机械能吸收材料的粘附力。示例性的后处理包括上述载体的预处理。在一个实施例中,阳光控制膜的两侧均可采用等离子体后处理。
可以将各种官能层或元件添加到本发明所公开的膜中,尤其是在膜表面中的一个处,以改变或改善其物理性质或化学性质。这样的层或涂层可包括(例如):低摩擦涂层或滑动粒子,其使膜在制备过程中更易于处理;粒子,其增加膜的漫射性质或抑制将膜布置成紧接其它膜或表面时出现润湿或牛顿环;粘合剂,例如压敏粘合剂或热熔粘合剂;引物,其促进对相邻层的粘附力;低粘附力背胶材料,其当膜有待以粘合剂辊形式使用时使用;以及电极,其允许通过金属层中的一者或两者进行电流感测、电压感测或电容感测。官能层或涂层也可以包括防碎、抗侵入或耐撕扯的膜和涂层,例如公布的PCT专利申请No.WO 01/96115 A1中所述官能层。另外的官能层或涂层也可以包括例如在美国专利No.6,132,882和No.5,773,102中所述减振膜层或吸声膜层,以及屏蔽层,从而得到保护膜的透射性质或将其朝例如水或有机溶液的液体或朝例如氧气、水蒸气或二氧化碳的气体改变。这些官能组分可掺入到膜最外层中的一个或多个中,或它们可作为单独的膜或涂层来涂覆。对于某些应用,可能有利的是改变阳光控制膜的外观或性能,例如通过将染色的膜层层合到导电性膜,着色的涂层涂布到阳光控制膜的表面,或在用于制备阳光控制膜的材料中的一种或多种中包括染料或颜料来改变。染料或颜料可在光谱的一个或多个所选区域中具有吸收性,包括光谱的红外线部分、紫外线部分或可见光部分。可将染料或颜料用于补充阳光控制膜的性质,尤其在阳光控制膜透射某些频率而反射其它频率的情况下。可在本发明所公开的膜中采用的特别可用的着色层在美国专利No.6,811,867 B1中有所描述。可将该层层合、挤出涂覆或共挤出为膜上的表皮层。颜料装填量在约0.01重量%至约1.0重量%之间可有差别,以根据需要改变可见光透射率。添加UV吸收型包覆层也是理想的,以便保护暴露于UV辐射时可能不稳定的膜中的任何内层。可以添加到阳光控制膜中的其它官能层或涂层包括(例如):防静电涂层或膜;阻燃剂;UV稳定剂;耐磨或硬涂层材料;光学涂层;防雾材料;磁性或磁光涂层或膜;液晶面板;电致变色或电致发光面板;感光乳剂;棱镜膜;以及全息膜或全息图像。例如,在美国专利No.6,368,699、No.6,352,761和No.6,830,713中描述了另外的官能层或涂层。可以用(例如)油墨或其它印刷标记(例如用于显示产品标识、取向信息、广告、警告、装饰或其它信息的标记)处理阳光控制膜。可使用多种技术在阳光控制膜上进行印刷,例如为网版印刷、喷墨印刷、热转印印刷、凸版印刷、橡皮版印刷、柔性版印刷、打点印刷、激光印刷等;并且可使用多种类型的油墨,包括具有一种和两种组分的油墨、氧化干燥型和UV干燥型油墨、溶解型油墨、分散型油墨和100%的油墨系统。
当设置有电极时,本发明所公开的阳光控制膜可用于(例如)天线、电磁干扰屏蔽(EMI)的用途,以及用于(例如)玻璃窗、车窗和显示器的扫雾、除雾、除霜或除冰的电热膜。电热膜应用会要求基本的载流能力,但当要求可见光的透射率时必须采用很薄的(并且相应地非常易碎的)金属或金属合金层。在美国专利申请No.3,529,074、No.4,782,216、No.4,786,783、No.5,324,374和No.5,332,888中公开了电热膜的应用。电热膜在车辆安全玻璃窗方面特别受到关注,例如在汽车、飞机、火车或其它车辆挡风玻璃、后照灯、天窗或侧窗中。可以通过以下方式制备电热玻璃窗:在玻璃层之间设置PVB层、电热膜层和合适的电极;从接合表面除去空气;然后将组件在高压釜中设置到高温高压,以将PVB、电热膜层和玻璃熔合粘合成光学透明的结构。在低电压下这种膜中使用的金属层有利地具有低电阻,如每平方小于约20欧姆的电阻。例如,金属层的电阻每平方可以为约5欧姆至约20欧姆、约7.5欧姆至约15欧姆或约7.5欧姆至约10欧姆。
本发明所公开的膜可接合或层合到各种各样的基底上。通常的基底包括玻璃窗材料,例如玻璃(其可以是绝缘玻璃、钢化玻璃、层合玻璃、退火玻璃的或热强化玻璃)和塑料(例如聚碳酸酯和聚甲基丙烯酸甲酯)。可以将膜接合到基底的一个主面上或夹在两个或更多个基底之间。这种膜尤其可用于与非平面基底连接,特别是具有复杂弯曲的基底。膜有利地为可延展的并且在层合和除气的过程中能够适形于这种非平面基底,而基本上没有开裂或褶皱。在足够有助于膜对于非平面基底适形而基本没有褶皱的条件下,本发明所公开的膜可被取向并可选地被热定型。当要与膜层合的非平面基底具有已知的形状或曲率时,尤其是当基底具有已知的严重空间弯曲时,这是特别可用的。通过在每个面内方向单独地控制膜回缩,可在层合期间(如在轧辊层合或在高压釜中处理期间)以可控的方式引起膜回缩。例如,如果要与膜层合的非平面基底具有空间弯曲,那么可修整在每一个面内方向的膜回缩,以在这些方向与基底的具体曲率特性匹配。可以将回缩最大的面内膜方向与曲率最小(即曲率半径最大)的基底维度对齐。除了或取代根据曲率半径表征曲率,如果需要,也可使用其它测量方法(例如从由基底主表面限定的几何表面测量的凸起区域或凹陷区域的深度)。为了层合到通常的非平面基底,膜回缩可在两个面内方向均大于约0.4%、在至少一个面内方向大于约0.7%或在至少一个面内方向大于约1%。在一个实施例中,整个膜回缩被限制为减少边缘分层或“拉进”。因此,在每一个面内方向,膜回缩可小于约3%,或在每一个面内方向小于约2.5%。回缩行为将主要受以下因素的控制:例如所采用的膜或基底材料、膜拉伸率、热固温度、停留时间和内束(相对于最大导轨定型测量的在拉幅机热固区域中的导轨间距的减小)。涂层也可改变膜回缩性质。例如,引物涂层可以将横向(“TD”)回缩减少约0.2%至约0.4%,并且将纵向(“MD”)回缩增加约0.1%至约0.3%。取向设备和热固设备可有广泛的差别,并且通常在每一种情况下通过实验来确定理想的处理设置。有关制备具有目标回缩性质的制品的技术的进一步详情在美国专利No.6,797,396中有所描述。有关制备采用MOF载体制备制品和采用玻璃窗中的一层或两层制备层合物的技术的进一步详情在美国专利No.7,189,447 B2中有所描述。
可以将本发明所公开的阳光控制膜和制品用于各种目的,包括车辆玻璃窗、建筑玻璃窗、太阳能电池、太阳能收集器和器械。膜可以具有各种可见光透射率(Tvis)值,如沿着法向轴测量的为至少约60%、至少约70%或至少约75%。膜优选地具有高的Re值并且具有低的TSHT值。可以根据ISO标准9050:2003确定TSHT,并且TSHT是由玻璃窗吸收并辐射到建筑物、车辆或其它封闭体中的能量加上传输到封闭体中的能量的测量。TSHT和Re通过下面的公式与Te(通过膜或制品传输的能量百分比)相关:
TSHT=(8/31)*(100-Te-Re)+Te
当将本发明所公开的阳光控制膜包括到层合的安全玻璃窗中并且在0°入射角处进行测量时,玻璃窗的TSHT优选小于约60%、更优选小于约55%并且最优选小于约50%;并且其Re至少约20%、更优选至少约25%并且最优选至少约30%。
在以下的实例中对本发明进行进一步说明,其中除非另外指明,否则所有份数、百分比和比率均按重量计。
实例1
用包含氧化锌成核晶种层、银金属层和有机层的光学叠堆来涂覆聚对苯二甲酸乙二醇酯载体,该有机层使用两种不同的丙烯酸酯混合物(丙烯酸酯A或丙烯酸酯B)、以丙烯酸酯A/ZnO/Ag/丙烯酸酯B/ZnO/Ag/丙烯酸酯B的堆叠模式制备。丙烯酸酯A包含64%的IRR214丙烯酸酯(UCB Chemicals)、28%的正丙烯酸月桂酯和8%的乙二醇双-硫基乙醇酸酯。丙烯酸酯B包含80%的苯硫基乙醇丙烯酸酯和20%的季戊四醇三丙烯酸酯。按以下方式形成各个层:
(第1层)将0.05mm厚、508mm宽的聚对苯二甲酸乙二醇酯膜的卷筒(得自DuPont Teijin Films的MELINEXTM453)装入类似图3示出的滚筒式设备,使之位于真空室的内部。将室中的压力降低到3×10-4托并且将筒308冷却到-18℃。如由制造商供应的聚对苯二甲酸乙二醇酯膜的一面上具有未标识的处理。在氮等离子体中,将聚对苯二甲酸乙二醇酯膜未处理过的一面暴露于使用在1kW直流电下操作的钛靶磁控管的等离子体预处理。然后,以38.1米/分钟的幅材速度,使用脱气的、闪蒸过的丙烯酸酯A的单体混合物涂覆聚对苯二甲酸乙二醇酯膜的预处理过的一面。通过将丙烯酸酯A暴露在压力为大约1×10-3托中的方式去除单体混合物中的气体,并且接着通过超声喷雾器以2毫升/分钟的速度将其泵送到保持在274℃下的蒸汽室中来将其闪蒸。闪蒸过的丙烯酸酯A混合物从室内喷涂到移动的聚对苯二甲酸乙二醇酯膜上,由于筒的温度低,丙烯酸酯A混合物在此凝结。然后,使用在7.5kV下操作的单个原丝枪将凝结的丙烯酸酯A单体混合物与电子束辐射交联。交联的丙烯酸酯A基部涂层的最终厚度为大约140nm。预处理、涂覆和交联在单程中顺序进行。
(第2层)翻转膜的方向。将第一氧化锌(ZnO)成核晶种层以约1nm的厚度涂覆到丙烯酸酯A基部涂层上。
(第3层)接着,在同一单程中,将第一银(Ag)金属层以约6.75nm的厚度涂覆到第一ZnO晶种层上。
(第4层)接着,在同一单程中,将由丙烯酸酯B单体混合物制成的间隔层涂覆到Ag层上并且以与第1层中所述方式相同的方式交联,但交联的间隔层的厚度为约120nm。
(第5层)翻转膜的方向。将第二ZnO成核晶种层以约1nm的厚度将涂覆到丙烯酸酯B间隔层上。
(第6层)接着,在同一单程中,将第二Ag金属层以约6.75nm的厚度涂覆到第二ZnO晶种层上。
(第7层)接着,在同一单程中,将由丙烯酸酯B制成的保护层涂覆到第二Ag层上,并且以与第1层中所述方式相同的方式交联,但保护层的厚度为约65nm。
随后,对所得的阳光控制膜的两面均进行等离子体处理。将膜层合到5层具有玻璃/PVB/膜/PVB/玻璃模式的汽车挡风安全玻璃窗构造的中心中。
实例2
使用实例1中的大体方法,多层光学膜(得自3M公司的3MTM阳光反射膜)被包括氧化锌成核氧化物晶种层、银金属层和有机层的光学叠堆涂覆,该有机层使用丙烯酸酯混合物(丙烯酸酯C)、以丙烯酸酯C/ZnO/Ag/丙烯酸酯C/ZnO/Ag/丙烯酸酯C叠堆的模式制成。丙烯酸酯C包含90%的苯硫基乙醇丙烯酸酯、5%的季戊四醇三丙烯酸酯和5%的双官能双酚A-基环氧-丙烯酸酯和乙氧基化的三羟甲基丙烷三丙烯酸酯的50∶50的混合物。与实例1同样地形成各个层,不同之处在于,丙烯酸酯C基部涂层的厚度为约120nm、第一Ag层和第二Ag层的厚度为约8nm、丙烯酸酯C间隔层的厚度为约112nm、丙烯酸酯C保护层的厚度为约62nm并且在涂覆金属层和之上的有机层的过程中间使用等离子体预处理。
随后,对所得的阳光控制膜的两面均进行等离子体处理。将膜层合到5层具有玻璃/PVB/膜/PVB/玻璃模式的汽车挡风安全玻璃窗构造的中心中。
实例1和实例2的评估
对实例1和实例2的挡风玻璃构造进行评估,以确定在0°的入射角处的Tvis、Re和TSHT,并且在表1和图5中分别将实例1和实例2的挡风玻璃构造标识为样品A和样品B。针对以下构造获得比较量度:使用未涂覆的3M阳光反射膜制成的5层构造(样品C)、使用得自Southwall Corporation的XIR-75膜制成的5层构造(样品D)、使用S-LEC阳光膜(得自Sekisui Chemical Co.,Ltd.的吸收IR填料粒子的PVB替代物)制成的玻璃/膜/玻璃的模式的3层构造(样品E)和使用得自PPG Industries,Inc.的SUNGATE金属涂覆的玻璃以涂覆的玻璃/PVB/未涂覆的玻璃的模式(玻璃涂层面向PVB层)制成的3层构造(样品F)。以下在表1中示出Tvis结果,并且在图5中示出Re和TSHT的结果。
表1
样品 | 阳光控制元件 | 层合模式 | Tvis,% |
A | 实例1膜 | 玻璃/PVB/膜/PVB/玻璃 | 77 |
B | 实例2膜 | 玻璃/PVB/膜/PVB/玻璃 | 78 |
C | 3M阳光反射膜 | 玻璃/PVB/膜/PVB/玻璃 | 79 |
D | XIR-75膜 | 玻璃/PVB/膜/PVB/玻璃 | 79 |
E | S-LEC膜 | 玻璃/膜/玻璃 | 83 |
F | SUNGATE被金属涂覆的玻璃 | 玻璃/膜/玻璃 | 77 |
实例1和实例2的膜满足欧洲、美国和日本对汽车挡风玻璃的可见光透射率的要求,并提供具有很好的Re和TSHT性能的层合物。与使用未涂覆的多层光学膜(样品C)、XIR-75膜(样品D)或S-LEC膜(样品E)制造的层合物相比,实例1(样品A)和实例2(样品B)的膜的层合物提供更好的(即数值更大)Re性能。与使用未涂覆的多层光学膜或S-LEC膜制成的层合物相比,实例1的层叠薄膜提供更好的(即数值更小)的TSHT性能,并且与使用未涂覆的多层光学膜、XIR-75膜或S-LEC膜制造的层合物相比,实例2的层叠薄膜提供更好的TSHT性能。尽管具有更多的反射界面,实例2的层叠薄膜也提供了与金属涂覆的玻璃层合物所提供的相当的Re性能,并且虽然Re性能略低但也是非常好的。实例1和实例2的膜均是可延展的、稳固的并且在处理和加工期间能够防止受损。
实例3
使用实例1的大体方法,使用包含氧化锌成核氧化物晶种层、银金属层和有机层的光学叠堆涂覆聚对苯二甲酸乙二醇酯载体,该有机层使用丙烯酸酯混合物(丙烯酸酯A)、以丙烯酸酯A/ZnO/Ag/丙烯酸酯A/ZnO/Ag/丙烯酸酯A叠堆的模式制成。以与实例1中同样的方式形成各个层,不同之处在于,采用32米/分钟的幅材速度,丙烯酸酯A基部涂层的厚度为约120nm并且第一Ag层和第二Ag层的厚度为约6.5nm。随后,对所得的阳光控制膜的两面均进行等离子体处理。将膜层合到5层具有玻璃/PVB/膜/PVB/玻璃模式的汽车侧灯安全玻璃窗构造的中心中。
实例4
使用实例2的大体方法,使用包含氧化锌成核氧化物晶种层、银金属层和有机层的光学堆叠涂覆多层光学膜载体,该有机层使用丙烯酸酯混合物(丙烯酸酯A)、以丙烯酸酯A/ZnO/Ag/丙烯酸酯A/ZnO/Ag/丙烯酸酯A的叠堆模式制成。以与实例2中同样的方式形成各个层,不同之处在于,采用32米/分钟的幅材速度,并且第一Ag层和第二Ag层的厚度为约6.5nm。随后,对所得的阳光控制膜的两面均进行等离子体处理。将膜层合到5层具有玻璃/PVB/膜/PVB/玻璃模式的汽车侧灯安全玻璃窗构造的中心中。
实例3和实例4的评估
对实例3和实例4的侧灯构造进行评估,以确定在0°和60°的入射角处的Tvis、Re和TSHT,在表2和图6中分别将实例3和实例4的侧灯构造标识为样品A和样品B。针对以下构造获得比较量度:使用未涂覆的3M阳光反射膜制成的5层构造(样品C)、使用XIR-70膜制成的5层构造(样品D)、(c)使用S-LEC阳光膜以玻璃/膜/玻璃模式制成的3层构造(样品E)和使用SUNGATE金属涂覆的玻璃以涂覆的玻璃/PVB/未涂覆的玻璃模式(玻璃涂层面向PVB层)制成的3层构造(样品F)。以下在表2中示出Tvis的结果,并且图6中示出Re和TSHT的结果。每一个样品连接的端值表示在0°和60°的入射角处获得的结果,观察到的60°的值总体上位于0°值的左上方(即60°的Re值大于0°的Re的值,并且60°的TSHT的值小于0°的TSHT值)。在60°的入射角处的量度没有正常地记录结果,但其在图6示出以示出Re和TSHT性能是斜向相关的。
表2
样品 | 阳光控制元件 | 层合模式 | Tvis,% |
A | 实例3膜 | 玻璃/PVB/膜/PVB/玻璃 | 73 |
B | 实例4膜 | 玻璃/PVB/膜/PVB/玻璃 | 72 |
C | 3M阳光反射膜 | 玻璃/PVB/膜/PVB/玻璃 | 73 |
D | XIR-70膜 | 玻璃/PVB/膜/PVB/玻璃 | 74 |
E | S-LEC膜 | 玻璃/膜/玻璃 | 73 |
F | SUNGATE被金属涂覆的玻璃 | 玻璃/膜/玻璃 | 71 |
实例3和实例4的膜满足欧洲、美国和日本对于汽车侧灯的可见光透射率的要求,并且提供了具有良好的Re和TSHT性能的层合物。仔细观察0°处的结果,可以看出实例1(样品A)和实例2(样品B)的层叠薄膜提供的Re性能优于(即,数值更大)使用未涂覆的多层光学膜制成的层合物(样品C)或S-LEC膜制成的层合物(样品E)提供的(Re)性能。实例2的层叠薄膜也提供了优于XIR-75膜制成的层合物(样品D)或金属涂覆的玻璃层合物(样品F)的Re性能,并且提供了优于使用未涂覆的多层光学膜、XIR-75膜或S-LEC膜制成的层合物的(即数值较小)TSHT性能,并且实例2的层叠薄膜提供了优于使用未涂覆的多层光学膜、XIR-75膜或S-LEC膜制成的层合物的TSHT性能。实例3和实例4两者的膜均具有延展性、稳固性并且能够在处理和加工期间防止受损。
Claims (18)
1.一种阳光控制膜,所述阳光控制膜至少依次包括能透射可见光的柔性载体、形成为一系列小的岛状物的第一不连续成核氧化物晶种层、第一金属层、有机间隔层、形成为一系列小的岛状物的第二成核氧化物晶种层、第二金属层和聚合物型保护层,其中所述晶种层各自具有大于0并小于5nm的物理厚度,所述金属层各自具有5至12nm的物理厚度,所述有机间隔层具有1.3至1.7的折射率以及75至275nm的光学厚度,并且其中所述阳光控制膜能透射可见光并且能反射红外线。
2.根据权利要求1所述的阳光控制膜,其中所述载体包括多层光学膜。
3.根据权利要求1所述的阳光控制膜,在所述载体和所述第一不连续成核氧化物晶种层之间还包括有机基部涂层。
4.根据权利要求3所述的阳光控制膜,其中所述有机基部涂层包含丙烯酸酯聚合物。
5.根据权利要求1所述的阳光控制膜,其中晶种层包含氧化镓、氧化铟、氧化镁、氧化锌或其混合物。
6.根据权利要求1所述的阳光控制膜,其中所述第一不连续成核氧化物晶种层和所述第二成核氧化物晶种层包含氧化锌。
7.根据权利要求1所述的阳光控制膜,其中所述第一不连续成核氧化物晶种层和所述第二成核氧化物晶种层包含掺杂有铝或氧化铝的氧化锌。
8.根据权利要求1所述的阳光控制膜,其中所述第一金属层和所述第二金属层包含银。
9.根据权利要求1所述的阳光控制膜,其中所述有机间隔层包含丙烯酸酯聚合物。
10.根据权利要求1所述的阳光控制膜,其中对应于所述阳光控制膜的法向轴线在0°的入射角处进行测量时,包括所述阳光控制膜的层合的安全玻璃窗制品显示具有至少70%的可见光透射率。
11.根据权利要求1所述的阳光控制膜,其中对应于所述阳光控制膜的法向轴线在0°的入射角处进行测量时,包括所述阳光控制膜的层合的安全玻璃窗制品显示具有至少75%的可见光透射率。
12.一种层合的玻璃窗制品,所述层合的玻璃窗制品至少依次包括第一玻璃窗材料层、第一机械能吸收层、根据权利要求1所述的阳光控制膜、第二机械能吸收层和第二玻璃窗材料层。
13.根据权利要求12所述的制品,其中所述制品的可见光透射率为至少70%,总太阳热透射率小于60%,并且反射能量为至少20%。
14.根据权利要求12所述的制品,其中所述制品的可见光透射率为至少75%,总太阳热透射率小于60%,并且反射能量为至少25%。
15.一种用于形成阳光控制膜的方法,所述方法包括:
a)提供能透射可见光的柔性载体;
b)在所述载体的顶上形成第一不连续成核氧化物晶种层,所述第一不连续成核氧化物晶种层形成为一系列小的岛状物;
c)在所述第一不连续成核氧化物晶种层的顶上形成第一金属层;
d)在所述第一金属层的顶上形成有机间隔层;
e)在所述有机间隔层的顶上形成第二不连续成核氧化物晶种层,所述第二不连续成核氧化物晶种层形成为一系列小的岛状物;
f)在所述第二不连续成核氧化物晶种层的顶上形成第二金属层;以及
g)在所述第二金属层的顶上形成能透射可见光的聚合物型保护层;
其中所述不连续成核氧化物晶种层各自具有大于0并小于5nm的物理厚度,所述金属层各自具有5至12nm的物理厚度,所述有机间隔层具有1.3至1.7的折射率以及75至275nm的光学厚度,并且其中所述阳光控制膜能透射可见光并且能反射红外线。
16.根据权利要求15所述的方法,其中所述载体包括多层光学膜。
17.根据权利要求15所述的方法,还包括在所述载体和所述第一不连续成核氧化物晶种层之间形成有机基部涂层。
18.根据权利要求15所述的方法,其中对应于所述阳光控制膜的法向轴线在0°的入射角处进行测量时,包括所述阳光控制膜的层合的安全玻璃窗制品表现出至少70%的可见光透射率。
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KR20100103832A (ko) | 2010-09-28 |
US20100316852A1 (en) | 2010-12-16 |
KR101550946B1 (ko) | 2015-09-07 |
JP2011509193A (ja) | 2011-03-24 |
BRPI0821436A2 (pt) | 2015-06-16 |
WO2009085741A2 (en) | 2009-07-09 |
CN101909873A (zh) | 2010-12-08 |
US9034459B2 (en) | 2015-05-19 |
WO2009085741A3 (en) | 2009-10-01 |
EP2231395A2 (en) | 2010-09-29 |
JP5475685B2 (ja) | 2014-04-16 |
EP2231395A4 (en) | 2014-01-29 |
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