CN101044283A - 改进的透气性、低发射率镀金属片材 - Google Patents
改进的透气性、低发射率镀金属片材 Download PDFInfo
- Publication number
- CN101044283A CN101044283A CNA2005800362637A CN200580036263A CN101044283A CN 101044283 A CN101044283 A CN 101044283A CN A2005800362637 A CNA2005800362637 A CN A2005800362637A CN 200580036263 A CN200580036263 A CN 200580036263A CN 101044283 A CN101044283 A CN 101044283A
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- sheet
- coating
- composite sheet
- layer
- plating
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Links
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Classifications
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N7/00—Flexible sheet materials not otherwise provided for, e.g. textile threads, filaments, yarns or tow, glued on macromolecular material
- D06N7/0094—Fibrous material being coated on one surface with at least one layer of an inorganic material and at least one layer of a macromolecular material
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Abstract
一种湿蒸汽可透镀金属复合片材通过湿蒸汽可透片材涂以至少一个金属层和至少一个外有机涂层而制成。该复合片材的湿蒸汽通透性是初始片材湿蒸汽通透性的至少约80%。该复合片材提供对空气和液态水渗入的阻挡,同时具有高湿蒸汽渗透性和良好隔热性能。该复合片材材料适合用作建筑结构包裹材料如屋顶衬和住房包裹材料。
Description
背景技术
1.技术领域
本发明涉及具有改进的湿蒸汽渗透性和隔热性,适合作为建筑结构中的热障使用的镀金属(metalized)片材。
2.相关技术的描述
本领域已知在建筑结构中使用湿蒸汽可透(透气性(breath able))镀金属片材作为住房包裹材料(wrap)。该镀金属片材允许湿蒸汽透过片材,从而防止湿气在安装于片材后面的绝热层内凝结,同时提供对空气和液态水的阻挡并提高建筑物的能量效率。美国专利号4,999,222,授予Jones等人,描述一种具有低发射率的湿蒸汽可透镀金属聚乙烯片材,它是通过压光超细纤维丛丝状薄膜-原纤片材,随后真空镀金属制成的。美国专利号4,974,382,授予Avellanet,描述一种蒸汽可透或不透性防渗入和能量阻挡层,其表面具有至少一个镀金属层。公开的PCT国际申请号WO 01/28770,授予Squires等人,描述一种透气性建筑膜,包括微孔膜底层和由丝状聚合物布料,例如,纺粘布,成形的顶(top)层,该顶(top)层备有湿蒸汽可透反射性金属涂层。虽然上面描述的透气性镀金属片材通过反射红外辐射来提供热障,但它们容易在暴露于空气和潮湿后金属层发生氧化。氧化的金属层通常具有比对应金属高的发射率,因此作为热障其效率较低。另外,外露的薄金属层会在加工、安装之类期间受到损伤。
公开的欧洲专利申请号EP 1400348,授予Avril等人,描述一种液体不可透、湿蒸汽/气体可透层合布,适合用作建材布料,例如,住房包裹材料和屋顶衬底,包括反射薄膜层,它是通过在第一聚合物薄膜层上蒸汽沉积金属层并将该金属层夹在第一聚合物薄膜层与第二聚合物薄膜层之间制成的。薄膜层保护金属层以免在使用期间损伤但不透湿气,而是在镀金属以后经微穿孔获得所要求的湿蒸汽渗透性的。
已涂有机聚合物涂层的镀金属非织造布已知被用于建筑最终用途,例如,住房包裹材料。然而,该聚合物涂层是采用,与未涂布的镀金属非织造布片材相比,显著降低湿蒸汽渗透性的方法施涂的。美国专利申请公开号2003/0136078,授予Brown等人,描述一种给建筑物热绝缘的方法,包括在外包层与框架之间的空腔内引入包含反射层和透气性纺织物层的绝缘膜的步骤。该镀金属层可任选地涂以塑料或清漆保护层以保护金属表面。
当湿蒸汽可透片材沿着基本上整个表面采用传统方法,例如,气刀涂布、苯胺印刷、凹版印刷等涂布时,涂层将降低片材的湿蒸汽渗透性。如果初始片材具有稀松(open)结构并且是高度透气的,则在涂布以便用于某些最终用途,例如,服装之后,该片材将保持充分的湿蒸汽渗透性。例如,在授予Culler的美国专利号5,955,175中所描述的布料在镀金属并涂以疏油涂层后将既透空气也透湿蒸汽。然而,当初始湿蒸汽可透片材具有高度封闭的结构,其透气性将非常低,例如,用非织造布和其它作为建筑结构中住房包裹材料或屋顶衬的片材时,则传统涂层将导致片材表面上的孔隙被显著地覆盖。这将导致所涂布的片材具有明显低于初始片材的湿蒸汽渗透性。这对于作为住房包裹材料和屋顶衬产品是不可心的,因为希望这样的材料可透湿蒸汽,同时又形成阻挡空气和液态水渗入的屏障。
若能提供一种镀金属片材,它具有对液态水的高阻挡能力,并且具有高湿蒸汽渗透性和优良隔热性能,适用于建筑用途,例如,住房包裹材料和屋顶衬,则将是可心的。
发明概述
按照第一实施方案,本发明涉及一种镀金属复合片材,它包含具有第一和第二外表面的湿蒸汽可透片材层,该片材层包含非织造布、机织织物、非织造布-薄膜层合物、机织织物-薄膜层合物、湿蒸汽可透薄膜及其复合材料至少之一,其中湿蒸汽可透片材层的第一外表面是多孔片材,选自微穿孔薄膜、机织织物和非织造布,以及在该片材层的所述第一外表面上的至少一个多层涂层,所述多层涂层包含与该片材层的第一外表面相邻、厚度介于约15nm~200nm的第一金属涂层,以及沉积在该金属层上的厚度介于约0.2μm~2.5μm的外有机涂层,其组成包含选自有机聚合物、有机低聚物及其组合的材料,其中复合片材的湿蒸汽透过速率(MVTR)是沉积该金属和涂层之前测定的片材层MVTR的至少约80%。
在替代的实施方案中,本发明镀金属复合片材可具有一种多层涂层,它还包含沉积在湿蒸汽可透片材层第一外表面、介于片材层与金属涂层之间、厚度介于约0.02μm~2μm的中间有机涂层,其组成包含选自有机聚合物、有机低聚物及其组合的材料,其中中间与外有机涂层的总合计厚度不大于约2.5μm。
本发明另一实施方案涉及一种镀金属复合片材,它包含具有第一和第二外表面的多孔闪纺超细纤维丛丝状片材层,和至少一个多层涂层,后者包含沉积在该闪纺超细纤维丛丝状片材层第一外表面上、厚度介于约15nm~200nm的金属涂层,所述金属选自铝、银、铜、金、锡、锌及其合金,以及沉积在金属层上、厚度介于约0.2μm~1μm的其组成含交联聚丙烯酸酯的外有机涂层,其中多层涂层基本上覆盖闪纺超细纤维丛丝状片材的外表面但使得孔隙基本未覆盖。
本发明另一替代实施方案涉及一种镀金属复合片材,它包含具有第一和第二外表面的多孔闪纺超细纤维丛丝状片材层,和至少一个多层涂层,后者包含沉积在所述闪纺超细纤维丛丝状片材层的第一外表面、厚度介于约0.02μm~1μm的中间有机涂层,其组成包含交联的聚丙烯酸酯,沉积在所述中间有机涂层上、厚度介于约15nm~200nm的金属涂层,所述金属选自铝、银、铜、金、锡、锌及其合金,以及沉积在金属层上、厚度介于约0.2μm~1μm的外有机涂层,其组成含交联聚丙烯酸酯,其中多层涂层基本上覆盖闪纺超细纤维丛丝状片材的外表面,但使得孔隙基本未覆盖。
附图简述
图1是适用于形成本发明复合片材的设备的示意图。
图2A和2B是原子力显微照片,分别显示未涂布和聚丙烯酸酯-涂布的高密度聚乙烯超细纤维丛丝的表面特征。
图3是本发明墙壁系统的示意图。
图4A~4C是本发明屋顶系统的示意图。
图4D是展示镀金属复合片材在一顶楼中地板托架上的安装的示意图。
图5是实施例7的复合片材和现有技术(in cumbent)镀金属和未镀金属住房包裹材料的屏蔽效力对EMF频率的曲线图。
图6是实施例8的复合片材和现有技术镀金属和未镀金属住房包裹材料的屏蔽效力对EMF频率的曲线图。
发明详述
术语“非织造布”、“非织造布片材”、“非织造布层”和“非织造纤网”在这里被用来指由单根丝(例如,纤维、长丝或单纱)以无规方式铺置形成平面材料,而不是像针织或机织织物那样按可辨认的图案,所构成的结构。术语“纤维”在这里被用来涵盖短纤维以及连续长丝。非织造布的例子包括熔喷纤网、纺粘非织造布纤网、闪纺纤网、基于短纤维的纤网,包括梳理和气流铺网的纤网,射流喷网纤网和包含一种以上非织造纤网的复合片材。
术语“机织片材”在这里被用来指通过织造一种经纱和纬纱交叉的组织所成形的片材结构。
术语“纺粘纤维”在这里被用来指按如下方法熔纺的纤维:将熔融热塑性聚合物材料从纺丝板的大量细小,通常为圆形的纺丝孔中挤出成为纤维,随后通过拉伸,再骤冷该纤维使挤出纤维的直径迅速减小。
术语“熔喷纤维”在这里被用来指通过熔喷方法熔纺的纤维,包括将可熔融加工聚合物以熔融流股的形式挤过大量毛细孔,进入到高速气(例如,空气)流中。
术语“纺粘-熔喷-纺粘非织造布”(″SMS″)在这里被用来指一种多层复合片材,它包含在2个纺粘层之间并与其粘合着一层熔喷纤维纤网。在该复合片材中可加入附加的纺粘和/或熔喷层,例如,纺粘-熔喷-熔喷-纺粘纤网(″SMMS″),等。
术语“超细纤维丛丝状”在这里被用来指由无规长度的薄、带状、薄膜-原纤基元组成的三维整体网络或纤网,平均膜厚小于约4μm,中位数原纤宽度小于约25μm。在超细纤维丛丝状结构中,薄膜-原纤基元通常沿结构的纵轴共延伸地排齐并且它们按不规则的间距在沿结构的长度、宽度和厚度不同的地方到处断断续续地结合再分开,从而形成连续的三维网络。超细纤维丛丝状薄膜-原纤基元组成的非织造纤网在这里被称作“闪纺超细纤维丛丝状片材”。
这里所使用的术语“带”指的是扁平状的单纱,例如,由劈切膜构成的扁平纱。
这里所使用的术语“金属”包括金属合金以及金属。
术语“墙壁系统”在这里用来指建筑结构的墙壁。墙壁系统包括内衬和外皮层以及夹在内衬和外皮层之间的其它墙壁要素。中间要素可包括支撑框架要素,例如,垂直木壁骨、至少一个空气空间、隔热材料、任选的蒸汽阻挡层,以及本发明湿蒸汽可透镀金属复合片材。
术语“屋顶系统”在这里被用来指建筑结构中的屋顶。屋顶系统包括支撑屋顶框架要素如涂沥青的木椽,外屋顶材料和其它屋顶要素。屋顶系统可划分为暖屋顶系统和冷屋顶系统。在冷屋顶系统中,其它屋顶要素可以包括任选的蒸汽阻挡层、至少一个空气空间(它可以是顶楼空气空间)、夹在支撑屋顶框架要素与外屋顶材料如板条或实心盖板之间的元素、本发明湿蒸汽可透镀金属复合片材,以及安装在顶楼空间的地板标高、高于屋内天花板标高的隔热材料。在暖屋顶系统中,其它屋顶要素可包括,除了上面针对冷屋顶系统列举的之外,顶楼天花板和安装在顶楼天花板上方(而不是在顶楼空间的地板标高)的隔热层。其它屋顶要素可夹在支撑屋顶框架要素与外屋顶材料中间,或者可固定在支撑屋顶框架要素的面朝顶楼空间这一侧,或者安装在相邻的屋顶框架要素之间,等等,视具体屋顶要素而定。
在一种实施方案中,本发明涉及一种镀金属湿蒸汽可透复合片材,它是通过在湿蒸汽可透片材层的至少一侧涂以至少一个金属层,并在金属层的背向片材层的那侧涂以至少一个薄有机涂层而制成的。涂层优选在真空下采用蒸汽沉积技术在基本上覆盖片材层却不明显降低其湿蒸汽渗透性的条件下形成。复合片材具有高湿蒸汽渗透性和优良隔热性能。该复合片材也可选择为能提供对液态水的渗入的高阻挡能力(高静水压头),这对于作为建筑的最终用途如住房包裹材料和屋顶衬来说也很重要。本发明复合片材所提供的性能的均衡性优于目前可获得的建筑工业中使用的镀金属片材。本发明复合片材提供一种薄、结实、透气的热障,适合用于现有或新的结构中。本发明复合片材,当用作墙壁和/或屋顶系统中的热障时,有利于满足有关新建和翻修建筑物要求有较高能量效率的建筑规范。
本发明复合片材包括以下结构:片材/M/L2、片材/L1/M/L2和片材/L1/M/L2/M/L3等,其中片材是湿蒸汽可透片材层、M是低发射率金属层,L1、L2和L3是包含有机聚合物或有机低聚物或其共混物的有机涂层。缩写“L1”在这里被用来指先沉积在片材层表面上,然后再在其上沉积金属层的任选中间有机涂层。该中间涂层据发现能改善该复合片材的隔热性能,与不包括中间涂层的复合片材相比。该复合片材包括至少一个覆盖在金属层上面的外有机涂层,如上面描述的结构中的L2和L3。在具有多于1个金属层的复合片材结构中,各单个金属层可由相同或不同金属形成并且可具有相同或不同的厚度。类似地,在具有多于1个有机涂层的结构中,各单个有机涂层可具有相同或不同的组成和/或厚度。每个金属层可包含多于1个相邻的金属层,其中相邻金属层可相同或不同。类似地,每个有机层可包含多于1个相邻有机层,其中相邻有机层可相同或不同。该片材可在一侧涂布,正如在上面的结构中那样,或者在两侧都涂布,例如,在下面的结构中:L2/M/片材/M/L2、L2/M/L1/片材/L1/M/L2等。
在本发明一种实施方案中,湿蒸汽可透片材层的一或两侧包含多孔外表面,例如,涂以有机和金属层的纤维表面或多孔薄膜。该有机和金属层沉积在多孔表面上,使得在涂布侧(们)的纤维或薄膜的外露或“外”表面被涂布,而不覆盖孔隙。这包括纤维之间的间隙空间或孔隙的壁的内表面,以及当从涂布那侧(们)的片材层外表面看去外露的纤维表面;但布料内部结构中的纤维表面则依然未涂布。
适合形成本发明复合片材的湿蒸汽可透片材层可具有较低空气渗透性,例如,介于约5~约12,000Gurley秒,甚至介于约20~约12,000Gurley秒,甚至介于约100~约12,000Gurley秒,甚至介于约400~约12,000Gurley秒,这样的水平一般认为能提供对空气渗入的阻挡。替代地,湿蒸汽可透片材层可选择为具有较高空气渗透性,例如,Gurley Hill空气渗透性小于5s的那些片材,其空气渗透性落在Frazier空气渗透性范围内。具有较高空气渗透性的复合片材可具有至少约35g/m2/24h的湿蒸汽参透性,甚至至少约200g/m2/24h,甚至至少约600g/m2/24h以及至少约20cm H2O的静水压头,甚至至少约50cm H2O的静水压头,甚至至少约100cm H2O的静水压头,甚至至少约130cmH2O的静水压头。当作为住房包裹材料使用时,复合片材优选具有至少约35N/cm的抗张强度。
适合的湿蒸汽可透片材层是多孔片材,包括机织织物如机织纤维或带的片材,或者非织造布,例如,闪纺超细纤维丛丝状片材、纺粘非织造布片材、纺粘-熔喷非织造布片材、纺粘-熔喷-纺粘非织造布片材,和包括非织造布或机织织物或稀松布层和湿蒸汽可透薄膜层,例如,微孔薄膜、微穿孔薄膜或湿蒸汽可透整体薄膜,的层合物。初始片材层可包含预先采用传统涂布方法涂布的湿蒸汽可透片材。例如,目前在建筑工业中使用的片材包括预先涂以聚合物薄膜层并微穿孔的机织带的片材。片材层可由各种各样聚合物组合物形成。例如,建筑工业中使用的片材一般由聚烯烃如聚丙烯或高密度聚乙烯、聚酯,或聚酰胺形成。
在一种实施方案中,湿蒸汽可透片材是一种闪纺超细纤维丛丝状聚烯烃片材,例如,Tyvek闪纺高密度聚乙烯,由杜邦公司E.I.du Pontde Nemours and Company,Inc.(Wilminton,DE)供应。合适的闪纺超细纤维丛丝状薄膜-原纤材料也可由聚丙烯制成。湿蒸汽可透片材可以是由闪纺超细纤维丛丝状片材与1或多个附加层组成的层合物,例如,包含闪纺超细纤维丛丝状片材和熔纺纺粘片材的层合物。形成超细纤维丛丝状薄膜-原纤单纱材料的纤网层的闪纺方法公开在美国专利号3,081,519(Blades等人)、3,169,899(Steuber)、3,227,784(Blades等人)、3,851,023(Brethauer等人),在此将其内容收入本文作为参考。
湿蒸汽可透片材可以是市售供应的住房包裹材料或屋顶衬产品。建筑结构中使用的闪纺超细纤维丛丝状片材包括TyvekSUPRO屋顶衬、TyvekHomeWrap、TyvekCommercialWrap。适合作湿蒸汽可透片材层的其它住房包裹产品包括Air-GuardBuildingwrap(由Fabrene公司,North Bay,安大略,制造),这是一种高密度聚乙烯劈切膜的机织织物,由单面涂以加入白颜料并微穿孔的聚乙烯构成,PinkwrapHousewrap(由Owens Corning,Toledo,OH,制造),这是一种聚丙烯劈切膜的机织织物,单面涂布并穿孔,Pinkwrap PlusHousewrap(由Owens Corning,Toledo,OH,制造),这是一种交叉铺置的层合聚烯烃薄膜,进行过微穿孔并具有波纹状表面,Tuff WrapHousewrap(由Cellotex公司,Tampa,FL,制造),这是一种一面涂层并穿孔的高密度聚乙烯薄膜的机织织物,Tuff Weather Wrap(由Cellotex公司,Tampa,FL,制造),这是一种聚烯烃片材粘合到一种压花以便在表面形成小凹窝的非织造稀松布上,Greenguard UltraAmowrap(由Amoco(Smyrna,GA)制造),这是一种一面涂布并穿孔的聚丙烯劈切膜的机织织物,Weathermate Plus Housewrap(由Dow化学公司(Midland,MI)制造),这是一种涂以透明涂层、未穿孔的非织造膜,以及TyparHousewrap(由Reemay,Old Hickory,TN)制造),这是一种涂布的纺粘聚丙烯片材。
在某些情况下,可心的是使用基本上是空气不可渗透的湿蒸汽可透片材层。例如,湿蒸汽可透片材层可包含非织造布或机织织物或稀松布与湿蒸汽可透薄膜层的层合物,其中湿蒸汽可透薄膜层是一种微孔薄膜或整体薄膜。一般而言,一或多种湿蒸汽可透薄膜层被夹在外非织造布或机织织物或稀松布层之间,而金属和有机涂层则沉积在外层至少之一上面,因此外有机涂层构成复合片材的外表面。在一种此类实施方案中,湿蒸汽可透薄膜层被夹在2个短纤维非织造布层,或2个连续长丝非织造布层,或2片机织织物之间。该外布层或稀松布层可相同或不同。
湿蒸汽可透整体(无孔)薄膜由可作为薄、连续湿蒸汽可透,并且基本上不透液的薄膜挤出的聚合物材料来形成。薄膜层可利用传统挤出涂布方法直接挤出到第一非织造布或机织基材层上。优选的是,整体薄膜的厚度不大于约3密耳(76μm)厚,甚至不大于约1密耳(25μm)厚,甚至不大于约0.75密耳(19μm)厚,甚至不大于约0.60密耳(15.2μm)厚。在挤出涂布方法中,挤出的层和基材层一般被送过2个辊筒(加热或不加热)之间形成的辊隙,通常在薄膜层完全固化之前,以便改善各层之间的粘合。第二非织造布或机织基材层可引入到薄膜的与第一基材相反的一侧上的辊隙中,结果形成湿蒸汽可透、基本上不透空气的层合物,其中整体薄膜被夹在2个基材层之间。
适合形成湿蒸汽可透整体薄膜的聚合物材料包括嵌段聚醚共聚物如嵌段聚醚酯共聚物、聚醚酰胺共聚物、聚氨酯共聚物、聚(醚酰亚胺)酯共聚物、聚乙烯醇或其组合。优选的共聚醚酯嵌段共聚物是具有软聚醚链段和硬聚酯链段的嵌段弹性体,正如在Hagman,美国专利号4,739,012中公开的,在此将其收入本文作参考。合适的共聚醚酯嵌段共聚物包括Hytrel共聚醚酯嵌段共聚物,由杜邦公司(E.I.du Pont deNemours and company)(Wilmington,DE)销售,和Arnitel聚醚酯共聚物,由DSM Engineering Plastics(Heerlen,荷兰)制造。适合的共聚醚酰胺聚合物是由Atochem公司(Glen Rock,N.J.,USA)以商品名Pebax销售的共聚酰胺。Pebax是Elf Atochem(S.A.of Paris,法国)的注册商标。合适的聚氨酯是由固特异公司(克里夫兰,俄亥俄,美国)以商品名Estane销售的热塑性聚氨酯。合适的共聚(醚酰亚胺)酯描述在Hoeschele等人的美国专利号4,868,062中。整体薄膜层可由多层湿蒸汽可透薄膜层构成。此类薄膜可以是共挤出的,其中的层由1或多种上面描述的透气性热塑性薄膜材料构成。
微孔薄膜是本领域公知的,例如,由聚烯烃(例如,聚乙烯)和细颗粒填料的混合物形成的那些,该混合物经熔融挤出,流延或吹胀成为薄膜并进行拉伸,或者单轴或者双轴,最后形成形状不规则的连续延伸薄膜上下表面的微孔。美国专利5,955,175公开一种微孔薄膜,它具有约0.2μm的公称孔隙尺寸。微孔薄膜可利用本领域已知的方法,例如,热或粘合剂层合方法,层合到非织造布或机织层之间。
微穿孔薄膜通过将聚合物流延或吹胀变成薄膜,随后给薄膜机械地穿孔而制成,正如在欧洲专利公开号EP 1 400 348 A2中一般地公开的,该公开物中指出,微穿孔一般介于0.1mm~1.0mm直径的数量级。
按照本发明,金属和有机涂层利用基本上不降低片材的湿蒸汽渗透性的方法沉积到多孔片材上。该涂层沿着基本上整个片材的表面沉积,但使得材料的孔隙口基本上未覆盖。按照本发明一种实施方案,该湿蒸汽可透片材层包含纤维非织造布或机织织物。替代地,该湿蒸汽可透片材层可以是布料-薄膜层合物,其中布料包含层合物的外表面,或者层合物的外表面可以是微穿孔的薄膜。将金属和有机涂层沉积到布料或微穿孔薄膜上,结果,在布料的情况下,在复合片材涂布表面的单根布料纱线外露表面被基本上覆盖,但使得单纱之间的间隙或孔隙基本上未被涂复材料覆盖。所谓“基本上未覆盖”是指,纤维之间的间隙空间的至少35%不含涂料。在一种实施方案中,有机涂层的总合计厚度小于非织造纤网的纤维的直径。在非纤维片材的情况下,片材表面上的表面孔隙的至少35%基本上未被覆盖。这提供了一种湿蒸汽渗透性是初始片材材料的湿蒸汽渗透性的至少约80%,甚至至少约85%,甚至至少约90%的涂布复合片材。
当比较涂布的复合片材的湿蒸汽渗透性与未涂布初始片材的湿蒸汽渗透性时,作为对照样使用的初始片材应与要比较湿蒸汽渗透性的具体复合片材所使用的初始片材材料基本上等效。例如,应使用与制造涂布片材所使用的同一卷或批次等的片材样品来测定初始片材的湿蒸汽渗透性。可在涂布前遮盖一段片材层,以便使被遮盖的段在涂布加工期间不被涂布,然后从片材的相邻未涂布和涂布的部分取样并测定。替代地,未涂布样品可取自片材层的那卷的开头和/或末尾,并与由同一卷制成的涂布样品进行比较。
鉴于涂层不连续覆盖孔隙,故湿蒸汽渗透性不明显地受到影响。本领域已知的真空蒸汽沉积方法优选用于沉积该金属和有机涂层。金属和有机涂层的厚度优选控制在能提供具有不超过约0.15,甚至不超过约0.12,甚至不超过约0.10发射率的复合片材的范围。
外有机涂层的厚度和组成应选择得,除了基本上不改变片材层的湿蒸汽渗透性之外,它也不明显增加镀金属基材的发射率。外有机涂层优选的厚度介于约0.2μm~2.5μm,这对应于约0.15g/m2~1.9g/m2有机涂层材料。在一种实施方案中,外涂层的厚度介于约0.2μm~1.0μm(约0.15g/m2~0.76g/m2),或者介于约0.2μm~0.6μm(约0.15g/m2~0.46g/m2)。当采用中间涂层时,中间与外有机涂层的合计厚度优选不超过约2.5μm,甚至不超过约2.0μm,甚至不超过约1.5μm,以保证湿蒸汽可透片材的表面上的孔隙基本上未覆盖。在一种实施方案中,中间与外有机涂层的合计厚度不超过约1.0μm。就结构,片材/L1/M/L2而言,中间涂层的厚度优选介于约0.02μm~2μm,对应于约0.015g/m2~1.5g/m2。在一种实施方案中,中间涂层的厚度介于约0.02μm~1μm(0.015g/m2~0.76g/m2)或介于约0.02μm~0.6μm(0.015g/m2~0.46g/m2)。当沉积附加金属和有机涂层时,应调节每个有机涂层的厚度,使得所有有机涂层的总合计厚度不超过约2.5μm,或不超过约1.0μm。如果外有机涂层过薄,它可能不能保护金属层免遭氧化,从而导致复合片材发射率的增加。如果外有机涂层过厚,则复合片材的发射率可能增加,从而造成隔热性能较低。
可心的是,在某些情况下的中间有机涂层非常薄,例如,介于约0.02μm~0.2μm(约0.015g/m2~0.15g/m2)。一种此类例子是当片材层包含闪纺超细纤维丛丝状或其它非织造片材,其中超细纤维丛丝或纤维在其表面具有等于或小于500nm数量级的特征时。此特征比非织造片材的表面“宏观粗糙”细小得多,其中宏观粗糙特征乃是由纤维本身(峰和谷)以及纤维之间的间隙造成的。图2A是一幅原子力显微照片(AFM),显示由单根未涂布高密度聚乙烯超细纤维丛丝表面上的无定形区域(暗)和结晶薄片造成的表面特征。结晶薄片(lamellae)的厚度大约为25nm,长120~450nm。重要的是,片材的宏观粗糙不因镀金属和涂层而明显改变,因为这样作将导致纤维之间的间隙空间缩小或被堵塞并导致片材湿蒸汽渗透性的降低。非常薄的聚合物层将使存在于单根纤维表面的微观-粗糙光滑,而不影响纤维片材的宏观-粗糙。在闪纺聚乙烯的情况下,涂层将需要至少与聚乙烯片状结晶一样厚,后者为约25nm厚。图2B是涂以约25nm厚聚丙烯酸酯聚合物蒸汽沉积层的高密度聚乙烯超细纤维丛丝的表面AFM。比较图2B与图2A,可以看出,涂布的超细纤的表面已被聚丙烯酸酯涂层光滑化,却又不影响片材的宏观-粗糙。一般而言,厚度超过纤维或其它表面的平均微观-粗糙特征的有机涂层L1将使纤维表面变得光滑。此种光滑作用可使单根纤维表面的金属层变得更光滑,从而,与不包括L1的片材相比,降低复合片材的发射率。例如,厚度介于约0.025μm~0.2μm的中间涂层L1适合用于闪纺聚乙烯片材。
适合有机涂层(们)的组合物包括聚丙烯酸酯聚合物和低聚物。涂层材料可以是交联的化合物或组合物。适合制备有机涂层的前体化合物包括真空相容的单体、低聚物或低分子量聚合物及其组合。真空相容单体、低聚物或低分子量聚合物应具有高到足以在蒸发器中迅速蒸发从而不发生热降解或聚合的蒸气压,同时其蒸气压又不应高到主导真空系统的程度。蒸发的容易程度取决于单体、低聚物或聚合物的分子量及分子间力。典型地,可用于本发明的真空相容单体、低聚物和低分子量聚合物的重均分子量可最高至约1200。本发明中使用的真空相容单体优选是辐射可聚合单体,或者自己或者借助光引发剂,并包括以羟基、醚、羧酸、磺酸、酯、胺和其它官能团官能化的丙烯酸酯单体。涂层材料可以是疏水化合物或组合物。涂层材料可以是可交联、疏水和疏油的氟化丙烯酸酯聚合物或低聚物,按照本发明一种优选的实施方案。真空相容低聚物或低分子量聚合物包括按如上所述官能化的二丙烯酸酯、三丙烯酸酯和更高分子量的丙烯酸酯,脂族、脂环族或芳族低聚物或聚合物以及氟化的丙烯酸酯低聚物或聚合物。氟化丙烯酸酯,表现出非常低的分子间相互作用,用于本发明,可具有最高约6000的重均分子量。优选的丙烯酸酯在分子中具有至少一个双键,优选至少2个双键,以便提供高速的聚合。可用于本发明涂层中的丙烯酸酯以及该丙烯酸酯平均分子量的例子描述在美国专利6,083,628和WO 98/18852中。
适合形成本发明复合片材的金属层(们)的金属包括铝、金、银、锌、锡、铅、铜和它们的合金。金属合金可包括其它金属,只要该合金组合物提供低发射率复合片材。每个金属层的厚度介于约15nm~200nm,或介于约30nm~60nm。在一种实施方案中,金属层包含厚度介于约15~150nm,或介于约30~60nm的铝。形成金属层的方法在本领域是公知的,包括电阻蒸发、电子束金属蒸汽沉积,或溅射。如果金属层过薄,则所要求的隔热性能将达不到。如果金属层过厚,则它可能龟裂和剥落。一般而言,优选使用能提供要求的隔热性能的最低金属厚度。当采用本发明复合片材作为住房包裹材料或屋面衬时,金属层将反射红外辐射或很少发射红外辐射,从而提供减少能量损失和保持建筑物冬暖夏凉的隔热性能。
一种材料的隔热性能可用其发射率表征。发射率是某一表面辐射的与在同样温度下黑体辐射的单位面积的功率之比。因此,黑体的发射率是1,而理想反射体的发射率是0。发射率越低,隔热性能越高。每一金属层和相邻外有机涂层优选地在真空、不暴露于空气和氧的作用下顺序地进行沉积,以便使金属层基本上不氧化。抛光铝的发射率介于0.039~0.057,银的介于0.020~0.032,金介于0.018~0.035。一层未涂布的铝通常在暴露于空气和潮湿后立即在其表面形成薄氧化铝层。该氧化膜的厚度在几小时的时间里随着继续暴露于空气中而增加,此后,氧化层达到阻止或明显阻碍氧与金属层接触的厚度,从而能减少进一步的氧化。氧化铝的发射率介于约0.20~0.31。通过在铝层暴露于大气之前沉积外有机涂层从而最大限度地减少铝的氧化程度,复合片材的发射率比未保护的铝层明显改善。外有机涂层也保护金属免遭在卷材搬运、运输和最终使用安装期间的机械磨损。
图1是适用于片材层在真空下蒸汽沉积涂布有机和金属层的设备10的示意图。在下面的描述中,术语“单体”被用来指可蒸发单体、低聚物和低分子量聚合物。真空室12连接真空泵14,后者将真空室抽真空到要求的压力。合适的压力介于2×10-4~2×10-5Torr(2.66×10-5~2.66×10-6kPa)。湿蒸汽可透片材20通过导辊24从退绕辊18喂入到冷却转鼓16上,转鼓沿箭头″A″所示方向旋转。转鼓16的表面速度一般介于1~1000cm/s。片材穿过几个沉积站,随后它被导辊26从转鼓表面揭下并随后由卷取辊22卷绕成为涂布的复合片材。转鼓16被冷却到用于形成有机涂层的具体单体特有的温度,并可冷却到-20℃以促使单体的凝结。从辊18退绕以后,片材层穿过任选的等离子处理单元36,在此,片材的表面暴露于等离子体以赶出吸附的氧、潮湿以及任何存在于片材表面的任何低分子量化学种,然后再在其上成形金属或单体涂层。通常对基材表面能量进行改性,以改善该表面被涂料(coatinglayers)的润湿。等离子源可以是低频RF、高频RF、DC或AC。合适的等离子处理方法描述在美国专利号6,066,826、WO 99/58757和WO99/59185中。
任选在沉积金属层之前在片材层上形成中间有机层。在一种实施方案中,有机单体由单体蒸发器28沉积到湿蒸汽可透片材层上,蒸发器由储罐40通过超声波雾化器42获得液态单体进料,在雾化器中,借助加热器(未画出),液态单体被瞬间蒸发,即,闪蒸蒸发,以便最大限度减少在沉积到片材层上之前聚合或热降解的机会。该单体、低聚物或低分子量聚合物液体或淤浆在将它以蒸汽的形式注入到真空室去之前优选地进行脱气,正如在美国专利号5,547,508中描述的,在此收入本文作参考。闪蒸和单体沉积过程的具体方面详细地描述在美国专利号4,842,893;4,954,371;和5,032,461,在此将它们全部收入本文作参考。
闪蒸的单体在片材表面凝结并形成液态单体薄膜层。该单体涂层薄到足以不显著覆盖片材层的孔隙,以便使复合片材的湿蒸汽渗透性至少是初始片材层的约80%。凝结的液态单体在凝结到片材上去之后的数毫秒时间内便借助辐射固化装置30固化。合适的辐射固化装置包括通过引起凝结层的聚合或交联来固化单体薄膜层的电子束和紫外线辐射源。如果采用电子束枪,则电子的能量应足以使涂层沿其整个厚度发生聚合,正如在美国专利号6,083,628中描述的,在此收入本文作参考。单体和低聚物层的聚合或固化也描述在美国专利号4,842,893、4,954,371和5,032,461中。替代地,低聚物或低分子量聚合物可在冷却的同时凝固。由于低聚物或低分子量聚合物在室温下为固体,所以可能不需要固化,正如在美国专利6,270,841中描述的,在此将其收入本文作参考。
沉积了中间有机层之后,涂布的片材层随后被送到镀金属系统32,在此,金属层被沉积到固化并任选地固化的有机层上。当采用电阻金属蒸发系统时,镀金属系统被连续地供应来自金属丝进料44的金属源。
在镀金属步骤之后,按照类似于上面针对中间聚合物层所描述的方法利用蒸发器128、单体储罐140、超声波雾化器142和辐射固化装置130沉积外有机涂层。外有机涂层的组成可与中间有机涂层相同或不同。任选地,片材层的金属或有机涂层的一侧可先接受等离子处理,然后再在其上沉积附加有机或金属涂层。
该涂层的厚度由蒸汽沉积方法中使用的闪蒸蒸发器的线速度和蒸汽流量控制。随着涂层厚度的增加,电子束的能量必须不断调节以便使电子穿透涂层并达到有效的聚合。例如,10kV和120mA的电子束能有效地聚合最高2μm厚的丙烯酸酯涂层。
如果要求1个以上金属层和/或2个以上有机层,则可在真空室内增设附加的闪蒸蒸发设备和镀金属站。替代地,可先让片材层在图1所示设备中第一次通过以接受涂布,然后取出涂布的片材并让它第二次通过该设备。替代地,镀金属和有机涂布步骤可分别使用各自的设备。本领域技术人员将会认识到,要求的话,可在片材层的反面施加涂层,可在真空室12内增设第二转鼓16,连同附加的等离子处理单元36、单体蒸发器28、128,辐射固化装置30、130和镀金属系统32,这些都可按要求独立地操作。此种双鼓涂布系统表示在WO 98/18852的图1中,在此收入本文作为参考。优选的是,先在金属层上沉积有机涂层,然后再从真空室中取出涂布的片材,以防止金属层的显著氧化。最优选在单程中就沉积上有机涂层(们)和金属层(们)以最大限度地降低加工成本。
本发明镀金属复合片材尤其适合用于建筑结构中的屋顶和墙壁系统。该复合片材的高反射性镀金属表面提供低发射率表面,从而提高隔热表现和改善墙壁和屋顶系统的能量效率,进而降低建筑物业主的燃料花费。附加的好处包括在寒冷气候中大大减少在墙和屋顶结构内的凝结以及在夏天月份荫庇建筑物避免过热。在本发明一种实施方案中,该湿蒸汽可透复合片材被用于墙壁和屋顶系统中,并具有不大于约0.15的发射率,至少约600g/m2/24h的湿蒸汽渗透性,和至少约100cm的静水压头。复合片材优选安装在墙壁或屋顶系统中,使镀金属一侧与空气空间相邻。替代地,可让镀金属一侧的反面与空气空间相邻。在复合片材和与之形成空气空间的第二表面之间的距离优选至少为约0.75英寸(1.9cm)。据信,安装与空气空间相邻的镀金属复合片材能最大限度发挥复合片材作为热障的效力,因为这能让它几乎不发射辐射能,或者能反射辐射能。如果镀金属一侧大面积地紧密接触建筑结构的固体零部件,则能量将通过建筑零部件的传导来传递,于是镀金属片材的效力将降低。在涂沥青的屋顶结构中,安装复合片材以便使镀金属一侧面朝下,朝向顶楼空间,这也将最大限度地减少由于灰尘、污垢等的积累所致隔热性能的任何下降。
图3是采用本发明镀金属复合片材作为住房包裹材料的框架结构建筑中墙壁系统50的示意图。盖板层51,例如,胶合板,安装在构成建筑物承重框架的框架元件53外面。垂直框架元件53一般由木材(例如,木立筋)构成,但在某些结构中也可由金属构成。本发明透气性镀金属复合片材55安装在盖板51的外表面。在某些建筑结构中,不使用盖板51,镀金属复合片材55直接安装在框架元件53上。金属带59将构成建筑物的外部(例如,砖、混凝土块、纤维增强水泥、岩石等)的外皮57与镀金属复合片材分开从而在二者其间形成空气空间61。木条或其它间隔件可替代金属条59。镀金属复合片材优选地安装成,使复合片材面朝空气空间的表面是片材的镀金属的一侧。替代地,复合片材可安装成使镀金属的一侧背向空气空间。内衬63(例如,石膏板)构成建筑物的内墙。绝缘层65安装在相邻框架元件之间并在内衬与盖板层之间(或在内衬与复合片材之间,如果不使用盖板层的话)的墙内。墙壁结构任选地包括被夹在内衬与绝缘材料之间的漏气屏障和蒸汽阻挡层66。层66防止对流热损失和防止在住房内产生的过多潮湿渗透到绝缘层中。该镀金属复合片材的高湿蒸汽渗透性允许水蒸气沿箭头″B″的方向透过复合片材并在此分散到空气空间61中,从而防止潮湿在绝缘层内的凝结。在镀金属片材具有低空气渗透性和高静水压头的情况下,它还可起到防止风和水渗入的作用。
图4A~4C是包括本发明镀金属复合片材的框架结构建筑物的屋顶系统示意图。图4A表示一种“冷屋顶”系统的例子,其中内顶楼空间60不住人。镀金属复合片材55安装在涂沥青的屋顶框架元件(例如,木椽)67上方。绝缘材料65安装在顶楼地板托架(未画出)之间后者高于并与内天花板71的标高相邻。任选的蒸汽阻挡层70可安装在中间绝缘层65与内天花板71之间。间隔件(板条)76放在与镀金属复合片材上表面相邻的位置,而外屋顶材料73(例如,瓦等)安装在间隔件上。在镀金属复合片材上方和间隔件(板条)76与外屋顶材料之间是板条空气空间74。屋面系统的屋脊用代号75表示。镀金属复合片材55是湿蒸汽可透的并包括片材层77,其上涂有金属和有机涂层,被表示为层79。复合片材55安装成使镀金属的一侧面朝顶楼空间。
图4B是贯通冷屋顶系统部分的断面图,包括全铺的盖板而不是板条系统。镀金属复合片材55安装在屋顶椽子67顶面,优选以镀金属一侧79朝下、面朝内顶楼空间60。坚固的屋顶板64(例如,胶合板)安装在镀金属复合片材上方,同时外屋顶安装在坚固的盖板上方。外屋顶的例子包括涂沥青毛毡或其它屋顶衬底材料68,并以外屋顶材料73如瓦或沥青叠瓦覆盖在屋顶衬底上。在图4C所示全铺盖板的另一种实施方案中,镀金属片材55固定在屋顶椽子67的底侧,以镀金属的一侧79优选地朝下、面朝顶楼空间60。复合片材可安装成以其镀金属的一侧79背向顶楼空间,然而,镀金属的一侧上的灰尘和污垢积累可能造成随时间推移发射率的增加和隔热性能的下降。
镀金属复合片材也可安装在顶楼地板托架88的顶面,如图4D所示。复合片材55优选地安装成以镀金属的一侧79朝下,背向内顶楼空间60并面向绝缘材料65,基于以上原因的考虑。优选地在绝缘材料和镀金属复合片材之间留出空气空间78。
除了起热障作用之外,本发明镀金属复合片材还可,当安装成住房包裹材料和/或屋顶衬时,为建筑物屏蔽掉电磁频率辐射(EMF)。该复合片材能衰减进来和/或出去的EMF信号以致它们无法传送进出该建筑物。虽然可用铝箔或其它金属片材,但此类片材不透气,因此它们作为建筑包裹材料不可心。可采用标准住房包裹材料和屋顶衬安装方法来获得EMF屏蔽的好处。为达到最完全的保护,复合片材应作为包裹材料安装在所有墙壁和屋顶中。
试验方法
在下面的非限制性实施例中,将采用以下试验方法确定各种报告的特征和性质。ASTM是指美国试验材料学会。ISO指的是国际标准组织。TAPPI指纸桨与造纸工业技术协会。
对于采用卷材形式的片材层的实施例而言,从每卷的开头、中间和末尾共取3个样品(S1、S2和S3),对这些样品每一个进行多次测定,并求取静水压头、Gurley Hill孔隙率、MVTR和发射率测定值的平均值。
基重(Bw)按照ASTM D-3776,在此收入本文作参考,测定,并以g/m2为单位报告。
静水压头(HH)采用ISO 811,在此收入本文作参考,测定,并以厘米水柱的形式报告。该试验测定片材对液态水在静载荷作用下渗透的阻力。将100cm2样品安装在Shirley静水压头试验机(Shirley研发有限公司,Stockport,英国)上。抵住样品一侧泵水,直至表面出现3个泄漏点。每种样品总共测定18个样品的静水压头,将测定结果取平均就得到实施例中报告的平均HH。
Gurley Hill孔隙率是片材材料阻挡气体的能力的尺度。具体地说,它测定一定体积气体需要多长时间透过其中存在一定压力梯度的某一面积的材料。Gurley-Hill孔隙率按照TAPPI T-460om-88使用Lorentzen & Wettre Model 121D型Densometer测定。该试验测定100cm3空气在大约12.45cm水柱压力作用下被压过2.54cm直径样品的时间。结果以秒数表示,通常被称作Gurley秒数。Gurley Hill孔隙率在每个实施例总共测定18个样品并将测定结果平均从而得到实施例中报告的平均Gurley秒数。
发射率是材料的热吸收和反射性质的度量,按照ASTM C1371-98和ASTM C408-71采用AE D&S型发射率计(由Devices and Services公司,达拉斯,TX,制造)以片材样品的镀金属的一侧面朝辐射源测定。检测器被加热到82℃,并以低发射率(反射性、发射率=0.07)和高发射率(吸收性、发射率=0.89)的标准物进行标定。仪器在每次测定开始和结束时以及每隔30min至少标定一次。对于每个实施例总共测定27个样品并将测定结果平均得到实施例中报告的平均发射率,来测定发射率。对应于S1、S2和S3样品的每一个,从3个区域,即,靠近卷材宽度两边的和中点的区域,取得3个发射率测定值。重复同样的测定3次,每次都用新的S1、S2和S3测定,总共27个发射率测定值,将它们取平均得到实施例中报告的平均发射率。
热阻(Rg)是通过具有平行约束表面的单一反射空气空间(“空气腔”)的热流量的度量,根据EN ISO 6946从发射率计算并以m2 K/W为单位报告:
Rg=1/(hc+hr),
其中hc:传热系数(传导、对流),
hr:传热系数(辐射)
hr=E hro
E=(1/ε1+1/ε2-1)-1和hro=4σTm 3
E:发射率等级
hro:黑体的辐射传热系数
σ:斯特藩-玻尔兹曼常数(5.67·10-8W m-2K-4)
Tm:表面及其周围的平均热力学温度
水平传热:hc=1.25W/m2K或hc=0.025/d,如果>1.25W/m2K
垂直向上传热:hc=1.95W/m2K或hc=0.025/d,如果>1.95W/m2K
d:空气腔厚度
ε1,ε2=包围空气腔的表面的发射率。
在实施例中,计算在以下条件下的Rg:Tm=283°K,d=50mm,ε1=片材的发射率,和ε2=0.9(砖墙的发射率)。采用0.38W/mK的矿渣棉的导热率计算矿渣棉的等效厚度。
屏蔽效力是材料阻挡电磁频率(EMF)辐射的能力的度量,以-分贝(-dB)为单位报告并定义如下,
屏蔽效力=-10log10(PT/PI)
其中PT是透过样品传播的辐射功率,PI是入射到样品上的辐射功率。屏蔽效力-dB=100意味着比值PT/PI已被减小1010倍。PT和PI按照ASTM D4935-99(测定平面材料的电磁屏蔽效力的标准试验方法)采用EIgal SET 19-A同轴屏蔽效力试验仪和惠普8753C矢量网络分析仪进行测定。
测定是以复合片材的镀金属的一侧面朝信号发生器进行的。屏蔽效力采用上式计算。
湿蒸汽透过速率(MVTR)是材料的湿蒸汽渗透性的度量,按照ASTM F1249,在此收入本文作参考,在23℃和85%相对湿度条件下测定并以g/m2/24h为单位报告的。对于每个实施例总共测定9个样品,将测定值取平均得到实施例中报告的平均MVTR,来进行MVTR的测定。
片材层的抗张强度按照ASTM D5035-90测定。
蒸汽沉积有机层的厚度是针对冰冻切片的样品采用透射式电子显微镜法测定并以微米(μm)为单位报告的。
金属层的厚度是针对冰冻切片的样品采用透射式电子显微镜法测定并以纳米(nm)为单位报告的。
具体实施方式
实施例
下面定义的缩写将在下面的实施例中用到:
单体/低聚物组成:
1.TRPGDA=三丙二醇二丙烯酸酯
2.SR606=活性聚酯二丙烯酸酯
3.SR9003=丙氧基化新戊二醇二丙烯酸酯
4.HDODA20%C18=己二醇二丙烯酸酯与硬脂酸一丙烯酸酯的混合物(80/20(重量))
5.ZonylTM/TRPGDA=80/20(重量)ZonylTM/TRPGDA
其中ZonylTM是氟化甲基丙烯酸酯低聚物TRPGDA、SR606、SR9003、HDODA和硬脂酸一丙烯酸酯由Sartomer公司(Exton,PA)供应。
ZonylTM氟化甲基丙烯酸酯低聚物由杜邦公司(Wilmington,DE)供应。上面的缩写也将用在通过对应单体的固化形成的聚丙烯酸酯层的实施例中。
实施例1~8中使用的片材层总括在表I并由杜邦公司(Wilmington,DE)供应。
表I.实施例中使用的片材层
片材层 | BW(g/m2) | 厚度(μm) |
Tyvek1560B HomeWrap(HW1) | 61 | 180 |
Tyvek1580B HomeWrap(HW2) | 80 | 216 |
Tyvek1162B CommercialWrap(CW1) | 82 | 180 |
TyvekSuproRooflining(RF1) | 160 | 500 |
TyvekReflex3460M房屋包裹材料(HWM1) | 62 | 185 |
TyvekReflex3480M房屋包裹材料(HWM2) | 84 | 222 |
HW1、HW2、CW1和RF1未经镀金属。HWM1和HWM2镀以铝层并具有2.5的复合光密度(约36nm厚铝层)并采用苯胺印刷方法涂以1.5g/m2有机漆涂层。
实施例1
本实施例显示,具有低空气渗透性的湿可透非织造布片材的湿蒸汽渗透性当片材按照本发明涂布并镀金属时基本上不变。
表1所载HW1、HW2、CW1和RF1的卷材样品(460m长×41cm宽)在真空涂布/镀金属机器上涂以各种聚丙烯酸酯层并镀以铝金属,形成表II所载结构(其中Al=铝,L1、L2和L3是选自TRPGDA、SR606、HDODA20%C18、SR9003和ZonylTM/TRPGDA的二丙烯酸酯)。在包含一种以上聚丙烯酸酯层的结构中,聚丙烯酸酯层的组成在某些实施例中相同,在其它实施例中不同。铝层的厚度或者是22或者是36nm,聚合物层的厚度(L1、L2、L3)是0.5μm。
真空涂布/镀金属机器的真空室包括等离子处理站、1个蒸汽沉积站,和1个镀金属站。涂布的样品因此在2或3个步骤中制成,取决于沉积的层数。
在第一步骤中,一卷未涂布片材层被置于通往大气的真空室中退绕的位置。在与聚丙烯薄膜引导带接头以后,基材被从退绕位置穿引通过机器直至卷曲位置。随后,关闭真空室并抽真空至10-2~10-3Torr。卷材以91m/min的速度退绕,同时片材层的一个表面接受300W的Ar/N2(80/20)等离子体的处理。等离子处理之后,紧接着沉积铝层,随后沉积丙烯酸酯单体或单体共混物,接着固化,从而形成片材层/Al/L2的卷材。替代地,将丙烯酸酯单体或单体共混物闪蒸并凝结到片材层的等离子-处理过的表面上。在ZonylTM/TRPGDA组合物沉积期间,片材层在冷却鼓上被冷却至约-15℃~-20℃。对于其它单体组合物则不采用冷却。单体蒸汽发生在位于真空室外面的闪蒸蒸发器中,并通过加热的管道和喷咀缝隙被吸入到真空室中。一旦接触到片材层的表面,单体蒸汽就凝结成为薄液体层,随后该层借助电子束固化从而在纤维表面上获得约0.5μm厚的丙烯酸酯聚合物层。固化后,真空室放空,将聚丙烯酸酯-涂布的片材层(片材层/L1)的卷材从真空室中取出。
在第二步骤中,涂布的卷材(片材层/L1)被置于退绕位置,同时真空室泵抽真空至<10-4Torr。涂布的片材以91m/min的速度退绕并如同在第一步骤中一样对丙烯酸酯-涂布侧进行等离子处理,随后以铝真空镀金属,随后立即在金属层顶面沉积相同或不同丙烯酸酯或掺混物的0.5μm厚第二层,并且固化从而形成涂布的镀金属的片材(片材层/L1/Al/L2)。在镀金属期间,片材在冷却鼓上被冷却至约-15℃~-20℃。典型单体进料速率为约14g/min。随后,真空室放空,取出涂布的片材材料的卷材。对于具有按照构型——片材层/L1/Al/L2/Al/L3沉积涂层的样品来说,重复第二步骤以沉积铝的第二层和丙烯酸酯聚合物的外层L3。
从每卷材的开头、中间和末尾获得多个样品并采用上面描述的试验方法测定其性质,然后与其对应未镀金属前体片材进行比较。性质数据报告在下表II中,包括对照样(不具有丙烯酸酯或金属涂层的片材层)和具有各种金属和丙烯酸酯涂层的组合的本发明样品。
表II.聚丙烯酸酯/金属-涂布的片材和未镀金属对照样的平均性质
片材层 | 结构 | Gurley(s) | MVTR(g/m2/24hrs) | HH(cm H2O) | 发射率 |
HW1 | HW1对照样 | 164±14 | 1530±45 | 186±12 | 0.64±0.01 |
HW1/Al/L2 | 180±51 | 1600±98 | 173±17 | 0.14±0.04 | |
HW1/L1/Al/L2 | 179±40 | 1540±76 | 167±28 | 0.11±0.02 | |
HW1/L1/Al/L2/Al/L3 | 178±110 | 1499±274 | 165±1 | 0.11±0.01 | |
HW2 | HW2对照样 | 191±19 | 1430±133 | 225±16 | 0.64±0.01 |
HW2/L1/Al/L2 | 209±66 | 1470±74 | 181±48 | 0.10±0.02 | |
HW2/L1/Al/L2/Al/L3 | 165±82 | 1560±148 | 190±20 | 0.11±0.01 | |
CW1 | CW1对照样 | 3670±888 | 1005±98 | 434±47 | 0.65±0.06 |
CW1/L1/Al/L2 | 3343±792 | 1041±23 | 428±12 | 0.10±0.01 | |
RF1 | RF1对照样 | 882±220 | 1588±106 | 297±21 | 0.62±0.01 |
RF1*/L1/Al/L2 | 639±61 | 1651±90 | 285±13 | 0.13±0.01 |
*RF1是闪纺聚乙烯和纺粘聚丙烯的层合物。RF1是在层合物的闪纺侧涂布的。
表II中的数据所示,按本发明制备的样品(片材层/Al/L2、片材层/L1/Al/L2和片材层/L1/Al/L2/Al/L3)的空气渗透性、湿蒸汽渗透性和静水压头与初始片材层相比基本上未变。本发明涂布/镀金属的样品提供明显好于初始片材层的热阻(较低发射率),同时不明显影响片材的其它对建筑最终用途如作为住房包裹材料和屋顶衬重要的性能。这些观察与所使用的丙烯酸酯单体无关。其它测定的但未列在表II中的性能是抗张强度(纵向和横向)、Mullen顶破强度、Elmendorf(埃尔曼多夫撕裂强度)和抗钉撕裂强度,据发现这些在所有情况下都在对照样的正常波动范围之内。
实施例2和对比例2
本实施例比较了适合用作住房包裹材料的本发明涂布镀金属片材与TyvekReflex住房包裹材料,后者是一种现有技术市售镀金属住房包裹材料。
实施例2a、2b和2c涂有聚丙烯酸酯并镀以铝金属,正如上面实施例1中所述,采用HW1作为实施例2a和2b的初始片材层,并以HW2作为实施例2c的初始片材层,结果提供表III所载结构。对比例2a和2b分别为市售镀金属住房包裹材料Reflex3460M和Reflex3480M。
表III.聚丙烯酸酯/金属-涂布的片材和未镀金属的对照例的平均性能
实施例 | 结构 | Gurley(s) | MVTR(g/m2/24hrs) | HH(cmH2O) | 发射率 | 热阻(m2K/W) | 矿渣棉的等效厚度(mm) |
HW1对照样 | 164±14 | 1530±45 | 186±12 | 0.64±0.012 | 0.23 | 8 | |
实施例2a | HW1/Al/L2 | 180±51 | 1600±98 | 173±17 | 0.14±0.04 | 0.50 | 19 |
实施例2b | HW1/L1/Al/L2 | 179±40 | 1540±76 | 167±28 | 0.11±0.02 | 0.58 | 22 |
对比例2a | HWM1=HW1/Al/聚合物涂层 | 269±31 | 1030±150 | 135±13 | 0.23±0.02 | 0.42 | 16 |
HW2对照样 | 191±19 | 1430±133 | 225±16 | 0.64±0.01 | 0.23 | 8 | |
实施例2c | HW2/L1/Al/L2 | 209±66 | 1470±74 | 181±48 | 0.10±0.02 | 0.59 | 22 |
对比例2b | HWM2=HW2/Al/聚合物涂层 | 490±85 | 900±23 | 204±9 | 0.18±0.02 | 0.45 | 17 |
表III中的数据证明,本发明的样品(实施例2a~2c)具有与对照例样品HW1和HW2基本相同的Gurley Hill孔隙率、湿蒸汽透过速率和静水压头,而对比例2a和对比例2b(具有有机涂层,但它不但覆盖金属层而且还覆盖片材层纤维之间的间隙空间)的镀金属样品具有,与对照样HW1和HW2相比,降低的MVTR(分别下降约33%和37%),降低的Gurley Hill孔隙率(分别约64%和156%)。本发明实施例和对比例的静水压头,与对照样相比没有明显改变。
除了比市售镀金属住房包裹材料样品明显高的MVTR之外,本发明实施例还具有比市售镀金属住房包裹材料产品低约40~50%的发射率,对应于该复合片材加上空气腔在热阻上的约19~38%的改善。这相当于29~38%矿渣棉绝缘层等效厚度的改进。本发明复合湿蒸汽可透片材层非常薄的金属和有机涂层提供相当于19~22mm矿渣棉绝缘层的绝缘性能的改进,相比之下现有技术HWM1和HWM2(Reflex)材料只相当于16~17mm。
实施例3
本实施例显示在片材层和金属层之间采用中间聚合物涂层(L1)对按照本发明制备的镀金属片材发射率的影响。
测定尺寸为30.5cm×30.5cm的CW1住房包裹材料的样品分别采用单独的镀金属机和真空闪蒸机涂布和/或镀金属,致使在镀金属或聚合物沉积以后,在从一台机器到另一台转移期间样品暴露于空气之中。样品按照实施例1所述接受等离子处理。采用金或铝金属形成具有10、50和100nm不同金属层厚度的镀金属样品。丙烯酸酯层的厚度为约0.5μm。聚合物沉积和/或镀金属后,在多个部位测定沿样品区域各处的发射率。结构及其性能示于下表IV中。
表IV:有与没有中间聚丙烯酸酯层的镀金属片材的发射率比较
金属层厚度(nm) | |||
10 | 50 | 100 | |
发射率:CW1/Au | 0.43±0.02 | 0.21±0.01 | 0.19±0.02 |
发射率:CW1/SR606/Au | 0.24±0.02 | 0.10±0.01 | 0.09±0.001 |
发射率:CW1/Al | 0.81±0.01 | 0.31±0.01 | 0.19±0.01 |
发射率:CW1/SR606/Al | 0.84±0.01 | 0.18±0.02 | 0.09±0.01 |
表IV中的数据显示,在片材层与金属层之间具有聚丙烯酸酯层的样品具有比具有同样片材层和金属层厚度但没有中间聚丙烯酸酯涂层的对应样品明显低的发射率。据信,0.5μm厚的聚合物层使片材层中的纤维表面微观粗糙变得光滑,因而改善了发射率。
实施例4
本实施例证实外聚丙烯酸酯涂层(L2)对镀金属片材的发射率的影响。
按照实施例3所述制备涂布的镀金属片材样品(30.5cm×30.5cm)。两种样品都是在同一涂布操作下用SR606进行,随后以铝进行同一镀金属操作期间制成的,以保证金属和聚合物涂层的厚度对于所有样品来说基本上一样。涂布的样品的结构以及发射率示于下表V。
表V:有与没有聚丙烯酸酯外层的镀金属片材的发射率
涂布的片材结构 | 发射率 |
CW1/SR606(0.5μm)/Al(50nm) | 0.18±0.02 |
CW1/SR606(0.5μm)/Al(50nm)/SR606(0.5μm) | 0.14±0.0001 |
在表V中的数据显示,具有L2的样品具有比同样地镀金属和涂布操作但不带L2制成的样品相比低的发射率。
实施例5
本实施例证实外涂层的特定二丙烯酸酯组成对镀金属片材的发射率的影响。
采用上面实施例1中所述方法制成具有各种聚丙烯酸酯组成的L1和L2的具有结构——片材层/L1/Al/L2——的涂布卷材样品。中间和外聚丙烯酸酯层的厚度是0.5μm,而铝层的厚度是36nm。当丙烯酸酯组合物是TRPGDA、SR606、SR9003时,L1=L2。当L2是ZonylTM/TRPGDA时,L1是SR606和SR9003。
表VI比较了作为L2使用各种不同类型二丙烯酸酯的样品的发射率。
表VI.不同L2聚丙烯酸酯组合物的基材/L1/Me/L2的发射率
片材层 | L2 | 发射率平均值 |
HW1 | TRPGDA | 0.12±0.02 |
SR606 | 0.10±0.02 | |
SR9003 | 0.09±0.01 | |
ZonylTM/TRPGDA | 0.09±0.01 | |
HW2 | TRPGDA | 0.11±0.01 |
SR606 | 0.11±0.03 | |
SR9003 | 0.10±0.01 | |
HDODA-20%C18 | 0.12±0.02 | |
ZonylTM/TRPGDA | 0.08±0.01 |
表VI中的数据显示,外聚合物层(L2)中使用的二丙烯酸酯的选择对决定涂布片材的发射率起作用。最佳发射率表现在使用SR9003和ZonylTM/TRPGDA(80/20)时观察到。发射率等于或低于0.10,当L2=SR9003时;但发射率一致地小于0.10,当L2=ZonylTM/TRPGDA(80/20)时。据信,L2中的丙烯酸酯的化学结构和L2的厚度通过其在测定发射率所处的近红外、红外和远红外区间的吸收来影响发射率。碳氟化合物,与烃类相比,在近红外区间似乎吸收较少,因为烃的C-H键在那一区间存在泛频并且泛频强度较大。
实施例6
本实施例证实实施在真空下对外聚合物层L2的真空镀金属和真空沉积但在沉积L2之前让金属层不暴露于大气的影响。
制备真空涂布的镀金属样品30.5cm×30.5cm,其中中间和外聚丙烯酸酯层的厚度是0.5μm,沉积在中间聚丙烯酸酯层上的铝层的厚度是50nm。聚丙烯酸酯单体是SR606。制备了结构如表VII所载的样品。每种结构采用2种不同方法制备。暴露于空气的样品分3个步骤制造,如同在实施例3中所述。铝层在涂布外聚丙烯酸酯层以前在空气中暴露几个小时,以便让铝表面形成氧化铝层。铝层未暴露于空气中的样品分2个步骤制造,正如在实施例1中所述,于是铝层和外聚丙烯酸酯层在同一真空室内沉积,在金属与单体沉积/固化步骤之间不将真空室放空。这些样品的铝层未暴露于空气中,因此氧化铝只能靠氧和水分透过L1或L2的扩散,如果有的话,生成。
表VII.镀金属/聚合物沉积期间暴露和不暴露于空气的聚丙烯酸酯涂布的镀金属片材的发射率
暴露于空气的样品 | 发射率 |
CW1/SR606/Al/SR606 | 0.14+/-0.0001 |
不暴露于空气的样品 | |
CW1/SR606/Al/SR606 | 0.10+/-0.01 |
HW1 or HW2/SR606/Al/SR606 | 0.10+/-0.01 |
表VII中的数据证实,在真空中实施涂布和镀金属步骤但在沉积有机涂层之前镀金属的样品不暴露于空气中所提供的镀金属片材具有较低发射率(改进的热障)。据信,这是由于阻止在金属表面明显形成氧化物而实现的。
实施例7和8
这些实施例证实本发明镀金属复合片材对电磁频率屏蔽效力的改进。
所有样品都是按照实施例1制备的,其中铝层厚度为22或36nm,正如图5和6所画出的结构表示的。中间和外聚丙烯酸酯层的厚度是0.5μm。图5是本发明镀金属并涂布的HW1材料、HW1以及HWM1的EMF屏蔽效力对EMF频率的曲线图。图6是本发明镀金属并涂布的HW2材料、HW2以及HWM2的EMF屏蔽效力对EMF频率的曲线图。
未镀金属的HW1和HW2样品对EMF辐射基本上透明,因此不提供EMF屏蔽。本发明的镀金属复合片材表现出约20~45dB的相当大的屏蔽效力改善,这相当于HW1和HW2的100~32,000倍大。现有技术镀金属片材HWM1和HWM2也提供对EMF辐射的屏蔽,但效力不如本发明的复合片材。具有较厚金属层的样品提供的屏蔽程度最高,其中结构HW1/SR606/Al(36nm)/SR606/Al(36nm)/SR606和HW2/SR606/Al(36nm)/SR606/Al(36nm)/SR606提供约50dB的屏蔽效力,或比未镀金属对照样的屏蔽大100,000倍。
令人惊奇的是,包括中间有机涂层(L1)的样品一般提供比不包括中间涂层的样品更好的屏蔽作用。虽然连续768μm厚铝箔层(图6)提供约100dB的最佳屏蔽效力,然而它不具有本发明复合片材的透气性。
实施例9
本实施例证实采用各种住房包裹材料产品作为初始湿蒸汽可透片材层制备本发明镀金属复合片材的方法。
作为湿蒸汽可透片材层使用的市售住房包裹材料产品是:
PinkwrapHousewrap(制造商
Owens Corning,Toledo,OH),Greenguard Ulfra Amowrap(制造商Amoco,Smyrrna,GA),TyparHousewrap(制造商Reemay,Old Hickory,TN),和WeathermatePlusHousewrap(制造商Dow Chemical Company,Midland,MI).
尺寸为约2英尺×4英尺(0.61m×1.22m)住房包裹材料样品采用在实施例1中描述的方法进行镀金属和涂布。该镀金属并涂布的样品的结构是片材/L1/Al/L2,其中有机涂层L1和L2是采用SR9003单体制备的,各自具有0.5μm的涂层厚度。铝层为约36nm厚。
发射率、湿蒸汽渗透性和空气渗透性载于表VIII。对照样是未涂布的住房包裹材料片材。
表VIII.镀金属前后性能比较
样品 | 结构 | Gurley(s) | MVTR(g/m2/24hrs) | 发射率 |
Pinkwrap | 对照样 | 7±4 | 670 | 0.91±0.01 |
Pink Wrap/L1/Al/L2 | 3±1 | 822 | 0.07±0.02 | |
TyparHousewrap | 对照样 | >8000* | 317 | 0.79±0.01 |
Typar/L1/Al/L2 | >8000* | 377 | 0.10±0.01 | |
GreenguardUltra Amowrap | 对照样 | 301±55 | 1502 | 0.83±0.02 |
GreenGuard/L1/Al/L2 | 214±21 | 1248 | 0.14±0.01 | |
WeathermatePlus | 对照样 | >8000* | 110 | 0.75±0.03 |
WeatherMate/L1/Al/L2 | >8000* | 100 | 0.09±0.01 |
*试验在8000s时停止;材料几乎不透空气。
表VIII中的数据证明,与初始住房包裹材料相比,金属和有机涂层不显著改变MVTR。镀金属样品的发射率比对照例改进了83~92%。
Claims (25)
1.一种镀金属复合片材,它包含:
具有第一和第二外表面的湿蒸汽可透片材层,该片材层包含非织造布、机织织物、非织造布-薄膜层合物、机织织物-薄膜层合物、湿蒸汽可透薄膜及其复合材料至少之一,其中湿蒸汽可透片材层的第一外表面是多孔片材,其选自微穿孔薄膜、机织织物和非织造布;以及在该片材层的所述第一外表面上的至少一个多层涂层,所述多层涂层包含:
与该片材层的第一外表面相邻、厚度介于约15nm~200nm的第一金属涂层;以及
沉积在该金属层上的厚度介于约0.2μm~2.5μm的外有机涂层,其组成包含选自有机聚合物、有机低聚物及其组合的材料;
其中复合片材的MVTR是沉积该金属和涂层之前测定的片材层MVTR的至少约80%。
2.权利要求1的镀金属复合片材,所述多层涂层还包含:
沉积在湿蒸汽可透片材层第一外表面、介于片材层与金属涂层之间、厚度介于约0.02μm~2μm的中间有机涂层,其组成包含选自有机聚合物、有机低聚物及其组合的材料;
其中中间与外有机涂层的总合计厚度不大于约2.5μm。
3.权利要求2的镀金属复合片材,其中外有机涂层的厚度介于约0.2μm~1μm,中间有机涂层的厚度介于约0.02μm~1μm,并且有机涂层的总合计厚度不大于约1.5μm。
4.权利要求1~3中任何一项的镀金属复合片材,还包含沉积在片材层第二外表面上的权利要求1~3中任何一项的第二多层涂层,其中有机涂层的总合计厚度不大于约2.5μm。
5.权利要求1~3中任何一项的镀金属复合片材,其中多层涂层基本上覆盖多孔片材的外表面但使得孔隙基本上未覆盖。
6.权利要求1~3中任何一项的镀金属复合片材,其静水压头至少为约20cm H2O并且MVTR至少为约35g/m2/24h。
7.权利要求1~3中任何一项的镀金属复合片材,其发射率不大于约0.12。
8.权利要求1~3中任何一项的镀金属复合片材,其中金属选自铝、银、铜、金、锡、锌及其合金。
9.权利要求8的镀金属复合片材,其中金属是铝。
10.权利要求1的镀金属复合片材,其中湿蒸汽可透片材层包含非织造布。
11.权利要求1的镀金属复合片材,其中湿蒸汽可透片材是选自纺粘布、纺粘-熔喷布、纺粘-熔喷-纺粘布、闪纺超细纤维丛丝状片材及其复合材料的非织造布。
12.权利要求1的镀金属复合片材,其中所述湿蒸汽可透片材层的第一面是穿孔薄膜。
13.权利要求1的镀金属复合片材,其中湿蒸汽可透片材层包含机织带的机织织物。
14.权利要求1的镀金属复合片材,其中湿蒸汽可透片材选自非织造布-薄膜层合物和机织织物-薄膜层合物,并且该薄膜选自微孔薄膜、穿孔薄膜和无孔湿蒸汽可透薄膜。
15.权利要求1的镀金属复合片材,其中外有机涂层包含交联的聚丙烯酸酯。
16.权利要求2或3的镀金属复合片材,其中中间和外有机涂层各自包含交联的聚丙烯酸酯。
17.权利要求1~3中任何一项的镀金属复合片材,其中湿蒸汽可透片材层包含闪纺超细纤维丛丝状片材。
18.权利要求17的镀金属复合片材,其中闪纺超细纤维丛丝状片材被层合到纺粘非织造布上,并在闪纺片材上沉积多层涂层。
19.权利要求1的镀金属复合片材,其中外有机涂层包含氟化丙烯酸酯低聚物。
20.一种镀金属复合片材,其包含:
具有第一和第二外表面的多孔闪纺超细纤维丛丝状片材层和至少一个多层涂层,该涂层包含:
沉积在闪纺超细纤维丛丝状片材层的第一外表面上、厚度介于约15nm~200nm的金属涂层,所述金属选自铝、银、铜、金、锡、锌及其合金;以及
沉积在该金属层上的厚度介于约0.2μm~1μm的外有机涂层,其组成包含交联的聚丙烯酸酯;
其中多层涂层基本上覆盖闪纺超细纤维丛丝状片材的外表面,但使得孔隙基本未覆盖。
21.一种镀金属复合片材,其包含:
具有第一和第二外表面的多孔闪纺超细纤维丛丝状片材层和至少一个多层涂层,该涂层包含:
沉积在所述闪纺超细纤维丛丝状片材层的第一外表面上的厚度介于约0.02μm~1μm的中间有机涂层,其组成含有交联的聚丙烯酸酯;
沉积在所述中间有机涂层上、厚度介于约15nm~200nm的金属涂层,所述金属选自铝、银、铜、金、锡、锌及其合金;以及
沉积在金属层上、厚度介于约0.2μm~1μm的外有机涂层,其组成包含交联的聚丙烯酸酯;
其中多层涂层基本上覆盖闪纺超细纤维丛丝状片材的外表面,但使得孔隙基本未覆盖。
22.权利要求21的镀金属复合片材,其中中间涂层的厚度介于约0.025μm~0.2μm。
23.一种建筑结构中的屋顶系统,它包含权利要求1、2、3、20或21中任何一项的镀金属复合片材。
24.一种建筑结构中的墙壁系统,它包含权利要求1、2、3、20或21中任何一项的镀金属复合片材。
25.一种减少EMF辐射穿透建筑物的方法,该方法包含在建筑物的墙壁或屋顶中安装权利要求1的镀金属复合片材。
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PCT/US2005/030291 WO2006024013A1 (en) | 2004-08-23 | 2005-08-23 | Improved breathable low-emissivity metalized sheets |
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Also Published As
Publication number | Publication date |
---|---|
BRPI0515220A (pt) | 2008-07-08 |
EP1789622B1 (en) | 2014-12-10 |
US8431209B2 (en) | 2013-04-30 |
JP4731560B2 (ja) | 2011-07-27 |
US20060040091A1 (en) | 2006-02-23 |
WO2006024013A1 (en) | 2006-03-02 |
US7805907B2 (en) | 2010-10-05 |
US20080057292A1 (en) | 2008-03-06 |
US8497010B2 (en) | 2013-07-30 |
US20080060302A1 (en) | 2008-03-13 |
JP2008510640A (ja) | 2008-04-10 |
CN101044283B (zh) | 2010-09-08 |
US20080187740A1 (en) | 2008-08-07 |
EP1789622A1 (en) | 2007-05-30 |
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