CN1176695A - 用于电化学电池测试器的多层防潮层 - Google Patents
用于电化学电池测试器的多层防潮层 Download PDFInfo
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Abstract
可用于防止水分破坏在电化学电池(50)上的湿敏电池状态测试器(60)的有效性的光透明防潮层(70),包括多重在柔性聚合物基体上的很薄的交替无机材料和有机材料层(40,38)。所述层不是层压的,而是通过淀积或涂覆方法在基体(12)上形成,且所述层的厚度小于5微米。该有机材料是疏水性聚合物,且该无机材料是金属氧化物、氮化物、玻璃或硅。
Description
本发明的背景
本发明的领域
本发明涉及一种光透明的多层防潮层。更具体地说，本发明涉及可用作湿敏电池上测试器的防潮层的光透明、薄膜、多层复合物，它包括多重交替的无机材料和有机材料层，还涉及制备所述防潮层的方法和具有湿敏电池上测试器和所述防潮层的电化学电池。
背景技术
使用电池状态测试器如热致变色电压测试器来从视觉上显示通称为电池的电化学电池的状态已变得很普遍了，并且这给电池制造者和消费者带来了增值的益处。这些测试器与一次电化学电池一起使用，但如需要它们也可被消费者用来测试二次或可充电电化学电池的状态。目前应用最普通的测试器是与电阻元件接触的热致变色材料，所述变色材料构成电池包装的一体化部件，其中电池是碱性一次电池。使用者将电池的电极置于测试器的触点之间，并挤压测试器的触点端以使之与电池电极即电池端部电接触。测试器的电阻元件与电池电压成正比地被加热，热致变色材料定性地显示其范围表明“良好”或“更换”的电池状态。例如在美国专利4,723,656中公开了这种类型的测试器。在美国专利5,188,231中公开了一体化、热致变色外壳测试器，该测试器可从外壳上取出。近来开发的电池上测试器中电池状态显示器是电池标签的一个整体部分。这些电池上测试器包括热致变色类型和新的电化学类型测试器。热致变色类型电池上测试器的一个实例公开在欧洲专利公开No.0523901 A1中，该公开内容在这里引入供参考。热致变色类型采用电阻元件产生热量，因而它不能长久地连接在电池的电极上而不使其连续放电，与这种热致变色类型不同，新的电化学类型不从电池中引出电流，因而它可长久地连接在电池的电极上而不使电池放电。这种新型测试器公开在美国专利5,250,905和5,339,024中，该公开内容在这里引入供参考。如在美国专利5,355,089中所公开的，一些电化学类型的电池上状态测试器采用吸湿或换句话说湿敏的电解质组合物，并需要防止水分接触电解质的装置，因为这种接触会损害测试器的有效性。该专利公开了解决这一问题的许多方法，其中最佳的是云母。但是，虽然云母较便宜，却得不到可使之卷成云母卷的长带状或其它形状的云母，而经济可行的商用生产方法需要这种云母卷。
本发明的概述
本发明总体上涉及可用作防潮层的光透明多层复合物，它包括多重交替的固体无机材料和固体有机材料层，且它是通过在基体上淀积或形成所述层而制成的。更具体来说，本发明涉及一种薄膜、多层复合物，它包括在适当的基体上淀积或形成的交替无机和有机层，且它可用作防潮层。在一个实施方案中，本发明的复合物用作湿敏的电池上测试器的防潮层，所述测试器以视觉显示电化学电池的状态。在另一实施方案中，本发明涉及制备多层复合物的方法。在再一个实施方案中，本发明涉及本发明多层复合防潮层与电池上测试器的组合，还涉及一种电化学电池，该电池具有由所述复合物防护水分的湿敏电池上测试器。在进一步的实施方案中，本发明复合物用作湿敏材料和物品的包装材料。这样，当用作电池上测试器的防潮层时，薄膜、多层复合物的光透明性能使得人们可以观察到测试器用来指示电池状态的颜色、标记或其它视觉手段所显示的电池状态。在一个实施方案中，其中本发明复合物用作电化学电池的电池上测试器的防潮层，基体是柔性聚合物，所述复合物是柔性、光透明、薄膜复合物，其中各层的厚度不超过5微米，优选不超过1微米。所谓电池上测试器是指以视觉指示电池状态的测试器，它通过电池标签或其它手段与电池长久连接，但本发明并不仅限于这种实施方案。可使用本发明防潮层复合物的一类湿敏电池上测试器是包括至少一种吸湿材料的测试器，如果它吸收了水蒸气，就会损害或破坏测试器的有效性。另一类型测试器包括需要存在预定量的水以发挥作用的至少一种组分，因而它需要防潮层以在测试器中保持那一数量的水。
无机材料和有机材料均是固体，且除硅外，均是化合物而不是元素。有机材料一般是聚合物，除硅外，无机材料是非金属的且为化合物如氮化物、氧化物等。由于其对电的半导体性质，硅一般认为不是金属。无机和有机材料均是不溶于水的，且对于防潮层应用来说，其水蒸气渗透率应尽可能的低，在这些应用中，有机材料优选包括疏水性聚合物。制备多层复合物的方法包括在基体上淀积或形成第一层，接着在该第一层上淀积第二层，其中第一和第二层是不同的材料，其中之一是有机材料，另一种是无机材料，重复交替的层淀积直至涂覆了所需的层数以制备出具有所需性能的多层复合物。因而，本发明复合物与其中各种预先存在的层通过粘合或其它方式互相连接的层压品不同，其区别在于本发明复合物的交替层是通过淀积或涂覆方法在基体或复合物的其它层上就地形成的。有机材料以液体涂覆，然后固化或干燥，或者通过物理气相淀积(PVD)方法、溅射、等离子体强化的物理气相淀积、化学气相淀积或其它适当途径以单体、预聚物或聚合物来涂覆所述有机材料。无机材料层也通过本领域技术人员公知的方法来涂覆，包括各种(PVD)方法、溅射、等离子体强化的物理气相淀积、化学气相淀积(CVD)以及取决于所用材料的其它适用方法，以下将对此进一步进行说明。
附图的简要说明
图1图示说明按照本发明的十四层防潮层。
图2(a)图示说明在带有本发明防潮层的电池上的电池上测试器的剖面图，图2(b)以部分剖视图图示说明具有电池上测试器和本发明防潮层的电池的侧视图。
详细说明
图1图示说明本发明的薄膜、多层防潮层10，它包括塑料或聚合物基体12，在该基体上淀积有多层结构，该结构包括如层14、18、22、26、30、34和38的七层无机材料和如层16、20、24、28、32、36和40的七层有机材料。各有机层的厚度一般为约100埃至约5微米，优选为约1000埃至约1微米。无机层的厚度一般为约100埃至10,000埃，优选为约200埃至5,000埃，更优选约300至3,000埃。因而，除使用了有机材料层和使用了塑料基体外，图1所示防潮层的结构就交替材料结构和层厚度而言与灯、透镜、反射镜和其它光学制品上所用的薄膜、多层光学干涉涂层相似。再有，在这些范围内的各层的厚度确信使本发明的复合物处于薄膜的范畴。当然，层数和层厚度取决于多层复合物的预计用途并取决于用作无机层和有机层的材料。在图1所示具体结构中，所有有机层的厚度相同且材料相同，所有无机层的厚度相同且材料相同。然而，本发明包括其中并非全部无机层厚度相同或材料相同以及其中并非全部有机层厚度相同或材料相同的多层复合物，这是本领域技术人员可理解的。再者，虽然为方便起见仅图示了一种十四层(除基体外)的复合物，但本发明的复合物可具有更多或更少的层，根据实施者的意愿和能力，总层数(不含基体)的范围可为3至100或更高，优选至少4层且更优选至少6层交替层。另外，在附图所示的实施方案中，所有层均在基体的一侧。如需要，可在基体的两侧(顶部和底部)涂覆交替的无机和有机层以形成本发明的复合物。
再有，本发明的多层复合物不仅可用作电池上电化学测试器的薄膜防潮层，而且它还可用作湿敏食品、化学品、药物、电子设备和如上所述物品的防潮层。本领域技术人员可理解它还可被设计并用于其它用途，包括如选择性透射和反对电磁谱的各部分的光学应用。在再一种实施方案中，基体12是具有可脱离的表面的织物，在该织物上淀积第一层，使得可移出多层结构并以无形成所述多层结构的基体的状态来使用，或者可在第一基体上形成多层结构，然后将其转移到第二基体上。对大多数应用来说，要求基体的强度能使得多层复合物在制造过程中处理并使用而不发生断裂。在图1所示实施方案中，基体不具有可脱离的表面，在基体上涂覆的第一层是无机层，涂覆的最后一层是有机材料层。如需要，淀积在基体上的第一层可以是有机材料层，所述复合物的最后一层根据预计的用途可以是无机或有机材料层。已发现，如果无机材料是较脆的材料或易于破裂的材料，例如玻璃、金属氧化物或金属氮化物，对其涂覆有机材料层可防止它在操作时损坏，降低它在弯曲或折曲时破裂的趋向，还防止该无机材料直接接触腐蚀性环境。在这种情况下，复合物的外层是有机材料，其中之一可以是塑料或聚合物基体，如图1中所示。
还已发现且对实施本发明有重要意义的是，以有机材料来分隔无机材料层对于避免裂纹和缺陷在无机材料中蔓延很重要。也就是说，已发现通过如下所述的一种淀积方法淀积的无机层中的裂纹、小孔或其它缺陷易于带入下一无机材料层中，如果下一无机材料层直接淀积在第一层无机材料上而在该两无机层之间没有无机材料的干涉层的话。这一现象会显著降低复合物作为防潮层的实用性，因为如果在无机层之间不设置无机材料的干涉层则这类缺陷常常会在全部无机材料中蔓延。对于作为实施本发明的层而淀积的有机材料有时会发生类似的现象。因而，在淀积过程中会出现宏观或微观小孔，包入灰尘颗粒，等等，且这为水蒸气的透过提供了流畅的通道。通过交替淀积无机材料层和有机材料层，在任何具体层中的这类层或薄膜缺陷不趋向于在覆盖缺陷的覆盖层中蔓延，由此给水蒸气穿透提供了更长且更曲折的路径，甚至可达到这样的程度，即净效果如同不存在这类缺陷。从技术观点来看，层越薄且层越多给水蒸气透过复合物提供更大的阻力。但淀积每层而制备防潮层的费用增加。再有，如果层过薄，在该层中会有空隙或不完全覆盖，这会增加该复合物的渗透性。
如上所述，本发明的薄膜、多层复合物与现有技术的层压品的不同之处在于本发明的各层是通过由除层压外的方法在各层之上交替淀积无机和有机材料形成的，而层压是通过对预成形的材料条带或层片进行粘合或以其它方式连接而形成层状结构。再有，本发明的范围还包括一层或更多的有机层自身由两层或更多层不同的有机材料构成，例如，在无机材料层上使用底层和涂层以达到更好的层间粘合，在该底层上淀积不同的有机材料，该两种不同的有机材料的复合物形成有机层。类似地，可以涂覆两层或更多层的无机材料以形成本发明上下文中的无机层。本发明的范围还包括且这也构成其一种实施方案，即，本发明的一或多片复合物(它们不是层压的复合物)可以互相或与其它复合物或材料或它们的组合进行层压，形成包括至少一片或至少两片或更多片本发明复合物的层压结构。再者，虽然本发明的薄膜多层复合物不包括使用金属层，但本发明的复合物可与一或多层金属层压，或可在本发明的复合物上淀积一或多层金属，在该金属层上再淀积一层本发明的复合物以形成包括交替的本发明复合物和金属层的结构。本领域技术人员可理解，金属镀层是光不透明的。但这种结构可用于不需要透光性能的应用。
可用来实施本发明的层淀积方法包括例如溅射和蒸镀的各种PVD方法，其中包括射频(RF)溅射和磁控管溅射。还可使用的是等离子体聚合、单体气相淀积、各种CVD、低压化学气相淀积(LPCVD)和等离子体辅助化学气相淀积(PECVD)方法，这些都是本领域技术人员公知的。在滚筒或卷筒上对基体涂覆涂层或层状物的高速方法也是公知的，例如公开在美国专利4,543,275和5,032,461中。一般在真空室中一次仅淀积一层。这样，例如在基体的一侧或两侧上淀积一层二氧化硅或氮化硅。然后将真空室中的靶材料更换为聚合物或将涂有二氧化硅的基体转移至其中靶材料是聚合物的另一室中。然后在该二氧化硅层上淀积一层聚合物。然而如需要，通过在一个真空室中采用至少两种淀积溅射靶(在溅射淀积的情况下)，可在该室中在基体的一侧或两侧上淀积至少一层无机材料和至少一层聚合物。例如在基体的一侧上淀积一层的情况下，在通过磁控管强化的溅射进行层淀积的真空室中，基体是一个电极，要在基体上淀积的靶材料是另一个电极，电极之间是等离子体。另外，对于同时在基体的两侧上淀积一层，则在基体的两侧均有靶材料和等离子体，在该情况下在基体的两侧或涂有无机层的基体的两侧上淀积一层无机材料或有机材料。再者，如基体是移动的条带或薄膜，通过在真空室中顺序采用多于一个的靶，可在基体的一次通过中淀积多于一种的材料。这样，如基体是移动的条带或薄膜，当基体移动经过第一靶或靶组时，就在基体的一或两侧上淀积了一层无机材料。当涂覆有无机材料的基体在室中继续移动至第一靶下游的第二靶或靶组时，在无机材料层上就淀积了一层有机材料，等等。从而基体在真空室中的一次通过中在该基体上涂覆了多层以形成图1所示的复合物或具有比图1所示更多或更少层数的复合物。
如上所述，美国专利5,250,905和5,339,024公开了可含有一或多种湿敏组件的电池上测试器，因而需要采用防潮层与湿敏测试器相结合以防止水分损害如美国专利5,355,089中公开的测试器的有效性。取得了一定效果的一种方法是使用设置在电池上测试器上的小片云母，并用适当的防水材料密封，防水材料例如聚异丁烯，如’089专利中所公开的。图2(a)和2(b)分别示意了带有本发明防潮层的电池上的电池上测试器的侧视图和部分剖视的顶视图。这样，图2所示为一种电化学电池50，它具有’089专利中公开类型的电池上测试器60，该测试器含有至少一种吸湿组件(未示出)，在测试器上设置本发明的薄膜、多层防潮层70并通过密封胶62密封在金属电池容器52的外侧，塑料标签70环绕电池并设置在测试器、密封处和防潮层之上。测试器60约10密耳厚且它通过未示出的手段连接在正极54和负极56端点上。如’089专利中所公开的，测试器60含有例如对质子惰性的有机电解质，例如在一种溶剂混合物中的0.5M三氟甲磺酸锂，所述溶剂混合物是碳酸亚乙酯∶碳酸亚丙酯∶聚偏二氟乙烯为2.4∶2.4∶5.2(体积份数)的混合物，该电解质是很吸湿的。密封胶材料例如是由在Piscataway，NJ.的Huls，Inc.以Vestoplast V 3645出售的马来酸酐改性的聚丁烯弹性体。标签是环绕电池和防潮层/测试器/密封胶的PVC薄膜，然后加热收缩。实际来说，对于用作电化学电池上的电池上测试器的防潮层，例如上述专利中公开的电池上标签测试器，防潮层(包括基体)的总厚度不超过约1.5密耳，优选为约1密耳或25微米以内。
在图2所示实施方案中，本发明防潮层10包括作为基体的1密耳厚的聚环烷酸亚乙酯膜，在该基体上淀积有如图1所示的交替14层无机材料和有机材料以制得1.3密耳厚的防潮层，按如下所述方法测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积低于5微克水。该7层无机层均为500埃厚的防水玻璃层，该防水玻璃具有约为350℃的较低熔化温度，各层均通过溅射淀积。该7层有机层各为1微米厚的一氯化二对二甲苯聚合物，所述各层通过在各层溅射的玻璃上一氯化对二甲苯单体的气相聚合淀积在玻璃层上。在基体上淀积的第一层是玻璃，最后的或第14层是聚合物，如图1所示。这样，各玻璃层的两侧均覆盖有有机材料层，其中之一是一氯化二对二甲苯聚合物，其中的另一种是基体。
多层防潮层的水渗透按如下所述进行测量，即，将0.25英寸宽及3密耳厚的无水聚偏二氟乙烯条带放置在0.5密耳厚的铝箔上，在所述条带上涂覆1英寸宽及1.7英寸长的本发明长方形防潮层，所述防潮层通过2.5密耳厚的密封胶密封在铝箔上，如图2总体所示，其中所述聚偏二氟乙烯条带含70wt％的环丁砜以及对质子惰性的有机电解质，该电解质例如在碳酸亚乙酯∶碳酸亚丙酯∶聚偏二氟乙烯为2.4∶2.4∶5.2(体积份数)的溶剂混合物中的0.5M三氟甲磺酸锂，该电解质是很吸湿的。密封胶是马来酸酐改性的聚丁烯弹性体。在密封的手套箱中在无水条件下来完成这种装配。将如此形成的层压板在60℃及100％相对湿度下保持一周，之后，移出含有环丁砜的聚偏二氟乙烯条带，并通过Karl Fischer滴定法分析水含量。这就是如下实施例中所指并使用的测试方法和测试条件。按照这种测试方法和条件来测量，本发明的防潮层的水蒸气透过率为每24小时时间每平方英寸表面积低于15、优选低于5、更优选低于2微克水。
在制备可作为电池上测试器的防潮层的本发明多层薄膜复合物中，所述的层是淀积在柔性基体上，例如呈带状物、条带或织物形态的柔性聚合物薄膜或其它适当的基体材料。所述基体不必须是柔性的，但在制备用作防潮层的本发明多层复合物中，优选柔性基体以使得在防潮层的制备过程中及将其应用于电池过程中经得起弯曲。在基体上淀积的第一层一般是无机层，但如需要可将有机材料作为第一层涂覆。作为本发明方法的说明性、但非限制性实施例，在基体上淀积第一层无机材料，在该第一层无机材料上淀积第一层有机材料。然后在第一层有机材料上淀积第二层无机材料。在这之后，在第二层无机材料上淀积第二层有机材料。然后在该第二层有机材料上淀积第三层无机材料，并在该第三层无机材料上淀积第三层有机材料。重复这种交替层的淀积直至达到所需的层数，如图1所示。虽然图1图示的总共为十四层或七对层，但实际层数取决于应用和所使用的材料，广义来说，本发明多层复合物可用于除防潮层外的其它应用，且层数可从4变至多于100。
无机层是固体无机化合物如选自主要由金属、硅、硼、砷及它们的混合物所组成的组中的至少一种元素的氧化物、氮化物、碳化物、磷化物或磷酸盐等及这些化合物的混合物。在一个实施方案中，无机材料是硅。例如无机化合物是一种氮化物、磷化物、磷酸盐、氧化物、碳化物、卤氧化物、硼酸盐、硅酸盐、钨酸盐等及它们的混合物。其中无机层为无机化合物的混合物的实施方案的一个说明性，但非限制性实例是包含通过PVD溅射方法涂覆的含有锡-铅-磷-氟氧化物组合物的耐水玻璃。其它的耐水玻璃组合物也可使用，其说明性但非限制性实例包括硼-磷-硅酸盐、硅酸盐、磷酸盐、砷酸盐、钒酸盐、铌酸盐(niobiates)、钽酸盐、钨酸盐、硼硅酸盐、硅铝酸盐、calchoginide玻璃例如硫化物、硒化物、碲化物等。在另一实施方案中，无机层是例如非晶态氮化硅的氮化物或任何适宜的金属氮化物，单一氧化物如SiOx、Al2O3、Nb2O5，或例如SixNyOz的混合物，或一种或多种金属间化合物等。对于在本发明的用于电池上测试器的防潮层中使用，无机层在有水分存在的条件下是稳定的，并具有一定程度的柔性以使得多层复合物可弯曲而不使无机层破裂，从而不降低复合物作为防潮层的有效性。在防潮层应用中，无机化合物是不溶于水的，这意味着在25℃时在水中的溶解速率低于1×10-4g/cm2-分，优选在25℃下低于1×10-5g/cm2-分，更优选在25℃下低于1×10-6g/cm2-分。有机层是固体的，且最普通的是聚合材料。根据复合物的用途和其应用的环境，聚合材料是非晶态或晶态的、弹性的、交联或非交联等。一些适用的有机材料的实例包括微晶蜡、稠合芳烃、聚烯烃、聚氯乙烯和其共聚物、聚对二甲苯、含氟聚合物和共聚物、弹性体、聚酰亚胺、聚酰胺、环氧化物、聚酯、聚醚、聚碳酸酯、卤化聚合物等，这些是说明性但非限制性的实例。卤化聚合物(包括氟碳聚合物)也可用于实施本发明。丙烯酸类聚合物可用于实施本发明，特别是具有至少6个碳原子的烃链的丙烯酸类聚合物，例如由其中单体包括甲基丙烯酸己酯和/或丙烯酸己酯等的反应所生成的丙烯酸类聚合物。可用于实施本发明的非聚合物类固体有机材料包括例如硬脂酸甲酯、硬脂酸等。对于用于防潮层，有机材料优选是疏水性的、在湿环境下稳定，且对水分或水蒸气的渗透性尽可能的小。按照1994 AnnualBook of ASTM Standards的15.09卷中的ASTM F 372-78测量，对于防潮层应用，有机材料层的水分渗透率为在100°F和90％RH下低于20gm-mil/100in2-24hr，优选低于10gm-mil/100in2-24hr，更优选低于1gm-mil/100in2-24hr。根据复合物所需的性能，本领域技术人员可理解的有机层的性质和所采用的淀积方法，有机层可通过如下方法淀积，这些方法有流涂法、凝聚、单体或预聚物反应、PVD如溅射、CVD及上面总体提到的任何其它方法。
参照以下实施例可进一步理解本发明，其中所有的防潮层均是光透明的。
实施例
实施例1
在这一实施例中，基体是1密耳厚的聚环烷酸亚乙酯(polyethylenenaphthenate)(Kalodex)薄膜，该基体在1.5毫乇氩气氛中用防水玻璃溅射涂覆以形成在该薄膜上的500埃厚玻璃层。该玻璃的熔点为约350℃，通过对具有SnO∶SnF2∶PbO∶P2O5的比值为32∶37∶8∶23的组成的配合料在500℃下熔融30分钟来制备。在这之后，在该玻璃层上涂覆1微米厚的一氯化二对二甲苯聚合物层，涂覆方法是将固体一氯化二对二甲苯二聚物(Union Carbide的Parylene C)加热至约160℃的温度以使该二聚物气化，使该蒸气流经加热管以使该二聚物在约600℃下分解成单体，并将如此形成的单体通入压力为20乇及温度为约30℃的真空室中，在该室中单体就地在涂覆有玻璃的基体上冷凝并聚合，直接在玻璃层上形成1微米厚的聚合物层或涂层。这种聚合物是直链、非交联、主要为烃类的聚合物。这种交替层淀积方法再重复二次以在基体上形成交替6层玻璃和聚合物(3层玻璃及3层聚合物)，按在“详细说明”部分提到的测试方法来测定，如此形成的薄膜、多层防潮层的水蒸气透过率为每24小时时间每平方英寸表面积52微克水。
实施例2
重复实施例1，但在基体上淀积总共交替10层玻璃和聚合物(5层玻璃及5层聚合物)，形成的防潮层按以上“详细说明”部分提及的测试方法来测定，其水蒸气透过率为每24小时时间每平方英寸表面积24微克水。
实施例3
再重复实施例1，但以交替14层玻璃和聚合物(7层玻璃及7层聚合物)形成如图1所示的防潮层，按在以上“详细说明”部分提及的测试方法来测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积4.7微克水。
实施例4
在这一实施例中，基体是1密耳厚的聚环烷酸亚乙酯(Kalodex)薄膜，在该基体上在1.5毫乇氩气氛中以二氧化硅进行RF磁控管溅射涂覆以形成约500埃厚的SiOx层或涂层。然后将涂覆了SiOx的基体在溶于MIBK中的乙烯醚单体(Vectomer，Allied-Signal)溶液中浸涂，所述MIBK含有三乙烯基甲基硅烷粘合促进剂和Cyracure 6974(三芳基锍盐)UV引发剂。湿涂覆的复合物经受数秒种UV辐射并固化成3微米厚的干燥聚乙烯醚涂层。这种交替层淀积方法再重复6次以在基体上形成如图1所示的交替14层(7层SiOx及7层聚合物)，得到2密耳厚的透明防潮层，使用实施例1的测试方法对其测试，按以上“详细说明”部分所提到的测试方法测定，它的水蒸气透过率为每24小时时间每平方英寸表面积21微克水。
实施例5
在这一实施例中，基体是1密耳厚聚环烷酸亚乙酯(Kalodex)薄膜，并在该基体上用实施例1的玻璃在1.5毫乇氩气氛中进行RF磁控管溅射涂覆以在该薄膜上形成500埃厚的玻璃层。在这之后，在该玻璃层上溅射涂覆1微米厚的以上实施例4中所述的聚乙烯醚层(Vectomer 40105F，Allied-signal)。这种交替层淀积方法再重复6次，以在基体上形成如图1所示具有交替14层玻璃和聚乙烯醚的防潮层(7层玻璃及7层聚乙烯醚)，按以上“详细说明”部分提到的测试方法测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积28微克水。
实施例6
在这一实施例中，基体是1密耳厚的聚环烷酸亚乙酯(Kalodex)薄膜，用实施例1的玻璃在1.5毫乇氩气氛中在该基体上进行RF磁控管溅射涂覆以在该薄膜上形成500埃厚的玻璃层。在这之后，在该玻璃层上通过RF磁控管溅射涂覆1微米厚的聚三氟氯乙烯层(Aclar，Allied-Signal)。这种交替层淀积方法再重复6次以在基体上形成如图1所示的具有交替14层玻璃和聚乙烯醚的防潮层(7层玻璃和7层聚乙烯醚)，按以上“详细说明”部分提到的测试方法测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积28微克水。
实施例7
在这一实施例中，基体是1密耳厚的聚环烷酸亚乙酯(Kalodex)薄膜，用氮化硅在1.5毫乇氩气氛中对该基体进行RF磁控管溅射涂覆以形成约500埃厚的非晶态氮化硅层或涂层。然后在该氮化硅层上RF磁控管溅射PTFE以形成1微米厚的PTFE层。该方法重复一次以形成在基体上包括交替4层非晶态氮化硅和PTFE(2层氮化硅和2层PTFE)的薄膜、多层防潮层，按以上“详细说明”部分提到的测试方法测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积28微克水。
实施例8
在这一实施例，基体是1密耳厚的聚环烷酸亚乙酯(Kalodex)薄膜，在1.5毫乇氩气氛中在该基体的一侧通过RF磁控管溅射涂覆500埃厚的非晶态氮化硅涂层。在这之后，在该氮化硅层上用如下方法涂覆1微米厚的一氯化二对二甲苯聚合物层：将固态一氯化二对二甲苯二聚物(ParyleneC，得自Union Carbide)加热至约160℃的温度以使该二聚物气化，使该蒸气流经加热管以使该二聚物在约600℃下分解成单体，并将如此形成的单体通入压力为20乇且温度为约30℃的真空室中，在该室中单体就地在涂覆了玻璃的基体上冷凝并聚合，直接在该玻璃层上形成1微米厚的聚合物层或涂层。这种聚合物是直链、非交联的、主要是烃类型的聚合物。该交替层淀积方法再重复三次以在基体上形成交替8层的氮化硅和聚合物(4层氮化硅和4层聚合物)，按以上“详细说明”部分提到的测试方法测定，如此形成的薄膜、多层防潮层的水蒸气透过率为每24小时时间每平方英寸表面积52微克水。
对比实施例A
在这一实施例中，基体是1密耳厚的聚环烷酸亚乙酯(Kalodex)薄膜，该基体在1.5毫乇氩气氛中用二氧化硅进行RF磁控管溅射涂覆以形成约500埃厚的SiOx层或涂层。然后在SiOx上通过RF磁控管溅射1微米厚的PTFE层。这种交替层淀积方法再重复4次以在基体上形成包括交替10层SiOx和PTFE(5层SiOx和5层PTFE)的复合防潮层，按以上“详细说明”部分提到的测试方法测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积570微克水。
对比实施例B
在这一实施例中，基体是1密耳厚的聚环烷酸亚乙酯(Kalodex)薄膜，该基体在1.5毫乇氩气氛中用二氧化硅进行RF磁控管溅射涂覆以形成约500埃厚的SiOx层或涂层。然后通过甲烷的等离子体强化的CVD在SiOx上溅射一层1微米厚的交联聚乙烯。这种交替层淀积方法再重复4次，以在基体上形成包括交替10层(5层SiOx和5层聚乙烯)的SiOx和聚乙烯的薄膜、多层防潮层，按以上“详细说明”部分提到的测试方法测定，该防潮层的水蒸气透过率为每24小时时间每平方英寸表面积340微克水。
可理解，在不偏离以上公开的本发明的范围和实质的条件下，本领域技术人员显而易见并可容易地做出实施本发明的各种其它实施方案和改进。因此，这里所附权利要求书的范围不应限于上述的说明，而应将权利要求书理解成包括本发明中存在的可授予专利的新颖性的所有特征，包括本发明所属技术领域的技术人员认为是其等同物的全部特征和实施方案。
Claims (4)
1.一种电化学电池，具有湿敏电池状态测试器和光透明的防潮层，其中所述防潮层包括在聚合物基体上的复合物，所述复合物包括交替的水不溶性无机材料层和水不溶性有机材料层，所述无机材料选自由至少一种无机化合物、硅和它们的混合物组成的组，其中所述无机化合物层和所述有机化合物层的厚度范围分别为约100至10,000埃和约100埃至5微米。
2.一种光透明的多层复合物，包括交替的选自由至少一种无机化合物、硅和它们的混合物组成的组中的水不溶性无机材料层和水不溶性有机材料层，其中所述无机化合物层和所述有机化合物层的厚度范围分别为约100至10,000埃和约100埃至5微米。
3.一种制备非层压、光透明、多层薄膜复合物的方法，所述复合物包括交替的选自由至少一种无机化合物、硅和它们的混合物组成的组中的水不溶性无机材料层和水不溶性有机材料层，其中所述无机化合物层和所述有机化合物层的厚度范围分别为约100至10,000埃和约100埃至5微米，所述方法包括在基体上淀积第一层所述无机材料，然后在所述第一无机材料层上淀积第一层固体有机材料，接着在所述第一层有机材料上淀积第二层所述固体无机材料，然后在第二层所述无机材料上淀积第二层所述有机材料。
4.如权利要求3的方法，其中重复所述交替层淀积直至达到所需的层数。
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| US08/376,274 US5607789A (en) | 1995-01-23 | 1995-01-23 | Light transparent multilayer moisture barrier for electrochemical cell tester and cell employing same |
| US08/376,274 | 1995-01-23 |
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| CN1176695A true CN1176695A (zh) | 1998-03-18 |
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-
1995
- 1995-01-23 US US08/376,274 patent/US5607789A/en not_active Expired - Lifetime
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1996
- 1996-01-01 IL IL11663996A patent/IL116639A/en not_active IP Right Cessation
- 1996-01-16 AR ARP960101036A patent/AR000729A1/es unknown
- 1996-01-22 PL PL96321474A patent/PL180653B1/pl unknown
- 1996-01-22 CZ CZ972211A patent/CZ221197A3/cs unknown
- 1996-01-22 DE DE69636718T patent/DE69636718T2/de not_active Expired - Lifetime
- 1996-01-22 JP JP8522931A patent/JPH10513003A/ja active Pending
- 1996-01-22 RU RU97114135A patent/RU2142626C1/ru active
- 1996-01-22 MX MX9705538A patent/MX9705538A/es unknown
- 1996-01-22 NZ NZ302500A patent/NZ302500A/en unknown
- 1996-01-22 BR BR9606781A patent/BR9606781A/pt not_active IP Right Cessation
- 1996-01-22 WO PCT/US1996/000684 patent/WO1996023217A1/en active IP Right Grant
- 1996-01-22 CN CN96192245A patent/CN1106575C/zh not_active Expired - Fee Related
- 1996-01-22 EP EP96904475A patent/EP0820588B1/en not_active Expired - Lifetime
- 1996-01-22 CA CA002210232A patent/CA2210232C/en not_active Expired - Fee Related
- 1996-01-22 KR KR1019970704956A patent/KR19980701565A/ko not_active Application Discontinuation
- 1996-01-22 AT AT96904475T patent/ATE346291T1/de not_active IP Right Cessation
- 1996-01-22 AU AU48572/96A patent/AU691092B2/en not_active Ceased
- 1996-04-19 TW TW085104659A patent/TW303531B/zh active
- 1996-08-08 US US08/695,092 patent/US5681666A/en not_active Expired - Lifetime
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1997
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- 1997-07-22 NO NO973379A patent/NO973379L/no not_active Application Discontinuation
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI564618B (zh) * | 2012-04-18 | 2017-01-01 | 伊文修股份有限公司 | 可發光透明面板、手扶梯、移動步道及升降機之升降車廂 |
Also Published As
| Publication number | Publication date |
|---|---|
| CZ221197A3 (cs) | 1998-04-15 |
| US5681666A (en) | 1997-10-28 |
| IL116639A0 (en) | 1996-05-14 |
| IL116639A (en) | 1998-10-30 |
| KR19980701565A (ko) | 1998-05-15 |
| RU2142626C1 (ru) | 1999-12-10 |
| NZ302500A (en) | 1998-07-28 |
| WO1996023217A1 (en) | 1996-08-01 |
| US5607789A (en) | 1997-03-04 |
| JPH10513003A (ja) | 1998-12-08 |
| TW303531B (zh) | 1997-04-21 |
| AU691092B2 (en) | 1998-05-07 |
| CA2210232A1 (en) | 1996-08-01 |
| NO973379D0 (no) | 1997-07-22 |
| NO973379L (no) | 1997-09-12 |
| PL321474A1 (en) | 1997-12-08 |
| MX9705538A (es) | 1998-02-28 |
| EP0820588A4 (en) | 1999-07-28 |
| EP0820588A1 (en) | 1998-01-28 |
| AR000729A1 (es) | 1997-08-06 |
| IS4524A (is) | 1997-07-14 |
| DE69636718T2 (de) | 2007-09-20 |
| DE69636718D1 (de) | 2007-01-04 |
| EP0820588B1 (en) | 2006-11-22 |
| BR9606781A (pt) | 1997-12-30 |
| PL180653B1 (pl) | 2001-03-30 |
| ATE346291T1 (de) | 2006-12-15 |
| CA2210232C (en) | 2001-05-29 |
| BG101818A (en) | 1998-04-30 |
| AU4857296A (en) | 1996-08-14 |
| CN1106575C (zh) | 2003-04-23 |
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