CN101622524B - 响应活化剂的胶体晶体阵列 - Google Patents
响应活化剂的胶体晶体阵列 Download PDFInfo
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- CN101622524B CN101622524B CN2007800511005A CN200780051100A CN101622524B CN 101622524 B CN101622524 B CN 101622524B CN 2007800511005 A CN2007800511005 A CN 2007800511005A CN 200780051100 A CN200780051100 A CN 200780051100A CN 101622524 B CN101622524 B CN 101622524B
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Abstract
公开一种制备根据布拉格定律衍射辐射的辐射衍射传感器的方法。如下制成该传感器：在基底上形成有序周期性颗粒阵列，用聚合物基质涂布该颗粒阵列，固化该基质以将该颗粒阵列固定在基质内并使该固定的阵列与活化剂接触，其中该活化剂使由该传感器衍射的辐射的波长从第一波长移位至第二波长。
Description
发明领域
本发明涉及由辐射衍射材料制成的传感器，更特别地涉及当与活化剂组合物接触时显示衍射波长变化的辐射衍射传感器。
背景技术
基于胶体晶体阵列的辐射衍射材料已经用于多种目的。胶体晶体阵列(CCA)是单分散的胶体颗粒的三维有序阵列。该颗粒通常由诸如聚苯乙烯的聚合物胶乳或诸如二氧化硅的无机材料构成。
颗粒的这类胶态分散体可以形成晶体结构，其具有与紫外、可见光或红外辐射的波长相当的点阵间距。这些晶体结构已经用于从入射辐射的宽光谱中过滤选定波长的窄谱带，同时允许邻近辐射波长的透射。已经通过将颗粒分散在液体介质中而产生现有器件，由此该颗粒自排列成有序阵列。所述颗粒通过相互聚合或者通过引入使颗粒溶胀并融合在一起的溶剂而融合在一起。
在CCA的其他应用中，有序阵列被固定在基质中而且当该固定阵列衍射可见光谱中的辐射时可以被用作着色剂。作为选择，制造CCA衍射辐射以便用作滤光器、光开关和光学限幅器。虽然这些CCA使用恒定的粒子间距，但是当粒子间距响应刺激而变化时CCA可以用作传感器。
近来，已经由含有在水凝胶内聚合的CCA的水凝胶制备这类传感器。包围着CCA的水凝胶的聚合物响应特定的外部刺激而改变构象。例如，水凝胶的体积可以响应刺激而改变，所述刺激包括化学品的存在，诸如溶液中的金属离子和有机分子例如葡萄糖，使得该器件可用于化学分析。在水凝胶基器件中，单分散的高度带电的胶体颗粒被分散在低离子强度的液体介质中。所述颗粒由于其静电荷而自组装成 CCA。这些有序结构根据布拉格定律衍射辐射，其中反射满足布拉格条件的辐射而不满足布拉格条件的邻近光谱区域透射通过该器件。
根据布拉格定律衍射辐射的有序周期性颗粒阵列满足以下方程式：
mλ＝2ndsinθ
其中m为整数，λ为被反射的辐射的波长，n为该阵列的有效折射率，d为颗粒层之间的距离，θ为被反射的辐射与颗粒层平面产生的角度。入射辐射在该阵列中的最上颗粒层处以角度θ被部分反射至第一层的平面并被部分透射至下方颗粒层。虽然也发生一些入射辐射的吸收，但是一部分被透射的辐射在该阵列中的第二颗粒层处以角度θ被部分反射并被部分透射至下方颗粒层。这种以角度θ的部分反射以及部分透射至下方颗粒层的特征持续穿过该阵列的厚度。被衍射的辐射的波长(λ)可以由尺寸d控制，该尺寸可以是每一层中颗粒中心的平面之间的距离。最初，对于填充颗粒的阵列而言被衍射的波长λ与颗粒直径成比例。然而，当周期性有序阵列中的颗粒层之间的距离(d)增大时，被衍射的辐射的波长也增大。响应特定化学物种而增大器件内的层际空间体积的传感器器件增大颗粒层之间的层际空间距离，从而改变被衍射的辐射的波长。
在水凝胶基CCA中，当水凝胶的体积改变时，CCA的衍射波长改变。基于水凝胶的这些CCA器件通常含有高百分比的水，例如约30体积％。这些水凝胶基CCA是脆的而且当该CCA的含水量改变时具有其光学性能显著改变的倾向。
为了克服水凝胶基CCA的这些缺陷，一种方法在于制备水凝胶基CCA，使包围该CCA的水凝胶基质脱水，然后用可聚合单体回填该阵列。聚合该单体以产生基本上不含水的聚合的胶体晶体阵列。这些阵列响应某些环境刺激，例如压缩应力(由此改变点阵间距)，从而改变CCA的衍射波长。
然而，这些现有的水凝胶基CCA体系具有显著的生产和处理缺陷。需要更增强的CCA，其响应外加的化学刺激等表现辐射衍射性能而且 当除去该刺激时基本上恢复其初始的光学特性。
发明概述
本发明涉及一种辐射衍射传感器，其包括在基底上形成的有序周期性颗粒阵列和涂布于所述颗粒阵列上的固体基质组合物，其中选择所述基质组合物以响应活化剂，以至于对所述活化剂的暴露使由所述传感器衍射的辐射的波长从第一波长移位至第二波长。本发明还包括一种制备传感器的方法，其包括在基底上形成有序周期性颗粒阵列；用基质涂布所述颗粒阵列；和固化所述基质以将所述颗粒固定在该基质内，其中选择所述基质以响应活化剂，以至于对所述活化剂的暴露使由所述传感器衍射的辐射的波长移位。
本发明还包括一种鉴定制品的方法，其包括在基底上形成有序周期性颗粒阵列；用基质涂布所述颗粒阵列；固化所述基质以将所述颗粒阵列固定在该基质内，从而制成衍射第一波长的辐射的传感器；将所述传感器施用于制品；和使所述传感器与活化剂接触，以至于所述活化剂使得所述衍射波长移位，其中移位的衍射波长指示所述制品的真实性。
发明详述
本发明包括辐射衍射传感器及其制造方法，其中该传感器衍射可见和/或不可见光谱中的辐射。所述辐射衍射传感器包括保持在聚合物基质中的有序周期性颗粒阵列。该阵列包括多个颗粒层而且满足下式的布拉格定律：
mλ＝2ndsinθ
其中m为整数，n为该阵列的有效折射率，d为颗粒层之间的距离，λ为以角度θ从颗粒层平面反射的辐射的波长。本文使用的“一(个)”被衍射的辐射的波长包括一电磁辐射谱带。例如，提及600nm波长可以包括590-610nm。
可以将各种组成用于所述颗粒，包括但不限于有机聚合物例如聚 苯乙烯、聚氨酯、丙烯酸类聚合物、醇酸树脂聚合物、聚酯、含硅氧烷的聚合物、聚硫化物、含环氧的聚合物，以及无机材料例如金属氧化物(例如氧化铝、二氧化硅、氧化锌或二氧化钛)或半导体例如镉。作为选择，所述颗粒可以具有核-壳结构，其中所述核可以由与上述单一颗粒相同的材料制成。所述壳可以由与核材料相同的聚合物制成，其中对于该核-壳颗粒的特定阵列而言该颗粒壳的聚合物与核材料不同。核材料和壳材料可以具有不同的折射率。另外，壳的折射率可以在穿过该壳厚度的折射率梯度的形式中作为壳厚度的函数变化。壳材料是非成膜的，由此壳材料保留在每个颗粒核周围的位置而不形成壳材料的膜，以使得该核-壳颗粒作为离散颗粒保留在聚合物基质内。
通常，所述颗粒一般是球形。对于核-壳颗粒，核的直径可以占总粒径的70-95％或者总粒径的90％，壳占该粒径的余量而且具有径向厚度尺寸。
在一种实施方案中，在表面活性剂存在下经由乳液聚合制成具有单一结构(非核-壳)的颗粒，产生带电颗粒的分散体。适合胶乳颗粒分散的表面活性剂包括但不限于苯乙烯磺酸钠、1-烯丙氧基-2-羟基丙基磺酸钠(可作为SIPOMER COPS-I购自Rhodia Corporation)、丙基磺酸丙烯酰胺(acrylamide propyl sulfonate)、和烯丙基磺酸钠。特别有用的表面活性剂为在该颗粒分散体的分散用流体(例如水)中溶解性最小的那些。由该分散体通过诸如超滤、渗析或离子交换之类的技术纯化带电颗粒，从而除去不期望的材料，例如未反应的单体、小聚合物、水、引发剂、表面活性剂、未结合的盐和粗粒(聚集颗粒)以产生带电颗粒的单分散体。超滤特别适合纯化带电颗粒。当所述颗粒与其他材料例如盐或副产物处于分散体中时，可能缓和带电颗粒的排斥力；因此，将颗粒分散体纯化至基本上只含带电颗粒，于是它们易于相互排斥并形成有序阵列。
在除去过量原料、副产物、溶剂等的情况下，带电颗粒的静电排斥导致颗粒将它们自身排列成有序阵列。将纯化过的颗粒分散体施涂于基底上并且干燥。施涂于基底上的颗粒分散体可以含有10-70vol％ 带电颗粒或30-65vol％带电颗粒。可以通过浸涂、喷涂、刷涂、辊涂、幕涂、流涂或模具涂布将分散体施涂于基底上达到期望的厚度。湿涂层可以具有4-50微米、例如40微米的厚度。干燥后，材料基本上只含有已经自排列成布拉格阵列并因此衍射辐射的颗粒。
所述基底可以是挠性材料，例如金属片或箔(例如铝箔)、纸或者聚酯或聚对苯二甲酸乙二醇酯(PET)膜(或片)，或非挠性材料例如玻璃或塑料。“挠性”是指基底可以经受机械应力，例如弯曲、拉伸、压缩等而没有显著的不可逆变化。一种适合的基底是微孔片。微孔片的一些实例在美国专利4,833,172、4,861,644和6,114,023中得到公开，这些专利通过引用并入本文。市售微孔片以名称TESLIN由PPGIndustries，Inc销售。其他适合的挠性基底包括天然皮革、合成皮革、整饰过的天然皮革、整饰过的合成皮革、绒面革、乙烯基尼龙(vinylnylon)、乙烯-乙酸乙烯酯泡沫(EVA泡沫)、热塑性聚氨酯(TPU)、填充流体的囊状物、聚烯烃和聚烯烃共混物、聚乙酸乙烯酯和共聚物、聚氯乙烯和共聚物、聚氨酯弹性体、合成织物和天然织物。
在某些实施方案中，所述挠性基底为可压缩基底。“可压缩基底”和类似术语是指能够经历压缩形变而且一旦该压缩形变终止就恢复至基本上相同形状的基底。术语“压缩形变”是指在至少一个方向上至少暂时地减小基底体积的机械应力。
“EVA泡沫”可以包括开孔泡沫和/或闭孔泡沫。“开孔泡沫”是指该泡沫包含多个互相连通的气室；“闭孔泡沫”是指该泡沫包含不连续的封闭孔。EVA泡沫可以包括平坦片材或板坯或模塑EVA泡沫，例如鞋底夹层。不同类型的EVA泡沫可以具有不同类型的表面孔隙率。模塑EVA可以包含致密的表面或“表皮”，然而平坦片材或板坯可以显示多孔表面。本发明的聚氨酯基底包括芳族、脂族和混杂(混杂实例为有机硅聚醚或聚酯型聚氨酯和有机硅碳酸酯聚氨酯)聚酯或聚醚基热塑性聚氨酯。“塑料”是指常见的热塑性或热固性合成材料中的任一种，包括热塑性聚烯烃(“TPO”)例如聚乙烯和聚丙烯及其共混物、热塑性聚氨酯、聚碳酸酯、片状模塑料、反应注射模塑料、丙烯腈基 材料、尼龙等。一种具体的塑料为包含聚丙烯和EPDM(乙烯丙烯二烯单体)的TPO。
在本发明的另一实施方案中，如下制备核-壳颗粒：将核单体与引发剂分散在溶液中以产生核颗粒。将壳单体连同乳化剂和/或表面活性剂(如上对于单一颗粒所述的)一起加入到核颗粒分散体中，以使得壳单体聚合到核颗粒上。如上所述纯化核-壳颗粒的分散体以产生只有带电的核-壳颗粒的分散体，其然后在施涂于基底上时在其上形成有序阵列。
基底上干燥过的(单一或核-壳)颗粒阵列通过以下方式固定在聚合物基质中：用包含单体或其他聚合物前体材料的流动性的可固化基质组合物涂布该颗粒阵列、接着固化该基质组合物。如美国专利6,894,086(通过引用并入本文)中公开的那样，已经自排列成干燥阵列的颗粒可以与该流动性的可固化基质组合物、例如紫外线(UV)可固化的组合物相互渗透。可以通过浸涂、喷涂、刷涂、辊涂、凹面涂布、幕涂、流涂、狭缝涂布或喷墨式涂布将可固化的基质组合物材料涂布至干燥过的颗粒阵列上。涂布是指该聚合物前体材料覆盖整个阵列而且填充颗粒间的至少一些间隙空间。将基质组合物固化(例如通过暴露于UV辐射)以固定该填充颗粒阵列。其他固化机理可以用于将基质组合物固定在颗粒周围。
对于具有核-壳颗粒的辐射衍射传感器，当阵列与流动性的可固化基质组合物相互渗透时，该基质的一些单体可能扩散到壳中，由此增加壳厚度(和颗粒直径)直到基质组合物固化为止。溶剂也可能扩散到壳中并且产生溶胀。最终将溶剂从阵列中除去，但是这种来自溶剂的溶胀可能影响壳的最终尺寸。单体向阵列中的相互渗透与单体固化之间的时间长度部分地决定壳溶胀的程度。
本发明的辐射衍射传感器是非凝胶状的并且基本上是固体的。非凝胶状的是指该辐射衍射传感器不含诸如水之类的流态化材料并且不是水凝胶。所述传感器产品也不是由水凝胶制成的，水凝胶将会被本领域技术人员理解为产生与本发明要求保护的产品不同的产品。在某 些实施方案中，本发明的辐射衍射传感器基本上仅包含所述颗粒和聚合物基质连同一些可能的残余溶剂，因此基本上是固体的。该辐射衍射传感器中颗粒与聚合物基质的体积比通常为约25∶75-约80∶20。
可以用多种方式将所述辐射衍射传感器施加在制品上。可以在基底上制备辐射衍射传感器和然后将它从基底上除去并粉碎成颗粒形式，例如呈薄片形式。该粉碎的辐射衍射传感器可以作为添加剂引入涂料组合物、例如色漆或油墨中以便施涂于制品上。作为选择，可以将辐射衍射传感器直接施加在制品上，由此所述基底为制品的表面，例如制造制品的包装和/或外壳。例如，制造制品可以包括消费品(包括药品或食品)，其中所述基底为该消费品的包装。作为选择，通过将颗粒阵列直接施加在制品的外壳、例如电子器件的外壳上或者直接施加在诸如服装、鞋类、运动装备等的物品上，该制品本身可以充当基底。类似地，该制品可以是证明文件、法律文件或者其它需要确认其真实性的文件。
另外，可以将辐射衍射传感器制成膜或片的形式，然后例如通过粘合剂等将它施加在制品上。应当意识到这些在基底上制备传感器的方法与其他制备传感器的技术不同，那些技术不是首先直接在基底上形成有序阵列接着用基质材料涂布该阵列。
所述辐射衍射传感器响应一种或多种活化剂的存在，该活化剂使得基质在不同的波长处衍射。根据本发明，选择基质组成以使得基质与特定活化剂的接触改变基质的尺寸和/或改变基质的折射率。如果所述尺寸被改变，阵列中的颗粒和/或颗粒层之间的层际空间距离可能变化。本文使用的“活化剂”是使基质的尺寸和/或折射率改变的任何材料。“改变基质的尺寸”和类似术语是指基质响应该活化剂而膨胀(即“溶胀”)或缩小(即“收缩”)。“改变基质的折射率”是指基质的有效折射率响应该活化剂而改变，因此改变由该传感器衍射的辐射的波长和/或强度。可以改变基质的折射率而不改变其尺寸，反之亦然。活化剂可以例如是化学物种，例如水或有机溶剂，或者含有溶质的液体或气体。选择基质以响应特定的活化剂。“响应”活化剂是指该活化 剂改变基质的尺寸和/或改变基质的折射率。在某些实施方案中，当活化剂接触传感器的基质时，活化剂与基质缔合并增加基质体积。基质体积的这种增加使颗粒层展开。根据布拉格定律，粒子间距离(d)的增加使被衍射的辐射的波长(λ)从初始或第一波长(λ1)移位至可以比初始波长更长的第二波长(λ2)。作为选择，在另外的实施方案中，第二波长(λ2)可以比初始波长(λ1)更短。波长λ1和λ2可以通过选择颗粒组成、粒度、基质组成和/或活化剂组成进行调节。颗粒和基质组成决定传感器的有效折射率(n)。粒度决定阵列层之间的初始距离(d)。选择基质组成和活化剂组成以使得活化剂显示出与基质的足够亲合力而保留在基质内，从而使基质衍射不同的波长。波长λ1和λ2可以都在辐射的可见光谱内，以使得通过可见的色移显示出活化剂的存在。λ1和λ2可以都在不可见光谱内，其中波长移位可用合适的仪器检测。作为选择，λ1可以在不可见光谱(UV或IR)内而λ2在可见光谱内，其中当该传感器与活化剂接触时显露颜色。同样，λ1可以在可见光谱内而λ2在不可见光谱内，以至于该传感器接触活化剂时被衍射的光的颜色消失。任何其他波长组合也都在本发明的范围内。
当除去活化剂(例如通过蒸发)时，传感器的基质可以至少基本上恢复至原始的衍射波长，即λ1。基本上是指衍射波长恢复至其原始波长的5-10nm范围内。理论上，当完全除去活化剂时，基质将会恢复至其原始的衍射波长。然而，实际上，一些活化剂可能留在基质内以至于对于某些基质和活化剂对而言，衍射波长不可能完全恢复至其原始波长。在任一情况下，当传感器完全恢复或基本上恢复至其原始状态后，传感器用于检测活化剂的存在或不存在。当除去活化剂时基质至少基本上恢复至其原始的衍射波长可以具有从立即到逐渐的任意速率。某些实施方案中，传感器可以为单次设计(single use design)，其中无法容易地从基质中除去活化剂以使传感器恢至其原始状态。
在一种实施方案中，所述基质组成为水溶性或亲水性丙烯酸类聚合物，活化剂为水。适合制备水溶性或亲水性基质的单体包括但不限于乙氧基化15的三羟甲基丙烷三丙烯酸酯、乙氧基化20的三羟甲基丙 烷三丙烯酸酯、聚乙二醇(600)二丙烯酸酯、聚乙二醇(400)二丙烯酸酯、聚乙二醇(200)二丙烯酸酯、和丙烯酸。
其他适合制备水溶性或亲水性聚合物基质的单体可以包括聚乙二醇(1000)二丙烯酸酯、甲氧基聚乙二醇(350)单丙烯酸酯、甲氧基聚乙二醇(350)单甲基丙烯酸酯、甲氧基聚乙二醇(550)单甲基丙烯酸酯、甲氧基聚乙二醇(550)单丙烯酸酯、乙氧基化30的双酚A二丙烯酸酯、2(2-乙氧基乙氧基)乙基丙烯酸酯、丙烯酰胺、丙烯酸羟基乙酯、丙烯酸羟基丙酯、聚乙二醇(600)二异丁烯酸酯、聚乙二醇(400)二异丁烯酸酯、乙氧基化30的双酚A二异丁烯酸酯、甲基丙烯酸羟基乙酯、和甲基丙烯酸羟基丙酯。
由这些单体制成的水溶性或亲水性聚合物可用水溶胀。向具有水溶性或亲水性聚合物的基质的本发明辐射衍射传感器施加水使得颗粒之间的基质接收水并且溶胀。水溶胀增加颗粒之间的层际空间距离(布拉格定律的变量(d))，从而增大被衍射的辐射的波长。
作为选择，所述基质可以是通过有机溶剂溶胀的组合物。合适的有机溶剂可溶胀的基质材料为对有机溶剂具有亲合力的聚合物，意味着该基质聚合物可通过有机溶剂溶胀至被衍射辐射的波长的变化可检测的程度。合适的有机溶剂可溶胀的聚合物可以由下列非限制性的单体制成：烷氧基化己二醇二丙烯酸酯、乙氧基化3的三羟甲基丙烷三丙烯酸酯、季戊四醇四丙烯酸酯、季戊四醇三丙烯酸酯、丙氧基化3的三羟甲基丙烷三丙烯酸酯、丙氧基化6的三羟甲基丙烷三丙烯酸酯、1，4-丁二醇二丙烯酸酯、乙氧基化3的双酚A二丙烯酸酯、三羟甲基丙烷三丙烯酸酯、丙氧基化2的新戊二醇二丙烯酸酯、乙氧基化3的三羟甲基丙烷三丙烯酸酯、乙氧基化6的三羟甲基丙烷三丙烯酸酯、乙氧基化9的三羟甲基丙烷三丙烯酸酯、乙氧基化3的双酚A二异丁烯酸酯、新戊二醇二丙烯酸酯、和1，6-己二醇二丙烯酸酯。
其他适合制备有机溶剂可溶胀的丙烯酸类聚合物基质的单体可以包括丙氧基化3的甘油三丙烯酸酯、丙烯酸硬脂酯、丙烯酸四氢糠基酯、丙烯酸月桂酯、丙烯酸2-苯氧基乙酯、丙烯酸异癸酯、丙烯酸异 辛酯、丙烯酸辛酯、丙烯酸癸酯、丙烯酸十三烷基酯、己内酯丙烯酸酯、乙氧基化4的壬基苯酚丙烯酸酯、丙烯酸异冰片酯、丙烯酸丁酯、四甘醇二丙烯酸酯、三甘醇二丙烯酸酯、双三羟甲基丙烷四丙烯酸酯、乙氧基化4的季戊四醇四丙烯酸酯、丙烯酸乙酯、丙烯酸2-乙基己酯、苯乙烯、丙烯腈、三羟甲基丙烷三丙烯酸酯、甲基丙烯酸甲酯、甲基丙烯酸丁酯、甲基丙烯酸环己酯、甲基丙烯酸异冰片酯、甲基丙烯酸月桂酯、聚丙二醇单异丁烯酸酯、丙氧基化2的烯丙基异丁烯酸酯、甲基丙烯酸烯丙酯、甲基丙烯酸乙氧基鲸蜡酯、甲基丙烯酸乙氧基硬脂酯、乙氧基化2的羟基乙基异丁烯酸酯、乙氧基化5的羟基乙基异丁烯酸酯、乙氧基化10的羟基乙基异丁烯酸酯、乙氧基化4的壬基苯酚异丁烯酸酯、乙氧基三甘醇异丁烯酸酯、甲基丙烯酸四氢糠基酯、甲基丙烯酸异癸酯、甲基丙烯酸月桂酯、甲基丙烯酸硬脂酯、甲基丙烯酸2-苯氧基乙酯、甲基丙烯酸缩水甘油酯、甲基丙烯酸异冰片酯、甲基丙烯酸十三烷基酯、环己烷二甲醇二异丁烯酸酯、乙氧基化4的双酚A二异丁烯酸酯、乙氧基化8的双酚A二异丁烯酸酯、三甘醇二异丁烯酸酯、乙二醇二异丁烯酸酯、四甘醇二异丁烯酸酯、1，4-丁二醇二异丁烯酸酯、1，6-己二醇二异丁烯酸酯、新戊二醇二异丁烯酸酯、1，3-丁二醇二异丁烯酸酯、乙氧基化2的双酚A二异丁烯酸酯、乙氧基化 10的双酚A二异丁烯酸酯、乙氧基化6的双酚A二异丁烯酸酯、脂族氨基甲酸酯丙烯酸酯、脂族氨基甲酸酯低聚物、丙烯酸类低聚物、聚醚丙烯酸酯低聚物、聚丁二烯二异丁烯酸酯低聚物、二丙烯酸酯低聚物、三丙烯酸酯低聚物、聚酯丙烯酸酯低聚物、环氧丙烯酸酯和芳族氨基甲酸酯丙烯酸酯。
合适的有机溶剂包括脂族烃类(例如石油醚、戊烷、己烷、庚烷和异十二烷)；脂环族烃类(例如环己烷、甲基环己烷、乙基环己烷、四氢化萘和十氢化萘)；萜烯和类萜(例如松节油、松油、α-蒎烯、β-蒎烯、二戊烯和d-柠檬烯)；芳族烃类(例如苯、甲苯、二甲苯、乙苯、异丙基苯、均三甲苯、偏三甲苯、连三甲苯、甲基异丙基苯和苯乙烯)；氯代烃类(例如二氯甲烷、三氯甲烷、氯乙烷、1，2-二氯乙烷、1，1，1- 三氯乙烷、三氯乙烯、全氯乙烯和1，2-二氯丙烷)；醇类(例如甲醇、乙醇、丙醇、异丙醇、丁醇、仲丁醇、叔丁醇、戊醇、异戊醇、己醇、庚醇、辛醇、壬醇、甲基异丁基甲醇、2-乙基丁醇、异辛醇、2-乙基己醇、异壬醇、异癸醇、二异丁基甲醇、环己醇、甲基环己醇、三甲基环己醇、苄醇、甲基苄醇、糠醇、四氢糠醇、和双丙酮醇)；酮类(例如丙酮、甲乙酮、甲基丙基酮、甲基异丙基酮、甲基丁基酮、甲基异丁基酮、甲基戊基酮、甲基异戊基酮、二乙酮、乙基丁基酮、乙基戊基酮、二异丙基酮、二异丁基酮、环己酮、甲基环己酮、二甲基环己酮、三甲基环己酮、异丙叉丙酮、异佛尔酮、和乙酰丙酮)；酯类(例如甲酸甲酯、甲酸乙酯、甲酸丁酯、甲酸异丁酯、乙酸甲酯、乙酸丙酯、乙酸异丙酯、乙酸丁酯、乙酸异丁酯、乙酸仲丁酯、乙酸戊酯、乙酸异戊酯、乙酸己酯、乙酸庚酯、乙酸2-乙基己酯、乙酸环己酯、乙酸苄酯、丙二醇二乙酸酯、丙酸甲酯、丙酸乙酯、丙酸丙酯、丙酸丁酯、丙酸戊酯、丁酸乙酯、丁酸丙酯、丁酸丁酯、丁酸异丁酯、丁酸戊酯、异丁酸甲酯、异丁酸乙酯、异丁酸异丙酯、异丁酸异丁酯、乳酸甲酯、乳酸乙酯、乳酸异丙酯、乳酸丁酯、乙醇酸丁酯、乙二醇单甲醚乙酸酯、乙二醇单乙醚乙酸酯、乙二醇单丁醚乙酸酯、二甘醇单乙醚乙酸酯、二甘醇单丁醚乙酸酯、乙酸甲氧基丙酯、乙酸乙氧基丙酯、乙酸3-甲氧基丁酯、3-乙氧基丙酸乙酯、二酸酯、碳酸亚乙酯、碳酸亚丙酯和丁内酯)；二元醇醚类(例如乙二醇单甲醚、乙二醇单乙醚、乙二醇单丙醚、乙二醇单异丙醚、乙二醇单丁醚、乙二醇单己醚、乙二醇单苯醚、二甘醇单甲醚、二甘醇单乙醚、二甘醇单丁醚、二甘醇单己醚、三甘醇单甲醚、三甘醇单乙醚、三甘醇单丁醚、四甘醇单丁醚、1-甲氧基-2-丙醇、乙氧基丙醇、异丙氧基丙醇、丁氧基丙醇、异丁氧基丙醇、叔丁氧基丙醇、苯氧基丙醇、二丙二醇单甲醚、二丙二醇单异丙醚、二丙二醇单丁醚、三丙二醇单甲醚、三丙二醇单丁醚、二甘醇二甲醚和二丙二醇二甲醚)；醚类(例如二乙醚、二异丙醚、二丁醚、甲基叔丁基醚、四氢呋喃、二噁烷、2，2-二甲基-4-羟基甲基-1，3-二噁烷和1，2-环氧丙烷)；以及其他溶剂(例如二甲基乙缩醛、二甲基 甲酰胺、二甲基乙酰胺、二甲亚砜、环丁砜、二硫化碳、糠醛、硝基乙烷、1-硝基丙烷、2-硝基丙烷、N-甲基吡咯烷酮、N-乙基吡咯烷酮、N-环己基吡咯烷酮、N-(2-羟基乙基)吡咯烷酮、1，3-二甲基-2-咪唑烷酮和六亚甲基磷酰三胺)。这些有机溶剂也可以用于溶胀水溶性或亲水性丙烯酸类聚合物的基质。
在另一实施方案中，可以选择所述聚合物基质以使得该基质响应特定的活化剂而衍射不同的波长，所述活化剂例如溶液中的金属离子、有机分子例如葡萄糖、溶液中的气体、不同来源的抗原、不同来源的抗体、以及病毒例如HIV。例如，具有酸官能团的聚合物基质对含有碱的活化剂成分呈反应性，反之亦然，即其中基质具有碱官能团而活化剂具有酸官能团。可以选择聚合物基质以至于该基质响应不同的活化剂而溶胀、收缩或改变尺寸和/或折射率。基质可以包括抗原，当暴露于抗体时抗体与其结合。类似地，传感器可以基于酶和底物对、螯合剂、络合剂或适体(aptamers)。对于某些传感器，活化剂与基质的结合可能足够牢固以至于该活化剂保持与基质吸引、结合和/或处于其中，并且传感器很少或不恢复至其原始状态。在这些实施方案中，活化剂与基质之间可能存在共价键或离子键。本领域技术人员将会意识到本文公开的各种实施方案以及在本发明范围内的其他实施方案将在环境、医药、冶金和化学领域具有众多应用。
将意识到通过选择特定的基质组成和适当的活化剂，可以调节基质的衍射波长。本发明的辐射衍射传感器可以用于多种应用，包括标记或识别物品(例如在药物包装上鉴定药物来源)、用于鉴定文件等的安全装置、作为化学物种存在的传感器或者作为新型物品例如玩具。本发明的辐射衍射传感器可以单独提供或者以成套形式提供，连同接触该传感器的活化剂一起，该活化剂使衍射辐射移位至移位的波长。
本发明的传感器可以用于鉴定物品，例如鉴定文件或装置或者识别制造制品的来源。如果传感器响应活化剂，带有本发明传感器的文件、例如安全卡会被认为是真实的。“安全卡”包括鉴定其持有者的身份或者允许访问设施的文件或装置，例如是徽章形式。安全卡可以 识别该卡的持有者(例如图片身份卡或护照)或者可以用作指示其持有者被允许访问安全设施的文件或装置。例如，安全卡可能看来像是真实的，当施加合适的活化剂时，卡上的传感器将会显示被衍射的辐射的波长的移位。伪造的安全卡将不能显示该波长移位。同样地，在带有本发明传感器的包装中提供的物品(例如药品)的消费者可以通过向该包装施加合适的活化剂而检验其真实性。不响应活化剂的包装将被认为是伪造的，而响应该活化剂的包装将被认为是真实的。其他消费品可以包括本发明的传感器，例如在制造制品(例如电子器件)的外壳上或在衣着用品(例如鞋类)的表面上。消费品的真实性可以通过向其施加活化剂而进行检验或者传感器的活化可以是该物品的新颖特征。“物品”包括任意制品，其包括但不限于本文所述的那些，其中本发明传感器可以施加在其上。
在基底上形成有序的周期性颗粒阵列并用基质涂布，如上所述固化该基质以制成传感器。其上形成传感器的基底可以是随后施加在物品或另一表面(例如微孔片或金属箔的表面)上的膜或片。作为选择，物品的表面可以充当制备传感器的基底。在该情况下，在物品表面上形成有序周期性阵列并在其上涂布基质组合物。可以通过掩模将传感器施加在物品的一部分上从而将传感器设置在特定位置。物品表面的任何其余部分可以涂布或基本上涂布有合适的涂料组合物从而制成其中露出传感器但是任何的其余基底被涂布的基底。例如，可以将本发明的传感器施加在微孔片上，而且该片的其余部分可以被涂布、层叠等。如此可以制成安全卡。另外，传感器能够与合适的活化剂接触，同时该卡的其余部分通过涂布或层叠而被保护免于磨损和撕裂等。
使设置在物品上的传感器与使衍射辐射波长移位的活化剂接触。该移位的波长可以是在可见或不可见光谱内。除去活化剂后该传感器至少基本上恢复至其原始状态。例如，亲水性丙烯酸类聚合物基质通过暴露于水可溶胀。如果带有该传感器的身份卡与水接触，将会发生衍射波长的移位，由此证明该身份卡的真实性。当水蒸发时，衍射波长基本上恢复至其原始状态。
用于本文时，除非另作明确说明，诸如表示值、范围、量或百分比的那些的所有数值可以如同由措辞“约”作为前缀一样来理解，即使该术语没有明确出现。本文列举的任何数值范围意图包括其中包含的所有子范围。复数包括单数，反之亦然。例如，虽然在包括权利要求的本文中提及“一种”有序周期性阵列、“一种”基质、“一种”活化剂等等，但是可以使用多于一种，以及尽管提及改变基质的尺寸，但是可能仅改变一个尺寸。另外，本文使用的术语“聚合物”意味着指预聚物、低聚物以及均聚物和共聚物；前缀“多”是指二或更多。
辐射衍射传感器作为水印的这些示例性用途并不意味着是限制性的。另外，下列实施例只是说明本发明而且不意在限制。
实施例
实施例1：可固化的丙烯酸类基质
经由下列过程制成紫外辐射可固化的有机组合物。将来自Aldrich Chemical Company，Inc.，Milwaukee，Wis.的二苯基(2，4，6-三甲基苯甲酰)氧化膦和2-羟基-2-甲基-苯丙酮的50/50共混物(0.15g)在搅拌下加入到5.0g来自Sartomer Company，Inc.，Exton，Pa.的乙氧基化20的三羟甲基丙烷三丙烯酸酯中。
实施例2：可固化的丙烯酸类基质
经由下列过程制成紫外辐射可固化的有机组合物。将来自Aldrich Chemical Company，Inc.，Milwaukee，Wis.的二苯基(2，4，6-三甲基苯甲酰)氧化膦和2-羟基-2-甲基-苯丙酮的50/50共混物(0.15g)在搅拌下加入到4.0g来自Sar tomer Company，Inc.，Exton，Pa.的乙氧基化20的三羟甲基丙烷三丙烯酸酯中。然后将来自AldrichChemical Company，Inc.的丙烯酸(1.0g)在搅拌下加入到混合物中。
实施例3：可固化的丙烯酸类基质
经由下列过程制成紫外辐射可固化的有机组合物。将来自 Aldrich Chemical Company，Inc.，Milwaukee，Wis.的二苯基(2，4，6-三甲基苯甲酰)氧化膦和2-羟基-2-甲基-苯丙酮的50/50共混物(0.15g)在搅拌下加入到5g来自Sartomer Company，Inc.，Exton，Pa.的丙氧基化2的新戊二醇二丙烯酸酯中。
实施例4：核-壳颗粒的阵列
经由下列过程制备聚苯乙烯-二乙烯基苯核/苯乙烯-甲基丙烯酸甲酯-乙二醇二异丁烯酸酯-二乙烯基苯壳颗粒在水中的分散体。
将来自Aldrich Chemical Company，Inc.的碳酸氢钠(4.9g)与4090g去离子水混合并且加入到配备热电偶、加热套、搅拌器、回流冷凝器和氮气入口的12升反应釜中。在搅拌下用氮气吹扫混合物43分钟然后用氮气保护。将来自Cytec Industries，Inc.的气溶胶MA80-I(46.8g于410g去离子水中)在搅拌下加入到混合物中，接着是48g去离子水漂洗液。使用加热套将混合物加热至约50℃。在搅拌下加入出自Aldrich Chemical Company，Inc.的苯乙烯单体(832.8g)。将混合物加热至60℃。将来自Aldrich Chemical Company，Inc.的过硫酸钠(12.5g于144g去离子水中)在搅拌下加入到混合物中。将混合物的温度保持恒定40分钟。在搅拌下，将来自AldrichChemical Company，Inc.的二乙烯基苯(205.4g)加入到混合物中并且将温度保持在约60℃下2.3小时。将来自Aldrich ChemicalCompany，Inc.的Brij 35(聚氧乙烯(23)月桂醚)(5.0g于100g去离子水中)在搅拌下加入到混合物中。接下来，将来自AldrichChemical Company，Inc.的过硫酸钠(9.1g于900g去离子水中)在搅拌下加入到混合物中。将全都出自Aldrich Chemical Company，Inc.的苯乙烯(200g)、甲基丙烯酸甲酯(478.8g)、乙二醇二异丁烯酸酯(48g)和二乙烯基苯(30.2g)的混合物在搅拌下加入到反应混合物中。将来自Rhodia，Inc.Cranbury，NJ.的Sipomer COPS-I(3-烯丙氧基-2-羟基-1-丙烷磺酸82.7g)在搅拌下加入到反应混合物中接着加入(100g)去离子水进料。将混合物的温度保持在60℃下约4.0小时。
通过5微米滤袋将所得的聚合物分散体过滤。使用均来自PTIAdvanced Filtration，Inc.，Oxnard，CA.的具有2.41英寸聚偏氟乙烯膜的4英寸超滤外套超滤该聚合物分散体，并用蠕动泵以约170ml/s的流速泵送。在除去3000g超滤液之后向分散体中加入去离子水(2985g)。重复这种交换几次直到以11348g去离子水代替11349g超滤液为止。然后除去另外的超滤液直到混合物的固含量为44.8wt％为止。
通过来自Frontier Industrial Technology，Inc.，Towanda，PA的狭缝涂布机将材料施涂于2mil厚的聚对苯二甲酸乙二醇酯(PET)基底上并在180°F干燥40秒至约7微米的干燥厚度。用来自Varian，Inc.的Cary 500分光光度计测量，所得材料衍射518nm处的光。
实施例5：水溶性的固定阵列
用刮涂棒(drawdown bar)将实施例1制成的材料施涂于实施例4的聚苯乙烯-二乙烯基苯核/苯乙烯-甲基丙烯酸甲酯-乙二醇二异丁烯酸酯-二乙烯基苯壳颗粒的固定阵列上。然后将一片2mil厚的PET膜放在沉积的实施例1的材料上以使得完全覆盖该材料。在PET基底的顶面上使用辊从而使实施例1的UV可固化涂层展开并压入实施例4的固定阵列的间隙空间中。用100W汞灯将试样紫外辐射固化。然后分离两层PET。
该膜在与观察者垂直或成0度观察时显示出绿色，在与观察者成45度或以上观察时显示蓝色。用Cary 500分光光度计测量该膜的衍射波长。随后，将该膜暴露于水并再次测量衍射波长。在水蒸发之后最后一次测量该膜。下面在表1中列出的结果显示在施加水时该材料的衍射波长增大而除去水后基本上恢复至其原始状态。
表1
| 试样 | 衍射波长 |
| 初始状态 | 560nm |
| 水合(H2O) | 602nm |
| 干燥 | 558nm |
[0063] 实施例6：官能团可溶胀的固定阵列
除了用实施例2的材料(含有酸基)代替实施例1的材料以外，重复实施例5的过程。该膜在与观察者垂直或成0度观察时显示出绿色，在与观察者成45度或以上观察时显示蓝色。用Cary 500分光光度计测量该膜的衍射波长。随后，将该膜暴露于水并再次测量衍射波长。将该膜暴露于碱(二甲基乙醇胺(DMEA))在去离子水中的5％溶液，重新测量衍射波长。在DMEA溶液蒸发之后最后一次测量该膜。在表2中列出的结果显示含有酸基的膜的丙烯酸类聚合物基质材料既可由水又可由碱溶胀，而且在除去水和碱之后基本上恢复至其原始状态。
实施例6的制品与实施例5制品的区别在于实施例6的基质材料中包含酸官能团。与水接触时两种制品都溶胀，如同被衍射的辐射的波长从560nm变化为602nm所证实的那样。实施例6的制品在与碱(DMEA)接触时进一步改变，如同被衍射的辐射的波长进一步增大到623nm所证实的那样。
表2
| 试样 | 衍射波长 |
| 初始状态 | 560nm |
| 水合(H2O) | 602nm |
| 水合(H2O和DMEA) | 623nm |
| 干燥(H2O和DMEA) | 562nm |
实施例7：有机溶剂可溶胀的固定阵列
除了用实施例3的材料代替实施例1的材料以外，重复实施例5的过程。该膜在与观察者垂直或成0度观察时显示出绿色，在与观察者成45度或以上观察时显示蓝色。用Cary 500分光光度计测量该膜的衍射波长。随后，将该膜暴露于水并再次测量衍射波长，基本上没有变化。然后将该膜暴露于95％变性乙醇并测量衍射波长。在乙醇蒸发后最后一次测量该膜。在表3中列出的结果显示该膜不可由水溶胀，而是可由乙醇溶胀，并且在除去乙醇之后几乎恢复至其原始状态。
表3
| 试样 | 衍射波长 |
| 初始状态 | 556nm |
| 水合(H2O) | 556nm |
| 暴露于乙醇 | 610nm |
| 乙醇蒸发 | 564nm |
如本文表明的那样，本发明的辐射衍射材料可以用于感知水或有机溶剂的存在。
虽然上面描述了本发明的优选实施方案，但是在不脱离本发明的精神和范围的情况下，可以进行本发明的明显改进和变动。本发明的范围在所附权利要求及其等价物中限定。
Claims (30)
1.一种辐射衍射传感器，其包括：
在基底上形成的有序周期性颗粒阵列；和
涂布于所述颗粒阵列上的固体基质组合物；
其中所述基质组合物不是由水凝胶制成的，并且选择所述基质组合物以响应活化剂，以至于对所述活化剂的暴露使由所述传感器衍射的辐射的波长从第一波长移位至第二波长。
2.权利要求1的传感器，其中当从所述传感器处除去所述活化剂时，所述被衍射的辐射的波长基本上恢复至第一波长。
3.权利要求1的传感器，其中所述基质包括响应水的亲水性丙烯酸类聚合物。
4.权利要求1的传感器，其中所述基质包括响应有机溶剂的聚合物。
5.权利要求1的传感器，其中所述基底为膜。
6.权利要求1的传感器，其中所述基底为微孔片。
7.权利要求1的传感器，其中所述基底为制品的表面。
8.权利要求7的传感器，其中所述表面为制品的包装和/或外壳。
9.一种制备传感器的方法，其包括：
在基底上形成有序周期性颗粒阵列；
用固体基质组合物涂布所述颗粒阵列，所述基质组合物不是由水凝胶制成的；和
固化所述固体基质组合物以将所述颗粒阵列固定在该基质内，其中选择所述基质组合物以响应活化剂，以至于对所述活化剂的暴露使由所述传感器衍射的辐射的波长移位至移位的波长。
10.权利要求9的方法，其中所述活化剂包括水。
11.权利要求10的方法，其中所述基质包括亲水性丙烯酸类聚合物。
12.权利要求9的方法，其中所述活化剂包括有机溶剂。
13.权利要求12的方法，其中所述基质包括响应有机溶剂的聚合物。
14.权利要求9的方法，其中所述移位的波长在可见光谱内。
15.权利要求9的方法，其中所述移位的波长在可见光谱外。
16.权利要求9的方法，其进一步包括从所述基底处除去所述传感器。
17.权利要求16的方法，其进一步包括将所述传感器粉碎成颗粒形式。
18.权利要求9的方法，其中所述活化剂包含对所述基质呈反应性的官能团。
19.具有根据权利要求9的方法制成的传感器的制品。
20.一种鉴定制品的方法，其包括：
在基底上形成有序周期性颗粒阵列；
用非水凝胶基质涂布所述颗粒阵列；
固化所述基质以将所述颗粒阵列固定在该基质内，从而制成衍射第一波长的辐射的传感器；
将所述传感器施用于制品；和
使所述传感器与活化剂接触，以至于所述活化剂使得衍射波长移位，其中移位的衍射波长指示所述制品的真实性。
21.权利要求20的方法，其中所述移位的波长在可见光谱内。
22.权利要求20的方法，其中所述移位的波长在可见光谱外。
23.权利要求20的方法，其中所述基底为施加在所述制品上的膜。
24.权利要求20的方法，其中所述基底为所述制品的表面。
25.权利要求20的方法，其中所述基底为微孔片。
26.权利要求20的方法，其进一步包括从所述传感器处除去所述活化剂，以使得所述被衍射的辐射的波长基本上恢复至第一波长。
27.权利要求20的方法，其中所述制品为安全卡。
28.权利要求20的方法，其中所述基底为挠性的。
29.权利要求20的方法，其中所述基底为EVA泡沫。
30.权利要求20的方法，其中所述基底为金属。
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| Hiroshi Fudouzi等.Colloidal crystals with tunable colors and their use as photonic papers.《Langmuir》.2003,第19卷(第23期),9653-9660. * |
Also Published As
| Publication number | Publication date |
|---|---|
| RU2436072C2 (ru) | 2011-12-10 |
| US20080185498A1 (en) | 2008-08-07 |
| BRPI0720803A2 (pt) | 2014-03-04 |
| PE20081239A1 (es) | 2008-10-10 |
| TW200837343A (en) | 2008-09-16 |
| CA2676734C (en) | 2013-02-26 |
| EP2122335A1 (en) | 2009-11-25 |
| JP2012215893A (ja) | 2012-11-08 |
| AU2007346613B2 (en) | 2011-02-24 |
| CN101622524A (zh) | 2010-01-06 |
| TWI359267B (en) | 2012-03-01 |
| JP2010518447A (ja) | 2010-05-27 |
| RU2009133272A (ru) | 2011-03-20 |
| AR064094A1 (es) | 2009-03-11 |
| AU2007346613A1 (en) | 2008-08-14 |
| NZ578623A (en) | 2012-04-27 |
| KR101114588B1 (ko) | 2012-03-05 |
| NO20092971L (no) | 2009-09-04 |
| CL2007003492A1 (es) | 2008-07-04 |
| US7682530B2 (en) | 2010-03-23 |
| UA94646C2 (ru) | 2011-05-25 |
| KR20090123872A (ko) | 2009-12-02 |
| CA2676734A1 (en) | 2008-08-14 |
| UY30765A1 (es) | 2008-07-03 |
| HK1137806A1 (en) | 2010-08-06 |
| MX2009008457A (es) | 2009-08-17 |
| WO2008097397A1 (en) | 2008-08-14 |
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