CN101094936B - 使用有图案的形貌和自组装单层的微组装 - Google Patents
使用有图案的形貌和自组装单层的微组装 Download PDFInfo
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- 229910001936 tantalum oxide Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 238000005406 washing Methods 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- 229910000500 β-quartz Inorganic materials 0.000 description 1
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- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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Abstract
公开了将金属选择性无电沉积在具有金属性微结构表面上的方法。所述方法包括在所述金属性微结构表面上形成自组装的单层，将所述自组装单层暴露到含有可溶形式沉积金属的无电镀溶液中，并将所述金属选择性地无电沉积在所述金属性微结构表面上。还公开了由本方法形成的制品。
Description
背景
本公开涉及在基质上制造有图案的金属性沉积物的方法以及由此制造的制品。
具有金属材料图案的聚合物膜具有多种工业应用。有些情况下，人们要求的是导电栅板足够细以至肉眼不可见，并负载在透明的聚合物基质上。透明的导电薄片具有各种用途包括，例如，耐加温玻璃窗，电磁干扰(EMI)屏蔽层，静电耗散元件，天线，用于计算机显示器的触摸屏，以及用于铬电极(electrochromic)窗口的表面电极，光电装置，电场致发光器件，以及液晶显示器。
将基本透明的导电栅板用于例如电磁干扰保护等应用是已知的。栅板可以由网络或金属线栅网形成，其插入或叠压在透明的薄片之间，或嵌入基质当中(美国专利3,952,152；4,179,797；4,321,296；4,381,421；4,412,255)。使用金属丝网筛的一个缺点是操作极细金属丝或制备以及操作极细金属丝栅网时的困难性。例如，直径20微米的铜丝其拉伸强度仅为1盎司(28克力)因此容易损坏。用直径20微米的导线制造的金属丝网筛可以购得但是由于在极细金属丝操作中的困难而非常昂贵。
与其将已存在的金属丝网筛嵌入基质当中，不如在原位制造出导电图形，即先在基质中形成凹槽或通道的图案然后用导电的材料填充凹槽或通道。该方法已经用于通过各种方法制备导电的线路图线路和图案，尽管一般都是针对相对粗糙尺度上的线路和图案。基质中的凹槽可以通过塑模，压印，或通过平版印刷技术形成。然后凹槽可以用导电的油墨或环氧树脂类充填(美国专利5,462,624)，充填方法包括蒸发，溅射，或镀金属(美国专利3,891,514；4,510,347；和5,595,943)，通过熔融金属(美国专利4,748,130)，或通过金属粉末(美国专利2,963,748；3,075,280；3,800,020；4,614,837；5,061,438；和5,094,811).已经可以通过印刷导电胶(美国专利5,399,879)或通过光刻和蚀刻法(美国专利6,433,481)在聚合物膜上制备导电的栅板。这些先有技术方法具有局限性。例如，导电油墨或环氧树脂带有的一个问题是电导率取决于邻近的导电颗粒之间形成的接触，并且总电导率通常大大低于固体金属。金属的气相沉积或电镀通常是缓慢的并且随后经常需要后继步骤，即除去沉积在凹槽之间的多余金属。熔融金属可以置于凹槽中但是通常需要在凹槽中沉积金属可润湿的材料。否则熔融金属由于熔融金属的表面张力而无法穿透也不会停留在凹槽中。
通过将金属粉末放入凹槽中随后压紧粉末以增强颗粒之间的电接触已经制备出了电路。Lillie等(美国专利5,061,438)和Kane等(美国专利5,094,811)已经用该方法制成了印刷电路板。但是，这些方法实际上无法用于制备精细的电路和精细的金属图形。在精细尺度上，在压印图案内更换或再对准机具以施行金属压紧是困难的。例如，带有20微米宽通道图案的薄片要求机具从薄片的一侧到另一侧以大致3微米的精度放置在图案内。对于许多应用，薄片的尺度可能是30cm乘30cm。从成型温度到室温的冷却过程中由于热塑片的热收缩产生的尺寸变化通常为约百分之一或更多。因此，对于30cm乘30cm的薄片，百分之一的收缩将导致0.3厘米的总体收缩。该值较所需的3微米放置精度大出约1000倍，精确地将机具复位是困难的。
概述
本公开涉及包含具有有图案的金属性沉积的基质的制品。更具体地说，制品是通过选择性且无电地将金属沉积在具有金属性微结构表面的基质上制备的。
第一方面涉及的方法包括提供具有金属性微结构表面的基质，在金属性微结构表面上形成自组装单层，将自组装单层暴露到含有可溶形式的沉积金属的无电镀溶液中，并无电地将沉积金属选择性地沉积到金属性微结构表面上。
可用不同的方法形成具有金属性微结构表面的基质。在一个实施方案中，可以用机械机具在金属性表面上形成微结构。机械机具可以将微结构压印，划割，或塑模到金属性表面上。在另外的实施方案中，微结构可以利用机械机具在基质表面上形成，然后可以在微结构表面上布置金属层以形成金属性微结构表面。机械机具可以将微结构压印，划割，或塑模到基质表面上。在又一个实施方案中，微结构可以通过在基质表面上沉积金属或通过从金属性基质表面上除去金属而形成。
在另一个方面中，提供了制品。在一个实施方案中，制品包括的基质具有基质表面和布置在基质表面上的形貌特征。连续的均匀金属层布置在邻近形貌特征的基质表面上和形貌特征上。自组装单层布置在连续的均匀金属层上，而沉积金属布置在形貌特征上的连续均匀金属层上，并且未布置在邻近形貌特征的连续均匀金属层表面上。
在另一个实施方案中，制品包括的基质具有基质表面和布置在基质表面上且延伸离开基质表面的形貌特征。形貌特征的曲率半径为500纳米或更小。金属层布置在邻近形貌特征的基质表面上和形貌特征上。自组装单层布置在金属层上，而沉积金属布置在形貌特征上的金属层上，并且未布置在邻近形貌特征的金属层基质表面上。
本发明上述摘要不打算描述实施方案的每一公开或本发明的每一个实施方案。下述的附图，发明详述和实施例将更具体地举例说明本实施方案。
附图简述
考虑到以下本发明各个实施方案的详细说明连同附图，本发明可被更完全地理解，其中：
图1是使用有图案的形貌和自组装单层的微组装的说明性方法的简图；
图2是使用有图案的形貌和自组装单层的微组装的另一个说明性方法的简图；
图3是在微结构上形成沉积金属的说明性微结构的剖视图简图；
图4是实施例1中所得结构的扫描电镜照片；
图5是实施例2中所得结构的扫描电镜照片；
图6是实施例3中所得结构的照片；以及
图7是实施例4中所得结构的照片。
虽然本发明可接受不同的修改和替代的形式，其细节已经在附图中通过实例示出并且将详细描述。但是，应该理解其目的不是将本发明限制于所述特定的实施方案。相反地，目的是包括所有修改，同等物，以及替代方案，只要其符合本发明的实质和范围。
发明详述
本公开涉及在基质上制造有图案的金属性沉积物的方法以及由此制造的制品。更具体地说，在具有金属性微结构表面的基质上的金属性沉积是有图案的。
对于以下定义词，应该适用以下定义，除非在本说明书中的权利要求或其它地方给出了不同的定义。
″区域″是指整个表面，例如基质表面的邻接的部分的区域。
术语″沉积金属″和″金属性沉积″以及″沉积的金属″被可交换地使用并指代沉积在基质(即，具有金属性微结构表面的基质)上的金属。沉积金属通常由无电镀溶液形成。沉积金属可以是图案的形式，诸如电路图中的线性痕迹，电气装置中的接触垫，或大面积涂层。
表层区如果包括形貌特征就可以描述为具有微结构或是一个微结构。″形貌特征″是指不同于光滑的基质表面的故意的几何图形。应当理解，根据术语，形貌学，的一般定义，所有表面都会表现出一定的形貌。但是，用于本文时″形貌特征″不包括大量偶然的形貌学类型，其为本领域技术人员所熟知。″形貌特征″不包括原子尺度上表面高度偶然的变化。″形貌特征″也不包括大表面积中通常存在的，相对于相同表面积中的平均高程而言的，表面高度偶然的逐渐变化。例如，″形貌特征″不包括″峰-至-谷″形式的平滑的高度波动，其实质上在尺寸上小于其空间离距。仅仅包括上述形貌学的偶然形式的表面被认为是名义上光滑的。名义上光滑的表面可以是平坦的或弯曲的，其中弯曲度小于0.1(微米)-1。″形貌特征″可以包括伸出的元素，侵入的几何元素，或两者都有。作为基质表面形貌特征一部分存在的线性伸出性几何元素的一种实例是一个峰脊，其从名义上光滑的表面上伸出。作为基质表面形貌特征一部分存在的线性伸出性几何元素的另一个实例是一个正方形脊，其从名义上光滑的表面上伸出。作为基质表面形貌特征一部分存在的线性侵入性几何元素的实例是凹槽，其具有正方形或三角形的横截面例如，其可在名义上光滑的表面之下延伸。
″选择性地″沉积金属是指在一个表层区沉积金属而不在另一个表层区沉积金属。对于要在基质表面上选择性沉积的金属，其不沉积在整个基质表面上。即，沉积金属在基质表面上形成图案。图4至7示出了铜在金基质表面上的选择性沉积。例如，金属可以沉积在金属性表面的形貌特征上(即，金属不沉积在名义上光滑的金属性表面的区域中)。
所述带有终点的数值范围包括所有包含在范围内部的数字(例如1至5包括1，1.5，2，2.75，3，3.80，4，和5)。
用于本说明书及所附加权利要求时，单数形式″一个″包括多于一个对象，除非内容清楚地另有所指。因此，例如，指出一个组合物含有″一个金属″包括两种或多种金属的混合物。用于本说明书及附带的权利要求时，术语″或者″通常在语句中表示″和/或″，除非内容清楚地另有所指。
除非另有陈述，所有用于本说明书及权利要求的数字均应被理解为在一切情况下由术语″约″修饰。因此，除非表明有相反的意思，示于上文说明书及所附权利要求中的数字参数是近似值，其可根据设法得到的希望的性能而由本领域技术人员利用本发明指导进行改变。至少，且不试图限制与本权利要求范围等效的原则的应用，各数字参数至少应该视为按照所报导有效数字的数目并且适用于普通的舍入方法。尽管阐明本发明宽的范围的数值范围和参数是近似值，示于实施例中的数值在报导时尽可能精确。但是任何数值必然含有某些误差，这由其相应的试验测定中产生的标准偏差确定。
本发明主要涉及在具有金属性微结构表面的基质上形成金属性沉积(即，沉积金属)图案的方法。在一些实施方案中，沉积金属无电地沉积在基质上，沉积仅发生在基质表面上选定的区域中。这些选定的区域在基质上可能表现出规则的或重复的几何排列，例如一系列多角形或痕迹的图案定义出离散的未沉积区域，所述区域包括了一系列多角形。在另一个实施方案中，选定的区域可能在基质上表现出无规的排列，例如无规的痕迹的网络，其定义了不规则的形状的未沉积区域的边界。在又一个实施方案中，选定的区域可能表现出不规则，不重复的，或无规的排列，但它是特别的设计，其包括或没有对称性或重复的形状。有图案的沉积金属可能仅存在于基质表面的一个区域之中，或者可能存在于基质表面的一个以上的区域之中；但是作为图案其可能不存在于基质表面的所有区域之中。
具有包括微结构的区域和不包括微结构的区域的基质可具有大量不同的形式。在一个实施方案中，基质表面可能包括相邻的区域，其各自是光滑的且没有形貌特征，而且可能互相平行，但是相对于彼此高出或者降低。后一种结构必然导致一种渐变区的存在，其相对于上述的光滑区域具有斜率和角度或者高的弯曲度。渐变区可以定义光滑区域之间的边界并且是一种形貌特征。在另一个实施方案中，基质表面包括光滑的而且没有微结构的区域，以及那些可以描述为织构形式的微结构的区域。该构造可以包括界定的几何元素诸如峰脊，角锥，桩，或者凹槽。替代地，该构造可能包括无规形状的几何元素。包括微结构的表层区中的微结构是这样的构造，其在空间上相对于光滑的，可能平坦的，并且没有形貌特征的区域而言在空间上平均高度更高一些。基质表面构造区域的空间的平均高度可能低于或高于邻近的光滑的并且可能平坦的基质表面区域。这样的构造区域可以分别从相邻区凹入或伸出。
基质上有图案的金属性沉积，其中包括金属性沉积的表层区的排列根据基质的形貌特征决定，可能表现为该形貌特征可能具有的大量空间关系中的一种。例如，对于那些包括形貌特征的区域，各区域可以包括单个的由没有形貌特征的相邻区间隔开来的几何元素，并且有图案的金属性沉积可以选择性地沉积在单个形貌特征上。在这种情况下，该金属性沉积的图案实质上将会和单个形貌特征的图案一致。或者，如果形貌特征密集地分布在基质的一个区域中，金属性沉积可以将包括形貌特征的区域中的几何图形或形貌单元跨接。如果基质表面包括了织构形式的微结构的区域，所述构造由多个密集间隔的形貌特征组成，还包括那些没有这样的微结构的区域，有图案的金属性沉积可以将密集间隔的形貌特征跨接，得到在整个具有织构形式的微结构的区域上的沉积。
用于形成具有有结构表面的制品的方法，例如，使用机械机具，将材料沉积在基质上，或从基质上除去材料。示例的机械机具通过将微结构压印，划割，或塑模到基质表面上以形成微结构。
用于形成具有有结构的表面的制品的方法的部分列表包括钻石机械加工(M.A.Davies，C.J.Evans，S.R.Patterson，R.Vohra，和B.C.Bergner，″Application of Precision Diamond Machining to theManufacture of Micro-photonics Components，″Proc.of SPIE 5183 94-108(2003))，光刻，电子束蚀刻，X射线蚀刻，激光束书写，电子束书写，和激光烧蚀(E.B.Kley，″Continuous Profile Writing by Electronand Optical Lithography，″Microelectronic Engineering 34 261-298(1997)).用于形成有结构表面的方法可以包括这样的步骤，其中材料暴露于光线，X-射线，或电子之下，然后显影并选择性地除去，或这样的步骤，其中材料被蚀刻(Y.Hagiwara，N.Kimura，and K.Emori，U.S.Patent 4,865,954″Process for Formation of Metallic Relief(1989))。材料(例如，金属)可以通过常规方法选择性地添加到基质表面上，以形成有结构的表面，所述方法包括，例如，溅射，气相沉积，等等。材料(例如，金属)可以通过常规方法包括，例如，蚀刻等等从基质上去掉，以形成有结构的表面。这些添加和除去方法可以与其他方法诸如，例如，光刻法以及揭除方法结合。
用于制备有结构的表面的特别有利的方法包括用机械机具复制或形成微结构。机械机具通过将微结构压印，划割，或塑模到基质表面上以形成微结构。复制包括将表面结构特征从样板机具传输到另一个材料并包括压印或塑模。包含复制的方法是值得注意的，因为这样可以容易并快速地形成具有的结构的表面的材料。同样值得注意的是通过复制使所形成的表面结构特征达到小的尺寸。可以复制尺寸小于10纳米的钠米级构造(S.R.Quake and A.Scherer，″From Micro-toNanofabrication with Soft Materials，″Science 290 1536-1540(2000)；V.J.Schaeffer and D.Harker，″Surface Replicas for Use in the ElectronMicroscope，″Journal of Applied Physics 13，427-433(1942)；以及H.Zhang和G.M.Bensen，WO 0168940 A1，″Methods for replication，replicated articles，and replication tools″(2001))。
复制可以通过任何数量的方式实现。将样板机械机具的表面结构特点复制入另一个材料表面的示例性方法是通过热压印(M.J.Ulsh，M.A.Strobel，D.F.Serino，和J.T.Keller，U.S.Patent No.6,096,247″Embossed Optical Polymeric Films″(2000)；和D.C.Lacey，U.S.PatentNo.5,932,150″Replication of Diffraction Images in Oriented Films″(1999)).热压印包括将样板机械机具压到可变形的材料上，导致样板机具的表面结构引起可变形的材料的表面产生变形，从而形成样板机具表面的负复型。可以被表面结构压印的材料包括，例如，软金属和有机材料如聚合物。可以被压印的软金属实例包括铟，银，金，和铅。适用于热压印的聚合物包括热塑性塑料。热塑性塑料的实例包括聚烯烃，聚丙烯酸酯，聚酰胺，聚酰亚胺，聚碳酸酯，和聚酯。热塑性塑料另外的实例包括聚乙烯，聚丙烯，聚苯乙烯，聚(甲基丙烯酸甲酯)，双酚A聚碳酸酯，聚(氯乙烯)，聚(对苯二甲酸乙二酯)，和聚(偏二氟乙烯)。为了制备热压印材料，从膜形式的材料开始常常是方便的并且可用的。任选，用于压印的膜可以包括多个层(J.Fitch，J.Moritz，S.J.Sargeant，Y.Shimizu，和Y.Nishigaki，U.S.Patent No.6,737,170″Coated Film with Exceptional Embossing Characteristics and Methods forProducing It″(2004)；和W.W.Merrill，J.M.Jonza，O.Benson，A.J.Ouderkirk，和M.F.Weber，U.S.Patent No.6,788,463，″Post-FormableMultilayer Optical Films and Methods of Forming″(2004)).
另一个用于将主机械机具的表面结构复制入聚合物表面里的方法是将聚合物的可流动前体当与样板机械机具接触的时候固化。将可流动前体在其与主机械机具接触时固化为聚合物是一种形式的塑模。可流动前体的实例包括纯的单体，单体混合物，单体溶液或可能含有可除去的溶剂，以及未交联的聚合物的聚合物。通常，待固化为聚合物的前体可以浇铸在样板机械机具上或浇铸到塑模里，随后固化(J.A.Martens，U.S.Patent No.4,576,850″Shaped Plastic Articles HavingReplicated Microstructure Surfaces″(1986)).固化指形成提高的弹性模数，通常通过化学反应。固化以发展弹性模数包括加热，添加催化剂，添加引发剂，或暴露于紫外光，可见光，红外光，X射线，或电子束下。聚合物一旦固化，其可作为固体脱离与样板机具或塑模的接触。适用于塑模的聚合物实例包括聚丙烯酸酯，聚酰亚胺，环氧树脂类，聚硅氧烷，聚氨酯，以及聚碳酸酯。
使用机械机具在基质表面上形成微结构图案的另一个示例性方法是划割。″划割″指将尖笔施加至另外的无特定结构的表面上并使尖笔在表面上按压或移动，以形成表面微结构。尖笔尖端可以由任何材料如，例如，金属，陶瓷，或聚合物制成。尖笔尖端可以包括钻石，氧化铝，或碳化钨。尖笔尖端还可能包括涂层，例如抗磨耗覆盖层如一氮化钛。
基质可以由任何适合的材料制备。在一些实施方案中，基质用金属或有机物质如聚合物制成。金属的实例包括铟，银，金，和铅。聚合物的实例包括热塑性聚合物。热塑性聚合物的实例包括聚烯烃，聚丙烯酸酯，聚酰胺，聚碳酸酯，和聚酯。热塑性塑料另外的实例包括聚乙烯，聚丙烯，聚苯乙烯，聚(甲基丙烯酸甲酯)，双酚A聚碳酸酯，聚(氯乙烯)，聚(对苯二甲酸乙二酯)，和聚(偏二氟乙烯)。
在另一个实施方案中，基质可以由玻璃，玻璃-陶瓷，陶瓷，半导体，或其组合制备。可用玻璃的实例包括硅酸盐，锗酸盐，磷酸盐，和硫属化物。在硅酸盐当中，可以使用碱-石灰-氧化硅和硼硅玻璃。熔融石英也可以作为有用的基质材料。与硅酸盐玻璃相比，如果希望提高红外透射能力，则锗酸盐和硫属玻璃是特别适用的。磷酸盐玻璃的方便之处在于通常表现出低成型温度，但是也常常表现出较低的化学稳定性。其他可用玻璃中的网络成形剂和改性剂包括氧化铝，五氧化二锑，氧化钽，氧化铌，氧化铅，氧化铋，氧化锌，氧化镁，氧化锶，氧化钡，氧化锂，和氧化钾。含有晶化微结构的玻璃-陶瓷也可用作基底材料。可用的玻璃-陶瓷的实例包括焦硅酸锂，β-石英，顽辉石，堇青石，尖晶石，β-锂辉石，β-锂霞石，和磷灰石组合物。玻璃-陶瓷可提供玻璃的易于模锻性，以及高的强度和韧性。基质还可以包括陶瓷。可用陶瓷的实例包括氧化物，氮化物，硼化物，和碳化物。可用陶瓷的实例包括钛酸钡、钡钛酸锶、锆钛酸铅、钛酸铋、氧化铝、氧化铍、氮化铝、四氮化三硅、和碳化硅。基质还可以包括半导体。可用半导体的实例包括IV族元素、II族和VI族元素的二元化合物、III族和V族元素的二元化合物、及其各种合金。一些可用的半导体包括硅、锗、砷化镓、磷化铟、硫化锌、和碲化镉。基质可以由这些材料中一种以上制备。例如，基质可以包括具有玻璃或陶瓷材料涂层的半导体晶体。
″自组装的单层″指与表面连接(例如，通过化学键)的一层分子，且其相对于该表面采用优选取向。已经表明自组装的单层如此完全地覆盖了表面以致于表面的性能被改变。例如，自组装单层的应用可以导致表面能降低。
适用于形成自组装单层的化学物种的实例包括有机化合物如有机硫化合物、硅烷、膦酸、苯并三唑、和羧酸。这样的化合物的实例参见Ulman的综述(A.Ulman，″Formation and Structure of Self-AssembledMonolayers，″Chem.Rev.961533-1554(1996))。除了有机化合物之外，某些有机金属化合物可用于形成自组装单层。适于形成自组装单层的有机硫化合物的实例包括烷基硫醇、二烷基二硫化物、二烷基硫化物、烷基黄原酸酯、和二烷基硫代氨基甲酸酯。适于形成自组装单层的硅烷的实例包括有机氯硅烷和有机烷氧基硅烷。适于形成自组装单层的膦酸的实例参见Pellerite等的文献(M.J.Pellerite，T.D.Dunbar，L.D.Boardman，and E.J.Wood，″Effects of Fluorination on Self-AssembledMonolayer Formation from Alkanephosphonic Acids on Aluminum：Kinetics and Structure，″Journal of Physical Chemistry B 107 11726-11736(2003))。适于形成自组装单层的化学物种可以包括，例如，烃类化合物、部分氟化烃化合物、或全氟化化合物。自组装单层可以包括两种或多种不同的化学物种。在使用两种或多种不同的化学物种时，化学物种可以作为混合物或以相分离形态存在于自组装单层中。
可用于形成自组装单层的示例性分子包括，例如，(C3-C20)烷基硫醇、(C10-C20)烷基硫醇或(C15-C20)烷基硫醇。烷基可以是线性或支链的，并且可以被那些不干扰自组装单层形成的取代基所取代或未被取代。
自组装单层可以用各种方法在金属表面上形成。例如，金属表面可以浸入含有所述化学物种的溶液中，金属表面可以被含有所述化学物种的溶液喷雾处理，或金属表面可以在气相中暴露于所述化学物种下。任何过量的不连接到金属表面的化学物种可以被除去，例如，通过用适合的溶剂冲洗。
金属性表面可用于负载自组装单层。所述金属表面包括，例如，金属元素、金属合金、金属间化合物、金属氧化物、金属硫化物、金属碳化物、金属氮化物、及其组合。用于负载自组装单层的金属性表面包括金、银、钯、铂、铑、铜、镍、铁、铟、锡、钽，及其混合物、合金、以及这些元素的化合物。
术语″无电镀″指用于自催化镀金属的方法。其通常包括使用含有可溶形式的沉积金属以及还原剂的无电镀溶液。所述可溶形式的沉积金属通常是离子形式或金属配合物(即，与一种或多种配体配位的金属物种)。在许多实施方案中，无电镀不包括对待涂覆工件施加电流。Mallory和Hajdu著作中详细地描述了所述工艺(Electroless Plating-Fundamentals and Applications，Ed.G.O.Mallory and J.B.Hajdu，William Andrew Publishing，Norwich(1990))。无电镀中包含的步骤包括制备具有催化表面(例如，金属性微结构表面)的基质，随后将基质浸泡在适当的镀浴中。催化表面催化金属从溶液中的沉积。一旦开始，镀的过程会通过持续还原溶液金属源进行下去，被其自己的金属表面催化，即所谓″自催化″。可以用无电镀形成的金属性沉积包括铜、镍、金、银、钯、铑、钌、锡、钴、锌，以及这些金属相互之间或与磷或硼的合金，以及这些相互之间或与磷或硼的化合物。适合的还原剂包括，例如，甲醛、肼、氨基硼烷，和次磷酸盐。用于催化无电镀的适合的金属性微结构表面包括钯、铂、铑、银、金、铜、镍、钴、铁、和锡，以及所述元素相互之间或与其他元素的合金和化合物。沉积金属和包括在金属性微结构表面中的金属可以是相同或不同的。
不希望受缚于任何特定的理论，我们认为表面上形貌特征对连接到所述表面的自组装单层的结构的破坏性会足以使得自组装单层改变表面性能的能力受到损害。例如，已知金表面具有负载自组装单层的性能和催化金属非电沉积的性能。在过去，已经表明在金上的自组装单层将阻遏其对于无电镀的催化活性(A.Kumar and G.M.Whitesides，U.S.Patent No.5,512,131，″Formation of Microstamped Patterns onSurfaces and Derivative Articles，″(1996))。
另外，假定金属如金表面的形貌特征可能干扰自组装单层的能力以阻遏其催化活性，从而形成用于形成图案的方法的基础。导致如此明显的催化活性上的破环的形貌特征可以方便地通过压印、划割、或塑模方法形成。
图1是使用有图案的形貌和自组装单层的微组装的说明性方法的简图。基质105含有布置在所述基质105上的金属层110。在一个实施方案中，基质105由聚合物材料形成，而金属层110由金属形成。在许多实施方案中，金属层110是连续均匀金属层。在一个实施方案中，所述连续均匀金属层110由单一金属或合金形成。
显示机械机具120具有形成于机械机具120第一表面135之上的形貌特征130。机械机具120可以施用于金属层110的表面140上从而机械机具120第一表面135与金属层110的表面140接触。在一个实施方案中，压力(如图中向下的箭头所示)施用于机械机具120上从而微结构或形貌特征130的负复型转移到或压印到金属层110的表面140上，在金属层110的表面140上形成微结构131。这样机械地形成的微结构131称为金属性微结构表面136。微结构制品101含有具有金属性微结构表面136的基质。
如上所述，在102步中在金属性微结构表面136上形成自组装单层150。在这个实施方案中，显示自组装单层150布置穿过金属层110的整个表面140。自组装单层150可以沿着金属层110表面140均匀地布置。自组装单层150可以在微结构131上或靠近微结构131处具有中断的区域。至少在一些实施方案中，在微结构131上或靠近微结构131处的中断区域由微结构131的形貌引起。
自组装单层150在103步暴露至含有沉积金属可溶形式的无电镀溶液160中。沉积金属可以在104步中沉积在金属性微结构表面136上以形成沉积金属图案165。在一个实施方案中，沉积金属含有铜而金属性微结构表面136由金形成。在一些实施方案中，至少一部分金属层110可以在沉积金属沉积之后通过蚀刻除去。
不希望受缚于任何特定的理论，相信自组装单层150中的中断区域使得沉积金属可以在形成于微结构131之上或附近的中断区域处与金属层140结合。
图2是另一个使用有图案的形貌和自组装单层的微组装的说明性方法的简图；显示机械机具220具有形成于机械机具220的第一表面235之上的形貌特征230。机械机具可以施用于基质205的表面206上从而机械机具220第一表面235与基质205的表面206接触。在一个实施方案中，压力(如图中向下的箭头所示)施用于机械机具220上从而微结构或形貌特征230被转移到基质205的表面206上从而在步骤201中在基质205表面206上形成微结构208。机械地形成的微结构208被定义为基质微结构表面207。
然后金属层210在步骤202中布置在基质微结构表面207上以形成金属性微结构表面236。在一个实施方案中，基质205由聚合物材料形成，而金属层210由金属形成。在许多实施方案中，金属层210是连续均匀金属层。在一个实施方案中，连续均匀金属层210由单一金属或合金形成。
如上所述，在202步骤中在金属性微结构表面236上形成自组装单层250。显示自组装单层250布置在金属层210的整个表面240上。在一个实施方案中，自组装单层250沿着金属层210表面240均匀地布置。自组装单层250可以在微结构231上或靠近微结构231处具有中断的区域。至少在一些实施方案中，在微结构231上或靠近微结构231处的中断区域由微结构231的形貌引起。
自组装单层250在203步暴露至含有可溶形式沉积金属的无电镀溶液260中。沉积金属可以在204步中沉积在金属性微结构表面236上以形成沉积金属图案265。在一个实施方案中，沉积金属含有铜而金属性微结构表面236由金形成。在一些实施方案中，至少部分金属层210可以在沉积金属沉积之后通过蚀刻除去。
不希望受缚于任何特定的理论，相信自组装单层250中的中断区域使得沉积金属可以在形成于微结构231之上或附近的中断区域处与金属层240结合。
图3是示例性微结构与在微结构上形成的沉积金属365的剖视图。金属性微结构表面336含有邻近形貌特征320的光滑区域330。显示形貌特征320是向外延伸离开基质的突起的构造。在这个实施方案中，平滑区域330和形貌特征320由单一连续均匀金属层336形成。自组装单层350布置在所述单个连续均匀金属层336上。沉积金属365通过无电镀浴360选择性地形成于形貌特征320的中断区域361上。
在一些实施方案中，形貌特征320延伸离开基质并且其曲率半径R为500纳米或更小，或从5至500纳米，或从10至500纳米，或从20至250纳米，或从50至200纳米。曲率半径R可以通过，例如，扫描探针显微镜，例如原子力显微镜测量
在许多实施方案中，从基质伸出的有用形貌特征的高度范围可以从1纳米至100微米，或从10纳米至10微米，或从20纳米到1微米。
沉积金属可以描述为在基质表面上具有一定区域形状和区域大小，以及厚度。沉积金属的区域形状在基质上可能表现出规则的或重复的几何排列，例如一系列沉积金属多角形或沉积金属痕迹的图案定义出离散的未沉积区域的边界，所述区域包括了一系列多角形。在其他实施方案中，沉积金属形状可能在基质上表现出无规的排列，例如无规的痕迹的网络，其定义了不规则的形状的未沉积区域的边界。在又一个实施方案中，沉积金属形状可能表现出不规则，重复的，或无规的排列，但它是特别设计的，其包括或没有对称性或重复的几何元素。在一个实施方案中，可用于产生光传输，EMI屏蔽材料的沉积金属形状是方格网，其含有沉积金属的痕迹的特征在于宽度，厚度，和斜角。其他用于产生光传输，EMI屏蔽材料的有用的形状包括连续的金属性痕迹，其界定的开放区具有正六边形形状而且以密堆积的秩序排列。
在一些实施方案中，沉积金属外形的最小区域尺寸，例如沉积金属的线性痕迹的宽度，范围可以是1纳米至1毫米，或从10纳米至50微米，或从100纳米至25微米，或从1微米到15微米。在一个制备光传输EMI屏蔽材料的示例性实施方案中，沉积金属线性痕迹的宽度范围为5微米至15微米；厚度范围为1微米至5微米；而斜角范围为25微米至1毫米。上述沉积金属外形的最大区域尺寸，例如沉积金属的线性痕迹的长度，范围可以从1微米至5米，或从10微米到1米。为了制备光传输EMI屏蔽材料，一张EMI屏蔽材料沉积金属线性痕迹的长度范围可以，例如，从1厘米至1米。
本发明不应该被认为局限于的描述于此的特定实例，而是应该明白其覆盖了本发明的全部方面，正如所附权利要求中所完全地提出的那样。各种修改，同等物工艺，以及本发明可以适用的众多结构对于本领域技术人来说直接参考本说明书就应是显而易见的。
实例
除非另有说明，化学试剂和溶剂是或可以得自Aldrich ChemicalCo.，Milwaukee，WI。
用于本文时，″FM-2″指金-涂覆的聚(对苯二甲酸乙二酯)膜，其得自CPFilms，Canoga Park，CA。
无电的镀铜溶液
将如下试剂混合制备无电的镀铜溶液：去离子水(199.29g)，五水硫酸铜(1.50g)，氢氧化钠(1.35g)，甲醛(1.32g 37wt％的水溶液，得自Mallinckrodt Baker Inc.，Phillipsburg，NJ)，N，N，N′，N′-四(2-羟丙基)乙二胺(2.31g；得自Lancaster Synthesis Inc.，Pelham，NH)，乙二胺四乙酸(1.17g)，以及2，2′-二吡啶(0.03g)。用2.0摩尔每升氢氧化钠水溶液将所得溶液pH值调节至12.3。电镀液在68℃温度下使用。
实施例1
在通过机械划割得到图案的基质上沉积铜
镀金的1英寸(25.4mm)乘1.5英寸(38.1mm)FM-2样品用OMNISCRIBE钻石尖划线针(得自Lunzer，Inc.，Saddle Brook，NJ)划割为矩形栅格图案。膜样品浸没于0.1wt％的1-十八烷硫醇在乙醇中的溶液中2分钟，到时间后用乙醇漂洗。然后膜样品在68℃下浸于无电的镀铜溶液中。30分钟之后，从无电的镀铜溶液中取出膜样品，用去离子水漂洗，并在室温下于空气中干燥。样品的一部分表面示于图4。在图4中，光着色区域是沉积了铜的区域。
然后膜样品在另一溶液中浸没大约15秒时间，所述溶液通过将碘化钾(2g)，然后是碘(1g)溶解于去离子水(40mL)中制备，以通过蚀刻除去在膜上暴露的金涂层。然后用去离子水漂洗膜样品并在室温下于空气中干燥。
实施例2
在通过机械划割得到图案的基质上沉积铜
镀金的1英寸(25.4mm)乘1.5英寸(38.1mm)FM-2样品随机地用CUT-CAT旋转纸张修剪机划割(得自Dahle North America，Inc.，Peterborough，NH)。膜样品浸没于0.1wt％的1-十八烷硫醇在乙醇中的溶液中2分钟，到时间后用乙醇漂洗。然后膜样品在68℃下浸于无电的镀铜溶液中。30分钟之后，从无电的镀铜溶液中取出膜样品，用去离子水漂洗，并在室温下于空气中干燥。样品的一部分表面示于图5。在图5中，光着色区域是沉积了铜的区域。
实施例3
在通过机械划割得到图案的基质上沉积铜
镀金的1英寸(25.4mm)乘1.5英寸(38.1mm)FM-2样品用旋转玻璃刀(得自Fletcher-Terry Co.，Farmington，CT)划割为大致平行的直线图案。膜样品部分浸没于0.1wt％的1-十八烷硫醇在乙醇中的溶液中2分钟，到时间后用乙醇漂洗。然后膜样品在68℃下部分浸于无电的镀铜溶液中。30分钟之后，将膜样品从无电的镀铜溶液中取出，用去离子水漂洗，并在室温下于空气中干燥。样品表面(即，整个表面)示于图6。在图6中，光着色的大致平行的直线是铜沉积的区域。
实施例4
在由压印得到图案的基质上沉积铜
通过在玻璃板上蚀刻图案制备玻璃压印机具。尺寸为12.7cm乘7.6cm乘0.05cm的玻璃板，在其一个表面上用一层3M Polyimide FilmTape 5413(得自3M Company，St.Paul，MN)覆盖，覆盖区域尺寸为约3cm乘4cm。其施用于玻璃板上之后，用剃须刀片切割带以提供大致0.05cm宽的条，条相隔大致0.07cm。0.05厘米宽的条之间的带被除去，留下的玻璃板上具有一系列附着于表面上的大致为0.05cm乘大约4cm的带的条。然后玻璃板浸没在25wt％氢氟酸水溶液之中10分钟。之后玻璃板从酸性溶液中取出并用水漂洗，并在室温下于空气中干燥。除去聚酰亚胺带的条以暴露出未被带的条所覆盖的玻璃板部分，其已被氢氟酸蚀刻并除去。玻璃板的图案为宽大约0.05cm的隆起，其高度约为0.06cm。包括隆起的玻璃表面用Model Somaca BM-106G-RP24砂带抛光机(得自Sommer & Maca Industries，Chicago，IL)，用柔性的M74级钻石带(得自3M Company，St.Paul，MN)轻轻地磨蚀。
玻璃压印机具用于制备压印的聚丙烯酸酯板材，将大约3.8cm乘7.6cm乘0.3cm的OPTIX聚丙烯酸酯板材片(得自Plaskolite，Inc.，Columbus，OH)相对于玻璃板放置，放置时薄片接触玻璃上的隆起图案。玻璃压印机具和聚丙烯酸酯板材一同放置在Model AUTO M层压机(得自Carver，Inc.，Wabash，IN)的加热压板之间，于130℃保持30分钟。然后，利用压力，玻璃压印机具被压入聚丙烯酸酯板材中，压制在3560牛顿的压力下在130℃温度下持续20分钟。之后玻璃/板材组件从压机中取出而压印片材冷却到室温，聚丙烯酸酯板材的压印侧(即，该侧压在玻璃压印机具上)利用热蒸发器(得自Kurt J.Lesker Co.，Pittsburgh，PA)依次涂敷50埃钛然后600埃金。
镀了金属的压印聚丙烯酸酯板材浸没于0.1wt％的1-十八烷硫醇在乙醇中的溶液中2分钟，到时间后用乙醇漂洗。然后膜样品在68℃下浸于化学的镀铜溶液中。30分钟之后，将膜样品从无电的镀铜溶液中取出，用去离子水漂洗，并在室温下于空气中干燥。样品的一部分表面示于图7。在图7中，光着色区域是沉积了铜的区域。
Claims (10)
1.一种制备具有微结构表面的制品的方法，所述微结构表面带有金属性沉积物，该方法包括：
提供具有金属性微结构表面的基质，在该基质上，所述微结构的特征为故意形成的形貌特征，该形貌特征的形式为规则的、重复的几何排列，该几何排列选自一系列多角形或金属痕迹，或无规排列，该无规排列选自无规的痕迹的网络，或者没有对称性或重复几何元素的形状的图案，在所述微结构中从所述基质表面伸出的有用的形貌特征具有1nm-100μm的高度；
在金属性微结构表面上形成自组装单层；
将自组装单层暴露至含有可溶形式的沉积金属的无电镀溶液中；和
将沉积金属选择性地无电沉积在金属性微结构表面上。
2.根据权利要求1的方法，另外包括在提供步骤之前用机械机具，在基质金属性表面上形成微结构，以形成金属性微结构表面。
3.根据权利要求1的方法，另外包括在提供步骤之前，用机械机具，在基质表面上形成微结构，以形成基质微结构表面，并在该基质微结构表面上布置金属层以形成金属性微结构表面。
4.根据权利要求1的方法，另外包括在提供步骤之前通过将金属沉积到基质表面上形成微结构以形成金属性微结构表面。
5.根据权利要求1的方法，另外包括在提供步骤之前通过将金属从基质表面上除去形成微结构以形成金属性微结构表面。
6.根据权利要求1的方法，其中所述提供具有金属性微结构表面的基质的步骤包括提供基质，所述基质含有聚合物材料并具有布置在基质上的金属性微结构表面。
7.根据权利要求1的方法，其中所述提供具有金属性微结构表面的基质的步骤包括提供基质，所述基质包括玻璃、陶瓷、玻璃-陶瓷、或半导体，并具有布置在基质上的金属性微结构表面。
8.根据权利要求1的方法，其中提供具有金属性微结构表面的基质的步骤包括提供具有金属性微结构表面的基质，所述金属性微结构表面包括形貌特征，该形貌特征的曲率半径小于0.5微米。
9.一种具有基质的制品，所述基质具有图案化的金属沉积物，该制品包括：
基质，其具有表面以及布置在基质表面上的形貌特征，在所述基质上从该基质表面伸出的有用的形貌特征具有的高度的范围为1nm至100μm；
连续均匀金属层，其布置在邻近形貌特征的基质表面上和形貌特征上；
自组装单层，其布置在连续均匀金属层上；和
沉积金属，其布置在形貌特征上的连续均匀金属层上，而未布置在邻近形貌特征的连续均匀金属层基质表面上，所述沉积金属的特征在于：选自如下形式的区域形状：规则的、重复的几何排列，该几何排列选自一系列多角形或金属痕迹，其定义了未沉积区域的规则的、重复的几何形状的边界，或者无规排列，该无规排列选自无规的金属痕迹的网络，其定义了不规则的形状的未沉积区域的边界，或者没有对称性或重复几何元素的形状的排列，和沉积金属的线性痕迹的宽度范围为1nm-1mm。
10.如权利要求9中所述的具有基质的制品，所述基质具有图案化的金属沉积物，其中所述形貌特征具有的曲率半径为500纳米或更小。
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Also Published As
| Publication number | Publication date |
|---|---|
| ATE397680T1 (de) | 2008-06-15 |
| WO2006062575A3 (en) | 2007-09-13 |
| US7682703B2 (en) | 2010-03-23 |
| US20060121271A1 (en) | 2006-06-08 |
| EP1825021A2 (en) | 2007-08-29 |
| US7160583B2 (en) | 2007-01-09 |
| US20070098996A1 (en) | 2007-05-03 |
| CN101094936A (zh) | 2007-12-26 |
| WO2006062575A2 (en) | 2006-06-15 |
| DE602005007379D1 (de) | 2008-07-17 |
| JP2008522038A (ja) | 2008-06-26 |
| JP4662994B2 (ja) | 2011-03-30 |
| EP1825021B1 (en) | 2008-06-04 |
| KR20070085612A (ko) | 2007-08-27 |
| KR101298808B1 (ko) | 2013-08-22 |
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