CN102695817A - 通过气相沉积的多层生长 - Google Patents

通过气相沉积的多层生长 Download PDF

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CN102695817A
CN102695817A CN2010800609787A CN201080060978A CN102695817A CN 102695817 A CN102695817 A CN 102695817A CN 2010800609787 A CN2010800609787 A CN 2010800609787A CN 201080060978 A CN201080060978 A CN 201080060978A CN 102695817 A CN102695817 A CN 102695817A
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M·R·林福德
D·S·詹森
F·张
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Brigham Young University
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Abstract

一种多层系统，其中中间充分键合并交联的层为具有期望的反应部位的终饰层提供附连。

Description

通过气相沉积的多层生长
相关申请的交叉引用
要求于2009年11月10日提交的美国临时专利申请号61/280,866的优先权，其通过引用并入。
背景技术
涂布在多种应用中使用的基底以提供期望的表面性质。对于施加这种涂层的方法存在持续的需要，该涂层提供强键合涂层和改造表面的反应性或非反应性的能力。现有的涂层比如用于色谱法的那些中可发生问题为涂层和基底之间的键合失效。这些涂层系统中的许多使用强共价键和离子键，但在使用的条件下，即便少量的键合可能失效，也会导致涂层中出现暴露基底表面的缝隙。如果未键合的涂层化学品在该系统中具有任何溶解性，则这种情况可能加剧。该未覆盖的基底缝隙可能对该系统引入反应性，其潜在地危害或妨碍涂层的功能。
发明内容
该发明的一个方面是在可用于色谱法和其它应用的基底上的涂层。该涂层用强离子键或共价键附连到基底。然而，该涂层系统也是高度交联的。因此，如果键失效，由于相邻的键将其保持在原位使得涂层得以保持。即便在数个键失效的情况下，基本上为非常大的交联分子的涂层由于其尺寸而非常不溶。结果是在广泛的操作条件下非常耐失效的涂层。
另一方面为通过施加多层或通过选择特定的涂层化学品，改造涂层厚度的能力。最末层或活性层可以通过最终施加具有期望活性的终饰层(finishing layer)来容易地确定。
一方面是在具有活性化学部位或可以被改性以包含活性化学部位的基底上制造均匀多层的方法。气相沉积被用作在各种不同的基底上沉积多层的主要工具。在一个方面，该方法如下：
（1）将化学品A气相沉积在基底上。
（2）沉积可以与化学品A反应的另一个化学品——化学品B——以增加另一层。
（3）沉积化学品C通过与沉积的化学品B上的反应部位反应以提供终饰层，或形成具有期望活性的最终表面。根据选择的化学性质，化学品C可以用于形成中间层，其随后用于通过与形成终饰层的化学品D反应而沉积。
步骤（1）和（2）可以在C沉积之前进行一次或者如果期望较厚的层步骤（1）和（2）可以在C沉积之前进行重复。化学品A、B、C和D是可蒸发的，在反应的情况下以气相的形式。选择沉积条件和化学品以提供气相中合适的沉积反应。
对于步骤（1），基底可以是硅、玻璃、金属、陶瓷、二氧化硅、铝、钛、氧化锆或可以被活化以与化学品A键合的任何其它材料。化学品A可以包括可选自下述的任何合适的化学品中的一种或混合物：具有活性基（例如，胺、琥珀酸酐、戊二酸酐(gluteric anhydride)、环氧、异氰酸根、醇、硫代异氰酸根(thioisocynates)等等）的硅烷，或其它具有多胺或多异氰酸根或如前所述的其它反应性基团组合的双官能、三官能或四官能分子。化学品A还可以包括含单官能或双官能异氰酸根(isocynate)或胺的分子。合适的化学品A是具有至少两个官能团的胺、环氧化物或异氰酸酯。这允许在沉积层中交联，同时也提供用于键合化学品B的未反应基团。
对于步骤（2），化学品B可以是任何可蒸发的化学品，其包括可以与分子A反应从而借助共价键或静电键将两个分子拴在一起的官能团。化学品B应当为在合理温度下可以与A反应的分子。
对于步骤（3），C和/或D必须包括可与A或B反应的反应性杂原子或部分。每个都可以是单官能分子或双官能分子，其可以与来自A和/或B的可获得官能团反应。化学品C可以与化学品A相同或不同，并可以提供终饰表面或功能为化学品D沉积的中间键合层。
随着施加层，气相化学品将与之前施加的层反应。例如，B将与A反应，C将与B反应，但是也可以与A的剩余活性部位反应。此外，化学品A、B、C中的气相沉积的化学品在沉积期间将相互反应，从而产生交联系统。可获得的活性部位将保持不反应，以提供用于与随后施加的层反应的活性部位。在最终产品中，基底和施加的化学品的反应产物为以共价键合或离子键合并且在层内和层间高度交联的多层形式。
用于施加化学品A、B、C和D的方法是通过气相化学沉积或化学气相沉积。这类方法是众所周知的。选择准确的操作条件和精选的化学品，其中化学品以气相的形式且稳定，并且可以可靠地与基底接触用于在沉积时与基底反应。
多层生长对于半导体制造、生物吸附和色谱法，以及新材料开发可以是重要的。
分子的类型和实例
可以作为A、B或C发挥功能的示例性分子，包括
Figure BDA00001865407200031
其中R可以代表：异氰酸根、醇、胺、硫代异氰酸根、酰基氯、酮、醛、氢、带电种类，比如磺酸根（-SO3）、磷酸根（-PO4）、碳酸根（-CO2）。
合适的化学品也包括选自三胺、双胺、四胺(tetraamine)、二异氰酸酯、三异氰酸酯、双环氧化合物、三环氧化合物、二酰氯、三酰氯(triacidchloride)的任何合适的。具体的化合物是二亚乙基三胺和三(2-氨基乙基)胺。为了促进在层中的交联，至少一部分化学品A或化学品B是具有多于两个可以参与交联反应以及A与B反应的官能团的化合物。
最末层是终饰层，化学品C或D可与下面的层反应并且也包含提供期望的最末层反应性的基团，可以是任何合适的这类基团。也可以选择终饰层化学品不提供反应性。实例包括具有烷基链的一元胺、环氧化物或异氰酸酯（用于与下面的层反应），并可以包括反应性硫醇基。对于色谱法，其可以包括烷基链。对于离子色谱法或其它类型的色谱法，其可以包含胺基、磺酸基或硝基。
本发明提供了优于先前分层系统的下述优势。
+最终活性部位通过经过层的共价键或离子键与基底键合，所述层不但被牢固地键合而且被交联，以提供稳定和牢靠的附连。
+层可以构建成任何期望的厚度，允许构建成用于如微芯片制造这类应用的相对厚的层，或用于如色谱法这类应用的薄层。例如，较厚的层可以用于小分子分离。较薄的层将用于高分子例如蛋白质、生物分子的色谱分离。较薄的层提供高分子的适度保留。
附图简述
图1显示了在基底上施加层作为多层系统形成中的初始步骤。
图2显示了在基底上施加层作为多层系统形成中的初始步骤。
图3A和3B显示了多层系统形成的反应步骤。
图4A、4B和4C显示了多层系统形成的反应步骤。
图5A、5B和5C显示了多层系统形成的反应步骤。
图6阐明了获得期望厚度的多层系统的重复反应步骤。
图7为显示多层系统厚度对层数的图。
图8为显示多层系统厚度对层数的图。
具体实施方式
示例性的应用
半导体
表面官能化可以在半导体行业中使用。这里介绍的系统可以用以允许精确布置某些类型的金属或金属离子，所述金属或金属离子可以与存在于表面上的杂原子反应，例如，在终饰层中使用的双官能分子可以具有可与金属或金属离子反应或相互作用的化学部分。用于终饰层的化学品在一端包括反应性基团即氨基或异氰酸根，以与由化学品A或B形成的下面的层反应。另一端官能团为例如硫醇，以提供用于金属或金属离子反应的活性。
反应性氨基或异氰酸根可以与表层硅烷醇（化学品A）或可以与已经官能化表面上的杂原子（在来自化学品C或化学品的下层上）反应。游离硫醇基随后可以进一步与金、银、铜或其它类型的贵金属纳米点(nanodots)反应；从而允许放置纳米点材料。
色谱法
多层系统可以施加于色谱法以提供将供给不同化学选择性的官能化表面。该方法将提供高度交联的固定相。色谱法的典型基底为：二氧化硅、氧化铝、氧化锆和二氧化钛。提到的基底包含可以与胺或可以与异氰酸酯反应的表面部分(通常是OH基团)，如实施例1和2所示。
实施例1
在图1中显示了施加化学品A以开始施加多层系统的实施例。具有-OH反应部位的基底与异氰酸酯反应。
R可以是碳链，其中n为1到30，R是用于阳离子/阴离子色谱法的带电种类，或异氰酸根或硫代异氰酸根。
实施例2
在图2中显示施加化学品A形成多层系统的另一个实施例，其中化学品A为三胺。由于表面醇为酸性的，其可以与三胺形成离子键。此外，游离胺——-NH2官能团——可以与化学品比如具有异氰酸根基团的那些反应，以制造键合且交联的层。
实施例3
如在实施例2中的氨基末端的单层可以与化学品B——异氰酸酯反应，以产生将在酸性条件下稳定的交联材料。施加单层并反应，如图3A所示。AB多层随后与三胺（与化学品A相同）反应，其随后与具有末端反应基的化学品C反应，如图3B所示。
该多层系统可以表征为ABCD，其中C=A，其中A=三胺，B=二异氰酸酯，D=具有2-30个碳单位长度的烷基链的单异氰酸酯或单环氧化物。该方法产生高度交联的固定相，其可以归因于二异氰酸酯或三胺。此外，可以类似地施加A和B层以形成AB)nCD或(AB)nC多层系统，其中n为2以上。
实施例4
如在实施例2中的氨基末端的单层可以与化学品B——双环氧化物反应，以产生将在酸性条件下稳定的交联材料，如图4A所示。这可以进一步如图4B所示与三胺反应，其又如图4C所示与单环氧化物反应。
所得的多层系统可以表征为ABCD，其中A=三胺，B=双环氧化物，C=A，D=具有2-30个碳单位长度的烷基链的单环氧化物。该方法产生高度交联的固定相，其可以归因于双环氧化物或三胺。
实施例5
如在实施例1中的异氰酸根末端的单层可以与化学品B——一种胺——反应以产生将在酸性条件下稳定的交联材料，如图5A、图5B和图5C所示。
异氰酸根末端的单层与化学品B——一种胺——反应以形成交联的胺末端的层，其又如图5B所示与异氰酸酯反应（与化学品A相同），其又如图5C所示与化学品C——一种一元胺——反应。
该多层系统可以表征为ABCD，其中A=二异氰酸酯，B=三胺，C=A，D=具有2-30个碳单位长度的烷基链的一元胺。该方法产生高度交联的固定相，其可以归因于二异氰酸酯或三胺。
实施例6
这个实施例显示了可以如何重复施加层A和B以形成期望厚度的多层。将多层涂层施加到硅基底。参照图6，硅基底用氧等离子体处理或活化，以产生具有-OH自由基的表面。
第一个循环通过-OH自由基与化学品A——二异氰酸酯（六亚甲基-1,6-二异氰酸酯）——反应进行。二异氰酸酯表面随后与化学品B——三胺（二亚乙基三胺）——反应。两个涂层都使用常规的气相涂布技术来完成。
在第一个循环后，使用与第一个循环基本相同的反应物和条件，使用相同的化学品A和化学品B，进行第二个循环。
进一步的循环以相同的方式进行。在选择的循环后，使用椭圆偏振光谱法（spectroscopic ellipsometry）测量厚度。图7是显示对上至6层的厚度测量的结果的图。该最后的多层系统可以表征为ABABABABABAB。每个层数包括二异氰酸酯和三胺沉积物。
如果化学品B提供期望的反应性，其可以为最末层。但是如上，最末层可以是化学品D以提供期望的反应性。
实施例7
除了化学品A为三胺、化学品B为二异氰酸酯之外，基本上如实施例6，制造多层系统。重复循环。图8显示了来自二亚乙基三胺和六亚甲基-1,6-二异氰酸酯层生长所得到的多层系统的厚度测量值。三胺首先沉积，随后二异氰酸酯沉积。重复该循环直至获得合适的厚度。每个层数包括二异氰酸酯和三胺沉积物。

Claims (20)

1.将涂层施加到基底的方法，所述方法包括：
(a)通过所述基底上的活性部位与来自气相的化学品A反应，涂布所述基底；
(b)通过与来自气相的化学品B反应涂布与化学品A反应的所述基底；
化学品A具有官能团，其用于与所述基底上的所述活性部位反应，并且用于交联反应和用于与化学品B反应，以形成附连到所述基底的交联层，至少一部分的化学品A和化学品B的任一个或两者包括具有至少三个官能团的化合物，所述官能团参与交联以及化学品A与化学品B的反应；
(c)通过所述交联层与来自气相的化学品C反应，用终饰层涂布所述基底；
其中化学品C是与所述交联层中的官能团反应的。
2.权利要求1所述的方法，还包括(d)用来自气相的化学品D涂布所述基底；其中化学品D具有与来自化学品C的层中的官能团反应的官能团，并且其中化学品D具有对所述表面赋予选择的反应性的结构。
3.权利要求1所述的方法，还包括在步骤(b)之后(a1)使所述表面与来自气相的化学品A反应，和(b1)使所述表面与化学品B反应，其中(a1)和(b1)在步骤(c)之前进行一次或多次。
4.权利要求1所述的方法，其中化学品C与化学品A相同。
5.权利要求1所述的方法，其中化学品A和化学品B不同，并且是三胺、双胺、四胺、二异氰酸酯、三异氰酸酯、双环氧化物、三环氧化物、二酰氯、三酰氯中的一种或混合物。
6.权利要求1所述的方法，其中化学品A和化学品B不同，并且包括环氧化物官能团、异氰酸根官能团或氨基官能团。
7.权利要求1所述的方法，其中化学品A或化学品B包括二亚乙基三胺或三(2-氨基乙基)胺。
8.权利要求1所述的方法，其中化学品A或化学品C包括选自异氰酸根、醇、胺、硫代异氰酸根、酰基氯、酮、醛、氢、磺酸根、磷酸根和碳酸根的官能团。
9.权利要求1所述的方法，其中所述基底被活化以提供所述活性部位。
10.权利要求1所述的方法，其中化学品A包括三胺，化学品B包括多官能环氧化物或异氰酸酯。
11.权利要求1所述的方法，其中化学品C提供具有适合于色谱分离应用的化学选择性的最终官能化表面。
12.权利要求2所述的方法，其中化学品D提供具有适合于色谱分离应用的化学选择性的最终官能化表面。
13.权利要求1所述的方法，其中化学品C包括选自胺、环氧化物或异氰酸根的官能团。
14.权利要求1所述的方法，其中化学品C包括选自烷基链、反应性硫醇基、胺基、磺酸基或硝基的一种或多种基团。
15.权利要求2所述的方法，其中化学品D包括选自烷基链、反应性硫醇基、胺基、磺酸基或硝基的一种或多种基团。
16.一种分层制品，包括基底；和为化学品A和化学品B反应产物的化学键合层，其中化学品A和B是不同的且分别气相沉积的，所述键合层具有所述层中的交联，和化学品A和化学品B之间的键合；以及气相沉积在化学品A和B交联且键合的层上的化学品C。
17.权利要求16所述的制品，还包括由化学品C提供的具有化学选择性的官能化表面。
18.权利要求17所述的制品，其中化学品A和化学品B具有选自胺、环氧化物和异氰酸根的不同的官能团。
19.权利要求16所述的制品，还包括由与化学品A、B和C的反应产物反应的化学品D提供的具有化学选择性的官能化表面。
20.权利要求16所述的制品，其中化学品A和化学品C相同。
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