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首页> 外文会议>Second International Symposium on Polyimides and Other High Temperature Polymers: Synthesis, Characterization and Applications Dec 3-6, 2001 Newark, New Jersey >New developments in the adhesion promotion of electroless Ni or Cu films to polyimide substrates
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New developments in the adhesion promotion of electroless Ni or Cu films to polyimide substrates

机译：化学镀镍或铜膜与聚酰亚胺基材的粘合促进作用的新进展

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Electroless metallization (or electroless plating) of polymers and composite materials is a multi-step chemical process requiring: (ⅰ) the pre-conditioning of the sample surface to render it chemically reactive, (ⅱ) the activation of the so-modified surface through the adsorption of a palladium-based catalyst, and (ⅲ) the metallization operation itself. In the present work, electroless plating was carried out on polyimide substrates and step (ⅰ) was performed via plasma or VUV irradiation-assisted treatments operating especially in nitrogenated atmospheres (NH_3 or N_2). In addition, step (ⅱ) was accomplished using two different routes. The one is based on the chemisorption of Pd~(+2) species (from a PdCl_2 solution) on surfaces which are previously grafted with nitrogenated functionalities. The other involves deposition (e.g. by spin-coating) of a palladium acetate (Pdac) thin film on the same substrates functionalized in the same way. In both cases, the so-grafted Pd~(+2) species have to be subjected to a reduction to Pd~0 before becoming catalytically active towards the metallization initiation. In laboratory-made Ni plating baths in which there are no stabilizers this occurs through the reducing agent (sodium hypophosphite NaH_2PO_2). On the other hand, in laboratory-made Cu plating baths, such a reduction by formaldehyde (HCHO), although thermodynamically possible, does not take place because of a too slow kinetics. Note that a similar behavior is observed with both commercial Ni or Cu plating baths due to the presence of stabilizers which probably mask the potential catalytic sites when the Pd~(+2)-grafted surfaces are dipped in these baths, and therefore prevent Pd~(+2) species from being reduced. Under these conditions, the reduction of the Pd~(+2) species has to be performed prior to the surface immersion in the Ni or Cu plating baths. For this, one simple method consists in dipping the Pd~(+2)-grafted surfaces in a hypophosphite solution. Another route consists in subjecting the same samples to a VUV irradiation under vacuum. However, the experiments show that the kinetics of the Pd~(+2) reduction to Pd~0 is clearly more favorable in the first case and under the experimental conditions used. In short, the work described in this paper has been successful in leading to a better understanding of the chemisorption mechanisms of the palladium-based catalysts on functionalized surfaces and of their role in initiating the electroless deposition, as well as in allowing the development of new approaches for electrolessly metallizing polymer-based materials. Finally, this work has shown that electrical measurements carried out in conjunction with a fragmentation test appear to be able to distinguish the effects of different surface treatments of polymer substrates on the practical adhesion of the metal film on the polymer surface.
机译：聚合物和复合材料的化学镀（或化学镀）是一个多步骤的化学过程，需要：（ⅰ）预处理样品表面以使其具有化学反应性；（through）如此改性的表面通过钯基催化剂的吸附，以及（ⅲ）金属化操作本身。在本工作中，化学镀是在聚酰亚胺衬底上进行的，步骤（ⅰ）是通过等离子或VUV辐照辅助处理（特别是在氮化气氛（NH_3或N_2）中进行）进行的。另外，步骤（different）使用两种不同的途径完成。一种是基于Pd〜（+2）物种（从PdCl_2溶液中）在预先接有氮化功能的表面上的化学吸附。另一个涉及在以相同方式功能化的相同基板上沉积（例如，通过旋涂）乙酸钯（Pdac）薄膜。在这两种情况下，都必须对接枝的Pd〜（+2）物种还原成Pd〜0，然后才对金属化反应起催化作用。在没有稳定剂的实验室制镍电镀液中，这是通过还原剂（次磷酸钠NaH_2PO_2）发生的。另一方面，在实验室制造的铜镀浴中，尽管甲醛在热力学上是可行的，但由于动力学太慢，因此不会发生甲醛（HCHO）的还原反应。请注意，由于存在稳定剂，当将Pd〜（+2）接枝的表面浸入这些镀液中时，它们可能掩盖了潜在的催化部位，因此在商用的Ni或Cu镀液中均观察到了类似的行为。 （+2）种被减少。在这些条件下，必须先将Pd〜（+2）物种还原，然后再将其浸入Ni或Cu镀液中。为此，一种简单的方法是将Pd〜（+2）接枝表面浸入次磷酸盐溶液中。另一种途径是在真空下对相同样品进行VUV照射。然而，实验表明，在第一种情况下和所使用的实验条件下，Pd〜（+2）还原为Pd〜0的动力学明显更有利。简而言之，本文所描述的工作已成功地导致人们更好地理解了钯基催化剂在功能化表面上的化学吸附机理以及它们在引发化学沉积中的作用，以及允许开发新的化学镀聚合物基材料的方法。最后，这项工作表明，结合碎裂测试进行的电学测量似乎能够区分聚合物基材的不同表面处理对金属膜在聚合物表面上实际附着力的影响。

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