Transition Metal β-Diketonate Adhesion Promoters in Epoxy-Anhydride Resin,Macromolecular Rapid Communications

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Transition Metal β-Diketonate Adhesion Promoters in Epoxy-Anhydride Resin
Macromolecular Rapid Communications ( IF 4.2 ) Pub Date : 2023-03-25 , DOI: 10.1002/marc.202200973
Jiaxiong Li ₁ , Dylan Cheung ₁ , John Wilson ₁ , Zhijian Sun ₁ , Frank Yu ₁ , Doyoub Kim ₁ , Mohanalingam Kathaperumal ₂ , Kyoung-Sik Moon ₁ , Chingping Wong ₁

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Epoxy to copper adhesion supports the reliability of numerous structures in electronic packaging. Compared to substrate pre-treatment, processing and cost considerations are in favor of adhesion promoters loaded in epoxy formulations. In this work, first row transition metal β-diketonates present such a compelling case when added in epoxy/anhydride resins: over 30% (before moisture aging) and 50% (after moisture aging) enhancement in lap shear strength are found using Co(II) and Ni(II) hexafluoroacetylacetonate. From extensive X-ray photoelectron spectroscopy (XPS) analyses on the adhesively failed sample surfaces, increased population of oxygen-containing functional groups, especially esters, is linked to the adhesion improvement. Assisted by XPS depth profile on the fractured epoxy side and in situ Fourier-transform infrared spectroscopy (FTIR), the previously discovered latent cure characteristics endowed by the metal chelates interacting with phosphine catalysts are regarded pivotal for pacing the anhydride consumption and allowing interfacial esterification reactions to occur. Further examinations on the XPS binding energy shifts and dielectric properties of the doped epoxy also reveal metal–polymer coordination that contribute to the adhesion and moisture resistance properties. These findings should stimulate future research of functional additives targeting at cure kinetics control and polar group coordination ideas for more robust epoxy–Cu joints.

中文翻译：

环氧树脂中过渡金属β-二酮酸盐助粘剂

环氧树脂与铜的粘合力支持电子封装中众多结构的可靠性。与基材预处理相比，加工和成本方面的考虑有利于在环氧配方中加入附着力促进剂。在这项工作中，第一行过渡金属β当添加到环氧树脂/酸酐树脂中时，-二酮酸盐呈现出如此引人注目的情况：使用六氟乙酰丙酮钴 (II) 和镍 (II) 发现搭接剪切强度提高超过 30%（湿气老化前）和 50%（湿气老化后）。通过对粘合失败的样品表面进行广泛的 X 射线光电子能谱 (XPS) 分析，含氧官能团（尤其是酯类）的数量增加与粘合力的改善有关。借助断裂环氧树脂侧的 XPS 深度剖面和原位傅立叶变换红外光谱 (FTIR)，先前发现的金属螯合物与膦催化剂相互作用所赋予的潜在固化特性被认为是调节酸酐消耗和允许界面酯化反应的关键发生。对掺杂环氧树脂的 XPS 结合能变化和介电性能的进一步检查也揭示了有助于粘附和防潮性能的金属-聚合物配位。这些发现应该会激发未来针对固化动力学控制和极性基团配位思想的功能性添加剂的研究，以获得更坚固的环氧铜接头。

更新日期：2023-03-25

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