Buried Microphase Separation by Dynamic Interplay of Crystallization and Microphase Separation in Semicrystalline PEO-Rich PS-b-PEO Block Copolymer Thin Films,Macromolecules

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Buried Microphase Separation by Dynamic Interplay of Crystallization and Microphase Separation in Semicrystalline PEO-Rich PS-b-PEO Block Copolymer Thin Films
Macromolecules ( IF 5.1 ) Pub Date : 2020-06-24 , DOI: 10.1021/acs.macromol.9b02760
Tobias Rejek ₁ , Peter Schweizer ₂ , Daniel Joch ₁ , Luis Portilla ₁ , Erdmann Spiecker ₂ , Marcus Halik ₁

Affiliation

The interplay between microphase separation and crystallization in the semicrystalline PS-b-PEO system is investigated in the context of solution-based thin film formation. For this end, the film morphology is studied depending on the PEO volume fraction in a broad f_vol^PEO range from 0.17 to 0.8. Topographical two-dimensional AFM measurements are extended to the third dimension to gain information about the vertical film structure by successive removal of the surface layer by controlled O₂ plasma etching. The depth profiling reveals a dynamic film formation process where competing microphase separation and crystallization forces create a two-layered BCP film composed of a buried microphase-separated layer featuring cylinder morphology under a fine-structured crystalline lamellae surface layer. An explanation is presented considering the thermal properties and solvent interactions. Phase-selective TiO₂ nanoparticles addressing the PEO block are further used to demonstrate the accessibility of the buried microphase-separated layer and thus that we were able to extend the usable range of the phase diagram of PS-b-PEO thin films to the PEO-rich regime. Lastly, the impact of a second film–air interface is shown, which is formed in free-standing BCP membranes.

中文翻译：

半结晶PEO-富PS- b -PEO嵌段共聚物薄膜中结晶和微分离的动态相互作用的埋藏式微分离

在溶液基薄膜形成的背景下，研究了半结晶PS- b - PEO系统中微相分离与结晶之间的相互作用。为此目的，膜形态取决于在宽的PEO体积分数研究˚F_体积^PEO范围从0.17至0.8。二维二维AFM地形测量扩展到第三维，以通过受控O ₂连续去除表面层来获得有关垂直膜结构的信息等离子蚀刻。深度剖析揭示了动态的膜形成过程，其中竞争的微相分离和结晶力产生了两层BCP膜，该BCP膜由掩埋的微相分离层组成，其特征是在精细结构的晶体薄层表面层下具有圆柱体形态。给出了考虑热性质和溶剂相互作用的解释。针对PEO嵌段的相选择TiO ₂纳米粒子进一步用于证明掩埋微相分离层的可及性，因此我们能够将PS- b -PEO薄膜的相图的适用范围扩展到PEO丰富的政权。最后，显示了第二个膜-空气界面的冲击，该界面在独立的BCP膜中形成。

更新日期：2020-07-14

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