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Sub‐Micrometer Structure Formation during Spin Coating Revealed by Time‐Resolved In Situ Laser and X‐Ray Scattering
Advanced Functional Materials ( IF 18.5 ) Pub Date : 2017-09-12 , DOI: 10.1002/adfm.201702516 Jacobus J. van Franeker 1, 2 , Daniel Hermida-Merino 3 , Cedric Gommes 4 , Kirill Arapov 5 , Jasper J. Michels 6 , René A. J. Janssen 1, 7 , Giuseppe Portale 8
Advanced Functional Materials ( IF 18.5 ) Pub Date : 2017-09-12 , DOI: 10.1002/adfm.201702516 Jacobus J. van Franeker 1, 2 , Daniel Hermida-Merino 3 , Cedric Gommes 4 , Kirill Arapov 5 , Jasper J. Michels 6 , René A. J. Janssen 1, 7 , Giuseppe Portale 8
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Solution‐processed thin polymer films have many applications, such as organic electronics and block‐copolymer nanofabrication. These films are often made by spin coating a solution that contains one or more solids and can show different phase‐separated structures. The formation mechanism of the droplet‐like morphology is studied here by processing polystyrene (PS) and a fullerene derivative ([6,6]‐phenyl‐C71‐butyric acid methyl ester, [70]PCBM) from o‐xylene. The final structure consists of [70]PCBM droplets partially embedded in a PS‐rich matrix showing interdomain distance of 100–1000 nm as determined from transmission electron microscopy and grazing incidence small angle X‐ray scattering (GISAXS). To elucidate the formation of these morphologies in real time, ultrafast in situ GISAXS coupled with laser interferometry and laser scattering is performed during spin coating. In situ thickness measurements and laser scattering show that liquid–liquid phase separation occurs at ≈70 vol% solvent. Subsequently, in only 100–400 ms, almost dry [70]PCBM domains start to protrude from the swollen PS‐rich matrix. These results are used to verify the ternary phase diagram calculated using Flory–Huggins theory. The discussed multitechnique approach can be applied to study fundamental aspects in soft matter such as phase separation in thin films occurring at very short time scales.
中文翻译：
时间分辨原位激光和X射线散射揭示了旋涂过程中亚微米结构的形成
溶液处理的聚合物薄膜具有许多应用，例如有机电子学和嵌段共聚物纳米制造。这些薄膜通常是通过旋涂包含一种或多种固体并显示出不同相分离结构的溶液来制成的。液滴状形态的形成机理是通过处理聚苯乙烯（PS）和富勒烯衍生物这里研究（[6,6] -苯基-C 71 -丁酸甲酯，[70] PCBM）从ø二甲苯。最终结构由[70] PCBM小滴组成，这些小滴部分地嵌入富含PS的基质中，根据透射电子显微镜和掠入射小角X射线散射（GISAXS）确定，其畴间距离为100-1000 nm。为了实时阐明这些形态的形成，在旋涂过程中执行了结合激光干涉测量法和激光散射的超快原位GISAXS。原位厚度测量和激光散射表明，液相-液相分离发生在≈70vol％的溶剂下。随后，仅在100-400毫秒内，几乎干燥的[70] PCBM域开始从溶胀的富含PS的基质中突出。这些结果用于验证使用Flory-Huggins理论计算的三元相图。
更新日期：2017-09-12
中文翻译：
时间分辨原位激光和X射线散射揭示了旋涂过程中亚微米结构的形成
溶液处理的聚合物薄膜具有许多应用，例如有机电子学和嵌段共聚物纳米制造。这些薄膜通常是通过旋涂包含一种或多种固体并显示出不同相分离结构的溶液来制成的。液滴状形态的形成机理是通过处理聚苯乙烯（PS）和富勒烯衍生物这里研究（[6,6] -苯基-C 71 -丁酸甲酯，[70] PCBM）从ø二甲苯。最终结构由[70] PCBM小滴组成，这些小滴部分地嵌入富含PS的基质中，根据透射电子显微镜和掠入射小角X射线散射（GISAXS）确定，其畴间距离为100-1000 nm。为了实时阐明这些形态的形成，在旋涂过程中执行了结合激光干涉测量法和激光散射的超快原位GISAXS。原位厚度测量和激光散射表明，液相-液相分离发生在≈70vol％的溶剂下。随后，仅在100-400毫秒内，几乎干燥的[70] PCBM域开始从溶胀的富含PS的基质中突出。这些结果用于验证使用Flory-Huggins理论计算的三元相图。
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