Wagner Alexandra, Wagner Stefanie, Bredfeldt Jan-Erik, Steinbach Julia C, Mukherjee Ashutosh, Kronenberger Sandra, Braun Kai, Kandelbauer Andreas, Mayer Hermann A, Brecht Marc
Process Analysis and Technology (PA&T), Reutlingen Research Institute, Reutlingen University, Alteburgstrasse 150, 72762 Reutlingen, Germany.
Institute of Inorganic Chemistry, University of Tübingen, Auf der Morgenstelle 18, 72076 Tübingen, Germany.
Polymers (Basel). 2021 Apr 29;13(9):1438. doi: 10.3390/polym13091438.
Monodisperse polystyrene spheres are functional materials with interesting properties, such as high cohesion strength, strong adsorptivity, and surface reactivity. They have shown a high application value in biomedicine, information engineering, chromatographic fillers, supercapacitor electrode materials, and other fields. To fully understand and tailor particle synthesis, the methods for characterization of their complex 3D morphological features need to be further explored. Here we present a chemical imaging study based on three-dimensional confocal Raman microscopy (3D-CRM), scanning electron microscopy (SEM), focused ion beam (FIB), diffuse reflectance infrared Fourier transform (DRIFT), and nuclear magnetic resonance (NMR) spectroscopy for individual porous swollen polystyrene/poly (glycidyl methacrylate-co-ethylene di-methacrylate) particles. Polystyrene particles were synthesized with different co-existing chemical entities, which could be identified and assigned to distinct regions of the same particle. The porosity was studied by a combination of SEM and FIB. Images of milled particles indicated a comparable porosity on the surface and in the bulk. The combination of standard analytical techniques such as DRIFT and NMR spectroscopies yielded new insights into the inner structure and chemical composition of these particles. This knowledge supports the further development of particle synthesis and the design of new strategies to prepare particles with complex hierarchical architectures.
单分散聚苯乙烯微球是具有有趣特性的功能材料，如高内聚强度、强吸附性和表面反应性。它们在生物医学、信息工程、色谱填料、超级电容器电极材料等领域显示出很高的应用价值。为了全面理解和定制颗粒合成，需要进一步探索表征其复杂三维形态特征的方法。在此，我们展示了一项基于三维共聚焦拉曼显微镜（3D-CRM）、扫描电子显微镜（SEM）、聚焦离子束（FIB）、漫反射红外傅里叶变换（DRIFT）和核磁共振（NMR）光谱的化学成像研究，用于单个多孔溶胀聚苯乙烯/聚（甲基丙烯酸缩水甘油酯 - 二甲基丙烯酸乙二酯）颗粒。合成了具有不同共存化学实体的聚苯乙烯颗粒，这些化学实体可以被识别并分配到同一颗粒的不同区域。通过SEM和FIB的组合研究了孔隙率。研磨颗粒的图像表明表面和内部的孔隙率相当。DRIFT和NMR光谱等标准分析技术的结合为这些颗粒的内部结构和化学成分提供了新的见解。这些知识有助于颗粒合成的进一步发展以及设计制备具有复杂层次结构颗粒的新策略。
