AVS 64th International Symposium & Exhibition
    Applied Surface Science Division Monday Sessions
       Session AS+BI+MI-MoM

Paper AS+BI+MI-MoM5
New Insights on Layered Polymer Systems, Polymer Networks and Polymerization in Defined Geometries by Combining Surface Analysis with Depth Profiling using ToF-SIMS and XPS as Analytical Tools

Monday, October 30, 2017, 9:40 am, Room 13

Session: Practical Surface Analysis: Getting the Most Out of Your Analysis using Complementary Techniques
Presenter: Sven Steinmüller, Institute for Applied Materials, Karlsruhe Institute of Technology, Germany
Authors: S.O. Steinmüller, Institute for Applied Materials, Karlsruhe Institute of Technology, Germany
A. Llevot, Institute of Organic Chemistry, Karlsruhe Institute of Technology, Germany
D. Moock, Institute for Applied Materials, Karlsruhe Institute of Technology, Germany
B. Bitterer, Institute of Organic Chemistry, Karlsruhe Institute of Technology, Germany
F. Cavalli, Institute for Biological Interfaces, Karlsruhe Institute of Technology, Germany
S. Hurrle, Institute for Chemical Technology and Polymer Chemistry, Karlsruhe Institute of Technology, Germany
M. Bruns, Institute for Applied Materials, Karlsruhe Institute of Technology, Germany
Correspondent: Click to Email

Surface analytical characterization of polymers is still a tough topic if precise information are favored. Especially for characterization of stepwise layered systems and for studying reaction rates and composition of network formation or to confirm polymerization within defined geometries a lot of techniques are not sensitive enough to fulfill the desired degree of precision and resolution. Within the recently installed Cooperate Research Center “SFB 1176” at KIT (Molecular Structuring of Soft Matter), a high degree of precision is necessary to qualitatively and quantitatively confirm the defined structures achieved during the polymer syntheses. Here a new surface analysis approach combining X-ray Photoelectron Spectroscopy (XPS) and Time of Flight Secondary Ion Mass Spectrometry (ToF-SIMS) including Ar cluster ion sputter depth profiling for three dimensional systems is utilized to prove every reaction step of polymer syntheses and to evidence three-dimensional structures at high lateral resolution. By using different marker molecules as well as specific molecule ion fragments, the combination of these two methods enables to obtain the precise characterization and evaluation of the different polymeric systems.

We present our results on the implementation of new methods for precise surface analysis of polymers. Starting with the investigation of molecular layered systems prepared via electrografting of surfaces followed by successive thiol-yne or thiol-ene reactions, we show controlled functionalization on silicon as well as on highly oriented pyrrolytic graphit substrates. Finally the developed strategy will be transferred to real graphite electrodes. This is an important step to design and tailor the properties of artificial solid electrolyte interfaces (SEI) for lithium ion batteries.

From the characterization of these two dimensional systems (according to the surface analytical tasks), we follow up with polymer systems with three dimensional analysis questions. We present analytical results of network formation using the Para-fluoro-thiol reaction and strategies for the confirmation of polymer position after polymerization within defined geometries. Surface analytical recipes to confirm synthesis routes were established. The analytical results of the three dimensional chemical picture are taken to further optimize the synthesis routes and network properties.

We kindly acknowledge the SFB 1176, funded by the German Research Council (DFG), in the context of projects B2, C1, C4 and Z1 for funding. The K-Alpha+ instrument was financially supported by the Federal Ministry of Economics and Technology on the basis of a decision by the German Bundestag.