The Combination of Electron Microscopy, Raman Microscopy and Energy Dispersive X‐Ray Spectroscopy for the Investigation of Polymeric Materials

Abstract

Polymers play an important role in materials science, because of their advantages over other types of materials. The huge variety in terms of the types, arrangements and combinations of monomers found in polymers leads to an extremely wide diversity of different polymeric materials. Although there is a wide range of analytical techniques to characterize polymeric materials, here the focus is laid on a novel correlative microscopy method, combining Raman microscopy, scanning electron microscopy (SEM) and energy dispersive X‐ray spectroscopy (EDXS). Therefore, three polymeric specimens were analysed by the new system RISE (Raman Imaging and Scanning Electron microscopy) in combination with EDXS. The aim of this contribution is to demonstrate the potential of the new system to characterize different polymeric layers, as well as fillers and additives in polymeric materials. In addition to the results, a methodical chapter deals with preparation aspects, investigation skills and imaging modes of the electron microscope. Here the so‐called variable pressure mode (VP) is mentioned, where nitrogen is used as imaging gas at pressures between 10 and 133 Pa. Furthermore, the low‐voltage mode in the high vacuum is discussed which gives a better surface resolution due to a smaller interaction volume of the electrons in the material and furthermore causes lower beam damage. Both modes work without a conductive coating on the specimen, which is a requirement for Raman investigations. Further capabilities of the RISE system in combination with the EDXS will be discussed afterwards.

Multiscale and Correlative Analytical Electron Microscopy of Extraterrestrial Minerals

“…The SEM imaging was performed using the scanning electron microscope Sigma 300 VP (Zeiss, Oberkochen, Germany) and the chemical analysis with the attached Raman microscope from WITec (Ulm, Germany). The electron microscope is also equipped with a silicon drift detector from Oxford (UK) for EDXS that allows for fast acquisition of spectra and maps (Schmidt et al, 2019). The energy resolution of the Oxford EDS detector as specified by the provider is: at C Ka −50 eV, F Ka −57 eV, Mn Ka −127 eV.…”

“…In this work in addition to SEM and TEM, we apply a new correlative microstructure analysis of the Seymchan meteorite by using the Raman Imaging and Scanning Electron Microscopy RISE (Jiruše et al, 2014;Schmidt et al, 2019). The RISE method is a seamless combination of two techniques, that offers the possibility of imaging by SEM and chemical analysis with the attached Raman microscope.…”

Recent Progress on Advanced Imaging Techniques for Lithium‐Ion Batteries

“…(Left) Correlative SEM and Raman system, where the Raman optics is located outside the SEM electron beam axis; measurement takes place sequentially after a precise displacement of the stage. (Right) [ 81 ] Reproduced with permission. [ 81 ] Copyright 2019, Wiley‐VCH.…”

“…(Right) [ 81 ] Reproduced with permission. [ 81 ] Copyright 2019, Wiley‐VCH. d) The photo of SEM–Raman system.…”

“…[ 81 ] Reproduced with permission. [ 81 ] Copyright 2019, Wiley‐VCH. e) Thermal images on the same Li/β‐Li 3 PS 4 /Li cell collected using a top contact made of steel foil painted in matte black, or steel wire.…”