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  • https://doi.org/10.1002/9783527808465.emc2016.7044Copy DOI Icon

3D investigation of a PS / ABS polymer using different microscopy techniques

  • Dec 20, 2016
  • X Jaurand +8 more
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Abstract

This study is developed in the framework of RéCaMiA, a French regional (Rhône‐Alpes / Auvergne) microscopy network, which offers facilities through a panel of microscopes such as SEM, TEM, FIB, AFM, Confocal. The objective of the study is to compare results obtained with different microscopy techniques currently employed in three‐dimensional imaging, but it focuses more specifically on polymers [1‐3]. For the purpose a blend of polystyrene / acrylonitrile butadiene styrene (PS/ABS) is chosen. This material allows to obtain good contrast in SEM or TEM; microstructural features exist at the submicronic and nano scales; and its glass transition temperature T g is above 50°C. Two samples are stained by contact with a 4% osmium tetraoxide (OsO 4 ) water solution to reveal contrasts. 2 FIB–SEM (FEI Helios600, Zeiss NVisio40 dual beam), 2 TEM (JEOL JEM 1400, JEOL 2100F), 2 SEM (FEI ESEM XL30, FEI Quanta250) are used to study the 3D structure of the polymer. This study develops a multiscale approach. The tools used require 2 different procedures to get a 3D image: (a) to acquire a stack of individual imaging planes and to transform it into the corresponding 3D data volume or (b) to perform electron tomography. In the first case individual images are obtained through a slice and view approach in FIB, or through individual observations, in SEM or TEM, of several thin foils prepared by ultramicrotomy method at room temperature (serial sectioning). Backscattered electron images are collected. The 3D reconstructions of the polymer obtained by the different tools are compared each other. Whatever the approach used, the morphology “salami” shape is observed in the structure of the polymer. Structure parameters, such as size distribution of the nodules and the anisotropy coefficient, are extracted and compared. Different test parameters effects are investigated, the preparation of the sample (compression of the microstructure more or less), the voltage, the spacing between the individual imaging planes, etc. The balance between the reconstructed volume size, the voxel resolution, the total time to get the 3D data volume, the advantages and limitations of the methods used in this multiscale approach will also be discussed.

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