Characterization of the interphase in an aluminium/epoxy joint by using controlled pressure scanning electron microscopy coupled with an energy dispersive X-ray spectrometer

Abstract

The aim of this work is to introduce the use of low vacuum scanning electron microscopy (LVSEM) coupled with an X-ray energy dispersive spectrometer (EDS) in the field of structural adhesives, more precisely aluminium/epoxy resin assembly. Such assembly is characterized by the creation of an interphase resulting from the metal diffusion inside the resin during cross-linking. As the performance of the final bond is strongly links by the interphase properties, fine characterization of this interphase, in particularity the evaluation of its thickness is essential to understand the macroscopic properties of the adhesive assembly. First, the EDS acquisition parameters were investigated in order to limit the sample/resin damage/degradation due to the incident electrons beam irradiation. Then a specific methodology of stacked profiles was defined to improve the precision of the measures. To evaluate the true Al diffusion profile, the impact of the interaction volume of incident electron in the material on the Al signal variation during the interface crossing was calculated and the effect of the gas pressure on the electron beam characteristic and so on the measured profiles was examinated. According to our developed methodology and data treatments, Al diffusion profile was interpreted and interphase thickness was qualitatively determined by comparison with an experimental baseline. This innovative methodology promotes the use of LVSEM–EDS in the field of adhesive structural assemblies, but also, deals with a comparative study on the effect of the gas pressure on the EDS profile analysis.