Impact of Sample Preparation Approach on Transmission Electron Microscopy Investigation of Sputtered AlNi Multilayers Used for Reactive Soldering

This work presents studies of sputtered Al/Ni reactive multilayers by transmission electron microscopy. They are prepared for these analyses by three methods (both Ga‐ and Xe‐based focused ion beam, FIB, and tripod polishing plus Ar + ion milling in precision ion polishing system, PIPS) to check their impact on these materials. Every sample shows polycrystalline and mostly chemically pure Al/Ni layers. They also hint existence of intermetallic compounds, especially the tripod‐prepared sample. These intermetallics first originate from the sputtering process. The layers are increasingly rough along the growth direction. Other remarkable findings can be highlighted. First, the heating operations applied during the tripod polishing preparation lead to recrystallization and blurred Al/Ni interfaces due to increased metals reactions, although additional contributions by roughness and preparation thickness to the current compositional uncertainties must be distinguished by optimizing future sample fabrications and preparations. Second, Xe‐based FIB leads to lamellae with seemingly low contamination, although Ga‐FIB is a potentially good alternative. Finally, FIB is better to study cross‐section preparations of pristine Al/Ni multilayers, whereas the present tripod polishing procedures are unsuitable for this purpose but allow to observe the beginning of Al/Ni transformations upon heating, which is interesting for the technological optimization of these materials.