Reactive multilayer systems represent an innovative approach for potential usage in chip joining applications. As there are several factors governing the energy release rate and the stored chemical energy, the impact of the morphology and the microstructure on the reaction behavior is of great interest. In the current work, 3D reactive microstructures with nanoscale Al/Ni multilayers were produced by alternating deposition of pure Ni and Al films onto nanostructured Si substrates by magnetron sputtering. In order to elucidate the influence of this 3D morphology on the phase transformation process, the microstructure and the morphology of this system were characterized and compared with a flat reactive multilayer system on a flat Si wafer. The characterization of both systems was carried out before and after a rapid thermal annealing treatment by using scanning and transmission electron microscopy of the cross sections, selected area diffraction analysis, and differential scanning calorimetry. The bent shape of multilayers caused by the complex topography of silicon needles of the nanostructured substrate was found to favor the atomic diffusion at the early stage of phase transformation and the formation of two intermetallic phases Al0.42Ni0.58 and AlNi3, unlike the flat multilayers that formed a single phase AlNi after reaction.
Reactive multilayer systems are nanostructures of great interest for various technological applications because of their high energy release rate during the self‐propagating reaction of their components. Therefore, many efforts are aimed at controlling the propagation velocity of these reactions. Herein, reactive multilayer systems of Al/Ni in the shape of free‐standing foils with a wavelike surface morphology prepared by using sacrificial substrates with well‐aligned waves are presented and the propagation of the reaction along different directions of the reproduced waves is analyzed. During the ignition test, the propagation front is recorded with a high‐speed camera, and the maximum temperature is measured using a pyrometer. The propagation of the reaction is favored in the direction of the waves, which points out the influence of the anisotropy generated by this morphology and how it affects the propagation dynamics and the resulting microstructure. Furthermore, compared to their counterparts fabricated on flat substrates, these reactive multilayers with wavelike morphology exhibit a remarkable reduction in the propagation velocity of the reaction of about 50%, without significantly affecting the maximum temperature registered during the reaction.
Fast energy release, which is a fundamental property of reactive multilayer systems, can be used in a wide field of applications. For most applications, a self-propagating reaction and adhesion between the multilayers and substrate are necessary. In this work, a distinct approach for achieving self-propagating reactions and adhesion between deposited Ni/Al reactive multilayers and silicon substrate is demonstrated. The silicon surface consists of random structures, referred to as silicon grass, which were created by deep reactive ion etching. Using the etching process, structure units of heights between 8 and 13 µm and density between 0.5 and 3.5 structures per µm2 were formed. Ni and Al layers were alternatingly deposited in the stoichiometric ratio of 1:1 using sputtering, to achieve a total thickness of 5 µm. The analysis of the reaction and phase transformation was done with high-speed camera, high-speed pyrometer, and X-ray diffractometer. Cross-sectional analysis showed that the multilayers grew only on top of the silicon grass in the form of inversed cones, which enabled adhesion between the silicon grass and the reacted multilayers. A self-propagating reaction on silicon grass was achieved, due to the thermally isolating air pockets present around these multilayer cones. The velocity and temperature of the reaction varied according to the structure morphology. The reaction parameters decreased with increasing height and decreasing density of the structures. To analyze the exact influence of the morphology, further investigations are needed.
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