Impact of Microstructure of Nanoscale Magnetron Sputtered Ru/Al Multilayers on Thermally Induced Phase Formation

In this study, we report on phase formation and microstructure evolution in multiscale magnetron sputtered Ru/Al multilayers upon thermal annealing in vacuum at slow heating rates of 10 K/min. By specifically adjusting the microstructure and design of the as-deposited multilayers, the formation of certain desired phases can be tuned. We demonstrate that the synthesis of single phase RuAl thin films is possible in a very controlled manner in a solid state only via thermal activation without initiating the self-propagating exothermic reactions of Ru/Al multilayers. To investigate phase formation sequences and the resulting microstructures, Ru/Al multilayers were designed via magnetron sputtering with systematic variation of bilayer modulation periods and subsequent vacuum annealing. Thin films samples were characterized by in situ high-temperature XRD, TEM imaging and diffraction. It is shown that different phase sequences appear in strong correlation with the modulation length. Depending on the multilayer design, the phase formation toward single-phase RuAl thin films happens as either a multi-step or single-step event. In particular, below a critical threshold of the modulation period, the multi-step phase formation can be suppressed, and only the desired RuAl target phase is obtained with a pronounced growth in a preferred orientation. This finding may be versatile for the targeted synthesis of intermetallic phases, contributing to further understanding of phase formation in such nanoscale multilayer systems.