Correlation between deposition parameters of periodic titanium metal/oxide nanometric multilayers and their chemical and structural properties investigated by STEM-EELS

Valérie Potin; Arnaud Cacucci; Nicolas Martin

doi:10.1016/j.micron.2017.06.008

Correlation between deposition parameters of periodic titanium metal/oxide nanometric multilayers and their chemical and structural properties investigated by STEM-EELS

Micron. 2017 Oct:101:62-68. doi: 10.1016/j.micron.2017.06.008. Epub 2017 Jun 21.

Authors

Valérie Potin¹, Arnaud Cacucci¹, Nicolas Martin²

Affiliations

¹ Laboratoire Interdisciplinaire Carnot de Bourgogne (ICB), UMR 6303 CNRS, Univ. Bourgogne Franche-Comté, 9, Avenue Alain Savary, BP 47 870, F-21078 Dijon Cedex, France.
² Institut FEMTO-ST, UMR 6174 CNRS, Univ. Bourgogne Franche-Comté, 15B, Avenue des Montboucons, 25030 Besancon Cedex, France. Electronic address: nicolas.martin@femto-st.fr.

PMID: 28662412
DOI: 10.1016/j.micron.2017.06.008

Abstract

We analyze structure and composition of titanium-based metal/oxide periodic multilayers prepared by reactive sputtering. The reactive gas pulsing process is involved to periodically inject the oxygen gas during the multilayers deposition. This approach allows the growth of regular and tunable nanometric TiO₂/Ti periods with thicknesses ranging from 14 to 50nm. The interfacial layer between oxide and metallic layers is mainly the fcc-TiO phase as clearly pointed out by transmission electron microscopy and associated electron spectroscopies. In addition, sharp transitions are produced at Ti/TiO₂ interfaces (with a high density of defects) whereas the smoothest ones are obtained at TiO₂/Ti interfaces. Similarly, the real-time measurements of the target voltage vs. time correlate with periodic alternations formed by a mixture of amorphous+rutile TiO₂ compound, the fcc-TiO phase and the hcp metallic Ti phase through the films thickness. An abrupt transition from metallic to oxidized sputtering mode takes place when oxygen is injected and correlates with the sharp Ti/TiO₂ interface. On the other hand, when oxygen is stopped, the restoration to the metallic sputtering mode is longer and corresponds to the occurrence of the fcc-TiO phase at the smooth TiO₂/Ti interfaces.

Keywords: Electron energy loss spectroscopy; Gas pulsing; Periodic multilayers; Reactive sputtering; Titanium oxide; Transmission electron microscopy.