High Sensitivity of Fluorine Gas-Assisted FIB-TOF-SIMS for Chemical Characterization of Buried Sublayers in Thin Films.

In this work, we present the potential of high vacuum-compatible time-of-flight secondary ion mass spectrometry (TOF-SIMS) detectors, which can be integrated within focused ion beam (FIB) instruments for precise and fast chemical characterization of thin films buried deep under the sample surface. This is demonstrated on complex multilayer systems composed of alternating ceramic and metallic layers with thicknesses varying from several nanometers to hundreds of nanometers. The typical problems of the TOF-SIMS technique, that is, low secondary ion signals and mass interference between ions having similar masses, were solved using a novel approach of co-injecting fluorine gas during the sample surface sputtering. In the most extreme case of the Al/Al2O3/Al/Al2O3/.../Al sample, a <10 nm thick Al2O3 thin film buried under a 0.5 μm material was detected and spatially resolved using only 27Al+ signal distribution. This is an impressive achievement taking into account that Al and Al2O3 layers varied only by a small amount of oxygen content. Due to its high sensitivity, fluorine gas-assisted FIB-TOF-SIMS can be used for quality control of nano- and microdevices as well as for the failure analysis of fabrication processes. Therefore, it is expected to play an important role in the development of microelectronics and thin-film-based devices for energy applications.