Isotopic labelling study of Oxygen and Hydrogen in surface analysis of metal oxides

• Oxygen-18 ( 18 O) quantitative analysis by NRA provides unique information about the mechanism of the anodizing of light metals. • Deuterium isotopic tracing sheds new light on the ALD process of oxide formation from hydrogen-containing precursors. • Both NRDP and SIMS are used to determine isotope depth distributions within thin oxide films. • ToF-SIMS is faster and cheaper than NRDP, but quantification requires the application of NRA as a complementary technique. Stable isotopes, such as oxygen-18 ( 18 O) or deuterium (D), combined with particle accelerator-based techniques or mass spectrometry, represent powerful tools for identifying and tracking ion migration under diverse technological conditions. There is a relatively narrow range of techniques sensitive to isotope detection. This paper considers two sets of methods: (i) ion beam analysis (IBA), which utilizes specific nuclear reactions performed at tandem or Van de Graaff accelerators, and (ii) Secondary Ion Mass Spectrometry techniques (SIMS). IBA and SIMS methods have been well-established in physics and chemistry thanks to significant improvements in vacuum technology and detector systems. Despite the well-established use of isotopic tracing in silicon technology since the early 1970s, its application in applied electrochemistry or surface science to explore phenomena at the nanoscale remains relatively understated and unexplored by non-physicists. In this context, examples of quantitative and qualitative analyses of 18 O tracer in thin aluminum oxide and titanium films will be presented through a comparison of Nuclear Reaction Analysis (NRA), Narrow Resonance Depth Profiling (NRDP), and Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) and Elastic Recoil Detection Analysis (ERDA) applied to deuterium (D) tracing for optimizing atomic layer deposition (ALD) formation of titanium oxides.