Fabrication of Specimens for Atom Probe Tomography Using a Combined Gallium and Neon Focused Ion Beam Milling Approach.

We demonstrate a new focused ion beam sample preparation method for atom probe tomography. The key aspect of the new method is that we use a neon ion beam for the final tip-shaping after conventional annulus milling using gallium ions. This dual-ion approach combines the benefits of the faster milling capability of the higher current gallium ion beam with the chemically inert and higher precision milling capability of the noble gas neon ion beam. Using a titanium-aluminum alloy and a layered aluminum/aluminum-oxide tunnel junction sample as test cases, we show that atom probe tips prepared using the combined gallium and neon ion approach are free from the gallium contamination that typically frustrates composition analysis of these materials due to implantation, diffusion, and embrittlement effects. We propose that by using a focused ion beam from a noble gas species, such as the neon ions demonstrated here, atom probe tomography can be more reliably performed on a larger range of materials than is currently possible using conventional techniques.

Characteristics Comparison of Neon, Argon, and Krypton Ion Emissions from Gas Field Ionization Sources with a Single-Atom Tip.

A scanning ion beam instrument equipped with a gas field ionization source (GFIS) has been commercialized, but only helium and neon are currently available as GFISs. In this study, the characteristics of neon, argon, and krypton ion emissions from a single-atom tip are compared, specifically for faster fabrication by milling of a silicon sample. Although the boiling point of argon is about 87 K, our experiments on characterizing argon ion emission can be carried out at temperatures of about 50 K at an argon gas pressure lower than 0.1 Pa. Argon exhibits ion current characteristics, as a function of tip voltage, between those of neon and krypton. The value obtained by multiplying the ion emission current by the sputtering yield is suitable for a figure of merit (FOM) for faster fabrication. The FOM for argon is the highest among the three ion species. This value must be extensively evaluated from the viewpoint of practical nano-fabrication application. The instabilities of neon, argon, and krypton ion currents (3σ) become as low as 8% in 1 h, which is sufficient for fabrication applications. We conclude that an argon or krypton GFIS ion beam instrument will be a useful tool for nano-fabrication.