Systematic approaches for targeting an atom-probe tomography sample fabricated in a thin TEM specimen: Correlative structural, chemical and 3-D reconstruction analyses

Abstract

Atom-probe tomography (APT) is a unique analysis tool that enables true three-dimensional (3-D) analyses with sub-nano scale spatial resolution. Recent implementations of the local-electrode atom-probe (LEAP) tomograph with ultraviolet laser pulsing have significantly expanded the research applications of APT. The small field-of-view of a needle-shaped specimen with a less than 100 nm diam. is, however, a major limitation for analyzing materials. The systematic approaches for site-specific targeting of an APT nanotip in a transmission electron microscope (TEM) of a thin sample are introduced to solve the geometrical limitations of a sharpened APT nanotip. In addition to “coupling APT to TEM”, the technique presented here allows for targeting the preparation of an APT tip based on TEM observation of a much larger area than what is captured in the APT tip. The correlative methods have synergies for not only high-resolution structural analyses but also for obtaining chemical information. Chemical analyses in a TEM, both energy-dispersive X-ray spectroscopy (EDS) and electron energy-loss spectroscopy (EELS), are performed and compared with the APT chemical analyses of a carbide phase (M7C3) precipitate at a grain boundary in a Ni-based alloy. Additionally, a TEM image of a sharpened APT nanotip is utilized for calculation of the detection area ratio of an APT nanotip by comparison with a TEM image for precise tomographic reconstructions. A grain-boundary/carbide precipitate triple junction is used to attain precise positioning of an APT nanotip in an analyzed TEM specimen.