Exploration of atom probe tomography at sub-10K

Alec C Day; Andrew J Breen; David A Reinhard; Thomas F Kelly; Simon P Ringer

doi:10.1016/j.ultramic.2022.113595

Exploration of atom probe tomography at sub-10K

Ultramicroscopy. 2022 Nov:241:113595. doi: 10.1016/j.ultramic.2022.113595. Epub 2022 Jul 26.

Authors

Alec C Day¹, Andrew J Breen², David A Reinhard³, Thomas F Kelly⁴, Simon P Ringer²

Affiliations

¹ The University of Sydney, Australian Centre for Microscopy & Microanalysis, and School of Aerospace, Mechanical and Mechatronic Engineering. Sydney, NSW 2006, Australia; Steam Instruments, Inc., Madison, WI 53703, USA. Electronic address: alec.day@steaminstruments.com.
² The University of Sydney, Australian Centre for Microscopy & Microanalysis, and School of Aerospace, Mechanical and Mechatronic Engineering. Sydney, NSW 2006, Australia.
³ CAMECA Instruments, Inc. Madison, WI 53711, USA.
⁴ Steam Instruments, Inc., Madison, WI 53703, USA.

PMID: 36029636
DOI: 10.1016/j.ultramic.2022.113595

Abstract

The operating temperature is a critical parameter in atom probe tomography experiments. It affects the spatial precision, mass resolving power and other key aspects of the field-evaporation process. Current commercially available atom probes operate at a minimum temperature of ∼25 K when measured at the specimen. In this paper, we explore and implement changes to the mechanical design of both the LEAP^Ⓡ and EIKOS™ atom probe microscope systems manufactured by CAMECA^Ⓡ to enable a specimen temperature in the sub-10 K regime. We use these modified instruments to analyze four materials systems: pure Al (in both pulsed-voltage and pulsed-laser mode), pure W (pulsed-voltage mode only), doped Si, and GaN (pulsed-laser mode only). The effects of conducting atom probe experiments in the sub-10 K regime were assessed with reference to a range of quantitative analysis metrics related to spatial precision, mass resolving power, stoichiometry and charge-state ratio. We demonstrate that the spatial precision is significantly improved with decreasing temperature, whilst the effect on mass resolving power is relatively minor. The enhanced spatial precision is significant insofar as it enables lattice planes from the doped Si samples to be resolved. Furthermore, mass spectral analysis, lower noise floors and changes in the field evaporation process enabled more accurate GaN compositional measurements. We discuss the significance of these findings for the semiconductor and metallurgical industries and the potential opportunities for further investigations of this parameter space.

Keywords: Atom probe tomography; Cryogenic analysis; Mass resolving power; Spatial precision.