An in-situ approach for preparing atom probe tomography specimens by xenon plasma-focussed ion beam

Halpin, John E.; Webster, Robert W. H.; Gardner, Hazel; Moody, Michael P.; Bagot, Paul A.J.; MacLaren, Donald A.

doi:10.1016/j.ultramic.2019.04.005

Cited by 31 publications

(28 citation statements)

References 27 publications

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“…In most cases, a low kV (≤ 5 kV) final annular milling step is applied to APT tips to ensure beam damage and ion implantation are minimised. In addition, the recent development of xenon plasma FIB systems, which remove the Ga contamination problem, has significant potential for atom probe sample preparation (Halpin et al ).…”

Section: Sample Selection and Preparationmentioning

confidence: 99%

Atom Probe Tomography: Development and Application to the Geosciences

Reddy

Saxey

Rickard

et al. 2020

Geostandard Geoanalytic Res

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Atom probe tomography (APT) is an analytical technique that provides quantitative three‐dimensional elemental and isotopic analyses at sub‐nanometre resolution across the whole periodic table. Although developed and mostly used in the materials science and semiconductor fields, recent years have seen increasing development and application in the geoscience and planetary science disciplines. Atom probe studies demonstrate compositional complexity at the nanoscale and provide fundamental new insights into the atom‐scale mechanisms taking place in minerals over geological time. Here, we provide an overview of APT, including the historical development and technical aspects of the instrumentation, and the fundamentals of data acquisition, data processing and data reconstruction. We also review previous studies and highlight the potential future applications of nanoscale geochemical studies of natural materials.

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Section: Sample Selection and Preparationmentioning

confidence: 99%

Atom Probe Tomography: Development and Application to the Geosciences

Reddy

Saxey

Rickard

et al. 2020

Geostandard Geoanalytic Res

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“…APT requires the needle-shaped specimens to produce an electrostatic field sufficiently intense to provoke field evaporation of atoms on the surface. With the availability of PFIB, an in situ APT specimen preparation strategy was revisited recently (38,39), in which specimens were fabricated directly from the original flat sample prepared for scanning electron microscopy (SEM) imaging, eliminating the need for conventional liftout and Pt-welding procedures (40). The details of each step are described in Methods.…”

Section: Specimen Preparationmentioning

confidence: 99%

“…The protocol introduced by Halpin et al (38) was adapted to dig a moat and leave a pillar in the middle. The pillar is then sharpened using a Xe-plasma beam.…”

Section: Cryo-fib Equipmentmentioning

confidence: 99%

“…To prepare specimens suitable for field evaporation within a state-of-the-art atom probe microscope, we adapted the blotting and plunge-freezing approaches typically implemented for cryo-TEM. We used an in situ plasma focused ion beam (PFIB) (38) approach, albeit here at cryo-temperature. The low contact angle of the water droplet on the NPG substrate facilitated the preparation of stable specimens fully composed of frozen liquid.…”

Section: Introductionmentioning

confidence: 99%

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Enabling near-atomic–scale analysis of frozen water

et al. 2020

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Transmission electron microscopy went through a revolution enabling routine cryo-imaging of biological and (bio)chemical systems, in liquid form. Yet, these approaches typically lack advanced analytical capabilities. Here, we used atom probe tomography to analyze frozen liquids in three dimensions with subnanometer resolution. We introduce a specimen preparation strategy using nanoporous gold. We report data on 2- to 3-μm-thick layers of ice formed from both high-purity deuterated water and a solution of 50 mM NaCl in high-purity deuterated water. The analysis of the gold-ice interface reveals a substantial increase in the solute concentrations across the interface. We explore a range of experimental parameters to show that atom probe analyses of bulk aqueous specimens come with their own challenges and discuss physical processes that produce the observed phenomena. Our study demonstrates the viability of using frozen water as a carrier for near-atomic–scale analysis of objects in solution by atom probe tomography.

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“…The ability to accurately characterize grain boundaries in Al alloys, will undoubtedly enable the elucidation of intergranular corrosion mechanisms. While additional investigations are required to identify the exact influence of FIB-milling and transfer temperatures on Ga diffusivity in Al alloys, these preliminary results show that maintaining cryogenic temperatures is a way to obtain Ga-free grain boundaries in such materials without resorting to alternative plasma-based FIB systems [36][37][38].…”

Section: Plos Onementioning

confidence: 90%

A versatile cryo-transfer system, connecting cryogenic focused ion beam sample preparation to atom probe microscopy

et al. 2021

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Atom probe tomography (APT) is a powerful technique to obtain 3D chemical and structural information, however the ‘standard’ atom probe experimental workflow involves transfer of specimens at ambient conditions. The ability to transfer air- or thermally-sensitive samples between instruments while maintaining environmental control is critical to prevent chemical or morphological changes prior to analysis for a variety of interesting sample materials. In this article, we describe a versatile transfer system that enables cryogenic- or room-temperature transfer of specimens in vacuum or atmospheric conditions between sample preparation stations, a focused ion beam system (Zeiss Crossbeam 540) and a widely used commercial atom probe system (CAMECA LEAP 4000X HR). As an example for the use of this transfer system, we present atom probe data of gallium- (Ga)-free grain boundaries in an aluminum (Al) alloy specimen prepared with a Ga-based FIB.

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An in-situ approach for preparing atom probe tomography specimens by xenon plasma-focussed ion beam

Cited by 31 publications

References 27 publications

Atom Probe Tomography: Development and Application to the Geosciences

Atom Probe Tomography: Development and Application to the Geosciences

Enabling near-atomic–scale analysis of frozen water

A versatile cryo-transfer system, connecting cryogenic focused ion beam sample preparation to atom probe microscopy

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