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Atom probe tomography

Nature Reviews Methods Primers volume 1, Article number: 51 (2021) Cite this article

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Abstract

Atom probe tomography (APT) provides three-dimensional compositional mapping with sub-nanometre resolution. The sensitivity of APT is in the range of parts per million for all elements, including light elements such as hydrogen, carbon or lithium, enabling unique insights into the composition of performance-enhancing or lifetime-limiting microstructural features and making APT ideally suited to complement electron-based or X-ray-based microscopies and spectroscopies. Here, we provide an introductory overview of APT ranging from its inception as an evolution of field ion microscopy to the most recent developments in specimen preparation, including for nanomaterials. We touch on data reconstruction, analysis and various applications, including in the geosciences and the burgeoning biological sciences. We review the underpinnings of APT performance and discuss both strengths and limitations of APT, including how the community can improve on current shortcomings. Finally, we look forwards to true atomic-scale tomography with the ability to measure the isotopic identity and spatial coordinates of every atom in an ever wider range of materials through new specimen preparation routes, novel laser pulsing and detector technologies, and full interoperability with complementary microscopy techniques.

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Fig. 1: Microstructural features with their typical size and some analytical techniques used to analyse them.
Fig. 2: Schematics of the atom probe instrumentation and the field evaporation process.
Fig. 3: FIB lift-out specimen preparation.
Fig. 4: Specimen preparation techniques for non-bulk samples.
Fig. 5: Ranged mass spectrum and reconstruction protocol.
Fig. 6: Examples of reconstruction and data visualization and analysis from engineering alloys.
Fig. 7: Spatial resolution of APT in the analysis of precipitates.

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Acknowledgements

This Primer was a collaborative effort and, even though the authors tried to be inclusive of all perspectives on various aspects of atom probe tomography (APT) research, it reflects our experiences and some articles likely escaped our attention. Apologies to those forgotten — it was not intentional. B.G. is thankful to past and present members of the Atom Probe group at Max-Planck-Institut für Eisenforschung (MPIE) and financial support from the European Research Council (ERC) (ERC-CoG-SHINE-771602), the Max-Planck Society, the BMBF (Federal Ministry of Education and Research), the Deutsche Forschungsgemeinsschaft (DFG) including for the Leibniz Prize, the Volkswagen Stiftung, the Alexander von Humboldt Stiftung and the Engineering and Physical Sciences Research Council (EPSRC) (and some companies). J.M.C. is grateful to the Australian Research Council (ARC) for her Future Fellowship. O.C.-M. is grateful for funding from the BMWi EFFCIS II and DFG 917 Nanoswitches. T.L. thanks the DFG for financial support (project number 407513992). R.D. acknowledges NSERC (Natural Sciences and Engineering Research Council of Canada) for her doctoral postgraduate scholarship (PGS-D). P.S. is grateful for funding from the BMBF (VIP 03V0756). S.K.M. acknowledges financial support from AVH and funding from the DFG SFB-TR103 project A4. M.M. acknowledges financial support EPSRC grants EP/M022803/1 and EP/S021663/1.

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Authors and Affiliations

  1. Max-Planck-Institut für Eisenforschung, Düsseldorf, Germany

    Baptiste Gault & Christoph Freysoldt

  2. Department of Materials, Royal School of Mines, Imperial College, London, UK

    Baptiste Gault

  3. National Institute of Standards and Technology, Applied Chemicals and Materials Division, Boulder, CO, USA

    Ann Chiaramonti

  4. I. Institute of Physics (IA), RWTH Aachen University, Aachen, Germany

    Oana Cojocaru-Mirédin

  5. Institute of Materials Science, University of Stuttgart, Stuttgart, Germany

    Patrick Stender

  6. Department of Earth and Environmental Sciences, University of Ottawa, Ottawa, Ontario, Canada

    Renelle Dubosq

  7. Department of Materials Engineering, Indian Institute of Science, Bangalore, India

    Surendra Kumar Makineni

  8. Institute for Materials, Ruhr-Universität Bochum, Bochum, Germany

    Tong Li

  9. Department of Materials, University of Oxford, Oxford, UK

    Michael Moody

  10. Australian Centre for Microscopy and Microanalysis, University of Sydney, Sydney, New South Wales, Australia

    Julie M. Cairney

  11. School of Aerospace, Mechanical and Mechatronic Engineering, University of Sydney, Sydney, New South Wales, Australia

    Julie M. Cairney

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Contributions

Introduction (B.G.); Experimentation (P.S., S.K.M., B.G. and C.F.); Results (M.M. and B.G.); Applications (J.M.C., M.M., O.C.-M., A.C., R.D., T.L. and B.G.); Reproducibility and data deposition (B.G.); Limitations and optimizations (B.G.); Outlook (B.G., O.C.-M., P.S., R.D., S.K.M., T.L., M.M., A.C., J.M.C. and C.F.); Overview of the Primer (B.G. and A.C.).

Corresponding authors

Correspondence to Baptiste Gault or Ann Chiaramonti.

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Competing interests

The authors declare no competing interests.

Additional information

Peer review information

Nature Reviews Methods Primers thanks C. Cappelli, D. Perea, A. Perez-Huerta, H. Wen, J. Zimmerman and the other, anonymous, reviewer(s) for their contribution to the peer review of this work.

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Related links

APT-HDF5 file specification: https://docs.google.com/document/u/2/d/e/2PACX-1vRxcJ_xF_jiNS77CoeZdQdDXD8l2BebL-DoOBkDrAsGTrkArdjLHEMCXAifBieeS8pTO9jJ9xnstKxs/pub

APT Technical Committee: https://groups.google.com/g/atomprobe-tc?pli=1

INSPICO High Resolution Analysis: https://www.inspico.eu/Home/

Software tools for APT analysis: https://tinyurl.com/APM-SoftwareList

Steam Instruments: https://steaminstruments.com/

Glossary

Solutes

Atoms of a species different from the main constituent atoms, which correspond to the solvent in a mixture. Solutes, often called dopants in electronic materials, are added to modify the material’s properties.

Microstructural imperfections

Irregularities in the arrangement of atoms in a crystal, often modifying a material’s physical properties. These include lattice defects as well as inclusions of isolated or clustered foreign atoms, second phases or particles forming in a matrix of the main constituting element (solvent).

Vacancies

Atoms missing from one of the crystal lattice sites forming a point defect.

Dislocations

Linear crystal defects typically associated with the plastic deformation of a material. There are two main types of dislocation, edge and screw. A single defect can exhibit both characteristics in different parts along the dislocation line. Mobile (glissile) and immobile (sessile) dislocations both exist. In the case of an edge dislocation, the addition of an extra half-plane of atoms in the structure results in a compressive stress on one side of the dislocation and a tensile stress on the other. Segregation of solute elements to the dislocation helps reduce the free energy associated with these defects.

Stacking faults

Local changes in the stacking sequence of atomic layers in a crystal.

Twins

Two crystals with a defined crystallographic relationship with each other, formed typically by a cooperative displacement of atoms along a specific plane referred to as a twin boundary, which can be caused by plastic deformation. The organization of atoms on either side of the twin boundary can be such that they are mirror images of each other, or follow a specific rational twin law. Twin boundaries are often considered low-energy.

Grain boundaries

Junctions of two crystals (most crystalline materials are made of an ensemble of individual crystals, referred to as grains). The local discontinuity of the atomic arrangement makes grain boundaries loci of interest for microstructure design. Segregation of solutes typically happens to minimize the system’s free energy, and grain boundaries assist with heterogeneous nucleation of secondary phases, for instance. The grain boundary energy depends on the magnitude of the change in orientation between the two grains as well as the crystallographic plane at the junction of the two grains.

Secondary phases and phase boundaries

Solids formed by a mixture of species can adopt one or more thermodynamic phases, which can sometimes co-exist. The formation of such secondary phases can be hindered by the kinetics, often associated with lattice diffusion and thermal activation. The discontinuity in the crystal lattice introduced by the presence of this second phase forms a phase boundary. The difference in the lattice unit cell can make secondary phases only partially or completely incoherent with the host lattice. Often, there exists a relationship in the crystalline orientation between the matrix and the secondary phase particle.

Composition

The relative quantity of atoms of a species with respect to all atoms of all the detected species given in atomic per cent.

Polarity

Here, the electrical polarity, used to represent the electric positive (+) or negative (−) sign of the electrical potential at the ends of an electrical circuit.

Field ionization

A physical phenomenon whereby atoms or molecules can be ionized because of an intense electric field.

Field evaporation

A physical phenomenon whereby atoms constituting a material can be removed in the form of ions because of an intense electric field.

Projection optic

In microscopy, the transfer of the image of an object onto a surface through an optical system that can contain lenses or mirrors, for instance.

Time-of-flight mass spectrometer

A spectrometer that exploits the proportionality of an ion’s mass to charge ratio with its time of flight from a source to a particle detector to deduce the nature of atomic or molecular ions.

Reflectron

An electrostatic mirror that can be flat or concave helping to correct spread in the time of flight associated with energy deficits by allowing adjustment of the ions’ flight distance proportionally to their incoming energy.

Delay-line detector

A type of particle detector where the particle impact location on the detector’s surface is deduced from the difference in the arrival time of electrical signals at the two ends of a line, that is, a wire. Delay-line detectors typically contain two or three lines to obtain the lateral and vertical coordinates of the impact position, with the signals forming the third line used to disambiguate combinations of signals coming from multiple impacts.

Molecular ions

Ions containing more than one atom (as opposed to atomic ions) that have, overall, lost one or more electrons. Molecular ions are usually metastable, but some are sufficiently long-lived to be detected.

Micro-tip coupon

A support for lift-out specimen preparation, typically made of silicon processed by a reactive ion and/or chemical etching.

Local electrode

A conical microelectrode implemented on the commercial local electrode atom probe (LEAP), positioned approximately 40 μm away from the specimen, enabling a strong localized increase in the electric field at the apex of the specimen. The implementation of such microelectrodes enabled mounting multiple specimens at once into the instrument and, then, analysis in succession.

Mass peak ranging

The definition of the lower and higher mass to charge values of each individual mass peak in the mass spectrum to associate the mass to charge with one element or a combination of atoms from one or multiple elements.

Image compression

An atom probe-specific term describing the angular compression associated with the ion projection; that is, the ratio of the crystallographic angle to the imaged angle.

Quasi-stereographic projection

A model of point projection of a sphere onto a plane, which is bijective and preserves angles but neither distances nor areas. The standard projection has the projection point and the projection plane diametrically opposed. In a quasi-stereographic projection, this is not necessarily the case.

Voxelization

In an atom probe, the conversion of the three-dimensional point cloud into an array or grid of volumetric elements containing a certain number of atoms of a certain size. Following voxelization, the number of atoms of each defined species can be used to calculate a local composition, and is usually subject to a smoothing process termed delocalization.

Iso-surface

A three-dimensional surface representing points of a given threshold value of composition, concentration or density within the 3D point cloud. The iso-surface is built from the grid of voxels and, hence, subject to the delocalization.

Iso-concentration

The concentration is a quantity per unit volume expressed in atoms per cubic nanometre, for instance, equivalent to a density. Owing to trajectory aberrations and reconstruction issues, volume estimations from reconstructed atom probe data are typically not precise.

Interfacial excess

The number of excess atoms of a certain species per unit area of an interface.

Round robin experiments

A set of interlaboratory measurements independently performed that allows for direct comparison of analyses and results, and that can help guide establishing best practice.

Rayleigh criterion

The shortest distance below which the diffraction-limited image of two point sources can no longer be separated.

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Gault, B., Chiaramonti, A., Cojocaru-Mirédin, O. et al. Atom probe tomography. Nat Rev Methods Primers 1, 51 (2021). https://doi.org/10.1038/s43586-021-00047-w

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