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Atom Probe Tomography

APT
APT
APT
APT
APT

The LEAP® 4000 XHR local electrode atom probe instrument from Cameca Instruments Inc. is used to perform the analytical analysis known as atom probe tomography (APT). APT analysis results in three-dimensional (3-D) atom-by-atom point cloud maps with atomic-scale resolution and part per million elemental sensitivity of a wide variety of materials ranging from soft biological materials to metal alloys, including low electrical conductivity materials such as ceramics, semiconductors, and oxides. At the Environmental Molecular Sciences Laboratory (EMSL), APT advances science relevant to the Department of Energy, Office of Science, Biological and Environmental Research program. It does so by providing unique compositional interface analysis and microstructural characterization of bioorganic-mineral interfaces and chemical gradients in biological systems to better understand the complex chemical language nature uses to communicate and perform fundamental functions relevant to energy and the environment. APT is available to researchers around the world through EMSL's open calls for proposals.

Research application

  • Supporting the Structural Biology Integrated Research Platform, APT provides atomic-scale resolution, and compositional and structural information for proteins and other biomolecular complexes to inform structure-based computational chemistry and simulation models aimed at understanding key biochemical functions and pathways.
  • Supporting the Biogeochemical Transformations Integrated Research Platform, APT provides atomic-scale insight at the interface between microbes and soil minerals that affect the transformation and mobility of critical nutrients, contaminants, aerosols, particles, and compounds within the environment.

EMSL is working to expand the application of APT to materials traditionally not studied using this technique such as hydrated biological materials and reactive metal surfaces. This involves the development of a vacuum chamber system called the Environmental Transfer Hub that enables the environmentally protected transfer of cryogenic and/or air sensitive specimens between the tools used to prepare them such as a focused ion beam-scanning electron microscope (FIB/SEM) or a gas-phase reactor, as well as the LEAP. As a result, this capability allows for the analysis of cryogenically prepared, hydrated biological materials to map ionic gradients and even potentially map atomic-scale macromolecular structure. Additionally, new modes of APT analysis are also possible, including in situ and in operando modes, providing insight into both corrosion and surface chemistry dynamics and the influence of strong electric fields on such phenomena.

Available instruments

  • LEAP® 4000 XHR Local Electrode Atom Probe (Cameca Instruments Inc.)
    (Instr. ID 34110, Availability: 10 hours/day 5 days/week)
    • Maximum Pulse Repetition Rate – Voltage Mode: 200 kHz
    • Maximum Pulse Repetition Rate – Laser Mode: 250 kHz
    • Laser Power: > 300 mW
    • Laser Wavelength: 355 nm
    • Sample Temperature: 25–150K
    • Maximum Energy per Pulse: 0.5 nJ
    • Dynamic Range: > 1000X
    • Field-of-View: > 200 nm (limited by the specimen geometry)
    • Typical Analysis Volume: approx. 100 nm x 100 nm x 300 nm
    • Collection Rate: > 50 M ions per hour
    • Detection Efficiency: approx. 40%
    • Lateral Resolution: 0.2 nm (using W-tip)
    • Depth Resolution: 0.1 nm (using W-tip)
    • Mass Resolution: Full FoV is ≥ 60° solid angle as measured from position of poles in the aluminum ion-desorption image (all results stem from using Al specimen)
    • Sensitive to every elemental isotope
    • Full Width at Half Maximum: 1/1000
    • Full Width at 10% Maximum: 1/475
    • Full Width at 1% Maximum: 1/300
    • Generally, no matrix corrections or sensitivity factors required for quantification
  • In Situ Reactor
    • Temperature Range: Room temperature to 500oC
    • Pressure Range: 10-9 bar to 1 bar
    • Tungsten sample holder available
    • Gases Available: D2, O2, 18O2, CO/Ar(10%), CO2, N2, Ar, H2O
  • Operando Mode
    • Temperature Range: 100 to 320 K
    • Pressure Range: 10-10 to 10-8 mbar
    • Gases Available: He, Ne, O2, CO

Tips for success

  • Specimens for analysis with APT must be solid. It is not possible to have materials in the gas or liquid phase during analysis.

Contributing teams and resources

EMSL develops and deploys capabilities for the user program by conducting original research independently or in partnership with others and by adapting/advancing science and technologies developed outside of EMSL. In some instances, EMSL directly deploys mature capabilities developed by others where there is value for the EMSL user community. The following grants/activities, PI’s and teams contributed to the development of this capability:

 

  • Daniel Perea, S&T Capability Development, Environmental Molecular Sciences Laboratory
  • James Evans and Daniel Perea, Chemical Imaging Initiative LDRD, Pacific Northwest National Laboratory
  • James Evans, DOE-BER Mesoscale to Molecules Bioimaging Project #66382
  • Daniel Schreiber and Daniel Perea, DOE-BES, WastePD Energy Frontier Research Center DE-SC0016584
  • Arun Devaraj, DOE-BES Early Career Research Program FWP #76052
  • Arun Devaraj, DOE Office of Vehicle Technology powertrain materials core program FWP #73557 and lightweight materials core programs FWP #77209

Related publications

  • Perea, D. E.; Liu, J.; Bartrand, J.; Dicken, Q.; Thevuthasan, S. T.; Browning, N. D.; Evans, J. E. Atom Probe Tomographic Mapping Directly Reveals the Atomic Distribution of Phosphorus in Resin Embedded Ferritin. Scientific Reports 2016, 6, 22321. https://doi.org/10.1038/srep22321.
  • Perea, D. E.; Gerstl, S. S. A.; Chin, J.; Hirschi, B.; Evans, James. E. An Environmental Transfer Hub for Multimodal Atom Probe Tomography. Advanced Structural and Chemical Imaging 2017, 3, 12. https://doi.org/10.1186/s40679-017-0045-2.
  • Perea, D. E.; Schreiber, D. K.; Ryan, J. V.; Wirth, M. G.; Deng, L.; Lu, X.; Du, J.; Vienna, J. D. Tomographic Mapping of the Nanoscale Water-Filled Pore Structure in Corroded Borosilicate Glass. npj Mater Degrad 2020, 4 (1), 1–7. https://doi.org/10.1038/s41529-020-0110-5.
  • Zachman, M. J.; Jonge, N. de; Fischer, R.; Jungjohann, K. L.; Perea, D. E. Cryogenic Specimens for Nanoscale Characterization of Solid–Liquid Interfaces. MRS Bulletin 2019, 44 (12), 949–955. https://doi.org/10.1557/mrs.2019.289.
  • Barton, D. J.; Nguyen, D.-T.; Perea, D. E.; Stoerzinger, K. A.; Lumagui, R. M.; Lambeets, S. V.; Wirth, M. G.; Devaraj, A. Towards Quantitative Analysis of Deuterium Absorption in Ferrite and Austenite during Electrochemical Charging by Comparing Cyclic Voltammetry and Cryogenic Transfer Atom Probe Tomography. International Journal of Hydrogen Energy 2023. https://doi.org/10.1016/j.ijhydene.2023.06.256.
  • Li, T.; Perea, D. E.; Schreiber, D. K.; Wirth, M. G.; Orren, G. J.; Frankel, G. S. Cryo-Based Structural Characterization and Growth Model of Salt Film on Metal. Corrosion Science 2020, 174, 108812. https://doi.org/10.1016/j.corsci.2020.108812.
  • Schreiber, D. K.; Perea, D. E.; Ryan, J. V.; Evans, J. E.; Vienna, J. D. A Method for Site-Specific and Cryogenic Specimen Fabrication of Liquid/Solid Interfaces for Atom Probe Tomography. Ultramicroscopy 2018, 194, 89–99. https://doi.org/10.1016/j.ultramic.2018.07.010.
  • B. Gwalani, J. Liu, S. Lambeets, M. Olszta, J. Poplawsky, A. Shyam, A. Devaraj, Rapid assessment of interfacial stabilization mechanisms of metastable precipitates to accelerate high-temperature Al-alloy development, Materials Research Letters, 2022, 10, 12,  https://doi.org/10.1080/21663831.2022.2102947

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