Skip to main content Accessibility help

We use cookies to distinguish you from other users and to provide you with a better experience on our websites. Close this message to accept cookies or find out how to manage your cookie settings.

Close cookie message
×
Hostname: page-component-8448b6f56d-t5pn6 Total loading time: 0 Render date: 2024-04-23T14:34:40.324Z Has data issue: false hasContentIssue false

6 - Instrumentation for ASAT

from Core Section

Published online by Cambridge University Press:  03 March 2022

Thomas F. Kelly ,
Brian P. Gorman  and
Simon P. Ringer
Thomas F. Kelly
Affiliation:
Steam Instruments, Inc.
Brian P. Gorman
Affiliation:
Colorado School of Mines
Simon P. Ringer
Affiliation:
University of Sydney
Get access

Summary

Based on the discussion in Chapters 4 and 5, combining information from both electron microscopy, presumably (Scanning) Transmission Electron Microscopy ((S)TEM), and Atom Probe Tomography (APT) is a likely path toward ASAT. Experimentally, concurrent (S)TEM and APT may appear to be a straightforward experiment, but the instrumentation required can be complex and require significant capital investment. In this chapter, we consider what instrumentation is necessary for each technique and what could be done to both simplify and improve the ASAT technique in a combined instrument that solves many of the complexities in experimentation. Experimental conditions such as vacuum pressure, cryogenic temperatures, electron imaging and diffraction, laser wavelength and positioning, and specimen holder designs must all be taken into account.

Keywords

correlative TEM and APToff-axis electron holographycryogenic specimenelectron diffractionatomscopeATOM ProjectErnst Ruska CenterColorado School of MinesUniversity of SydneySteam Instruments
Type
Chapter
Information
Atomic-Scale Analytical Tomography
Concepts and Implications
 , pp. 98 - 124
Publisher: Cambridge University Press
Print publication year: 2022

Access options

Get access to the full version of this content by using one of the access options below. (Log in options will check for institutional or personal access. Content may require purchase if you do not have access.)

References

Kirchhofer, R., Diercks, D. R., and Gorman, B. P., “Electron Diffraction and Imaging for Atom Probe Tomography,” Rev. Sci. Instrum., vol. 89, no. 5, p. 053706, May 2018, doi: https://doi.org/10.1063/1.4999484.Google Scholar
Nordén, H. and Bowkett, K. M., “Electron Microscope Holders for Viewing Thin Wire Specimens and Field-Ion Microscope Tips,” J. Sci. Instrum., vol. 44, pp. 238–240, 1967.Google Scholar
Fischione, P. E., Haugh, J. J., and Burke, M. G., “An Advanced Technique for the Preparation and TEM Examination of FIM Specimens,” J. Phys. Paris Colloq., vol. 50, pp. 555–560, 1989.Google Scholar
Instruments, Fischione, “2Model 2050 | Fischione,” Model 2050 On-Axis Rotation Tomography Holder, 2020. www.fischione.com/products/holders/model-2050-axis-rotation-tomography-holder (accessed May 31, 2020).Google Scholar
Kotula, P. G., Brewer, L. N., Michael, J., and Giannuzzi, L., “Computed Tomographic Spectral Imaging: 3D STEM-EDS Spectral Imaging,” Microsc. Microanal., vol. 13, no. S02, pp. 1324–1325, Aug. 2007, doi: https://doi.org/10.1017/S1431927607071851.CrossRefGoogle Scholar
Gorman, B. P., Improving AP Reconstructions through Combined FIB, STEM, and LEAP. M&M 2006, 2006.Google Scholar
Gorman, B. P., Diercks, D., Salmon, N. et al., “Hardware and Techniques for Cross-Correlative TEM and Atom Probe Analysis,” Microsc. Today, vol. 16, no. 4, pp. 42–47, 2008.Google Scholar
Thompson, K., Lawrence, D. J., Larson, D. J. et al., “In-Situ Site-Specific Specimen Preparation for Atom Probe Tomography,” Ultramicroscopy, vol. 107, no. 2–3, pp. 131–139, 2007.Google Scholar
Miller, M. K., “Sculpting Needle-Shaped Atom Probe Specimens with a Dual Beam FIB,” Microsc. Microanal., vol. 11, p. 808, 2005.Google Scholar
Kirchhofer, R., “Development of a Dynamic Atom Probe,” Ph.D. thesis, Colorado School of Mines, Golden, Colorado, 2014.Google Scholar
Diercks, D. R. and Gorman, B. P., “Self-Consistent Atom Probe Tomography Reconstructions Utilizing Electron Microscopy,” Ultramicroscopy, vol. 195, pp. 32–46, Dec. 2018, doi: https://doi.org/10.1016/j.ultramic.2018.08.019.Google Scholar
Burton, G. L., Ricote, S., Foran, B. J., Diercks, D. R., and Gorman, B. P., “Quantification of Grain Boundary Defect Chemistry in a Mixed Proton-Electron Conducting Oxide Composite,” J. Am. Ceram. Soc., vol. 103, no. 5, pp. 3217–3230, 2020, doi: https://doi.org/10.1111/jace.17014.Google Scholar
Stokes, A., Al-Jassim, M., Diercks, D., Clarke, A., and Gorman, B., “Impact of Wide-Ranging Nanoscale Chemistry on Band Structure at Cu(In, Ga)Se 2 Grain Boundaries,” Sci. Rep., vol. 7, no. 1, p. 14163, Oct. 2017, doi: https://doi.org/10.1038/s41598-017-14215-0.Google Scholar
Stokes, A., Al-Jassim, M., Diercks, D. R., Egaas, B., and Gorman, B., “3-D Point Defect Density Distributions in Thin Film Cu(In,Ga)Se2 Measured by Atom Probe Tomography,” Acta Mater., vol. 102, pp. 32–37, 2016.Google Scholar
Gorman, B. P., Burton, G., and Diercks, D. R., “Utilizing Atom Probe Tomography for 3-D Quantification of Point Defects,” Microsc. Microanal., vol. 23, no. S1, pp. 1574–1575, Jul. 2017, doi: https://doi.org/10.1017/S1431927617008534.Google Scholar
Clark, D. R. et al., “Probing Grain-Boundary Chemistry and Electronic Structure in Proton-Conducting Oxides by Atom Probe Tomography,” Nano Lett., vol. 16, no. 11, pp. 6924–6930, Nov. 2016, doi: https://doi.org/10.1021/acs.nanolett.6b02918.Google Scholar
Diercks, D. R. et al., “Three-Dimensional Quantification of Composition and Electrostatic Potential at Individual Grain Boundaries in Doped Ceria,” J. Mater. Chem. A, vol. 4, no. 14, pp. 5167–5175, Mar. 2016, doi: https://doi.org/10.1039/C5TA10064 J.Google Scholar
Diercks, D. R., Gorman, B. P., Manerbino, A., and Coors, G., “Atom Probe Tomography of Yttrium-Doped Barium-Cerium-Zirconium Oxide with NiO Addition,” J. Am. Ceram. Soc., vol. 97, no. 10, pp. 3301–3306, Oct. 2014, doi: https://doi.org/10.1111/jace.13093.Google Scholar
Kirchhofer, R., Teague, M. C., and Gorman, B. P., “Thermal Effects on Mass and Spatial Resolution during Laser Pulse Atom Probe Tomography of Cerium Oxide,” J. Nucl. Mater., vol. 436, no. 1–3, pp. 23–28, 2013.Google Scholar
LeBlanc, E. G. et al., “Determining and Controlling the Magnesium Composition in CdTe/CdMgTe Heterostructures,” J. Electron. Mater., vol. 46, no. 9, pp. 5379–5385, Sep. 2017, doi: https://doi.org/10.1007/s11664-017-5589-3.CrossRefGoogle Scholar
Kuzmina, M., Herbig, M., Ponge, D., Sandlobes, S., and Raabe, D., “Linear Complexions: Confined Chemical and Structural States at Dislocations,” Science, vol. 349, no. 6252, pp. 1080–1083, Sep. 2015.Google Scholar
Gorman, B., Ballard, J., Romanes, M. et al., “Mediation of Electrostatic Discharge Induced Morphological Damage in Atomically Precise Tips,” Microsc. Microanal., vol. 16, no. S2, pp. 480–481, 2010.Google Scholar
Beleggia, M., Kasama, T., Larson, D. J. et al., “Towards Quantitative Off-Axis Electron Holographic Mapping of the Electric Field around the Tip of a Sharp Biased Metallic Needle,” J. Appl. Phys., vol. 116, no. 2, p. 024305, 2014, doi: https://doi.org/10.1063/1.4887448.Google Scholar
Zheng, F., Migunov, V., Caron, J. et al., “Three-Dimensional Electric Field Mapping of an Electrically Biased Atom Probe Needle Using Off-Axis Electron Holography,” Microsc. Microanal., vol. 25, no. (Supp. 2), pp. 326–327, 2019.Google Scholar
Rose, H., “Nonstandard Imaging Methods in Electron Microscopy,” Ultramicroscopy, vol. 2, pp. 251–267, Jan. 1976, doi: https://doi.org/10.1016/S0304-3991(76)91538-2.Google Scholar
Savitzky, B. H. et al., “py4DSTEM: A Software Package for Multimodal Analysis of Four-Dimensional Scanning Transmission Electron Microscopy Datasets,” Microsc. Microanal., Mar. 2020, Accessed: May 19, 2020. [Online]. doi: http://arxiv.org/abs/2003.09523.Google Scholar
Müller, E. W., “Resolution of the Atomic Structure of a Metal Surface by the Field Ion Microscope,” J. Appl. Phys., vol. 27, no. 5, pp. 474–476, 1956.Google Scholar
Tsong, T. T., Atom-Probe Field Ion Microscopy: Field Ion Emission and Surfaces and Interfaces at Atomic Resolution. Cambridge, UK: Cambridge University Press, 1990.Google Scholar
Day, A. C., Ph.D. thesis, University of Sydney, 2021. Thesis Advisor: Simon P. Ringer.Google Scholar
Stephenson, L. T. et al., “The Laplace Project: An Integrated Suite for Preparing and Transferring Atom Probe Samples under Cryogenic and UHV Conditions,” PLOS ONE, vol. 13, no. 12, p. e0209211, Dec. 2018, doi: https://doi.org/10.1371/journal.pone.0209211.Google Scholar
Chang, Y. et al., “Ti and Its Alloys as Examples of Cryogenic Focused Ion Beam Milling of Environmentally-Sensitive Materials,” Nat. Commun., vol. 10, no. 1, Art. no. 1, Feb. 2019, doi: https://doi.org/10.1038/s41467-019-08752-7.Google Scholar
Lilensten, L. and Gault, B., “New Approach for FIB-Preparation of Atom Probe Specimens for Aluminum Alloys,” PLOS ONE, vol. 15, no. 4, p. e0231179, Apr. 2020, doi: https://doi.org/10.1371/journal.pone.0231179.Google Scholar
Rivas, N. A. et al., “Cryo-Focused Ion Beam Preparation of Perovskite Based Solar Cells for Atom Probe Tomography,” PLOS ONE, vol. 15, no. 1, p. e0227920, Jan. 2020, doi: https://doi.org/10.1371/journal.pone.0227920.Google Scholar
Miller, M. K. and Kelly, T. F., “The Atom TOMography (ATOM) Concept,” Microsc. Microanal., vol. 16 (S2), pp. 1856–1857, 2010.Google Scholar
Kelly, T. F. et al., “Toward Atomic-Scale Tomography: The ATOM Project,” Microsc. Microanal., vol. 17 (Suppl 2), pp. 708–709, 2011, doi: https://doi.org/10.1017/S1431927611004417.Google Scholar
Kelly, T. F., Miller, M. K., Rajan, K., and Ringer, S. P., “Visions of Atomic-Scale Tomography,” Microsc. Today, 2012, doi: https://doi.org/10.1017/S1551929512000211.CrossRefGoogle Scholar
Kelly, T. F., Miller, M. K., Rajan, K., and Ringer, S. P., “Atomic-Scale Tomography: A 2020 Vision,” Microsc. Microanal., vol. 19, no. 3, pp. 652–664, 2013.Google Scholar
Poppa, H., “High Resolution, High Speed Ultrahigh Vacuum Microscopy,” J. Vac. Sci. Technol. A, vol. 22, no. 5, pp. 1931–1947, Sep. 2004, doi: https://doi.org/10.1116/1.1786304.Google Scholar
Jungjohann, K. and Carter, C. B., “In Situ and Operando,” in Transmission Electron Microscopy: Diffraction, Imaging, and Spectrometry, Carter, C. B. and Williams, D. B., eds. Cham: Springer International Publishing, 2016, pp. 17–80.Google Scholar
Ross, F. M. and Minor, A. M., “In Situ Transmission Electron Microscopy,” in Springer Handbook of Microscopy, Hawkes, P. W. and Spence, J. C. H., eds. Cham: Springer International Publishing, 2019, pp. 2–2.Google Scholar
Tromp, R. M. and Ross, F. M., “Advances in In Situ Ultra-High Vacuum Electron Microscopy: Growth of SiGe on Si,” Annu. Rev. Mater. Sci., vol. 30, no. 1, pp. 431–449, 2000, doi: https://doi.org/10.1146/annurev.matsci.30.1.431.Google Scholar
Ross, F. M., Tersoff, J., Tromp, R. M., Reuter, M. C., and Bennett, P., “Island Growth of Ge on Si(001) and CoSi2 on Si(111) Studied with UHV Electron Microscopy,” J. Electron Microsc. (Tokyo), vol. 48, no. SUPPL., pp. 1059–1066, 1999.Google Scholar
Collazo-Davila, C. et al., “Design and Initial Performance of an Ultrahigh Vacuum Sample Preparation Evaluation Analysis and Reaction (SPEAR) System,” Microsc. Microanal., vol. 1, no. 6, pp. 267–279, Dec. 1995, doi: https://doi.org/10.1017/S1431927695112672.Google Scholar
Jayaram, G., Plass, R., and Marks, L. D., “UHV-HREM and Diffraction of Surfaces,” Interface Sci., vol. 2, no. 4, pp. 379–395, Dec. 1995, doi: https://doi.org/10.1007/BF00222625.Google Scholar
McDonald, M. L., Gibson, J. M., and Unterwald, F. C., “Design of an Ultrahigh‐Vacuum Specimen Environment for High‐Resolution Transmission Electron Microscopy,” Rev. Sci. Instrum., vol. 60, no. 4, pp. 700–707, Apr. 1989, doi: https://doi.org/10.1063/1.1141004.Google Scholar
Sun, J. and Li, H., “Chapter Ten – How to Operate a Cryo-Electron Microscope,” in Methods in Enzymology, vol. 481, G. J. Jensen, ed. Press, Academic, 2010, pp. 231–249.CrossRefGoogle Scholar
Salome, M., Raynaud, B., Schack, M. et al., “A Side-Entry Liquid He Cooled Stage for the Philips EM400 Electron Microscope (Ion Implantation Application),” J. Phys. [E], vol. 18, no. 4, pp. 331–333, Apr. 1985, doi: https://doi.org/10.1088/0022-3735/18/4/018.Google Scholar
Murooka, S. and Fujiki, H., “A Side-Entry Helium-Cooled Stage for Electron Microscopy,” Jpn. J. Appl. Phys., vol. 30, no. 2 R, p. 411, Feb. 1991, doi: https://doi.org/10.1143/JJAP.30.411.Google Scholar
Jones, J. S. and Swann, P. R., “Specimen Cooling Holder for Side Entry Transmission Electron Microscopes,” US Patent: US4950901A, Aug. 21, 1990.Google Scholar
Fujiyoshi, Y. et al., “Development of a Superfluid Helium Stage for High-Resolution Electron Microscopy,” Ultramicroscopy, vol. 38, no. 3, pp. 241–251, Dec. 1991, doi: https://doi.org/10.1016/0304-3991(91)90159-4.Google Scholar
Minor, A. M., Denes, P., and Muller, D. A., “Cryogenic Electron Microscopy for Quantum Science,” MRS Bull., vol. 44, no. 12, pp. 961–966, Dec. 2019, doi: https://doi.org/10.1557/mrs.2019.288.Google Scholar
Pfeil-Gardiner, O., Mills, D. J., Vonck, J., and Kuehlbrandt, W., “A Comparative Study of Single-Particle Cryo-EM with Liquid-Nitrogen and Liquid-Helium Cooling,” IUCrJ, vol. 6, no. 6, pp. 1099–1105, Nov. 2019, doi: https://doi.org/10.1107/S2052252519011503.Google Scholar
Radebaugh, R., “Cryocoolers: The State of the Art and Recent Developments,” J. Phys. Condens. Matter, vol. 21, p. 9, 2009, doi: https://doi.org/10.1088/0953-8984/21/16/164219.Google Scholar
Advanced Research Systems, Inc., “CS202-DMX-20B,” Advanced Research Systems, 2020. www.arscryo.com/cs202-dmx-20b (accessed May 31, 2020).Google Scholar
Janis Research Company, LLC, “Vibration Isolated Closed Cycle Refrigerator Systems,” 2020. www.janis.com/Products/productsoverview/10KelvinCryocoolers/VibrationIsolated10KCryocooler.aspx (accessed May 31, 2020).Google Scholar
Völkl, E., Allard, L. F., and Joy, D. C., eds., Introduction to Electron Holography. Springer US, 1999.Google Scholar
Larson, D. J., Camus, P. P., and Kelly, T. F., “Simulated Electron Beam Trajectories toward a Field Ion Microscopy Specimen,” Appl. Surf. Sci., vol. 67, no. 1–4, pp. 473–480, 1993.Google Scholar
Larson, D. J., Camus, P. P., and Kelly, T. F., “Scanning Electron Microscopy in Very High Electric Fields near Field Ion/Emission Specimens,” in 53rd Annual Meeting of the Microscopy Society of America, 1995, pp. 624–625.Google Scholar
Petford‐Long, A. K. and Graef, M. D., “Lorentz Microscopy,” in Characterization of Materials, American Cancer Society, 2012, pp. 1–15.Google Scholar
Gorman, B. P., “Systems and Methods of Aberration Correction for Atom Probe Tomography,” US Patent: US20190318907A1, Oct. 17, 2019.Google Scholar
Chiaramonti, A. N., Miaja-Avila, L., Blanchard, P. T. et al., “A Three-Dimensional Atom Probe Microscope Incorporating a Wavelength-Tuneable Femtosecond-Pulsed Coherent Extreme Ultraviolet Light Source,” MRS Adv., vol. 4, no. 44–45, pp. 2367–2375, 2019, doi: https://doi.org/10.1557/adv.2019.296.Google Scholar
Chiaramonti, A. N. et al., “Field Ion Emission in an Atom Probe Microscope Triggered by Femtosecond-Pulsed Coherent Extreme Ultraviolet Light,” Microsc. Microanal., vol. 26, no. 2, pp. 258–266, Apr. 2020, doi: https://doi.org/10.1017/S1431927620000203.Google Scholar
Migunov, V., London, A., Farle, M., and Dunin-Borkowski, R. E., “Model-Independent Measurement of the Charge Density Distribution along an Fe Atom Probe Needle Using Off-Axis Electron Holography without Mean Inner Potential Effects,” J. Appl. Phys., vol. 117, no. 13, 2015, doi: https://doi.org/10.1063/1.4916609.Google Scholar
Wu, M., Tafel, A., Hommelhoff, P., and Spiecker, E., “Determination of 3D Electrostatic Field at an Electron Nano-Emitter,” Appl. Phys. Lett., vol. 114, no. 1, p. 013101, Jan. 2019, doi: https://doi.org/10.1063/1.5055227.CrossRefGoogle Scholar
Ceguerra, A. V., Breen, A. J., Cairney, J. M., Ringer, S. P., and Gorman, B. P., “Integrative Atom Probe Tomography Using STEM-Centric Atom Placement as a Step Towards Atomic-Scale Tomography,” Microsc. Microanal., vol. 27, no. 1, pp. 140–148, 2020, doi: https://doi.org/10.1017/S1431927620024873Google Scholar
Gorman, B. P., “Systems and Methods of Aberration Correction for Atom Probe Tomography,” US Patent: US10755891B2, Aug. 25, 2020.Google Scholar

Save book to Kindle

To save this book to your Kindle, first ensure coreplatform@cambridge.org is added to your Approved Personal Document E-mail List under your Personal Document Settings on the Manage Your Content and Devices page of your Amazon account. Then enter the ‘name’ part of your Kindle email address below. Find out more about saving to your Kindle.

Note you can select to save to either the @free.kindle.com or @kindle.com variations. ‘@free.kindle.com’ emails are free but can only be saved to your device when it is connected to wi-fi. ‘@kindle.com’ emails can be delivered even when you are not connected to wi-fi, but note that service fees apply.

Find out more about the Kindle Personal Document Service.

Available formats
×

Save book to Dropbox

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Dropbox.

Available formats
×

Save book to Google Drive

To save content items to your account, please confirm that you agree to abide by our usage policies. If this is the first time you use this feature, you will be asked to authorise Cambridge Core to connect with your account. Find out more about saving content to Google Drive.

Available formats
×