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Novel Applications of FIB-SEM-Based ToF-SIMS in Atom Probe Tomography Workflows

Published online by Cambridge University Press:  09 March 2020

William D.A. Rickard Open the ORCID record for William D.A. Rickard [Opens in a new window] ,
Steven M. Reddy Open the ORCID record for Steven M. Reddy [Opens in a new window] ,
David W. Saxey Open the ORCID record for David W. Saxey [Opens in a new window] ,
Denis Fougerouse Open the ORCID record for Denis Fougerouse [Opens in a new window] ,
Nicholas E. Timms Open the ORCID record for Nicholas E. Timms [Opens in a new window] ,
Luke Daly Open the ORCID record for Luke Daly [Opens in a new window] ,
Emily Peterman ,
Aaron J. Cavosie Open the ORCID record for Aaron J. Cavosie [Opens in a new window]  and
Fred Jourdan Open the ORCID record for Fred Jourdan [Opens in a new window]
William D.A. Rickard*
Affiliation:
John de Laeter Centre, Curtin University, GPO Box U1987, Perth, WA6845, Australia
Steven M. Reddy
Affiliation:
School of Earth and Planetary Sciences, Curtin University, GPO Box U1987, Perth, WA6845, Australia
David W. Saxey
Affiliation:
John de Laeter Centre, Curtin University, GPO Box U1987, Perth, WA6845, Australia
Denis Fougerouse
Affiliation:
School of Earth and Planetary Sciences, Curtin University, GPO Box U1987, Perth, WA6845, Australia
Nicholas E. Timms
Affiliation:
School of Earth and Planetary Sciences, Curtin University, GPO Box U1987, Perth, WA6845, Australia
Luke Daly
Affiliation:
School of Earth and Planetary Sciences, Curtin University, GPO Box U1987, Perth, WA6845, Australia School of Geographical and Earth Sciences, University of Glasgow, GlasgowG12 8QQ, UK Australian Centre for Microscopy and Microanalysis, University of Sydney, Sydney2006, NSW, Australia
Emily Peterman
Affiliation:
Earth and Oceanographic Science, Bowdoin College, Brunswick, ME, USA
Aaron J. Cavosie
Affiliation:
School of Earth and Planetary Sciences, Curtin University, GPO Box U1987, Perth, WA6845, Australia
Fred Jourdan
Affiliation:
John de Laeter Centre, Curtin University, GPO Box U1987, Perth, WA6845, Australia School of Earth and Planetary Sciences, Curtin University, GPO Box U1987, Perth, WA6845, Australia
*
*Author for correspondence: William D.A. Rickard, Email: [email protected]
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Abstract

Atom probe tomography (APT) is used to quantify atomic-scale elemental and isotopic compositional variations within a very small volume of material (typically <0.01 µm3). The small analytical volume ideally contains specific compositional or microstructural targets that can be placed within the context of the previously characterized surface in order to facilitate a correct interpretation of APT data. In this regard, careful targeting and preparation are paramount to ensure that the desired target, which is often smaller than 100 nm, is optimally located within the APT specimen. Needle-shaped specimens required for atom probe analysis are commonly prepared using a focused ion beam scanning electron microscope (FIB-SEM). Here, we utilize FIB-SEM-based time-of-flight secondary ion mass spectrometry (ToF-SIMS) to illustrate a novel approach to targeting <100 nm compositional and isotopic variations that can be used for targeting regions of interest for subsequent lift-out and APT analysis. We present a new method for high-spatial resolution targeting of small features that involves using FIB-SEM-based electron deposition of platinum “buttons” prior to standard lift-out and sharpening procedures for atom probe specimen manufacture. In combination, FIB-ToF-SIMS analysis and application of the “button” method ensure that even the smallest APT targets can be successfully captured in extracted needles.

Keywords

FIB-SEMatom probe tomograpysample preparationFIB-ToF-SIMS
Type
Australian Microbeam Analysis Society Special Section AMAS XV 2019
Information
Microscopy and Microanalysis , Volume 26 , Issue 4 , August 2020 , pp. 750 - 757
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Copyright
Copyright © Microscopy Society of America 2020

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References

Alberts, D, Von Werra, L, Oestlund, F, Rohner, U, Hohl, M, Michler, J & Whitby, JA (2014). Design and performance of two orthogonal extraction time-of-flight secondary ion mass stectrometers for focused ion beam instruments. Instrum Sci Technol 42(4), 432–445.CrossRefGoogle Scholar
Babinsky, K, De Kloe, R, Clemens, H & Primig, S (2014). A novel approach for site-specific atom probe specimen preparation by focused ion beam and transmission electron backscatter diffraction. Ultramicroscopy 144, 9–18.CrossRefGoogle ScholarPubMed
Benninghoven, A, Rudenauer, F & Werner, HW (1987 ) Secondary ion mass spectrometry: Basic concepts, instrumental aspects, applications and trends. University of Chicago, J. Wiley. Accessed date 15 Jan 2011.Google Scholar
Breen, AJ, Babinsky, K, Day, AC, Eder, K, Oakman, CJ, Trimby, PW, Primig, S, Cairney, JM & Ringer, SP (2017). Correlating atom probe crystallographic measurements with transmission Kikuchi diffraction data. Microsc Microanal 23(2), 279–290.CrossRefGoogle ScholarPubMed
Buening, D & Buseck, PR (1973). Fe-Mg lattice diffusion in olivine. J Geophys Res 78(29), 6852–6862.CrossRefGoogle Scholar
Cavosie, AJ, Erickson, TM, Timms, NE, Reddy, SM, Talavera, C, Montalvo, SD, Pincus, MR, Gibbon, RJ & Moser, D (2015). A terrestrial perspective on using ex situ shocked zircons to date lunar impacts. Geology 43(11), 999–1002.CrossRefGoogle Scholar
Daly, L, Forman, LV, Bland, PA, Fougerouse, D, Reddy, SM, Saxey, DW & Rickard, WDA (2017). Nebula sulfidation and evidence for migration of “free-floating” refractory metal nuggets revealed by atom probe microscopy. Geology 45(9), 847–850.CrossRefGoogle Scholar
Fougerouse, D, Reddy, SM, Kirkland, CL, Saxey, DW, Rickard, WD & Hough, RM (2019). Time-resolved, defect-hosted, trace element mobility in deformed Witwatersrand pyrite. Geosci Front 10 (1). 55-63CrossRefGoogle Scholar
Fougerouse, D, Reddy, SM, Saxey, DW, Rickard, WDA, Van Riessen, A & Micklethwaithe, S (2016). Nanoscale gold clusters in arsenopyrite controlled by growth-rate not concentration: Evidence from atom probe microscopy. Am Mineral 101, 1916–1919.CrossRefGoogle Scholar
Fujiwara, A, Kawaguchi, J, Yeomans, D, Abe, M, Mukai, T, Okada, T, Saito, J, Yano, H, Yoshikawa, M & Scheeres, D (2006). The rubble-pile asteroid Itokawa as observed by Hayabusa. Science 312(5778), 1330–1334.CrossRefGoogle ScholarPubMed
Kelly, TF & Larson, DJ (2012). Atom probe tomography 2012. Annu Rev Mater Res 42(1), 1–31.CrossRefGoogle Scholar
Lotharukpong, C, Tweddle, D, Martin, TL, Wu, M, Grovenor, CRM, Moody, MP & Wilshaw, PR (2017). Specimen preparation methods for elemental characterisation of grain boundaries and isolated dislocations in multicrystalline silicon using atom probe tomography. Mater Charact 131, 472–479.CrossRefGoogle Scholar
Mcmahon, G, Nxumalo, J & Phaneuf, M (2002). Applications of a novel FIB-SIMS instrument in SIMS image depth profiling. Microsc Microanal 8(S02), 1212–1213.CrossRefGoogle Scholar
Mcphail, DS, Li, L, Chater, RJ, Yakovlev, N & Seng, H (2011). From FIB-SIMS to SIMS-FIB. The prospects for a 10 nm lateral resolution SIMS instrument with full FIB functionality. Surf Interface Anal 43(1–2), 479–483.CrossRefGoogle Scholar
Meher, S, Nandwana, P, Rojhirunsakool, T, Tiley, J & Banerjee, R (2015). Probing the crystallography of ordered phases by coupling of orientation microscopy with atom probe tomography. Ultramicroscopy 148, 67–74.CrossRefGoogle ScholarPubMed
Miller, MK & Forbes, RG (2014). Introduction to atom-probe tomography. In Atom-Probe Tomography: The Local Electrode Atom Probe, pp. 1–49. Boston, MA: Springer US.Google Scholar
Nakamura, T, Noguchi, T, Tanaka, M, Zolensky, ME, Kimura, M, Tsuchiyama, A, Nakato, A, Ogami, T, Ishida, H & Uesugi, M (2011). Itokawa dust particles: A direct link between S-type asteroids and ordinary chondrites. Science 333(6046), 1113–1116.CrossRefGoogle ScholarPubMed
Peterman, EM, Reddy, SM, Saxey, DW, Snoeyenbos, DR, Rickard, WDA, Fougerouse, D & Kylander-Clark, ARC (2016). Nanogeochronology of discordant zircon measured by atom probe microscopy of Pb-enriched dislocation loops. Sci Adv 2(9). e1601318.CrossRefGoogle ScholarPubMed
Piazolo, S, La Fontaine, A, Trimby, P, Harley, S, Yang, L, Armstrong, R & Cairney, JM (2016). Deformation-induced trace element redistribution in zircon revealed using atom probe tomography. Nat Commun 7.10490.CrossRefGoogle ScholarPubMed
Ping, D-H, Hono, K & Nie, J (2003). Atom probe characterization of plate-like precipitates in a Mg–RE–Zn–Zr casting alloy. Scr Mater 48(8), 1017–1022.CrossRefGoogle Scholar
Reddy, SM, Van Riessen, A, Johnson, TE, Saxey, DW, Fischer, S, Rickard, WDA, Fougerouse, D, Prosa, T, Rice, K, Reinhard, DA & Chen, Y (2016). Mechanisms of deformation-induced trace element migration in zircon resolved by atom probe and correlative microscopy. Geochim Cosmochim Acta 195, 158–170.CrossRefGoogle Scholar
Rice, KP, Chen, Y, Prosa, TJ & Larson, DJ (2016). Implementing transmission electron backscatter diffraction for atom probe tomography. Microsc Microanal 22(3), 583–588.CrossRefGoogle ScholarPubMed
Schwarz, T, Stechmann, G, Gault, B, Cojocaru-Mirédin, O, Wuerz, R & Raabe, D (2018). Correlative transmission Kikuchi diffraction and atom probe tomography study of Cu(In,Ga)Se2 grain boundaries. Prog Photovoltaics 26(3), 196–204.CrossRefGoogle Scholar
Smith, NS, Skoczylas, WP, Kellogg, SM, Kinion, DE, Tesch, PP, Sutherland, O, Aanesland, A & Boswell, RW (2006). High brightness inductively coupled plasma source for high current focused ion beam applications. J Vac Sci Technol B 24(6), 2902–2906.CrossRefGoogle Scholar
Stephan, T (2001). TOF-SIMS in cosmochemistry. Planet Space Sci 49(9), 859–906.CrossRefGoogle Scholar
Stoffers, A, Cojocaru-Mirédin, O, Seifert, W, Zaefferer, S, Riepe, S & Raabe, D (2015). Grain boundary segregation in multicrystalline silicon: Correlative characterization by EBSD, EBIC, and atom probe tomography. Prog Photovoltaics 23(12), 1742–1753.CrossRefGoogle Scholar
Sui, T, Song, B, Dluhos, J, Lu, L & Korsunsky, AM (2015). Nanoscale chemical mapping of Li-ion battery cathode material by FIB-SEM and TOF-SIMS multi-modal microscopy. Nano Energy 17, 254–260.CrossRefGoogle Scholar
Thompson, K, Flaitz, PL, Ronsheim, P, Larson, DJ & Kelly, TF (2007 a). Imaging of arsenic Cottrell atmospheres around silicon defects by three-dimensional atom probe tomography. Science 317(5843), 1370–1374.CrossRefGoogle ScholarPubMed
Thompson, K, Lawrence, D, Larson, D, Olson, J, Kelly, T & Gorman, B (2007 b). In situ site-specific specimen preparation for atom probe tomography. Ultramicroscopy 107(2), 131–139.CrossRefGoogle ScholarPubMed
Tytko, D, Choi, P-P, Klöwer, J, Kostka, A, Inden, G & Raabe, D (2012). Microstructural evolution of a Ni-based superalloy (617B) at 700°C studied by electron microscopy and atom probe tomography. Acta Mater 60(4), 1731–1740.CrossRefGoogle Scholar
Valley, JW, Cavosie, AJ, Ushikubo, T, Reinhard, DA, Lawrence, DF, Larson, DJ, Clifton, PH, Kelly, TF, Wilde, SA, Moser, DE & Spicuzza, MJ (2014). Hadean age for a post-magma-ocean zircon confirmed by atom-probe tomography. Nat Geosci 7(3), 219–223.CrossRefGoogle Scholar
Whitby, JA, Östlund, F, Horvath, P, Gabureac, M, Riesterer, JL, Utke, I, Hohl, M, Sedláček, L, Jiruše, J & Friedli, V (2011). High spatial resolution time-of-flight secondary ion mass spectrometry for the masses: A novel orthogonal ToF FIB-SIMS instrument with in situ AFM. Adv Mater Sci Eng 2012. Article ID 180437, 13 pages.Google Scholar
Yano, H, Kubota, T, Miyamoto, H, Okada, T, Scheeres, D, Takagi, Y, Yoshida, K, Abe, M, Abe, S & Barnouin-Jha, O (2006). Touchdown of the Hayabusa spacecraft at the Muses Sea on Itokawa. Science 312(5778), 1350–1353.CrossRefGoogle ScholarPubMed