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Analysis of Natural Rutile (TiO2) by Laser-assisted Atom Probe Tomography

Published online by Cambridge University Press:  01 February 2019

Rick Verberne*
Affiliation:
John de Laeter Centre, Geoscience Atom Probe, Advanced Resource Characterisation Facility, Curtin University, GPO Box U1987, Perth, WA 6845, Australia Applied Geology, School of Earth and Planetary Sciences, Curtin University—Perth City Campus, GPO Box U1987, Perth, WA 6845, Australia
David W. Saxey
Affiliation:
John de Laeter Centre, Geoscience Atom Probe, Advanced Resource Characterisation Facility, Curtin University, GPO Box U1987, Perth, WA 6845, Australia
Steven M. Reddy
Affiliation:
John de Laeter Centre, Geoscience Atom Probe, Advanced Resource Characterisation Facility, Curtin University, GPO Box U1987, Perth, WA 6845, Australia Applied Geology, School of Earth and Planetary Sciences, Curtin University—Perth City Campus, GPO Box U1987, Perth, WA 6845, Australia
William D. A. Rickard
Affiliation:
John de Laeter Centre, Geoscience Atom Probe, Advanced Resource Characterisation Facility, Curtin University, GPO Box U1987, Perth, WA 6845, Australia
Denis Fougerouse
Affiliation:
John de Laeter Centre, Geoscience Atom Probe, Advanced Resource Characterisation Facility, Curtin University, GPO Box U1987, Perth, WA 6845, Australia Applied Geology, School of Earth and Planetary Sciences, Curtin University—Perth City Campus, GPO Box U1987, Perth, WA 6845, Australia
Chris Clark
Affiliation:
Applied Geology, School of Earth and Planetary Sciences, Curtin University—Perth City Campus, GPO Box U1987, Perth, WA 6845, Australia
*
Author for correspondence: Rick Verberne, E-mail: rick.verberne89@gmail.com
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Abstract

Since the introduction of laser-assisted atom probe, analysis of nonconductive materials by atom probe tomography (APT) has become more routine. To obtain high-quality data, a number of acquisition variables needs to be optimized for the material of interest, and for the specific question being addressed. Here, the rutile (TiO2) reference material ‘Windmill Hill Quartzite,’ used for secondary ion mass spectrometry U–Pb dating and laser-ablation inductively coupled plasma mass spectrometry, was analyzed by laser-assisted APT to constrain optimal running conditions. Changes in acquisition parameters such as laser energy and detection rate are evaluated in terms of their effect on background noise, ionization state, hit-multiplicity, and thermal tails. Higher laser energy results in the formation of more complex molecular ions and affects the ionization charge state. At lower energies, background noise and hit-multiplicity increase, but thermal tails shorten. There are also correlations between the acquisition voltage and several of these metrics, which remain to be fully understood. The results observed when varying the acquisition parameters will be discussed in detail in the context of utilizing APT analysis of rutile within geology.

Type
Materials Science: Non-Metals
Copyright
Copyright © Microscopy Society of America 2019 

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References

Blum, TB, Darling, JR, Kelly, TF, Larson, DJ, Moser, DE, Perez-Huerta, A, Prosa, TJ, Reddy, SM, Reinhard, DA and Saxey, DW (2018) Best practices for reporting atom probe analysis of geological materials. Microstruc Geochronol: Planet Rec Down Atom Scale 232, 369373.Google Scholar
Clark, DJ, Hensen, BJ and Kinny, PD (2000) Geochronological constraints for a two-stage history of the Albany-Fraser Orogen, Western Australia. Precambrian Res 102(3–4), 155183.10.1016/S0301-9268(00)00063-2Google Scholar
Dachille, F, Simons, P and Roy, R (1968) Pressure-temperature studies of anatase, brookite, rutile and TiO2-II. Am Mineral 53, 19291939.Google Scholar
Ewing, TA (2011) Hf isotope analysis and U-Pb geochronology of rutile: technique development and application to a lower crustal section. Australian National University, Ivrea-Verbano Zone, Italy. https://openresearch-repository.anu.edu.au/handle/1885/1138917Google Scholar
Fougerouse, D, Reddy, SM, Kirkland, CL, Saxey, DW, Rickard, WD and Hough, RM (2018 a) Time-resolved, defect-hosted, trace element mobility in deformed Witwatersrand pyrite. Geosci Front 101, 19161919Google Scholar
Fougerouse, D, Reddy, SM, Saxey, DW, Erickson, TM, Kirkland, CL, Rickard, WDA, Seydoux-Guillaume, AM, Clark, C and Buick, IS (2018 b) Nanoscale distribution of Pb in monazite revealed by atom probe microscopy. Chem Geol 479, 251258.10.1016/j.chemgeo.2018.01.020Google Scholar
Fougerouse, D, Reddy, SM, Saxey, DW, Rickard, WDA, van Riessen, A and Micklethwaite, S (2016) Nanoscale gold clusters in arsenopyrite controlled by growth rate not concentration: Evidence from atom probe microscopy. Am Mineral 101(8), 19161919.10.2138/am-2016-5781CCBYNCNDGoogle Scholar
Gault, B, Moody, MP, Cairney, JM and Ringer, SP (2012) Atom Probe Microscopy. New York: Springer-Verlag.10.1007/978-1-4614-3436-8Google Scholar
Kingham, DR (1982) The post-ionization of field evaporated ions: A theoretical explanation of multiple charge states. Surf Sci 116(2), 273301.10.1016/0039-6028(82)90434-4Google Scholar
Kirchhofer, R, Teague, MC and Gorman, BP (2013) Thermal effects on mass and spatial resolution during laser pulse atom probe tomography of cerium oxide. J Nucl Mater 436(1–3), 2328.Google Scholar
Kirkland, C, Fougerouse, D, Reddy, S, Hollis, J and Saxey, D (2018) Assessing the mechanisms of common Pb incorporation into titanite. Chem Geol 483, 558566.Google Scholar
Kooijman, E, Mezger, K and Berndt, J (2010) Constraints on the U-Pb systematics of metamorphic rutile from in situ LA-ICP-MS analysis. Earth Planet Sci Lett 293(3–4), 321330.Google Scholar
Kooijman, E, Smit, M, Mezger, K and Berndt, J (2012) Trace element systematics in granulite facies rutile: Implications for Zr geothermometry and provenance studies. J Metamorph Geol 30(4), 397412.10.1111/j.1525-1314.2012.00972.xGoogle Scholar
La Fontaine, A, Piazolo, S, Trimby, P, Yang, L and Cairney, JM (2017) Laser-assisted atom probe tomography of deformed minerals: A zircon case study. Microsc Microanal 23(2), 404413.10.1017/S1431927616012745Google Scholar
Larson, DJ, Prosa, TJ, Ulfig, RM, Geiser, BP and Kelly, TF (2013) Local Electrode Atom Probe Tomography. New York, NY: Springer.10.1007/978-1-4614-8721-0Google Scholar
Meinhold, G (2010) Rutile and its applications in earth sciences. Earth Sci Rev 102(1–2), 128.10.1016/j.earscirev.2010.06.001Google Scholar
Meinhold, G, Morton, AC, Fanning, CM and Whitham, AG (2010) U–Pb SHRIMP ages of detrital granulite-facies rutiles: Further constraints on provenance of Jurassic sandstones on the Norwegian margin. Geol Mag 148(03), 473480.Google Scholar
Peng, Z, Choi, P-P, Gault, B and Raabe, D (2017) Evaluation of analysis conditions for laser-pulsed atom probe tomography: Example of cemented tungsten carbide. Microsc Microanal 23(2), 431442.10.1017/S1431927616012654Google Scholar
Peterman, EM, Reddy, SM, Saxey, DW, Snoeyenbos, DR, Rickard, WD, Fougerouse, D and Kylander-Clark, AR (2016) Nanogeochronology of discordant zircon measured by atom probe microscopy of Pb-enriched dislocation loops. Sci Adv 2(9), e1601318.10.1126/sciadv.1601318Google Scholar
Piazolo, S, La Fontaine, A, Trimby, P, Harley, S, Yang, L, Armstrong, R and Cairney, JM (2016) Deformation-induced trace element redistribution in zircon revealed using atom probe tomography. Nat Commun 7, 10490.10.1038/ncomms10490Google Scholar
Plavsa, D, Reddy, SM, Agangi, A, Clark, C, Kylander-Clark, A and Tiddy, CJ (2017) Microstructural, trace element and geochronological characterization of TiO2 polymorphs and implications for mineral exploration. Chem Geol 476, 130149.10.1016/j.chemgeo.2017.11.011Google Scholar
Reddy, SM, van Riessen, A, Saxey, DW, Johnson, TE, Rickard, WDA, Fougerouse, D, Fischer, S, Prosa, TJ, Katherine, PRE, Reinhard, DA, Chen, YM and Olson, D (2016) Mechanisms of deformation-induced trace element migration in zircon resolved by atom probe and correlative microscopy. Geochim Cosmochim Acta 195, 158170.Google Scholar
Reinhard, DA, Moser, DE, Martin, I, Rice, KP, Chen, Y, Olson, D, Lawrence, D, Prosa, TJ and Larson, DJ (2018) Atom probe tomography of phalaborwa baddeleyite and reference zircon BR266. Microstruc Geochronol: Planet Rec Down Atom Scale 315326.Google Scholar
Saxey, D, Moser, D, Piazolo, S, Reddy, S and Valley, J (2018 a) Atomic worlds: Current state and future of atom probe tomography in geoscience. Scr Mater 148, 115121.10.1016/j.scriptamat.2017.11.014Google Scholar
Saxey, DA, Reddy, SM, Fougerouse, D and Rickard, WD (2018 b) The Optimization of Zircon Analyses by Laser-Assisted Atom Probe Microscopy: Insights from the 91500 Zircon Standard. Microstructural Geochronology: Planetary Records Down to Atom Scale, pp. 293313.10.1002/9781119227250.ch14Google Scholar
Schreiber, DK, Chiaramonti, AN, Gordon, LM and Kruska, K (2014) Applicability of post-ionization theory to laser-assisted field evaporation of magnetite. Appl Phys Lett 105(24), 244106.10.1063/1.4904802Google Scholar
Scott, KM (2005) Rutile geochemistry as a guide to porphyry Cu-Au mineralization, Northparkes, New South Wales, Australia. Geochem-Explor Env A 5(3), 247253.10.1144/1467-7873/03-055Google Scholar
Scott, KM and Radford, NW (2007) Rutile compositions at the Big Bell Au deposit as a guide for exploration. Geochem-Explor Env A 7(4), 353361.Google Scholar
Swope, RJ, Smyth, JR and Larson, AC (1995) H in rutile-type compounds: I. Single-crystal neutron and X-ray diffraction study of H in rutile. Am Mineral 80(5–6), 448453.Google Scholar
Thompson, K, Lawrence, D, Larson, DJ, Olson, JD, Kelly, TF and Gorman, B (2007) In situ site-specific specimen preparation for atom probe tomography. Ultramicroscopy 107(2–3), 131139.Google Scholar
Thuvander, M, Kvist, A, Johnson, LJ, Weidow, J and Andrén, H-O (2013) Reduction of multiple hits in atom probe tomography. Ultramicroscopy 132, 8185.10.1016/j.ultramic.2012.12.005Google Scholar
Tomkins, HS, Powell, R and Ellis, DJ (2007) The pressure dependence of the zirconium-in-rutile thermometer. J Metamorph Geol 25(6), 703713.10.1111/j.1525-1314.2007.00724.xGoogle Scholar
Valley, JW, Reinhard, DA, Cavosie, AJ, Ushikubo, T, Lawrence, DF, Larson, DJ, Kelly, TF, Snoeyenbos, DR and Strickland, A (2015) Nano- and micro-geochronology in Hadean and Archean zircons by atom-probe tomography and SIMS: New tools for old minerals. Am Mineral 100(7), 13551377.Google Scholar
Vurpillot, F, Houard, J, Vella, A and Deconihout, B (2009) Thermal response of a field emitter subjected to ultra-fast laser illumination. J Phys D: Appl Phys 42(12), 125502.Google Scholar
Watson, EB, Wark, DA and Thomas, JB (2006) Crystallization thermometers for zircon and rutile. Contrib Mineral Petrol 151(4), 413433.10.1007/s00410-006-0068-5Google Scholar
White, LF, Darling, J, Moser, D, Reinhard, D, Prosa, T, Bullen, D, Olson, D, Larson, D, Lawrence, D and Martin, I (2017) Atomic-scale age resolution of planetary events. Nat Commun 8, 15597.10.1038/ncomms15597Google Scholar
Zack, T, Moraes, R and Kronz, A (2004 a) Temperature dependence of Zr in rutile: Empirical calibration of a rutile thermometer. Contrib Mineral Petrol 148(4), 471488.10.1007/s00410-004-0617-8Google Scholar
Zack, T, Stockli, DF, Luvizotto, GL, Barth, MG, Belousova, E, Wolfe, MR and Hinton, RW (2011) In situ U–Pb rutile dating by LA-ICP-MS: 208Pb correction and prospects for geological applications. Contrib Mineral Petrol 162(3), 515530.Google Scholar
Zack, T, von Eynatten, H and Kronz, A (2004 b) Rutile geochemistry and its potential use in quantitative provenance studies. Sediment Geol 171(1–4), 3758.Google Scholar
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