Hostname: page-component-848d4c4894-wg55d Total loading time: 0 Render date: 2024-06-04T19:59:45.779Z Has data issue: false hasContentIssue false
  • English
  • Français

Correlative Atom Probe Tomography and Transmission Electron Microscopy Analysis of Grain Boundaries in Thermally Grown Alumina Scale

Published online by Cambridge University Press:  04 February 2019

Ivan Povstugar Open the ORCID record for Ivan Povstugar [Opens in a new window] ,
Juliane Weber ,
Dmitry Naumenko ,
Taihong Huang ,
Martina Klinkenberg Open the ORCID record for Martina Klinkenberg [Opens in a new window]  and
Willem J. Quadakkers
Ivan Povstugar*
Affiliation:
Central Institute for Engineering, Electronics and Analytics (ZEA-3) –– Analytics, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
Juliane Weber
Affiliation:
Institute of Energy and Climate Research (IEK-6) –– Nuclear Waste Management and Reactor Safety, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany Chemical Science Division, Oak Ridge National Laboratory, 37831 Oak Ridge, TN, USA
Dmitry Naumenko
Affiliation:
Institute of Energy and Climate Research (IEK-2) –– Microstructure and Properties of Materials, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
Taihong Huang
Affiliation:
Institute of Energy and Climate Research (IEK-2) –– Microstructure and Properties of Materials, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany Faculty of Materials Science and Engineering, Kunming University of Science and Technology, 650093 Kunming, China
Martina Klinkenberg
Affiliation:
Institute of Energy and Climate Research (IEK-6) –– Nuclear Waste Management and Reactor Safety, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
Willem J. Quadakkers
Affiliation:
Institute of Energy and Climate Research (IEK-2) –– Microstructure and Properties of Materials, Forschungszentrum Jülich GmbH, 52425 Jülich, Germany
*
*Author for correspondence: Ivan Povstugar, E-mail: i.povstugar@fz-juelich.de
Get access

Abstract

We employed correlative atom probe tomography (APT) and transmission electron microscopy (TEM) to analyze the alumina scale thermally grown on the oxide dispersion-strengthened alloy MA956. Segregation of Ti and Y and associated variation in metal/oxygen stoichiometry at the grain boundaries and triple junctions of alumina were quantified and discussed with respect to the oxidation behavior of the alloy, in particular, to the formation of cation vacancies. Correlative TEM analysis was helpful to avoid building pragmatically well-looking but substantially incorrect APT reconstructions, which can result in erroneous quantification of segregating species, and highlights the need to consider ionic volumes and detection efficiency in the reconstruction routine. We also demonstrate a cost-efficient, robust, and easy-handling setup for correlative analysis based solely on commercially available components, which can be used with all conventional TEM tools without the need to modify the specimen holder assembly.

Keywords

aluminaatom probe tomographycorrelative microscopythermally grown oxidetransmission electron microscopy
Type
Materials Science Applications
Information
Microscopy and Microanalysis , Volume 25 , Issue 1 , February 2019 , pp. 11 - 20
Copyright
Copyright © Microscopy Society of America 2019 

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

Aguiar, JA, Stokes, A, Jiang, C-S, Aoki, T, Kotula, PG, Patel, MK, Gorman, B & Al-Jassim, M (2016). Revealing surface modifications of potassium-fluoride-treated Cu(In,Ga)Se2: A study of material structure, chemistry, and photovoltaic performance. Adv Mater Interfaces 3, 1600013.Google Scholar
Arslan, I, Marquis, EA, Homer, M, Hekmaty, MA & Bartelt, NC (2008). Towards better 3-D reconstructions by combining electron tomography and atom-probe tomography. Ultramicroscopy 108, 1579–1585.Google Scholar
Baik, S-I, Yin, X & Seidman, DN (2013). Correlative atom-probe tomography and transmission electron microscope study of a chemical transition in a spinel on an oxidized nickel-based superalloy. Scr Mater 68, 909–912.Google Scholar
Bale, CW, Bélisle, E, Chartrand, P, Decterov, SA, Eriksson, G, Gheribi, AE, Hack, K, Jung, I-H, Kang, Y-B, Melançon, J, Pelton, AD, Petersen, S, Robelin, C, Sangster, J, Spencer, P & Van Ende, M-A (2016). Factsage thermochemical software and databases, 2010–2016. Calphad 54, 35–53.Google Scholar
Bas, P, Bostel, A, Deconihout, B & Blavette, D (1995). A general protocol for the reconstruction of 3D atom probe data. Appl Surf Sci 87–88, 298–304.Google Scholar
Birks, N, Meier, GH & Pettit, FS (2006). Introduction to the High-Temperature Oxidation of Metals. Cambridge, UK: Cambridge University Press.Google Scholar
Boll, T, Unocic, KA, Pint, BA & Stiller, K (2017). Interfaces in oxides formed on NiAlCr doped with Y, Hf, Ti, and B. Microsc Microanal 23, 396–403.Google Scholar
Chen, Y, Reed, RC & Marquis, EA (2014). Interfacial solute segregation in the thermally grown oxide of thermal barrier coating structures. Oxid Met 82, 457–467.Google Scholar
Chen, Y, Rice, KP, Prosa, TJ, Marquis, EA & Reed, RC (2015). Integrated APT/t-EBSD for grain boundary analysis of thermally grown oxide on a Ni-based superalloy. Microsc Microanal 21, 687–688.Google Scholar
Chen, YM, Ohkubo, T, Kodzuka, M, Morita, K & Hono, K (2009). Laser-assisted atom probe analysis of zirconia/spinel nanocomposite ceramics. Scr Mater 61, 693–696.Google Scholar
Clemens, D, Bongartz, K, Speier, W, Hussey, RJ & Quadakkers, WJ (1993). Analysis and modelling of transport processes in alumina scales on high temperature alloys. Fresenius J Anal Chem 346, 318–322.Google Scholar
Cojocaru-Mirédin, O, Schwarz, T & Abou-Ras, D (2018). Assessment of elemental distributions at line and planar defects in Cu(In,Ga)Se2 thin films by atom probe tomography. Scr Mater 148, 106–114.Google Scholar
Devaraj, A, Colby, R, Hess, WP, Perea, DE & Thevuthasan, S (2013). Role of photoexcitation and field ionization in the measurement of accurate oxide stoichiometry by Laser-assisted atom probe tomography. J Phys Chem Lett 4, 993–998.Google Scholar
Diercks, DR, Gorman, BP, Manerbino, A & Coors, G (2014). Atom probe tomography of yttrium-doped barium-cerium-zirconium oxide with NiO addition Salvador, P. (Ed.). J Am Ceram Soc 97, 3301–3306.Google Scholar
Diercks, DR, Tong, J, Zhu, H, Kee, R, Baure, G, Nino, JC, O'Hayre, R & Gorman, BP (2016). Three-dimensional quantification of composition and electrostatic potential at individual grain boundaries in doped ceria. J Mater Chem A 4, 5167–5175.Google Scholar
Felfer, P & Cairney, J (2011). New equipment for correlative FIB/TEM/atom probe and site-specific preparation using STEM live imaging. Microsc Microanal 17, 756–757.Google Scholar
Gault, B, de Geuser, F, Stephenson, LT, Moody, MP, Muddle, BC & Ringer, SP (2008). Estimation of the reconstruction parameters for atom probe tomography. Microsc Microanal 14, 296–305.Google Scholar
Gault, B, Loi, ST, Araullo-Peters, VJ, Stephenson, LT, Moody, MP, Shrestha, SL, Marceau, RKW, Yao, L, Cairney, JM & Ringer, SP (2011). Dynamic reconstruction for atom probe tomography. Ultramicroscopy 111, 1619–1624.Google Scholar
Gorman, BP, Diercks, DR, Salmon, D, Stach, E, Amador, G & Hartfield, C (2008a). Hardware and techniques for cross-correlative TEM and atom probe analysis. Micros Today 16, 42–47.Google Scholar
Gorman, BP, Puthucode, A, Diercks, DR & Kaufman, MJ (2008b). Cross-correlative TEM and atom probe analysis of partial crystallisation in NiNbSn metallic glasses. Mater Sci Technol 24, 682–688.Google Scholar
Gülgün, MA, Voytovych, R, Maclaren, I, Rühle, M & Cannon, RM (2002). Cation segregation in an oxide ceramic with low solubility: Yttrium doped α-alumina. Interface Sci 10, 99–110.Google Scholar
Hellman, OC & Seidman, DN (2002). Measurement of the Gibbsian interfacial excess of solute at an interface of arbitrary geometry using three-dimensional atom probe microscopy. Mater Sci Eng A 327, 24–28.Google Scholar
Herbig, M, Choi, P & Raabe, D (2015). Combining structural and chemical information at the nanometer scale by correlative transmission electron microscopy and atom probe tomography. Ultramicroscopy 153, 32–39.Google Scholar
Herbig, M, Raabe, D, Li, YJ, Choi, P, Zaefferer, S & Goto, S (2014). Atomic-scale quantification of grain boundary segregation in nanocrystalline material. Phys Rev Lett 112, 126103.Google Scholar
Huang, T, Naumenko, D, Song, P, Lu, J & Quadakkers, WJ (2018). Effect of Titanium addition on alumina growth mechanism on yttria-containing FeCrAl-base alloy. Oxid Met 90, 671–690.Google Scholar
Huczkowski, P, Gopalakrishnan, SG, Nowak, W, Hattendorf, H, Iskandar, R, Mayer, J & Quadakkers, WJ (2016). Effect of Zr content on the morphology and emissivity of surface oxide scales on FeCrAlY alloys. Adv Eng Mater 18, 711–720.Google Scholar
Karahka, M, Xia, Y & Kreuzer, HJ (2015). The mystery of missing species in atom probe tomography of composite materials. Appl Phys Lett 107, 062105.Google Scholar
Kim, J-H, Kim, BK, Kim, D-I, Choi, P-P, Raabe, D & Yi, K-W (2015). The role of grain boundaries in the initial oxidation behavior of austenitic stainless steel containing alloyed Cu at 700°C for advanced thermal power plant applications. Corros Sci 96, 52–66.Google Scholar
Kirchhofer, R, Diercks, DR & Gorman, BP (2015). Near atomic scale quantification of a diffusive phase transformation in (Zn, Mg)O/Al2O3 using dynamic atom probe tomography. J Mater Res 30, 1137–1147.10.1557/jmr.2015.86Google Scholar
Kontis, P, Pedrazzini, S, Gong, Y, Bagot, PAJ, Moody, MP & Reed, RC (2017). The effect of boron on oxide scale formation in a new polycrystalline superalloy. Scr Mater 127, 156–159.Google Scholar
La Fontaine, A, Yen, H-W, Felfer, PJ, Ringer, SP & Cairney, JM (2015). Atom probe study of chromium oxide spinels formed during intergranular corrosion. Scr Mater 99, 1–4.Google Scholar
Larson, DJ, Prosa, TJ, Ulfig, RM, Geiser, BP & Kelly, TF (2013). Local Electrode Atom Probe Tomography. New York, US: Springer New York.Google Scholar
Loi, ST, Gault, B, Ringer, SP, Larson, DJ & Geiser, BP (2013). Electrostatic simulations of a local electrode atom probe: The dependence of tomographic reconstruction parameters on specimen and microscope geometry. Ultramicroscopy 132, 107–113.Google Scholar
London, AJ, Lozano-Perez, S, Moody, MP, Amirthapandian, S, Panigrahi, BK, Sundar, CS & Grovenor, CRM (2015). Quantification of oxide particle composition in model oxide dispersion strengthened steel alloys. Ultramicroscopy 159, 360–367.Google Scholar
Marquis, EA, Yahya, NA, Larson, DJ, Miller, MK & Todd, RI (2010). Probing the improbable: imaging C atoms in alumina. Mater Today 13, 34–36.Google Scholar
Maugis, P & Hoummada, K (2016). A methodology for the measurement of the interfacial excess of solute at a grain boundary. Scr Mater 120, 90–93.Google Scholar
Miller, MK & Hetherington, MG (1991). Local magnification effects in the atom probe. Surf Sci 246, 442–449.Google Scholar
N'Dah, E, Galerie, A, Wouters, Y, Goossens, D, Naumenko, D, Kochubey, V & Quadakkers, WJ (2005). Metastable alumina formation during oxidation of FeCrAl and its suppression by surface treatments. Mater Corros 56, 843–847.Google Scholar
Naumenko, D, Gleeson, B, Wessel, E, Singheiser, L & Quadakkers, WJ (2007). Correlation between the microstructure, growth mechanism, and growth kinetics of alumina scales on a FeCrAlY alloy. Metall Mater Trans A 38, 2974–2983.Google Scholar
Nguyen, TD, La Fontaine, A, Yang, L, Cairney, JM, Zhang, J & Young, DJ (2018). Atom probe study of impurity segregation at grain boundaries in chromia scales grown in CO 2 gas. Corros Sci 132, 125–135.Google Scholar
Nychka, JA & Clarke, DR (2005). Quantification of aluminum outward diffusion during oxidation of FeCrAl alloys. Oxid Met 63, 325–352.Google Scholar
Pedrazzini, S, Child, DJ, West, G, Doak, SS, Hardy, MC, Moody, MP & Bagot, PAJ (2016). Oxidation behaviour of a next generation polycrystalline Mn containing Ni-based superalloy. Scr Mater 113, 51–54.Google Scholar
Perea, DE, Arslan, I, Liu, J, Ristanović, Z, Kovarik, L, Arey, BW, Lercher, JA, Bare, SR & Weckhuysen, BM (2015). Determining the location and nearest neighbours of aluminium in zeolites with atom probe tomography. Nat Commun 6, 7589.Google Scholar
Pint, BA (1996). Experimental observations in support of the dynamic-segregation theory to explain the reactive-element effect. Oxid Met 45, 1–37.Google Scholar
Pint, BA (1997). On the formation of interfacial and internal voids in α-Al2O3 scales. Oxid Met 48, 303–328.Google Scholar
Pint, BA (2003). Optimization of reactive-element additions to improve oxidation performance of alumina-forming alloys. J Am Ceram Soc 86, 686–695.Google Scholar
Pint, BA, Garratt-Reed, AJ & Hobbs, LW (1995). The reactive element effect in commercial ODS FeCrAl alloys. Mater High Temp 13, 3–16.Google Scholar
Quadakkers, WJ, Elschner, A, Holzbrecher, H, Schmidt, K, Speier, W & Nickel, H (1992). Analysis of composition and growth mechanisms of oxide scales on high temperature alloys by SNMS, SIMS, and RBS. Mikrochim Acta 107, 197–206.Google Scholar
Quadakkers, WJ, Holzbrecher, H, Briefs, KG & Beske, H (1989). Differences in growth mechanisms of oxide scales formed on ODS and conventional wrought alloys. Oxid Met 32, 67–88.Google Scholar
Schreiber, DK, Olszta, MJ & Bruemmer, SM (2013). Directly correlated transmission electron microscopy and atom probe tomography of grain boundary oxidation in a Ni-Al binary alloy exposed to high-temperature water. Scr Mater 69, 509–512.Google Scholar
Stiller, K, Viskari, L, Sundell, G, Liu, F, Thuvander, M, Andrén, H-O, Larson, DJ, Prosa, T & Reinhard, D (2013). Atom probe tomography of oxide scales. Oxid Met 79, 227–238.Google Scholar
Sundell, G, Thuvander, M & Andrén, H-O (2012). Enrichment of Fe and Ni at metal and oxide grain boundaries in corroded Zircaloy-2. Corros Sci 65, 10–12.Google Scholar
Thompson, K, Lawrence, D, Larson, DJ, Olson, JD, Kelly, TF & Gorman, B (2007). In situ site-specific specimen preparation for atom probe tomography. Ultramicroscopy 107, 131–139.Google Scholar
Toji, Y, Matsuda, H, Herbig, M, Choi, P-P & Raabe, D (2014). Atomic-scale analysis of carbon partitioning between martensite and austenite by atom probe tomography and correlative transmission electron microscopy. Acta Mater 65, 215–228.Google Scholar
Unocic, KA, Chen, Y, Shin, D, Pint, BA & Marquis, EA (2018). STEM and APT characterization of scale formation on a La,Hf,Ti-doped NiCrAl model alloy. Micron 109, 41–52.Google Scholar
Unocic, KA, Essuman, E, Dryepondt, S & Pint, BA (2012). Effect of environment on the scale formed on oxide dispersion strengthened FeCrAl at 1050°C and 1100°C. Mater High Temp 29, 171–180.Google Scholar
Yang, JC, Nadarzinski, K, Schumann, E & Rühle, M (1995). Electron microscopy studies of NiAl/γ-Al2O3 interfaces. Scr Metall Mater 33, 1043–1048.Google Scholar
Young, DJ (2016). High Temperature Oxidation and Corrosion of Metals. Amsterdam, Netherlands: Elsevier.Google Scholar
Young, DJ, Naumenko, D, Niewolak, L, Wessel, E, Singheiser, L & Quadakkers, WJ (2010). Oxidation kinetics of Y-doped FeCrAl-alloys in low and high pO2 gases. Mater Corros 61, 838–844.Google Scholar
Zanuttini, D, Blum, I, Rigutti, L, Vurpillot, F, Douady, J, Jacquet, E, Anglade, P-M & Gervais, B (2017). Simulation of field-induced molecular dissociation in atom-probe tomography: Identification of a neutral emission channel. Phys Rev A 95, 061401.Google Scholar
Zhou, X, Yu, X, Kaub, T, Martens, RL & Thompson, GB (2016). Grain boundary specific segregation in nanocrystalline Fe(Cr). Sci Rep 6, 34642.Google Scholar