Abstract
Advanced electron microscopy and surface science techniques were applied to characterize inter- and intragranular oxidation in Ni–Fe–Cr alloys after exposure to 480 °C hydrogenated steam. Intragranular internal Fe and Cr oxidation was observed in all cases while intergranular oxidation, exclusively external or penetrative, varied depending on the Cr content of the alloy. The kinetics and morphology of intragranular internal oxidation and nodule growth were studied through successive short-term exposures with characterization performed between exposures. FIB 3D serial sectioning was used to reconstruct volumes containing oxidized grain boundaries and revealed that diffusion-induced grain boundary migration may play a fundamental role in increasing the outward flux of Cr, Ti, and Al near grain boundaries, depending on the extent of intergranular Cr carbide precipitation. In addition, atom probe tomography was used to study the behaviour of minor impurity elements, Al and Ti, and initial oxidation processes. Further analyses of oxidized samples using three-dimensional ToF-SIMS are also discussed.
This is a preview of subscription content, log in via an institution.
Buying options
Tax calculation will be finalised at checkout
Purchases are for personal use only
Learn about institutional subscriptionsReferences
S. Lozano-Perez, J.M. Titchmarsh, TEM investigations of intergranular stress corrosion cracking in austenitic alloys in PWR environmental conditions. Mater. High Temp. 20(4), 573–579 (2003)
S. Lozano-Perez, P. Rodrigo, L.C. Gontard, Three-dimensional characterization of stress corrosion cracks. J. Nucl. Mater. 408(3), 289–295 (2011)
L.E. Thomas, S.M. Bruemmer, High-resolution characterization of intergranular attack and stress corrosion cracking of alloy 600 in high-temperature primary water. Corrosion 56(6), 572–587 (2000)
S.M. Bruemmer, L.E. Thomas, High-resolution analytical electron microscopy characterization of corrosion and cracking at buried interfaces. Surf. Interface Anal. 31(7), 571–581 (2001)
J. Panter, B. Viguier, J.M. Cloué, M. Foucault, P. Combrade, E. Andrieu, Influence of oxide films on primary water stress corrosion cracking initiation of alloy 600. J. Nucl. Mater. 348(1–2), 213–221 (2006)
M. Sennour, P. Laghoutaris, C. Guerre, R. Molins, Advanced TEM characterization of stress corrosion cracking of alloy 600 in pressurized water reactor primary water environment. J. Nucl. Mater. 393(2), 254–266 (2009)
G.A. Young, W.W. Wilkening, D.S. Morton, E. Richey, N. Lewis, The mechanism and modeling of intergranular stress corrosion cracking of nickel-chromium-iron alloys exposed to high purity water, in Proceedings of the 12th International Conference on Environmental Degradation of Materials in Nuclear Power Systems—Water Reactors, ed. T.R. Allen, P.J. King, L. Nelson (The Minerals, Metals & Materials Society (TMS), Salt Lake City, UT, 2005), pp. 913–924
P.M. Scott, M. Le Calvar, Some possible mechanisms of intergranular stress corrosion cracking of alloy 600 in PWR primary water, in Proceedings of the 6th International Conference on Environmental Degradation of Materials in Nuclear Power Systems—Water Reactors, ed by E.P. Simonen (The Minerals, Metals, and Materials Society (TMS), San Diego, CA, 1993), pp. 657–665
H.-B. Park, Y.-H. Kim, B.-W. Lee, K.-S. Rheem, Effect of heat treatment on fatigue crack growth of Inconel 690 and Inconel 600. J. Nucl. Mater. 231(3), 204–212 (1996)
G.S. Was, J.K. Sung, T.M. Angeliu, Effects of grain boundary chemistry on the intergranular cracking behaviour of Ni-16Cr-9Fe in high-temperature water. Metall. Trans. A 23A(1), 3343–3359 (1992)
G.P. Airey, Microstructural aspects of the thermal treatment of Inconel alloy 600. Metallography 13(1), 21–41 (1980)
S.M. Bruemmer, G.S. Was, Microstructural and microchemical mechanisms controlling intergranular stress corrosion cracking in light-water-reactor systems. J. Nucl. Mater. 216, 348–363 (1994)
T.S. Gendron, S.J. Bushby, R.D. Cleland, R.C. Newman, Oxidation embrittlement of alloy 600 in hydrogenated steam at 400 °C, in Proceedings of the Second International Conference on Corrosion Deformation Interactions CDI ‘96 in Conjunction with EUROCORR ‘96 (The Institute of Materials, Nice, France, 1997) pp. 484–495
T.S. Gendron, S.J. Bushby, R.D. Cleland, R.C. Newman, Oxidation embrittlement of alloy 600 in hydrogenated steam at 400 °C. Analusis Mag. 25, 24–28 (1997)
S.M. Bruemmer, M.J. Olszta, M.B. Toloczko, L.E. Thomas, Linking grain boundary microstructure to stress corrosion cracking of cold-rolled alloy 690 in pressurized water reactor primary water. Corrosion 69(10), 953–963 (2013)
Q.J. Peng, J. Hou, T. Yonezawa, T. Shoji, Z.M. Zhang, F. Huang, E.H. Han, W. Ke, Environmentally assisted crack growth in one-dimensionally cold worked alloy 690TT in primary water. Corros. Sci. 57, 81–88 (2012)
B. Langelier, S.Y. Persaud, R.C. Newman, G.A. Botton, An atom probe tomography study of internal oxidation processes in alloy 600. Acta Mater. 109, 55–68 (2016)
S.Y. Persaud, A. Korinek, J. Huang, G.A. Botton, R.C. Newman, Internal oxidation of alloy 600 exposed to hydrogenated steam and the beneficial effects of thermal treatment. Corros. Sci. 86, 108–122 (2014)
S.Y. Persaud, J. Smith, A. Korinek, G.A. Botton, R.C. Newman, High resolution analysis of oxidation in Ni–Fe–Cr alloys after exposure to 315 °C deaerated water with added hydrogen. Corros. Sci. 106, 236–248 (2016)
B.M. Capell, G.S. Was, Selective internal oxidation as a mechanism for intergranular stress corrosion cracking of Ni–Cr–Fe alloys. Metall. Mater. Trans. A 38(6), 1244–1259 (2007)
D.K. Schreiber, M.J. Olszta, D.W. Saxey, K. Kruska, K.L. Moore, S. Lozano-Perez, S.M. Bruemmer, Examinations of oxidation and sulfidation of grain boundaries in alloy 600 exposed to simulated pressurized water reactor primary water. Microsc. Microanal. 19(3), 676–687 (2013)
G. Bertali, F. Scenini, M.G. Burke, Advanced microstructural characterization of the intergranular oxidation of alloy 600. Corros. Sci. 100, 474–483 (2015)
G. Bertali, F. Scenini, M.G. Burke, The intergranular oxidation susceptibility of thermally-treated alloy 600. Corros. Sci. 114, 112–122 (2017)
R.C. Newman, F. Scenini, Another way to think about the critical oxide volume fraction for the internal-to-external oxidation transition? Corrosion 64(9), 721–726 (2008)
F. Scenini, R.C. Newman, R.A. Cottosi, R.J. Jacko, Alloy oxidation studies related to PWSCC, in Proceedings of the 12th International Conference on Environmental Degradation of Materials in Nuclear Power Systems—Water Reactors, ed. by T.R. Allen, P.J. King, L. Nelson (The Minerals, Metals & Materials Society (TMS), Salt Lake City, UT, 2005), pp. 891–902
F. Scenini, R.C. Newman, R.A. Cottis, R.J. Jacko, Effect of surface preparation on intergranular stress corrosion cracking of alloy 600 in hydrogenated steam. Corrosion 64(11), 824–835 (2008)
G. Bertali, F. Scenini, M.G. Burke, The effect of residual stress on the preferential intergranular oxidation of alloy 600. Corros. Sci. 111, 494–507 (2016)
P. Laghoutaris, J. Chêne, C. Guerre, O. Raquet, M. Sennour, R. Molins, F. Vaillant, P. Scott, Contribution to understanding of stress corrosion cracking of alloy 600 in PWR primary water. Energy Mater. 3(2), 119–125 (2013)
X. Li, J. Wang, E.-H. Han, W. Ke, Corrosion behavior for alloy 690 and alloy 800 tubes in simulated primary water. Corros. Sci. 67, 169–178 (2013)
P.M. Scott, An overview of internal oxidation as a possible explanation of intergranular stress corrosion cracking of alloy 600 in PWRs, in Proceedings of the 9th International Conference on Environmental Degradation of Materials in Nuclear Power Systems - Water Reactors, ed. by F.P. Ford, S.M. Bruemmer, G.S. Was (The Minerals, Metals & Materials Society (TMS), Newport Beach, CA, 1999), pp. 3–14
B. Langelier, S.Y. Persaud, A. Korinek, T. Casagrande, R.C. Newman, G.A. Botton, Effects of boundary migration and pinning particles on intergranular oxidation revealed by 2D and 3D analytical electron microscopy. Acta Mater. 131, 280–295 (2017)
S.Y. Persaud, B. Langelier, A. Korinek, S. Ramamurthy, G.A. Botton, R.C. Newman, Characterization of initial intergranular oxidation processes in alloy 600 at a sub-nanometer scale (2017) (manuscript submitted for publication)
J.R. Mackert, R.D. Ringle, C.W. Fairhurst, High-temperature behavior of a Pd–Ag alloy for porcelain. J. Dent. Res. 62(12), 1229–1235 (1983)
R.A. Rapp, The transition from internal to external oxidation and the formation of interruption bands in silver-indium alloys. Acta Metall. 9(8), 730–741 (1961)
S. Guruswamy, S.M. Park, J.P. Hirth, R.A. Rapp, Internal oxidation of Ag–In alloys: stress relief and the influence of imposed strain. Oxid. Met. 26(1), 77–100 (1986)
F.H. Stott, Y. Shida, D.P. Whittle, G.C. Wood, B.D. Bastow, The morphological and structural development of internal oxides in nickel–aluminum alloys at high temperatures. Oxid. Met. 18(3), 127–146 (1982)
G.C. Wood, F.H. Stott, D.P. Whittle, Y. Shida, B.D. Bastow, The high-temperature internal oxidation and intergranular oxidation of nickel-chromium alloys. Corros. Sci. 23(1), 9–25 (1983)
H.C. Yi, S.W. Guan, W.W. Smeltzer, A. Petric, Internal oxidation of Ni–Al and Ni–Al–Si alloys at the dissociation pressure of NiO. Acta Metall. Mater. 42(3), 981–990 (1994)
S.Y. Persaud, S. Ramamurthy, R.C. Newman, Internal oxidation of alloy 690 in hydrogenated steam. Corros. Sci. 90, 606–613 (2015)
M.J. Olszta, D.K. Schreiber, M.B. Toloczko, S.M. Bruemmer, Alloy 690 surface nanostructures during exposure to PWR primary water and potential influence on stress corrosion crack initiation, in Proceedings of the 16th International Conference on Environmental Degradation of Materials in Nuclear Power Systems—Water Reactors, ed. by P.L. Andresen, M.D. Wright, G.O. Ilevbare (NACE International, Omnipress, Asheville, NC, 2013)
G. Economy, R.J. Jacko, F.W. Perment, IGSCC behaviour of alloy 600 steam generator tubing in water or steam tests above 360 °C. Corrosion 43(12), 727–734 (1987)
G.S. Was, H.H. Tischner, R.M. Latanision, The influence of thermal treatment on the chemistry and structure of grain boundaries in Inconel 600. Metall. Trans. A 12A(8), 1397–1408 (1981)
K. Thompson, D. Lawrence, D.J. Larson, J.D. Olson, T.F. Kelly, B. Gorman, In situ site-specific specimen preparation for atom probe tomography. Ultramicroscopy 107(2–3), 131–139 (2007)
B. Gault, M.P. Moody, J.M. Cairney, S.P. Ringer, Atom Probe Microscopy (Springer Science, New York, 2012)
K. Narayan, C.M. Danielson, K. Lagarec, B.C. Lowekamp, P. Coffman, A. Laquerre, M.W. Phaneuf, T.J. Hope, S. Subramaniam, Multi-resolution correlative focused ion beam scanning electron microscopy: applications to cell biology. J. Struct. Biol. 185(3), 278–284 (2014)
J.W. Cahn, J.D. Pan, R.W. Balluffi, Diffusion induced grain boundary migration. Scr. Metall. 13(6), 503–509 (1979)
J.W. Cahn, R.W. Balluffi, On diffusional mass transport in polycrystals containing stationary or migrating boundaries. Scr. Metall. 13(6), 499–502 (1979)
M. Hillert, G.R. Purdy, Chemically induced grain boundary migration. Acta Metall. 26(2), 333–340 (1978)
R.W. Balluffi, J.W. Cahn, Mechanism for diffusion induced grain boundary migration. Acta Metall. 29(3), 493–500 (1981)
H. Aaron, H.I. Aaronson, Growth of grain boundary precipitates in Al–4%Cu by interfacial diffusion. Acta Metall. 16(6), 789–798 (1968)
D.K. Schreiber, M.J. Olszta, S.M. Bruemmer, Grain boundary depletion and migration during selective oxidation of Cr in a Ni–5Cr binary alloy exposed to high-temperature hydrogenated water. Scr. Mater. 89, 41–44 (2014)
D.K. Schreiber, M.J. Olszta, L.E. Thomas, S.M. Bruemmer, Grain boundary characterization of alloy 600 prior to and after corrosion by atom probe tomography and transmission electron microscopy, in Proceedings of the 16th International Conference on Environmental Degradation of Materials in Nuclear Power Systems—Water Reactors, ed. by P.L. Andresen, M.D. Wright, G.O. Ilevbare (NACE International, Omnipress, Asheville, NC, 2013)
D.K. Schreiber, M.J. Olszta, S.M. Bruemmer, 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(7), 509–512 (2013)
C.M. Wang, D.K. Schreiber, M.J. Olszta, D.R. Baer, S.M. Bruemmer, Direct in situ TEM observation of modification of oxidation by the injected vacancies for Ni–4Al alloy using a microfabricated nanopost. Appl. Mater. Interfaces 7(31), 17272–17277 (2015)
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2019 The Minerals, Metals & Materials Society
About this paper
Cite this paper
Persaud, S.Y., Langelier, B., Eskandari, A., Zhu, H., Botton, G.A., Newman, R.C. (2019). Advanced Characterization of Oxidation Processes and Grain Boundary Migration in Ni Alloys Exposed to 480 °C Hydrogenated Steam. In: Jackson, J., Paraventi, D., Wright, M. (eds) Proceedings of the 18th International Conference on Environmental Degradation of Materials in Nuclear Power Systems – Water Reactors. The Minerals, Metals & Materials Series. Springer, Cham. https://doi.org/10.1007/978-3-030-04639-2_24
Download citation
DOI: https://doi.org/10.1007/978-3-030-04639-2_24
Published:
Publisher Name: Springer, Cham
Print ISBN: 978-3-030-04638-5
Online ISBN: 978-3-030-04639-2
eBook Packages: Chemistry and Materials ScienceChemistry and Material Science (R0)