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Steel Corrosion and Actinide Sorption by Iron Corrosion Products Under Saline Conditions

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Steel Corrosion and Actinide Sorption by Iron Corrosion Products Under Saline Conditions Institute for Nuclear Waste Disposal Steel corrosion and actinide sorption by iron corrosion products under saline conditions. Zur Erlangung des akademischen Grades einer DOKTORIN DER NATURWISSENSCHAFTEN (Dr. rer. nat.) von der KIT-Fakultät für Chemie und Biowissenschaften des Karlsruher Instituts für Technologie (KIT) genehmigte DISSERTATION von Nikoleta Morelová aus Bratislava, Slowakei Dekan: Prof. Dr. Manfred Wilhelm Referent: Prof. Dr. Horst Geckeis Korreferent: Prof. Dr. Thorsten Schäfer Tag der mündlichen Prüfung: 20.07.2020 Declaration of Originality Ich versichere hiermit die vorliegende Arbeit selbstständig verfasst zu haben und keine anderen Quellen oder Hilfsmittel verwendet zu haben als die hier angegebenen. Außerdem versichere ich, dass alle Stellen der Arbeit, die aus anderen Quellen wörtlich oder sinngemäß übernommen wurden, als solche kenntlich gemacht worden sind und die schriftliche Version der Arbeit mit der digitalen übereinstimmt. Die Arbeit wurde in gleicher oder ähnlicher Form noch bei keiner anderen Prüfungsbehörde vorgelegt. Die Satzung des Karlsruher Instituts für Technologie zur Sicherung guter wissenschaftlicher Praxis wurde in der jeweils gültigen Fassung beachtet. Acknowledgments This PhD work was performed at Institute for Nuclear Waste Disposal (INE) of the Karlsruhe Institute of Technology (KIT). I would like to express my gratitude to Prof. Horst Geckeis for giving me the opportunity to perform my PhD at his institute and for offering his supervision after I have unexpectedly changed faculty. I have gathered a lot of valuable scientific experience and was given a chance to contribute to high-level scientific research. I would also like to thank Dr. Marcus Altmaier, head of the Radiochemistry Division at INE, which I was part of. I am grateful for his positive attitude, guidance and many fruitful scientific discussions. I especially would like to express my gratitude to my direct supervisor, Dr. Nicolas Finck for always finding time for my questions, ideas and discussions, and for his endless support when I was doubting myself. I feel very lucky and honoured to be supervised by such great scientist and kind person. I am also delighted to thank Dr. Johannes Lützenkirchen for his guidance, lot of dedicated time and sharing his knowledge on surface complexation modelling. I would like to thank my colleagues, Dr. Dieter Schild for SEM, XPS measurements, Ms. Eva Soballa for SEM measurements, Mr. Frank Geyer for ICP-MS measurements, Ms. Stephanie Kraft for AFM and ICP- OES measurements, Ms. Tanja Kissely for BET measurements, Ms. Elke Bohnert for MS measurements and KIT-INE beamline scientists Dr. Jorg Rothe and Kathy Dardenne for XAS measurements at INE beamline for actinide research. I would like to acknowledge the Soleil synchrotron and thank DIFFABS beamline scientist Solenn Réguer for assistance with XAS, XRD and XRF measurements and help with XRD data evaluation. I would like to thank Dr. Michel Schlegel for his assistance with steel samples preparation for synchrotron measurements and his guidance in corrosion science. I am very grateful to the Radioprotection group at INE, especially Mr. Gerhard Christill for helping me with samples transfers, many lovely chats and his endless optimism. I would also like to thank the Workshop group, especially Mr. Volker Krepper for always managing to fulfil my demands for equipment construction and endless samples cutting. i I would like to thank the members of my Secondary Phases group, Tim and Pelin for their support, knowledge sharing and optimism. I would like to thank my student Eleanor, who has helped me with sorption experiments during her Internship stay. I am very grateful to my girlfriends, Alexandra, Emi and Sohae for their patience and never ending support whenever I needed it. A huge thank you goes to my dear parents, Milan and Naďa, and my lovely sister Natália for their endless support and understanding during stressful periods. The biggest thank you goes to my amazing husband Sylvain for his limitless love and patience. He never stopped taking care of me, supported me and trusted in me when times were difficult, which kept me going. This work has been supported within the framework of KORSO project, funded by the German Federal Ministry of Economic Affairs and Energy (BMWi) under contract no. 02 E 11496 B. ii Abstract In deep geological repositories for nuclear waste disposal, the canister of the spent fuel or vitrified waste provides temporarily a barrier against radionuclide migration from the repository near-field. Some countries consider salt rock as potential host rock for a nuclear waste disposal repository, among those Germany and the US. In case of unlikely but possible groundwater intrusion, the conditions in this repository type are expected to evolve into reducing and mildly alkaline with groundwater containing high salt content. Corrosion rates determine the integrity of the container. In turn, secondary corrosion phases form, which may contribute to the retention of radionuclides. The role of such secondary corrosion phases is widely unexplored. The first part of this PhD thesis addresses the corrosion behaviour of the two different materials used for spent fuel canister and vitrified waste canister under conditions relevant for the repository in salt rock, with a focus laid on the examination of corrosion rates and corrosion mechanisms. The stainless steel 309S (Cr-Ni steel) used to construct coquilles containing vitrified waste and the spheroidal graphite iron GGG 40.3 (SGI), one constituent of the POLLUX container for heat generating high-level radioactive waste in Germany, were corroded under anoxic conditions in dilute to concentrated NaCl and MgCl2 brines in the presence and absence of sulfate at room and at elevated temperature (90 °C) for various exposure times. The corrosion rate was estimated for these systems, allowing better predictions of the integrity of the canister under repository conditions. The corrosion rates for the SGI in 5 M NaCl brine were found 1.22±0.05 µm/a at 90 °C and 1.11±0.05 µm/a at room temperature, considering 42 weeks and 49 weeks exposure time, respectively. For the 5 M NaCl brine in the presence of accessory components (e.g. K+, 2+ 2- Ca , SO4 ) representing realistic brine composition, the corrosion rates were 9.6±1.0 µm/a at 90 °C and 0.79±0.05 µm/a at room temperature considering 26 weeks exposure time. In the dilute brines at 90 °C (0.1 M NaCl and 0.033 M MgCl2), the corrosion rate was found 10.0±1.0 µm/a for both brine types. The corrosion rates for the SGI in 3.4 M MgCl2 based brines were substantially higher, 16.9±1.5 µm/a after 42 weeks and 26.3±1.5 µm/a after 26 weeks at 90 °C in the absence and presence of sulfate respectively. For the room temperature, the corrosion rate in the 3.4 M MgCl2 brine without sulfate presence was found similar to NaCl brine, 1.22±0.05 µm/a after 49 weeks. For the same system with the sulfate presence, the iii corrosion rate was found 3.65±0.05 µm/a after 26 weeks. For the systems, in which the corrosion rate evolution with time was followed, the corrosion rate has decreased with increasing time due to precipitates passivating the steel and hindering iron oxidation. The observed corrosion rates can be clearly related to the measured pHM values, with higher rates corresponding to lower pHM. Furthermore, the MgCl2 based concentrated brines at elevated temperature showed significantly higher corrosion rates compared to NaCl concentrated brines. The corrosion rates obtained for the Cr-Ni steel are very low, <0.1 µm/a for almost all systems. Two systems run at 90 °C, showed slightly higher corrosion rates of 0.49±0.05 µm/a for the 5 M NaCl system with sulfate and 0.44±0.05 µm/a for 3.4 M MgCl2 system with sulfate, respectively. For this steel type, no considerable effect of brine or temperature on corrosion rate has been observed. The solid phase characterization allowed identifying the nature of the formed corrosion products, while the pH, 퐸ℎ evolution and analysis of metal ions in the aqueous phase allowed setting up a preliminary thermodynamic model, which could predict the long-term stability of corrosion products and thus their relevance as potential radionuclide sorbents in the context of waste disposal. A corrosion mechanism was subsequently derived for the two steel types in various brines. A part of this study was performed at the synchrotron light source SOLEIL (Saint-Aubin, France), allowing the application of spectroscopic techniques with high spatial resolution (µXRF, µXAS, µXRD) for detailed characterisation of the corrosion front. For SGI, the presence of the corrosion product magnetite was verified in dilute to concentrated NaCl brines at elevated under mildly alkaline (pHM 9.0) and reducing conditions (퐸ℎ of -210 mV). The thermodynamic model suggests stability of this phase under strongly reducing conditions (퐸ℎ ~ -400 mV), thus its formation hints at locally different environments and the role of kinetic effects on solid phase formation. Other corrosion phases were identified, such as silicate phase cronstedtite, co-present with magnetite in dilute NaCl and MgCl2 systems to concentrated NaCl systems in the absence and presence of sulfate at elevated temperature. Additionally, iron(II) hydroxychloride was found at the bulk steel/corrosion layer interface by the techniques with high spatial resolution for concentrated NaCl brine at elevated temperature. This phase, along with cronstedtite, is not relevant as potential radionuclide sorbent in the NaCl systems due to its lower stability compared to magnetite. The presence of green rust chloride was also established in concentrated NaCl brine at room temperature for this steel type as an intermediate iron corrosion product, which likely transforms into magnetite. iv Similarly, the presence of iron(II) hydroxychloride was established in the concentrated MgCl2 brine at room and elevated temperature in the absence of sulfate and at elevated temperature in the presence of sulfate in the pHM range of 6.6-8.6 and reducing conditions with 퐸ℎ of -110 to -300 mV as a dominant corrosion product.
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