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Dissolution Behaviour of Innovative Inert Matrix Fuels for Recycling of Minor Actinides

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Dissolution Behaviour of Innovative Inert Matrix Fuels for Recycling of Minor Actinides Dissolution Behaviour of Innovative Inert Matrix Fuels Energie & Umwelt Energie for Recycling of Minor Actinides Energy & Environment Energy Elena Laura Mühr-Ebert 378 Dissolution Behaviour of Inert Matrix Fuels of InertDissolution Behaviour Fuels Matrix Member of the Helmholtz Association Member of the Elena Laura Mühr-Ebert Energie & Umwelt / Energie & Umwelt / Energy & Environment Energy & Environment Band/ Volume 378 Band/ Volume 378 ISBN 978-3-95806-238-2 ISBN 978-3-95806-238-2 Dissolution Behaviour of Innovative Inert Matrix Fuels for Recycling of Minor Actinides Von der Fakultät für Georessourcen und Materialtechnik der Rheinisch-Westfälischen Technischen Hochschule Aachen zur Erlangung des akademischen Grades eines Doktors der Naturwissenschaften genehmigte Dissertation vorgelegt von Dipl.-Chem. Elena Laura Mühr-Ebert Berichter: Univ.-Prof. Dr. rer. nat. Dirk Bosbach Univ.-Prof. Dr. rer. nat. Rainer Telle Tag der mündlichen Prüfung: 16. Februar 2017 Diese Dissertation ist auf den Internetseiten der Hochschulbibliothek online verfügbar Forschungszentrum Jülich GmbH Institut für Energie- und Klimaforschung Nukleare Entsorgung und Reaktorsicherheit (IEK-6) Dissolution Behaviour of Innovative Inert Matrix Fuels for Recycling of Minor Actinides Elena Laura Mühr-Ebert Schriften des Forschungszentrums Jülich Reihe Energie & Umwelt / Energy & Environment Band / Volume 378 ISSN 1866-1793 ISBN 978-3-95806-238-2 Bibliographic information published by the Deutsche Nationalbibliothek. The Deutsche Nationalbibliothek lists this publication in the Deutsche Nationalbibliografie; detailed bibliographic data are available in the Internet at http://dnb.d-nb.de. Publisher and Forschungszentrum Jülich GmbH Distributor: Zentralbibliothek 52425 Jülich Tel: +49 2461 61-5368 Fax: +49 2461 61-6103 Email: [email protected] www.fz-juelich.de/zb Cover Design: Grafische Medien, Forschungszentrum Jülich GmbH Printer: Grafische Medien, Forschungszentrum Jülich GmbH Copyright: Forschungszentrum Jülich 2017 Schriften des Forschungszentrums Jülich Reihe Energie & Umwelt / Energy & Environment, Band / Volume 378 D 82 (Diss. RWTH Aachen University, 2017) ISSN 1866-1793 ISBN 978-3-95806-238-2 The complete volume is freely available on the Internet on the Jülicher Open Access Server (JuSER) at www.fz-juelich.de/zb/openaccess. This is an Open Access publication distributed under the terms of the Creative Commons Attribution License 4.0, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. Die Neugier steht immer an erster Stelle des Problems, das gelöst werden will. Galileo Galilei i Abstract During the peaceful use of nuclear energy high level wastes, which contain long-lived radionu- clides (plutonium, minor actinides) with high radiotoxicity, are generated worldwide. About 10,000 t of spent fuel are unloaded from commercial reactors each year. Most countries in- cluding Germany favour the direct disposal of spent fuel in deep geological formations. Other countries prefer the reprocessing of the spent fuel to recycle uranium and plutonium. In Europe commercial reprocessing is currently performed in La Hague and Sellafield. A future alternative would be provided by closing the fuel cycle in the context of the partitioning and transmutation strategy (P&T). This method separates and converts the long-lived radionuclides into stable or short-lived nuclides via neutron induced reactions in dedicated facilities. The P&T strategy has potential to significantly reduce the radiotoxicity and the volume of the radioactive waste; how- ever it cannot obviate the need of a final repository. The transmutation of minor actinides can be performed in different reactor types, including accelerator driven systems, which consist of a subcritical reactor core and an external accelerator. The accelerator driven system (ADS) fuel consists of the fissile material (AnO2) which is spread in an inert matrix to improve the thermal properties of the fuel. Within this work two different fuels containing actinide oxides as fissile material and ceramic magnesium oxide (CerCer) or metallic molybdenum (CerMet) as matrix material are under investigation. The dissolution and separation issues for inert matrix fuels (IMF) have not yet been investigated coherently. It is of crucial importance to take into account the behaviour of the matrix elements in the dissolution and separation processes and to check their compatibility with future waste management requirements. The dissolution and the subsequent hydro or pyrometallurgical treatment of the fuel are crucial steps in the repro- cessing process. A complete dissolution of the actinide oxide and the matrix material, or a selective dissolution, where one of the components remains undissolved, can be considered. To investigate the reprocessability of molybdenum and magnesia based inert matrix fuels reference samples containing variable amounts of CeO2, which serves as surrogate for plutonium dioxide, have been prepared based on a comprehensive compactibility and sinterability investigation. The pellets were thoroughly characterized by means of density measurements, micro hardness measurements, scanning electron microscopy (SEM) investigation, and X-ray diffraction (XRD). The dissolution rate was studied in macroscopic experiments as a function of acid con- centration and temperature. Magnesium oxide is soluble even under mild conditions. The dissolution rates of MgO at dif- ferent acid concentrations are rather similar, whereas the dissolution rate is strongly dependent on the temperature. Additionally, the MgO dissolution process was investigated following a microscopic approach. Detailed SEM investigations show a heterogeneous reactivity of the MgO pellet’s surface. A model was developed to describe the evolution of the pellet surface area and a surface normalized dissolution rate was calculated. The activation energies of MgO dissolution in nitric acid have been calculated from the Arrhenius plot for different acid concen- trations and indicate a surface controlled dissolution mechanism. During the dissolution of MgO/CeO2 pellets the MgO dissolves completely, while the bulk of CeO2 remains undissolved, allowing a separation of the actinides and the matrix during the dissolution process. ii The dissolution of molybdenum is more complex due to its specific aqueous redox chemistry (Mo(-II) – Mo(VI)). Molybdenum metal is soluble in nitric acid. However, it is oxidized to MoO3, which then precipitates. The dissolution rate strongly depends on the acid concentration. Higher acid concentrations or temperatures result in faster dissolution but also in more precipitation. The addition of ferric nitrate to the acid improves the dissolution properties and prevents precipitations at low acid concentrations. However, the addition of a great amount of Fe3+ to the solution might influence the extraction process. To get closer to the real system, unirradiated PuO2/Mo pellets were dissolved in collaboration with NRG and the Karlsruher In- stitut für Technologie, Institut für Nukleare Entsorgung. The presence of Fe(III) increases the solubility of Mo as described above, while the solubility of the actinides is decreased. In 1 and 3 mol/L HNO3 without the addition of iron about 2 and 3% of the plutonium dissolved respec- tively, while less than 0.1% of the Pu dissolved in the presence of iron. Dissolution in nitric acid is the first step in the head end of the reprocessing of spent fuel. Therefore, detailed knowledge of the speciation of molybdenum in nitric acid medium is crucial on the one hand to understand this dissolution process and on the other hand as a basis for the design of a tailored extraction process. The solution species of Mo in strongly acidic media have been characterized and quantified comprehensively. For this purpose electrospray ioni- zation mass spectrometry (ESI-MS), which can probe the stoichiometry and relative abun- dances of solution species, was applied in collaboration with the Leibniz Universität Hannover, Institut für Radioökologie und Strahlenschutz. The method delivers unique insights into the solution speciation of molybdenum as a function of acid- and Fe(III)-concentration. The solu- tion species Mo forms in the presence of iron were investigated in order to understand the effect of Fe(III) on the dissolution. The ESI-MS reveals the formation of mixed Mo-Fe species which explains the increased solubility. Moreover, a method to analyse solutions of molyb- denum with natural isotopic composition with a commercially available ESI/MS/MS instrument (QTrap) was developed in collaboration with the Forschungszentrum Jülich, Zentralinstitut für Engineering, Elektronik und Analytik 3. The commercial instrument permits routine measure- ments due to significantly reduced measurement times. As an alternative to the very complex dissolution of Mo based IMF the separation of the matrix material from the fuel by thermal treatment was considered. This exploits that molybdenum is oxidized in air at temperatures from 400 °C and the resulting MoO3 sublimes at 800 °C. It is expected that the volatile components of the fuel are not deposited together with the molyb- denum and the remaining components of the fuel do not evaporate at these temperatures. Molybdenum was quantitatively evaporated and recovered as MoO3, confirmed by XRD. In the case of thermal treatment of Mo/CeO2 mixtures a solid state reaction of MoO3 and CeO2 occurs at 674 °C. Depending on the
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