Structure-formulation-property relationships of bio-based eutectogel vitrimer electrolytes for next-generation batteries
Current batteries primarily rely on the use of liquid electrolytes composed of flammable solvents that are unstable in contact with lithium metal, posing safety issues. The development of gel polymer electrolytes (GPEs) is expected to lead to new generations of safer batteries. To maintain their environmental relevance, these new batteries should ideally be made of bio-based materials, have an extended lifespan, and be recyclable. In this context, this thesis aims to develop bio-based GPEs cross-linked by vitrimer chemistry that allows for their recyclability. The swelling of electrolytes in green, non-flammable deep eutectic solvents (DESs) is considered to achieve ionic conductivities greater than 10-4 S.cm-1 at room temperature. The PhD student will study the influence of the chemical structure of the polymer and the DES on the physicochemical, mechanical, and electrochemical properties of these eutectogels to optimize their formulation for integration into a complete pouch-cell system.
Development of Microfluidic Platforms for In Situ Monitoring of Monoamide Solvent Radiolysis for Nuclear Fuel Reprocessing
Monoamides (N,N-dialkylamides) are being investigated as alternatives to TBP for the liquid–liquid extraction of uranium and plutonium in the reprocessing of spent nuclear fuel. Their qualification requires an assessment of their resistance to ionising radiation, which is essential to ensuring process robustness.
Conventional radiolysis studies conducted at the macroscopic scale require large volumes of radioactive materials and offer limited control over dose rate and hydrodynamic conditions, while also involving significant radiological protection constraints. Microfluidics can reduce the volumes required and provide improved control over the experimental conditions.
This PhD project, carried out in collaboration with an industrial partner in the nuclear sector as part of the ORACLE industrial research chair (Outil microfluidique Reconfigurable Automatisé pour le Cycle du combustibLE), aims to design and implement microfluidic systems enabling precise control of irradiation, residence time and hydrodynamics during the study of the radiolysis of novel solvents. The candidate will develop dedicated platforms for radiolysis experiments (X-rays, alpha and gamma radiation), with in situ monitoring of degradation products, under conditions representative of those encountered in nuclear fuel reprocessing.
This project is aimed at rigorous students with an interest in experimental work, in the final year of an engineering degree or undertaking a Master’s degree (Master 2) in analytical chemistry, separation science, instrumentation or microfluidics. Analytical thinking and strong scientific writing skills will also be highly valued.
Design and Synthesis of grafted silicas towards Boron isotopes separation by liquid chromatography
Design of an industrial process aiming at the production of boron 10 (10B) enriched boron carbide (B4C) is key to reach PPE 3 general strategic goals. Indeed, production of new Evolutionary Power Reactors (EPR) for electrical power output and Rapid Neutron Reactor (RNR) to ensure fuel cycle closure will put a tremendous strain on 10B enriched stocks.
Isotopic fractionation by means of boric acid liquid chromatography over an ad hoc material could be an industrially viable process. If anionic resins are strong historical candidates for this purpose the Laboratoire des Procédés Supercritiques et de Décontamination (LPSD) at CEA Marcoule focuses at developing original hybrid materials with enhanced properties.
The PhD work will focus on the synthesis and characterization (NMR, IR, LC-UV, GC) of organic molecules for the separation of boric acid boron isotopes. These molecules will be grafted over silicas to obtain hybrid materials with fine tuning of their physicochemical properties (SEM, BET, TGA, XRB, microscopy). Separative properties will be evaluated by column chromatography foreshadowing the industrial process.
This offer is aimed at a final year MSc student in organic synthesis or materials chemistry interested in the field of analytical and process development. The candidate should be meticulous and demonstrate analytical thinking. This is an opportunity to develop an expertise in organic synthesis applied to the production of hybrid material applicable to the development of an industrial process.
Development of a Hydrothermal Oxidation (HTO) Process for the Mineralization of PFAS-Containing Effluents
Due to their unique physicochemical properties, PFAS used in numerous industrial applications pose a problem regarding their accumulation in groundwater. This situation highlights the need for innovative treatment technologies aimed at minimizing PFAS levels in effluents. Various methods (thermal, biological, chemical) have been investigated, but they suffer from drawbacks such as high energy consumption or the generation of toxic secondary effluents. In this context, hydrothermal oxidation (HTO) offers a promising alternative, achieving PFAS mineralization rates exceeding 99.9% at temperatures of 600°C and above. Under these conditions, water becomes a reaction medium conducive to the mineralization of organic compounds. However, applying such operating conditions at an industrial scale presents a technological challenge due to significant heat loss and the *in situ* formation of HF, which can cause corrosion issues. This thesis aims to investigate the HTO process using a co-fuel and the *in situ* use of a silica-based material designed to sequester all fluoride ions. Defining the process's operating regime requires a detailed understanding of mass balances as well as the mechanisms of PFAS oxidation. Elucidating these mechanisms will require the implementation of a precise and rigorous analytical protocol to quantify all residual organofluorine compounds. Modeling high-pressure/high-temperature phase equilibria for fluorinated species can be performed using PhreeQC and Prosim Simulis software. Finally, the process's versatility regarding other organofluorine waste streams will also be considered. The candidate will work within the Supercritical Processes and Decontamination Laboratory, in collaboration with the Measurement, Safety, and Environment Laboratory (LITEN/Grenoble) and in interaction with technicians, engineers, and doctoral students. They will benefit from the expertise of these laboratories in hydrothermal processes and the analysis of perfluorinated compounds. The skills acquired during the PhD will open up numerous career opportunities in academic research and industrial R&D within the fields of chemistry and the environment..
Contribution of microfluidics to the study of liquid-liquid demixing in 2-compound extractant systems
This thesis aims to develop an instrumented and automated microfluidic platform dedicated to studying third-phase demixion in liquid-liquid extraction processes, applied to the challenge of securing diluent supply for the process implemented at the La Hague plant. As the diluent is essential to the plant's proper hydrodynamic operation, yet its supply has historically been fragile (production shutdowns, non-conformities, non-renewal of supplier contracts), this platform will enable rapid and automated characterization of alternative diluents with respect to third-phase formation in the TBP/diluent solvent system heavily loaded with actinides (U(VI), Pu(IV)). The device will ensure controlled contact between the aqueous and organic phases while automatically adjusting their respective compositions, with continuous in situ monitoring of actinide concentration along the flow channel via UV-Vis spectroscopy, as well as detection of third-phase onset, notably through light extinction methods particularly suited to the characterization of colloidal suspensions. This instrumental approach will be complemented by online SAXS measurements, enabling investigation of the local molecular arrangement of TBP and diluent in the biphasic domain for modeling purposes. The development of this tool will first draw on a literature review of the conditions governing third-phase formation and the mechanisms of binodal/spinodal decomposition in liquid-liquid systems. At least three candidate diluents will be evaluated on this platform following an experimental plan varying temperature, pH, and actinide composition, with tests conducted successively on surrogates, U alone, Pu alone, and finally a U+Pu mixture.
Impact of the microstructure and the O/M ratio on the thermophysical properties of (U,Pu)O2-x fuel SFR
Closing the nuclear fuel cycle is essential for the development of low-carbon energy systems. In France, plutonium resulting from the reprocessing of irradiated UOX fuels is recycled through the fabrication of MOX (U,Pu)O2 fuel and used in some pressurized water reactors (PWRs). MOX fuel is also envisaged for future Generation IV sodium-cooled fast reactors (SFRs), including some concepts of small modular reactors (SMRs). In these reactors, the strong radial thermal gradient modifies the fuel microstructure and leads to a radial redistribution of oxygen, and therefore of the O/M ratio (M = U + Pu). The safe deployment of this fuel cycle therefore relies on obtaining new data, currently inaccessible, on the properties that govern heat transfer in MOX, notably thermal conductivity (lambda, W.M-1.K-1) and heat capacity (Cp, J.kg-1.K 1). Indeed, the available data remain limited for sub-stoichiometric MOX and for irradiated MOX. Fuel performance codes (FPCs) currently use correlations established from data obtained on UO2 or on MOX within restricted composition and temperature ranges. These extrapolations are particularly limiting for describing the hot zones of irradiated MOX, where the O/M ratio can reach values inaccessible by direct fabrication of a single-phase MOX. This PhD work therefore aims to study the impact of the O/M ratio and of the microstructure on the thermophysical properties of MOX fuel, currently inaccessible, between ~500 and ~3000 K. The measurements will be carried out by laser flash on MOX fabricated according to the RNR and COCA processes, in order to compare the impact of the different initial microstructures resulting from these two fabrication routes. In order to study and reproduce the most sub-stoichiometric states observed in reactor, an innovative strategy of in-situ adjustment of the O/M ratio will be developed in the CLASH device. The PhD will take place at CEA Marcoule, where the characterizations of the materials before and after thermophysical measurements will be carried out which will, for their part, be performed at JRC Karlsruhe (Germany) during a 12-month mobility. In parallel, thermodynamic calculations (CALPHAD) will be carried out in order to interpret the phase equilibria at high temperature, and thus relate the measured properties to the structural and physico-chemical evolutions of MOX. These new data will feed the FPCs in order to more precisely evaluate the temperature and the margin to MOX melting.
Study of the selective extraction of rare earth elements by solvent extraction
The recycling of rare earths elements (REE) from conventional and unconventional sources is of economic and strategic importance for industrial sovereignty in the face of the challenges posed by the energy transition. The dissolution of phosphate and sulphate minerals results in the production of acidic effluents rich in metal ions, which must then be selectively separated in order to be valorised. To this end, the Laboratory for Laboratory of Recycling and Valorization Processes for Energy (LRVE) is interested in the development of extracting systems allowing the separation of REE from each other according to their atomic weight.
In this context, this PhD research topic aims to evaluate the applicability of extractants in a sulfuric or phosphoric acid medium. These may include phosphoric, phosphonic or phosphinic acids, or solvating molecules such as diglycolamide-type moieties. The main objectives will be, firstly, to understand the coordination mechanisms involved during the extraction stages for the separation of rare earth elements into groups (e.g. light and heavy elements) and to assess the impact of the presence and nature of counter-ions. This will be achieved by conducting dynamic sorption/desorption tests using a liquid-liquid extraction process, and by evaluating parameters such as capacity, selectivity and separation factors (ICP-AES, ICP-MS) of commercial or custom-synthesised molecules (NMR, IR, LC-UV, GC). Subsequently, the ideally selective stripping step will be investigated to ensure the reversibility of the extraction step and to prepare the technological building blocks not addressed in this study (conversion, resin capture, etc.). These results will enable an assessment of the ability of the extractant molecules to separate rare earth elements into several fractions within complexing media.
This project will be carried out at the CEA Marcoule site and is aimed at students in their second year of a Master’s degree or third year of an engineering programme specialising in organic chemistry or separative chemistry, with an interest in organic synthesis, analysis and the development of separation processes. Rigorous thinking, an analytical mind and scientific writing skills are required. This project will enable students to acquire skills in synthetic chemistry and separative chemistry within the context of a topic of significant strategic importance.
Development and validation of materials simulating MOx fuel dissolution residues
Dissolution in nitric acid is a key step in the recycling of spent nuclear fuels. In the case of MOx fuels (U,Pu)O2, it generates complex solid residues containing potentially recoverable actinides and fission products, some of which are critical metals of strategic interest for technologies such as semiconductors, photovoltaics, and fuel cells. A second oxidative dissolution step is currently being investigated to enable their recovery. However, the nature and physicochemical properties of these residues remain difficult to study due to their high radioactivity and limited availability.
The objective of this PhD thesis is to establish and validate a methodology for developing surrogate materials representative of the residues generated during the dissolution of MOx fuels.
The first step will consist of reviewing the literature to establish a comprehensive overview of the main physicochemical characteristics of actual residues, including their composition, particle size, and the nature and structure of the phases present, as well as the oxidation states of the cations. Dissolution experiments on simulated MOx fuels (simMOx) will then be carried out to produce residues that can be characterized using techniques that are difficult to apply to irradiated materials. These results will be used to define the properties to be reproduced when developing the surrogate materials. Their representativeness will be assessed by comparison with actual residues and those obtained from the dissolution of simMOx. Finally, their behavior during oxidative dissolution will be compared with that of actual residues and simMOx-derived residues, in order to validate their relevance as experimental model materials.
At the end of the PhD, the candidate will have acquired strong expertise in the study of complex systems, the physicochemical characterization of materials, and the critical analysis of literature and experimental data. This multidisciplinary training will open up a wide range of career opportunities in academic research and industrial R&D, both within and beyond the nuclear sector.
In-depth understanding of the dedensification phenomenon during MOX sintering and during a pseudo-thermal stability test
MOX (mixed uranium and plutonium oxide) is a civil nuclear fuel. It comes in the form of cylindrical pellets with a diameter and height of approximately 10 mm. It is produced using a process that includes a high-temperature sintering step in a controlled atmosphere. During the sintering of MOX fuel pellets—formed via uniaxial pressing from a previously prepared granular feedstock—a phenomenon of dedensification resulting in swelling may occur under certain conditions. This swelling can persist during thermal stability tests intended to simulate specific in-reactor irradiation conditions.
The aim of this thesis is to identify the physicochemical mechanisms underlying this dedensification phenomenon and to formulate them mathematically in order to develop a model.
The thesis therefore includes an experimental component—to be conducted at Cadarache (using UO2) and Marcoule (using MOX)—to provide data for the model, which will be mathematically formulated during a theoretical phase carried out in collaboration with modelers at Cadarache.
TEM study of the fine microstructure of sintered MOX
Transmission electron microscopy (TEM) is a key characterization tool for studying the microstructure of MOX (mixed uranium-plutonium oxide) fuel, regardless of the degree of homogeneity in the spatial distribution of plutonium. Preliminary results have shown that MOX fuel appearing homogeneous at the electron probe microanalysis scale was not homogeneous at the sub-micron scale of its constituent grains (Siméon et al., Journal of the European Ceramic Society 42 (2022) 7237-7246). One of the objectives of this thesis is to gain a detailed understanding of the formation of the MOX fuel microstructure, paying particular attention to potential plutonium-rich heterogeneities, given their significance for reprocessing (nitric acid dissolution). The impact of the manufacturing process (e.g., the MIMAS approach versus the direct co-milling approach) and sintering parameters (atmosphere, isothermal holding temperature, and holding time) on the development of these plutonium-rich zones must be taken into account. To this end, the student will need to identify existing sintered MOX samples (with a Pu/(U+Pu) content of 11 mol%) from previous studies and/or fabricate specific ones. These samples will differ based on the granular material preparation method used prior to uniaxial pressing and on the sintering conditions (specifically, oxygen partial pressure). In addition to standard microstructural characterization (grain size, pore size, and pore location via scanning electron microscopy; plutonium spatial distribution via electron microprobe and Raman spectroscopy), thin-foil preparation using a focused ion beam (FIB) and TEM characterization will be performed on the samples deemed most significant. Particular attention will be paid to plutonium localization (grain bulk, grain boundaries, space-charge layer formation) and local chemical composition (plutonium content, local O/M ratio) using EDS/EELS analysis. Alongside detailed microstructural characterization, the student will conduct nitric acid dissolution tests to attempt to establish correlations between plutonium heterogeneity (size, volume fraction, location, etc.) and the content of undissolved residue. The experimental work will be carried out at Marcoule (Atalante facility) and Cadarache (LECA-STAR laboratory). The results will be disseminated through scientific publications in peer-reviewed international journals.