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DOE OSTI2018

In situ observation of phase changes of a silica-supported cobalt catalyst for the Fischer–Tropsch process by the development of a synchrotron-compatible in situ/operando powder X-ray diffraction cell

In situ characterization of catalysts gives direct insight into the working state of the material. Here, the design and performance characteristics of a universal in situ synchrotron-compatible X-ray diffraction cell capable of operation at high temperature and high pressure, 1373 K, and 35 bar, respectively, are reported. Its performance is demonstrated by characterizing a cobalt-based catalyst used in a prototypical high-pressure catalytic reaction, the Fischer–Tropsch synthesis, using X-ray diffraction. Cobalt nanoparticles supported on silica were studied in situ during Fischer–Tropsch catalysis using syngas, H 2 and CO, at 723 K and 20 bar. Post reaction, the Co nanoparticles were carburized at elevated pressure, demonstrating an increased rate of carburization compared with atmospheric studies.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2018

Colloidal Synthesis of Bulk-Bandgap Lead Selenide Nanocrystals

Lead selenide quantum dots (QDs) are low-bandgap IV-VI semiconducting nanomaterials that have been studied for a variety of applications. Their preparation using colloidal methods can create small spherical to larger cubic nanocrystals, with an upper limit of ~17 nm reported to date. Here we describe methods for preparing cubic PbSe nanocrystals over a 20–40 nm size range using a twostep procedure. Specifically, ~10 nm PbSe QDs are generated using the rapid injection method, the products from which are overcoated with additional lead and selenium precursors. The use of two lead reagents were studied; lead oleate resulted in a maximum of 20 nm cubes, while more reactive lead hexyldecanoate resulted in much larger nanomaterials with bulk bandgaps. However, PbSe samples prepared with lead hexyldecanoate also contained agglomerates. Special care must be taken when characterizing larger strained nanomaterials with X-ray powder diffraction, for which the Scherrer equation is inadequate. A more rigorous approach using the Williamson–Hall method provides characterizations that are consistent with electron microscopy analysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Structure-property relation and Weibull analysis of calcium aluminate cement pastes

Highlights: • Weibull distribution analysis was conducted for calcium aluminate cement pastes with 52 wt% and 71 wt% of alumina contents. • Compressive strength ranged from 10 to 45 MPa. • The hydrated phases found showed diverse polymorphisms of Gibbsite (Nordstrandite, Bayerite, Hidrogarnet and Gehlenite). - Abstract: In this investigation calcium aluminate cement (CAC) pastes with 52 wt% and 71 wt% of alumina contents were fabricated and characterized with different techniques. Samples were made with 0.4 and 0.5 water to cement (W/C) ratios. Both the raw cement powders and their corresponding samples after hydration were characterized in their microstructure by scanning electron microscopy, X-ray diffraction (with Rietveld refinement), X-ray fluorescence (XRF), Fourier Transform Infrared Spectroscopy (FTIR), density, and compression tests. With the compressive strength results, Weibull distribution analysis was conducted for 20 samples per composition. The higher compression strength obtained was about 45 MPa, which corresponds to samples with the higher W/C contents. The hydrated phases found showed diverse polymorphisms of Gibbsite (Nordstrandite, Bayerite, Hidrogarnet and Gehlenite).

36 MATERIALS SCIENCE↗

DOE OSTI2019

Characteristics and Processing of Hydrogen-Treated Copper Powders for EB-PBF Additive Manufacturing

The fabrication of high purity copper using additive manufacturing has proven difficult because of oxidation of the powder feedstock. Here, we present work on the hydrogen heat treatment of copper powders for electron beam powder bed fusion (EB-PBF), in order to enable the fabrication of high purity copper components for applications such as accelerator components and vacuum electronic devices. Copper powder with varying initial oxygen contents were hydrogen heat-treated and characterized for their chemistry, morphology, and microstructure. Higher initial oxygen content powders were found to not only reduce surface oxides, but also reduce oxides along the grain boundaries and form trapped H 2 O vapor inside the particles. The trapped H 2 O vapor was verified by thermogravimetric analysis (TGA) and residual gas analysis (RGA) while melting. The mechanism of the H 2 O vapor escaping the particles was determined by in-situ SEM heated stage experiments, where the particles were observed to crack along the grain boundaries. To determine the effect of the EB-PBF processing on the H 2 O vapor, the thermal simulation and the validation of single melt track width wafers were conducted along with melting single layer discs for chemistry analysis. A high speed video of the EB-PBF melting was performed in order to determine the effect of the trapped H 2 O vapor on the melt pool. Finally, solid samples were fabricated from hydrogen-treated copper powder, where the final oxygen content measured ~50 wt. ppm, with a minimal residue hydrogen content, indicating the complete removal of trapped H 2 O vapor from the solid parts.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Characterization of Urbix Resources Natural Flake Graphite Material for Nuclear Applications (CRADA NFE-18-07340 Final Report)

Urbix Resources is a company specializing in graphite powder processing and purification. Urbix is looking to become the first domestic supplier of nuclear-grade graphite in the United States. This has led to a Cooperative Research and Development Agreement (CRADA) being established between the Oak Ridge National Laboratory (ORNL) and Urbix Resources, with the goal of characterizing a purified graphite feedstock supplied by Urbix Resources. The resulting data will then be used to determine the viability of a large-scale nuclear graphite production and qualification campaign. These characterization methods have been performed on the as-received graphite feedstock, a heat-treated batch of the feedstock, a milled batch of the feedstock, and a nuclear-grade graphite powder historically used in fuel production. The data from the heat-treated and milled feedstock will determine how different processing methods affect the powder’s physical properties, whereas the data from the nuclear grade graphite will provide information about the characteristics of a graphite previously accepted for nuclear applications. All of these powders have been characterized individually and as part of a resin-graphite blend (herein referred to as matrix) that has been used in past fuel experiments. The results of these experiments show that the Urbix powder and nuclear-grade graphite powder display notably different properties from one another in many cases, but this discrepancy may have been the result of the typical particle size of each powder. This hypothesis is supported by tests conducted on the milled powder, which showed a closer resemblance in properties to the nuclear-grade graphite than the as-received powder. The method for pressing the graphite matrix also had a noticeable effect on the measured properties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Hierarchical microstructure of Yb-filled skutterudites through ultrasonically atomized spherical powders for enhanced thermoelectric performance

Hierarchical microstructures are widely explored as a strategy to reduce lattice thermal conductivity in thermoelectric materials while preserving favorable electronic transport. Here we demonstrate that ultrasonic atomization of precursor powders provides an intrinsic pathway to generate such architectures in n-type Yb0.3Co4Sb12 skutterudites. Materials were synthesized by both conventional sealed-ampoule and ultrasonic atomization routes, each yielding essentially single-phase skutterudite after densification. However, the atomized spherical powders undergo a distinct reaction-driven microstructural evolution during thermal treatment prior to densification. Electron microscopy reveals that the skutterudite phase within the particles induces swelling, cracking, and fragmentation of the droplets before consolidation. Multimodal structural and microstructural characterizations show that densification of these fragmented powders produces a hierarchical microstructure consisting of submicron grains, micrometer-scale faceted crystallites, and powder-derived domains separated by oxide-decorated boundaries. Comprehensive thermoelectric transport measurements evidence that this multiscale architecture lowers the lattice thermal conductivity while maintaining favorable electronic transport, leading to an average ~10% enhancement in the thermoelectric figure of merit. Complementary 121Sb Mössbauer spectroscopy further indicates lattice softening in the atomized material. These results demonstrate that ultrasonic atomization provides an effective route to engineer hierarchical microstructures in skutterudite thermoelectrics and offers a promising strategy for tailoring thermal transport in energy-conversion materials.

Bouteiller, Hugo [ORNL] (ORCID:0009000421322962)↗

DOE OSTI2026

Investigation of the Surface Chemistry of Magnesium and Magnesium Alloy Powders

Magnesium (Mg) and Mg alloy powders are generally difficult to sinter at atmospheric pressure in inert atmospheres purportedly due to the presence of powder particle surface oxide layers. To better understand sintering of Mg and Mg alloy powders, x-ray photoelectron spectroscopy (XPS) was performed to characterize the surface chemistry of gas atomized pure Mg and Mg alloys AZ91D and WE43 powders. These results are used to quantitatively determine the surface chemistry of these powders. Additionally, equilibrium thermodynamic modeling of these Mg/Mg alloys materials exposed to oxygen down to part per billion concentrations are presented for relative comparison to experimental XPS results. Analysis of these results are intended to improve sintering of Mg and Mg alloy powder materials through more quantitative knowledge of powder surface chemistry.

25 ENERGY STORAGE↗

DOE OSTI2018

Synthesis and Structural Characterization of Sb-Doped TiFe{sub 2}Sn Heusler Compounds

Ternary Heusler compounds form a numerous class of intermetallics, which include two families with general compositions ABC and AB{sub 2}C, usually referred to as half- and full-Heusler compounds, respectively. Given their tunable electronic properties, made possible by adjusting the chemical composition, these materials are currently considered for the possible use in sustainable technologies such as solar energy and thermoelectric conversion. According to theoretical predictions, Sb substitution in the TiFe{sub 2}Sn full-Heusler compound is thought to yield band structure modifications that should enhance the thermoelectric power factor. In this work, we tested the phase stability and the structural and microstructural properties of such heavily doped compounds. We synthesized polycrystalline TiFe{sub 2}Sn{sub 1−x}Sb{sub x} samples, with x = 0, 0.1, 0.2 and 1.0 by arc melting, followed by an annealing treatment. The structural characterization, performed by x-ray powder diffraction and microscopy analyses, confirmed the formation of the pseudo-ternary Heusler structure (cF16, Fm-3m, prototype: MnCu{sub 2}Al) in all samples, with only few percent amounts of secondary phases and only slight deviations from nominal stoichiometry. With increasing Sb substitution, we found a steady decrease in the lattice parameter, confirming that the replacement takes place at the Sn site. Quite unusually, the as-cast samples exhibited a higher lattice contraction than the annealed ones. The fully substituted x = 1.0 compound, again adopting the MnCu{sub 2}Al structure, does not form as stoichiometric phase and turned out to be strongly Fe deficient. The physical behavior at room temperature indicated that annealing with increasing temperature is beneficial for electrical and thermoelectrical transport. Moreover, we measured a slight improvement in electrical and thermoelectrical properties in the x = 0.1 sample and a suppression in the x = 0.2 sample, as compared to the undoped x = 0 sample.

36 MATERIALS SCIENCE↗

DOE OSTI2017

“Synthesis-on” and “synthesis-off” modes of carbon arc operation during synthesis of carbon nanotubes

Arc discharge synthesis of single-walled carbon nanotubes (SWCNTs) remains largely uncontrollable, due to incomplete understanding of the synthetic process itself. Here, we show that synthesis of SWCNTs by a carbon arc may not constitute a single continuous process, but may instead consist of two distinct modes. One of these, a “synthesis-on” mode, produces the majority of the nanomaterials. During the synthesis-on mode, proportionally more carbon nanotubes are collected than in another mode, a “synthesis-off” mode. Both synthesis-on and synthesis-off modes for a typical arc configuration, employing a hollow anode filled with a mixture of powdered metal catalyst and graphite, were characterized by using in situ electrical, imaging, and spectroscopic diagnostics, along with ex situ imaging and spectroscopy. The synthesis-on mode duration is rare compared to the total arc run-time, helping to explain the poor selectivity found in the final collected products, a known inadequacy of arc synthesis. Finally, the rarity of the synthesis on mode occurence may be due to the synthesis off mode being more favorable energetically.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Chemical stability and long-term cell performance of low-cobalt, Ni-Rich cathodes prepared by aqueous processing for high-energy Li-Ion batteries

Cobalt content in Li-ion battery cathodes has become a top concern due to its price volatility and limited source availability. Low-cobalt, Ni-rich active materials are promising candidates for next-generation cathodes due to their high capacities, and water-based processing of these materials can further reduce both cost and environmental impact. We systematically evaluated the water compatibility of four different LiNi x Mn 1-x-y Co y O 2 (NMC) powders with increasing nickel contents. Comprehensive characterization verified there is no major change to their bulk structures, and only slight surface modifications related to the removal of contaminant species. For the first time, we demonstrate that LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC 811) cathodes can be formulated in water and cycled 1000 times in full pouch cells with excellent capacity retention (~70% compared to ~76% for NMP-processed cells). When implemented in future battery production lines, aqueous processing of Ni-rich NMC will simultaneously enable cost reductions and higher cell energy densities.

25 ENERGY STORAGE↗

DOE OSTI2017

Structure and properties of silver sulfate complexes derived from dipyridyl methylthio ligands with secondary donor site

Dipyridyl sulphide ligands 4-(pyridin-4-ylmethylthio)pyridine (abbreviated as L1) and 3-(pyridin-4-ylmethylthio)pyridine (abbreviated as L2) have been designed and used as μ-{sub N},{sub N}-bridging linkages to construct coordination polymers with free –S–CH{sub 2}– groups as secondary donor sites. By use solvent control method, coordination polymers ([Ag{sub 3}SO{sub 4}(L1){sub 3}](Cl)·4.5H{sub 2}O){sub ∞}(1), ([Ag{sub 2}SO{sub 4}(L1){sub 2}]·6H{sub 2}O·2CH{sub 3}OH){sub ∞}(2), ([Ag{sub 2}SO{sub 4}(L2){sub 2}]·H{sub 2}O){sub ∞}(3) and ([Ag{sub 4}(SO{sub 4}){sub 2}(L2){sub 4}]·5H{sub 2}O){sub ∞}(4) with different architectures were obtained. Complexes 1, 3 and 4 feature 1D channel with different sizes and structures. Complex 1 exhibits guest exchange by THF and 1,4-dioxane, and Hg{sup 2+} sorption ability from solution due to its relative larger channel and available bonding sites of –S– exposed to the channel region. All complexes have been characterized through single-crystal and powder X-ray diffraction (PXRD), FT-IR spectra, X-ray photoelectron spectroscopy (XPS), elemental and thermogravimetric analyses. The guest exchange and Hg{sup 2+} sorption were monitored and identified, and the structure-property relationship of coordination polymers 1–4 are discussed. - Graphical abstract: Coordination polymers of silver(I) sulfate with secondary donor sites are shown guest exchange property and Hg{sup 2+} absorb ability from solution. This work provides a new method to construct functional materials with potential application. - Highlights: • New example of constructing functional coordination polymer with secondary donor methylthio group. • Guest exchange and interesting Hg(II) absorb ability from solution are investigated. • New method to construct functional materials with potential application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Mixed nickel-gallium tellurides Ni{sub 3−x}GaTe{sub 2} as a matrix for incorporating magnetic cations: A Ni{sub 3−x}Fe{sub x}GaTe{sub 2} series

Using a high-temperature ampoule technique, a series of mixed nickel-iron-gallium metal-rich tellurides with layered structures, Ni{sub 3-x}Fe{sub x}GaTe{sub 2}, were prepared and characterized based on X-ray powder diffraction, energy-dispersive spectroscopy, and {sup 57}Fe Mössbauer spectroscopy data. These compounds may be regarded as a result of partial substitution of nickel by iron in the recently reported ternary Ni{sub 3-x}GaTe{sub 2} series, which are based on NiAs/Ni{sub 2}In type of structure. The compositional boundary for the substitution was found to be at x~1. According to the Mössbauer spectroscopy data, the substitution is not statistical, and iron atoms with the increase in x tend to preferentially occupy those nickel positions that are partially vacant in the initial ternary compound. Magnetic measurements data for the Ni{sub 3-x}Fe{sub x}GaTe{sub 2} series show dramatic change in behavior from temperature-independent paramagnetic properties of the initial matrix to a low-temperature (~75 K) ferromagnetic ordering in the Ni{sub 2}FeGaTe{sub 2}. - Graphical abstract: Ordered substitution of nickel by iron in the Ni{sub 3−x}GaTe{sub 2} series leading to ferromagnetic ordering. - Highlights: • A series of Ni{sub 3−x}Fe{sub x}GaTe{sub 2} compounds were synthesized. • They adopt the NiAs/Ni{sub 2}In type of structure with ordered iron distribution. • The distribution of iron was studied using {sup 57}Fe Mössbauer spectroscopy. • An increase in iron content leads to the strong ferromagnetic coupling.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2017

Synthesis and structural characterization of the hexagonal anti-perovskite Na{sub 2}CaVO{sub 4}F

The structural details of the ordered hexagonal oxyfluoride Na{sub 2}CaVO{sub 4}F prepared by solid-state synthesis using stoichiometric amounts of V{sub 2}O{sub 5}, CaCO{sub 3}, Na{sub 2}CO{sub 3} and NaF were characterized using high-resolution neutron powder diffraction. The structural changes between 25 °C and 750 °C revealed that the two structural subunits in this material behave different when heated: there is an expansion of the face-shared FNa{sub 4}Ca{sub 2} octahedra while the VO{sub 4} tetrahedra due to increased thermal disorder reveal marginal bond contractions. Bond valences and the global instability index point to significant structural disorder at 750 °C. - Graphical abstract: The structure of the novel oxyfluoride Na{sub 2}CaVO{sub 4}F is studied at room temperature and high-temperatures. The structure can be viewed as layers of compression and elongation of polyhedral subunits, which change as a function of temperature. - Highlights: • The novel oxyfluoride, Na{sub 2}CaVO{sub 4}F, is synthesized via solid-state method. • High-resolution neutron diffraction data is used to analyze the structure of Na{sub 2}CaVO{sub 4}F. • Structural subunits exhibit expansion and contraction with increasing temperature. • Higher temperatures increase instability within the structure of Na{sub 2}CaVO{sub 4}F.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Solar light driven photocatalytic degradation of Ofloxacin based on ultra-thin bismuth molybdenum oxide nanosheets

Highlights: • Facile synthesis of ultra-thin Bi{sub 2}MoO{sub 6} nanosheets. • Solar-light driven photocatalytic degradation of antibiotic Ofloxacin. • Almost 70% photocatalytic degradation of Ofloxacin under optimized conditions. - Abstract: Herein, we report the facile synthesis, characterization and solar-light driven photocatalytic degradation of ultra-thin bismuth molybdenum oxide (Bi{sub 2}MoO{sub 6}) nanosheets. The nanosheets were synthesized by hydrothermal process and characterized using several techniques such as powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDS), UV-diffusive reflectance spectroscopy (UV-DRS), transmission emission microscopy (TEM) and X-ray photon electron spectroscopy (XPS). The detailed morphological and structural studies confirmed the growth of ultra-thin Bi{sub 2}MoO{sub 6} nanosheets in large density with orthorhombic crystal structure. The calculated bandgap energy from Tauc’s plot for the synthesized nanosheets was found to be 2.73 eV, which shows maximum absorption toward higher wavelength. The XPS studies confirmed the successful formation Bi{sub 2}MoO{sub 6} nanosheets. The synthesized material was used as efficient solar light driven photocatalyst for the photocatalytic degradation of Ofloxacin. The mineralization of ofloxacin was confirmed using total organic carbon (TOC) analysis and photocatalytic experiments were performed under optimized conditions. It was observed that TOC value decreased with increasing the irradiation time. Under optimized photocatalytic degradation conditions, the observed extent of degradation was found to be ∼ 71%. The observed results confirm that the synthesized Bi{sub 2}MoO{sub 6} nanosheets are efficient and promising visible light responsive catalyst for the degradation of persistent organic pollutants.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

Materials for learning use of GSAS-II

The General Structure Analysis System (GSAS-II) package provides materials and crystallographic analysis for all types of diffraction data. It was initially made available with very limited capabilities, but over much of the last decade the features have been expanded, so that GSAS-II is now a comprehensive tool for nearly all types of structural and materials characterization studies. The need to provide materials to teach use of GSAS-II, while the software has been undergoing constant revision and expansion, has required new approaches for documentation. This has included providing tutorials, as each major new capability has been added, and context-sensitive help for each section of the program. Comments in the code are also expanded into a software reference guide. Finally, most recently, video versions of more than half of the tutorials were created and others were provided with animated graphics. All GSAS-II documentation is web-based.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2018

Quantitative Attachment of Bimetal Combinations of Transition-Metal Ions to the Surface of TiO 2 Nanorods

Here we report the sequential, quantitative loading of transition-metal ions (Cr 3+ , Mn 2+ , Fe 2+ , Co 2+ , Ni 2+ , and Cu 2+ ) onto the surface of rod-shaped anatase TiO 2 nanocrystals in bimetallic combinations ( 6 C 2 = 15) to form M,M'-TiO 2 nanocrystals. The materials were characterized with transmission electron microscopy (TEM), powder X-ray diffraction (XRD), elemental analysis, X-ray photoelectron spectroscopy (XPS), and UV–visible spectroscopy. TEM and XRD data indicate that the sequential adsorption of metal ions occurs with the retention of the phase and morphology of the nanocrystal. Atomistic models of the M,M'-TiO 2 nanocrystals were optimized with density functional theory calculations. Calculated UV–visible absorption spectra and partial charge density maps of the donor and acceptor states for the electronic transitions indicate the importance of metal-to-metal charge transfer (MMCT) processes.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Observation of an Intermediate to H 2 Binding in a Metal–Organic Framework

Coordinatively unsaturated metal sites within certain zeolites and metal–organic frameworks can strongly adsorb a wide array of substrates. While many classical examples involve electron-poor metal cations that interact with adsorbates largely through physical interactions, unsaturated electron-rich metal centers housed within porous frameworks can often chemisorb guests amenable to redox activity or covalent bond formation. Despite the promise that materials bearing such sites hold in addressing myriad challenges in gas separations and storage, very few studies have directly interrogated mechanisms of chemisorption at open metal sites within porous frameworks. Here, we show that nondissociative chemisorption of H 2 at the trigonal pyramidal Cu + sites in the metal–organic framework Cu I -MFU- 4 l occurs via the intermediacy of a metastable physisorbed precursor species. In situ powder neutron diffraction experiments enable crystallographic characterization of this intermediate, the first time that this has been accomplished for any material. Evidence for a precursor intermediate is also afforded from temperature-programmed desorption and density functional theory calculations. Here, the activation barrier separating the precursor species from the chemisorbed state is shown to correlate with a change in the Cu + coordination environment that enhances p-backbonding with H 2 . Ultimately, these findings demonstrate that adsorption at framework metal sites does not always follow a concerted pathway and underscore the importance of probing kinetics in the design of next-generation adsorbents.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Investigations towards incorporation of Eu 3+ and Cm 3+ during ZrO 2 crystallization in aqueous solution

Nuclear energy provides a widely applied carbon-reduced energy source. Following operation, the spent nuclear fuel (SNF), containing a mixture of radiotoxic elements such as transuranics, needs to be safely disposed of. Safe storage of SNF in a deep geological repository (DGR) relies on multiple engineered and natural retention barriers to prevent environmental contamination. In this context, zirconia (ZrO 2 ) formed on the SNF rod cladding, could be employed as an engineered barrier for immobilization of radionuclides via structural incorporation. This study investigates the incorporation of Eu 3+ and Cm 3+ , representatives for trivalent transuranics, into zirconia by co-precipitation and crystallization in aqueous solution at 80 °C. Complementary structural and microstructural characterization has been carried out by powder X-ray diffraction (PXRD), spectrum imaging analysis based on energy-dispersive X-ray spectroscopy in scanning transmission electron microscopy mode (STEM-EDXS), and luminescence spectroscopy. The results reveal the association of the dopants with the zirconia particles and elucidate the presence of distinct bulk and superficially incorporated species. Hydrothermal aging for up to 460 days in alkaline media points to great stability of these incorporated species after initial crystallization, with no indication of phase segregation or release of Eu 3+ and Cm 3+ over time. These results suggest that zirconia would be a suitable technical retention barrier for mobilized trivalent actinides in a DGR.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗