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DOE OSTI2024

Experience with Noble Metals During HLW Vitrification at FZK, Germany (Rev. 0)

The noble metals ruthenium (Ru), rhodium (Rh), and palladium (Pd) are present to various extents in defense and commercial high-level nuclear waste streams. Usually, their concentrations are higher in commercial waste. Ru, Rh, and Pd are sparingly soluble in silicate glass melts and they therefore form separate metal, oxide, or other phases. These phases are generally denser than the glass melt and tend to sediment to the bottom of the melter, where they form a "sludge" layer. Since the sludge layer has a higher electrical conductivity than the molten glass, accumulation of sludge can ultimately lead to electrical disruption of the operation of the melter. In addition, the sludge reduces the melt volume, which also changes the operational characteristics of the melter.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Modeling the Behavior of Noble Metals During HLW Vitrification in the DM1200 Melter

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Processes in Salt Repositories for Radioactive Waste Disposal

This document summarizes the key processes (thermal, hydrological, mechanical, and chemical; THMC) impacting the features of a deep geological repository for radioactive waste in salt. Some processes are natural and on-going whether the repository is there or not, and other processes are driven by the perturbation associated with the repository. The features considered here include both engineered and natural components of the repository system. The engineered barrier system (EBS) in a salt repository is quite different from those implemented for a repository in clay or crystalline rocks, because it is comprised mostly of granular salt and salt-compatible cements, rather than bentonite. When compared to other rocks (i.e., silicates), salt has unique properties that make it an excellent potential host rock. Openings and fractures in salt creep closed readily. Salt has high thermal conductivity, which can reduce peak temperatures. Additionally, far away from the excavations the porosity of salt is unconnected, which leads to essentially zero advective or diffusive transport. The small amount of hypersaline brine occurring in salt minimizes microbial activity, reduces colloid-assisted transport, and eliminates in-package criticality (i.e., chloride is a neutron poison). At the end of the report, we present a brief outline for a potential salt repository, including considerations avoided in previous repository disposal concepts. We propose considering higher-temperature processes in future disposal concepts, rather than trying to minimize the thermal perturbation of the repository. Since hot salt is drier, a dry repository would limit corrosion, gas generation, and solute transport. Openings and fractures creep shut faster in hot salt. Therefore, higher temperatures could be seen as beneficial, rather than something to minimize, through increased spacing between waste packages (increasing repository costs).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2026

Distributed Mafic Rock Resources for Carbon Mineralization in Arizona

Ex-situ carbon mineralization is a process by which CO2 is reacted with alkaline silicate minerals and rocks to produce stable carbonate materials, which can be used for other industrial processes. Arizona, U.S.A., hosts abundant surficial mafic rocks in three young volcanic fields, Geronimo-San Bernardino, San Francisco, and Springerville, and other distributed locations throughout the state. We created a Mafic Rock Resource Inventory (MRRI) that categorizes geochemical, physical, and textural characteristics of a diverse suite of surficial mafic rock samples and provide a benchmark reaction dataset parameterizing the temperature, pressure, and pH conditions best suited ex-situ mineralization in different rock types. MRRI data is publicly available online via a map-viewer. We establish two reaction condition sets, varied in temperature, pressure, and pH, where crystal-rich and glassy rocks reach maximum reaction extent and different carbonate phases are formed. Systematic ex-situ mineralization experiments on 21 diverse rock types show trends in geochemical, mineralogical, and reactivity behavior and establish maximum effective capture capacity. From this, scoria cones in three Arizona volcanic fields have a ~62 Gt effective CO₂ storage capacity with one of the fields having a ~42 Gt storage capacity in lava flows. Reactivity results have applications to alkaline mafic rock resources exposed globally, including producing additional effective storage capacity estimates and scaled commercialization of mafic rock ex-situ mineralization, should reaction extents be improved through advances in mineralization techniques. MRRI data were used to create a Direct Air Capture to Mineralization (DACM) systems model, technoeconomic analysis, and life-cycle assessment. These documents are presented as three appendices.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2026

Characterization and effects of impurities on carbonate quantification in heterogenous matrices

Mineral carbonation simulates a natural weathering phenomena by breaking down silicates and oxides to form Ca & Mg carbonates. Various mineralization methods have been demonstrated as a potential technique to improve the quality of slags and tailings through neutralization and stabilization of problematic species to yield a product better suited for use in concrete. This study aims to characterize, quantify and analyze carbonates in various carbonated products such as mineralized CaCO 3 , CO 2 mineralized Steel Slags and Mine Tailings. More than 10 samples were analyzed for carbonate measurement and verification from industrial and academic partners that pioneer commercial CO 2 mineralization technologies. The samples were characterized primarily by using X-ray diffraction (XRD), Thermogravimetric Analyses (TGA), and Scanning Electron Microscopy (SEM) to gain insights into CaCO 3 content. A baseline characterization of lab-grade CaCO 3 and MgCO 3 also revealed important considerations for CaCO 3 measurement using TGA alone. The experiments using synthetic lab-grade samples also revealed that the presence of MgCO 3 /MgO can accelerate the decomposition of CaCO 3 and thus can affect measurement parameters. Lab-grade CaCO 3 samples dosed into steel slag and mine tailing also showed significant deviation in their decomposition behavior. These insights are used to inform the development of a standardized protocol for the measurement and verification of carbonate-bearing products.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2024

Iron Bonding with Light Elements: Implications for Planetary Cores Beyond the Binary System

Light element alloying in iron is required to explain density deficit and seismic wave velocities in Earth’s core. However, the light element composition of the Earth’s core seems hard to constrain as nearly all light element alloying would reduce the density and sound velocity (elastic moduli). The alloying light elements include oxidizing elements like oxygen and sulfur and reducing elements like hydrogen and carbon, yet their chemical effects in the alloy system are less discussed. Moreover, Fe-X-ray Absorption Near Edge Structure (Fe-XANES) fingerprints have been studied for silicate materials with ferrous and ferric ions, while not many X-ray absorption spectroscopy (XAS) studies have focused on iron alloys, especially at high pressures. To investigate the bonding nature of iron alloys in planetary interiors, we presented X-ray absorption spectroscopy of iron–nitrogen and iron–carbon alloys at high pressures up to 50 GPa. Together with existing literature on iron–carbon, –hydrogen alloys, we analyzed their edge positions and found no significant difference in the degree of oxidation among these alloys. Pressure effects on edge positions were also found negligible. Our theoretical simulation of the valence state of iron, alloyed with S, C, O, N, and P also showed nearly unchanged behavior under pressures up to 300 GPa. This finding indicates that the high pressure bonding of iron alloyed with light elements closely resembles bonding at the ambient conditions. We suggest that the chemical properties of light elements constrain which ones can coexist within iron alloys.

Advanced Photon Source↗

DOE OSTI2025

Reactivity of Shale to Supercritical CO 2 : Insights from Microstructural Characterization and Mineral Phase Evolution in Caney Shales for CCUS Applications

Understanding mineral–fluid interactions in shale under supercritical CO 2 (scCO 2 ) conditions is relevant for assessing long-term geochemical containment. This study characterizes mineralogical transformations and elemental redistribution in five Caney Shale samples serving as proxies for reservoir (R1, R2, R3) and caprock (D1, D2) facies, subjected to 30-day static exposure to pure scCO 2 at 60 °C and 17.23 MPa (2500 psi), with no brine or impurities introduced. SEM-EDS analyses were conducted before and after exposure, with mineral phases classified into silicates, carbonates, sulfides, and organic matter. Initial compositions were dominated by quartz (38–47 wt.%), illite (16–23 wt.%), carbonates (12–18 wt.%), and organic matter (8–11 wt.%). Post-exposure, carbonate loss ranged from 15 to 40% in reservoir samples and up to 20% in caprock samples. Illite and K-feldspar showed depletion of Fe 2+ , Mg 2+ , and K + at grain edges and cleavages, while pyrite underwent oxidation with Fe redistribution. Organic matter exhibited scCO 2 -induced surface alteration and apparent sorption effects, most pronounced in R2 and R3. Elemental mapping revealed Ca 2+ , Mg 2+ , Fe 2+ , and Si 4+ mobilization near reactive interfaces, though no secondary mineral precipitates formed. Reservoir samples developed localized porosity, whereas caprock samples retained more structural clay integrity. The results advance understanding of mineral reactivity and elemental fluxes in shale-based CO 2 sequestration.

geochemical CO2 sequestration↗

DOE OSTI2025

Spectroscopy of the Hamburg Meteorite, Michigan H4

Spectroscopic studies of the Hamburg (Michigan H4) meteorite using visible–near-infrared (VNIR), mid-infrared (MIR), Raman, and Mössbauer data reproduce the results of more conventional laboratory measurements of petrology and geochemistry. This combination provides general information on the mineral modes of silicates, although spectroscopy was performed on different splits of this meteorite, and varying results may be explained by heterogeneity that is typical of ordinary chondrites. Raman also detects small features assigned to first-order D and G carbon bands, while Mössbauer data show the presence of Fe oxides and carbides. The electron microprobe (EMPA) composition of olivine in this meteorite is accurately measured to be Fo 81.3 , while MIR and Raman closely agree with Fo 80 and Fo 82 , respectively, and Mössbauer, at Fo 60 − Fo 70 , is in the ballpark. Similarly, P. R. Heck et al. report pyroxenes with compositions of Fs 16 Wo 1 , while Raman suggests a somewhat similar composition of Fs 28 Wo 0 . Both VNIR and MIR detect the presence of small amounts of feldspar, while EMPA identifies its composition as An 14 Ab 8 Or 5 . VNIR data were matched to spectral libraries of meteorite and asteroid data and shown to closely match other L and H meteorites. The best spectral matches to the Michigan H4 meteorite are to asteroid classes L/H/LL/URE, EH/EL/AUB, and CO/CV from M. D. Dyar et al.; objects in this group are intermediate in semimajor axis lengths for their orbits. The results highlight the strengths and weaknesses of each technique and show their collective strength when applied together to a single meteorite sample.

58 GEOSCIENCES↗

DOE OSTI2026

Induction Melter Processing Alternatives for High Level Radioactive Wastes – 26198

This work investigates the potential to vitrify nuclear fuel directly, as well as the vitrification potential associated with experimental dissolver solutions. Greater understanding of the exothermicity is needed to quantify processing risk, especially with respect to potential phase changes and associated explosion hazards present in some systems. Thermal analysis was carried out on various simulants to elucidate the exothermic reaction potential from solid metal dissolution in glass and from the drying of alternative process dissolver solutions. Results from experimental testing of simulants to demonstrate vitrification potential and compatibility indicate that alternative dissolver flowsheets suppress the heat released during processing and that common silicate- and phosphate- based glass systems are potential candidates for direct vitrification. Direct vitrification (conversion) of fuel simulants was assessed using laboratory scale glass melts to obtain qualitative information on dissolution rates and waste loadings. Initial tests were successful to dissolve and incorporate metal directly into glass, although the kinetics and limits of dissolution and incorporation into glass are not fully understood.

Amoroso, Jake [Savannah River National Laboratory ↗

DOE OSTI2025

Oxidation of n-alkanes using TS-1 and H 2 O 2 : Effects of chain length and solvents

The selective oxidation of n-C 8 H 18 , n-C 12 H 26 , n-C 16 H 34 , n-C 20 H 42 , and n-C 36 H 74 was studied with a goal of using these as models to provide insight into how to functionalize polyolefins. Reactions were carried out using a TS-1 catalyst and H 2 O 2 in a batch reactor with different cosolvents, including methanol, acetone, acetonitrile, methyl ethyl ketone, and methyl butyl ketone. Rates decreased with increasing alkane size, possibly due to the reduced solubility of larger alkanes into the water-rich phases. Cosolvents that promote the partitioning of alkanes in the aqueous phase increased the rates. 1 H NMR spectroscopy demonstrated that ketones were the primary products, although some alcohols also formed. There was preferential reaction at the 2 position in the alkanes, but reaction at central carbons was also observed. The results of this study suggest strategies for using this catalytic chemistry to functionalize polyolefins.

Alkane oxidation↗

DOE OSTI2025

Intrinsic mechanical properties and seeding effect of tobermorite synthesized in supercritical water

This publication reports for the first time the physiochemical, the intrinsic mechanical properties and the seed effect of anomalous Al-substituted 11 Å tobermorite synthesized via the innovative supercritical hydrothermal flow process at 400 °C and 25 MPa. This approach allows synthesizing highly crystalline tobermorite fibers in only 8 s, with characteristics very close to the natural tobermorite. The anomalous 11 Å tobermorite exhibits aluminosilicate chains with a high polymerisation degree and a less defective structure compared to materials produced via the conventional hydrothermal method. Furthermore, the intrinsic mechanical properties of Al-tobermorite synthesized in supercritical water are investigated for the first time by High-Pressure XRD. This Al-substituted 11 Å tobermorite is characterised by higher incompressibility along the b-axis and bulk modulus K0 in comparison with what is commonly observed for other synthetic tobermorite. The tobermorite acts as nucleation points to trigger the quick formation of the hydration product in Portland cement paste.

Calcium silicate hydrate↗

DOE OSTI2024

The structure of CaO–MgO–Al 2 O 3 –SiO 2 melts and glasses doped with FeO X –NiO

Neutron and x-ray diffraction measurements have been performed on CaO–MgO–Al 2 O 3 –SiO 2 (CMAS) glasses doped with NiO–Fe X O at room temperature, along with x-ray measurements on aerodynamically levitated liquids at ≥2000 K. The disordered structures have been modeled using empirical potential structure refinement to investigate the relation between the aluminosilicate network and the modifying cations. The SiO 4 and AlO 4 tetrahedra are found to have wider Si–O and Al–O bond distance distributions in the glass, and the first Ca–O n coordination shell is highly distorted, redistributing different populations of long and short bonds between the liquid and the glass. The addition of Fe and Ni at low aluminosilicate content increases the number of free oxygens not bonded to AlO 4 or SiO 4 . Mg–O and Fe–O are both found to be predominantly fourfold and fivefold in the liquid and glassy states. Despite these low coordination numbers, their bond angle distributions indicate that they are predominantly in nontetrahedral-type geometries, with ferrous and ferric iron possessing similar coordination environments. The Ca–O and Mg–O average coordination numbers and enthalpies of solution are consistent with their higher reactivity within relatively acidic aluminosilicate melts.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Waste-to-Energy (WTE)-derived Low-Carbon-Footprint Concrete (LCFC)

The construction industry is estimated to generate around 600 million tons of concrete and demolition waste annually in the US. In comparison, Waste-To-Energy (WTE) plants generate about 6.6 million tons of ash from the combustion of municipal solid waste.1–4 Research has been ongoing for decades to upcycle WTE-ash and C&D waste.

36 MATERIALS SCIENCE↗