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DOE OSTI2025

K-3 Refractory Corrosion Test Results, HAL24M2

This report summarizes the refractory corrosion data of the high-Al matrix of Direct Feed High-Level Waste (DFHLW) glasses generated to expand glass compositional ranges. Design of a 20 high-Al glass matrix, HAL24M2, was reported in Russell et al. (2025, in progress). The HAL24M2 glasses were tested for K-3 corrosion and the results are presented in this report. Corrosion of Monofrax K-3 refractory materials in the HAL24M2 glass melts was measured using a crucible-scale method. Two test conditions, 1150 °C/7days and 1200 °C/7days were applied. The melt-line neck corrosion depth of the test coupons was measured by micro-computed tomography (micro-CT). The measured K-3 neck corrosion values were compared to predicted values using the model in Vienna et al. (2024). The model slightly over-predicted the neck corrosion depth of these glasses.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Alternative reductants for foam control during vitrification of high-iron High Level Waste (HLW) feeds

Foaming during vitrification of radioactive waste in Joule-Heated Ceramic Melters (JHCM) is exacerbated by trapping of evolving gases, such as CO 2 , NO x and O 2 , beneath a viscous reaction layer. Foaming restricts heat transfer during melting. Sucrose is employed as the baseline additive at the Hanford site in Washington State, USA to reduce foaming. Alternative carbon-based reductant additives were explored in simulated, inactive Hanford high-iron HLW-NG-Fe2 feeds, for both their effect on foaming and to give insight to the behaviour of multivalent species in glass melts under different redox conditions. Graphite, coke (93% C), formic acid and HEDTA additives were compared with sucrose, and a feed with no additive. Graphite and coke additions proved most effective in reducing the maximum foam volume by 51 ± 3% and 54 ± 2%, respectively, compared with 24 ± 5% for sucrose. Lower foaming could result in more efficient vitrification in JHCMs. Reductants also affected redox ratios in the multivalent species present in the feed. The order of reduction, Mn 3+ /Mn 2+ > Cr 6+ /Cr 3+ > Ce 3+ /Ce 4+ > Fe 3+ /Fe 2+ was as predicted on the basis of their redox potentials. There is less reduction overall, particularly in the Fe 3+ → Fe 2+ , than predicted by the calculations, attributed to the oxygenated atmosphere of the experiments.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Segmental Dynamics and Vitrification in Associating Copolymer Melts: Role of Cluster Formation, Microdomains, and Cross-Linking

A microscopic statistical mechanical theory of the structure, self-assembly, and activated segmental relaxation is employed to study associating copolymer melts with high attractive sticker fractions, local clustering, and disordered microphase ordering. The stickers are dynamically pinned in a manner that does not affect equilibrium structure which mimics the much slower physical bond breaking process or postassembly cross-linking of sticky monomers. Local sticker clustering and microdomain spatial correlations significantly modify the activated relaxation of nonstickers and glass transition temperature, T g . A re-entrant glass-melting feature is predicted as sticker attraction strength is initially increased corresponding to a speed up of segmental relaxation, and hence reduction of T g relative to the cross-linked homopolymer network. A mechanistic analysis reveals three competing effects: a purely kinetic slowing down of nonstickers down due to cross-linking, disordering of the nonsticker local cage and weakening of effective forces they experience due to sticker physical clustering, and a longer range impact of microdomain scale correlations that results in nonmonotonic dynamical effects. At high enough attraction strength, a qualitative change emerges corresponding to a sticker fraction dependent elevation of T g , which eventually surpasses that of the cross-linked homopolymer network. Dynamically, the new physics arises from a complex evolution of the amplitude of the collective elastic field that dresses the large amplitude mobile segment hopping within a coupled local-nonlocal description of the alpha relaxation. Furthermore, the results are qualitatively consistent with recent experiments on associating PDMS and PPG telechelics of fixed sticker fraction but with chemically different end groups of variable attraction strengths. Finally, possible tests using simulation and the influence of material or model specific interaction potentials and other real world complications are discussed.

Copolymers↗

DOE OSTI2026

Reduced-Order CFD Modeling to Support Waste Loading Optimization in Hanford WTP Vitrification

The U.S. DOE Hanford Site stores over 56 million gallons of radioactive liquid tank waste that must be treated and immobilized for long-term disposal The Waste Treatment and Immobilization Plant (WTP) will vitrify this waste by feeding it into Joule-heated melters, where it is incorporated into a stable borosilicate glass Computational fluid dynamics (CFD) simulations of glass melters can provide insight into the maximum achievable waste loading under varying melter operating conditions Fully resolved VOF multiphase simulations were used as the reference model to capture bubble-driven convection in the melter, including bubble formation, rise behavior, and induced glass melt circulation Effective bubble column diameter and rise velocity were extracted from the resolved simulations, compared with empirical correlations, and refit across relevant viscosity and gas flow rate conditions Explicit gas–liquid interface tracking was replaced with a single-phase momentum source term model, enabling faster steady-state CFD simulations while preserving the dominant hydrodynamic effects of bubbling New empirical correlations were developed for effective bubble column diameter and bubble rise velocity by fitting resolved simulation data across expected melter viscosity and gas flow rate ranges, providing improved inputs for the momentum source term model compared with existing literature correlations The momentum source term model reduced fluid-domain mesh size by 89% and achieved an 8.4× computational speedup relative to resolved bubbling simulations The validated momentum source term approach enables prediction of process-relevant heat transfer behavior in the integrated melter model, including heat transfer from the molten glass to the cold cap, plenum, refractory walls, and surrounding structural regions under varying melter operating conditions

12 - MGMT OF RADIOACTIVE AND NON-RADIOACTIVE WASTE↗

DOE OSTI2026

Closed‐Loop Recycling of Poly(pentylene Adipate‐ co ‐Terephthalate) via Amine‐Catalyzed Methanolysis

Advancing circularity through effective chemical recycling strategies is essential for enabling the sustainable use of emerging biodegradable polyesters in film applications. In this context, poly(pentylene adipate-co-terephthalate) with a 40/60 adipate-to-terephthalate ratio (PPeAT60), a significantly stiffer and partially biobased copolyester recently reported by our team, offers improved mechanical performance and processability compared to commercial poly(butylene adipate-co-terephthalate), while providing a platform to evaluate advanced recycling approaches for film applications. Here, this study describes depolymerization of PPeAT60 through amine-catalyzed methanolysis, followed by the repolymerization of the recovered monomers. The resulting repolymerized material exhibited a molar mass distribution, chemical structure, and thermal stability comparable to the virgin polymer, confirming the technical feasibility of the methanolysis-based recycling route. Both polymers displayed nearly identical melting, glass transition, and decomposition temperatures, crystallinity, and modulus, demonstrating full structural and mechanical reproducibility after recycling. Variations in crystallization kinetics, elongation at break, and barrier properties likely arise from trace impurities (<1%) introduced during processing acting as nucleating and stress-inducing agents. Overall, these results demonstrate that PPeAT60 retains its key properties after chemical recycling, establishing methanolysis as a promising platform for recycling of this partially biobased polymer that may be able to replace both conventional polyolefins and PBAT in flexible packaging applications.

09 BIOMASS FUELS↗

DOE OSTI2020

Constraining the behavior of gallium isotopes during evaporation at extreme temperatures

Renewed interest in gallium isotope systematics has stemmed from the fact that Ga is moderately volatile and is hypothesized to undergo kinetic fractionation during evaporation. In this work, we present the first Ga isotope data from terrestrial volatile depleted samples including a suite of experimentally heated rhyolitic soils, fallout melt glass, and splash-form tektites from the Australasian strewn field (hereafter termed australite tektites). The Ga in these samples is isotopically heavy compared to Ga in terrestrial basalts and estimates for the composition of the bulk silicate Earth (BSE). For each sample suite the isotopic fractionation of Ga scales with the degree of Ga depletion, consistent with isotopic fractionation caused by evaporation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Evaluation of several relevant fractionation processes as possible explanation for radioxenon isotopic activity ratios in samples taken near underground nuclear explosions in shafts and tunnels

Gas samples taken from two historic underground nuclear tests done in 1989 at the Nevada National Security Site (NNSS), formerly the Nevada Test Site (NTS), were examined to determine how xenon isotopes fractionate because of early-time cavity processes, transport through the rock, or dispersal through tunnels. Xenon isotopes are currently being used to distinguish civilian sources of xenon in the atmosphere from sources associated with underground nuclear explosions (UNEs). The two nuclear tests included (1) BARNWELL, a test conducted in a vertical shaft approximately 600 m below ground surface at Pahute Mesa, and (2) DISKO ELM, a horizontal line-of-sight test done in P-tunnel approximately 261 m below the surface of Aqueduct Mesa. Numerical flow and transport models developed for the two sites had mixed success when attempting to match the observed xenon isotope ratios. At the BARNWELL site, the simulated xenon isotope ratios were consistent with measurements from the chimney and ground surface and appeared to have been affected primarily by fractionation during subsurface transport. At the DISKO ELM site, samples taken from two elevations in the chimney failed to show the degree of fractionation predicted by the models during transport and did not show evidence for significant fractionation due to early-time condensation of refractory xenon-precursor radionuclides into the melt glass. Gas samples taken from the adjacent tunnels in the days following the test showed mixed evidence for early-time separation of xenon isotopes from their iodine precursors.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2021

Iron-rich microstructure records of high temperature multi-component silicate melt behavior in nuclear fallout

Above-ground nuclear explosions that interact with the surface of the earth entrain materials from the surrounding environment, influencing the resulting physical and chemical evolution of the fireball, which can affect the final chemical phase and mobility of hazardous radionuclides that are dispersed in the environment as fallout particles. The interaction of iron with a nuclear explosion is of specific interest due to the potential for iron to act as a redox buffer and because of the likelihood of significant masses of metals to be present in urban environments. We investigated fallout from a historic surface interacting nuclear explosion conducted on a steel tower and report the discovery of widespread and diverse iron-rich micro-structures preserved within the samples, including crystalline dendrites and micron-scale iron-rich spheres with liquid immiscibility textures. We assert these micro-structures reflect local redox conditions and cooling rates and can inform interpretation of high temperature events, enabling new insights into fireball condensation physics and chemistry when metals from the local environment (i.e. structural steel) are vaporized or entrained. Finally, these observations also significantly expand the availability of silicate immiscibility datasets applicable to rapidly quenched systems such as meteorite impact melt glass.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2023

Heat capacity of microgram oxide samples by fast scanning calorimetry

Quantitative scanning calorimetry on microgram-sized samples opens a broad, new range of opportunities for studying the thermodynamic properties of quantity-limited materials, including those produced under extreme conditions or found as rare accessory minerals in nature. We calibrated the Mettler Toledo Flash DSC 2+ calorimeter to obtain quantitative heat capacities in the range 200–350 °C, using samples weighing between 2 and 11.5 μg. Our technique is applied to a new set of oxide materials to which it has never been used before, without the need for melting, glass transitions, or phase transformations. Heat capacity data were obtained for silica in the high pressure stishovite (rutile) structure, dense post-stishovite glass, standard fused quartz, and for TiO2 rutile. These heat capacities agree within 5%–15% with the literature values reported for rutile, stishovite, and fused SiO2 glass. The heat capacity of post-stishovite glass, made by heating stishovite to 1000 °C, is a newly reported value. After accurate calibrations, measured heat capacities were then used to calculate masses for samples in the microgram range, a substantial improvement over measurement in conventional microbalances, which have uncertainties approaching 50%–100% for such small samples. Since the typical uncertainty of heat capacities measured on 10–100 mg samples in conventional differential scanning calorimetry is typically 7% (1%–5% with careful work), flash differential scanning calorimetry, using samples a factor of 1000 smaller, increases the uncertainty of heat capacity measurements by a factor of <3, opening the door for meaningful measurements on ultra-small, high-pressure samples and other quantity-limited materials.

Instruments & Instrumentation↗

DOE OSTI2022

Thermophysical modeling of raw glaze liquidus temperature and viscosity

Raw glazes, which do not contain pre-melted glass frits, are widely used due to their low cost. The natural variability of the mineral compositions used in raw glazes affects their viscosity during firing. Molten glaze viscosity plays an important role in determining the final surface quality; therefore, it is important to determine how raw glaze composition and firing conditions affect viscosity. Thermophysical modeling provides a way to evaluate the liquidus temperature and viscosity of molten glazes as a function of composition and oxygen activity. Equilibrium phase volume fraction and composition of 242 raw glaze recipes were evaluated under oxidizing and reducing conditions. Undissolved or precipitation of solid phases explain the secondary flux transition from anti-fluxing to fluxing near the liquidus temperature. The liquidus temperature and viscosity of iron glazes decrease as a function of increasing iron content under a reducing atmosphere. The empirical probability distribution of molten glaze viscosity follows a lognormal distribution, with lead glazes having significantly lower viscosity compared with glazes without lead. Here, the peak firing temperature viscosity of lead-free glazes is near the working point of glass. Multiple linear regression analysis shows that the peak firing temperature viscosity and liquidus temperature significantly predict the viscosity factor.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Literature Review of Thermomechanical Analysis, Its Instrument Components and Applications

Thermomechanical analysis (TMA) is used to measure the dimensional changes in a sample as a function of temperature. TMA allows for several modes of analysis, with expansion and compression being the most common. TMA is based on the theory of dilatometry and relies on the fact that polymers are viscoelastic materials, possessing both viscous and elastic properties. TMA yields information about the thermal effects on a polymer such as shrinkage, expansion, softening, melting, glass transition temperature and allows for the calculation of the coefficient of thermal expansion (CTE), which can be useful for many applications of polymers.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Literature Review of Thermomechanical Analysis, Its Instrument Components and Applications

36 MATERIALS SCIENCE↗

DOE OSTI2020

Radionuclide Screening Analysis and Transport Parameters for Pahute Mesa Detonations, Nevada National Security Site

A “screening analysis” is implemented at Pahute Mesa (PM), Nevada National Security Site (NNSS), to determine subsets of the 43 radionuclides listed in the radionuclide inventory of Finnegan et al. (2016) that are of relevance or potential relevance to the hydrologic source term (HST) for assessment of radionuclide transport in groundwater. Consideration is added to how levels of contamination are defined and whether any other radionuclides not in the inventory are relevant to the HST. A model is developed to estimate a range of possible source concentrations in groundwater that account for uncertainty in partitioning into melt glass and sorption into surrounding rock of the exchange zone for the 82 PM underground nuclear tests detonated in vertical shafts. The model also accounts for the varied hydrogeochemical settings. Transport parameters needed for the screening model calculations are developed from databases for hydrogeologic units, chemistry, mineralogy, fracture spacing, fracture aperture, fracture openness, matrix porosity, bulk density, saturation, and alteration. Of key importance is consideration of diagenetic zonation of the mineralogy related to hydrothermal alteration. The screening analysis compares model results with available groundwater radiochemistry data. Consistency between screening model results and available data helps validate the model for application to all 43 radionuclides, most of which have no measurements or only non-detect measurements of concentration in groundwater. The screening analysis determines that ten radionuclides – tritium, Sr-90, I-129, Cs-137, U-232, U-233, U-234, U-238, and the total of Pu-239 and Pu-240 are relevant to the HST. Determination of relevance is primarily based on data and/or model results indicating source concentration exceeding a maximum contaminant level (MCL) out to 100 years since the time of detonation. U-238 is relevant to assessment of contamination relative to MCLs for uranium and gross alpha particle activity. Five other radionuclides – C-14, Cl-36, Tc-99, Np-237, and Pu-238 – are determined potentially relevant to the HST based on a 0.1 MCL threshold. The screening analysis recommends additional attention to the natural daughter radionuclides of the uranium series (U-238) and thorium series (Th-232) decay chains, particularly Ra-226 and Ra-228, that were not included the inventory.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2021

Review of Cavity Radius and Chimney Height Information for Underground Nuclear Tests at Nevada National Security Site

Underground nuclear explosions release an immense amount of thermal and mechanical energy that alter the geologic materials surrounding the “working point” (WP = underground location) of the detonation. Explosion effects produce mechanically and thermally altered zones such as the “cavity,” “chimney,” and “melt glass puddle,”as well as concentric zones of crushed, compressed, and fractured rock extending away from the cavity wall.

58 GEOSCIENCES↗

DOE OSTI2022

Characterization of actinide abundances and isotopic compositions by HR-ICP-MS

In this report, we present actinide isotopic and elemental data from fallout melt glass using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). This is an analytical technique that requires minimal sample preparation. These data are directly compared to the results of high precision isotopic analyses and elemental assay by multi-collector (MC-) ICP-MS, which requires lengthy sample processing involving spiking and purifying aliquots of individual elements. The comparison shows broad overlap between the results of the two techniques. Thus, although the data obtained by HR-ICP-MS is of significantly lower precision, it is a viable method to obtain actinide elemental and isotopic data on a more rapid timeframe than traditional high-precision techniques.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Characterization of actinide abundances and isotopic compositions by HR-ICP-MS. Part 2: Results from actinide doping studies

Previously, we presented actinide isotopic and elemental data from fallout melt glass that was measured using high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). Direct comparison between these measurements and ‘gold standard’ data obtained by multi-collector ICP-MS showed broad overlap, indicating that HR-ICP-MS is a potentially valuable technique for producing actinide elemental and isotopic data on a relatively rapid timescale. To test the usefulness of this technique further, we doped varying amounts of uranium certified reference materials (CRMs) into a rhyolitic rock standard to establish the effects of uranium concentration and isotopic composition on the accuracy of uranium isotopic analyses by HR-ICP-MS. This also enabled us to quantify peak tailing effects from 238 U on the measurement of 239 Pu and 237 Np, which in turn allows us to constrain correction factors based on measured 237 Np/ 238 U and 239 Pu/ 238 U ratios. A second doping study involved the addition of a mixed actinide standard into three samples with different matrix compositions (termed soil, city, and seawater) to assess whether sample chemistry affects the accuracy and precision of these analyses. Results suggest that this is not the case. Systematic offsets were not observed in elemental or isotopic data derived from the three matrix samples. Results indicate that useful actinide isotopic data can be obtained from whole rock solutions by HR-ICP-MS. Our findings also have implications for solid sampling techniques such as laser ablation ICP-MS, which do not require sample dissolution.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2024

Compositional Variation Tests on DuraMelter 100 with LAW Sub-Envelope C2 Feed in Support of the LAW Pilot Melter (Final Report)

One of the principal objectives of the DM100 melter tests was to demonstrate that the LAW Sub-Envelope C2 feeds with ± 15% variations in the amounts of waste simulant are suitable for large-scale tests on the LAW Pilot melter. The other principle objective for the DM100 tests was to determine the relative effects of sugar versus waste organics on glass redox state, NOx emissions, sulfur emissions, sulfur retention in the glass, secondary sulfate layer formation, and glass-melt foaming. Additional objectives included measurement of the feed rheological properties and collection of melter emissions data. Screening tests are conducted at the DM100 scale in order to identify and correct potential problems before testing at the larger scale LAW Pilot melter. Testing goals were met in that the results of the DM100 melter test resulted in selection of LAW Sub-Envelope C2 feed suitable for Pilot Melter testing.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

AOI [1] Advanced Manufacturing of Ceramic Anchors with Embedded Sensors for Process and Health Monitoring of Coal Boilers

Researchers at West Virginia University (WVU) developed methods to fabricate and test ceramic anchors with an embedded sensor technology for monitoring the health and processing conditions within pulverized coal (PC) and fluidized-bed combustion (FBC) boiler systems. The technology included the development of advanced manufacturing processes for 2D/3D printing electroceramic (conductive ceramic) sensor designs within the ceramic anchor microstructure during the manufacturing process. This advanced manufacturing process would allow for the precise control of local microstructure and composition in order to engineer layer-by-layer any protective and electrically active materials within the refractory anchor. This 3D printing technology would permit the rapid and controlled design of the refractory microstructure and embedded sensor design throughout the volume of the ceramic anchor. The work also included a method to interconnect the sensors to boiler shell through the anchor clamp, where the sensor signals will be processed by low-power electronics and transmitted wirelessly to a central processing hub. The end-goal of the program was to produce a ceramic anchor sensor system which would be ready for implementation within a coal boiler, and/or other similar refractory liner systems (such as that in the glass and metal manufacturing areas). The project objectives were to: 1) Define the chemical and microstructural stability, in addition to the electrical properties, of oxide and non-oxide ceramic composites to be embedded within the ceramic anchor compositions that may operate up to 1400ºC; 2) Develop and implement the 2D/3D printing technology to pattern and control the microstructure of the ceramic anchor and embedded sensor circuits; 3) Develop an interconnect technology which will permit easy installation of the ceramic anchors and signal collection at the boiler shell; 4) Develop low power analog electronics and wireless communication hardware to efficiently collect the sensor signal at each processing unit and transmit data to a central hub for data analysis; 5) Demonstrate the smart ceramic anchor system for temperature and liner fracture within a high-temperature processing unit, such as a boiler furnace or glass melting furnace floor/wall liner.

20 FOSSIL-FUELED POWER PLANTS↗