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DOE OSTI2026

Evaluation of Iron‐Phosphate Glass–Ceramic Waste Form for Electrorefiner Salt Waste Simulant Dechlorinated With Phosphoric Acid

The importance of glass and glass–ceramic nuclear waste forms has been reaffirmed in recent years by the growing interest in nuclear power as a reliable energy source. Determination of processing methods for the disposal of halide-containing wastes will be essential for the advancement of nuclear technologies such as non-aqueous fuel reprocessing. Phosphate-based dechlorination and subsequent vitrification of radioactive salt waste into an iron-phosphate waste form have been identified as a potential processing scheme for electrochemical processing waste. The impact of H 3 PO 4 -based dechlorination of complex salt mixtures on the vitrification process and structure of the final iron-phosphate waste form has not yet been investigated. In this work, iron-phosphate glass–ceramics were made from simulant salt waste (48LiCl–33KCl–19NaCl mol%) dechlorinated with the H3PO4-based method. The glass-forming region was compared to that of traditionally prepared Na 2 O–Fe 2 O 3 –P 2 O 5 systems. For a candidate glass-forming composition, the processing scheme presented here was determined to favor Fe 3+ species. The O/P molar ratio was consistent for the candidate composition when dechlorinated at 400°C and 600°C in air and argon environments, indicating glass network connectivity was maintained despite variations in processing parameters. The results presented here validate processing schemes requiring iron-phosphate waste form synthesis following H 3 PO 4 -based dechlorination.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2026

Direct Processing of Lithium Chloride Based Waste Salt in a Ceramic Waste Form

Ceramic waste form materials were fabricated with a LiCl based salt mixture to demonstrate the suitability of direct processing of waste salt from an all LiCl pyroprocessing flow sheet on the formation, microstructure, and durability of ceramic waste forms. Materials were successfully synthesized by using the simplified direct processing technique with salt loadings of 5, 7.5, and 10 wt% at the laboratory scale. Materials fabricated with LiCl based salt indicated full conversion of zeolite to sodalite occurred to form products with low open porosity. This indicates that the Na 2 O content of NBS4 glass is suitable for processing salt chemistries which do not contain NaCl. Generated sodalite was microencapsulated by the glass binder, halite occlusions were detected within sodalite domains at all salt loadings, and a Cs-rich phase believed to be Cs-pollucite was detected in the material made with the lowest salt loading (5 wt%). Salt inclusions were encapsulated within the binder glass at all loadings, and found to consist primarily of NaCl with Cs present. A small amount of salt was found at the surface of the wasteform made with the highest salt loading of 10 wt%, which may indicate an upper limit to the amount of salt that can be accommodated or incomplete mechanical mixing of the reagents. Durability testing by using the ASTM C1308 method indicated that initial rapid dissolution of exposed halite inclusion phases was directly correlated to salt loading. Wasteform degradation during all tests occurred primarily due to dissolution of the sodalite phase. Durability of the binder glass was found to increase as the waste salt loading increased. Results for the release of cations from the salt indicate the changes in wasteform durability and halite inclusion chemistry are strongly influenced by ion exchange phenomena between the salt and the glass. This appears to be the result of the relatively stronger affinity for the glass phase of Li, compared to that of other cations such as Na and Cs. The effects from cation exchange were diminished at lower salt loadings.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Synergy in Materials: Leveraging Phosphosilicate Waste Forms for Electrochemical Salt Waste

Here, waste forms containing glassy and crystalline phosphate and silicate phases were produced to immobilize salt waste simulants from pyroprocessing and characterized by using Raman spectroscopy, Mössbauer spectroscopy, X-ray diffraction, scanning electron microscopy, heat capacity, and chemical durability measurements. In this work, a phosphosilicate waste form is presented to leverage the benefits of both borosilicate glasses and iron phosphate glasses. To improve waste loading, prior to immobilization, salt simulants were successfully dechlorinated using ammonium dihydrogen phosphate, mixed with a borosilicate frit (5–30 wt %) and Fe 2 O 3 , and vitrified. Additions of 2.5–15 wt % borosilicate glass (NBS3) improved normalized release rates for Cs relative to iron-phosphates without NBS3, resulting in chemical durabilities similar to high-level waste borosilicate glass reference materials. The release rates of the alkalis (i.e., Li, Na, K, Cs) were the lowest with the addition of 5 wt % NBS3. Although Sr was not specifically targeted in this study, evidence exists that it preferentially partitioned with Si to form an amorphous droplet phase within the iron phosphate glass matrix.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Semi-Dynamic Leach Testing of Densified Silicon-based Iodine Waste Forms

Iodine waste forms (IWF) require a conceptual corrosion release model (CCRM) to provide iodine (I) release rates for performance modeling nuclear waste disposal repositories. To develop a CCRM, an understanding of the corrosion mechanisms of the IWF are required along with data from consistent test methods to parameterize the model. The present study has advanced both areas by providing and assessing the corrosion resistance of IWF types based on their processing history in minor variations of semi-dynamic leach tests. The test included a series of semi-dynamic leach tests using monolithic IWFs in deionized water (leachant). Several experiments were conducted under alternate test conditions with changes to temperature, leachant replacement, leachant pH, leachant volume, masking, and surface finish to elucidate if varying these conditions impacted IWF corrosion behavior. Tests were conducted on two classes of IWFs: (1) I-bearing silver-mordenite (AgZ) materials processed by hot isostatic pressing (HIP) at different temperatures, pressures, sizes, and times; and (2) I-bearing silver-functionalized silica aerogels (SFA) processed by either HIP or spark plasma sintering (SPS). The corrosion susceptibility of AgZ samples was influenced by HIP temperature and pressure. The SPS SFAs retained I far better than HIP SFAs. Additional findings in this study include: (1) The iodine dissolution rate decreased with decreasing temperature, (2) a common ion effect may occur and slow dissolution of the host phase if the leachant is not regularly replaced, (3) pH controls the dissolution rate, and (4) the iodine dissolution rate slows with extended test time (up to 224 days). Based on this work, these parameters should thus be represented when developing a CCRM.

corrosion↗
DOE OSTI2023

Aluminophosphate Waste Forms for Immobilizing Cations from Electrochemical Salt Wastes

This report provides experimental details and results of evaluating aluminophosphate waste forms for treating and immobilizing the salt cations from salt wastes generated during electrochemical reprocessing of used nuclear fuel. In the waste form process for these materials, chloride salt streams are reacted with NH 4 H 2 PO 4 , the chlorine is removed from the salts and driven off as NH 4 Cl (a solid condensate that can be captured), and then the product can be vitrified in conjunction with glass-forming chemicals (e.g., Fe 2 O 3 , Al 2 O 3 ) to create a high-durability waste form. This study was initiated with some literature review on aluminophosphates containing high alkali oxide content and some of this information is summarized in this report. Following literature review, three new samples were synthesized where two contained Fe 2 O 3 +Al 2 O 3 (i.e., samples G3 and G5 ) and one was only Al 2 O 3 (Fe 2 O 3 -free) (i.e., sample G6 ). In addition to these samples, G1 was also made, which is the baseline reference waste form referred to as DPF5-336 (made without Al 2 O 3 ). Samples G1, G3, G5, and G6 had phases of Li 3 Fe 2 (PO 4 ) 3 (likely), monazite (below XRD detection limits), AlPO 4 , and AlPO 4 , respectively. Characterizations on these materials included optical images, scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. These samples were shipped to Argonne National Laboratory for chemical durability testing. Depending on how the samples perform in these tests, an additional phase of aluminophosphate formulations could be designed and tested. This report completes the milestone M4FT-23PN030104041 with details provided in Appendix B.

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DOE OSTI2025

FY24 Development of Improved Grout Waste Forms for Alternative Low Activity Waste Treatment

Since the WTP Low Activity Waste (LAW) Vitrification Facility was not designed to process the entire inventory of Hanford LAW, up to half of the retrieved Hanford LAW will require supplemental immobilization. Immobilizing LAW in a cementitious waste form known as Cast Stone has been investigated as a possible candidate supplemental immobilization technology. In FY21, Washington River Protection Solutions, LLC (WRPS) tasked Atkins and the Vitreous State Laboratory (VSL) of The Catholic University of America (CUA) to perform testing to evaluate methods for reducing the release of COCs, particularly nitrate, 99Tc, and 129I, from cementitious waste forms made from aqueous LAW derived from Hanford Tank Waste. FY22 work built on the FY21 results and further developed formulations while targeting higher waste loadings. The objective of this work was to perform laboratory-scale testing to further refine the most promising formulation(s) that were identified in the FY23 work. The goal of the refinement was to further reduce the release rates for 99Tc, Cr, 129I, and nitrate while maintaining workability of the fresh grout, and to increase waste loading.

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DOE OSTI2024

Glass-bonded ceramic waste forms for immobilization of radioiodine from caustic scrubber wastes

Glass-bonded sodalite composite waste forms have been developed for the immobilization of liquid radioactive wastes resulting from off-gas treatment during aqueous reprocessing of used nuclear fuel, with a particular focus on 129I. The proposed composite waste form is comprised of aluminosilicate ceramic phases containing volatile radionuclides bonded with a glassy matrix. In this work, a suite of ten candidate low-temperature glass binders (ZnO-Bi2O3-based glasses and a Na2O-B2O3-SiO2 glass) were examined. Six glasses were mixed with caustic scrubber waste simulant previously converted into a sodalite-rich material (to provide glass fractions of 10 and 20 wt.%), uniaxially pressed into pellets, and sintered at 350 °C or 550 °C for 8 h in air. Iodine retention after heat treatment was assessed by neutron activation analysis, showing retention of 67-100 % of expected iodine. The aqueous durabilities of the resulting materials were then determined, following the ASTM C1308 standard test, showing iodine releases of 1 to 23 g m-2 after 4 d. The cumulative iodine release for the best performing system (a zinc-bismuth-borate glass binder) was <1 g m-2, and its iodine retention from processing was 67 %. The iodine releases compared favorably with other waste forms. In parallel, this best-performing composition was also consolidated via hot isostatic pressing (HIP) in a stainless-steel canister at 550 °C for 2 h under 100 MPa pressure. The HIPed sample was produced at the ~20 g scale and showed improved densification and minimal reaction with the canister.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

AI/ML-assisted Design of Phosphate Glass and Ceramic Nuclear Waste Forms

Borosilicate glass is the widely accepted waste form for immobilization of high and medium level nuclear wastes. Advances in nuclear energies and new reactor designs require the development of new waste forms. For example, wastes from molten salt reactors and reprocessing of nuclear fuels lead to salt-based wastes that are difficult to be immobilized by conventional borosilicate glasses due to limited solubility and waste loading. In designing new waste forms, machine learning (ML) and artificial intelligence (AI) based approaches are much needed and can be beneficial in enabling a more efficient design in large parameter spaces as compared to traditional Edisonian trial-and-error approaches. Here, we report in this paper the rationale and latest progress of our ML/AI-based design of phosphate-based waste forms.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

FY22 Development of Improved Grout Waste Forms for Supplemental Low Activity Waste Treatment

About 54 to 56 million gallons of radioactive mixed waste is currently stored in underground tanks at the United States Department of Energy’s (DOE’s) Hanford site in the State of Washington. This waste will be separated into low- and high activity waste fractions, which will then be vitrified respectively into Immobilized Low Activity Waste (ILAW) and Immobilized High Level Waste (IHLW) products for subsequent disposal. The ILAW product will be disposed of in an engineered facility at the Hanford site while the IHLW product is designed for acceptance into a national deep geological disposal facility for high level nuclear waste. Treatment of the tank waste will take place in the Hanford Tank Waste Treatment and Immobilization Plant (WTP), which is under construction. However, since the WTP Low Activity Waste (LAW) Vitrification Facility was not designed to process the entire inventory of Hanford LAW, up to half of the retrieved Hanford LAW will require supplemental immobilization. Immobilizing LAW in a cementitious waste form known as Cast Stone has been investigated as a possible candidate supplemental immobilization technology

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Developments in Processing Criteria for Iron Phosphate Waste Form Design for Treating Electrorefiner Salt Wastes

This report describes work done under a Nuclear Energy University Partnership (NEUP) project that included a collaborative effort between Pacific Northwest National laboratory, University of Nevada Reno, University to Utah, and Missouri University of Science and Technology. In this project, the main goals were the following: (1) to assess H3PO4 dechlorination parameters for halide removal from salt simulants, (2) to evaluate crucible compatibility with iron phosphate glass melts, and (3) to evaluate waste form properties within a ternary system of P2O5 (added as H3PO4), Fe2O3 and fission product simulants.

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DOE OSTI2025

Evaluating High-Halide Waste Form Options for Salt-Based Nuclear Waste Simulants

In this study, waste forms were being explored for an electrochemical salt simulant, , referred to as ERV3, which is a high-LiCl/KCl salt containing simulated fission products (i.e., Sr, Cs, Nd) and Na to represent bond sodium from Experimental Breeder Reactor-II metallic fast reactor fuel. The goal was to find glassy systems that could be used to immobilize the salt in a single-step process. The envisionment of this process would be find a frit glass that could be added to the salt waste, heat treated, poured into waste canisters, and then stored for disposal. To perform this study, a literature review was conducted, the most promising seven systems were fabricated without the salt, and then mixed with salt simulant and heat treated under different processes. The criteria that were used to screen potential compositions included demonstrated alkali incorporation, could be melted at reasonably low temperature ( T ≤ 1000°C), and if the compositions had some demonstrated data for waste-form-related properties, that was a benefit. High marks were given for compositions that showed amorphous nature after slow cooling of samples containing ERV3.

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DOE OSTI2023

Computational Materials Design for Ceramic Nuclear Waste Forms Using Machine Learning, First-Principles Calculations, and Kinetics Rate Theory

Ceramic waste forms are designed to immobilize radionuclides for permanent disposal in geological repositories. One of the principal criteria for the effective incorporation of waste elements is their compatibility with the host material. In terms of performance under environmental conditions, the resistance of the waste forms to degradation over long periods of time is a critical concern when they are exposed to natural environments. Due to their unique crystallographic features and behavior in nature environment as exemplified by their natural analogues, ceramic waste forms are capable of incorporating problematic nuclear waste elements while showing promising chemical durability in aqueous environments. Recent studies of apatite- and hollandite-structured waste forms demonstrated an approach that can predict the compositions of ceramic waste forms and their long-term dissolution rate by a combination of computational techniques including machine learning, first-principles thermodynamics calculations, and modeling using kinetic rate equations based on critical laboratory experiments. By integrating the predictions of elemental incorporation and degradation kinetics in a holistic framework, the approach could be promising for the design of advanced ceramic waste forms with optimized incorporation capacity and environmental degradation performance. Such an approach could provide a path for accelerated ceramic waste form development and performance prediction for problematic nuclear waste elements.

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DOE OSTI2025

Reduction of Porosity in Cementitious Waste Forms to Reduce Effective Diffusivity

Although current practices meet regulations for grout waste forms, development of sequestration materials and techniques for contaminants of concern could expand the use of grout waste forms and reduce risk to established processes from future compositional changes. There are contaminants in waste streams that are not permanently and completely sequestered in current grout waste forms under certain conditions. These contaminants include methyl mercury, 129 I, 99 Tc, and nitrate. Each of these species have minor fractions that are not permanently and completely isolated from the environment and therefore potentially contribute to long-term environmental impacts. An approach of interest includes the technique of reducing porosity to result in reduced leachability of all contaminants simultaneously. The current Savannah River Site (SRS) saltstone formulation was used to evaluate the relationship between leachability and porosity reduced waste forms by altering the water-to-binder ratio. Results indicated decreasing the water-to-binder directly reduced porosity and resulted in the waste form’s ability to more effectively immobilize nitrate. This work was funded by the Department of Energy Office of Environmental Management (DOE-EM) Technology Operations Office (TOO) Project # HQ221818.

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DOE OSTI2023

The Center for Performance and Design of Nuclear Waste Forms and Containers (WastePD) Energy Frontier Research Center (Final Report)

The DOE Office of Environmental Management is responsible for high level nuclear waste that must be safely isolated from humans and the environment for extremely long periods. The waste forms and containers are made of glass, ceramics, and metals. Verified safe disposal requires understanding the fundamental mechanisms of waste form degradation and the design of new waste forms with improved performance, which comprise the goals of the Energy Frontier Research Center known as the Center for the Performance and Design of Nuclear Waste Forms and Containers, WastePD. WastePD was constructed to develop innovative approaches and solutions to those goals through the synergistic interactions of individuals who are experts in the degradation behavior, modeling, and design of glasses, ceramics and metal alloys. WastePD is the first center ever created to address this diverse group of materials in a comprehensive and coordinated manner. The science goals are grouped into three common topics: corrosion mechanisms via advanced characterization, environmental impacts, and materials design. Synergistic interactions in these areas were a key component of WastePD. The fundamental understanding of the degradation mechanisms of the waste forms and containers as well as the development of new materials with improved properties will allow DOE to prevent environmental contamination and to explore totally new repository concepts. WastePD was operational from August 2016 through July 2022, but the DOE support was drastically reduced for the last two years. This final technical report covers the full period of performance. However, much of what was accomplished in the first four years is nicely summarized in a review paper published in 2021, which is appended to this report. Therefore, this final report focuses on the technical findings from the last two years of WastePD activities. Considerable progress was made in the areas of a) the environmental and compositional impacts on the corrosion of borosilicate and aluminosilicate glasses, b) the mechanism of glass corrosion and the structure and evolution of the surface alteration layer, c) the effects of environment and composition on the corrosion of pyrochlore, perovskite, hollandite, and other oxide ceramics, d) the corrosion mechanism of multi-principal element metallic alloys, and e) a new framework for understanding the pitting corrosion of metals.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Replacement of Fly Ash with Natural Pozzolans in Cementitious Waste Forms

OBJECTIVE Address long-term and emerging issues for Cementitious Waste forms • Future availability of fly ash from coal fired power plants is uncertain • Improve waste form properties • Regionally available ingredients • Reduce cost and embodied Energy • Increase Salt Solution Waste Loading (water : cementitious reagents) in cement waste forms

Hill, Katie A. [Savannah River National Laboratory↗
DOE OSTI2025

Thermal properties and Thermodynamic Equilibrium Modeling of Cementitious Waste Forms

INTRODUCTION Cementitious matrices are used in the US DOE complex and worldwide to solidify aqueous radioactive, hazardous, mixed salt solutions, and sludges to meet low-level radioactive waste (LLW) disposal requirements. Blended formulations are used for most waste form mix designs. Substitution of pozzolans for Class F fly ash has the potential to alter the processing properties and stabilization properties of the resulting waste forms because they add chemical and mineralogical complexity to the final material. The Savannah River Site saltstone waste form was selected as the test case material. CemGEMS software was chosen as the model for predicting hydrated cementitious phases assemblages and phase evolution. Isothermal calorimetry was used as the method for evaluating processing and properties of fresh, uncured waste forms. The test cases consisted of reference case saltstone, and five natural pozzolan substituted saltstone mixes.

Bustamante, Michael E. [Savannah River National La↗
DOE OSTI2022

Modeling Activities Related to Waste Form Degradation: Progress Report

This report represents the milestone deliverable M4SF-22SN010309092 “Modeling Activities Related to Waste Form Degradation: Progress Report” that describes the progress of R&D activities of ongoing modeling investigations specifically on nuclear waste glass degradation, Density Functional Theory (DFT) studies on clarkeite structure and stability, and electrochemical model development of spent nuclear fuel (SNF). These activities are part of the Waste Form Testing, Modeling, and Performance work package at Sandia National Laboratories (SNL). This work package is part of the “Inventory and Waste Form Characteristics and Performance” control account that includes various experimental and modeling activities on nuclear waste degradation conducted at Oak Ridge National Laboratory (ORNL), SNL, Argonne National Laboratory (ANL), and Pacific Northwest National Laboratory (PNNL).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Alternative Pozzolans for Replacement of Fly Ash in Grout: Literature Review for Continuous Improvement of Cement Waste Forms

The Department of Energy (DOE) is currently responsible for treating radioactive and mixed waste, performing environmental restoration, and closing contaminated tanks and facilities resulting from nuclear weapons production during the Cold War. Cementitious reagents are the most widely used materials for (1) chemically stabilizing and encapsulating radionuclides and hazardous metals and (2) solidifying radioactive wastewater. Cementitious grouts and flowable concretes are also the most widely used materials for tank and facility closures and are used extensively for physical as well as chemical stabilization in environmental restoration projects. Ambient temperature radioactive waste cementation is a widely used technology for producing waste forms for final disposal. The current practice of designing and testing waste forms is based on a mid to late 20th century technology approach (i.e., materials, characterization, and test methods) for generating parameters for risk assessments. DOE technology development is needed to address both current, long-term, and emerging issues in this area as new waste streams come online and as regulations, performance knowledge, and risk assessment methodology continue to evolve. Consequently, the use of cementation as a means of treating chemically challenging radioactive liquid waste streams and reactive debris requires an enduring effort.

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