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DOE OSTI2023

Progress Report: Continued Development and Advanced Testing of DPC Filler Cements

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Reinventing CEMENT: Carbonation-Enabled Mineralization to Engender Novel Technology

Cement is the most important building material used in civil infrastructure but it is extremely energy intensive to produce. We developed novel ways to make cements at low temperatures by mimicking the chemistry of the calcium silicate mineral pseudowollastonite. Pseudowollastonite is interesting because when it is exposed to hot (90-150oC), alkaline conditions with CO2 and water it reacts to form mineral phases that are much stronger than commercial cements. The resulting phases are also much more resistant to acid attack and have lower permeability, which will make them last longer. Many of the mineral phases in our cements are similar to those that exist in ancient Roman cements that have lasted thousands of years. Our objective was to understand how waste materials from industrial processes (such as power production, municipal solid waste treatment, or power plants) can be used to replicate the conditions that give pseudowollastonite cement its remarkable properties. We worked to optimize our formulations and incorporate the cements into concrete blends that the industry can test and consider using in different applications. Our cements could be used in pre-cast cement structural elements, which makes up nearly 20% of the total cement market and is growing rapidly. This work supports ARPA-E program objectives to significantly improve the industrial efficiency of materials production.

36 MATERIALS SCIENCE↗

DOE OSTI2022

High Yield, Economical and Environmentally Benign Production of Rare Earth Elements from Coal Ash [Abstract]

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2021

Reactivity in cement pastes bearing fine fraction concrete and glass from construction and demolition waste: Microstructural analysis of viability

Converting construction and demolition waste (CDW) into secondary raw materials is one of the priorities of environmental policy and circular economy strategy. This study analysed the variation in eco-efficient paste reactivity with OPC replacement ratio (5% to 10%) and hydration time (2 d, 28 d and 90 d). Three types of CDW were explored: two (calcareous and siliceous) consisting of fine (4 AH{sub 13} and C{sub 4}AcH{sub 11}, ettringite and portlandite, were the same as observed in OPC hydration. These findings attest to the scientific viability recycling such CDWs as mineral additions in eco-cement manufacture and consequently eliminating the need for stockpiling these materials at recycling/storage plants.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Biopolymer Concrete

Cement production for concrete has been responsible for ~7–8% of global greenhouse gas (GHG) emissions, and nearly equally contribution for steel production processes (EPA, 2020). In order to achieve carbon neutrality by 2050, a novel solution has to be investigated. This project aims to develop fundamental mechanistic understanding and experimental characterization to create a 3D printable biopolymer concrete using plant-based polyurethane as an innovative and sustainable alternative for Portland cement concrete, with significantly low carbon footprint. Future construction will utilize the advances in digital additive manufacturing (3D printing) to produce optimal geometries with a minimum waste of materials. Understanding the polymerization process, factors impacting the composite rheology, and the structural behavior of this biopolymer concrete will enable us to engineer the next generation of concrete structures with low carbon footprint. This project aims to improve the nation’s ability to control Greenhouse Gas emission neutrality for the set goal of 2050 via introducing a structurally viable bio-based polymer concrete.

42 ENGINEERING↗

DOE OSTI2024

Computational Analysis of the Effect of Structured Packing Design on Absorption Column Hydrodynamics for Post-Combustion Carbon Capture Applications

Solvent based post-combustion carbon capture technologies have a potential for reducing carbon emissions from fossil-fuel-fired power plants and industrial sources where CO2 emissions are inherently harder to mitigate, such as steel or cement industries. A prominent technology to achieve this is by retrofitting absorption columns to the existing infrastructure. While these systems have been among the less costly alternatives for carbon capture, they still impose a considerable energy penalty to the operation of power plants or industrial facilities. The optimization of CO2 capture rate in solvent-based absorption process is complex as it depends on several factors including CO2 solubility, solvent reaction kinetics and temperature effects on the solubility, reaction rates, surface tension, and thermophysical properties of the solvent and the flue gas. The overall heat and mass transfer also depends on the hydrodynamics, which in turn, is affected by the packing geometry. In the current work, we systematically quantify the effects the design of the structured packing has on the column hydrodynamics, by performing detailed CFD simulations for different geometrical configurations and operating conditions. We then obtain relationships between the key hydrodynamic metrics, such as liquid holdup, interfacial area, wetted area, and pressure drop to the parameters defining the packing geometries and identify new more effective packing designs for the given operating conditions.

Shah, Yash Girish↗

DOE OSTI2023

Continued Development and Advanced Testing of DPC Filler Cements (on FY22 R&D and Demonstration Activities) (Progress Report)

Commercial generation of energy by nuclear power plants in the United States (U.S.) has produced thousands of metric tons of spent nuclear fuel (SNF), the disposal of which is the responsibility of the U.S. Department of Energy (DOE). Utilities typically utilize the practice of storing this SNF in dual-purpose canisters (DPCs). DPCs were designed, licensed, and loaded to meet Nuclear Regulatory Commission (NRC) requirements that preclude the possibility of a criticality event during SNF storage and transport, but were not designed or loaded to preclude the possibility of a criticality event during the regulated post-closure period following disposal, which could be up to 1,000,000 years (Price, 2019). There are several options being investigated that could facilitate the disposal of SNF stored in DPCs in a geologic repository (Hardin et al., 2015; SNL 2020b; SNL 2021b). These include: (1) repackage the SNF into canisters that are designed to prevent criticality during the regulated post-closure period following disposal, but with an increased disposal cost estimated at approximately $\$$20B in United States dollars (USD) (Freeze et al., 2019); (2) analysis of the probability and consequences of criticality from the direct disposal of DPCs during a 1,000,000-year post-closure period in several geologic disposal media (Price, 2019); and (3) filling the void space of a DPC with a material before its disposal that significantly limits the potential for criticality over the post-closure regulatory period. This report further investigates the third option, filling DPC already containing SNF with a material to limit the potential for criticality over the post-closure regulatory period.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

A pilot-process for calcium hydroxide production from iron slag by low-temperature precipitation

The production of Ca(OH) 2 via thermal decomposition of limestone is an energy intensive process resulting in significant CO 2 emissions. However, if produced in a manner that obviates the need for the thermal decomposition of limestone, Ca(OH) 2 could be a “CO 2 -negative” material. Herein, we design and demonstrate the operation of a continuous, low-temperature (< 100 °C), aqueous-phase pilot-process to produce Ca(OH) 2 using calcium extracted from alkaline industrial wastes. The three-step process encompasses unit operations including: (i) calcium leaching from basic oxygen furnace BOF slag, (ii) leachate concentration by reverse osmosis (RO), and (iii) Ca(OH) 2 precipitation by temperature swing. Here this process presents several advantages compared to the traditional route. First, it advances the recycling of waste from the steel industry. Second, it operates significantly below the temperature used in conventional lime production (900 °C) as it bypasses limestone calcination, responsible for ~65% of the CO 2 emissions from the current process. Thus, the new process has a lower CO 2 footprint and enables the use of industrial waste heat. The mass and energy balances were quantified to reveal that increasing the calcium concentration of the feed solution and the precipitation temperature, decrease the energy demands of the RO step, thereby reducing the process’s overall CO 2 footprint. The pilot system operated continuously and achieved a production rate of nearly 1 kg per day of Ca(OH) 2 with a purity greater than 95 wt%. The average particle size of the precipitates depended on the residence time in the precipitation reactor, demonstrating an ability to produce size-controlled particulates. Importantly, the process achieved full water recirculation/reutilization level indicative of a low-consumable water demand. The outcomes offer new insights and understanding relevant to developing and upscaling low-CO 2 processes for cement, lime, and portlandite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Solidification of SRPPF Aqueous Recovery Liquid: Process Disruptions

Savannah River National Laboratory has identified a magnesium oxysulfate grout formulation to solidify the liquid effluent from the Savannah River Plutonium Processing Facility (SRPPF) Aqueous Recovery System (ARS). The formulation uses reactive, light burnt MgO, anhydrous MgSO 4 , and dead burnt MgO and provides good mixability, similar density to the original Portland Cement-based mix, and a leachate pH of 9.39, within the assumed Waste Isolation Pilot Plant (WIPP) brine pH range. The formulation will solidify the effluent using a solid first, lost paddle design, within a 55-gallon drum. A series of seven different process disruptions, or irregular processing during the expected ARS liquid effluent solidification process, were completed to assess the severity of the impact of the process disruption and how the formulation behaves under these conditions. Seven process disruptions were investigated including: No Mixing, Partial Mixing, Compacted/Stratified, Sealed, Overfilled, Underfilled, and Undermixed. The impact on solidification, leachate pH, Er (a Pu/Am surrogate) distribution, and density of the resulting grout were established. Overall, four of the process disruptions, No Mixing, Partial Mixing, Compacted/Stratified, and Overfilled, resulted in basic, unabsorbed liquid that would require additional solidification to be acceptable for WIPP. Most solids generated in this testing met the expected WIPP leachate pH requirements. Solids from the Compacted/Stratified process disruption test, however, produced a leachate pH slightly above the assumed range in the WIPP performance assessment. The distribution of Er for most of the tests was relatively consistent. The No Mixing process disruption test, however, resulted in non-homogeneous Er distribution, indicating that radioactive material would not be evenly distributed throughout this solid’s matrix. The Overfilled test is the only mix with a density slightly below the acceptable value. The Sealed and Overmixed tests produced a solid closest to the standard mix with no unabsorbed liquid, expected leachate pH levels, consistent Er concentrations, and expected density, indicating these process disruptions do not have a negative impact on the final grout form. Based on the other process disruptions, it is critical to have premixed dry materials and a well-defined mixing process to produce a solid, homogeneous magnesium oxysulfate cement, with no unabsorbed liquid. These process disruption tests show that the lack of adequate mixing is fundamental to creating an improperly solidified material that may require remediation.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Radiation Effects in Concrete for Nuclear Systems

Concrete is massively used in the construction of critical safety-related components in nuclear power plants. Among those, the concrete biological shield is exposed to high levels of neutron and gamma irradiation exiting the reactor pressure vessel. This article provides a comprehensive overview of the state-of-the-art knowledge on irradiated concrete. First, the fundamental irradiation-induced degradation mechanisms occurring at the level of the concrete constituents such as rock-forming minerals and hydrated cementitious phases are examined. The critical role of the mineralogical and chemical composition regarding concrete resistance against radiation effects such as amorphization, irradiation-induced expansion and radiolytic gas release are detailed. Second, the interactions between the varied irradiated phases are comprehensively analyzed and put in perspectives with the effects of prolonged irradiation on the structural properties of concrete aggregates, cement paste, and concretes. Finally, the significance of irradiation for the long-term operation of nuclear power plants is discussed in the light of the most recent knowledge and its limitations.

Le Pape, Yann↗

DOE OSTI2026

State of Innovation 2025: Progress in Accelerating Next-Generation Cement and Concrete Technologies

The cement and concrete sectors are entering a decisive period as next-generation technologies advance from laboratory research to demonstration, early deployment, and first-of-a-kind commercial plants. Building on the 2024 State of Innovation report, the 2025 outlook highlights both the rapid acceleration of innovation and the urgent need for coordinated action across the value chain. Venture capital activity into the cement and concrete space stabilized following the record surge of 2022-2023, yet landmark financings, such as Sublime Systems' $200 million round and Terra CO2's $124 million Series B, signal continued investor confidence in companies approaching commercialization. Corporate procurement has become a powerful new catalyst, with Microsoft, Amazon, and CRH (Cement Roadstone Holdings) Ventures providing long-term commitments that underpin the first wave of next-generation cementitious products. The sector is shifting from early-stage experimentation toward the scaling of well-capitalized leaders capable of bridging the critical "capitalization gap." Early innovators continue to expand the toolkit through novel binders, electrochemical cements, biogenic limestone, and carbonate mineralization pathways. Going into 2026, cost competitiveness, durability validation, and scalability enabled by resilient supply chains remain the decisive factors for market adoption. At the 2025 Next Generation Cement and Concrete Critical Technologies Meeting, attendees emphasized dual-track funding strategies that integrate federal grants with private capital as key to enabling market breakthrough. State programs and corporate demand are sustaining momentum, while successful companies increasingly demonstrate both economic value and reduced dependence on imported materials. The National Concrete Pavement Technology Center and others underscored that broad integration of next-generation materials will hinge on standards compatibility, verified field performance, and workforce readiness. Colorado continues to serve as a proving ground through pilot programs that combine supplier training, phased implementation, and real-world data to de-risk innovation and provide replicable models for other regions. The 2025 Cement and Concrete Critical Technologies Workshop reinforced that scaling next-generation materials will require alignment among technology innovation, performance validation, and market demand. Stakeholders must move beyond siloed efforts toward collaborative frameworks that coordinate standards, funding, and infrastructure deployment. As a neutral convener and technical validator, the National Laboratory of the Rockies (NLR) plays a pivotal role in bridging innovation and market adoption through collaborative research, technology validation, and entrepreneurship programs. By uniting innovators, incumbents, policymakers, contractors, and investors, NLR and its partners are helping chart a credible pathway toward widespread commercialization in the decade ahead.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2020

Sulfuric Acid Improves the Reactivity of Zeolites via Dealumination

The demand for supplementary cementitious materials (SCMs), like fly ash, slag, and silica fume, is projected to rise over the next few decades. However, global decarbonization efforts, such as decommissioning of coal-fired power plants, will limit the supply of SCMs. Therefore, alternative SCM sources are a critical need for the cement and concrete industry. However, the high crystallinity of zeolites limits their pozzolanic reactivity. The goal of this work was to improve the reactivity of two common zeolites, namely clinoptilolite and SSZ-13, by treating them with sulfuric acid. The treatment enhanced zeolite reactivity via dealumination and decreased particle sizes, which led to increased reactivity with calcium hydroxide, as indicated by a 42.0% increase in reaction heat measured by isothermal calorimetry. Here, we elucidate mechanistic understanding that smaller particle sizes induced by acid treatment accelerated peak heat evolution, while free aluminates from dealumination increased heat via direct reaction with aqueous Ca 2+ .

36 MATERIALS SCIENCE↗

DOE OSTI2022

High Yield, Economical and Environmentally Benign Production of Rare Earth Elements from Coal Ash (Phase II Final Summary Report)

Fly ash stored in landfills and ponds across the United States is an attractive, abundant domestic resource for the cost-effective recovery of rare earth elements (REE) and other critical minerals (CM). Physical Sciences Inc. (PSI) and its team members, Winner Water Services (WWS) and University of Kentucky/Center for Applied Energy Research (UK/CAER) successfully executed a multiphase program that developed technologies and their implementation in a pilot plant. We demonstrated plant operations for cost-effective and environmentally-friendly production of rare earth element oxide (REO) concentrates, and the critical minerals scandium and aluminum (in the forms of salts or oxide products), from coal ash. We also constructed and demonstrated a research-scale (0.5 kg/day) micropilot facility to validate the key physical and chemical processing operations, predict yields, and troubleshoot process bottlenecks. The project team then designed, constructed and operated two decoupled pilot plants: (1) an operational pilot plant for physical separation processes with capacity of 0.4 metric tons per day (tpd), where we optimized processes to produce selected ash fractions as the feedstock for chemical processing and as valuable byproducts such as cenospheres, magnetic ash, and secondary fuel carbon, and (2) an operational pilot plant for chemical ash processing with a capacity of 0.5 tpd that developed optimized processes for the production of: (a) REO concentrates, (b) critical minerals (Sc, Al), and (c) beneficiated ash as a valuable byproduct suitable for cement applications. In Phase I, the project team (with Equinox Chemicals in place of WWS) developed and demonstrated the feasibility of the physical and chemical separation processes, developed the design of a pilot plant, and began the development of a preliminary techno-economic model. In the baseline (initial) Phase II program, the project team developed and demonstrated the above pilot scale plant, producing salable REE concentrates, including Y and Sc (REYSc), plus commercially viable byproducts, using environmentally safe and high-yield physical and chemical enrichment processes. The team successfully demonstrated chemical pilot design, construction, shakedown, and operations of the plant. We produced the Phase II deliverable REYSc concentrate ((50 g of >60 wt.% purity REYSc salts on elemental basis), generated the feed for the Phase II follow-on program, identified processing challenges for future optimizations, and refined the techno-economic model. In the Phase II follow-on program, the project team: (1) developed and demonstrated processes to increase the REE amount by 3X (content basis) and convert the Phase II REE salt mixture to an oxide mixture, (2) produced/delivered >38 g of REO mixture with >85 wt.% purity (elemental basis); (3) developed processes to recover critical minerals scandium and aluminum from intermediate streams; (4) produced/delivered > 1 g of scandium salt mixture with >85 wt. % purity (elemental basis); (5) produced/delivered > 100 g of aluminum oxide type material with >70% wt. purity (elemental basis); and (6) updated the techno-economic model from the baseline Phase II program to assess CAPEX and OPEX of a commercial operation. This program has developed extensive databases on process chemistry, unit operations, plant engineering, and techno-economics that will enable further scale-up toward commercial plant design. Specific future developments will be focused on achieving dramatic savings in energy, reagent usage, and operating costs. The combined results will contribute significantly for maturing the technologies of REE recovery from coal byproducts and promote the establishment of domestic REE and CM supply chains.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

LDR Inorganic Spiked Simulants in Pozzolan-Substituted Cast Stone for Hanford Pretreated Low-Activity Tank Waste

Pretreated Low Activity Waste (PTW/LAW) at the Hanford Site, is currently projected for disposition through a cementitious waste form. The current standard formulation, Cast Stone, uses Class F fly ash, blast furnace slag, and Portland cement. However, the future availability of Class F fly ash is uncertain, as many coal-fired power plants—the source of this byproduct—are being decommissioned or converted to natural gas. This issue has prompted research into identifying and evaluating suitable alternative materials to replace fly ash in the cementitious waste forms used by the Department of Energy (DOE). The Savannah River National Laboratory (SRNL) successfully identified four natural pozzolans for the replacement of Class F fly ash in the current Savannah River Site (SRS) low-level waste (LLW) form, Saltstone.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Evaluation of Pozzolan-substituted Cast Stone for Pretreated Hanford Tank Waste

Portland cement. The future availability of quality Class F fly ash has come into question as coal-fired power plants are being converted to gas or taken offline. Consequently, alternative pozzolanic reagents are being evaluated for fly ash replacement in cementitious matrices for treating radioactive waste and debris. In 2023 and 2024, Savannah River National Laboratory (SRNL) was funded to evaluate natural pozzolans for the replacement of Class F fly in the Savannah River Site (SRS) Saltstone formulation. Based on the promising results and uncertain availability of Class F fly ash in the northwestern US, Hanford Tank Waste Operations & Closure, LLC (H2C) requested SRNL to evaluate the potential for substituting natural pozzolans in the Hanford West Area Pretreated Low Activity Tank Waste (PTW/LAW) Cast Stone formulation1 . Task 1 in this request was to determine the change in Cast Stone volume resulting from stabilization/solidification of 1 L of PTW/LAW tank waste. The densities of three (Hess Pumice, tephra pumice, and clinoptilolite zeolite) pozzolan-substituted Baseline Cast Stone mixes were determined, and volume changes relative to the fly ash-Baseline Mix with a water-to-dry mix = 0.40 were calculated.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Quantifications of growth rate and particle size of magnesium silicate hydrate cement using small‐angle X‐ray scattering

The focus of recent research on cement binders has shifted to alternatives such as magnesium silicate hydrate (M-S-H) to mitigate the environmental impact of conventional concrete production. However, a detailed understanding of the morphology and growth rate of M-S-H, which informs its applicability as a cementing agent, is lacking. These properties are important as they influence cement hydration and consequently the development of macroscopic properties. Here, in this study, the particle size distribution and growth rate of M-S-H synthesized by mixing aqueous stock solutions were analyzed using synchrotron-based small-angle X-ray scattering. The reaction solutions contained dissolved magnesium and silicon with concentrations ranging from 2 to 500 mM, corresponding to saturation indices with respect to M-S-H endmembers, M 0.75 -S-H and M 1.50 -S-H, between 5.8 and 10.3. The precipitation rates of M-S-H align with affinity-based kinetic models and can be described by the following equations: For M 0.75 -S-H: 𝑟 M 0.75 −S−H =10 −9.54±0.70 ⁢(Ω$^{0.59±0.08}_{M_{0.75}⁢\textrm{SH}}$−1), and for M 1.50 -S-H: 𝑟 M 1.50 −S−H =10 −7.56±0.37 ⁢(Ω$^{0.34±0.04}_{M_{1.50}⁢\textrm{SH}}$−1), where 𝑟 is the rate in mol/L/s, and Ω represents the saturation ratio with respect to M-S-H. Moreover, we observed that changing the [Mg]/[Si] ratio affects particle size, a trend that cannot be fully explained by changes in the saturation index alone. These insights are critical for improving the predictability and control of cementation in concrete that utilizes M-S-H-based binders.

M-S-H↗

DOE OSTI2021

Lawrence Livermore National Laboratory (LLNL) Hybrid-Energy Technology for Power and Industrial Heat with Near-Zero or Negative CO 2 Emissions

Major contributors to global CO 2 emissions include electricity (27%) and industry (23%), such as cement manufacturing (8%). Using post-combustion technology to reduce CO 2 emissions by 85-90% could increase the cost of generating electricity with fossil fuel by 40-70%, while increasing cement-manufacturing cost by 75-140%. Both sectors are under pressure to reduce CO 2 emissions and are seeking cost-effective, energy-efficient solutions to decarbonizing energy.

54 ENVIRONMENTAL SCIENCES↗

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↗