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DOE OSTI2022

Analysis of DWPF Sludge Batch 6 (Macrobatch 7) Pour Stream Glass Samples

The Defense Waste Processing Facility (DWPF) began processing Sludge Batch 6 (SB6), also referred to as Macrobatch 7 (MB7), in June 2010. SB6 is a blend of the heel of Tank 40 from Sludge Batch 5 (SB5), H-Canyon Np transfers and SB6 that was transferred to Tank 40 from Tank 51. SB6 was processed using Frit 418. During processing of each sludge batch, the DWPF is required to take at least one glass sample to meet the objectives of the Glass Product Control Program and to complete the necessary Production Records so that the final glass product may be disposed of at a Federal Repository. Four pour stream glass samples and two Melter Feed Tank (MFT) slurry samples were collected while processing SB6. The samples were transferred to the Savannah River National Laboratory (SRNL) where they were analyzed.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Characterization of Saltstone Grout Line Samples

During a prestart recirculation operation in the Saltstone Processing Facility (SPF), operations staff noticed hardened scaling falling into the hopper. As a result, SPF operators and Saltstone Engineering decided to postpone operation and conduct a process room hopper cleanout. During the cleanout effort personnel noted greater than normal buildup of damp solid material in the transfer line. A borescope investigation was conducted and confirmed buildup was present throughout the transfer line to the downstream valves. Savannah River National Laboratory personnel were asked to characterize the scale material and samples collected from the saltstone grout line and provide recommendations and/or further guidance as to whether additional corrosion testing is needed for useful equipment operating life information. Based on the samples characterized results, the plug material contained only the 60:40 slag:fly ash saltstone. Portland cement in the original 10:45:45 Portland cement:slag:fly ash mix may result in a less abrasive slurry compared to the 60:40 slag:fly ash mix because the slag is > 95 % crushed angular, sharp edged glass. Saltstone grout erosion and corrosion testing of A36 carbon steel is needed to determine if the 60:40 mix is more abrasive and corrosive for A36 carbon steel than the 10:45:45 mix.

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DOE OSTI2021

Impacts of Substrate Thinning on FPGA Performance and Reliability [Slides]

Substrate thinning is necessary in devices with flip-chip BGA packages to enable both radiation testing and component qualification and high-spatial resolution beam-based failure analysis methods. We investigated three factors affecting device performance: subsurface damage from the thinning process, reduced heat spreading in thin substrates, and changes in device switching speed. We conclude subsurface damage to crystalline Si caused by the thinning process is removable with sufficient SiO 2 slurry polishing. Local temperature differences increase minimally in devices thinned to 3 μm. Compressive stress in the Si increases globally after device thinning and leads to slowing of ring oscillator frequency by about 0.5% compared to full-thickness devices. Future work will include extending the results to submicron Si thickness values, which also has important benefits for failure analysis, debug, and security assessments. We also plan to extend this type of work to other FPGAs and other devices like memory and processors.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Evaluation Of Glass Density to Support the Estimation of Fissile Mass Loadings in Sludge Batch 10 Glasses

Per a directive from the Department of Energy Savannah River Operations Office (DOE-SR) in 2008, the fissile mass loading concentration must remain below 897 g/m 3 in each high-level waste (HLW) glass canister produced by the Defense Waste Processing Facility (DWPF). To support Sludge Batch 5 (SB5) processing, the Savannah River National Laboratory (SRNL) developed a technical basis that facilitates the evaluation of fissile mass loading of the glass product. The calculation is based on the iron (Fe) concentration in the glass as determined by measurements from the Slurry Mix Evaporator acceptability analysis as well as the glass density. In April 2022, a subsequent DOE-SR directive increased the fissile mass loading limit to 2500 g/m 3 beginning with Sludge Batch 11. Thus, the 897 g/m 3 limit still applies to Sludge Batch 10 (SB10) processing. For SB5 through initial Sludge Batch 9 (SB9) processing prior to coupled operation with the Salt Waste Processing Facility (SWPF), SRNL provided DWPF a bounding glass density value that was based on a statistical evaluation of density measurements. To eliminate the need for experimental work, a composition-based density model for HLW glasses was developed at SRNL in 2019. The objective of this report is to present the bounding glass density determined with the composition-based density model for SB10 sludge-only (SO) and coupled processing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Radioactive Waste Sludge Washing and Demonstration of the Nitric-Glycolic Acid Flowsheet for Sludge Batch 10 Qualification

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) performs qualification testing to demonstrate that the sludge batch (SB) is processible. During processing of SB9, DWPF will be transitioning from the Nitric-Formic Acid (NFA) flowsheet to the Nitric-Glycolic Acid (NGA) flowsheet. Thus, the qualification of SB10 was requested to only be performed using the NGA flowsheet. In order to qualify the batch for the NGA flowsheet, Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) cycles, designated SC-19, were performed using SB10 Tank 51 sample material. SRNL received Tank 51 material in the midst of Tank Farm washing. SRNL continued the washing in the SRNL Shielded Cells. The SRNL process included the addition of Sodium Reactor Experiment (SRE) material from H Canyon, simulating the transfer of SRE from H Canyon to Tank 51 during Tank Farm washing. The washed SB10 Tank 51 material, with SRE, was characterized prior to flowsheet qualification testing.

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DOE OSTI2022

M-Star® Software Test and Verification for Impeller Mixing in a Tank

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DOE OSTI2023

Evaluation of Glass Density to Support the Estimation of Fissile Mass Loadings in Sludge Batch 10 Glasses

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

M-Star ® Modeling of SME Mixing with Three Impeller Blades

Before a sample of the Slurry Mix Evaporator (SME) can be taken, the SME product sampling procedure requires that the agitator power be stable between 20 and 30 kW for at least one hour. The SME transfer to Melter Feed Tank (MFT) procedure also requires the SME agitator power be stabilized between 20 and 30 kW prior to transfer. These requirements are specified to ensure samples are homogeneous, as discussed in the Waste Form Qualification Report. During SME Batch 804, the agitator power dropped to 19 kW and struggled to achieve and maintain 20 kW. It was later discovered that the cause of the power drop was due to one of the bottom blades of the agitator breaking off. Both the sample and the transfer occurred without the power stabilizing between 20 and 30 kW. Therefore, the quality of SME Batch 804 is indeterminate, and homogeneity was questionable. To evaluate mixing in the SME with a broken agitator containing only three blades (90 degrees apart with space for a missing blade) on the bottom impeller, the Savannah River National Laboratory (SRNL) was requested to perform computer simulations of impeller mixing in the SME using M-Star ® software. The simulations will be used to determine if SME Batch 804 was well mixed and satisfies homogeneity requirements.

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DOE OSTI2023

Milestone Report on Microstructure of Irradiated Sensors and Coupling Adhesive Bonds

This report describes the ORNL aspects of an NSUF project in collaboration between EPRI, ORNL, and NCSU. Preliminary characterizations at ORNL LAMDA laboratory on piezoelectric sensors and bonds before and after NCSU PULSTAR reactor irradiation. Five pre-irradiation and seven post-irradiation samples have been examined by scanning electron microscopy and related methods so far. Samples consisted of (Pb,Bi)(Sc,Ti)O 3 or LiNbO 3 ceramics. Bonding layers consisted of epoxy, zirconia, alumina, aluminosilicate, or a complex soda-lime type slurry.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Rheology of a Wet Waste Feedstock

The current study provides rheological characterization of a representative HTL feedstock, Wet Waste Feedstock # 22 (WW22), as a function of HTL-prototypic temperature and shear rates. Feed WW22 is derived from a regionally representative blend of food, waste water sludges, and FOG (fats, oils, and greases). Rheological characterization of WW22 as a function of temperature provides, in part, key information for development and economic assessment of HTL wet waste slurry handling and heating operations, which may facilitate improved design rigor and optimization of HTL unit operations.

09 BIOMASS FUELS↗

DOE OSTI2023

Technical Evaluation of Accelerated Basin De-Inventory Material Addition to Sludge Batch 11 (Rev. 1)

The Accelerated Basin De-inventory (ABD) program involves discarding spent nuclear fuel that is currently stored in L-Basin to the Defense Waste Processing Facility (DWPF) for vitrification. The first ABD discards will occur during the preparation of Sludge Batch (SB) 11. Savannah River Mission Completion has requested that the Savannah River National Laboratory assess the technical gaps related to the increased gadolinium poisoning requirement and the impacts of performing the Low Temperature Aluminum Dissolution (LTAD) process in Tank 51 with H-Canyon discards present. The following summarizes the evaluation of the impacts of increasing the quantity of gadolinium (and related topics) from what was previously evaluated in the SRNL studies of gadolinium-poisoned ABD material solubility, the overall ABD flowsheet review, and increasing the fissile mass loading in glass: 1) Based on literature surveys, there is no indication that organic interactions with gadolinium will be significant at the high pH (typically >13) conditions of the Concentration, Storage, and Transfer Facilities. Any interactions of gadolinium with organics in DWPF are not expected to adversely impact DWPF or downstream facilities. Thus, there is little-to-no residual risk from organic interactions with gadolinium [Gap closed]; 2) Adding depleted uranium to ABD material, targeting 235 U enrichment of 4.90% within each transfer window, will mitigate potential impacts from an increase in soluble 235 U enrichment during sludge washing and LTAD. The plan to take advantage of previous transfers and allow 235 U enrichment of >5% during the final transfer window carries a risk that Tank 51 supernate will have a 235 U enrichment of >5%, which should be evaluated for acceptance; 3) Increasing the gadolinium mass ratio to 3.0:1 Gd: 235 U(eq SLU ) should lead to the same or higher partitioning of gadolinium into the solid phase within the DWPF Chemical Process Cell, resulting in both liquid and solid phases with expected partitioning of Gd consistent with the prior solubility study [Gap closed for SB11]; 4) There are no expected impacts on DWPF melt temperature and melter operations due to the minimal ~0.2 weight percent (wt%) increase in Gd concentration relative to previous sludge batches [Gap closed for SB11]; 5) As observed previously, Gd is expected to enter the off-gas system via physical entrainment, but at a slightly higher concentration than what was observed for SB9 melter off-gas pluggage deposits (0.07 wt%) [Gap closed for SB11] ; 6) There are no expected impacts on DWPF recycle or the Recycle Collection Tank glycolate destruction process. [Gap closed for SB11]; 7) Gd is projected to be a trace component in the SB11 glass (<0.5 wt%) and can be ignored for process control. Trace components do not significantly impact glass durability, thus the conclusions of the previous Product Consistency Test evaluation at a fissile mass loading of 2,500 g fissile/m3 glass still applies to SB11. The ~0.1 wt% increase in Gd2O3 concentration relative to the previous study will not impact the predictability of SB11 glass with the DWPF Product Composition Control System (PCCS) models for durability or the acceptability of glass according to the Waste Acceptance Product Specifications (WAPS) criterion for product consistency [Gap closed for SB11]; 8) No additional Toxicity Characteristic Leaching Procedure testing is necessary for SB11 and the hazardous waste specification of the SB11 DWPF waste form is unchanged after the addition of the ABD stream [Gap closed for SB11]. The following summarizes the evaluation of the impacts of adding two-thirds of the ABD material to Tank 51 prior to LTAD: 1) The addition of two-thirds of the ABD increases overall aluminum mass from 1.39×10 4 kg to 1.64×10 4 kg (15.5% ABD Al). The form of the insoluble portion of the Al resulting from ABD addition should be the more readily dissolved Al(OH) 3 and amorphous forms. The portion of the ABD aluminum that is processed by LTAD is expected to be completely soluble, thus requiring that less of the boehmite in the sludge be dissolved to reach the same Al target in the SB. [Gap closed for SB11]; The expected LTAD impact on other components, as related primarily to the components in ABD, are discussed. Gd is expected to remain insoluble during LTAD and not impact the solubility of other components. [Gap closed for SB11]; The addition of two-thirds of the ABD increases overall projected SB11 uranium mass from 4,740 kg to 13,100 kg (63% ABD U) and the projected plutonium mass from 86.0 kg to 89.5 kg (3.9% ABD Pu). The addition of all of the ABD increases overall projected SB11 uranium mass from 4,740 kg to 16,100 kg (70% ABD U) and the projected plutonium mass from 86.0 kg to 90.4 kg (5.3% ABD Pu). The 235 U enrichment will be ≤5%. The fissile uranium will be adequately poisoned by Gd and the fissile Pu will be adequately poisoned by Fe from the sludge. [Gap closed for SB11]; There is a low risk that ABD addition will impact the rheology or pumpability of the slurry. There is a low but higher risk of ABD addition prior to LTAD impacting the settling rate; Based on the evaluation of adding two-thirds of the ABD material and all of the ABD material prior to the LTAD process, there is no volume or mass limit that would need to be imposed on ABD additions prior to LTAD. [Gap closed for SB11]. Revision 1 of this report addresses a variation on the ABD additions and LTAD strategy where sodium hydroxide additions for LTAD may be performed intermittently or concurrently with an ABD addition window. The proposed change does not alter the conclusions of this evaluation.

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DOE OSTI2023

Hexagonal Boron Nitride Reinforced Multifunctional Well Cement for Extreme Conditions

The overarching objective of this project was to provide a system approach for developing the next generation of well cementing with remarkable multifunctional, high performance characteristics including mechanical, thermal, rheological and durability properties to prevent offshore spill and leakage at extreme high temperature, high pressure (HTHP) and corrosive conditions. Building on our scientifically illustrated principles, the objective of Phase I was to develop and tune our current proof-of-concept hexagonal boron-nitride (hBN)/cement composite to offer the best hybrid nanostructure, and optimum slurry formulation and rheological properties in environments with a variety of extreme conditions including high temperature, high pressure, and high acidity. This phase also focused on testing the actual barrier efficiency and performance of our new cement formulation against gas/liquid leakage at HT, and/or corrosive conditions. The objective of Phase 2 was product validation (meeting API/EPA standards), cost/risk analysis, and scale-up to facilitate integration for primary well cementing with no/minimal modification.

02 PETROLEUM↗

DOE OSTI2023

Development of a Novel Magnesium Alloy for Thixomolding® of Automotive Components (Final Report)

Magnesium (Mg) alloy die-castings are increasingly used in the automobile industry to achieve cost effective mass reduction, especially in systems where multiple components can be integrated into a single thin wall die-casting. However, there are several component quality restrictions in thin-walled Mg die castings, including variability in dimensional accuracy, part-to-part variation in mechanical properties, and porosity in the final part, which has limited the continued growth of die-cast components in the automobile industry. An alternative to die-casting is the process of thixomolding®. While the die-casting process relies on filling a mold at high speeds with the alloy in the completely molten state, the thixomolding® process fills a mold with a thixotropic alloy in a semi-solid slurry state at a temperature between the liquidus and solidus temperatures. Ideally, the material should be ~30–65% solid rather than being completely liquid at the beginning of the injection process. Advantages of the thixomolding® process include a finer grain structure, lower porosity, improved dimensional accuracy, improved part-to part consistency, improved mechanical properties, particularly ductility in the component, the ability to reduce wall thickness for mass savings, and longer tool life due to lower process temperatures. The objective of this collaborative project between Oak Ridge National Laboratory, FCA US LLC, and Leggera Technologies was to develop one or more novel Mg alloys more suitable for thixomolding® automotive structural components than the current die-casting alloys used for this process. The primary interest was to improve ductility while maintaining tensile and fatigue strengths, as these are properties that are critical for use in body and chassis structural applications. Since good corrosion resistance is also desirable for this application, this property was also considered when evaluating promising alloy compositions. An initial evaluation of existing components thixomolded® using AM60 was performed and microstructure, and tensile properties were evaluated for the baseline alloy. Targets were established for ease of processing (characterized by the melting range defined as the difference between the liquidus and the solidus), strength, and ductility. Computational modeling was used to identify promising alloys and selected alloys were cast in laboratory scale heats. Properties measured from laboratory scale heats were used to down-select two alloys for further evaluation and component fabrication. Two alloys were prepared in industrial scale heats, cut into small pieces (chips), and thixomolding® trials were initiated. Trial components were successfully fabricated using one alloy composition, but it was concluded that further refinement of the thixomolding® process parameters are required to successfully fabricate component using second alloy. Microstructure and mechanical properties were evaluated on the material removed from the fabricated component and properties were compared to the baseline alloy. Although mechanical properties of the alloys showed improvement over the baseline alloy, it was determined that modifications to the thixomolding® process would result in better microstructure control with further improvement in properties leading to successful commercialization. A provisional patent application has already been filed on the new alloys developed as part of the project.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Analysis of Defense Waste Processing Facility (DWPF) Condensate Samples and Evaluation of the Glycolate Destruction Process during Nitric-Glycolic flowsheet Transition

Glycolate concentrations were measured by the Savannah River National Laboratory (SRNL) in Slurry Mix Evaporator Condensate Tank (SMECT) and Recycle Collection Tank (RCT) samples retrieved after implementation of the Nitric-Glycolic Acid flowsheet at the Defense Waste Processing Facility (DWPF). No glycolate has been detected in any sample using Ion Chromatography (IC) with a detection limit of 8 mg/L, and no glycolate has been detected using either IC or Proton Nuclear Magnetic Resonance Spectroscopy ( 1 HNMR) after a permanganate strike was performed in the RCT.

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DOE OSTI2023

Insoluble Solids from Salt Dissolution: Characterization and Testing

Savannah River National Laboratory (SRNL) has further characterized insoluble solids that were observed in a variable depth sample from a salt dissolution campaign in Tank 9H. The insoluble solids were determined to be predominately gibbsite, a mineral form of aluminum hydroxide. From a review of salt dissolution testing and field experience, SRNL provided a realistic estimate of 8 vol% for solids of this type is formed per volume of saltcake dissolved. This estimate was doubled to 16 vol% to account for dissolution test uncertainty and differences between in-tank settling and laboratory testing. Savannah River Mission Completion (SRMC) is currently assessing the solids formed during salt dissolution as slurried sludge for hydrogen retention and release, which is driving flammability controls during salt dissolution activities. SRMC has requested SRNL perform a gas retention and release study to better understand the impact of the insoluble solids on waste tank flammability, and to provide a more accurate estimate of their ability to retain and release flammable gases.

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DOE OSTI2022

Roll-to-Roll Advanced Materials Manufacturing DOE Laboratory Collaboration - Early Stage R&D: Phase 2 and FY21 (Final Report)

R2R processing is used to manufacture a wide range of products for various applications which span many industrial business sectors. The overall R2R methodology has been in use for decades and this continuous technique traditionally involves deposition of material(s) onto substrates or membranes that are on moving webs, carriers or other continuous belt-fed or conveyor-based processes that enable successive steps to build a final product. Established methods that typify R2R processing include tape casting, silk-screen printing, reel-to-reel vacuum deposition/coating, and R2R lithography. Products supported by R2R manufacturing include micro-electronics, electro-chromic window films, PVs, fuel cells for energy conversion, battery electrodes and electrolytes for energy storage, and barrier and membrane materials for decarbonization and air and water filtration. Due to innovation in materials and process equipment, high-quality yet very low-cost multilayer technologies have the potential to be manufactured on a very cost-competitive basis. To move energy-related products from high-cost niche applications to the commercial sector, the means must be available to enable manufacture of these products in a cost-competitive manner. Fortunately, products such as fuel cells, thin- and mid-film PVs, batteries, electrochromic and piezoelectric films, water separation membranes, and other energy saving technologies readily lend themselves to manufacture using R2R approaches. However, more early-stage research is needed to solve the challenge of linking the materials (particles, polymers, solvents, additives) used in ink and slurry formulations and the coating and heated drying processes to the ultimate performance of the final R2R product, especially for a process that uses multiple layers of deposition to achieve the end product.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Sludge Batch 11 Assembly: Tank 15

Savannah River Mission Completion Nuclear Safety and Engineering Integration (SRMC-E) has requested that Savannah River National Laboratory (SRNL) perform Tank 15 characterization analyses in support of Sludge Batch 11 (SB11) assembly. This report provides important characterization of the slurry in Tank 15 prior to transfer from Tank 15 to Tank 13 (prior to sending to Tank 51) in order to demonstrate that the transfer is "Low Rem" and ensure the sludge concurs with the estimated transfer mass for the SB11 recipe. A total of 3 sets of Tank 15 samples were delivered to SRNL from December 2022 to August 2023. The individual sets of composite samples were analyzed for density, weight percent solids, chemical composition, radionuclides, and/or supernate corrosion control tests.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Sum-of-Fractions Methodology for Actinides in Water- and Polyethylene-Moderated and -Reflected Systems

Sum-of-fractions is a method intended to make sure a subcritical margin for aqueous solutions and slurries of fissionable isotopes exists. The method indicates that a system is subcritical if the sum of the ratios of the mass of each isotope (in a mixture) to its individual minimum subcritical mass limit is less than or equal to one. Historically, the basis of the sum-of-fractions has been derived from allowances given in the American National Standards Institute (ANSI)/ American Nuclear Society (ANS)-8.15-1981. However, the allowance was removed in ANSI/ANS-8.15-2014 due to a lack of technical basis. A methodology was developed to assess the validity of using the sum-of-fractions for water- or polyethylene-moderated systems for the following nuclides: 232 U, 233 U, 234 U, 235 U, 237 Np, 236 Pu, 238 Pu, 239 Pu, 240 Pu, 241 Pu, 242 Pu, 241 Am, 242 m Am, 243 Am, 242 Cm, 243 Cm, 244 Cm, 245 Cm, 246 Cm, 247 Cm, 249 Cf, and 251 Cf. The methodology uses available benchmark data for mixtures of 233 U, 235 U, and 239 Pu to establish the calculational margin, and a mass limit reduction to establish the margin of subcriticality. Water- or polyethylene-moderated and -reflected mixtures containing the nuclides are evaluated with the code system, SCALE 6.2.4. Including the calculational margin, subcritical mass limits for each nuclide were computed for optimally water- or polyethylene-moderated and fully reflected systems. These masses were used to create nuclide mixtures in which the sum of the mass to subcritical mass limit ratios is one. The various nuclide mixtures were modeled over a range of moderation and demonstrate the keff does not exceed the calculational margin. For additional assurance of subcriticality, a significant mass reduction is applied to each computed minimum critical mass of the nuclides without adequate benchmark data consistent with the method in ANSI/ANS-8.15-2014.

07 ISOTOPE AND RADIATION SOURCES↗