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All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Nanomineralogy as a new dimension in understanding elusive geochemical processes in soils: The case of low-solubility-index elements

Nanomineralogical studies of mineral surface coatings in soils reveal insights into biogeochemical processes that heretofore were not known to exist. This is a new dimension in understanding past and present biogeochemical processes in soils, and in this study it is a way to better understand the behavior of low-solubility-index elements such as Al, Ti, and Zr. Soils were sampled from selected sites in Sudbury (Ontario, Canada) that have been affected by acidification and particulate matter emissions from base-metal smelters with subsequent remediation within the past century. These anthropogenic processes have affected an entire landscape, but are now recorded in assemblages of nano-size phases that can be only studied using a combination of focused ion beam technology (for sample preparation) and high-resolution analytical transmission electron microscopy (for phase identification). A first generation of clay minerals (pre-acidification phase), their partial replacement by nano-size hematite and amorphous silica (anthropogenic acidification), and a second generation of clay minerals (post-acidification, including soil remediation) are products of changes in soil biogeochemical processes during these natural and anthropogenic-induced weathering stages. Furthermore, complex assemblages of nanophases formed prior to the second generation of clay minerals depict underlying mechanisms for the mobilization and sequestration of the low-solubility-index elements Zr and Ti under acidic conditions. The occurrence of baddeleyite (ZrO 2 ), anatase (TiO 2 ), and the Magneli phases Ti 4 O 7 and Ti 5 O 9 (all present at the nanoscale) suggest an influx of nanocolloidal Zr and Ti oxides during weathering of smelter-derived particulate matter. Kelyshite {NaZr[Si 2 O 6 (OH)]}, authigenic zircon (ZrSiO 4 ), and kleberite [Fe 3+ Ti 6 O 11 (OH) 5 ] are most likely products of the sequestration of the Zr- and Ti-bearing nanocolloids.

58 GEOSCIENCES↗
DOE OSTI2016

Defense Waste Processing Facility (DWPF) Viscosity Model: Revisions for Processing High TiO 2 Containing Glasses

Radioactive high-level waste (HLW) at the Savannah River Site (SRS) has successfully been vitrified into borosilicate glass in the Defense Waste Processing Facility (DWPF) since 1996. Vitrification requires stringent product/process (P/P) constraints since the glass cannot be reworked once it is poured into ten foot tall by two foot diameter canisters. A unique “feed forward” statistical process control (SPC) was developed for this control rather than statistical quality control (SQC). In SPC, the feed composition to the DWPF melter is controlled prior to vitrification. In SQC, the glass product would be sampled after it is vitrified. Individual glass property-composition models form the basis for the “feed forward” SPC. The models transform constraints on the melt and glass properties into constraints on the feed composition going to the melter in order to guarantee, at the 95% confidence level, that the feed will be processable and that the durability of the resulting waste form will be acceptable to a geologic repository. The DWPF SPC system is known as the Product Composition Control System (PCCS). The DWPF will soon be receiving wastes from the Salt Waste Processing Facility (SWPF) containing increased concentrations of TiO 2 , Na 2 O, and Cs 2 O . The SWPF is being built to pretreat the high-curie fraction of the salt waste to be removed from the HLW tanks in the F- and H-Area Tank Farms at the SRS. In order to process TiO 2 concentrations >2.0 wt% in the DWPF, new viscosity data were developed over the range of 1.90 to 6.09 wt% TiO 2 and evaluated against the 2005 viscosity model. An alternate viscosity model is also derived for potential future use, should the DWPF ever need to process other titanate-containing ion exchange materials. The ultimate limit on the amount of TiO 2 that can be accommodated from SWPF will be determined by the three PCCS models, the waste composition of a given sludge batch, the waste loading of the sludge batch, and the frit used for vitrification.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Selective recovery of pure copper nanopowder from indium-tin-oxide etching wastewater by various wet chemical reduction process: Understanding their chemistry and comparisons of sustainable valorization processes

Sustainable valorization processes for selective recovery of pure copper nanopowder from Indium-Tin-Oxide (ITO) etching wastewater by various wet chemical reduction processes, their chemistry has been investigated and compared. After the indium recovery by solvent extraction from ITO etching wastewater, the same is also an environmental challenge, needs to be treated before disposal. After the indium recovery, ITO etching wastewater contains 6.11 kg/m{sup 3} of copper and 1.35 kg/m{sup 3} of aluminum, pH of the solution is very low converging to 0 and contain a significant amount of chlorine in the media. In this study, pure copper nanopowder was recovered using various reducing reagents by wet chemical reduction and characterized. Different reducing agents like a metallic, an inorganic acid and an organic acid were used to understand reduction behavior of copper in the presence of aluminum in a strong chloride medium of the ITO etching wastewater. The effect of a polymer surfactant Polyvinylpyrrolidone (PVP), which was included to prevent aggregation, to provide dispersion stability and control the size of copper nanopowder was investigated and compared. The developed copper nanopowder recovery techniques are techno-economical feasible processes for commercial production of copper nanopowder in the range of 100–500 nm size from the reported facilities through a one-pot synthesis. By all the process reported pure copper nanopowder can be recovered with>99% efficiency. After the copper recovery, copper concentration in the wastewater reduced to acceptable limit recommended by WHO for wastewater disposal. The process is not only beneficial for recycling of copper, but also helps to address environment challenged posed by ITO etching wastewater. From a complex wastewater, synthesis of pure copper nanopowder using various wet chemical reduction route and their comparison is the novelty of this recovery process. - Highlights: • From the Indium-Tin-Oxide etching wastewater, copper nanopowder was synthesized. • Solution chemistry of ITO etching wastewater is addressed. • A techno-economical feasible, environment friendly and occupational safe process. • Brings back the material to production stream and address the circular economy. • A cradle to cradle technology management lowers the futuristic carbon economy.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Computational framework for modeling membrane processes without process and solution property simplifications

Accurately modeling membrane processes is critical to evaluating novel process configurations, designing scalable membrane systems, informing process cost estimates, and directing future research. Most membrane process models trade accuracy for computational efficiency by employing simplified approximations of the process (i.e. no salt flux, no pressure drop) and solution properties (i.e. ideal solution, and constant density, viscosity, and diffusivity). Our report introduces a detailed one-dimensional finite difference model for evaluating membrane processes that avoids these common simplifications. We apply this model to quantify the error introduced by these simplifications for case studies of reverse osmosis, osmotically assisted reverse osmosis, forward osmosis, and pressure retarded osmosis. While the magnitude of error introduced by these simplifications is reliant on the case study parameters and specifications, we find that existing model formulations can underestimate or overestimate average water flux by nearly 50% for some membrane processes operating under standard conditions. Lastly we investigate the error introduced by simplified inlet-outlet models that do not solve the governing system of differential equations, and we assess the accuracy of novel inlet-outlet formulations that use a log and geometric mean, instead of the typical arithmetic mean, to represent non-linear water flux profiles.

42 ENGINEERING↗
DOE OSTI2015

Simulative design and process optimization of the two-stage stretch-blow molding process

The total production costs of PET bottles are significantly affected by the costs of raw material. Approximately 70 % of the total costs are spent for the raw material. Therefore, stretch-blow molding industry intends to reduce the total production costs by an optimized material efficiency. However, there is often a trade-off between an optimized material efficiency and required product properties. Due to a multitude of complex boundary conditions, the design process of new stretch-blow molded products is still a challenging task and is often based on empirical knowledge. Application of current CAE-tools supports the design process by reducing development time and costs. This paper describes an approach to determine optimized preform geometry and corresponding process parameters iteratively. The wall thickness distribution and the local stretch ratios of the blown bottle are calculated in a three-dimensional process simulation. Thereby, the wall thickness distribution is correlated with an objective function and preform geometry as well as process parameters are varied by an optimization algorithm. Taking into account the correlation between material usage, process history and resulting product properties, integrative coupled simulation steps, e.g. structural analyses or barrier simulations, are performed. The approach is applied on a 0.5 liter PET bottle of Krones AG, Neutraubling, Germany. The investigations point out that the design process can be supported by applying this simulative optimization approach. In an optimization study the total bottle weight is reduced from 18.5 g to 15.5 g. The validation of the computed results is in progress.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2016

A novel process for production of spherical PBT powders and their processing behavior during laser beam melting

Additive manufacturing processes like laser beam melting of polymers are established for production of prototypes and individualized parts. The transfer to other areas of application and to serial production is currently hindered by the limited availability of polymer powders with good processability. Within this contribution a novel process route for the production of spherical polymer micron-sized particles of good flowability has been established and applied to produce polybutylene terephthalate (PBT) powders. Moreover, the applicability of the PBT powders in selective laser beam melting and the dependencies of process parameters on device properties will be outlined. First, polymer micro particles are produced by a novel wet grinding method. To improve the flowability the produced particles the particle shape is optimized by rounding in a heated downer reactor. A further improvement of flowability of the cohesive spherical PBT particles is realized by dry coating. An improvement of flowability by a factor of about 5 is achieved by subsequent rounding of the comminution product and dry-coating as proven by tensile strength measurements of the powders. The produced PBT powders were characterized with respect to their processability. Therefore thermal, rheological, optical and bulk properties were analyzed. Based on these investigations a range of processing parameters was derived. Parameter studies on thin layers, produced in a selective laser melting system, were conducted. Hence appropriate parameters for processing the PBT powders by laser beam melting, like building chamber temperature, scan speed and laser power have been identified.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2017

Effect of HEH[EHP] impurities on the ALSEP solvent extraction process

In solvent extraction processes, organic phase impurities can negatively impact separation factors, hydrolytic performance, and overall system robustness. The resulting inconsistent performance can affect the process-level viability of a separation concept, and thus knowledge of the impurities present, their effects on the process, and how to remove them are vital. Deleterious impurities may be introduced into a system from reagent synthesis, or result from degradation via radiolysis and hydrolysis during use. In this work, the acidic extractant, 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH[EHP])—proposed for application in extractive processes aimed at separating trivalent minor actinides from lanthanides and other fission products—is characterized with respect to its common impurities and their impact on Am(III) stripping in the Actinide Lanthanide SEParation (ALSEP) system. Furthermore, to control impurities in HEH[EHP], existing purification technologies commonly applied for the acidic organophosphorus reagent were assessed and a new chromatographic purification method specific to HEH[EHP] is presented.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Effect of fiber reinforcement on the process parameters of injection molding manufacturing process

Use of fillers with the resin is common in injection molding manufacturing technique to enhance the stiffness and strength of the manufactured components. However, the addition of fillers changes the rheological and mechanical properties of the material, required adjustments in the process parameters used for the manufacturing. The present study aims to investigate this impact of fillers on the process parameters of the injection molding manufacturing process. Neat Acrylonitrile Butadiene Styrene (ABS) and ABS reinforced with short glass fibers are used as the materials to perform the comprehensive numerical analysis including complete process sequence, namely filling, packing, cooling and warpage. Parametric studies are conducted to optimize the manufacturing process for minimal warpage (or shrinkage) in the produced part. The selected process parameters for the parametric study include cooling time, packing pressure, and mold temperature, all of which directly impact the quality of the manufactured parts. The optimal values obtained for these parameters are compared to examine the effect fiber reinforcement has on the manufacturing process.

Garg, Nikhil↗
DOE OSTI2019

Permanganate Oxidation of Defense Waste Processing Facility (DWPF) Recycle Collection Tank (RCT) Simulants – Protocol Runs for Nominal and Chemical Process Cell (CPC) Foamover Conditions

Savannah River National Laboratory (SRNL) has completed a work scope in support of the Savannah River Remediation (SRR) Nitric-Glycolic flowsheet. Glycolic acid will replace formic acid as a reducing agent in the pre-processing of High-Level Waste sludge performed at the Defense Waste Processing Facility (DWPF). Glycolic acid will perform the same function as formic acid, namely reduction of mercury and adjustment of feed rheology and melter oxidation/reduction potential, while significantly reducing the potential for hydrogen generation in DWPF processing. Development testing has demonstrated glycolic acid virtually eliminates hydrogen production in the pre-processing steps. The Nitric-Glycolic flowsheet significantly improves DWPF’s ability to address one of the Savannah River Site’s key challenges - the incorporation of effluent received from the Salt Waste Processing Facility (SWPF). SWPF will deliver significant effluent volume to DWPF, resulting in a concurrent increase in DWPF effluent returned to the Concentration, Storage and Transfer Facilities (CSTF). This work scope demonstrates that glycolate can be destroyed under the Nitric-Glycolic flowsheet prior to returning the DWPF recycle stream to CSTF. To avoid potential flammability issues due to thermolysis of glycolate in CSTF, SRR tasked SRNL to quantify and mitigate glycolate returns via DWPF’s recycle stream. The development of a strategy for glycolic mitigation was initiated with a system’s engineering workshop. Various chemical and/or physical solutions for how and where to destroy glycolate were considered – consistent with DWPF’s operational capabilities and process requirements. The workshop identified chemical oxidation of glycolate within the DWPF Recycle Collection Tank (RCT) as the most promising option. (The RCT collects offgas condensate from pre-processing, vitrification, and other unit operations performed in DWPF and is the singular return vessel delivering recycle effluent back to CSTF.) A series of down-select experimental tests were performed that showed sodium permanganate was the most effective oxidant. This work was performed to identify an appropriate operational protocol for DWPF implementation. Building upon the downselect experiments, the work targeted an improved description of suitable RCT conditions prior to the strike (pH, etc.), permanganate addition rate, and destruction reaction kinetics. Data collected were also used to determine the best expression of reaction stoichiometry and the effective minimum permanganate addition required.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2022

Intelligent Process Visualization through Nuclear Operation Process Modeling, Reasoning, and Object Detection from Field Videos (Final Report)

This report is a deliverable for the “Final Report” task of DOE NEET Project 19-16790, "Context-Aware Safety Information Display for Nuclear Field Workers." This project's overall goal is to test the hypothesis that integrating computer vision and process reasoning methods will enable proactive visualization of the safe operation and maintenance processes of Nuclear Power Plants (NPP) for field workers. Augmented Reality (AR) glasses adopting such proactive safety information visualization techniques can significantly increase personnel safety and reduce the NPP’s operating costs. The current practice of monitoring NPPs requires workers to switch between digital models, data, and physical workspaces in identifying relevant but potentially occluded objects and in assessing the risks of operation and maintenance processes. On the other hand, frequently changed field conditions require field workers to report to supervisors for real-time guidance. Such guidance is essential to ensure that changing conditions will not invalidate or endanger the work order and other ongoing processes that may jeopardize NPP operations. Additionally, incorrect recognition of equipment objects can result in communication errors and safety problems. AR techniques can assist engineers in viewing the physical workspaces with objects labeled with detailed operation procedures and safety reminders during field operations. The project team developed an “Intelligent Context-Aware Safety Information Display” (ICAD) for supporting Nuclear Power Plant (NPP) field workers in achieving safe and efficient execution of a series of operational tasks in uncertain and changing workspaces of an NPP. Before designing the ICAD-AR prototype, the project team synthesized NPP operational knowledge models through literature review studies, surveys, interviews with domain experts, and knowledge modeling. The project team conducted an extensive study of the operational procedures of various NPPs, and digital technologies that can support the safe and efficient execution of those procedures in different NPP operational contexts. This literature review helped the project team conduct surveys and interviews with nuclear engineers and field workers to identify three categories of information. The NPP knowledge modeling efforts reveal that the three categories of information identified have different levels of importance in a typical procedure of carrying out a series of tasks to achieve a specific NPP operation goal (e.g., shutdown, mode changes). These three categories of information include 1) Workspace dynamics – the changing spatial arrangements of workspaces, tools, protection equipment, and supporting materials, 2) Workflow prognostics – the dynamic dependencies between different parts of an NPP that functionally support and influence each other in terms of safety and efficiency, and 3) Hazards – objects and spaces that contain hazardous materials or physical conditions that can pose risks to workers or mechanical systems. The project team has profiled the importance levels of these categories of information into a knowledge model. This knowledge model specifies what types of information are more critical for a given task in a given workspace so that computers can automatically identify critical objects and sensors in a scene for delivering context-ware safety information to field workers through AR devices. Significant research development of this project results in technical research outcomes and a prototyping system that illustrates the technical feasibility of establishing an ICAD-AR system supporting the proactive safety information display for nuclear field workers. This final report summarizes the project team’s technological achievements in the past three years. Overall, the project team completed the development and integration of five techniques into a prototype ICAD Augmented Reality (ICAD-AR) system and demonstrated the developed system’s real-time execution in a mechanical room. The project team completed the analysis of using this prototype in other types of workspaces based on 3D image data and digital design models collected from two additional workspaces (a water treatment plant and a flow loop training facility). The integrated techniques include 1) Natural Language Processing (NLP) algorithms supporting the generation and updates of nuclear fieldwork process models based on text analysis of work packages and operation manuals; 2) sensor log analysis for predicting control actions in given sensor reading contexts; 3) computer vision algorithms for automatic localization and navigation of workers; 4) object detection algorithms for identifying task-related objects and correlated sensors for safety checking; 5) AR technique as a platform for supporting the integration. The testing results of these five techniques have shown that 1) the sensor log analysis model can predict the next control action with an accuracy of 0.883; 2) the trained natural language processing model can extract more than 80% of the critical information from paper-based procedures (PBPs); 3) the navigation algorithm with the integration of Visual Inertial Odometry (VIO) and Non-Recursive Bayesian Filter methods make operator’s trajectory estimation resilient to drift error; 4) the computer vision algorithm can detect task-specific and safety-critical objects with an average accuracy of 95.3%. The project team used work procedures collected from a flow loop training facility and two datasets collected from two mechanical rooms simulating the workspaces of NPPs to demonstrate the technical capabilities of the developed ICAD-AR prototype. The demonstration validated the technical feasibility of establishing the ICAD-AR system for nuclear field workers and identified the challenges in 1) automatic text analysis of work packages; 2) use of limited samples of sensor logs for predicting the proper timings of control actions; 3) reliably tracking workers and their task progress in mechanical rooms with many similar objects.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2019

Actinide-rich and Actinide-poor r -process-enhanced Metal-poor Stars Do Not Require Separate r -process Progenitors

The astrophysical production site of the heaviest elements in the universe remains a mystery. Incorporating heavy-element signatures of metal-poor, $r$-process-enhanced stars into theoretical studies of $r$-process production can offer crucial constraints on the origin of heavy elements. In this study, we introduce and apply the "actinide-dilution with matching" model to a variety of stellar groups, ranging from actinide-deficient to actinide-enhanced, to empirically characterize r-process ejecta mass as a function of electron fraction. We find that actinide-boost stars do not indicate the need for a unique and separate $r$-process progenitor. Rather, small variations of neutron richness within the same type of $r$-process event can account for all observed levels of actinide enhancements. The very low-$Y_e$ , fission-cycling ejecta of an $r$-process event need only constitute 10%–30% of the total ejecta mass to accommodate most actinide abundances of metal-poor stars. We find that our empirical $Y_e$ distributions of ejecta are similar to those inferred from studies of GW170817 mass ejecta ratios, which is consistent with neutron-star mergers being a source of the heavy elements in metal-poor, $r$-process-enhanced stars.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1993

AVIRIS and TIMS data processing and distribution at the land processes distributed active archive center

The U.S. Government has initiated the Global Change Research program, a systematic study of the Earth as a complete system. NASA's contribution of the Global Change Research Program is the Earth Observing System (EOS), a series of orbital sensor platforms and an associated data processing and distribution system. The EOS Data and Information System (EOSDIS) is the archiving, production, and distribution system for data collected by the EOS space segment and uses a multilayer architecture for processing, archiving, and distributing EOS data. The first layer consists of the spacecraft ground stations and processing facilities that receive the raw data from the orbiting platforms and then separate the data by individual sensors. The second layer consists of Distributed Active Archive Centers (DAAC) that process, distribute, and archive the sensor data. The third layer consists of a user science processing network. The EOSDIS is being developed in a phased implementation. The initial phase, Version 0, is a prototype of the operational system. Version 0 activities are based upon existing systems and are designed to provide an EOSDIS-like capability for information management and distribution. An important science support task is the creation of simulated data sets for EOS instruments from precursor aircraft or satellite data. The Land Processes DAAC, at the EROS Data Center (EDC), is responsible for archiving and processing EOS precursor data from airborne instruments such as the Thermal Infrared Multispectral Scanner (TIMS), the Thematic Mapper Simulator (TMS), and Airborne Visible and Infrared Imaging Spectrometer (AVIRIS). AVIRIS, TIMS, and TMS are flown by the NASA-Ames Research Center ARC) on an ER-2. The ER-2 flies at 65000 feet and can carry up to three sensors simultaneously. Most jointly collected data sets are somewhat boresighted and roughly registered. The instrument data are being used to construct data sets that simulate the spectral and spatial characteristics of the Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) instrument scheduled to be flown on the first EOS-AM spacecraft. The ASTER is designed to acquire 14 channels of land science data in the visible and near-IR (VNIR), shortwave-IR (SWIR), and thermal-IR (TIR) regions from 0.52 micron to 11.65 micron at high spatial resolutions of 15 m to 90 m. Stereo data will also be acquired in the VNIR region in a single band. The AVIRIS and TMS cover the ASTER VNIR and SWIR bands, and the TIMS covers the TIR bands. Simulated ASTER data sets have been generated over Death Valley, California, Cuprite, Nevada, and the Drum Mountains, Utah using a combination of AVIRIS, TIMS, amd TMS data, and existing digital elevation models (DEM) for the topographic information.

Mah, G. R.↗
DOE OSTI2024

Techno-economic analysis of biomass value-added processing informed by pilot scale de-ashing of paper sludge feedstock

Paper sludge biomass represents an underutilized feedstock rich in pulped and processed cellulose which is currently a waste stream with significant disposal cost to industry for landfilling services. Effective fractionation of the cellulose from paper sludge presents an opportunity to yield cellulose as feedstock for value-added processes. A novel approach to cellulose fractionation is the sidehill screening system, herein studied at the pilot-plant scale. Composition analysis determined ash removal and carbohydrate retention of both sidehill and high-performance benchtop screening systems. Sidehill screening resulted in greater carbohydrates retention relative to benchtop screening (90% vs 66%) and similar ash removal (95% vs 98%). Techno-economic analysis for production of sugar syrup yielded a minimum selling price of $331/metric ton of sugar syrup including disposal savings, significantly less than a commercial sugar syrup without fractionation. Furthermore, sensitivity analysis showed that screening conditions played a significant role in economic feasibility for cellulosic yield and downstream processes.

09 BIOMASS FUELS↗
DOE OSTI2014

Heterogeneous recurrence monitoring and control of nonlinear stochastic processes

Recurrence is one of the most common phenomena in natural and engineering systems. Process monitoring of dynamic transitions in nonlinear and nonstationary systems is more concerned with aperiodic recurrences and recurrence variations. However, little has been done to investigate the heterogeneous recurrence variations and link with the objectives of process monitoring and anomaly detection. Notably, nonlinear recurrence methodologies are based on homogeneous recurrences, which treat all recurrence states in the same way as black dots, and non-recurrence is white in recurrence plots. Heterogeneous recurrences are more concerned about the variations of recurrence states in terms of state properties (e.g., values and relative locations) and the evolving dynamics (e.g., sequential state transitions). This paper presents a novel approach of heterogeneous recurrence analysis that utilizes a new fractal representation to delineate heterogeneous recurrence states in multiple scales, including the recurrences of both single states and multi-state sequences. Further, we developed a new set of heterogeneous recurrence quantifiers that are extracted from fractal representation in the transformed space. To that end, we integrated multivariate statistical control charts with heterogeneous recurrence analysis to simultaneously monitor two or more related quantifiers. Experimental results on nonlinear stochastic processes show that the proposed approach not only captures heterogeneous recurrence patterns in the fractal representation but also effectively monitors the changes in the dynamics of a complex system.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2022

Process Scale-Up of an Energy-Efficient Membrane Solvent Extraction Process for Rare Earth Recycling from Electronic Wastes

This study reports the process scale-up and long-term performance of an energy-efficient and cost-effective membrane solvent extraction (MSX) process for separation and recovery of high purity rare earth oxides (REOs) from scrap permanent magnets (SPMs). Here, the rare earth elements (REEs), including dysprosium, neodymium, and praseodymium, are recovered from SPMs using a neutral extractant, tetraoctyl diglycolamide (TODGA) embedded in a microporous polypropylene hollow fiber membrane module. The MSX process performance is demonstrated with bench scale module with membrane surface area of 1.4 m 2 to industrial scale modules with membrane surface area of up to 20 m2 to enable the processing of up to 1 ton month –1 of SPMs. The purity and the yield of the recovered REOs are >99.5 wt% and >95%, respectively. The average extraction rate of REOs is >10 g m –2 hr –1 . A skid of MSX system is assembled with a membrane area of 40 m 2 . The MSX skid successfully recovers REOs with a capacity of 300 kg REOs/month. Finally, it is determined that the organic phase containing the extractant maintains its performance up to 250 h. The results suggest that the MSX process is an economically viable and environmentally friendly process for separation and recovery of REOs from electronic wastes.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Multimodal Analysis of Spatially Heterogeneous Microstructural Refinement and Softening Mechanisms in Three-Pass Friction Stir Processed Al4Si Alloy

Multiple thermally and thermomechanically induced microstructural refinement mechanisms can be activated in metallic alloys when subjected to solid phase processing methods such as friction stir processing (FSP). In this work, we provide detailed descriptions of the relationship between region-specific microstructural refinement mechanisms and the variation in microhardness, through a systematic and multimodal microstructural characterization of an FSP-processed 75% cold-rolled Al-4 at.% Si model binary alloy. Spatially resolved high-energy synchrotron X-ray diffraction, electron backscattered diffraction, and scanning transmission electron microscopy were used to understand the spatially heterogeneous microstructural evolution due to FSP. Results provide insights into how mechanisms such as static recovery, static recrystallization, dynamic recovery and recrystallization, geometric and continuous dynamic recrystallization, and particle-stimulated static or dynamic grain nucleation may occur heterogeneously in the microstructure as a function of the distance from the stir zone in processed alloys, directly influencing the degree of softening. The systematic analysis of microstructures and hardness in the FSP-processed model binary alloy given in this work highlights the rich microstructural domains that can be uniquely harnessed through solid phase processing of metallic alloys.

Al4Si, Friction Stir Processing, Geometric Dynamic↗