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Microchannel-based Membrane-less Extraction of Li from Unconventional Lithium Sources & the Separation of REE

This final report provides an overview of the Project's entire duration, covering July 1, 2021 to December 31, 2023. It primarily focuses on the achievements, technological developments, and unique challenges the team faced while working on separating and extracting Lithium from produced waters. The project's primary aim was to create an integrated, high-throughput, membrane-less, and modular microfluidic platform that could extract Lithium from unconventional sources. We have successfully met all goals and milestones envisioned in the SOPO document. The most critical primary milestones, including the Go-No-Go milestone (refer to the Gantt chart in the Appendices), were successfully accomplished. We demonstrated phase separation (>90%) and extraction (>85%) performance in the MPSE using synthetic, and representative produced water composition feed at 50 ml/min total flow through MPSE 36. We have also performed a parametric study of the MPSE operations, beyond the scope of SOPO, exploring operating conditions of current and broader interest. The extended investigation of operational parameters is concurrent with our efforts to seek further development of the MPSE technology beyond the scope of the Project. Along these lines of development, we have made efforts to be responsive to DOE calls for technological developments of other types of resources (beyond PW) for the recovery of Critical Materials and higher TRL development (beyond TRL 4). During the work on this Project, we developed and implemented three innovative technical approaches that emerged from our efforts to successfully meet the Project milestones. The innovative & original technical approaches developed and implemented in this Project are now the contributions to process engineering that could be clearly credited to the Project. First, Convergent Design Approach is a comprehensive feedforward & feedback loop of four design phases: i) design for functionality, ii) design for manufacturing, iii) design for sustainability, and iv) design for market. Next was Process Intensification. A major aim of this Project was to create an innovative phase separation & extraction microscale-based technology for Li separation – thus the words microchannel-based in the Project title. A microscale-based technology is intrinsically in the center of the Process Intensification domain as defined by its unique principles. Therefore, Process Intensification was implicitly envisioned in the Project’s SOPO. Lastly, Time Scale Analysis is a novel tool for discovering the needs and directions of Process Intensification implementations in any process technology. This Project is fully credited for developing and implementing the three novel technical approaches mentioned above. These are general contributions to process engineering that emerged from this Project. Beyond the original SOPO scope, the OSU-U.Pitt research group utilized a Convergent Design methodology, integrating first-principles mathematical modeling with experimental validation on the Minimum Development Vehicle. By creating these Digital Twins, the team rapidly assessed manufacturing iterations to support TEA analysis. This framework further enabled the development of advanced Surface Modification Techniques, where hydrophobic and oleophobic coating strategies were optimized via Digital Twin tools and validated through rigorous 100-hour longevity testing. TEA Analysis: The closing efforts of this Project were focused on the TEA analysis. TEA analysis had two primary functions: i) enabling critical assessments of design variations withing 10 the Concurrent Design Approach, thus enabling evolution of the MPSE design to reach faster- better-cheaper alternatives; and ii) to create a bridge between the accomplishments of this Project and future projects of higher TRL, beyond TRL 6 level. It is important to note that the TEA model created in the Project stirred the technological solutions for the recovery of critical materials toward a vision of a very profitable modular plant that has unique zero-waste water discharge signature. More importantly, thanks to our experimental performance data and conservative assumptions, the TEA model predicts minimal technological and investment risks. Low cost of a modular unit of a nominal capacity of [1000 tons of Li 2 CO 3 /year] positions the MPSE based technology within the reach of community investors, thus offering a paradigm shift in the development of critical technologies. The project successfully navigated two primary challenges: solvent selection and manufacturing adaptation. Restricted by the SOPO to existing literature for lithium recovery, the team identified a critical need for a "material excellence program" to develop next-generation solvents, eventually concluding with a preliminary investigation into promising Ionic Liquids (ILs). Simultaneously, COVID-19 supply chain disruptions forced a pivot from traditional manufacturing to advanced additive methods at ATAMI-OSU. By transitioning from stainless steel to 3D-printed polymer substrates, the team achieved a transformative three-order-of- magnitude reduction in manufacturing costs and compressed prototyping timelines from several months to just two days. The MPSE technology offers significant energy, environmental, and economic advantages by overcoming the traditional bottlenecks of phase-separation hardware and contactor size. Unlike conventional mixer-settlers or membrane-based systems, MPSE operates without moving parts or fouling-prone membranes, achieving robust performance even with challenging, viscous, or particulate-heavy feeds. Key performance metrics include an energy intensity reduction of 5–50x (3–40 kJ/m 3 ) compared to incumbent technologies and a dramatic reduction of processing time to under 60 seconds, which drastically reduces the physical plant footprint. These technical efficiencies translate into superior economic outcomes; for a 100 t/year Li 2 CO 3 facility, implementing MPSE is projected to nearly halve contactor CAPEX (from $\$$6.08M to $\$$3.01M) and significantly increase the project's Net Present Value (NPV), derisking new investment and enabling distributed critical-mineral processing configurations. The commercialization of MPSE technology is being spearheaded by Vigsur Dynamics Inc., which has adopted a structured, parallel approach to technical and business development since its formation in January 2026. Following extensive customer discovery and engagement with the Oregon State University accelerator, Vigsur Dynamics is working to establish a business model that transitions from pilot demonstrations to modular hardware sales, ultimately aiming for a "build-own-operate" service strategy. Current technical milestones—including 100 hours of continuous operation, superior energy efficiency, and successful 6-unit modular scale-up— provide a foundation for this transition. Backed by ongoing IP licensing and a growing network of industrial and venture advisors, the company is actively de-risking the platform to replace conventional mixer-settler systems in the critical minerals market.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

The distribution of Sr and REE between diopside and silicate liquid

Experimental determination of the distribution coefficients in diopside-liquid pairs for strontium and nine rare-earth elements in the system CaMgSi2O6-NaAlSi3O8-CaAl2Si2O8. In experiments in air at 1265 C it is found that most of the Sr(2+), Eu(2+), and RE(3+) ions substitute for Ca(2+) and, in addition, a coupled substitution of Al(3+) for Si(4+) occurs. All of the trace ions considered are found to be excluded from the diopside lattice relative to the liquid. In the case of the trivalent ions the exclusion is much more pronounced for La and Ce, which have ionic radii larger than that of Ca(2+) in 8-fold oxygen coordination. Divalent Sr and Eu with even larger radii are also strongly excluded.

Grutzeck, M.

Mineralogy, petrology, and trace element geochemistry of the Johnstown meteorite - A brecciated orthopyroxenite with siderophile and REE-rich components

The compositional and petrologic characteristics of the Johnstown meteorite show it to contain uncontaminated and unbrecciated orthopyroxenite clasts of cumulative origin that (1) must have undergone subsolidus recrystalization, (2) are parental to the brecciated matrix, and (3) show no evidence of a xenolithic, meteoritic contribution to the matrix except for contamination by the projectile which crushed it on impact. The trapped liquid was not introduced in the impact process. The variability of such trace elements as the light rare earth elements, and the presence of plagioclase and olivine in only one of the thin sections studied, demonstrates the heterogeneity of coarse-grained diogenites on a millimeter scale and the difficulty of obtaining representative samples of such meteorites. The data presented indicate that this meteorite is a monominct breccia.

Floran, R. J.

A Nd isotopic study of the Hamersley and Michipicoten banded iron formations - The source of REE and Fe in Archean oceans

A detailed Nd isotopic study of the large and well-dated Hamersley and Michipicoten banded iron formations (BIFs) has been conducted. The Hamersley BIFs (Lake Superior type) are located in the Pilbara craton of Western Australia and the Michipicoten BIFs (Algoma type) are located in the northeastern corner of Lake Superior in Ontario, Canada. Their initial epsilon(Nd) values are variable and in the range of 0 to +4. The Fe/Nd ratio in present-day hydrothermal waters and BIFs are both 100,000, suggesting that the source of much of the Fe in BIFs (and Archean seawater) was hydrothermal water circulating through Archean midocean ridge systems.

Jacobsen, Stein B.

The Nakhla parent melt: REE partition coefficients and clues to major element composition

Nakhla is one of the SNC meteorites, generally believed to be of Martian origin. It is a medium-grained augite-olivine cumulate with a variolitic groundmass of sodic plagioclase, alkali feldspar, and Fe-rich pyroxenes and olivine. One of the major tasks in deciphering Nakhla's petrogenesis is determining the composition of its parent melt. Gaining an understanding of the composition and petrogenesis of this parent melt may help unravel Nakhla's relationship to the other SNCs, and provide clues to Martian petrogenesis in general. Our experimental partitioning studies provide new information that helps constrain both the major and trace element composition of the Nakhla parent melt.

Mckay, G.

Tambo Quemado: Extraordinary concentrations of REE and refractory trace elements caused by artificial heating

Buchwald examined samples of the IIIB iron Tambo Quemado (TAMQ) cut from the 130 kg main mass. He determined it had been artificially heated, at some time prior to being reported, in an attempt to obtain metal from it. Although the Widmanstatten structure appears relatively unaffected under macroscopic examination, microscopic study of etched sections reveals the effect of the heating. Taenite and plessite area boundaries are indistinct due to high temperature diffusion. Schreibersite, once present in significant amounts, has been melted. Schreibersites in the interior have resolidified in fine-grained eutectic textures surrounded by dark-etching metal rims supersaturated with phosphorus. Buchwald states that phosphate minerals were probably present originally, because graftonite, and its polymorph sarcopside (both essentially Fe3(PO4)2), are common in irons of the IIIB groups. Based on his metallographic study Buchwald estimates TAMQ was heated to 1000 C for about one hour. An interior sample from TAMQ was examined in order to determine what effect this unintended heating 'experiment' had upon the phosphate phases.

Olsen, E.

REE Partition Coefficients from Synthetic Diogenite-Like Enstatite and the Implications of Petrogenetic Modeling

Determining the petrogenesis of eucrites (basaltic achondrites) and diogenites (orthopyroxenites) and the possible links between the meteorite types was initiated 30 years ago by Mason. Since then, most investigators have worked on this question. A few contrasting theories have emerged, with the important distinction being whether or not there is a direct genetic link between eucrites and diogenites. One theory suggests that diogenites are cumulates resulting from the fractional crystallization of a parent magma with the eucrites crystallizing, from the residual magma after separation from the diogenite cumulates. Another model proposes that diogenites are cumulates formed from partial melts derived from a source region depleted by the prior generation of eucrite melts. It has also been proposed that the diogenites may not be directly linked to the eucrites and that they are cumulates derived from melts that are more orthopyroxene normative than the eucrites. This last theory has recently received more analytical and experimental support. One of the difficulties with petrogenetic modeling is that it requires appropriate partition coefficients for modeling because they are dependent on temperature, pressure, and composition. For this reason, we set out to determine minor- and trace-element partition coefficients for diogenite-like orthopyroxene. We have accomplished this task and now have enstatite/melt partition coefficients for Al, Cr, Ti, La, Ce, Nd, Sm, Eu, Dy, Er, Yb, and La.

Schwandt, C. S.

Ree in Shergottite Augites and Whole Rocks

Redox variations have been reported among the shergottites. Eu and Gd partitioning experiments designed for the LEW86010 angrite, to infer a range of fo2 for the shergottites have been used. Fo2 using equilibria between Fe-Ti oxides have been inferred. There is fairly good agreement between the Fe-Ti oxide determinations and the estimates from Eu anomalies in terms of which meteorites are more or less oxidized. The Eu anomaly technique and the Fe-Ti oxide technique both essentially show the same trend, with Shergotty and Zagami being the most oxidized and QUE94201 and DaG 476 being the most reduced. Thus, the variation in fo2 appears to be both real and substantive. However, although the redox trends indicated by the two techniques are similar, there is as much as a two log unit offset between the results. One explanation for this offset is that the Eu calibration used for the shergottites was actually designed for the LEW86010 angrite, a silica-undersaturated basalt whose pyroxene (diopside) compositions are rather extreme. To correct this, a set of experiments on the redox relationship of Eu partitioning relative to Sm and Gd for pyroxene and melt compositions more relevant to Martian meteorites were conducted. We have taken the experimentally determined relationship between D (sup Augite/melt) (Sm,Eu,Gd) and fO2 and applied it to augite Eu and Gd data for the basaltic Shergottites of as well as previously unreported augite Sm data.

Musselwhite, D. S.

REE in Shergottite Augites and Whole Rocks

Redox variations have been reported among the shergottites. Eu and Gd were used in partitioning experiments designed for the LEW86010 angrite, to infer a range of fO2 for the shergottites. Inferred fO2 using equilibria between Fe-Ti oxides was used. There is fairly good agreement between the Fe- Ti oxide determinations and the estimates from Eu anomalies in terms of which meteorites are more or less oxidized. The Eu anomaly technique and the Fe-Ti oxide technique both essentially show the same trend, with Shergotty and Zagami being the most oxidized and QUE94201 and DaG 476 being the most reduced. Thus, the variation in fO2 appears to be both real and substantive. However, although the redox trends indicated by the two techniques are similar, there is as much as a two log unit offset between the results of presented. One explanation for this offset is that the Eu calibration used for the shergottites was actually designed for the LEW86010 angrite, a silica-undersaturated basalt whose pyroxene (diopside) compositions are rather extreme. To correct this, a set of experiments were conducted on the redox relationship of Eu partitioning relative to Sm and Gd for pyroxene and melt compositions more relevant to Martian meteorites. We have taken the experimentally determined relationship between (Sm,Eu,Gd) and fO2 and applied it to augite Eu and Gd data for the basaltic Shergottites as well as previously unreported augite Sm data.

Musselwhite, D. S.

An experimental evaluation of the REE SIFT environment for spaceborne applications

This paper presents an experimental evaluation of a software-implemented fault tolerance environment built around a set of self-checking ARMOR proceses running on different machines that provide error detection and recovery services to themselves and to spaceborne scientific applications.

fault injection on-board processing cluster commut

SM-ND Age and REE Systematics of Larkman Nunatek 06319: Closed System Fractional Crystallization of a Shergottite Magma

Sm-Nd isotopic data were collected on mineral separates and bulk rock powders of LAR 06319, yielding an age of 180+/-13 Ma (2(sigma)). This age is concordant with the Lu-Hf age (197+/-29 Ma, [1]) determined in conjunction with these data and the Sm-Nd age (190+/-26 Ma) of Shih et al., 2009 [2]. The Sm-Nd data form at statistically significant isochron (Fig. 1) that is controlled largely by leachate-residue pairs (samples with the R suffix are residues after leaching in cold 2N HCl for 10 minutes).

Shafer, J. T.

Correlations Between Surficial Sulfur and a REE Crustal Assimilation Signature in Martian Shergottites

Compared to terrestrial basalts, the Martian shergottite meteorites have an extraordinary range of Sr and Nd isotopic signatures. In addition, the S isotopic compositions of many shergottites show evidence of interaction with the Martian surface/ atmosphere through mass-independent isotopic fractionations (MIF, positive, non-zero delta(exp 33)S) that must have originated in the Martian atmosphere, yet ultimately were incorporated into igneous sulfides (AVS - acid-volatile sulfur). These positive delta(exp 33)S signatures are thought to be governed by solar UV photochemical processes. And to the extent that S is bound to Mars and not lost to space from the upper atmosphere, a positive delta(exp 33)S reservoir must be mass balanced by a complementary negative reservoir.

Jones, J. H.