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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Concentrating lithium carbonate after regeneration of lithium sorbent

A system and method that includes flowing brine containing a metal ion through a reactor that includes porous particles having metal ion imprinted polymer having selective binding sites. The system and method further include discharging the brine from the reactor, contacting the porous particles with water, and pressurizing the reactor with carbon dioxide. The carbon dioxide reacts with the adsorbed metal ions to form a metal carbonate solution, where the metal carbonate solution can then be continuously purified with ion exchange. The method can include recycling eluent from the ion exchange back into the system for re-use. The method further includes depressurizing the reactor to precipitate metal carbonate from the metal carbonate solution and discharging the metal carbonate solution from the reactor.

Hornbostel, Marc↗
DOE OSTI2014

Modifications of impurity transport and divertor sources by lithium wall conditioning in the National Spherical Torus Experiment

In the National Spherical Torus Experiment (NSTX), lithium coatings are evaporated on graphite plasma facing components (PFCs) for wall conditioning. In lithium-conditioned H-mode discharges, carbon accumulation is observed with core concentrations <10%, leading to a lack of density control, while lithium ions have concentrations <0.1%. In this thesis, modifications of carbon and lithium divertor sources as well as scrape-off layer (SOL) and core transport due to lithium conditioning are studied. Spectroscopic impurity influxes (measured by filtered cameras) and 2D multi-fluid edge transport simulations via the UEDGE code are employed to study divertor impurity sources and SOL transport, respectively. Core transport of carbon and lithium is analyzed using the impurity transport code MIST and the neoclassical transport codes NEO and NCLASS. A reduction of the carbon sputtering yield in the lower divertor is observed with lithium evaporation. However, weaker divertor impurity retention resulting from reduced recycling (inferred from UEDGE simulations) and the possible importance of wall sources can counteract this reduction in divertor carbon influxes. The suppression of edge-localized-modes (ELMs) is the primary cause of the increased carbon inventories in lithium-conditioned discharges, leading to lack of density control. Deviations from neoclassical predictions for carbon transport are observed at the pedestal top in lithium-conditioned discharges, indicating the presence of anomalous outward convection. While the lithium sputtering yield from lithium-coated graphite in the divertor is consistent with physical and temperature-enhanced sputtering, a strong reduction in ionized lithium influxes is observed, possibly due to prompt re-deposition. The different poloidal source distribution and the stronger divertor retention for lithium (inferred from UEDGE simulations) contribute to a lower edge lithium source with respect to carbon. The latter is due to the shorter lithium ionization mean-free-path and weaker classical parallel forces. The high neoclassical lithium diffusivity, due to collisions with carbon ions, is partially responsible for the low lithium core densities. Furthermore, the higher neoclassical levels make lithium transport closer to neoclassical expectations. The NSTX-Upgrade baseline scenario includes lithium coatings on graphite PFCs for deuterium particle control. While the remarkably good lithium divertor retention makes it an attractive choice, the suppression of ELMs leads to carbon accumulation and therefore to the need to develop impurity mitigation techniques.

impurity trasport↗
DOE OSTI2021

Technology for the Recovery of Lithium from Geothermal Brines

Lithium is the principal component of high-energy-density batteries and is a critical material necessary for the economy and security of the United States. Brines from geothermal power production have been identified as a potential domestic source of lithium; however, lithium-rich geothermal brines are characterized by complex chemistry, high salinity, and high temperatures, which pose unique challenges for economic lithium extraction. The purpose of this paper is to examine and analyze direct lithium extraction technology in the context of developing sustainable lithium production from geothermal brines. In this paper, we are focused on the challenges of applying direct lithium extraction technology to geothermal brines; however, applications to other brines (such as coproduced brines from oil wells) are considered. The most technologically advanced approach for direct lithium extraction from geothermal brines is adsorption of lithium using inorganic sorbents. Other separation processes include extraction using solvents, sorption on organic resin and polymer materials, chemical precipitation, and membrane-dependent processes. The Salton Sea geothermal field in California has been identified as the most significant lithium brine resource in the US and past and present efforts to extract lithium and other minerals from Salton Sea brines were evaluated. Extraction of lithium with inorganic molecular sieve ion-exchange sorbents appears to offer the most immediate pathway for the development of economic lithium extraction and recovery from Salton Sea brines. Other promising technologies are still in early development, but may one day offer a second generation of methods for direct, selective lithium extraction. Initial studies have demonstrated that lithium extraction and recovery from geothermal brines are technically feasible, but challenges still remain in developing an economically and environmentally sustainable process at scale.

58 GEOSCIENCES↗
DOE OSTI2023

Geochemical characterization of lithium deposition in fossil energy wastes

Lithium is a critical mineral used in rechargeable batteries for electric vehicles (EVs) and future modernization of electric grids with sensitive supply chains that are subject to volatility. Therefore, methods to recover lithium from domestic unconventional sources are actively being pursued in the United States. Herein, we report on the lithium recovery potential from four fossil energy waste feedstocks: oil and gas drill cuttings (sample number n = 16); oil and gas produced waters (n > 200) from Marcellus, Bakken and Permian basins; coal byproducts (n>20), such as coal ash; and acid mine drainage treatment solids (AMD solids). Select solid samples underwent sequential extraction to explore lithium hosting phases and simple organic and inorganic acid extraction to explore lithium recovery potential. Our preliminary results found lithium concentrations up to 440 mg/kg in select AMD treatment solids and up to 300 mg/L in Marcellus Shale produced waters, demonstrating these sources have lithium yield potentials comparable to conventionally mined lithium ores and brines. Sequential extractions revealed that lithium is mostly associated with clay and silicate phases in shale drill cuttings, whereas lithium resides in Fe,Mn-oxide reducible phases in AMD solids. Further, the lithium content in produced waters has a strong linear relationship with total dissolved solid (TDS) levels in three separate oil and gas basins. At the same TDS level, Marcellus Shale produced waters contain more lithium compared to Bakken Shale and Permian Basin waters, with higher percentages of Ca and Mg, major cations that might impact lithium recovery efficiencies. Our study demonstrates the heterogeneity of lithium hosts from different fossil energy wastes. Characterization results will inform future lithium recovery from these different feedstocks.

Stuckman, Mengling↗
DOE OSTI2018

Energetics of Lithium Insertion into Magnetite, Defective Magnetite, and Maghemite

At low concentrations of lithium insertion into inverse spinel magnetite Fe 3 O 4 , a phase change to rock-salt-like Li x Fe 3 O 4 has been observed. Here, we used density-functional-theory-based (DFT-based) calculations to study the structural origins of this phase change, the concentration at which it occurs, the role of iron vacancies, and the stability of the various motifs that form during the electrochemical reduction process in the Li–Fe–O ternary space up to x = 1.33. We compared our results to new experimental measurements of the open circuit voltage for 8–9 nm magnetite particles over a comparable range of lithium insertion. Of the vacant sites in magnetite (16c, 8b, and 48f) lithium insertion was found to be most stable on 16c. Coulomb interactions between the added lithium and iron at the 8a site in magnetite led to substantial displacement of the iron. As further lithium was added, the most energetically favored motif involved lithium clustering in 16c sites around the shifted 8a iron up to a total of three lithiums. In competition with the lithium clustering motif, lithium insertion could be accompanied by the full displacement of all 8a iron to 16c sites, to form the rock-salt-like Li x Fe 3 O 4 , saturating at x = 1. The defective rock-salt structure was found to be more stable than the lithium clustering motif for x ≥ 0.5. The rock-salt-like LiFe 3 O 4 was found to be stable in the Li–Fe–O ternary space for a continuous range of Li–Fe organization on the 16c sites, stabilized by Coulomb interactions. For x < 1, neither the lithium clustering motif, nor the defective rock-salt-like structure for LixFe 3 O 4 were stable against phase segregation to LiFe 3 O 4 and Fe 3 O 4 . This phase segregation (0 < x < 1) occurred at a predicted voltage of ~2.0 V. However, when iron vacancies on the 16d site were introduced, lithium insertion to those vacant 16d sites in Fe 2.875 O 4 , and γ-Fe 2.67 O 4 (maghemite), resulted in stable intercalated materials at a predicted voltage of ~3.0 V. Beyond the concentration of such iron vacancy sites, phase segregation was predicted to the rock-salt-like Li 1.125 Fe 2.875 O 4 and Li 1.33 Fe 2.67 O 4 , again at ~2.0 V. These results were consistent with measured open circuit voltages. Finally, the relative stability for several lithium compositions along the FeO to LiFeO 2 tie line in the defective rock-salt structure suggested stable compound formation for a range of lithium–iron compositions, but without long-range order in the cation sublattice, consistent with what has been commonly observed in the literature.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Exposure to lithium through drinking water and calcium homeostasis during pregnancy: A longitudinal study

There is increasing evidence of adverse health effects due to elevated lithium exposure through drinking water but the impact on calcium homeostasis is unknown. This study aimed at elucidating if lithium exposure through drinking water during pregnancy may impair the maternal calcium homeostasis. In a population-based mother-child cohort in the Argentinean Andes (n=178), with elevated lithium concentrations in the drinking water (5–1660 μg/L), blood lithium concentrations (correlating significantly with lithium in water, urine and plasma) were measured repeatedly during pregnancy by inductively coupled plasma mass spectrometry and used as exposure biomarker. Markers of calcium homeostasis included: plasma 25-hydroxyvitamin D{sub 3}, serum parathyroid hormone (PTH), and calcium, phosphorus and magnesium concentrations in serum and urine. The median maternal blood lithium concentration was 25 μg/L (range 1.9–145). In multivariable-adjusted mixed-effects linear regression models, blood lithium was inversely associated with 25-hydroxyvitamin D{sub 3} (−6.1 nmol/L [95%CI −9.5; −2.6] for a 25 μg/L increment in blood lithium). The estimate increased markedly with increasing percentiles of 25-hydroxyvitamin D{sub 3}. In multivariable-adjusted mixed-effects logistic regression models, the odds ratio of having 25-hydroxyvitamin D3<30 nmol/L (19% of the women) was 4.6 (95%CI 1.1; 19.3) for a 25 μg/L increment in blood lithium. Blood lithium was also positively associated with serum magnesium, but not with serum calcium and PTH, and inversely associated with urinary calcium and magnesium. In conclusion, our study suggests that lithium exposure through drinking water during pregnancy may impair the calcium homeostasis, particularly vitamin D. The results reinforce the need for better control of lithium in drinking water, including bottled water. - Highlights: • Elevated drinking water lithium (Li) concentrations are increasingly reported. • We studied a Li-exposed population-based mother-child cohort in northern Argentina. • Li exposure during pregnancy affected maternal calcium homeostasis. • Blood Li was consistently inversely associated with maternal plasma vitamin D{sub 3}. • Associations were independent of season of sampling and lifestyle.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2018

Lithium metal stripping beneath the solid electrolyte interphase

Lithium stripping is a crucial process coupled with lithium deposition during the cycling of Li metal batteries. Lithium deposition has been widely studied, whereas stripping as a subsurface process has rarely been investigated. Here we reveal the fundamental mechanism of stripping on lithium by visualizing the interface between stripped lithium and the solid electrolyte interphase (SEI). We observed nanovoids formed between lithium and the SEI layer after stripping, which are attributed to the accumulation of lithium metal vacancies. High-rate dissolution of lithium causes vigorous growth and subsequent aggregation of voids, followed by the collapse of the SEI layer, i.e., pitting. We systematically measured the lithium polarization behavior during stripping and find that the lithium cation diffusion through the SEI layer is the rate-determining step. Nonuniform sites on typical lithium surfaces, such as grain boundaries and slip lines, greatly accelerated the local dissolution of lithium. As a result, the deeper understanding of this buried interface stripping process provides beneficial clues for future lithium anode and electrolyte design.

25 ENERGY STORAGE↗
DOE OSTI2022

First lithium experiments in HIDRA and evidence of helium retention during quasi-steady-state stellarator plasma operations

Recent experiments in Hybrid Illinois Device for Research and Applications (HIDRA) have had operational discharges between t discharge = 60 and 1000 s using electron cyclotron resonant heating (ECRH) of the plasma. This means that quasi-steady-state plasma discharges reach conditions to study long-pulse plasma material interactions (PMIs). The newly commissioned HIDRA-Material Analysis Test-stand PMI diagnostic is used to place a drop of lithium onto a heated tungsten surface, transfer the sample in-vacuo and expose it in a helium plasma. Helium is of interest as there is an open question to whether lithium will be able to remove helium ash in real fusion devices. The introduction of the W-Li sample in HIDRA resulted in evaporation of lithium into the helium plasma during a 600 s pulse and caused a reduction of over 90% in neutral pressure during the discharge. It was also observed that the plasma density and temperature increased by over 2.5 times. Using spectroscopy and a helium collisional radiative model, the peak temperature and density of the helium plasma can be monitored during the discharge. During lithium evaporation, as significant lithium ionization occurs, there is a 85% drop in the HIDRA vessel neutral pressure, despite a constant flow rate of He gas. This reduction in neutral pressure is supported by spectroscopy data with corresponding reductions in He I line intensities (587 nm, 667 nm, 706 nm, and 728 nm), as well as those of other impurities. At one point in the discharge a lithium plasma is created, as indicated by an increase in Li + emission and a complete reduction in He + emission, but the electron density jumps from ne = 3 × 10 18 m –3 to over ne = 8 × 10 18 m –3 while the core temperature stays relatively constant between Te = 16 eV and 20 eV. Once lithium has completely evaporated from the sample and the majority of the ionized lithium has diffused from the plasma to the vessel walls, pressure and spectroscopy data paired with He collisional radiative model calculations shows a re-establishment of a helium plasma in a low recycling regime. In this regime, the density drops down to ne = 2 × 10 18 m –3 and the electron temperature increases from T e = 20 eV to over T e = 50 eV indicating an increase in helium heating efficiency. This is also indicated by the He+ emission re-establishing and having a higher intensity. Here, we show the results from the first lithium campaign in HIDRA. In the presence of lithium, and in particular when lithium ions are present, the helium disappears from the plasma via an as of yet unknown complex relationship that needs to be further studied. The most likely explanation is that the lithium ions are distributed around the vessel and able to trap helium to the surface turning HIDRA into a large gettering surface. These results have potential implications on future plasma facing component design using liquid lithium for impurity and recycling control using limiters and divertors.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

Composite Solid Ion Conductor with Engineered Lithium Interface

Successful widespread commercialization of electric vehicles is contingent upon development of safe high energy density batteries capable of long cycle life. Lithium metal affords the highest theoretical capacity (3,860 mAh/g) and lowest electrochemical potential (-3.04V vs SHE), which offers the highest specific energy density of anode materials today. While Li-ion batteries are capable of delivering energy densities of 400-600 Wh/kg, the development of lithium metal batteries such as Li-S and Li-air may boost this number up to 650 and 950 Wh/kg, respectively. However, significant progress towards the passivation of lithium metal must occur before the energy density benefit can be realized. Issues with lithium dendrite formation, anode volume expansion, and continuous solid electrolyte interphase (SEI) build-up often result in significant safety concerns, high cell resistance, and poor cycle life. The intrinsic high reactivity between lithium metal with conventional lithium ion electrolytes (organic carbonate-based solvents) makes it extremely difficult to overcome these problems. In this project, Wildcat performed focused, fundamental research and development on composite polymer/ceramic electrolytes and protected lithium metal anodes to develop an all solid state lithium metal battery targeting the DOE requirements to enable commercialization. Wildcat successfully leveraged its high throughput battery platform and explored a broad composite electrolyte compositional space. Additionally, Wildcat screened large numbers of inorganic and organic coatings for lithium metal protection using in situ liquid methods and translated the best results to all solid cells. The proposed composite polymer/ceramic electrolyte and a protected lithium metal anode enabled a solid-state lithium metal battery. The ultimate targets from this effort will deliver a safe all solid-state lithium metal pouch cell with over 350 Wh/kg and over 1,000 cycles (C/3) with the cost estimate below $100/kWh. During the course of the project, we demonstrated stable cycling of 10’s of cycles with the composite SSE and our protected lithium. The work has continued after the conclusion of the DOE funding, demonstrating further improvements in catholyte composition and thinner composite solid electrolytes.

25 ENERGY STORAGE↗