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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↗

NASA NTRS2014

Mitigating Thermal Runaway Risk in Lithium Ion Batteries

The JSC/NESC team has successfully demonstrated Thermal Runaway (TR) risk reduction in a lithium ion battery for human space flight by developing and implementing verifiable design features which interrupt energy transfer between adjacent electrochemical cells. Conventional lithium ion (li-Ion) batteries can fail catastrophically as a result of a single cell going into thermal runaway. Thermal runaway results when an internal component fails to separate electrode materials leading to localized heating and complete combustion of the lithium ion cell. Previously, the greatest control to minimize the probability of cell failure was individual cell screening. Combining thermal runaway propagation mitigation design features with a comprehensive screening program reduces both the probability, and the severity, of a single cell failure.

Darcy, Eric↗

DOE OSTI2021

Nanostructured Block Polymer Electrolytes: Tailoring Self-Assembly to Unlock the Potential in Lithium-Ion Batteries

Ion-containing solid block polymer (BP) electrolytes can self-assemble into microphase-separated domains to facilitate the independent optimization of ion conduction and mechanical stability; this assembly behavior has the potential to improve the functionality and safety of lithium-ion batteries over liquid electrolytes to meet future demands (e.g., large capacities and long lifetimes) in various applications. However, significant enhancements in the ionic conductivity and processability of BPs must be realized for BP-based electrolytes to become robust alternatives in commercial devices. Toward this end, the controlled modification of BP electrolytes’ intra-domain (nanometer-scale) and multi-grain (micrometer-scale) structure is one viable approach; intra-domain ion transport and segmental compatibility (related to the effective Flory–Huggins parameter, χ eff ) can be increased by tuning the ion and monomer-segment distributions, and the morphology can be selected such that the multi-grain transport is less sensitive to grain size and orientation.

25 ENERGY STORAGE↗

DOE OSTI2024

Uncovering the predictive pathways of lithium and sodium interchange in layered oxides

Ion exchange is a powerful method to access metastable materials with advanced functionalities for energy storage applications. However, high concentrations and unfavourably large excesses of lithium are always used for synthesizing lithium cathodes from parent sodium material, and the reaction pathways remain elusive. Here, using layered oxides as model materials, we demonstrate that vacancy level and its corresponding lithium preference are critical in determining the accessible and inaccessible ion exchange pathways. Taking advantage of the strong lithium preference at the right vacancy level, we establish predictive compositional and structural evolution at extremely dilute and low excess lithium based on the phase equilibrium between Li 0.94 CoO 2 and Na 0.48 CoO 2 . Such phase separation behaviour is general in both surface reaction-limited and diffusion-limited exchange conditions and is accomplished with the charge redistribution on transition metals. Guided by this understanding, we demonstrate the synthesis of Na y CoO 2 from the parent Li x CoO 2 and the synthesis of Li 0.94 CoO 2 from Na y CoO 2 at 1-1,000 Li/Na (molar ratio) with an electrochemical assisted ion exchange method by mitigating the kinetic barriers. Our study opens new opportunities for ion exchange in predictive synthesis and separation applications. Ion exchange is a powerful method to access metastable materials for energy storage, but identifying lithium and sodium interchange in layered oxides remains challenging. Using such model materials, vacancy level and corresponding lithium preference are shown to be crucial for ion exchange pathway accessibility.

25 ENERGY STORAGE↗

DOE OSTI2026

A structural and electrochemical study of perfluoropolyether-poly(ethylene oxide) solid polymer electrolytes

Solid polymer electrolytes offer attractive safety, processability, and interfacial adhesion for enabling high–energy solid-state lithium batteries, but they are often limited by narrow oxidative stability windows and low lithium-ion transference numbers. In an attempt to broaden the electrochemical stability window and increase lithium-ion transference number of poly(ethylene oxide) (PEO)-based solid polymer electrolytes, we produce an optically clear, crosslinked membrane of PEO and perfluoropolyether (PFPE) using a mixed solvent method and subsequently infuse the membrane with a lithium salt. Structural and thermal analyses reveal nanoscale phase separation between fluorocarbon and hydrocarbon domains with characteristic spacings of 7–8 nm and an elevated glass transition for the hydrocarbon phase. Consistent with this, PFPE-containing membranes exhibit substantially lower ionic conductivity than PEO analogs (dry and plasticized). The transference number and electrochemical stability are similar to pure PEO. These results demonstrate that fluorination implemented as segregated nanoscale domains does not deliver the anticipated transport or stability benefits; instead, phase separation increases tortuosity and suppresses hydrocarbon-phase dynamics. The work underscores the importance of fluorine placement and morphology control, guiding the design of partially fluorinated solid polymer electrolytes toward architectures that avoid detrimental nanoscale phase separation.

Carden, Peyton [ORNL] (ORCID:0000000162296538)↗

NASA NTRS1987

The 1986 Goddard Space Flight Center Battery Workshop

The subjects covered include: lithium cell technology and safety improvements; nickel-cadmium separator and electrode technology along with associated modifications; flight experience and life testing of nickel-cadmium cell; and nickel-hydrogen applications and technology.

Morrow, George W.↗

NASA NTRSDate not supplied

Design Considerations for Practical Li-S Battery Components for Electric Aviaiton

The development of high-energy, high-safety, and high-power batteries beyond electric automobile requirements is vital for future electric aviation applications. The transition to non-volatile solid-state electrolytes (SSE) promises many advantages over traditional flammable liquid electrolytes, and may also be an enabling technology for next generation chemistries. However, significant manufacturing challenges must be overcome before the adoption of such technology. Electrolytes developed in this study were produced as sulfide-polymer composites with densified thicknesses between 20-30 microns using a tape-casting technique and elastomer binder [1]. The composites were determined to retain reasonable ionic conductivity with improved flexibility and scalability critical for practical manufacturing of such cells. Films were produced 10-15 times thinner than comparable bulk powder electrolytes and within the range of commercial polyolefin separators (25 micron) used in commercial liquid containing lithium-ion cells. Composite conductivities were maintained above 0.2mS/cm, which holds promise for future electric aviation applications. Processing techniques are investigated to further improve electrochemical performance.

battery↗

DOE OSTI2022

Multi-scale boron penetration toward stabilizing nickel-rich cathode

Nickel-rich layered oxides LiNi x Co y Mn 1-x-y O 2 (x≥0.8) have been recognized as the preferred cathode materials to develop lithium-ion batteries with high energy density (>300Wh kg -1 ). However, the poor cycling stability and rate capability stemming from intergranular cracks and sluggish kinetics hinder their commercialization. To address such issues, a multi-scale boron penetration strategy is designed and applied on the polycrystalline LiNi 0.83 Co 0.11 Mn 0.06 O 2 particles that are pre-treated with pore construction. The lithium-ion conductive lithium borate in grain gaps functions as the grain binder that can bear the strain/stress from anisotropic contraction/expansion, and provides more pathways for lithium-ion diffusion. As a result, the intergranular cracks are ameliorated and the lithium-ion diffusion kinetics is improved. Moreover, the coating layer separates the sensitive cathode surface and electrolyte, helping to suppress the parasitic reactions and related gas evolution. In addition, the enhanced structural stability is acquired by strong B-O bonds with trace boron doping. As a result, the boron-modified sample with an optimized boron content of 0.5% (B5-NCM) exhibits a higher initial discharge capacity of 205.5mAh g -1 at 0.1C (1C=200mA g -1 ) and improved capacity retention of 81.7% after 100 cycles at 1C. Furthermore, the rate performance is distinctly enhanced by high lithium-ion conductive LBO (175.6mAh g -1 for B5-NCM and 154.6mAh g -1 for B0-NCM at 5C).

25 ENERGY STORAGE↗

DOE OSTI2024

Rechargeable lithium sulfur and/or selenium battery

An electrochemical device includes a cathode comprising a first cathode component of lithium and Se x S y ; and a second cathode component of an alkali metal and/or alkaline earth metal sulfur and/or selenide, different from the first cathode component; an initial discharge product of a polyselenide and/or polysulfide anion charge compensated by an alkali metal and/or alkaline earth metal cation; an anode; a porous separator; and a non-aqueous electrolyte with one or more lithium salts, and one or more solvents; wherein the electrochemical device is a lithium sulfur and/or lithium selenide battery.

Li, Matthew↗

DOE OSTI2025

In Situ Synthesis of Phosphate-Based CelloMOF as a Promising Separator for Li–Ion Batteries

Nowadays, battery separators play a critical role in determining the sustainability, electrochemical efficiency, and safety of lithium-ion batteries (LIBs). In this contribution, we developed fire-resistant composite membranes called CelloMOF by in situ grafting of metal-organic framework, ZIF-67, onto phosphorylated cellulose nanofibers (P-CNFs) followed by a vacuum filtration process akin to papermaking. The hybrid ZIF-67@P-CNF membrane exhibits superior properties than a polyolefin-based commercial separator (CS) in terms of enhanced thermal and dimensional stability, flame-retardant properties, better surface wettability, and improved electrolyte uptake. Thermal dimensional stability tests revealed that the ZIF-67@P-CNF separator maintained its structure even at 200 °C, whereas CS suffered severe shrinkage, potentially leading to internal short circuits. Combustion tests showed a peak heat release rate (PHRR) of 34.5 W/g and a total heat release (THR) of 1.61 kJ/g for ZIF-67@P-CNF, significantly lower than the PHRR (1111.82 W/g) and THR (40.89 kJ/g) of CS. The composite separator also demonstrated significantly improved wettability, with a contact angle of 32 ± 1.04°, compared to 92 ± 1.07° for CS, highlighting its hydrophilic nature. Electrochemical evaluations in LiFePO 4 /Li half-cells indicated a higher discharge capacity of 149 mA h g -1 at 0.2 C and superior capacity retention of 86% after 50 cycles, outperforming CS (145 mA h g -1 and 84%, respectively). In conclusion, these results underscore the potential of the ZIF-67@P-CNF membrane to advance safe, high-performance LIBs by addressing critical challenges in thermal stability, flame retardancy, and electrolyte compatibility.

ZIF-67↗

DOE OSTI2021

Selective cobalt and nickel electrodeposition for lithium-ion battery recycling through integrated electrolyte and interface control

Abstract Molecularly-selective metal separations are key to sustainable recycling of Li-ion battery electrodes. However, metals with close reduction potentials present a fundamental challenge for selective electrodeposition, especially for critical elements such as cobalt and nickel. Here, we demonstrate the synergistic combination of electrolyte control and interfacial design to achieve molecular selectivity for cobalt and nickel during potential-dependent electrodeposition. Concentrated chloride allows for the speciation control via distinct formation of anionic cobalt chloride complex (CoCl 4 2- ), while maintaining nickel in the cationic form ([Ni(H 2 O) 5 Cl] + ). Furthermore, functionalizing electrodes with a positively charged polyelectrolyte (i.e., poly(diallyldimethylammonium) chloride) changes the mobility of CoCl 4 2- by electrostatic stabilization, which tunes cobalt selectivity depending on the polyelectrolyte loading. This strategy is applied for the multicomponent metal recovery from commercially-sourced lithium nickel manganese cobalt oxide electrodes. We report a final purity of 96.4 ± 3.1% and 94.1 ± 2.3% for cobalt and nickel, respectively. Based on a technoeconomic analysis, we identify the limiting costs arising from the background electrolyte, and provide a promising outlook of selective electrodeposition as an efficient separation approach for battery recycling.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Electrolyte compositions for stabilizing silicon electrodes in lithium batteries

A lithium-ion electrochemical cell comprises a first electrode, a second electrode comprising elemental silicon, a microporous separator membrane between the first and second electrodes, and an electrolyte in contact with the electrodes and the membrane. The electrolyte comprises a lithium salt at a concentration in the range of about 0.1 M to about 5 M, and an additional metal salt at a concentration in the range of about 0.001 to about 5 M dissolved in an organic solvent. The additional metal salt comprises a metal cation that can form a lithium-silicon-metal Zintl phase; and the first electrode comprises metallic lithium or a cathode active material capable of donating and accepting lithium ions to and from the second electrode during electrochemical cycling. Electrolytes for use with silicon-containing electrodes also are described.

Vaughey, John T.↗

DOE OSTI2021

Rapid charging made practical in graphite-based lithium batteries: surface-acoustic wave turbulent electrolyte mixing to overcome diffusion limited charging rates [Final Report]

One of the key limits in rapidly recharging a lithium-ion battery is the depletion of lithium ions within the electrolyte adjacent the anode during charging and long diffusion time to overcome this depletion. It also causes dendrite formation, inefficient use of the lithium, and battery degradation over many charge-discharge cycles. Because the liquid electrolyte remains quiescent and unmixed, this depletion layer’s depth rapidly grows to match the anode-cathode separation distance at even modest charge rates. The solution proposed by PI Prof. James Friend and Co-PI Prof. Ping Liu, both from the University of California, San Diego, is to mix the electrolyte and minimize the Li+ ion concentration gradient during charging. Even in the presence of the separator, the charging rate could then be significantly increased. They propose to accomplish this using surface acoustic wave (SAW)-driven acoustic streaming, a technique employing 10-mW fingernail-sized solid-state devices from the telecommunications industry to drive turbulent mixing to submicron length scales in a manner completely compatible with the typical 20700 and 18650 cells used in electric vehicles. 0.1. Turbulent acoustic streaming mixes the electrolyte during charging—even with separator Our proposed 100-MHz SAW device used to recirculate the electrolyte is compatible with lithium- ion battery electrochemistry, as it is made in our lab of single-crystal lithium niobate. Their solution is straightforward to drive from a DC power source alongside the signal provided during battery charging. The device is only needed during charging and does not consume power dur- ing battery discharge. Uniquely, SAW generates extreme accelerations of over 1 billion meters per second squared in the fluid, driving turbulent mixing from centimeter to submicron length scales, even through the porous separator materials that tend to be used in batteries, all while avoiding interfering with the anode’s solid electrolyte interphase layer that forms during use. By employing novel fluid mechanics, the investigators are proposing a new direction for battery research away from direct use of materials science and electrochemistry. The chemistry agnostic solution may be employed in any battery chemistry that makes use of liquid electrolytes, providing a broader transformative benefit to the battery research community. They are to produce a series of prismatic and 20700-cell sized 2 Ah batteries capable of being charged and discharged at least 500 times without more than 20% loss in battery capacity, and to provide analysis tools useful to the battery research and development community for adopting this approach for other battery chemistries and configurations.

25 ENERGY STORAGE↗

DOE OSTI2022

Electrochemical cells with ionic sequestration provided by porous separators

Provided are electrochemical cells including separators permeable to some materials and impermeable to other materials in electrolytes. Also provide are methods of forming such separators. The selective permeability of a separator is achieved by its specific pore diameter and a narrow distribution of this diameter. Specifically, a species responsible for ion transport in an electrochemical cell are allowed to pass through the separator, while another species is blocked thereby preventing degradation of the cell. For example, a species containing lithium ions is allowed to pass in rechargeable cells, while one or more species containing transition metals are blocked. In some embodiments, a separator may include a membrane layer with at least 90% of pores of this having a diameter of between about 0.1 nanometers and 1.0 nanometer. The membrane layer may be a standalone layer or supported by a membrane support.

25 ENERGY STORAGE↗

DOE OSTI2023

Solvents and catalyst preparations for lithium-oxygen batteries

An electrochemical device includes a lithium anode having a red poly(benzonitrile) coating covering at least a portion of the anode; a separator and an air cathode comprising reduced graphene oxide over gas diffusion layer; and an electrolyte comprising an ether solvent, benzonitrile, and a lithium salt.

Wang, Hsien-Hau↗

DOE OSTI2024

Solvents and catalyst preparations for lithium-oxygen batteries

Wang, Hsien-Han↗

DOE OSTI2022

A Dual–Phase Electrolyte for High–Energy Lithium–Sulfur Batteries

Dissolution of lithium polysulfides (LiPSs) is essential for fast cathode kinetics, but detrimental for anode stability, especially under lean electrolyte conditions. Here in this work, the phase separation phenomenon between solvents with different polarities (tetramethyl sulfone [TMS] and dibutyl ether [DBE]) is utilized to enable the design of a dual-phase electrolyte. High-polarity, high-density TMS–lithium bis(trifluoromethanesulfonyl)imide–ammonium trifluoroacetate as the cathode electrolyte strongly solvates LiPSs, which propel the sulfur redox reaction. Moreover, the composite of DBE and a polymeric ion conductor serves as the anode electrolyte. The addition of DBE in the anode side effectively prevents the crossover of corrosive species (LiPSs and ammonia trifluoroacetate), enabling a significant improvement in Li-metal anode stability. The electrode-specific dual-phase electrolyte design provides electrochemical performance superior to conventional electrolytes. Without additional electrode engineering, pouch cells assemble with the dual-phase electrolyte cycle under a lean electrolyte (4 µL mg –1 ) and low-Li-excess condition (N/P = 3) for 120 cycles.

25 ENERGY STORAGE↗

DOE OSTI2023

Sequential Recovery of Critical Metals from Leached Liquor of Processed Spent Lithium-Ion Batteries

The processing and extraction of critical metals from black mass is important to battery recycling. Separation and recovery of critical metals (Co, Ni, Li, and Mn) from other metal impurities must yield purified metal salts, while avoiding substantial losses of critical metals. Solvent extraction in batch experiments were conducted using mixed metal sulphates obtained from the leach liquor obtained from spent and shredded lithium-ion batteries. Selective extraction of Mn 2+ , Fe 3+ , Al 3+ and Cu 2+ from simulated and real leached mixed metals solution was carried out using di-2-ethylhexylphophoric acid (D2EPHA) and Cyanex-272 at varying pH. Further experiments with the preferred extractant (D2EPHA) were performed under different conditions: changing the concentration of extractant, organic to aqueous ratio, and varying the diluents. At optimum conditions (40% v/v D2EPHA in kerosene, pH 2.5, O:A = 1:1, 25 °C, and 20 min), 85% Mn 2+ , 98% Al 3+ , 100% Fe 3+ , and 43% Cu 2+ were extracted with losses of only trace amounts (<5.0%) of Co 2+ , Ni 2+ , and Li + . The order of extraction efficiency for the diluents was found to be kerosene > Exxal-10 >>> dichloromethane (CH 2 Cl 2 ) > toluene. Four stages of stripping of metals loaded on D2EPHA were performed as co-extracted metal impurities were selectively stripped, and a purified MnSO 4 solution was produced. Spent extractant was regenerated after Fe 3+ and Al 3+ were completely stripped using 1.0 M oxalic acid (C 2 H 2 O 4 ).

25 ENERGY STORAGE↗