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DOE OSTI2022

Binary Fe/Mn-Based Nanocomposites as Li-Free Cathode Materials for Li Batteries Assembled in Charged State

Li-ion batteries play important roles in this mobile society. The ever-increasing demand for energy storage, particularly from electric vehicles, requires next-generation Li batteries with higher energy density and better safety. In contrast to existing Li-ion batteries using lithiated cathodes and Li-free anodes, we explore Li-free cathodes coupled with lithium/ lithiated anodes in order to construct new Li batteries assembled in a charged state. Here, two highly promising Li-free cathode materials of 1-D FeOF nanorods and 2-D monolayer MnO 2 nanosheets are integrated to make FeOF@MnO 2 nanocomposites. FeOF nanorods are sandwiched by monolayer MnO 2 nanosheets where FeOF nanoparticles could prevent the restacking of the monolayer MnO 2 nanosheets and the presence of monolayer MnO 2 nanosheets could enhance the electrical integration of the FeOF nanorods. Synergistic effects of the binary Fe/Mn-based cathodes can lead to both high voltage and high capacity, compared to individual components. Electrochemical evaluation reveals that binary Fe/Mn-based Li-free cathodes demonstrate promising performances and are worthy of further investigation and optimization.

25 ENERGY STORAGE↗

DOE OSTI2023

Fluorinated Interphase Enables Reversible Zn 2+ Storage in Aqueous ZnSO 4 Electrolytes

Aqueous zinc-ion batteries (AZIBs) using ZnSO 4 aqueous electrolytes complement Li-ion batteries and offer high safety, low cost, and scalability. However, an inferior cycle life, attributed to the generation of basic layered double hydroxides (LDHs) on the cathode during cycling, hampers the development of AZIBs. Although Zn(CF 3 SO 3 ) 2 (Zn(OTf) 2 ) electrolytes demonstrate exceptional performance, their higher cost in comparison to ZnSO 4 offsets their electrochemical stability benefits. Toward this end, we propose a fluorinated interphase strategy to achieve a stable battery with ZnSO 4 electrolytes by in situ pre-constructing the cathode-electrolyte interphase (CEI) of ZnOTf-LDH on the cathode surface. Unlike ZnSO 4 - LDH, which obstructs the diffusion channel of zinc ions, ZnOTf-LDH facilitates the desolvation of zinc ions, thereby enhancing the cycling stability (over 50 cycles at a low current density of 200 mA g -1 ). Further, this work offers valuable insights into the degradation mechanism of AZIBs and provides an effective approach for developing stable and low-cost AZIBs.

25 ENERGY STORAGE↗

DOE OSTI2026

Strategies for Enhancing Battery Life Under Fast Charging: Insights from NMC-Based Cell Cycling

Fast charging improves the usability of consumer electronics and electric vehicles (EVs) by reducing range anxiety and downtime but accelerates battery degradation and raises safety concerns. Optimizing operational conditions during fast-charging is critical to mitigating aging and ensuring safety. This study evaluated multilayer Gr/NMC811 cells under various conditions, including depths of discharge (DODs of 68%, 84%, and 100%), upper charge cutoff voltages (4.1–4.2 V), and post-charge rest periods (2–30 min), using a 20 min fast charging protocol for up to 500 cycles (up to 150,000 miles of EV use assuming 3.3 mi/kWh vehicle level energy efficiency). Surprisingly, higher DODs under fast charging improved battery life and performance compared to lower DODs. Reducing the upper charge cut-off voltage helped mitigate degradation. A brief 2 min rest period after charging further reduced aging effects. The primary aging modes were loss of lithium inventory and cathode active material. Although minor lithium plating was observed within 500 cycles, it did not affect performance significantly. These findings suggest that, with optimized conditions, cells can sustain hundreds of fast charge cycles—equivalent to over 100,000 miles of EV use—without significant adverse effects on performance or longevity.

25 - ENERGY STORAGE↗

DOE OSTI2024

A Sulfide‐Based Solid Electrolyte With High Humid Air Tolerance for Long Lifespan All‐Solid‐State Sodium Batteries

Abstract Sulfide‐based superionic conductors present great promise to achieve high energy density and safety for all‐solid‐state sodium batteries (ASSSBs). However, the poor electrolyte/electrode interface compatibility and humid air stability seriously hinder their deployment in ASSSBs. Herein, a series of high‐performance Na 3‐□ Sb 1‐4x (SnWCaTi) x S 4 sulfide‐based solid electrolytes (SSEs) are reported by coupling the vacancy effect with configurational entropy, which displays an excellent interface stability against sodium metal and an extraordinary tolerance toward the moist atmosphere, even for water. The optimized electrolyte effectively inhibits the detrimental mixed ion‐electron conducting interphase formation, achieving the ultra‐stable operation of Na–Na symmetric cell up to 1000 h. Furthermore, the Na + diffusion kinetics is obviously enhanced by increasing the Na sites local anisotropy and Na vacancies. Eventually, the assembled TiS 2 //Na 5 Sn ASSSBs deliver a remarkable reversible capacity of 211.6 mAh g −1 at 0.5C with a long‐term cycling performance of 450 cycles at room temperature. More importantly, it achieves a steady running up to 100 cycles at 1C even if this electrolyte is placed in the air with a dew temperature of 13.8 °C for 30 min, the highest values in the state‐of‐the‐art sulfide‐based ASSSBs. The well‐designed SSEs open a new avenue for realizing the advanced and powerful ASSSBs.

Guo, Yayu↗

DOE OSTI2021

Roadmap of Solid-State Lithium-Organic Batteries toward 500 Wh kg –1

Over the past few years, solid-state electrolytes (SSEs) have attracted tremendous attention due to their credible promise toward high-energy batteries. In parallel, organic battery electrode materials (OBEMs) are gaining momentum as strong candidates thanks to their lower environmental footprint, flexibility in molecular design and high energy metrics. Integration of the two constitutes a potential synergy to enable energy-dense solid-state batteries (SSBs) with high safety, low cost, and long-term sustainability. Here, we present the technological feasibility of combining OBEMs with SSEs along with the possible cell configurations that may result from this peculiar combination. We provide an overview of organic SSBs and discuss their main challenges. We analyze the performance-limiting factors and the critical cell design parameters governing cell-level specific energy and energy density. Lastly, we propose guidelines to achieve 500 Wh kg –1 cell-level specific energy with solid-state Li–organic batteries.

25 ENERGY STORAGE↗

DOE OSTI2023

Development, Characterization, and Testing of Solid-State Electrolytes for Batteries

Traditional liquid electrolytes used in lithium (Li) metal batteries (LMBs) have severe safety issues, poor power density, as well as thermal and electrochemical instability that prevents their scaling to newer applications, such as electric vehicles. Using sulfide-based solid-state electrolytes (SSEs) is a viable method to address many of the issues that plague LMBs. However, the key issue preventing the expansion of sulfide-based SSEs is an interplay between poor interfacial stability with the electrodes and massive external stack pressure required to maintain electrode-electrolyte contact. The need for extensive pressure requires large system-level (i.e., battery pack used in an electric vehicle) housing that causes a disconnect between performance at a smaller scale and actual application. Secondary prevention to sulfide-based SSE adoption are difficulties in manufacturing, as toxic deterioration occurs when these materials are exposed to humidity, as well as drastic reduction in SSE performance at low temperature. This work hypothesizes that unique interfacial designs of electrodes and the modification of the sulfide-based SSE will enable reduction of necessary external cell pressure, and therefore support the design of practical LMBs. This will be done through collaboration within Idaho National Laboratory (INL), where manufacturing practices will be parameterized to produce low defect, low porosity SSEs with slight modifications. Next, artificial interfaces will be produced on electrodes to observe the conformality and mass transport properties between the modified SSE and pre-treated anode. External pressure on Li-metal cells will also be parameterized to reduce interfacial impedance while a reduction in the pressure will allot reasonable housing design for larger scale applications. Focus on novelty in this work occurs by modifications to the solid-solid interfaces between electrolyte and electrode, done through doping of the electrolyte and production of artificial interfaces on the Li-metal anode. The modifications at these interfaces, in addition to modified external pressure could identify and address the poor interfacial impedance that hinders high performance SSEs. Fundamental understanding on how to reduce the key hindrances of all-solid-state batteries (ASSBs) will support the advancement for larger scale production and performance, of which will be held in perspective for future works. Beyond battery development, the knowledge gained from process control and defect analysis is applicable to other ceramic systems, such as nuclear fuel coatings and high temperature electrolyzers.

25 ENERGY STORAGE↗

DOE OSTI2023

Development, Characterization, and Testing of Solid-State Electrolytes for Batteries

25 ENERGY STORAGE↗

DOE OSTI2024

Equipment Qualification Report Environmental Qualification of GNB Absolyte Valve Regulated Lead Acid (VRLA) 1600 Ah100G33 Battery Rack Assembly (24590-QL-POA-EDB0-00001-11-00002_00A)

Greenberry Environmental Qualification Report 550001.001-35.0.5 provides basis for assignment of qualified life for: GNB Absolyte Valve Regulated Lead Acid (VRLA) 1600 Ah 100G33 Battery Rack Assembly in accordance with the requirements specified 24590-WTP-3PS-G000-T0015 (Rev 2) and Environmental Qualification Plan 550001.001-35.0.1 (Rev. 3). The equipment qualification basis represents the most conservative capability of the equipment. The analysis performed for the qualification is not less conservative than the bounding environmental conditions detailed in contract documents issued to Greenberry in contract 24509-QL-POA-EDB0-00001 Rev.0. The qualified life of 10 years has been established based upon an end-condition objective of the equipment condition indicators that correlate to the ability of equipment to perform its safety function. The VRLA Battery Cell Assembly was aged by 10 years (minimum) in accordance with conditions specified by Bechtel Equipment Qualification Datasheet 24590-LAW-EUQ-UPE 00003 Rev. 3 and the process conditions specified by the Instrument Data Sheet 24590-LAW EUD-UPE-00009 Rev. 2. Greenberry Industrial has contracted with GNB Industrial Battery Co located at 4115 S Zero St, Fort Smith, AR 72908 to perform age conditioning, monitoring, and capacity testing in accordance with Environmental Qualification Plan 550001.001-35.0.1 Rev. 1. The required process at the stated conditions set by the parameters established by the plan were completed satisfactorily. The details of the of the test process observed by Greenberry is detailed in the attached Seismic Test Log 550001.001-7.0.3, including examples of the objective evidence collected during the qualification process.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2023

Energy and Power Evolution Over the Lifetime of a Battery

Li-ion batteries currently are dominant energy storage devices for electric vehicles. Rechargeable batteries with lower cost, longer lifetime, and higher safety are desired in support of building of a green grid infrastructure. The continued investment in new battery materials, novel battery structures, advanced manufacturing processes, and accelerated testing/validation of battery performance has led to significant progress in battery development and deployment. Battery safety/reliability, which is essential to the success of a battery technology in the real world, naturally becomes the next big topic in battery research. Recently, the increasing interest in long-duration storage, fast charging, battery secondary use, and material recycling to build a circular industry and sustainable material supply chain has compelled further attention to understand the energy/power evolution and safety over the lifetime of a battery. Here, in this short Viewpoint, we discuss some high-level analyses on the energy/power evolution of rechargeable batteries over their life cycles aiming to inspire more discussion on the safety and sustainability of some representative and emerging battery technologies.

25 ENERGY STORAGE↗

DOE OSTI2021

Tutorial: Machine Learning and Artificial Intelligence in Batteries

Machine learning (ML) promises to compress the time needed to characterize battery performance, lifetime and safety. By coupling ML with physical models and metrics, that learning can bridge across materials, chemistries and cell designs. This tutorial will discuss the most popular ML techniques and resources and review recent work in the electrochemical literature. Applications include materials discovery, image recognition for quantitative microscopy analysis, fast charge algorithm development and life prediction.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

Beyond conventional batteries: a review on semi-solid and redox targeting flow batteries-LiFePO{sub 4} as a case study.

Clean and sustainable energy is becoming increasingly crucial to tackle the current energy crisis. However, the intermittent nature of renewable energy sources presents a challenge for their effective implementation. Redox flow batteries (RFBs) have emerged as a promising solution to this problem, as they can help enhance the stability of grid networks and promote the use of renewable energy sources. RFBs are highly modular and scalable systems that can be customized to meet the power and energy requirements of different renewable energy plants. Moreover, they offer several advantages over conventional battery technologies, including cost and safety concerns. However, conventional RFBs have limited energy densities due to the low solubility of their active species in electrolyte. To overcome this limitation, semi-solid (SSRFBs) and redox targeting (RTFBs) flow batteries have been proposed. These systems feature high concentrations of active species and impressive energy densities, making them highly attractive for renewable energy applications. LiFePO4 (LFP) is a highly promising active material for semi-solid and targeting flow batteries. One of the key advantages of LFP is its low raw materials cost, as it is composed of Earth-abundant elements such as iron and phosphorus. This makes it an attractive option for large-scale battery production. The recent developments in SSRFBs and RTFBs using LFP as catholyte hold great promise for the future of sustainable energy storage. The combination of LFP's low cost, safety, durability, and high energy density with the modularity and scalability of flow battery systems make for a compelling solution to the challenges of intermittent renewable energy sources. Ongoing research and development in this area will likely yield even further improvements in the performance and efficiency of LFP-based flow batteries, opening exciting new possibilities for sustainable energy storage.

El Halya, Nabil↗

DOE OSTI2026

Particle‐Size‐Dependent Lithium‐Ion Transport in PEO/LLZO Composite Electrolytes

Lithium-metal batteries with solid electrolytes can deliver higher energy density and improved safety than conventional Li-ion batteries. Among solid electrolyte candidates, polymer/ceramic composite electrolytes are attractive because they combine polymer flexibility with the high ionic conductivity of ceramics. However, whether ceramic fillers synergistically reduce polarization losses in the polymer matrix remains unclear. A central unknown is the critical polymer/ceramic interfacial resistance (Rint,crit), below which adding ceramics lowers electrolyte overpotential. Here, we present the first macroscale model framework to quantify R int,crit for composite electrolytes based on polyethylene oxide (PEO) and Ta-doped Li 7 La 3 Zr 2 O 12 (LLZO). A 1D model for DC-polarization of tri-layer cells (PEO-LiTFSI/LLZO/PEO-LiTFSI) shows that LLZO surface functionalization reduces the PEO/LLZO interfacial resistance, consistent with electrochemical impedance measurements. Extending to a 2D composite model, we show notably that Rint,crit scales linearly with LLZO particle diameter and shifts toward experimentally accessible values (e.g., 28.8 Ωcm 2 ) as particle size increases. At fixed ceramic volume fraction, larger LLZO particles reduce the number of interfacial crossings, driving more current through the ceramic phase and lowering concentration polarization. In contrast, R int,crit is largely independent of ceramic volume fraction. These results demonstrate that ceramic filler-size engineering can enable synergistic, energy-efficient transport in polymer/ceramic composite electrolytes.

25 ENERGY STORAGE↗

DOE OSTI2021

Toward the Understanding of the Reaction Mechanism of Zn/MnO2 Batteries Using Non-alkaline Aqueous Electrolytes

Zn/MnO 2 systems using non-alkaline aqueous electrolytes have attracted tremendous interest as rechargeable aqueous Zn ion batteries due to their safety and high specific capacities. Despite their promising electrochemical performance, however, their reaction mechanism has remained elusive. Here in this paper, we examined the structural evolution of cryptomelane α-MnO 2 cathode by ex situ transmission electron microscopy after electrochemical testing using two different non-alkaline aqueous Zn electrolytes with acetate and triflate salts of different pH values. We have discovered that the systems tested in both electrolytes exhibit a dissolution–deposition reaction mechanism through dissolution–deposition of Mn 2+ ions from/on the cathodes with a display of similar discharge/charge product formation. We have also found that the cell tested using the acetate electrolyte shows evidence of structural irreversibility that might contribute to its rapid capacity degradation. This finding offers an important insight into optimizing the cathode design for enhanced electrochemical function of aqueous Zn/MnO 2 batteries.

25 ENERGY STORAGE↗

DOE OSTI2021

Depowering of Batteries to Reduce Cost of Ownership

(1) Executive Summary: End of life batteries (EOLBs) present a cost and safety liability for their owners and stakeholders. This is due flammability, energy, and power with EOLBs. Current approaches include cumbersome, expensive packaging, specialized shipping, regulated storage, and they are responsible for over half of the cost of recycling. They all expensively and inadequately address symptoms. OnTo has developed and proven a simple way to resolve the problem systemically, through depowering of lithium-ion batteries (and most any battery other than lead). The low-cost process removes flammability, power, and energy in EOLBs through non-toxic chemical processing. The opportunity for commerce of inert scrap is at least $5 billion greater than the commerce in hazardous scrap, all made possible through OnTo’s technology for efficiency and safety. (2) Depowering Improves Safety and Decreases Cost of Battery Ownership: OnTo’s depowering technology will remove half of the cost of EOLB management and recycling. Without this technology, EOLB recycling will always be a liability. EOLB is hazardous due to inherent flammability of electrolyte and lithium. The shipping and commerce of EOLBs is costly and dangerous all along the chain of custody from owner, dealership/shop, shipper, second-life sorter, (shipper again), and finally to the destination facility recycler. OnTo’s depowering service renders inert most any EOLB packs, modules, and cells. The technology uses a brief, non-toxic treatment applicable to most any chemistry. The industry needs a safe, simple, modular, and inexpensive method to render EOLBs as inert scrap. OnTo’s deactivation system is scalable to the needs of any customer along the EOLB chain of custody. (3) Evidence of Successful Depowering: Untreated batteries will catch fire and explode under abuse conditions such as heat or crush. Slide 2 below shows that untreated batteries will blow-up and expel their internal components with heating, after OnTo’s depowering treatment, the same battery is inert with the same heat treatment (Fig. 7 in the slide). Depowering also removes electrolyte reactivity, eliminating the production of HF and other toxins (Fig 6. in the slide) The depowering process is applicable to large, 26 Ah cells. Fig. 5 in the slide shows the removal of all the electrolyte from whole cells. Removal of flammable material from an EOLB contributes to the inert behavior. OnTo developed this technology through a project supported by the US Department of Energy EERE program, with partners including Seattle King County Metro Transit. While OnTo has generated evidence of successful depowering of batteries, in 2020, a follow-on voucher opportunity for third party analysis of depowered cells and materials was approved through CalTestBed. The expertise of the battery and materials research groups at Lawrence Berkeley National Laboratory will characterize these depowered cells to provide better understanding of the materials level changes in depowering. (4) Pilot Plant for Depowering EOLBs: Making the spoke work in hub-and-spoke While other companies are marketing the hub-and-spoke approach for recycling EOLBs, they rely on dangerous, expensive shredding methods with flimsy IP protection. OnTo offers the only patented, proven ability to depower EOLBs from most any chemistry – at half of the capital cost required for shredding, while eliminating the liability, danger, and waste streams inherent with shredding. The proposed commercial pilot facility is (5) OnTo Technology LLC Company: OnTo develops advanced battery recycling innovations that produce manufacturing quality electrode materials from recycled batteries. Their patented Cathode-healing™ and Deactivation/Depowering processes improve safety and reduce the cost of recycling. OnTo’s breakthrough technologies produce advanced materials for manufacturing batteries useful in applications from portable power to electric vehicles. Contact: Steve Sloop OnTo Technology LLC, 63221 Service Road, STE F, Bend, OR 97703, ssloop@onto-technology.com , 541-389-7897

deactivation↗

DOE OSTI2020

Identification and characterization of the dominant thermal resistance in lithium-ion batteries using operando 3-omega sensors

Poor thermal transport within lithium-ion batteries fundamentally limits their performance, safety, and lifetime, in spite of external thermal management systems. All prior efforts to understand the origin of batteries' mysteriously high thermal resistance have been confined to ex situ measurements without understanding the impact of battery operation. Here, we develop a frequency-domain technique that employs sensors capable of measuring spatially resolved intrinsic thermal transport properties within a live battery while it is undergoing cycling. Our results reveal that the poor battery thermal transport is due to high thermal contact resistance between the separator and both electrode layers and worsens as a result of formation cycling, degrading total battery thermal transport by up to 70%. We develop a thermal model of these contact resistances to explain their origin. These contacts account for up to 65% of the total thermal resistance inside the battery, leading to far-reaching consequences for the thermal design of batteries. Finally, our technique unlocks new thermal measurement capabilities for future battery research.

25 ENERGY STORAGE↗

DOE OSTI2020

Controlled Dy-doping to nickel-rich cathode materials in high temperature aerosol synthesis

Layered nickel-rich materials are promising next-generation cathode materials for lithium ion batteries due to their high capacity and low cost. However, the poor thermal stability and longtime cycling performance hinders the commercial applications of high nickel materials. Doping with heteroatoms has been an effective approach for improving electrochemical performance of cathode materials. Controlling doping concentration and geometrical distribution is desired for optimal electrochemical performance, but it is challenging in traditional co-precipitation methods. In this work, controlled dysprosium (Dy) doping to NCM811 was studied in an aerosol synthesis method by controlling the precursor concentrations and heating parameters. The obtained materials were characterized by SEM, XRD, and XPS, and their electrochemical properties and thermal stability were evaluated. By controlling the doping concentration (1.5%), Dy-doped NCM811 was improved simultaneously in long-term cycling and high-rate performance. Here, the thermal-chemical stability of the Dy-doped cathode materials was examined in a microflow reactor with a mass spectrometer. The results showed that Dy-doping shifted the O 2 onset temperature to a higher temperature and reduced O 2 release by 80%, thus dramatically increasing the thermal-chemical stability and improving the fire safety of cathode materials. Since high temperature aerosol synthesis is a low-cost and scalable method, the findings in this work have broad implications for commercial synthesis of novel materials with controlled doping modification to achieve high electrochemical performance and safety in lithium ion batteries.

25 ENERGY STORAGE↗

DOE OSTI2021

Single-Ion Conducting Polymer Electrolytes for Solid-State Lithium–Metal Batteries: Design, Performance, and Challenges

Realizing solid-state lithium batteries with higher energy density and enhanced safety compared to the conventional liquid lithium-ion batteries is one of the primary research and development goals set for next-generation batteries in this decade. In this regard, polymer electrolytes have been widely researched as solid electrolytes due to their excellent processability, flexibility, and low weight. With high cationic transference numbers (t Li + close to 1), single-ion conducting polymer electrolytes (SICPEs) have tremendous advantages compared to polymer electrolyte systems (t Li + < 0.4) because of their potential to reduce the buildup of ion concentration gradients and suppress growth of lithium dendrites. The current review covers the fundamentals of SICPEs, including anionic unit synthesis, polymer structure design, and film fabrication, along with simulation and experimental results in solid-state lithium–metal battery applications. Overall, a perspective on current challenges, possible solutions, and potential research directions of SICPEs is also discussed to provide the research community with the critical technical aspects that may advance SICPEs as solid electrolytes in next-generation energy storage systems.

25 ENERGY STORAGE↗

DOE OSTI2021

Case Study of Recycling of Low Cobalt Batteries, OnTo Technology and King County Transit

Lithium-ion recycling is challenged by cost and safety related to low value elements and battery reactivity. OnTo is the first to demonstrate and develop technologies that address these challenges. Battery deactivation eliminates hazards and enables a roadmap for safe, low-cost end-of-life battery services essential to the industry. Deactivation coupled with Cathode-healing provides safety and efficiency in material recycling that can be applied all along the manufacturing value chain and for numerous chemistries in the market. Dr. Sloop will present recent developments in application and scale of these innovative technologies.

25 ENERGY STORAGE↗