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All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Review of Ultrasonic Methods for Monitoring, Damage Detection, and Processing of Lithium-Ion Batteries Throughout Their Life Cycle

Lithium-ion batteries (LIBs) are the leading technology used in consumer electronics, electric vehicles, and grid-level electrochemical energy storage applications. The ever-increasing use of LIBs has highlighted a gap in understanding of their behavior throughout their life cycle. Current monitoring systems rely on electrical and sometimes temperature measurements to assess the internal state which limits information about complex electrochemical processes. In response, ultrasonic testing (UT) has shown promise for non-invasive assessment due to its ease of use and sensitivity to mechanical changes which are correlated with electrochemical changes within the battery. We summarize the research in UT methods applied to LIBs throughout their life cycle. We also discuss physics-based and data-driven modeling approaches used to interpret ultrasonic signals in the context of LIBs, with an emphasis on the existing challenge of establishing rigorous links between electrochemical behavior and elastic and poroelastic wave physics to gain insight regarding physical changes in the LIB that can be directly measured using UT. Finally, we discuss the challenges of implementing UT across the LIB life cycle and identify opportunities for further research. This review aims to provide helpful guidance to researchers and practitioners of UT in the growing field of UT for electrochemical battery systems.

25 ENERGY STORAGE↗
DOE OSTI2022

Gamma ray analysis of the K2 containers

The K2 containers contain PuO2 with 238 Pu being the most abundant isotope of all plutonium isotopes. The purpose of this analysis is to determine the light element impurities in the PuO2. These light elements can interact with the alpha particles from plutonium decay to release gamma rays, protons, and neutrons through the reactions (α,α’), (α,p), and (α,n) respectively. The gamma rays released by the interactions can be measured and compared with the gamma rays released by the plutonium. The ratios of the gamma rays from the interactions and the plutonium gamma rays allow for the determination of the impurities in the items. The elements that can be detected are Lithium (Z=3), Beryllium (Z=4), Boron (Z=5), Fluorine (Z=9), Sodium (Z=11), Magnesium (Z=12), Aluminum (Z=13), Silicon (Z=14), Phosphorous (Z=15), Chlorine (Z=17), and Potassium (Z=19).

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2022

Quantification of Dead Lithium on Graphite Anode under Fast Charging Conditions

A series of computational and experimental studies were conducted to understand the onset of lithium plating and subsequent quantification of dead lithium on graphite electrodes in the design of fast charging batteries. The experiments include titration and relaxation studies for detecting initiation of lithium metal plating for various SOC and C-rates, which are compared against the thermodynamically consistent phase field computational results. The collaborative study on "model graphite electrode" with 2.18 mAh cm-2 nominal capacity at 25 degrees C demonstrates: (1) the macroscopic voltage response during relaxation studies indicate the reintercalation of plated lithium into the graphite anode; (2) for SOC below 60% and low C-Rates, there is no dead lithium; (3) for SOC between 60% to 80%, and C-Rates in the range of 4C-6C show dead lithium both in experiments and simulations; (4) at 100% SOC and 4C-6C rates, large amounts of dead lithium are observed. The study presented here allows us to evaluate the effects of the physical properties of the electrochemical system on plating and stripping kinetics and the amount of dead lithium on graphite electrodes, which determines the cell capacity loss under fast charge.

batteries↗
DOE OSTI2022

Deep-Learning-Enabled Crack Detection and Analysis in Commercial Lithium-Ion Battery Cathodes

We report in Li-ion batteries, the mechanical degradation initiated by micro cracks is one of the bottlenecks for enhancing the performance. Quantifying the crack formation and evolution in complex composite electrodes can provide important insights into electrochemical behaviors under prolonged and/or aggressive cycling. However, observation and interpretation of the complicated crack patterns in battery electrodes through imaging experiments are often time-consuming, labor intensive, and subjective. Herein, a deep learning-based approach is developed to extract the crack patterns from nanoscale hard X-ray holo-tomography data of a commercial 18650-type battery cathode. Efficient and effective quantification of the damage heterogeneity with automation and statistical significance is demonstrated. The crack characteristics are further associated with the active particles’ packing densities and a potentially viable architectural design is discussed for suppressing the structural degradation in an industry-relevant battery configuration.

25 ENERGY STORAGE↗
DOE OSTI2021

Lithium indium diselenide — An advanced material for neutron detection

Here, this paper describes the synthesis, crystal growth, detector fabrication, radiation hardening studies, MCNP modeling, and characterization of lithium indium diselenide or LiInSe 2 . This newly-developed room temperature thermal neutron detector has semiconducting and scintillating properties and it is suitable for neutron detection application. LiInSe 2 was synthesized starting from elemental Li, In, Se in two steps due to high reactivity of Li. A single crystal of LiInSe 2 was grown using the Vertical Bridgman method. The room temperature band gap was found to be 2.8 eV using optical absorption measurements. Bulk resistivity was measured at ∼5 × 10 11 Ωcm. Photoconductivity measurements of LiInSe 2 wafers identified a peak in the photocurrent around 445 nm. Nuclear radiation detectors were fabricated from single crystal wafer and the responses to alpha particles at various biases were measured. The mobility-lifetime product was estimated. Gamma irradiation studies were performed with calculated absorbed doses ranging from 0.2126 to 21,262 Gy. The characterization of the two wafers for their scintillator performance was conducted after each irradiation. The gamma irradiation produced a reduction of the light yield that translated to a lower channel number for the centroid of alpha detection spectra. It also showed a considerable reduction of the decay time after the first irradiation. These are the first studies on gamma radiation hardening with this material.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2021

Degradation Diagnostics from the Subsurface of Lithium-Ion Battery Electrodes

Despite the long-established rocking-chair theory of lithium-ion batteries (LIBs), developing novel characterization methodology with higher spatiotemporal resolution facilitates a better understanding of the solid electrolyte interphase studies to shape the reaction mechanisms. In this work, we develop a Xenon ion plasma focused ion beam (Xe + PFIB)-based characterization technique to probe the cross-sectional interface of both ternary cathode and graphite anode electrodes, with the focus on revealing the chemical composition and distribution underneath the electrode surface by in-depth analysis of secondary ions. Particularly, the lithium fluoride is detected in the pristine cathode prior to contact with the electrolyte, reflecting that the electrode degradation is in the form of the loss of lithium inventory during electrode preparation. This degradation is related to the hydrolysis of the cathode material and the decomposition of the PVDF binder. Here, through the quantitative analysis of the transition-metal degradation products, manganese is found to be the dominant element in the newly formed inactive fluoride deposition on the cathode, while no transition metal signal can be found inside the anode electrode. These insights at high resolution implemented via a PFIB-based characterization technique not only enrich the understanding of the degradation mechanism in the LIBs but also identify and enable a high-sensitivity methodology to obtain the chemical survey at the subsurface, which will help remove the capacity-fade observed in most LIBs.

25 ENERGY STORAGE↗
DOE OSTI2022

Damage of prismatic lithium‐ion cells subject to bending: Test, model, and detection

Abstract The mechanically induced internal short circuit (ISC) is one of the major safety concerns of lithium‐ion batteries. Mechanical abuse tests are often performed to evaluate the integrity and safety of lithium‐ion batteries under mechanical loadings. Except for the widely explored compression‐dominated indentation tests, bending is another typical real‐world loading condition that is tension‐dominated. To investigate the mechanical damage and ISC behavior of batteries under bending, we carried out controlled three‐point bending tests in four progressive steps on prismatic battery cells with maximum deflections ranging from 38% to 76% of the cell thickness. None of the tested cells experienced an ISC. We then conducted 3D X‐ray computed tomography (CT) scanning on the bent cells after unloading. X‐ray CT images showed three out of the four tested cells have extensive cracking in the electrode layers at the bottom side (opposite to the loading head). This indicates that cracking does not necessarily lead to an ISC under bending. Electrochemical impedance spectroscopy was also measured on the bent cells and substantial changes were observed. Both the bulk resistance and charge‐transfer resistance increased significantly after bending, which could influence the battery performance and lifespan. We then developed a detailed finite (FE) element model to further investigate the mechanical deformation and failure mechanisms. The FE model successfully predicts the load–displacement response and reproduces the deformation patterns. The findings and the FE model developed in the present study provide useful insights and tools for the battery structure and crash safety design. image

25 ENERGY STORAGE↗
DOE OSTI2025

Quantifying the Reactivity of Isolated Li x Si Domains in Si Anodes Using Operando NMR

The use of Si anodes can greatly improve the energy density of Li-ion batteries. However, understanding and mitigation of calendar aging remains a barrier to commercialization. Here, in this short report, we utilize operando Nuclear Magnetic Resonance (NMR) spectroscopy to detect and quantify lithium silicides (Li x Si) as they form and react within Si anodes in pouch cells during calendar aging. We provide direct experimental evidence of complex aging phenomena in the Si anodes, including both SEI growth and dissolution during storage. Formation of electrochemically isolated Li x Si is also observed, as indicated by the partial persistence of highly lithiated phases after the cell is discharged. Remarkably, we show that these isolated domains can themselves self-discharge over time, suggesting that their detection can be challenging in post-mortem studies. Finally, we show that aging outcomes depend heavily on the type of silicon particles contained within the electrode, and that certain surface coatings can help decrease the reactivity between lithium silicides and the electrolyte.

Li-ion battery↗
DOE OSTI2024

Water acidification aggravates lithium-induced toxicity represented by energy supply, oxidative stress, and cell fate in Daphnia magna neonates

Lithium is extensively utilized in industrial energy production, particularly in lithium-ion batteries, and in pharmaceuticals for the treating clinical mood disorders. Consequently, lithium is frequently detected in various environmental matrices. It has been reported to cause a range of toxic effects on aquatic organisms including oxidative stress, neurological disorders, and reproductive suppression. Water acidification is a global issue with numerous negative impacts on aquatic organisms. It can alter the physio-chemical properties and bioavailability of metal ions. The acidic leaching process during lithium battery treatment and global water acidification both suggest that lithium contamination often occurs in acidic environments. In the present study, Daphnia magna neonates were exposed to four treatments (control, lithium alone, low pH, and combined) to investigate whether an acidic environment exacerbates the toxic effects of lithium on aquatic organisms and to explore potential toxic action mechanisms. The results indicated that low pH posed a significant threat to the growth and reproduction of D. magna. When exposed to both lithium and low pH, there was increased lithium accumulation and an energy trade-off response, leading to increased energy allocation to reproduction and reduced energy for growth. Lithium exposure stimulated D. magna activity, while low pH inhibited it, suggesting that an imbalance in energy consumption and supply. Combined exposure to lithium and low pH resulted in severe oxidative stress due to mitochondrial dysfunction, under-utilization of energy substances, and increased ionic homeostasis disturbances. Consequently, the exposed organism altered apoptosis and autophagy processes to maintain homeostasis. In conclusion, the present study demonstrated that lithium and water acidification posed a population-level threat to D. magna, and their combined exposure significantly largely exacerbated the toxic effects.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗
DOE OSTI2021

Comprehensive Insights into Nucleation, Autocatalytic Growth, and Stripping Efficiency for Lithium Plating in Full Cells

Synchrotron high-energy X-ray diffraction is used to enable nondestructive detection and quantification of heterogeneous lithium plating in working batteries. In this study a LiNi 0.5 Mn 0.3 Co 0.2 O 2 /graphite pouch cell was operated under 6C fast-charge rate for greater than 1200 cycles. The magnitude and spatial distribution of lithium plating, lithium stripping, and the effect of metallic lithium deposition on lithium intercalation into graphite were quantified. Fully intercalated graphite (LiC 6 ) was detected after discharge with a lateral distribution closely correlated with lithium plating, which can be used as a higher-sensitivity indicator for lithium plating. Over an extended cycle life, the overall metallic lithium concentration followed a sigmoidal curve indicating two-stage continuous nucleation and autocatalytic growth. The lithium stripping efficiency underwent an exponential decay as a function of cycle life as the buildup of metallic lithium hindered the efficient dissolution back into the electrolyte. The findings provide direct insights into the characteristics of lithium plating and stripping under realistic fast-charge conditions.

25 ENERGY STORAGE↗
DOE OSTI2021

In Situ Visualization of Li-Whisker with Grating-Interferometry-Based Tricontrast X-ray Microtomography

The lithium-ion battery has demonstrated tremendous economic and social impacts. Upon battery operation under different conditions, lithium changes its chemical state and physical formation, leading to undesired side reactions, e.g., lithium dendrite growth that degrades the cell performance and causes safety concerns. In situ detection and visualization of lithium metal in functional batteries could offer insights with both scientific and industrial significance but remain a frontier challenge. In this work, we demonstrate in situ three-dimensional imaging of lithium whisker using a grating-interferometry-based tricontrast X-ray microtomography method. Our approach explicitly reveals the micromorphology of the electrochemically developed porous lithium whisker with micrometer-level spatial resolution while offering sensitivity to the nanoporosity that is smaller than the nominal resolution limit. Our result reveals valuable structural information on the lithium whisker that is otherwise inaccessible. This method is also readily applicable to a broad range of battery research, including all-solid-state batteries.

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

Synthesis and processing of lithium-loaded plastic scintillators on the kilogram scale

Plastic scintillators that can discriminate between gamma rays, fast neutrons, and thermal neutrons were synthesized and characterized while considering the performance at the kilogram scale. The synthesis and processing of these plastic scintillators on the kilogram scale required examination of several factors. The examination of these factors was necessitated by the inclusion of 0.1 wt.% lithium-6 to enable detection of thermal neutrons. First, methacrylic acid was used as an additive to solubilize salts of lithium-6, which allow for a thermal-neutron capture reaction that produces scintillation light following energy transfer. Second, a trade-off between scintillation performance and processability was considered because the increasing content of the methacrylic acid that aided processability resulted in a sharp decrease in the light output. The use of small amounts of methacrylic acid (≤3 wt.%) resulted in better performance but required high processing temperatures. At large scales, these high temperatures could initiate exothermic polymerization that results in premature curing and/or defects. Additionally, the deleterious effects of the methacrylic acid may be mitigated by using m-terphenyl as a primary dye rather than 2,5-diphenyloxazole (PPO), which has been traditionally used in organic scintillators. Finally, the curing environment was controlled to avoid defects like cracking and discolouration​ while maintaining solubility of dopants during curing. For scintillators that were produced from kilogram-scale batches of precursors, the effective attenuation of scintillation light was characterized.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Electrical Detection of Spin-Hall-Induced Auto-oscillations in Lithium Aluminate Ferrite Thin Films

Ferrimagnetic insulators with ultralow damping are of great interest for their potential applications in energy-efficient computing devices. Here, we report the direct electrical detection of magnetic auto-oscillations in unpatterned ultralow damping ferrimagnetic insulator epitaxial Li 0.5 Al 0.5 Fe 2 O 4 thin films, driven by a current in a proximal Pt nanowire. Auto-oscillations occur for only one current polarity, consistent with the spin-Hall effect inducing the oscillation state. Micromagnetic modeling shows good agreement with the experimental frequency and field dispersions, showing only one dominant oscillation mode, in contrast to the multiple modes typically observed in transition-metal nanowire-type spin-Hall nanooscillators. This study illustrates a new material system for neuromorphic computing and magnonics, a simple material platform with the direct-current generation of high-frequency (~10 GHz) signals and their electrical detection.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Analysis of hydrogen and lithium isotopes using Laser-Induced Breakdown Spectroscopy

The detection and quantification of hydrogen (1,2,3H) and lithium (6,7Li) isotopes are critical to several energy and defense application areas, including hydrogen storage, nuclear forensics, and safeguards/non-proliferation. In this context, laser-induced breakdown spectroscopy (LIBS) is very promising and it comes with certain advantages such as rapid detection, and standoff capability. Although LIBS provides experimental simplicity and is capable of detecting all elements in the periodic table in any phase (solid, liquid, or gas), there exist certain challenges for isotopic analyses of H and Li due to spectral broadening, the presence of closely spaced fine and hyperfine structures, and line distortion effects (e.g., self-absorption and self-reversal) present in laser-produced plasmas. This article reports recent developments in H and Li isotopic analysis using LIBS, and existing challenges.

(020.3260) Isotope shifts, (140.3440) Laser-induce↗
DOE OSTI2022

Resolving Graphite‐Electrolyte Interphase of Lithium‐Ion Batteries using Air‐Tight Ambient Mass Spectrometry

Abstract The formation of a stable solid electrolyte interphase (SEI) at graphite electrode is necessary for lithium‐ion batteries (LIB) to prevent excessive degradation of electrolytes. Until now, the exact organic composition of SEI has not been decisively determined with lithium ethylene mono‐carbonate (LEMC) being one of the debated components. An air‐tight ambient mass spectrometry (MS) platform is developed to directly characterize the air‐sensitive organic components present in SEI. Ionization occurs via a solvent‐free field‐induced process at atmospheric pressure. Our experimental data, based on tandem MS analysis, revealed LEMC to be the major organic component in SEI. This result resolves a long‐standing mystery surrounding the composition of native SEI in LIB, where no trace of the other debated compound, lithium ethylene dicarbonate, was detected. The energetics of fragmentation of LEMC and the corresponding stabilities of various ionic species detected during the air‐tight ambient MS analysis were calculated using density functional theory (DFT). Our findings confirmed favorable protonation energies and suggested the molecular structures for many of the detected species. Solvent (i. e., ethylene carbonate)‐induced stabilization effects observed during the ionization process were also confirmed by DFT. The reported study encourages the routine use of ambient mass spectrometry to characterize both anodic and cathodic electrodes of all battery types as well as to study other air‐sensitive materials in their native state.

25 ENERGY STORAGE↗
DOE OSTI2023

A mathematical approach to survey electrochemical impedance spectroscopy for aging in lithium-ion batteries

Electrochemical impedance spectroscopy (EIS) is a valuable technique to detect the health status and aging phenomena in lithium-ion batteries (LiB). Equivalent circuit modeling (ECM) is conventionally used when interpreting EIS data and gaining physical insights into the aging mechanisms. However, performing ECM is resource intensive and expert-level of knowledge is usually required to select suitable models and fitting parameters. This article presents a quick and user-friendly data analysis algorithm as an alternative to ECM by mathematically fitting geometric features in Nyquist plots and obtaining the growth trends of the features. The evolving trends in the Nyquist plots, such as chord lengths of the arcs and interception points, are consistent with the growth of resistance components obtained using ECM with R 2 values from 0.67 to 0.99, and therefore can be used as indicators of battery aging. Our results show that the quick-fitting approach is suitable for analyzing a series of EIS data acquired during battery cycling and identifying the underlying aging mechanisms.

Chen, Bor-Rong↗