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NASA NTRS2010

FIB-NanoSIMS-TEM Coordinated Study of a Wark-Lovering Rim in a Vigarano Type A CAI

Wark-Lovering (WL) rims are thin multi layered mineral sequences that surround most Ca, Al-rich inclusions (CAIs). Unaltered WL rims are composed of the same primary high temperature minerals as CAIs, such as melilite, spinel, pyroxene, hibonite, perovskite, anorthite and olivine. It is still unclear whether the rim minerals represent a different generation formed by a separate event from their associated CAIs or are a byproduct of CAI formation. Several models have been proposed for the origins of WL rims including condensation, flashheating, reaction of a CAI with a Mg-Si-rich reservoir (nebular gas or solid); on the basis of mineralogy, abundances of trace elements, O and Mg isotopic studies. Detailed mineralogical characterizations of WL rims at micrometer to nanometer scales have been obtained by TEM observations, but so far no coordinated isotopic - mineralogical studies have been performed. Thus, we have applied an O isotopic imaging technique by NanoSIMS 50L to investigate heterogeneous distributions of O isotopic ratios in minerals within a cross section of a WL rim prepared using a focused ion beam (FIB) instrument. After the isotopic measurements, we determine the detailed mineralogy and microstructure of the same WL FIB section to gain insight into its petrogenesis. Here we present preliminary results from O isotopic and elemental maps by NanoSIMS and mineralogical analysis by FE-SEM of a FIB section of a WL rim in the Vigarano reduced CV3 chondrite.

Cai, A.↗

NASA NTRS2006

Tensile and Creep Property Characterization of Potential Brayton Cycle Impeller and Duct Materials

This paper represents a status report documenting the work on creep of superalloys performed under Project Prometheus. Cast superalloys have potential applications in space as impellers within closed-loop Brayton cycle nuclear power generation systems. Likewise wrought superalloys are good candidates for ducts and heat exchangers transporting the inert working gas in a Brayton-based power plant. Two cast superalloys, Mar-M247LC and IN792, and a NASA GRC powder metallurgy superalloy, LSHR, are being screened to compare their respective capabilities for impeller applications. Several wrought superalloys including Hastelloy X, (Haynes International, Inc., Kokomo, IN), Inconel 617, Inconel 740, Nimonic 263, and Incoloy MA956 (Special Metals Corporation, Huntington, WV) are also being screened to compare their capabilities for duct applications. These proposed applications would require sufficient strength and creep resistance for long term service at temperatures up to 1200 K, with service times to 100,000 h or more. Conventional tensile and creep tests were performed at temperatures up to 1200 K on specimens extracted from the materials. Initial microstructure evaluations were also undertaken.

Gabb, Timothy P.↗

DOE OSTI2025

Fatigue Performance of an Improved Creep Strength 10%Cr Steel

The deployment of 9-12% Cr steels for elevated temperature applications up to 650 °C presents a cost-effective alternative to more expensive nickel-based alloys in steam turbine power generation. To enhance creep resistance at this temperature range, a novel ferritic-martensitic steel, designated CPJ7, was developed and fabricated at the National Energy Technology Laboratory. The alloy design aimed to mitigate the transformation of strengthening carbides into deleterious phases that degrade creep performance. Results have demonstrated that CPJ7 exhibits favorable creep and oxidation resistance at 650 °C. However, its fatigue performance remains unexplored. This study builds upon prior research by evaluating the low cycle fatigue behavior of CPJ7 and verifying that modifications beneficial to creep performance were not detrimental to the fatigue performance. The alloy was tested at both 650 °C and ambient temperature under fully reversed bending conditions (R = − 1) and a load ratio of 0.05. Furthermore, the alloy exhibits cyclic softening, a behavior consistent with other 9-10 wt.% Cr steels. Analysis of the microstructure and hysteresis loops further corroborate cyclic softening mechanisms typical of ferritic-martensitic steels. Overall, the fatigue performance of CPJ7 meets or exceeds that of P91 steel, demonstrating its potential for high-temperature structural applications.

9% Cr ferritic-martensitic steel↗

DOE OSTI2023

Achieving superior mechanical properties: Tailoring multicomponent microstructure in AISI 9254 spring steel through a two-stage Q&P process and nanoscale carbide integration

In the pursuit of lightweight, durable steel, we have successfully developed a multicomponent structure in AISI 9254 spring steel using a two-stage quenching and partitioning (Q&P) process. The primary objective of this process was to engineer an optimized microstructure consisting of nanobainite, martensite, and nano-carbides. Utilizing the insights gained from the results of advanced techniques such as X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and atom probe tomography (APT) performed on the as-received AISI 9254 spring steel, we refined the quenching and partitioning (Q&P) path, leading to the successful establishment of a bainitic transformation for superior mechanical properties. Our tensile tests revealed a high yield strength (≈ 1600 ± 25 MPa) and ultimate tensile strength (≈ 1850 ± 50 MPa), along with considerable elongation (≈ 11.15 ± 0.25%). We also identified that pre-formed martensite lath defects and high silicon content play crucial roles during the Q&P process, preventing carbide coalescence and increasing strain-hardening capacity. Finally, this study demonstrates the potential of a Q&P process to generate high-strength, ductile steel for automotive and aerospace applications.

36 MATERIALS SCIENCE↗

NASA NTRS2015

Particle Morphology and Elemental Composition of Smoke Generated by Overheating Common Spacecraft Materials

Fire safety in the indoor spacecraft environment is concerned with a unique set of fuels which are designed to not combust. Unlike terrestrial flaming fires, which often can consume an abundance of wood, paper and cloth, spacecraft fires are expected to be generated from overheating electronics consisting of flame resistant materials. Therefore, NASA prioritizes fire characterization research for these fuels undergoing oxidative pyrolysis in order to improve spacecraft fire detector design. A thermal precipitator designed and built for spacecraft fire safety test campaigns at the NASA White Sands Test Facility (WSTF) successfully collected an abundance of smoke particles from oxidative pyrolysis. A thorough microscopic characterization has been performed for ten types of smoke from common spacecraft materials or mixed materials heated at multiple temperatures using the following techniques: SEM, TEM, high resolution TEM, high resolution STEM and EDS. Resulting smoke particle morphologies and elemental compositions have been observed which are consistent with known thermal decomposition mechanisms in the literature and chemical make-up of the spacecraft fuels. Some conclusions about particle formation mechanisms are explored based on images of the microstructure of Teflon smoke particles and tar ball-like particles from Nomex fabric smoke.

Smoke↗

DOE OSTI2021

Postirradiation characterization of palladium as an additive for fuel cladding chemical interaction mitigation in metallic fuel

This work describes the microstructural and elemental characterization of irradiated metallic fuels containing palladium as an additive. The use of additives has been proposed to control Fuel-Cladding Chemical Interaction (FCCI) and thus to promote higher fuel utilization (i.e., higher burnup). In this work, Pd has been investigated as a potential additive to metallic fuel to bind lanthanides, impeding their migration and attack on the cladding. The influence of Pd on the microstructure, chemistry and performance of metallic fuel has been characterized via scanning electron microscopy for two metallic fuel designs—namely, annular and solid fuel. Pd was observed to play an important role in the chemistry of the fuel. Indeed, the addition of Pd leads to the formation of new phases. Pd was detected to combine not only with the lanthanides, as intended, but also with Zr, a main element of the fuel matrix. While Pd proved to be effective in preventing lanthanide migration and their attack on the cladding, the Pd-Zr compound may potentially lead to other unexpected fuel-performance issues, such as the formation of low-melting point phases and increased unalloyed U available for FCCI interaction with Fe in the cladding. Even the increase of Zr to 13wt%. did not completely mitigate this adverse phenomenon generated by the Pd-Zr interaction. Furthermore, the efficacy of using this additive needs further investigation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1996

Investigation of Polymer Liquid Crystals

The positron annihilation lifetime spectroscopy (PALS) using a low energy flux generator may provide a reasonably accurate technique for measuring molecular weights of linear polymers and characterization of thin polyimide films in terms of their dielectric constants and hydrophobity etc. Among the tested samples are glassy poly arylene Ether Ketone films, epoxy and other polyimide films. One of the proposed techniques relates the free volume cell size (V(sub f)) with sample molecular weight (M) in a manner remarkably similar to that obtained by Mark Houwink (M-H) between the inherent viscosity (eta) and molecular wieght of polymer solution. The PALS has also demonstrated that free-volume cell size in thermoset is a versatile, useful parameter that relates directly to the polymer segmental molecular weight, the cross-link density, and the coefficient of thermal expansion. Thus, a determination of free volume cell size provides a viable basis for complete microstructural characterization of thermoset polyimides and also gives direct information about the cross-link density and coefficient of expansion of the test samples. Seven areas of the research conducted are reported here.

Han, Kwang S.↗

DOE OSTI2024

Development of creep resistant ferritic-martensitic steels for operation at 650°C

Creep resistant ferritic-martensitic steels capable of operating at 650°C have long been under development for electricity generation. This presentation will showcase the design and development of alloys CPJ-7 and JMP with approximately 420,000 h of in-house creep testing, the equivalent of ~50 years of cumulative creep tests. Approximately fifty different alloy compositions were manufactured as part of an ICME approach. CPJ-7 present superior creep properties compared to COST alloys for steam turbine and P91/92 for boiler applications. The prolonged creep life was attributed to slowing down the destabilization of fine precipitates at 650°C. The JMP steels were designed with higher Co for solid solution strengthening and increased W for matrix strength and stability. The creep life compared to CPJ-7 increased between 118 and 150% at 650°C depending on the stress. On a Larson-Miller plot, the performance of the JMP steels surpasses that of MARBN steel. Composition-microstructure-properties relationships will be discussed.

Detrois, Martin↗

DOE OSTI2025

Myna: Connecting powder bed fusion build data to simulation tools for digital twin applications

Additive manufacturing (AM), as a digital process, can generate a detailed digital thread linking a part’s design and manufacturing to its operational performance. As AM systems advance, an increasing amount of process data is stored in manufacturing databases. In principle, this data can be utilized by simulation-based digital twin approaches, such as real-time process control and asynchronous post-processing guidance. However, few tools currently exist for systematically integrating digital thread data with computational tools. Here, in this study, we propose a software package, called Myna, for connecting data from powder bed fusion processes to simulation tools. The utility of such a platform is demonstrated using build data from the Oak Ridge National Laboratory Manufacturing Demonstration Facility “Peregrine v2023-10” public dataset to automatically configure and run 54 semi-analytical 3DThesis melt pool simulations, 78 numerical Additive FOAM melt pool simulations, and 3 ExaCA microstructure simulations. The simulated, spatially registered microstructures are then compared directly with electron backscatter diffraction characterization of the corresponding as-built part locations. The resulting simulated microstructure showed variation as a function of process parameters, particularly stripe width; however, the experimental data had little variation between the microstructure texture and grain size resulting from different processing conditions. Analysis of the discrepancies suggest that it is possible a two-phase ferritic-austenitic solidification model is needed to accurately predict grain size and texture for certain stainless steel 316L feedstock compositions under powder bed fusion conditions, providing direction for future research. As illustrated here, due to the number and complexity of the simulations involved in AM process-structure–property predictions, automated methods to connect process data and simulations will remain necessary tools for testing hypotheses and implementing digital twin applications.

Knapp, Gerald L. [Oak Ridge National Laboratory (O↗

DOE OSTI2025

An engineering perspective on evaluating mechanisms governing ductility in pure molybdenum

The United States lacks a stable domestic supply of 99 mTc, a critical medical imaging isotope generated from 99 Mo. Accelerator-based production using 100 Mo targets (aMo) introduces mechanical concerns due to the ductile-to-brittle transition temperature inherent to refractory metals like Mo. This study evaluates the tensile behavior of aMo targets from 25 to 1000 °C, compared to powder-metallurgy-processed natural Mo (PMo) and cast-and-rolled Mo (RMo), both as-received and after 5 ppm O 2 exposure in flowing He. RMo showed superior ductility (7.3% at 25 °C, 48% at 1000 °C) and strength, attributed to its fine, elongated grains and high geometrically necessary dislocation density. PMo exhibited variable ductility (up to 33%), while aMo remained brittle, with a maximum elongation of 10.4% at 600 °C. EBSD analysis revealed weak texture in PMo and aMo, but high defect density in aMo limited dislocation mobility. This work links processing, microstructure, and deformation mechanisms to guide fabrication of ductile refractory targets.

Hyer, Holden C. [Oak Ridge National Laboratory (OR↗

NASA NTRS2022

Imaging the End-to-End Dynamics of the Global Solar Wind-Magnetosphere Interaction

Much of what we know about the solar wind’s interaction with the Earth’s magnetosphere has been gained from isolated in situ measurements by single or multiple spacecraft. Based on their observations, we know that reconnection, whether on the dayside magnetopause or deep within the Earth’s magnetotail, controls the flow of solar wind energy into and through the global system. We know that nightside activity provides the energized particles that power geomagnetic storms. But by their very nature these isolated in situ measurements cannot provide an instantaneous global view of the entire system or its cross-scale dynamics. As a result, we don’t know which mode of reconnection prevails on the dayside magnetopause or within the magnetotail as a function of solar wind and geomagnetic conditions. We don’t know which mode or modes of nightside activity supply the most energized particles to the ring current. Nor do we know the dominant loss mode for ring current decay: precipitation, magnetopause outflow, or charge exchange with neutrals. Nor do we know how processes deep within the magnetosphere provide feedback to those happening in the outer magnetosphere. The answers to these questions could have an impact far beyond magnetospheric physics, since magnetic reconnection, particle acceleration, and charge-exchange are fundamental plasma processes that operate at other planets and throughout the universe. Comprehensive end-to-end global imaging of the key micro, meso-, and macro-scale plasma structures that comprise the magnetosphere will provide the answers to these questions via observations with a spatial resolution that exceeds anything possible with in situ measurements. Each proposed interaction mechanism generates a diagnostic plasma structure or boundary signature. Global, end-to-end, imaging provides the pathway to understanding the system as a whole, its constituent parts, and its cross-scale processes on a continuous basis, as needed to quantify the flow of solar wind energy through the global magnetospheric system. The significance of each mechanism is the product of its amplitude and occurrence rate. This white paper describes how a comprehensively-instrumented single spacecraft in a high-latitude circular polar orbit can provide the essential observations needed to track and quantify the flow of solar wind energy through the magnetosphere, including the solar wind plasma and magnetic field input, the magnetopause location in soft X-rays, the auroral oval in far ultraviolet, the ring current in energetic neutrals, the plasmasphere in extreme ultraviolet, the exosphere in Lyman-, the microstructure of the nightside auroral oval in ground-based all sky cameras, and the magnetic perturbations of ionospheric current patterns seen by ground-based magnetometers.

D G Sibeck↗

NASA NTRS2003

Microsample Characterization of Coatings for Grcop-84 for High Heat Flux Applications

A multidisciplinary Johns Hopkins University-NASA Glenn team is undertaking a collaborative research program to elucidate and model the thermal stability and mechanical integrity of candidate coatings for GRCop-84. GRCop-84 is a high conductivity, high strength copper alloy that was recently developed at NASA Glenn for use in high temperature, high heat flux applications. With potential applications in rocket motor combustion chamber liners, nozzle ramps and other actively cooled structures, this new material offers great potential for decreasing weight and increasing reliability of third generation reusable launch vehicles. Current emphasis has turned toward the development of environmentally resistant and thermal barrier coatings for this alloy. Metallic coatings such as NiCrAlY and Cu-8-30%Cr have shown promise in: prohibiting blanching, reducing dog-house failures, increasing operating temperatures and decreasing cooling requirements. The focus of this research program is to develop a fundamental understanding of the substrate-coating interactions that occur during thermal cycling (inter-diffusion, viscoplasticity, morphological evolution, crack formation, etc.) and to derive a science-based protocol for future coating selection, optimization and reliability assurance. The microsample tensile testing approach adopted for this study allows us to characterize small-scale and highly scale-specific coatings and properties in a way not possible by conventional means. In addition to providing much needed design data, the integration of microsample testing with detailed microstructural observations provides a mechanistic foundation for coating optimization and life prediction modeling.

Hemker, Kevin↗

DOE OSTI2025

Demonstration of the Reproducibility Challenges in the Sintering Behavior of Lithium‐Stuffed Garnets in Scaling up Synthesis

Lithium-stuffed garnets, such as Li 7 La 3 Zr 2 O 12 (LLZO), are promising candidates for next-generation solid-state batteries because of their high room-temperature ionic conductivity and chemical stability against lithium metal anodes, which are crucial for achieving higher energy density. However, realizing LLZO's potential in practical devices requires synthesis methods that can be scaled reliably to large batch sizes for manufacturing. Herein, we investigate the sintering reproducibility of LLZO synthesized at larger scales using ultrasonic spray pyrolysis, a cost-effective and scalable synthesis route. Two 100 g batches of Al-doped LLZO are prepared and their sintering behavior is examined in detail. Both Al-LLZO batches contain over 90 wt.% cubic-phase LLZO, and both batches exhibit room temperature conductivities greater than 1 × 10 −4 S cm −1 at a relative density above 0.8. However, variations in secondary phases and subtle differences in Al content lead to significant differences in densification and microstructure. These results demonstrate that LLZO's sintering behavior is highly sensitive to small changes in secondary phases and Al content, creating reproducibility challenges when moving from laboratory- to manufacturing-scale synthesis.

36 MATERIALS SCIENCE↗

NASA NTRS1999

Feature Profile Evolution of SiO2 Trenches In Fluorocarbon Plasmas

Etching of silicon microstructures for semiconductor manufacturing in chlorine plasmas has been well characterized. The etching proceeds in a two-part process, where the chlorine neutrals passivate the Si surface and then the ions etch away SiClx. However, etching in more complicated gas mixtures and materials, such as etching of SiO2 in Ar/C4F8, requires knowledge of the ion and neutral distribution functions as a function of angle and velocity, in addition to modeling the gas surface reactions. In order to address these needs, we have developed and integrated a suite of models to simulate the etching process from the plasma reactor level to the feature profile evolution level. This arrangement allows for a better understanding, control, and prediction of the influence of equipment level process parameters on feature profile evolution. We are currently using the HPEM (Hybrid Plasma Equipment Model) and PCMCM (Plasma Chemistry Monte Carlo Model) to generate plasma properties and ion and neutral distribution functions for argon/fluorocarbon discharges in a GEC Reference Cell. These quantities are then input to the feature scale model, Simulation of Profile Evolution by Level Sets (SPELS). A surface chemistry model is used to determine the interaction of the incoming species with the substrate material and simulate the evolution of the trench profile. The impact of change of gas pressure and inductive power on the relative flux of CFx and F to the wafer, the etch and polymerization rates, and feature profiles will be examined. Comparisons to experimental profiles will also be presented.

Hwang, Helen↗

DOE OSTI2026

In-Situ TEM Molten Salt Corrosion

Molten salt reactors (MSRs) offer a compelling pathway for next-generation nuclear energy, with advantages in thermal efficiency, inherent safety, and flexible fuel management. Yet, halide-based molten salts introduce significant materials challenges, particularly alloy corrosion. Alloy performance in these environments ultimately depends on understanding how corrosion initiates and progresses at the nanoscale, however most existing models rely on post-exposure characterization, leaving degradation mechanisms largely inferred rather than directly observed. NiCr alloys have garnered interest in MSRs applications as the Ni-based matrix provides strength and creep resistance, while Cr content offers oxidation resistance in air. However, NiCr corrosion resistance in chloride salts has proven poor due to preferential chromium dissolution, the formation of Cr-depleted pathways, and grain-boundary attack. This work aims to directly visualize corrosion of Ni-20Cr exposed to LiCl-KCl using in-situ Transmission Electron Microscopy (TEM) to capture real-time microstructural evolution during corrosion. Experiments will be performed at ~800 °C under controlled pressure conditions while utilizing Energy-Dispersive X-ray Spectroscopy (EDS) to analyze elemental redistribution. Observation of chromium depletion fronts, associated surface restructuring, and localized chloride enrichment are expected. Ultimately, this study is expected to provide a link between microscale processes and the macroscopic degradation behaviors relevant to MSR operation in advanced reactor environments. Simultaneously, this approach enables future in-situ investigations regarding alloy composition, salt chemistry, and their influence on corrosion pathways and long-term stability.?

36 - MATERIALS SCIENCE↗

DOE OSTI2021

Bio-inspired strategies for next-generation perovskite solar mobile power sources

Smart electronic devices are becoming ubiquitous due to many appealing attributes including portability, long operational time, rechargeability and compatibility with the user-desired form factor. Integration of mobile power sources (MPS) based on photovoltaic technologies with smart electronics will continue to drive improved sustainability and independence. With high efficiency, low cost, flexibility and lightweight features, halide perovskite photovoltaics have become promising candidates for MPS. Realization of these photovoltaic MPS (PV-MPS) with unconventionally extraordinary attributes requires new ‘out-of-box’ designs. Natural materials have provided promising designing solutions to engineer properties under a broad range of boundary conditions, ranging from molecules, proteins, cells, tissues, apparatus to systems in animals, plants, and humans optimized through billions of years of evolution. Applying bio-inspired strategies in PV-MPS could be biomolecular modification on crystallization at the atomic/meso-scale, bio-structural duplication at the device/system level and bio-mimicking at the functional level to render efficient charge delivery, energy transport/utilization, as well as stronger resistance against environmental stimuli (e.g., self-healing and self-cleaning). In this paper, we discuss the bio-inspired/-mimetic structures, experimental models, and working principles, with the goal of revealing physics and bio-microstructures relevant for PV-MPS. Here the emphasis is on identifying the strategies and material designs towards improvement of the performance of emerging halide perovskite PVs and strategizing their bridge to future MPS.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2016

Development of Shape Memory Alloys- Challenges and Solutions

Shape memory alloys (SMAs) are a unique class of multifunctional materials that have the ability to recover large deformations or generate high stresses in response to thermal, mechanical andor electromagnetic stimuli. These abilities have made them a viable option for actuation systems in aerospace, medical, and automotive applications, amongst others. However, despite many advantages and the fact that SMA actuators have been developed and used for many years, so far they have only found service in a limited range of applications. In order to expand their applications, further developments are needed to increase their reliability and stability and to address processing, testing and qualification needed for large-scale commercial application of SMA actuators. In this seminar, historical inhibitors of SMA applications and current research efforts by NASA Glenn Research Center and collaborators will be discussed. Relationships between fundamental physicalscientific understanding, and the direct transition to engineering and design of mechanisms using these novel materials will be highlighted. Examples will be presented related to targeted alloy development, microstructural control, and bulk-scale testing as a function of stresses, temperatures and harsh environments. The seminar will conclude with a summary of SMA applications under development and current advances.

Shape Memory Alloy↗

DOE OSTI2025

Cold-Sprayed NMC622 Composite as a Cathode for Lithium-Ion Batteries

The growing demand for high-energy, low-cost lithium-ion batteries (LIBs) to power electric vehicles (EVs) necessitates advances in both materials and manufacturing processes. Conventional cathode fabrication methods, such as slurry casting and drying, are energy-intensive and pose challenges for scalability and environmental compliance. In this study, we propose cold-spray (CS) deposition as a solvent-free approach for fabricating LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622) composite cathodes. Powder blends of NMC622, poly(vinylidene fluoride) (PVDF), and carbon black (CB) are directly deposited onto stainless steel and Inconel substrates under varied gas temperatures, pressures (and thus velocities), and standoff distances. The effects of temperature on the deposit morphology, coating density, and volume are systematically investigated. Computational fluid dynamics simulations reveal that increasing the gas temperature enhances the particle velocity, narrows the spray angle, and reduces the mass concentration radially at the nozzle outlet. CS deposition results in a dense cathode microstructure, accompanied by fracture in polycrystalline NMC622 particles. X-ray diffraction analysis further verifies that there are no phase changes during the deposition process. The electrochemical performance of the cold-sprayed cathodes reveals an initial capacity of approximately 96 mAh g –1 for single-crystal NMC622 and 167 mAh g –1 for polycrystalline NMC622. While these values are modest compared to state-of-the-art slurry-cast cathodes, which typically exhibit 180–200 mAh g –1 under optimized conditions. The results demonstrate a competitive performance given the solvent-free nature of the CS process and compare favorably with tape-cast samples made from identical feedstock. In conclusion, he CS process enables the formation of dense, binder-integrated cathode coatings without the need for solvent processing, offering a promising pathway for scalable, energy-efficient dry electrode manufacturing of next-generation LIBs.

Batteries↗