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DOE OSTI2023

Suppressing Universal Cathode Crossover in High‐Energy Lithium Metal Batteries via a Versatile Interlayer Design**

Abstract The universal cathode crossover such as chemical and oxygen has been significantly overlooked in lithium metal batteries using high‐energy cathodes which leads to severe capacity degradation and raises serious safety concerns. Herein, a versatile and thin (≈25 μm) interlayer composed of multifunctional active sites was developed to simultaneously regulate the Li deposition process and suppress the cathode crossover. The as‐induced dual‐gradient solid‐electrolyte interphase combined with abundant lithiophilic sites enable stable Li stripping/plating process even under high current density of 10 mA cm −2 . Moreover, X‐ray photoelectron spectroscopy and synchrotron X‐ray experiments revealed that N‐rich framework and CoZn dual active sites can effectively mitigate the undesired cathode crossover, hence significantly minimizing Li corrosion. Therefore, assembled lithium metal cells using various high‐energy cathode materials including LiNi 0.7 Mn 0.2 Co 0.1 O 2 , Li 1.2 Co 0.1 Mn 0.55 Ni 0.15 O 2 , and sulfur demonstrate significantly improved cycling stability with high cathode loading.

Xie, Chuyi↗

DOE OSTI2023

Suppressing Universal Cathode Crossover in High‐Energy Lithium Metal Batteries via a Versatile Interlayer Design**

25 ENERGY STORAGE↗

DOE OSTI2020

Corrosion Mitigation and Increased Discharge Capacity in Aqueous Processed Thick Cathodes using Phosphoric Acid Additives

Aqueous processed cathodes for lithium-ion batteries are favorable for both cost and environmental reasons; however, these electrodes still face significant problems with increasing areal capacities (i.e. thickness). Highly basic slurry conditions (pH in excess of 12) corrode the current collector surface and evolve hydrogen gas. Consequently, bubbling at the electrode interface causes substantial damage to the dried electrode. As the loading of these electrodes is increased, damage becomes severe and results in lack of adhesion and cohesion. Here introduction of phosphoric acid to combat the rise in pH and suppress the corrosion at the current collector surface is investigated. Phosphoric acid was added in increments of 0.5, 1.0, and 1.5 wt% and the subsequent effects on slurry rheology, particle size, adhesion, and electrochemical cycling were investigated. A technique is reported for obtaining thick (6-8 mAh/cm2) cathodes that exhibit reduced surface cracking and improved rate performance as compared to control samples.

Kukay, Alexander↗

DOE OSTI2023

Galvanic corrosion of AZ31B joined to dual-phase steel with and without Zn layer by ultrasonic and friction stir welding

Galvanic corrosion of AZ31B joined with bare or Zn-coated DP590 steel by ultrasonic spot welding or linear friction stir welding was quantitatively studied by pre-defining anode and cathode in the lap joint samples. Corrosion volume and depth from Mg anode surfaces exposed to 0.1 M sodium chloride solution was analyzed as functions of cathode surface type and welding method. Characterization of as-welded joints was performed to identify any microstructural feature of the bonding zone that could impact galvanic corrosion behavior. COMSOL modeling with modified user subroutine was conducted to simulate the progression of Mg corrosion in the same joint and electrode configurations used for the corrosion experiments. The experimental results indicated that Zn-coated cathode surface can reduce Mg galvanic corrosion significantly as galvanic polarization and cathodic current on Zn-coated surface remained relatively low for Mg in the weld joints. COMSOL modeling described the growth of Mg galvanic corrosion in a reasonable manner but showed limitation by underestimating the corrosion volume as it did not capture self-corrosion.

36 MATERIALS SCIENCE↗

DOE OSTI2020

A Garnet-Type Solid-Electrolyte-Based Molten Lithium–Molybdenum–Iron(II) Chloride Battery with Advanced Reaction Mechanism

Solid-electrolyte-based molten-metal batteries have attracted considerable attention for grid-scale energy storage. Although ZEBRA batteries are considered one of the promising candidates, they still have the potential concern of metal particle growth and ion exchange with the β”-Al 2 O 3 electrolyte. Herein, a Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 solid-electrolyte-based molten lithium–molybdenum–iron(II) chloride battery (denoted as Li–Mo–FeCl 2 ) operated at temperature of 250 °C, comprising a mixture of Fe and LiCl cathode materials, a Li anode, a garnet-type Li-ion ceramic electrolyte, and Mo additive, is designed to overcome these obstacles. Different from conventional battery reaction mechanisms, this battery revolutionarily synchronizes the reversible Fe–Mo alloying–dealloying reactions with the delithiation–lithiation processes, meaning that the porous Mo framework derived from Fe–Mo alloy simultaneously suppresses the growth of pure Fe particles. By adopting a Li anode and a Li-ion ceramic electrolyte, the corrosion problem between the cathode and the solid electrolyte is overcome. With similar battery cost ($12 kWh –1 ), the theoretical energy density of Li–Mo–FeCl 2 battery surpasses that of a Na–FeCl 2 ZEBRA battery over 25%, to 576 Wh kg –1 and 2216 Wh L –1 , respectively. Experimental results further prove this cell has excellent cycling performance (472 mAh g LiCl –1 after 300 cycles, 50 mg active material) and strong tolerance against the overcharge–overdischarge (3–1.6 V) and freezing–thawing (25–250 °C) incidents.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Superior long-term cycling of high-voltage lithium-ion batteries enabled by single-solvent electrolyte

A new single-solvent electrolyte system comprising lithium bis(fluorosuflonyl) imide (LiFSI) and beta-fluorinated sulfone (TFPMS) was designed to enable very stable long-term cycling of high-voltage lithium-ion batteries. Compared to other fluorinated solvents such as alpha-fluorinated sulfone (FMES) and fluorinated carbonate (FEMC), which are prone to reduction on the graphite anode, the LiFSI-TFPMS system displayed outstanding compatibility with graphite. While regular carbonate and sulfone from the LiFSI electrolyte system are compatible with the graphite anode, their high solvating power not only induces severe corrosion on the aluminum cathode current collector at high voltage, but also renders a low aggregation level at a normal salt concentration (about 1.0 M), resulting in the formation of an unstable solid-electrolyte interphase (SEI) on the graphite anode. Owing to the low solvating power of TFPMS, the aggregation level of the LiFSI-TFPMS system is relatively high even at normal salt concentration, which not only facilitates the formation of a robust SEI by the sacrificial decomposition of LiFSI, but also suppresses the aluminum corrosion of the LiFSI electrolyte system at high voltage. Together with the high intrinsic anodic stability of TFPMS, the superior cycling performance of graphite parallel to LiNi 0.6 Co 0.2 Mn 0.2 O 2 cells was achieved by employing the non-flammable LiFSI-TFPMS single-solvent electrolyte system.

25 ENERGY STORAGE↗

DOE OSTI2020

Revealing the growth kinetics of atmospheric corrosion pitting in aluminum via in situ microtomography

Abstract Understanding the mechanistic relationship between the environment, microstructure, and local kinetics of atmospheric corrosion damage remains a central challenge. To address this challenge, this study used laboratory-based X-ray tomography to directly observe attack in-operando over an extended period, enabling insights into the evolving growth kinetics and morphology of individual pits over months of exposure. Damage progression associated with nine pits in a 99.9% pure aluminum wire exposed to chloride salts in humid air was characterized. Most pits grew at a nominally linear rate up until pit death, which occurred within 12–24 h of nucleation. Exceptions to this were observed, with three pits exhibiting bimodal growth kinetics and growing for 40 or more hours. This was explained by secondary droplets that formed near the pits, increasing the cathode area. A corrosion-driven drying mechanism likely contributed to pit death in both cases. Pits first grew into the material followed by lateral expansion.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Mitigating CO 2 Corrosion of Natural Gas Steel Pipelines by Thermal Spray Aluminum Coatings

We report internal pipeline corrosion due to carbon dioxide (CO 2 ) is a major challenge facing the oil and gas industry. The objective of this study was to investigate the corrosion behavior of aluminum (Al)-based alloys as sacrificial coatings to protect pipelines in a CO 2 -saturated aqueous electrolyte (3.5 wt% NaCl) at 4 bar CO 2 partial pressure (3 bar) and 40°C. The corrosion resistance of Al-based alloys and thermal spray coatings was evaluated in an electrochemical reaction autoclave using electrochemical methods (potentiodynamic polarization, linear polarization resistance, and electrochemical impedance spectroscopy). Post-corrosion surface characterization was performed by scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy. The obtained data show Al-based alloys demonstrated promising protection against CO 2 corrosion with no breakaway degradation issues.

36 MATERIALS SCIENCE↗

NASA NTRS1982

Mathematical and physical modelling of materials processing

Mathematical and physical modeling of turbulence phenomena in metals processing, electromagnetically driven flows in materials processing, gas-solid reactions, rapid solidification processes, the electroslag casting process, the role of cathodic depolarizers in the corrosion of aluminum in sea water, and predicting viscoelastic flows are described.

Source record↗

NASA NTRS1985

Measuring Hydrogen Concentrations in Metals

Commercial corrosion-measurement system adapted to electrochemical determination of hydrogen concentrations in metals. New technique based on diffusion of hydrogen through foil specimen of metal. In sample holder, hydrogen produced on one side of foil, either by corrosion reaction or by cathodic current. Hydrogen diffused through foil removed on other side by constant anode potential, which leads to oxidation of hydrogen to water. Anode current is measure of concentration of hydrogen diffusing through foil. System used to study hydrogen uptake, hydrogen elimination by baking, effect of heat treatment, and effect of electroplating on high-strength steels.

Danford, M. D.↗

NASA NTRS2018

Iodine Hall-Effect Electric Propulsion System Research, Development, and System Durability Demonstration

This paper reviews recent iodine electric propulsion research and development activities at the NASA Glenn Research Center (GRC). Activities included (i) investigation of the iodine compatibility of BaO-CaO-Al2O3 impregnated tungsten hollow cathodes based on a flight heritage design, (ii) investigation of the iodine compatibility of a handful of materials common to propulsion systems, spacecraft, and ground test facilities, (iii) development of reliable iodine feed system technologies, (iv) implementation of test facility improvements in an attempt to mitigate iodine associated negative impacts, and culminated in (v) an 1,174-hour hybrid iodine-xenon propulsion system durability demonstration (iodine fed Hall-effect thruster with xenon fed cathode). Each of the activities resulted in extensive insights that shall inform future iodine electric propulsion developments. While reliable operation of a BaO-CaO-Al2O3 impregnated tungsten hollow cathode on iodine vapor was not achieved, long-term operation on xenon gas in proximity to an iodine fed thruster was demonstrated without any measurable degradation or cross-contamination of the cathode. Furthermore, iodine material corrosion investigations conducted at 300degC over 5, 15, and 30 days showed significant deterioration of all materials evaluated, although the same materials with a silicon coating proved nearly impervious to iodine so long as the coating was not mechanically damaged. Finally, the 1,174-hour durability test demonstration showed that (i) iodine feed system technologies developed at GRC delivered well-regulated uninterrupted propellant, (ii) implementation of appropriate facility improvements and procedures can limit negative impacts of iodine on test hardware and ground support equipment, although facility challenges with iodine are extensive, and (iii) a Hall-effect thruster operates with similar performance whether employing iodine or xenon propellant over long durations. The work was motivated by strong government and commercial interest in the growing capabilities of small-spacecraft (<500 kg), in combination with interest for denser low-power, high delta-v in-space propulsion systems. This work adds to a growing body of research and development efforts aimed at addressing the many anticipated challenges of implementing iodine as an in-space propellant. This work was conducted under the Advanced In-Space Propulsion (AISP) project funded through the Game Changing Development (GCD) program within NASA's Science Technology Mission Directorate (STMD).

Benavides, Gabriel F.↗

NASA NTRS2018

Iodine Hall-Effect Electric Propulsion System Research, Development, and System Durability Demonstration

This paper reviews recent iodine electric propulsion research and development activities at the NASA Glenn Research Center (GRC). Activities included (i) investigation of the iodine compatibility of BaO-CaO-Al2O3 impregnated tungsten hollow cathodes based on a flight heritage design, (ii) investigation of the iodine compatibility of a handful of materials common to propulsion systems, spacecraft, and ground test facilities, (iii) development of reliable iodine feed system technologies, (iv) implementation of test facility improvements in an attempt to mitigate iodine associated negative impacts, and culminated in (v) an 1,174-hour hybrid iodine-xenon propulsion system durability demonstration (iodine fed Hall-effect thruster with xenon fed cathode). Each of the activities resulted in extensive insights that shall inform future iodine electric propulsion developments. While reliable operation of a BaO-CaO-Al2O3 impregnated tungsten hollow cathode on iodine vapor was not achieved, long-term operation on xenon gas in proximity to an iodine fed thruster was demonstrated without any measurable degradation or cross-contamination of the cathode. Furthermore, iodine material corrosion investigations conducted at 300 C over 5, 15, and 30 days showed significant deterioration of all materials evaluated, although the same materials with a silicon coating proved nearly impervious to iodine so long as the coating was not mechanically damaged. Finally, the 1,174-hour durability test demonstration showed that (i) iodine feed system technologies developed at GRC delivered well-regulated uninterrupted propellant, (ii) implementation of appropriate facility improvements and procedures can limit negative impacts of iodine on test hardware and ground support equipment, although facility challenges with iodine are extensive, and (iii) a Hall-effect thruster operates with similar performance whether employing iodine or xenon propellant over long durations. The work was motivated by strong government and commercial interest in the growing capabilities of small-spacecraft (<500 kg), in combination with interest for denser low-power, high delta-v in-space propulsion systems. This work adds to a growing body of research and development efforts aimed at addressing the many anticipated challenges of implementing iodine as an in-space propellant. This work was conducted under the Advanced In-Space Propulsion (AISP) project funded through the Game Changing Development (GCD) program within NASA's Science Technology Mission Directorate (STMD).

Benavides, Gabriel F.↗

NASA NTRS2018

Iodine Hall-Effect Electric Propulsion System Research, Development, and System Durability Demonstration

This paper reviews recent iodine electric propulsion research and development activities at the NASA Glenn Research Center (GRC). Activities included (i) investigation of the iodine compatibility of BaO-CaO-Al2O3 impregnated tungsten hollow cathodes based on a flight heritage design, (ii) investigation of the iodine compatibility of a handful of materials common to propulsion systems, spacecraft, and ground test facilities, (iii) development of reliable iodine feed system technologies, (iv) implementation of test facility improvements in an attempt to mitigate iodine associated negative impacts, and culminated in (v) an 1,174-hour hybrid iodine-xenon propulsion system durability demonstration (iodine fed Hall-effect thruster with xenon fed cathode). Each of the activities resulted in extensive insights that shall informfuture iodine electric propulsion developments. While reliable operation of a BaO-CaO-Al2O3 impregnated tungsten hollow cathode on iodine vapor was not achieved, long-term operation on xenon gas in proximity to an iodine fed thruster was demonstrated without any measurable degradation or cross-contamination of the cathode. Furthermore, iodine material corrosion investigations conducted at 300 degrees C over 5, 15, and 30 days showed significant deterioration of all materials evaluated, although the same materials with a silicon coating proved nearly impervious to iodine so long as the coating was not mechanically damaged. Finally, the 1,174-hour durability test demonstration showed that (i) iodine feed system technologies developed at GRC delivered well-regulated uninterrupted propellant, (ii) implementation of appropriate facility improvements and procedures can limit negative impacts of iodine on test hardware and ground support equipment, although facility challenges with iodine are extensive, and (iii) a Hall-effect thruster operates with similar performance whether employing iodine or xenon propellant over long durations. The work was motivated by strong government and commercial interest in the growing capabilities of small-spacecraft (<500 kg), in combination with interest for denser low-power, high delta-v in-space propulsion systems. This work adds to a growing body of research and development efforts aimed at addressing the many anticipated challenges of implementing iodine as an in-space propellant. This work was conducted under the Advanced In-Space Propulsion (AISP) project funded through the Game Changing Development (GCD) program within NASA's Science Technology Mission Directorate (STMD).

Benavides, Gabriel F.↗

NASA NTRS1998

Cathodic Protection Deployment on Space Shuttle Solid Rocket Boosters

Corrosion protection of the space shuttle solid rocket boosters incorporates the use of cathodic protection(anodes) in concert with several coatings systems. The SRB design has large carbon/carbon composites(motor nozzle) electrically connected to an aluminum alloy structure. Early in the STS program, the aluminum structures incurred tremendous corrosive attack due primarily to the galvanic couple to the carbon/carbon nozzle at coating damage locations. Also contributing to the galvanic corrosion problem were stainless steel and titanium alloy components housed within the aluminum structures and electrically connected to the aluminum structures. This paper will highlight the evolution in the protection of the aluminum structures, providing historical information and summary data from the operation of the corrosion protection systems. Also, data and information will be included regarding the evaluation and deployment of inorganic zinc rich primers as anode area on the aluminum structures.

Zook, Lee M.↗

DOE OSTI2020

Corrosion of AISI 310 and 316 in Molten Hydroxide Under Steam Electrolysis Conditions

Steam electrolyzers, utilizing molten hydroxide electrolyte, offers potential for improvement in electrochemical efficiency, cost reduction, use of conventional materials of construction and process scale up for large scale hydrogen production. Stainless steels, used for the fabrication of cell components (current collector, gas separator, wet seals, and manifolds) experience accelerated corrosion in the presence of molten hydroxide electrolyte in both oxidizing (anodic) and reducing (cathodic) atmospheres. In this study, the corrosion behavior of AISI 310 and 316 in hydroxide melt has been studied at 600°C for 50 h. Melt immersion tests revealed formation of the porous lithium iron oxide at the melt-oxide interface for both AISI 310 and 316. Inductively coupled plasma optical emission spectrometry (ICP-OES) analysis showed the presence of Cr in the electrolyte melt obtained from samples exposed to oxidizing atmosphere. Thermochemical analysis was performed to validate the experimental results.

corrosion↗

DOE OSTI2024

A Green, Fire–Retarding Ether Solvent for Sustainable High–Voltage Li–Ion Batteries at Standard Salt Concentration

Lithium-ion batteries (LIBs) are increasingly encouraged to enhance their environmental friendliness and safety while maintaining optimal energy density and cost-effectiveness. Although various electrolytes using greener and safer glyme solvents have been reported, the low charge voltage (usually lower than 4.0 V vs Li/Li + ) restricts the energy density of LIBs. Herein, tetraglyme, a less-toxic, non-volatile, and non-flammable ether solvent, is exploited to build safer and greener LIBs. It is demonstrated that ether electrolytes, at a standard salt concentration (1 m), can be reversibly cycled to 4.5 V vs Li/Li + . Anchored with Boron-rich cathode-electrolyte interphase (CEI) and mitigated current collector corrosion, the LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) cathode delivers competitive cyclability versus commercial carbonate electrolytes when charged to 4.5 V. Synchrotron spectroscopic and imaging analyses show that the tetraglyme electrolyte can sufficiently suppress the overcharge behavior associated with the high-voltage electrolyte decomposition, which is advantageous over previously reported glyme electrolytes. The new electrolyte also enables minimal transition metal dissolution and deposition. NMC811||hard carbon full cell delivers excellent cycling stability at C/3 with a high average Coulombic efficiency of 99.77%. In conclusion, this work reports an oxidation-resilient tetraglyme electrolyte with record-high 4.5 V stability and enlightens further applications of glyme solvents for sustainable LIBs by designing Boron-rich interphases.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Correlating the Morphological Changes to Electrochemical Performance During Carbon Corrosion in Polymer Electrolyte Fuel Cells

A mechanistic understanding of carbon corrosion in polymer electrolyte fuel cells (PEFCs) is required to design durable catalyst layers. Uncontrolled startup and shutdown of PEFCs cause electrochemical oxidation of carbon, which leads to several degradation phenomena, such as loss in electrochemical surface area (ECSA), pore structure collapse or increase in mass transport resistance. In this study, the chronology of morphological changes in the cathode catalyst layer due to carbon corrosion was identified and correlated with electrochemical performance degradation. PEFCs were subjected to the Department of Energy carbon corrosion accelerated stress test (AST) protocol. The study revealed two phases: in the initial phase (~500 AST cycles), amorphous carbon in contact with Pt nanoparticles oxidized fast. Rapid carbon loss and catalyst layer thinning occurred, but pore structure did not change significantly. Pt nanoparticles detached from the support and ECSA decreased drastically. In the second phase (~1500 AST cycles), carbon corrosion slowed down, but severe pore structure collapse was observed. Porosity and pore connectivity within the cathode catalyst layer decreased considerably. Electrochemical diagnostics corroborated this finding by showing significantly higher O2 mass transport resistance. Lastly, no significant change was observed in the concentration of oxides on the carbon surface after AST. But overall water management in the cathode catalyst layer deteriorated as the pore structure collapsed. This study provides an in-depth understanding of morphological changes during PEFC carbon corrosion AST protocol and motivates novel material design strategies to enable durable PEFCs.

catalyst layers↗

NASA NTRS1985

Develop and test fuel cell powered on-site integrated total energy systems: Phase 3, full-scale power plant development

A 25 cell stack of the 13 inch x 23 inch cell size (about 4kW) remains on test after 6000 hours, using simulated reformate fuel. A similar stack was previously shut down after 7000 hours on load. These tests were carried out for the purpose of assessing the durability of fuel cell stack components developed through the end of 1983. In light of the favorable results obtained, a 25kW stack that will contain 175 cells of the same size is being constructed using the same technology base. The components for the 25kW stack have been completed. A methanol steam reformer with a design output equivalent to 50kW has been constructed to serve as a hydrogen generator for the 25kW stack. This reformer and the balance of the fuel processing sub system are currently being tested and debugged. The stack technology development program focused on cost reduction in bipolar plates, nonmetallic cooling plates, and current collecting plates; more stable cathode catalyst support materials; more corrosion resistant metal hardware; and shutdown/start up tolerance.

Kaufman, A.↗