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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
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↗
NASA NTRS1993

Evaluation of inorganic zinc-rich primers using Electrochemical Impedance Spectroscopy (EIS)

This investigation explores the use of Electrochemical Impedance Spectroscopy (EIS) in combination with beach exposure as a short term method for analyzing the performance of twenty-one zinc-rich primers. The twenty-one zinc-rich primers were: Carboline CZ-11, Ameron Devoe-Marine Catha-Coat 304, Briner V-65, Ameron D-21-9, Sherwin Williams Zinc Clad II, Carboline CZ-D7, Ameron D-4, Dupont Ganicin 347WB, Porter TQ-4374H, Inorganic Coatings IC-531, Subox Galvanox IV, Southern Coatings Chemtec 600, Glidden Glidzinc 5530, Byco SP-101, Tnemec 90E-75, Devoe Catha-Coat 302H, Glidden Glidzinc 5536, Koppers 701, Ameron D-21-5, Coronado 935-152, and Subox Galvanoz V. Data were also collected on galvanized steel for comparison purposes. A library of Bode magnitude plots was generated for each coating including curves for the initial time and after each week of atmospheric exposure as Beach Corrosion Test Site near the Space Shuttle launch pad at the Kennedy Space Center for up to three weeks. An examination of the variation of the Bode magnitude plots with atmospheric exposure revealed no clearly identifiable trend at this point that could distinguish between the good and the poor coatings. The test will be continued by including EIS measurements after six months and one year of atmospheric exposure.

Calle, Luz M.↗
DOE OSTI2025

Mitigating Electrochemical Impedance Spectroscopy Artifacts in PEMWE Reference Electrode Measurements

This study investigates strategies to improve the quality of electrochemical impedance spectroscopy (EIS) measurements using reference electrodes (RE) in proton exchange membrane water electrolyzers (PEMWE). We demonstrate that adding a low impedance wire in parallel to the RE significantly enhances signal accuracy, especially at high frequencies. Additionally, we identify electrical pad heaters as a source of measurement noise. EIS measurements fulfilling Kramers–Kronig validity criteria were only achieved in their absence. These insights advance the diagnostic capabilities of REs in water electrolyzers and support more reliable, spatially resolved analysis of electrochemical losses within the cell.

08 HYDROGEN↗
NASA NTRS1990

Electrochemical impedance spectroscopy of metal alloys in the space transportation system launch environment

AC impedance measurements were performed to investigate the corrosion resistance of 18 alloys under conditions similar to the Space Transportation System (STS) launch environment. The alloys were: (1) zirconium 702; (2) Hastelloy C-22, C-276, C-4, and B-2; (3) Inconel 600 and 825; (4) Ferralium 255; (5) Inco Alloy G-3; (6) 20Cb-3; (7) SS 904L, 304LN, 316L, 317L, and 304L; (8) ES 2205; and (9) Monel 400. AC impedance data were gathered for each alloy at various immersion times in 3.55 percent NaCl-0.1N HCl. Polarization resistance values were obtained for the Nyguist plots at each immersion time using the EQUIVALENT CIRCUIT software package available with the 388 electrochemical impedance software. Hastelloy C-22 showed the highest overall values for polarization resistance while Monel 400 and Inconel 600 had the lowest overall values. There was good general correlation between the corrosion performance of the alloys at the beach corrosion testing site, and the expected rate of corrosion as predicted based on the polarization resistance values obtained. The data indicate that electrochemical impedance spectroscopy can be used to predict the corrosion performance of metal alloys.

Calle, Luz↗
NASA NTRS1994

Evaluation of inorganic zinc-rich primers using Electrochemical Impedance Spectroscopy (EIS) in combination with atmospheric exposure

This investigation explored the use of Electrochemical Impedance Spectroscopy (EIS) in combination with atmospheric exposure as a short term method for analyzing the performance of twenty-one commercially available zinc-rich primers. The twenty-one zinc-rich primers were: Carboline CZ-11, Ameron Devoe-Marine Catha-Coat 304, Briner V-65, Ameron D-21-9, Sherwin Williams Zinc Clad II, Carboline CZ-D7, Ameron D-4, Dupont Ganicin 347WB, Porter TQ-4374H, Inorganic Coatings IC-531, Subox Galvanox IV, Southern Coatings Chemtec 600, GLidden Glidzinc 5530, Byco SP-101, Tnemec 90E-75, Devoe Catha-Coat 302H, Glidden Glidzinc 5536, Koppers 701, Ameron D-21-5, Coronado 935-152, and Subox Galvanox V. Data were also collected on galvanized steel for comparison purposes. A library of Bode magnitude plots was generated for each coating including curves for the initial time and after each week of atmospheric exposure at the Beach Corrosion Test site near the Space Shuttle launch pad at the Kennedy Space Center for up to four weeks. Subsequent measurements were collected after 8 weeks and after one year of atmospheric exposure. Analysis of the impedance data was performed with the purpose of identifying parameters that could be used to predict the long-term performance of zinc-rich primers. It has been shown that there is a correlation between the long-term performance of zinc-rich primers and several parameters obtained from EIS measurements in combination with atmospheric exposure. The equivalent circuit R2(R2C(R3W)) provided a satisfactory fit for the EIS data. The corrosion potential and the R2 resistance are parameters indicative of the galvanic mechanism of protection. The capacitance of the coating is related to the barrier mechanism of protection.

Calle, Luz M.↗
NASA NTRS1989

The application of electrochemical impedance spectroscopy for characterizing the degradation of Ni(OH)2/NiOOH electrodes

The use of wide-band electrochemical impedance spectroscopy is described for characterizing the degradation of porous Ni(OH)2/NiOOH electrodes in concentrated KOH electrolyte solutions. The impedance spectra are interpreted in terms of a finite electrical transmission line and the changes in the components of the electrical analog are followed as a function of cycle number. The degradation of the capacity of rolled and bonded Ni(OH)2/NiOOH electrodes is caused by rupture of ohmic contacts within the active mass and by restructuring which results in a decrease in the number of active pores.

Macdonald, Digby D.↗
DOE OSTI2022

Disentangling Memristive and Memcapacitive Effects in Droplet Interface Bilayers Using Dynamic Impedance Spectroscopy

The underlying principles for generating intelligent behavior in living organisms are fundamentally different from those in traditional solid-state circuits. Biomimetic neuromorphic equivalents based on biological membranes offer novel implementation of tunable plasticity and diverse mechanisms to control functionality. Here, dynamic electrochemical impedance spectroscopy (dEIS) to probe diphytanoylphosphatidylcholine (DPhPC) droplet interface bilayers (DIBs) to better understand the differences in molecular level structure/dynamics that give rise to hysteretic loops and neuromorphic, memelement behaviors in lipid bilayers in response to electrical biasing is used. Importantly, this system does not have ion-conducting channels and is, therefore, not expected to show memristive behavior. Surprisingly, both memristive and memcapacitive behaviors by measuring the time-dependent complex impedance of DPhPC DIBs are detected. Furthermore, it is shown that nonlinear memristance can originate from structural changes in the bilayer, affecting its dielectric properties. This novel dEIS application allows for the simultaneous analysis of the system's changing memristive and memcapacitive properties, which originate from different molecular restructuring processes. Moreover, and importantly, access to this type of information increases the number of neuromorphic processes supported simultaneously in a single two-terminal device.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Probing transport energies and defect states in organic semiconductors using energy resolved electrochemical impedance spectroscopy

Abstract Determining the relative energies of transport states in organic semiconductors is critical to understanding the properties of electronic devices and in designing device stacks. Futhermore, defect states are also highly important and can greatly impact material properties and device performance. Recently, energy‐resolved electrochemical impedance spectroscopy (ER‐EIS) is developed to probe both the ionization energy (IE) and electron affinity (EA) as well as sub‐bandgap defect states in organic semiconductors. Herein, ER‐EIS is compared to cyclic voltammetry (CV) and photoemission spectroscopies for extracting IE and EA values, and to photothermal deflection spectroscopy (PDS) for probing defect states in both polymer and molecular organic semiconductors. The results show that ER‐EIS determined IE and EA are in better agreement with photoemission spectroscopy measurements as compared to CV for both polymer and molecular materials. Furthermore, the defect states detected by ER‐EIS agree with sub‐bandgap features detected by PDS. Surprisingly, ER‐EIS measurements of regiorandom and regioregular poly(3‐hexylthiophene) (P3HT) show clear defect bands that occur at significantly different energies. In regioregular P3HT the defect band is near the edge of the occupied states while it is near the edge of the unoccupied states in regiorandom P3HT.

14 SOLAR ENERGY↗
DOE OSTI2020

Electrochemical Impedance Spectroscopy and Cyclic Voltammetry Methods for Monitoring SmCl 3 Concentration in Molten Eutectic LiCl-KCl

Molten salt solutions consisting of eutectic LiCl-KCl and concentrations of samarium chloride (0.5 to 3.0 wt%) at 500 C were analyzed using both cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The CV technique gave the average diffusion coefficient for Sm 3+ over the concentration range. Equipped with Sm 3+ diffusion coefficient, the Randles-Sevcik equation predicted Sm 3+ concentration values that agree with the given experimental values. From CV measurements; the anodic, cathodic, and half-peak potentials were identified and subsequently used as a parameter to acquire EIS spectra. A six-element Voigt model was used to model the EIS data in terms of resistance-time constant pairs. The lowest resistances were observed at the half-peak potential with the associated resistance-time constant pairs characterizing the reversible reaction between Sm 3+ and Sm 2+ . By extrapolation, the Voigt model estimated the polarization resistance and established a polarization resistance-concentration relationship.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2021

Detecting onset of lithium plating during fast charging of Li-ion batteries using operando electrochemical impedance spectroscopy

Electrochemical plating of Li metal on the graphite electrode is the key limitation behind slow charging times of Li-ion batteries (LIBs) in electric vehicles (EVs). Currently, electrochemical methods to detect the onset of Li plating while a battery is fast charging are sparse. In this study, we use operando electrochemical impedance spectroscopy to reliably detect the onset of Li plating on graphite electrodes in three-electrode LIBs. An increase in the graphite solid-electrolyte interface (SEI) resistance indicates that Li plating has occurred. By cross-validating with a highly sensitive ex situ chemical titration, we determine that this technique can detect very small amounts of plated Li (<0.6% of the graphite electrode's capacity). We also offer physical explanations for the observed impedance behavior. Finally, we show that this technique can be applied to standard two-electrode LIB systems, making the method an important step toward safely implementing fast charging protocols for LIBs in EVs.

25 ENERGY STORAGE↗
NASA NTRS2004

Corrosion Behavior of Stainless Steels in Neutral and Acidified Sodium Chloride Solutions by Electrochemical Impedance Spectroscopy

The objective of this work was to evaluate the corrosion performance of three alloys by Electrochemical Impedance Spectroscopy (EIS) and to compare the results with those obtained during a two-year atmospheric exposure study.' Three alloys: AL6XN (UNS N08367), 254SM0 (UNS S32154), and 304L (UNS S30403) were included in the study. 304L was included as a control. The alloys were tested in three electrolyte solutions which consisted of neutral 3.55% NaC1, 3.55% NaC1 in 0.lN HC1, and 3.55% NaC1 in 1.ON HC1. These conditions were expected to be less severe, similar, and more severe respectively than the conditions at NASA's Kennedy Space Center launch pads.

Calle, L. M.↗
DOE OSTI2025

HunStat2 – a simple and low-cost potentiostat with electrochemical impedance spectroscopy capability

We have developed a low-cost (30 USD), simple do-it-yourself (DIY) potentiostat with cyclic voltammetry (CV), open circuit potential (OCP) and electrochemical impedance spectroscopy (EIS) capability. The HunStat2 potentiostat is based on Analog Devices' AD5941 Analog Front End chip, which significantly simplifies the construction of potentiostats for both direct and alternating current (DC and AC, respectively) techniques. Interested readers are provided with circuit diagrams and a bill of materials to build the potentiostat on their own. In addition, control software is also provided free of charge. The software enables acquisition and visualization of data. In summary, HunStat2 introduces a simple and low-cost DIY potentiostat recommended for both analytical and educational purposes.

Vamos, Istvan [Lajos Petrik Vocational Chemistry S↗
DOE OSTI2021

Interpreting Ionic Conductivity for Polymer Electrolyte Fuel Cell Catalyst Layers with Electrochemical Impedance Spectroscopy and Transmission Line Modeling

A cathode catalyst layer containing optimally distributed ionomer is critical to reduce the platinum loading and increase its utilization in polymer electrolyte fuel cells. Here, electrochemical impedance spectroscopy (EIS) was used to measure effective ionic conductivity of pseudo catalyst layers (PCLs) at a relative humidity (RH) range of 50%-120%. These results are compared to previous work using the hydrogen pump (HP) method. EIS effective ionic conductivity results reported here are higher than those from the HP because in the HP set-up ionic pathways must be effectively connected through the PCL to be counted, whereas in the EIS measurement, ionomer segments that are in contact with the membrane but are not effectively connected all the way through the PCL can be detected. Double layer capacitances and effective ionic conductivities of Pt/C catalyst layers with various supports and ionomer to carbon (I/C) ratios were studied. High surface area carbon support resulted in a lower effective ionic conductivity compared to the graphitized carbon support due to worse ionomer dispersion. Effective ionic conductivities of Pt/C layers were compared to that of PCLs. On average, effective ionic conductivities of Pt/C layers were higher than PCLs because of possible carbon agglomeratio n within the PCLs.

25 ENERGY STORAGE↗
DOE OSTI2021

Exploring Transport Behavior in Hybrid Perovskites Solar Cells via Machine Learning Analysis of Environmental-Dependent Impedance Spectroscopy

Hybrid organic–inorganic perovskites are one of the promising candidates for the next-generation semiconductors due to their superlative optoelectronic properties. However, one of the limiting factors for potential applications is their chemical and structural instability in different environments. Herein, the stability of (FAPbI3)0.85(MAPbBr3)0.15 perovskite solar cell is explored in different atmospheres using impedance spectroscopy. An equivalent circuit model and distribution of relaxation times (DRTs) are used to effectively analyze impedance spectra. DRT is further analyzed via machine learning workflow based on the non-negative matrix factorization of reconstructed relaxation time spectra. This exploration provides the interplay of charge transport dynamics and recombination processes under environment stimuli and illumination. The results reveal that in the dark, oxygen atmosphere induces an increased hole concentration with less ionic character while ionic motion is dominant under ambient air. Under 1 Sun illumination, the environment-dependent impedance responses show a more striking effect compared with dark conditions. In this case, the increased transport resistance observed under oxygen atmosphere in equivalent circuit analysis arises due to interruption of photogenerated hole carriers. The results not only shed light on elucidating transport mechanisms of perovskite solar cells in different environments but also offer an effective interpretation of impedance responses.

36 MATERIALS SCIENCE↗
NASA NTRS2003

Corrosion Study Using Electrochemical Impedance Spectroscopy

Corrosion is a common phenomenon. It is the destructive result of chemical reaction between a metal or metal alloy and its environment. Stainless steel tubing is used at Kennedy Space Center for various supply lines which service the orbiter. The launch pads are also made of stainless steel. The environment at the launch site has very high chloride content due to the proximity to the Atlantic Ocean. Also, during a launch, the exhaust products in the solid rocket boosters include concentrated hydrogen chloride. The purpose of this project was to study various alloys by Electrochemical Impedance Spectroscopy in corrosive environments similar to the launch sites. This report includes data and analysis of the measurements for 304L, 254SMO and AL-6XN in primarily neutral 3.55% NaCl. One set of data for 304L in neutral 3.55%NaCl + 0.1N HCl is also included.

Farooq, Muhammad Umar↗
NASA NTRS2005

Electrochemical Impedance Spectroscopy of Alloys in a Simulated Space Shuttle Launch Environment

Corrosion studies began at NASA/Kennedy Space Center in 1966 during the Gemini/Apollo Programs with the evaluation of long-term protective coatings for the atmospheric protection of carbon steel. An outdoor exposure facility on the beach near the launch pad was established for this purpose at that time. The site has provided over 35 years of technical information on the evaluation of the long-term corrosion performance of many materials and coatings as well as on maintenance procedures. Results from these evaluations have helped NASA find new materials and processes that increase the safety and reliability of our flight hardware, launch structures, and ground support equipment. The launch environment at the Kennedy Space Center (KSC) is extremely corrosive due to the combination of ocean salt spray, heat, humidity, and sunlight. With the introduction of the Space Shuttle in 1981, the already highly corrosive conditions at the launch pad were rendered even more severe by the acidic exhaust from the solid rocket boosters. Over the years, many materials have been evaluated for their corrosion performance under conditions similar to those found at the launch pads. These studies have typically included atmospheric exposure and evaluation with conventional electrochemical methods such as open circuit potential (OCP) measurements, polarization techniques, and electrochemical impedance spectroscopy (EIS). The atmosphere at the Space Shuttle launch site is aggressive to most metals and causes severe pitting in many of the common stainless steel alloys such as type 304L stainless steel (304L SS). A study was undertaken to find a more corrosion resistant material to replace the existing 304L SS tubing. This paper presents the results from atmospheric exposure as well as electrochemical measurements on the corrosion resistance of AL-6XN (UNS N08367) and 254-SMO (UNS S32154). Type 304L SS (UNS S30403) was used as a control. Conditions at the Space Shuttle launch pad were simulated by using a hydrochloric acid (HC1) and alumina (Al203) slurry rinse for the atmospheric exposure and an electrolyte consisting of 3.55% sodium chloride (NaC1) with increased concentrations of hydrochloric acid (HC1) for the electrochemical measurements. The results from both types of measurements revealed the superior corrosion performance of the higher-alloyed materials. Unlike 304L SS, 254-SMO and AL-6XN exhibited a significantly improved resistance to corrosion as the concentration of hydrochloric acid in he 3.55% NaCl electrolyte solution was increased.

Calle, L. M.↗
NASA NTRS2004

Electrochemical Impedance Spectroscopy of Alloys in a Simulated Space Shuttle Launch Environment

Type 304L stainless steel (304L SS) tubing is currently used in various supply lines that service the Orbiter at NASA's John F. Kennedy Space Center Launch Pads in Florida (USA). The atmosphere at the Space Shuffle launch site is very corrosive due to a combination of factors, such as the proximity of the Atlantic Ocean and the concentrated hydrochloric acid produced by the fuel combustion reaction in the solid rocket boosters. The acidic chloride environment is aggressive to most metals and causes severe pitting in many of the common stainless steel alloys such as 304L SS. Stainless steel tubing is susceptible to pitting corrosion that can cause cracking and rupture of both high-pressure gas and fluid systems. Outages in the systems where failures occur can impact the normal operation of the shuttle and launch schedules. The use of a more corrosion resistant tubing alloy for launch pad applications would greatly reduce the probability of failure, improve safety, lessen maintenance costs, and reduce downtime. A study which included ten alloys was undertaken to find a more corrosion resistant material to replace the existing 304L SS tubing. The study included atmospheric exposure at NASA's John F. Kennedy Space Center outdoor corrosion test site near the launch pads and electrochemical measurements in the laboratory which included DC techniques and electrochemical impedance spectroscopy (EIS). This paper presents the results from EIS measurements on three of the alloys: AL6XN (UN N08367), 254SMO (UNS S32l54), and 304L SS (UNS S30403). Type 304L SS was included in the study as a control. The alloys were tested in three electrolyte solutions which consisted of neutral 3.55% NaC1, 3.55% NaCl in O.1N HC1, and 3.55% NaCl in 1.ON HC1. The solutions were chosen to simulate environments that were expected to be less, similar, and more aggressive, respectively, than those present at the Space Shuttle launch pads. The results from the EIS measurements were analyzed to evaluate the corrosion susceptibility of the alloys and to predict the long-term corrosion performance of the subject materials. The results from the EIS measurements for the three alloys indicated that the higher-alloyed 254SMO and AL6XN exhibited a significantly improved resistance to corrosion than the 304L SS as the concentration of hydrochloric acid in the 3.55% NaC1 solution was increased. The polarization resistance values obtained from the EIS measurements were consistent with those from linear polarization measurements, and were indicative of the actual long-term corrosion performance of the alloys during a two-year atmospheric exposure study.

Calle, L. M.↗
DOE OSTI2021

Instrument for spatially resolved, temperature-dependent electrochemical impedance spectroscopy of thin films under locally controlled atmosphere

We demonstrate an instrument for spatially resolved measurements (mapping) of electrochemical impedance under various temperatures and gas environments. Automated measurements are controlled by a custom LabVIEW program, which manages probe motion, sample motion, temperature ramps, and potentiostat functions. Sample and probe positioning is provided by stepper motors. Dry or hydrated atmospheres (air or nitrogen) are available. The configurable heater reaches temperatures up to 500 °C, although the temperature at the sample surface is moderated by the gas flow rate. The local gas environment is controlled by directing flow toward the sample via a glass enclosure that surrounds the gold wire probe. Software and hardware selection and design are discussed. Reproducibility and accuracy are quantified on a Ba(Zr,Y)O 3-δ proton-conducting electrolyte thin film synthesized by pulsed laser deposition. The mapping feature of the instrument is demonstrated on a compositionally graded array of electrocatalytically active Ba(Co,Fe,Zr,Y)O 3-δ thin film microelectrodes. The resulting data indicate that this method proficiently maps property trends in these materials, thus demonstrating the reliability and usefulness of this method for investigating electrochemically active thin films.

47 OTHER INSTRUMENTATION↗