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1. Identifying thermal phase transitions of lignin–solvent mixtures using electrochemical impedance spectroscopy

   https://doi.org/10.1039/C5GC02342D  

   Klett, Adam S. ; Gamble, Jordan A. ; Thies, Mark C. ; Roberts, Mark E. ( January 2016 , Green Chemistry)

   Lignin is unique among renewable biopolymers in having significant aromatic character, making it potentially attractive for a wide range of uses from coatings to carbon fibers. Recent research has shown that hot acetic acid (AcOH)–water mixtures can be used to recover “ultraclean” lignins of controlled molecular weight from Kraft lignins. A key feature of this discovery is the existence of a region of liquid–liquid equilibrium (LLE), with one phase being rich in the purified lignin and the other rich in solvent. Although visual methods can be used to determine the temperature at which solid lignin melts in the presence of AcOH–water mixtures to form LLE, the phase transition can be seen only at lower AcOH concentrations due to solvent opacity. Thus, an electrochemical impedance spectroscopy (EIS) technique was developed for measuring the phase-transition temperature of a softwood Kraft lignin in AcOH–water mixtures. In electrochemical cells, the resistance to double-layer charging ( i.e. , polarization resistance R p ) is related to the concentration and mobility of free ions in the electrolyte, both of which are affected by the phases present. When the lignin–AcOH–water mixture was heated through the phase transition, R P was found to be a strong function of temperature, with the maximum in R P corresponding to the transition temperature obtained from visual observation. As the system is heated, acetate ions associate with the solid lignin, forming a liquefied, lignin-rich phase. This association increases the overall impedance of the system, as mobile acetate ions are stripped from the solvent phase and thus are no longer available to adsorb on the polarizing electrode surfaces. The maximum in R P occurs once the new lignin-rich phase has completely formed, and no further association of the lignin polymer with AcOH is possible. Except at sub-ambient temperatures, the phase-transition temperature was a strong function of solvent composition, increasing linearly from 18 °C at 70/30 AcOH/water to 97 °C at 10/90 wt% AcOH/water. 

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2. Comparison of Lithium Diffusion Coefficient Measurements in Tellurium Electrodes via Different Electrochemical Techniques

   https://doi.org/10.1149/1945-7111/acd43e  

   Wang, Jing ; Koenig, Jr, Gary M. ( May 2023 , Journal of The Electrochemical Society)

   Both thin (55μm) composite and thick (350μm) all active material battery porous electrodes were prepared for estimating the diffusion coefficient of Li⁺($D_{{\mathit{Li}}^{+}})$in tellurium (Te) during electrochemical lithiation. Galvanostatic intermittent titration technique (GITT), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) were applied to quantify the chemical lithium solid-state diffusion coefficient within the Te active material in the electrodes. Multiple methods of GITT and EIS were assessed. For the composite Te electrodes, the$D_{{\mathit{Li}}^{+}}$was on the order of 10⁻¹¹cm²s⁻¹from both CV and GITT methods, but 10⁻⁹cm²s⁻¹from EIS. For the thick tellurium electrodes, both GITT and EIS resulted in lithium diffusion coefficient estimates in the range of 10⁻¹¹–10⁻¹²cm²s⁻¹. The general trend across all methods that quantified the diffusion coefficient as a function of lithiation of tellurium was that the$D_{{\mathit{Li}}^{+}}$decreased rapidly when the Te material was initially lithiated. The$D_{{\mathit{Li}}^{+}}$at the phase transition voltage plateau (∼1.7 V, vs Li/Li⁺, where both Te and Li₂Te were expected) had the lowest$D_{{\mathit{Li}}^{+}},$while the$D_{{\mathit{Li}}^{+}}$both before and after the plateau was generally higher. Among all the electrochemical measurements of$D_{{\mathit{Li}}^{+}},$the modified GITT method with modelling the relaxation region resulted in relatively low scatter in the data, provided values as a function of lithiation, and was well suited to thick electrodes with a flat discharge plateau as was the case herein.

    

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3. Enhancement of Ni–(Y 2 O 3 ) 0.08 (ZrO 2 ) 0.92 fuel electrode performance by infiltration of Ce 0.8 Gd 0.2 O 2−δ nanoparticles

   https://doi.org/10.1039/c9ta12316d  

   Park, Beom-Kyeong ; Scipioni, Roberto ; Cox, Dalton ; Barnett, Scott A. ( February 2020 , Journal of Materials Chemistry A)

   This paper addresses the use of Ce 0.8 Gd 0.2 O 2−δ (GDC) infiltration into the Ni–(Y 2 O 3 ) 0.08 (ZrO 2 ) 0.92 (YSZ) fuel electrode of solid oxide cells (SOCs) for improving their electrochemical performance in fuel cell and electrolysis operation. Although doped ceria infiltration into Ni–YSZ has recently been shown to improve the electrode performance and stability, the mechanisms defining how GDC impacts electrochemical characteristics are not fully delineated. Furthermore, the electrochemical characteristics have not yet been determined over the full range of conditions normally encountered in fuel cell and electrolysis operation. Here we present a study of both symmetric and full cells aimed at understanding the electrochemical mechanisms of GDC-modified Ni–YSZ over a wide range of fuel compositions and temperatures. Single-step GDC infiltration at an appropriate loading substantially reduced the polarization resistance of Ni–YSZ electrodes in electrolyte-supported cells, as measured using electrochemical impedance spectroscopy (EIS) at various temperatures (600–800 °C) in a range of H 2 O–H 2 mixtures (3–90 vol% H 2 O). Fuel-electrode-supported cells had significant concentration polarization due to the thick Ni–YSZ supports. A distribution of relaxation times approach is used to develop a physically-based electrochemical model; the results show that GDC reduces the reaction resistance associated with three-phase boundaries, but also appears to improve oxygen transport in the electrode. Increasing the H 2 O fraction in the H 2 –H 2 O fuel mixture reduced both the three-phase boundary resistance and the gas diffusion resistance for Ni–YSZ; with GDC infiltration, the electrode resistance showed less variation with fuel composition. GDC infiltration improved the performance of fuel-electrode-supported full cells, which yielded a maximum power density of 2.28 W cm −2 in fuel cell mode and an electrolysis current density at 1.3 V of 2.22 A cm −2 , both at 800 °C. 

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4. Monitoring biofilm growth and dispersal in real-time with impedance biosensors

   https://doi.org/10.1093/jimb/kuad022  

   McGlennen, Matthew ; Dieser, Markus ; Foreman, Christine M. ; Warnat, Stephan ( August 2023 , Journal of Industrial Microbiology and Biotechnology)

   Microbial biofilm contamination is a widespread problem that requires precise and prompt detection techniques to effectively control its growth. Microfabricated electrochemical impedance spectroscopy (EIS) biosensors offer promise as a tool for early biofilm detection and monitoring of elimination. This study utilized a custom flow cell system with integrated sensors to make real-time impedance measurements of biofilm growth under flow conditions, which were correlated with confocal laser scanning microscopy (CLSM) imaging. Biofilm growth on EIS biosensors in basic aqueous growth media (tryptic soy broth, TSB) and an oil–water emulsion (metalworking fluid, MWF) attenuated in a sigmoidal decay pattern, which lead to an ∼22–25% decrease in impedance after 24 Hrs. Subsequent treatment of established biofilms increased the impedance by ∼14% and ∼41% in TSB and MWF, respectively. In the presence of furanone C-30, a quorum-sensing inhibitor (QSI), impedance remained unchanged from the initial time point for 18 Hrs in TSB and 72 Hrs in MWF. Biofilm changes enumerated from CLSM imaging corroborated impedance measurements, with treatment significantly reducing biofilm. Overall, these results support the application of microfabricated EIS biosensors for evaluating the growth and dispersal of biofilm in situ and demonstrate potential for use in industrial settings.

   This study demonstrates the use of microfabricated electrochemical impedance spectroscopy (EIS) biosensors for real-time monitoring and treatment evaluation of biofilm growth, offering valuable insights for biofilm control in industrial settings.

    

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5. Measurement of Polarization Resistance of LSM + YSZ Electrodes on YSZ using AC and DC Methods

   Alex Szendrei, Taylor D. ( January 2019 , Fuel cells)

   Most of the measurements of electrode polarization resistance are conducted using electrochemical impedance spectroscopy (EIS). The electrochemical devices, however, are typically used in a DC mode. The objective of the present work was to measure electrode polarization resistance using both EIS and DC techniques. A solid cylinder of 8YSZ of diameter ~1.17 cm and length ~5.00 cm was made by powder pressing followed by sintering. LSM + YSZ electrodes were applied on the two end surfaces of the cylinder upon which gold mesh was placed. Four Pt electrodes/probes were painted along the circumference. During DC measurements, DC voltage was applied across the end electrodes and potentials were measured at all four probes. The current was also measured. From these measurements electrode polarizations were estimated separately for the two electrodes as a function of current. EIS was conducted across the two end electrodes as well as across electrode-1 and probe-2, and across probe-2 and electrode-2. This allowed the determination of the polarization resistances of the two electrodes separately. Point by point additions of the electrode-1/probe-2 and probe-2/electrode-2 spectra matched the electrode-1/electrode-2 spectra. There was good agreement between the DC and the EIS measurements. 

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