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At least 307 records · Page 17
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Assessment of Readout Techniques for Passive Monitors

This fiscal year (FY) 2023 report on passive temperature sensors covers two main objectives: to demonstrate that the optical dilatometer can successfully process disc shaped silicon carbide (SiC) temperature monitors (TMs), and to demonstrate proof of concept for using the capacitance readout method to read printed melt wires. The SiC objective was successfully met by annealing and analyzing, via optical dilatometry, all eight 3-mm SiC discs provided by the Nuclear Science User Facilities (NSUF) Idaho State University (ISU) Nanostructured Steels for Enhanced Radiation Tolerance (N SERT) experiment, which was irradiated at Idaho National Laboratory (INL)’s Advanced Test Reactor (ATR). Per the ISU N SERT experiment, capsule 1 (KGT 3828 1 and KGT 3828-2) had a design temperature of 300°C +/- 50°C and an exposure of 2 dpa +/- 10%; capsule 2 (KGT 4600 and KGT 4609) had a design temperature of 300°C +/- 50°C and an exposure of 6 dpa +/- 10%; capsule 3 (KGT 4639 C and KGT 4639-D) had a design temperature of 500°C +/- 50°C and an exposure of 6 dpa +/- 10%; and capsule 4 (KGT 3841 3 and KGT 3841 4) had a design temperature of 500°C +/- 50°C and an exposure of 2 dpa +/- 10%. The target exposure rates, in dpa, are the neutron damage for various types of nanostructured steels. All but three SiC TMs (KGT 4600, KGT 4639 D, and KGT 3841 4) revealed averaged peak irradiation temperatures that fell within the design temperature ranges. The three SiC TMs that did not fall within the design temperatures ranges were at least 100°C below that target temperature. Furthermore, SiC TM KGT 3841 C revealed two irradiation regimes: one closer to the 300°C design temperature, and the other closer to the 500°C design temperature. Also, all the SiC TMs’ averaged peak irradiation temperatures came in anywhere between 20°C and 240°C below the irradiation temperatures predicted by the thermal models. This showed the optical dilatometry method to be a reliable and less time intensive process for determining averaged peak irradiation temperatures from passive SiC TMs such as rods and discs. Under the Advanced Sensors and Instrumentation (ASI) program in FY-23, Boise State University (BSU) proposed to demonstrate proof of concept for using a capacitance readout technique applicable to printed melt wires; however, they were stymied by the complexity of the capacitance readout method. In support of the BSU work, INL developed an additively manufactured (AM) ceramic package for encapsulating the new melt wires. Inks were synthesized at BSU that used new protocols rather than following previously established protocols implemented at INL, and testing of various temperatures was conducted at BSU to evaluate the melting behaviors of the printed melt wires. The result was that the capacitance readout technique showed promise but also created more challenges than originally anticipated. For example, the tin ink synthesized at BSU showed unusual melting behaviors that did nothing to enhance the performance of the final printed melt wire prototype in terms of the capacitance readout method. To make the proof of concept work when applied to the printed melt wires, the ASI program would need to invest further resources and time. Consequently, the program is not planning to continue this proof of concept work in FY-24, based on the progress and findings achieved in FY-23.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Additively Manufactured Strain Sensing for Nuclear Reactor Applications

Real-time monitoring of materials in harsh environments is a crucial technique towards reducing innovation time in nuclear systems. The successful measurement of real time, in-situ strain measurements during nuclear reactor operation requires innovative sensing solutions, including novel sensing strategies as well as advanced sensor design, manufacturing, and materials selection. In this paper, we will discuss two primary strategies for in-situ strain measurement strategies: additively manufactured (AM) capacitive strain gauges (CSGs) and digital image correlation (DIC). Current commercial strain gauges have limited applications in reactors due to the harsh operating conditions and non-trivial attachment strategies (i.e., welding, epoxy-adhesive) that can affect both the sensing performance and the underlying substrate under testing. AM CSGs are a viable solution as they have a low profile, low hysteresis, and wireless sensing integration capabilities that will enhance nuclear sensing technologies. In this work, the mechanical and thermal performance of the AM CSGs were tested up to 300 °C using ASTM standardized testing procedures to simulate the temperatures found in existing light water reactors. The AM CSGs had a similar performance across multiple samples which correlates to analytical models. This work leads towards the development of CSGs designed for higher temperatures and additional environmental factors found in Generation-IV reactors. Non-contact sensors, such as DIC, offer a less destructive way to measure deformation of materials when compared to alternative methods of in-situ strain determination, such as weldable strain gauges. However, DIC requires high contrast surfaces, which often relies on the implementation of artificial patterns. Using traditional splatter techniques to fabricate these patterns have limitations, including poor surface adhesion and reproducibility. In this work, AM fabrication techniques were implemented to avoid such limitations. Accordingly, aerosol jet printing (AJP) was used to print small scale periodic patterns of silver on stainless steel and aluminum tensile specimens. DIC was employed to monitor strain (up to 1100 µe) during temperature cycling from 23-600 °C. The results validated the use of AJP to better control pattern parameters for small fields of view applications at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Exceptional NH 3 Detection by Cu(cyhdc) MOF Sensor Due to H 2 O Coadsorption

Metal–organic framework (MOF)-based electrical impedance sensors are a growing class of sensors that show utility in the detection of environmentally toxic gases. Detection of trace NH 3 has been particularly difficult to design due to the low electrical response of NH 3 . However, this has been circumvented by judiciously selecting a MOF that has enhanced electrical response to NH 3 due to coadsorption with predominant atmospheric gases such as water. Herein, an MOF Cu(cyhdc) based sensor has been successfully demonstrated for the enhanced detection of environmentally toxic NH 3 gas. The sensor shows a change in impedance when it is exposed to 5 ppm of NH 3 . At 20 °C, >30% relative humidity (RH) is necessary to elicit a change, with the response increasing with RH and reaching 3170× at 92% RH, producing the largest published response to NH 3 for a MOF direct electrical sensor. In the absence of water, no change is observed toward 5 ppm of NH 3 over 20–50 °C. Here, this electrical response is largely driven by huge decreases in the imaginary component of the impedance, attributed to increased capacitance at the surface of the MOF crystallites upon NH 3 and H 2 O coadsorption. Complementary structural and microstructural characterization proves that the Cu(cyhdc) crystalline structure and morphology remain intact under trace NH 3 and/or H 2 O adsorption. Despite extremely low NH 3 , loadings seen in TGA, XPS, and FT-IR confirm NH 3 and H 2 O adsorption, and changes to the metal-carboxylate IR peak positions are observed upon NH 3 adsorption. Concentrated primarily at the outer surfaces of the MOF crystallites, this NH 3 and H 2 O coadsorption effectively increases the surface capacitance across the Cu(cyhdc) powder and enables direct electrical detection of trace NH 3 . Together, these results demonstrate how coadsorption of specific molecules (H 2 O) can be used to enable the electrical detection of trace toxic gases that would otherwise not have produced a MOF sensor response.

ammonia↗
DOE OSTI2018

Impedance Spectroscopy, Magnetic and Optical Analysis of Cadmium Tungstate Nanoparticles from Influence of Capping Agent Additives

Nano crystals of cadmium tungstate (CdWO{sub 4}) were obtained by facile precipitation route by using cadmium sulfate octahydrate and sodium tungstate dihydrate. These nanoparticles were then coated using different capping agents such as glucose, polyvinyl alcohol (PVA), and valine and their effects on the particle size, band gap, morphology, and magnetic character were investigated by powder X-ray diffraction, UV-Visible, FESEM, TEM, and VSM analysis. Capping agents are used in the synthesis of nanoparticles since they facilitate the growth and aggregation of particles in a precise manner, by usually acting as a physical barrier which controls the flow of free electron to the catalyst, so that they can be utilized by the catalyst and sensors of nanoparticle. Impedance spectroscopic technique was carried out, which was very useful in separating the grain boundary resistance and grain boundary capacitance contributions. We discuss the utilization of capping agents and their effects, including surface, optical and intergranular potential barriers in this work.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1984

Coupled orbiting inertial reference systems and Geopotential Research Mission (GRM) geodesy

Two spacecraft, one following the other with a separation of a few hundred kilometers and orbiting at an altitude of 160 km in a 90-degree polar orbit, are used to detect the minute variations in the earth's gravitational field. Housed in a capacitive cavity located at the centroid of the spacecraft is a free-floating metallic spherical proof-mass, which is the sensor controlling the thrusters that nullify all nongravitational forces on the spacecraft. The proof-mass in each spacecraft is the inertial-guidance reference for its host spacecraft, and the proof-masses are coupled together by a millimeter-wave link. This coupled system detects minute changes in the spacecraft's orbital positions and thus measures the anomalies present in the gravitational field of the earth. To derive a global geodetic model of the gravitational field with an amplitude resolution of 1 milligal and a spatial resolution of 100 km requires that the relative velocity between the proof-mass references be determined to within 1 micron/s.

Keating, T.↗
NASA NTRS2012

Capacitance Probe Resonator for Multichannel Electrometer

A multichannel electrometer voltmeter has been developed that employs a mechanical resonator with voltage-sensing capacitance-probe electrodes that enable high-impedance, high-voltage, radiation-hardened measurement of an Internal Electrostatic Discharge Monitor (IESDM) sensor. The IESDM is new sensor technology targeted for integration into a Space Environmental Monitor (SEM) subsystem used for the characterization and monitoring of deep dielectric charging on spacecraft. The resonator solution relies on a non-contact, voltage-sensing, sinusoidal-varying capacitor to achieve input impedances as high as 10 petaohms as determined by the resonator materials, geometries, cleanliness, and construction. The resonator is designed with one dominant mechanical degree of freedom, so it resonates as a simple harmonic oscillator and because of the linearity of the variable sense capacitor to displacement, generates a pure sinusoidal current signal for a fixed input voltage under measurement. This enables the use of an idealized phase-lock sensing scheme for optimal signal detection in the presence of noise.

Blaes, Brent R.↗
DOE OSTI2018

Synthesis of nitrogen and sulfur co-doped yolk-shell porous carbon microspheres and their application for Pb(II) detection in fish serum

Highlights: • N, S-YSPCMS was obtained via simple silica templating and pyrolysis method. • N, S-YSPCMS shows spherical morphology, porous structure and high N, S contents. • N, S-YSPCMS based electrochemical sensor shows good performance in Pb(II) analysis. • N, S-YSPCMS based sensor is feasible in detection of Pb(II) in fish serum. - Abstract: Nitrogen (N) and sulfur (S) co-doped carbonaceous material has shown remarkably improved performance in electrocatalysis, supercapacitor, and so on. While, the application of N, S co-doped carbon in electrochemical sensor was less investigated. Herein, N, S co-doped yolk-shell porous carbon microspheres (N, S-YSPCMSs) were synthesized by silica templating strategy and high-temperature pyrolysis method. The as-prepared N, S-YSPCMSs exhibited spherical morphologies, porous structures and high N, S-doping contents. Owing to the synergetic effect of the well-dispersed N, S-dopants, good conductivity of carbon skeleton, high surface area and pore volume of the microspheres, the N, S-YSPCMSs prepared at 900 °C showed good electrochemical performance for Pb(II) and with a linear range of 4–160 μg L{sup −1}, the limit of detection is 0.49 μg L{sup −1} (S/N = 3). The electrochemical sensor was consequently applied in detecting Pb(II) in fish serum samples with satisfying recoveries, indicating the N, S-YSPCMSs-900 are promising electrode components for electroanalysis.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Additively manufactured strain sensors for in-pile applications

Accurate, real-time monitoring of strain in fuel, cladding, and structural components of nuclear reactors is critical to better understand radiation induced phenomena during reactor tests and operations. The data provided is crucial to verify physics-based, multiscale modeling and simulation efforts, which aim to shorten the timeline for the development of new nuclear materials. Resistive strain gauges have limited performance during in-pile experiments due to the harsh operating conditions and limited physical space between fuel and cladding components. In this work, aerosol jet printing using silver nanoparticle inks was used to fabricate interdigitated electrode capacitive strain gauges on aluminum alloy 6061 tensile specimens. Here to simulate the temperatures of a traditional light water reactor, the capacitive strain gauges were tested with a mechanical test frame up to 300 °C and compared to commercially available bondable resistive strain gauges. The printed capacitive strain gauges exhibited a gauge factor of 1.0 and showed higher reproducibility and predictability of strain sensing performance than the resistive strain gauge. The results demonstrate the potential of aerosol jet printing to fabricate strain sensors with predictable performance and reduced invasiveness for high-temperature applications with confined spacing.

36 MATERIALS SCIENCE↗
DOE OSTI2025

M3AS-25IN1002073: Analysis of data from irradiation testing of printed strain gauges in prototypic nuclear environments

Advancement in additively manufactured strain gauges help address critical technology gaps to accurately monitor real-time materials behavior in reactor experiments. This is critical as it provides data to inform predictive models and simulations that enhance the development of reactors and fuel cycle systems. In this report, additively manufactured strain gauges are exposed to a neutron irradiation environment at the Ohio State University Research Reactor. This report goes over a 2-week campaign for neutron irradiating printed resistive strain gauges and capacitive strain gauges. These results complement the prior separate effects (i.e., mechanical strain, temperature, etc.) testing that were performed on these additive manufactured sensors and presented in prior milestone reports. These results also help progress our understanding of their usage in harsh environment applications. The outcome of developing advanced sensing and instrumentation capabilities plays an important role in increasing the safety, reliability, and energy efficiency of both next-generation and existing nuclear reactors.

36 - MATERIALS SCIENCE↗
NASA NTRS1989

A self diagnostic system for piezoelectric sensors

A technique for determining the mounting conditions of a piezoelectric accelerometer is presented. This technique electrically stimulates the piezoelectric element in the 'diagnostic' frequency band measuring the electrical frequency response characteristics across a capacitive load impedance. The diagnostic frequency band is tipically much higher than the operating bandwidth of the accelerometer. The resonant frequencies of the accelerometer are included in the diagnostic band. By monitoring the shift in these resonant frequencies, via electrical stimulation techniques, certain diagnostic conditions including mounting conditions can be determined. Experimental data from a compression mode accelerometer is used to demonstrate this technique.

Atherton, William J.↗
NASA NTRS1999

Silicon bulk micromachined, symmetric, degenerate vibratorygyroscope, accelerometer and sensor and method for using the same

When embodied in a microgyroscope, the invention is comprised of a silicon, four-leaf clover structure with a post attached to the center. The whole structure is suspended by four silicon cantilevers or springs. The device is electrostatically actuated and capacitively detects Coriolis induced motions of the leaves of the leaf clover structure. In the case where the post is not symmetric with the plane of the clover leaves, the device can is usable as an accelerometer. If the post is provided in the shape of a dumb bell or an asymmetric post, the center of gravity is moved out of the plane of clover leaf structure and a hybrid device is provided. When the clover leaf structure is used without a center mass, it performs as a high Q resonator usable as a sensor of any physical phenomena which can be coupled to the resonant performance.

Tang, Tony K.↗
DOE OSTI2019

Nonlinear size dependent analysis and effectiveness of nanocrystalline micro/nanogyroscopes

Vibratory micro/nanogyroscopes made of nanocrystalline silicon have a complex microstructure consisting of grains, voids, and interface material phases. Given that the length scale of such inertial sensors is close to the size of the grains themselves, classical continuum mechanics theories are no longer adequate to accurately model the dynamic behaviors of these sensors. In this work, the couple stress and surface elasticity are incorporated to the governing equations of an electrically-actuated, amplitude-based, capacitive sensing cantilever gyroscope to obtain a comprehensive model of the nano-system. Then, the impact of the size dependent effects on the nonlinear dynamic behavior of the gyroscope is investigated by studying its performance for gyroscopes ranging in size from the micro-to the nano-scale. The present numerical study shows that the additional stiffness contributions from the couple stress and surface elasticity and changes in scale cause significant changes in the frequency response, nonlinear behaviors, and sensitivity of the gyroscope to the rotation rates. Furthermore, this numerical analysis demonstrates the importance of accounting for size dependent effects for micro/nanogyroscopes in order to avoid any deterioration of the effectiveness of the gyroscope operability.

42 ENGINEERING↗
NASA NTRS2012

Amplitude-Stabilized Oscillator for a Capacitance-Probe Electrometer

A multichannel electrometer voltmeter that employs a mechanical resonator maintained in sustained amplitude-stabilized oscillation has been developed for the space-based measurement of an Internal Electrostatic Discharge Monitor (IESDM) sensor. The IESDM is new sensor technology targeted for integration into a Space Environmental Monitor (SEM) subsystem used for the characterization and monitoring of deep dielectric charging on spacecraft. Creating a stable oscillator from the mechanical resonator was achieved by employing magnetic induction for sensing the resonator s velocity, and forcing a current through a coil embedded in the resonator to produce a Lorentz actuation force that overcomes the resonator s dissipative losses. Control electronics employing an AGC loop provide conditions for stabilized, constant amplitude harmonic oscillation. The prototype resonator was composed of insulating FR4 printed-wireboard (PWB) material containing a flat, embedded, rectangular coil connected through flexure springs to a base PWB, and immersed in a magnetic field having two regions of opposite field direction generated by four neodymium block magnets. In addition to maintaining the mechanical movement needed for the electrometer s capacitor-probe transducer, this oscillator provides a reference signal for synchronous detection of the capacitor probe s output signal current so drift of oscillation frequency due to environmental effects is inconsequential.

Blaes, Brent R.↗
NASA NTRS2012

Self-Nulling Lock-in Detection Electronics for Capacitance Probe Electrometer

A multi-channel electrometer voltmeter that employs self-nulling lock-in detection electronics in conjunction with a mechanical resonator with noncontact voltage sensing electrodes has been developed for space-based measurement of an Internal Electrostatic Discharge Monitor (IESDM). The IESDM is new sensor technology targeted for integration into a Space Environmental Monitor (SEM) subsystem used for the characterization and monitoring of deep dielectric charging on spacecraft. Use of an AC-coupled lock-in amplifier with closed-loop sense-signal nulling via generation of an active guard-driving feedback voltage provides the resolution, accuracy, linearity and stability needed for long-term space-based measurement of the IESDM. This implementation relies on adjusting the feedback voltage to drive the sense current received from the resonator s variable-capacitance-probe voltage transducer to approximately zero, as limited by the signal-to-noise performance of the loop electronics. The magnitude of the sense current is proportional to the difference between the input voltage being measured and the feedback voltage, which matches the input voltage when the sense current is zero. High signal-to-noise-ratio (SNR) is achieved by synchronous detection of the sense signal using the correlated reference signal derived from the oscillator circuit that drives the mechanical resonator. The magnitude of the feedback voltage, while the loop is in a settled state with essentially zero sense current, is an accurate estimate of the input voltage being measured. This technique has many beneficial attributes including immunity to drift, high linearity, high SNR from synchronous detection of a single-frequency carrier selected to avoid potentially noisy 1/f low-frequency spectrum of the signal-chain electronics, and high accuracy provided through the benefits of a driven shield encasing the capacitance- probe transducer and guarded input triaxial lead-in. Measurements obtained from a 2- channel prototype electrometer have demonstrated good accuracy (|error| < 0.2 V) and high stability. Twenty-four-hour tests have been performed with virtually no drift. Additionally, 5,500 repeated one-second measurements of 100 V input were shown to be approximately normally distributed with a standard deviation of 140 mV.

Blaes, Brent R.↗
NASA NTRS2011

Circuit for Communication Over Power Lines

Many distributed systems share common sensors and instruments along with a common power line supplying current to the system. A communication technique and circuit has been developed that allows for the simple inclusion of an instrument, sensor, or actuator node within any system containing a common power bus. Wherever power is available, a node can be added, which can then draw power for itself, its associated sensors, and actuators from the power bus all while communicating with other nodes on the power bus. The technique modulates a DC power bus through capacitive coupling using on-off keying (OOK), and receives and demodulates the signal from the DC power bus through the same capacitive coupling. The circuit acts as serial modem for the physical power line communication. The circuit and technique can be made of commercially available components or included in an application specific integrated circuit (ASIC) design, which allows for the circuit to be included in current designs with additional circuitry or embedded into new designs. This device and technique moves computational, sensing, and actuation abilities closer to the source, and allows for the networking of multiple similar nodes to each other and to a central processor. This technique also allows for reconfigurable systems by adding or removing nodes at any time. It can do so using nothing more than the in situ power wiring of the system.

Krasowski, Michael J.↗
NASA NTRSDate not supplied

Electrostatic Regolith Interaction Experiment (ERIE) Electrometer Instrument Development

The Electrostatic Regolith Interaction Experiment (ERIE) is a joint venture between the University of Central Florida (UCF) Center for Microgravity Research (CMR) and the NASA Kennedy Space Center (KSC) Electrostatics and Surface Physics Laboratory (ESPL) seeking to examine charged dust grain behavior in a microgravity environment. Two separate systems have been combined for this suborbital flight experiment: the COLLisions Into Dust Experiment (COLLIDE) developed by the UCF CMR and the Wheel Electrostatic Spectrometer (WES) developed by the NASA KSC ESPL. This combination will advance the understanding of the natural and induced charged grain behavior on the Moon, asteroids, and other low gravity bodies comprised of charged dust particles. COLLIDE retains granular material under vacuum in a shallow tray behind a metal door, which then opens and releases the particles into a larger open volume when microgravity is achieved. The experiment is observed with a high-speed camera, such that the motions of these particles can then be tracked so the kinematics of each grain may be analyzed. The original application for this apparatus was to study cratering events into granular beds, but electrostatic repulsion was detected in the early frames of the video data returned from completed experiments, so a re-flight with a focus on these events was proposed. Agitation of the grains during launch combined with the frictional charge transfer between the grains and the door as it slides open provides an opportunity to use this setup to observe material tribocharging and charged particle behaviors in microgravity. In this updated version, the charged particles released into the chamber will traverse through an electric field produced by high voltage parallel plates and their resulting trajectories will be determined by their net charges. WES was originally developed to characterize the triboelectric properties of the Martian regolith through the contact of a rover wheel with the surface as it rotates. Improvements were made upon this legacy system to develop a sensor suite that will be installed within the COLLIDE door to measure charge transferred between the granular material and insulating disks protruding through the door. These insulator disks span the triboelectric series so, as they slide across the particulate matter when the door opens, each will accumulate a charge consistent with its relative position to the grains within the series. This charge on each insulator is distributed between two capacitances in series with an electrometer amplifier returning an analog voltage proportional to the charge accumulated. Calibration of this system has been performed using applications of known charge to the inputs and characterization of the frictional charge transfer between various regolith simulants and the sensor insulators is currently being examined in the lab.

Electrostatics↗
NASA NTRS2006

Carbon-Nanotube Schottky Diodes

Schottky diodes based on semiconducting single-walled carbon nanotubes are being developed as essential components of the next generation of submillimeter-wave sensors and sources. Initial performance predictions have shown that the performance characteristics of these devices can exceed those of the state-of-the-art solid-state Schottky diodes that have been the components of choice for room-temperature submillimeter-wave sensors for more than 50 years. For state-of-the-art Schottky diodes used as detectors at frequencies above a few hundred gigahertz, the inherent parasitic capacitances associated with their semiconductor junction areas and the resistances associated with low electron mobilities limit achievable sensitivity. The performance of such a detector falls off approximately exponentially with frequency above 500 GHz. Moreover, when used as frequency multipliers for generating signals, state-of-the-art solid-state Schottky diodes exhibit extremely low efficiencies, generally putting out only micro-watts of power at frequencies up to 1.5 THz. The shortcomings of the state-of-the-art solid-state Schottky diodes can be overcome by exploiting the unique electronic properties of semiconducting carbon nanotubes. A single-walled carbon nanotube can be metallic or semiconducting, depending on its chirality, and exhibits high electron mobility (recently reported to be approx.= 2x10(exp 5)sq cm/V-s) and low parasitic capacitance. Because of the narrowness of nanotubes, Schottky diodes based on carbon nanotubes have ultra-small junction areas (of the order of a few square nanometers) and consequent junction capacitances of the order of 10(exp -18) F, which translates to cutoff frequency >5 THz. Because the turn-on power levels of these devices are very low (of the order of nano-watts), the input power levels needed for pumping local oscillators containing these devices should be lower than those needed for local oscillators containing state-of-the-art solid-state Schottky diodes.

Manohara, Harish↗
DOE OSTI2019

Electroanalytical Investigation of the Electrode–Electrolyte Interface of Quaternary Ammonium Ionic Liquids: Impact of Alkyl Chain Length and Ether Functionality

The influence of ionic associations and potential-dependent interactions on the electrode–electrolyte interfacial structure of ionic liquids (ILs) is studied by electrochemical impedance spectroscopy (EIS) and surface-enhanced Raman spectroscopy (SERS) for a variety of asymmetric quaternary ammonium ILs. Specifically, the impact of cation alkyl chain length (C = 4, 8 and 16) and ether functionality on the interfacial structuring of ILs at the glassy carbon electrode surface is examined. Ammonium cations with alkyl chain length of 8 and 16 carbons are found to stabilize the formation of the bis(trifluorosulfonyl)imide, [TFSI], anion dense Stern layer at positive electrode potentials leading to larger capacitances. The longer alkyl chain of the cation is believed to screen the ion–ion repulsion among the anions by intruding into the interfacial anion layer. SERS suggests the presence of carbon-containing rings at the interface at both positive and negative electrode potentials, which can be explained by the buckling of the long alkyl chains. Inclusion of an ether functionality allowed for more symmetry in the camel-shaped potential-dependent differential capacitance curves, suggesting similar excess ion density at both positive and negative potentials. This work contributes to understanding and predicting the interfacial electrode capacitance in ILs by understanding the balance of ionic interactions and the associated repulsions at electrode–electrolyte interfaces that are pertinent to electrochemical energy storage, electrocatalysis, and electrochemical sensors.

25 ENERGY STORAGE↗