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NASA NTRS2014

Enabling More than Moore: Accelerated Reliability Testing and Risk Analysis for Advanced Electronics Packaging

For five decades, the semiconductor industry has distinguished itself by the rapid pace of improvement in miniaturization of electronics products-Moore's Law. Now, scaling hits a brick wall, a paradigm shift. The industry roadmaps recognized the scaling limitation and project that packaging technologies will meet further miniaturization needs or ak.a "More than Moore". This paper presents packaging technology trends and accelerated reliability testing methods currently being practiced. Then, it presents industry status on key advanced electronic packages, factors affecting accelerated solder joint reliability of area array packages, and IPC/JEDEC/Mil specifications for characterizations of assemblies under accelerated thermal and mechanical loading. Finally, it presents an examples demonstrating how Accelerated Testing and Analysis have been effectively employed in the development of complex spacecraft thereby reducing risk. Quantitative assessments necessarily involve the mathematics of probability and statistics. In addition, accelerated tests need to be designed which consider the desired risk posture and schedule for particular project. Such assessments relieve risks without imposing additional costs. and constraints that are not value added for a particular mission. Furthermore, in the course of development of complex systems, variances and defects will inevitably present themselves and require a decision concerning their disposition, necessitating quantitative assessments. In summary, this paper presents a comprehensive view point, from technology to systems, including the benefits and impact of accelerated testing in offsetting risk.

Ghaffarian, Reza↗

DOE OSTI2013

Life-Cycle Assessment of Energy and Environmental Impacts of LED Lighting Products, Part 3: LED Environmental Testing

This report covers the third part of a larger U.S. Department of Energy (DOE) project to assess the life- cycle environmental and resource impacts associated with the manufacturing, transport, use, and disposal of light-emitting diode (LED) lighting products in relation to incumbent lighting technologies. All three reports are available on the DOE website (www.ssl.energy.gov/tech_reports.html). Part 1: Review of the Life-Cycle Energy Consumption of Incandescent, Compact Fluorescent and LED Lamps; Part 2: LED Manufacturing and Performance; Part 3: LED Environmental Testing. Parts 1 and 2 were published in February and June 2012, respectively. The Part 1 report included a summary of the life-cycle assessment (LCA) process and methodology, provided a literature review of more than 25 existing LCA studies of various lamp types, and performed a meta-analysis comparing LED lamps with incandescent and compact fluorescent lamps (CFLs). Drawing from the Part 1 findings, Part 2 performed a more detailed assessment of the LED manufacturing process and used these findings to provide a comparative LCA taking into consideration a wider range of environmental impacts. Both reports concluded that the life-cycle environmental impact of a given lamp is dominated by the energy used during lamp operation—the upstream generation of electricity drives the total environmental footprint of the product. However, a more detailed understanding of end-of-life disposal considerations for LED products has become increasingly important as their installation base has grown. The Part 3 study (reported herein) was undertaken to augment the LCA findings with chemical analysis of a variety of LED, CFL, and incandescent lamps using standard testing procedures. A total of 22 samples, representing 11 different models, were tested to determine whether any of 17 elements were present at levels exceeding California or Federal regulatory thresholds for hazardous waste. Notably, this type of testing does not provide an indication of product safety during use. Key findings include: • The selected models were generally found to be below thresholds for Federally regulated elements, although volatile mercury in the CFLs is presumed to have escaped detection; • Nearly all of the lamps (regardless of technology) exceeded at least one California threshold— typically for copper, zinc, antimony, or nickel; • The greatest contributors were the metal screw bases, drivers, ballasts, and wires or filaments— internal LED light sources generally did not cause LED lamps to exceed thresholds. This study was exploratory in nature and was not intended to provide a definitive indication of regulatory compliance for any specific lamp model or technology. Further study would be needed to more broadly characterize the various light source technologies; to more accurately and precisely characterize a specific model; or to determine whether product redesign would be appropriate. However, concentrations of regulated elements in LED lamps were found to be comparable to cell phones and other types of electronic devices, which like incandescent lamps and CFLs have also have been shown to exceed the stringent California thresholds for hazardous waste. Although LED lamps offer reduced life-cycle energy and environmental impacts when compared to CFLs and incandescent lamps, recycling will likely gain importance as consumer adoption of this emerging technology continues to increase.

bulb↗

DOE OSTI2024

Comprehensive evaluation of commercially scalable atomic-layer-deposited alumina coating impact on full cell battery performance across varied test conditions

Atomic Layer Deposition (ALD) has emerged as a strategic enhancement method for lithium-ion battery (LIB) materials offering potential benefits and durability benefits for industrial battery production. However, the translation from laboratory achievements to commercial-scale applications has been limited. Here, this study aims to bridge this gap by comprehensively evaluating the effects of commercially scalable Al 2 O 3 ALD coatings using full pouch cell performance as a means to assess the ALD impact. We utilized large-scale slot-die coating techniques to ensure consistent electrode quality and tested four configurations of pouch cells to analyze the individual effects of ALD coating on anode and cathode electroactive materials. Our extensive testing matrix included long-term cycling, fast discharge, fast charge, leakage current, and high voltage tests. While at lower C-rates (<~1C), the influence of Al 2 O 3 coatings on cell performance is not significant. Fast charging conditions reveal that the anode ALD coating significantly enhances performance via a passivating effect, while on the cathode, it is detrimental, potentially due to increased resistance of the thin interfacial layer formed during the ALD processing. Leakage current and high-voltage tests show that the application of ALD coatings on either anode or cathode effectively minimizes side reactions at the electrode-electrolyte interface. Additionally, ALD coatings significantly mitigate concentrated and localized lithium plating on the anodes. These insights provide a valuable understanding of the potential of ALD technologies in LIB manufacturing to tailor cell performance, paving the way for safer, more efficient, and cost-effective battery solutions.

25 ENERGY STORAGE↗

NASA NTRS2020

MODIS TEB Calibration Algorithm Improvements for Future L1B Collection

Terra and Aqua MODIS have provided continuous global observations for scientific applications for more than 20 and 18 years, respectively. The radiometric calibration of the MODIS thermal emissive bands (TEB) is based on a quadratic approximation of the instrument response. The calibration coefficients look-up tables (LUTs) are updated using the response of the MODIS on-board blackbody (BB)with the response background subtracted by space view. The quarterly on-board BB warm-up and cool-down activity temperature ranges from 270 K to 315 K, and the derived offset has a relatively large uncertainty. Electronic cross-talk, an artifact that affects both instrument calibration and Earth view (EV) radiance retrievals, is corrected based on lunar observations. Calibration assessments using EV observations (e.g. ocean, desert, Antarctic Dome Concordia, and deep convective clouds) provide useful information to evaluate the impact of the Terra safe mode (February 2016) and Aqua MODIS formatter reset (January 2018) events on both MODIS instruments. This study focuses on the TEB radiometric calibration algorithm improvements for future collections based on calibration assessments using EV measurements and analytical modeling. Measurement stability and consistency over specific Earth scenes with a wide temperature range, as well as their brightness temperature (BT) dependency, are used for bias estimations in the calibration coefficients. Calibration coefficients are derived and updated after adjusting the current fitting algorithm. Thereafter, using the test LUTs, their impact on the Level 1B (L1B) data for different EV scenes is analyzed.

MODIS↗

DOE OSTI2020

Preliminary Evaluation of Driver Fuel Plates and Reduced Sodium Temperature to Increase Fast Test Reactor Experimental Neutron Irradiation Capabilities

All sodium-cooled fast test reactors operated so far have used essentially the same fuel geometrical ar-rangement, namely cylindrical fuel pins assembled into a triangular array in hexagonal fuel assemblies. Fuel compositions and dimensions may vary but the overall geometrical pattern remains identical. Fur-thermore, most sodium-cooled reactors have operated, and still operate, with core-average inlet and outlet sodium temperatures of, respectively, 350-400°C and 500-550°C. The present preliminary study revisits the standard fuel assembly geometry as well as operating tempera-tures to evaluate potential impact on fast test reactor neutron irradiation capabilities. The reference fuel is U-20Pu-10Zr. Pin (reference) and plate geometries are considered together with two sets of core-average sodium inlet/outlet temperatures: 350/500°C (reference) and 200/400°C. More prototypic environments could be obtained inside ad-hoc irradiation testing vehicles that are independent from the reactor primary coolant. Everything else being the same, fuel temperature is significantly lower in plates than in pins. Therefore, plates could in principle accommodate higher plutonium content, thus, reducing the need for uranium enrichment or allowing the use of lower quality plutonium (U-xPu-10Zr thermal conductivity and solidus temperature decrease as x increases, hence, necessitating additional thermal margins). For the reference pin configuration, lowering the inlet/outlet sodium temperatures from the reference 350/500°C down to 200/400°C provides additional thermal margins that can be used to increase the peak fast flux from about 4.5 × 10 15 n/cm 2 -s to 6 ×10 15 n/cm 2 -s for the same core power of 300 MW. Assuming 300 Equivalent Fuel Power Days (EFPD) of operation per calendar year, a (steel) test article could accu-mulate up to 75 dpa/year. The use of fuel plates provides even more thermal margins which may allow the peak fast flux to reach values as high as 8 × 10 15 n/cm 2 -s for both sets of inlet/outlet temperatures. In this environment, a test article could accumulate up to 95 dpa/year assuming 300 EFPD/year, hence greatly accelerating irradiation testing. Allowing a fast test reactor to operate over a wide range of inlet/outlet temperatures could add significant flexibility to its neutron irradiation capabilities. Steel present in the driver fuel assemblies is not expected to accumulate more than 90 displacements per atom (dpa) over its lifetime. Hence, steel alloys that are not suited for very high dpa but can operate over a wide range of temperatures (from low to high) would be appropriate for this application. Finally, because pin and plate assemblies fit on the same grid plate, a fast test reactor could in principle start-up with standard fuel pin assemblies and, later on, move to a plate-type Mark-II fuel to further in-crease its neutron irradiation capabilities while potentially reducing the level of uranium enrichment needed.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2026

Analysis of attenuation data from the decommissioned ZIon unit 1 reactor pressure vessel beltline weld

In order to examine the attenuation of radiation damage through the thickness of an irradiated reactor pressure vessel (RPV), four segments were acquired from the Zion Unit 1 power plant RPV after the plant was decommissioned. The Zion Unit 1 RPV Beltline Weld Segment 1 was cut into seven blocks, consisting of five base metal and two beltline welds from the high fluence region of the segment. Through-wall test specimens were machined and tested. Specimens included those used for Charpy impact, Master Curve fracture toughness testing, and chemical analysis. The observed through-thickness ductile-to-brittle transition temperatures in the beltline weld deviated significantly from the expected behavior based on the attenuation of fast fluence as a function of depth into the RPV. Beginning at the inside surface, the 41-J Charpy transition temperature was either flat or slightly increasing until the ¾ -T location. The results of a simple, model-based analysis of the Zion beltline weld material that included the irradiation conditions and material chemistry were generally consistent with industry trend curves and the standard attenuation model, rather than the observed data. Although there was no archive material from the RPV available to permit measurement of the unirradiated properties, fracture toughness specimens fabricated from archive surveillance weld were used to obtain an estimate of the initial through-thickness values of the Charpy transition temperature. The Charpy shifts obtained using this approach were similarly in disagreement with the predictions of the US NRC Regulatory Guide 1.99, Rev. 2. However, testing of irradiated Charpy specimens taken from the RPV following post-irradiation annealing (10 hr. at 500 °C) provided a quite different estimate of the unirradiated properties which improved the agreement between the inferred through-thickness Charpy shifts and exponential attenuation model included in Regulatory Guide 1.99/2. In conclusion, the analysis of the Zion data and data obtained in previous post-mortem examinations of decommissioned RPVs indicates that more work is needed to understand the through-thickness properties of RPV materials in order to properly assess through-wall damage attenuation.

Charpy impact↗

NASA NTRS1995

Effects of through-the-thickness stitching on impact and interlaminar fracture properties of textile graphite/epoxy laminates

This study investigated the effects of through-the-thickness stitching on impact damage resistance, impact damage tolerance, and mode I and mode II fracture toughness of textile graphite/epoxy laminates. Uniweave resin-transfer-molded 48 ply graphite/epoxy (AS4/3501-6) laminates were stitched with Kevlar and glass yarns of different linear densities and stitch spacings. Delaminations were implanted during processing to simulate impact damage. Sublaminate buckling tests were performed to determine the effects of stitching on the compressive strength. The results showed outstanding improvements of up to 400 percent in the compression strength over the unstitched laminates. In impact and static indentation tests the onset of damage occurred at the same level, but the extent of damage was less in stitched laminates. Mode I fracture toughness of 24 ply Uniweave unidirectional (AS4/3501-6) stitched laminates was measured by conducting double-cantilever-beam tests. The critical strain energy release rate (G(sub Ic)) was found to be up to 30 times higher than the unstitched laminates. Mode II fracture toughness of the Uniweave laminates was measured by performing end-notched-flexure tests. Two new methods to compute the apparent G(sub IIc) are presented. The apparent G(sub IIc) was found to be at least 5-15 times higher for the stitched laminates.

Sharma, Suresh K.↗

NASA NTRS2005

Results of Aero/Acoustic Tests and Analytical Studies of a Two-Dimensional Eight-Lobe Mixer-Ejector Exhaust Nozzle at Takeoff Conditions

Hot flow aero-acoustic tests were conducted with Pratt & Whitney's High-Speed Civil Transport (HSCT) Mixer-Ejector Exhaust Nozzles by General Electric Aircraft Engines (GEAE) in the GEAE Anechoic Freejet Noise Facility (Cell 41) located in Evendale, Ohio. The tests evaluated the impact of various geometric and design parameters on the noise generated by a two-dimensional (2-D) shrouded, 8-lobed, mixer-ejector exhaust nozzle. The shrouded mixer-ejector provides noise suppression by mixing relatively low energy ambient air with the hot, high-speed primary exhaust jet. Additional attenuation was obtained by lining the shroud internal walls with acoustic panels, which absorb acoustic energy generated during the mixing process. Two mixer designs were investigated, the high mixing "vortical" and aligned flow "axial", along with variations in the shroud internal mixing area ratios and shroud length. The shrouds were tested as hardwall or lined with acoustic panels packed with a bulk absorber. A total of 21 model configurations at 1:11.47 scale were tested. The models were tested over a range of primary nozzle pressure ratios and primary exhaust temperatures representative of typical HSCT aero thermodynamic cycles. Static as well as flight simulated data were acquired during testing. A round convergent unshrouded nozzle was tested to provide an acoustic baseline for comparison to the test configurations. Comparisons were made to previous test results obtained with this hardware at NASA Glenn's 9- by 15-foot low-speed wind tunnel (LSWT). Laser velocimetry was used to investigate external as well as ejector internal velocity profiles for comparison to computational predictions. Ejector interior wall static pressure data were also obtained. A significant reduction in exhaust system noise was demonstrated with the 2-D shrouded nozzle designs.

Harrington, Douglas↗

DOE OSTI2010

Corrective Action Investigation Plan for Corrective Action Unit 365: Baneberry Contamination Area, Nevada National Security Site, Nevada, Revision 0

Corrective Action Unit 365 comprises one corrective action site (CAS), CAS 08-23-02, U-8d Contamination Area. This site is being investigated because existing information on the nature and extent of potential contamination is insufficient to evaluate and recommend corrective action alternatives (CAAs). Additional information will be obtained by conducting a corrective action investigation before evaluating CAAs and selecting the appropriate corrective action for the CAS. The results of the field investigation will support a defensible evaluation of viable CAAs that will be presented in the Corrective Action Decision Document. The site will be investigated based on the data quality objectives (DQOs) developed on July 6, 2010, by representatives of the Nevada Division of Environmental Protection and the U.S. Department of Energy (DOE), National Nuclear Security Administration Nevada Site Office. The DQO process was used to identify and define the type, amount, and quality of data needed to develop and evaluate appropriate corrective actions for the Baneberry site. The primary release associated with Corrective Action Unit 365 was radiological contamination from the Baneberry nuclear test. Baneberry was an underground weapons-related test that vented significant quantities of radioactive gases from a fissure located in close proximity to ground zero. A crater formed shortly after detonation, which stemmed part of the flow from the fissure. The scope of this investigation includes surface and shallow subsurface (less than 15 feet below ground surface) soils. Radionuclides from the Baneberry test with the potential to impact groundwater are included within the Underground Test Area Subproject. Investigations and corrective actions associated with the Underground Test Area Subproject include the radiological inventory resulting from the Baneberry test.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2002

Composite Bending Box Section Modal Vibration Fault Detection

One of the primary concerns with Composite construction in critical structures such as wings and stabilizers is that hidden faults and cracks can develop operationally. In the real world, catastrophic sudden failure can result from these undetected faults in composite structures. Vibration data incorporating a broad frequency modal approach, could detect significant changes prior to failure. The purpose of this report is to investigate the usefulness of frequency mode testing before and after bending and torsion loading on a composite bending Box Test section. This test article is representative of construction techniques being developed for the recent NASA Blended Wing Body Low Speed Vehicle Project. The Box section represents the construction technique on the proposed blended wing aircraft. Modal testing using an impact hammer provides an frequency fingerprint before and after bending and torsional loading. If a significant structural discontinuity develops, the vibration response is expected to change. The limitations of the data will be evaluated for future use as a non-destructive in-situ method of assessing hidden damage in similarly constructed composite wing assemblies. Modal vibration fault detection sensitivity to band-width, location and axis will be investigated. Do the sensor accelerometers need to be near the fault and or in the same axis? The response data used in this report was recorded at 17 locations using tri-axial accelerometers. The modal tests were conducted following 5 independent loading conditions before load to failure and 2 following load to failure over a period of 6 weeks. Redundant data was used to minimize effects from uncontrolled variables which could lead to incorrect interpretations. It will be shown that vibrational modes detected failure at many locations when skin de-bonding failures occurred near the center section. Important considerations are the axis selected and frequency range.

Werlink, Rudy↗

NASA NTRS2010

Pulse-Echo Phased Array Ultrasonic Inspection of Pultruded Rod Stitched Efficient Unitized Structure (PRSEUS)

A PRSEUS test article was subjected to controlled impact on the skin face followed by static and cyclic axial compressions. Phased array ultrasonic inspection was conducted before impact, and after each of the test conditions. A linear phased array probe with a manual X-Y scanner was used for interrogation. Ultrasound showed a delamination between the skin and stringer flange adjacent to the impact. As designed, the stitching in the flange arrested the lateral flaw formation. Subsequent ultrasonic data showed no delamination growth due to continued loading. Keywords: Phased Array, Ultrasonics, Composites, Out-of-Autoclave

Phased array↗

NASA NTRS2010

TPSAS-NF1676L-11096-DND

Phased array↗

DOE OSTI2015

Measurements and modeling of the impact of weak magnetic fields on the plasma properties of a planar slot antenna driven plasma source

The radial line slot antenna plasma source is a type of surface wave plasma source driven by a planar slot antenna. Microwave power is transmitted through a slot antenna structure and dielectric window to a plasma characterized by a generation zone adjacent to the window and a diffusion zone that contacts a substrate. The diffusion zone is characterized by a very low electron temperature. This renders the source useful for soft etch applications and thin film deposition processes requiring low ion energy. Another property of the diffusion zone is that the plasma density tends to decrease from the axis to the walls under the action of ambipolar diffusion at distances far from where the plasma is generated. A previous simulation study [Yoshikawa and. Ventzek, J. Vac. Sci. Technol. A 31, 031306 (2013)] predicted that the anisotropy in transport parameters due to weak static magnetic fields less than 50 G could be leveraged to manipulate the plasma profile in the radial direction. These simulations motivated experimental tests in which weak magnetic fields were applied to a radial line slot antenna source. Plasma absorption probe measurements of electron density and etch rate showed that the magnetic fields remote from the wafer were able to manipulate both parameters. A summary of these results is presented in this paper. Argon plasma simulation trends are compared with experimental plasma and etch rate measurements. A test of the impact of magnetic fields on charge up damage showed no perceptible negative effect.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2013

On-Site Pilot Study - Removal of Uranium, Radium-226 and Arsenic from Impacted Leachate by Reverse Osmosis - 13155

Conestoga-Rovers and Associates (CRA-LTD) performed an on-site pilot study at the Welcome Waste Management Facility in Port Hope, Ontario, Canada, to evaluate the effectiveness of a unique leachate treatment process for the removal of radioactive contaminants from leachate impacted by low-level radioactive waste. Results from the study also provided the parameters needed for the design of the CRA-LTD full scale leachate treatment process design. The final effluent water quality discharged from the process to meet the local surface water discharge criteria. A statistical software package was utilized to obtain the analysis of variance (ANOVA) for the results from design of experiment applied to determine the effect of the evaluated factors on the measured responses. The factors considered in the study were: percent of reverse osmosis permeate water recovery, influent coagulant dosage, and influent total dissolved solids (TDS) dosage. The measured responses evaluated were: operating time, average specific flux, and rejection of radioactive contaminants along with other elements. The ANOVA for the design of experiment results revealed that the operating time is affected by the percent water recovery to be achieved and the flocculant dosage over the range studied. The average specific flux and rejection for the radioactive contaminants were not affected by the factors evaluated over the range studied. The 3 month long on-site pilot testing on the impacted leachate revealed that the CRA-LTD leachate treatment process was robust and produced an effluent water quality that met the surface water discharge criteria mandated by the Canadian Nuclear Safety Commission and the local municipality. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRSDate not supplied

Component Characterization of an eVTOL Reference Model for Crashworthiness Studies

Researchers at the National Aeronautics and Space Administration (NASA) Langley Research Center (LaRC) have conducted a series of structural component and seat level tests to improve finite element model (FEM) characterization of a representative vertical take-off and landing (eVTOL) test article developed by NASA. A full-scale dynamic test was conducted on the representative eVTOL test article in November of 2022. The test article represented a high wing, six passenger eVTOL design concept and is referred to as the lift plus cruise (LPC) test article. The full-scale test identified limitations in the analytical models used to predict aircraft structural response, in particular the composite material models did not effectively capture brittle failure of the structure which were measured during dynamic loading. To better understand the mechanism behind the composite material failure mechanisms observed and to improve the FEM, intact sample specimens of the composite airframe structure were recovered from the test article post-test and used in material characterization testing. In addition, the seat configurations used in the LPC test article were further studied using isolated seat and anthropomorphic test device (ATD) drop tower testing. Dynamic compression tests and three-point bend tests, conducted at varied impact speeds, were performed on the recovered frame section specimens. Additional testing was conducted to characterize the material properties of the forming foam, which remained in the frames after fabrication. These tests were used to improve characterization of the damage and failure parameters of the composite material model used in the FE model of the LPC test article. Seat level tests were conducted on the seats used in the LPC test article using acceleration pulses inclusive of current general aviation and rotorcraft certification load levels as well as conditions representative of those measured at the seat base during the LPC test. The structural material models and seat environment models of the LPC test article FEM were calibrated using the generated component test data. The updates made to these models were then integrated into the LPC FEM and simulated in the full-scale test condition. Results demonstrated the effectiveness of component testing to improve predictive capability of composite aerospace structural models within the crash and dynamic loading environments. Demonstration of the LPC FEM response across an accumulation of coupon, component, seat environment, and full-scale test levels provides confidence in the predictive capability of this model for future use in the study of occupant safety within eVTOL relevant crash environments.

Craswhorthiness↗

NASA NTRSDate not supplied

Component Characterization of an eVTOL Reference Model for Crashworthiness Studies

Craswhorthiness↗

DOE OSTI2012

Evaluation of Cavity Collapse and Surface Crater Formation at the Salut Underground Nuclear Test in U20ak, Nevada National Security Site, and the Impact of Stability of the Ground Surface

At the request of Jerry Sweeney, the LLNL Containment Program performed a review of nuclear test-related data for the Salut underground nuclear test in U20ak to assist in evaluating this legacy site as a test bed for application technologies for use in On-Site Inspections (OSI) under the Comprehensive Nuclear Test Ban Treaty. Review of the Salut site is complicated because the test experienced a subsurface, rather than surface, collapse. Of particular interest is the stability of the ground surface above the Salut detonation point. Proposed methods for on-site verification include radiological signatures, artifacts from nuclear testing activities, and imaging to identify alteration to the subsurface hydrogeologogy due to the nuclear detonation. Sweeney's proposal requires physical access at or near the ground surface of specific underground nuclear test locations at the Nevada Nuclear Test Site (NNSS, formerly the Nevada Test Site), and focuses on possible activities such as visual observation, multispectral measurements, and shallow, and deep geophysical surveys.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2026

The ionomer as an oxygen evolution reaction promoter: piperidinium’s impact on mechanistic pathways on NiO, IrO 2 , and Fe–NiO

The commercial viability of anion exchange membrane (AEM) electrolysis requires optimization of various stack components, with specific catalyst-ionomer combinations often yielding higher current densities, lowered Tafel slopes, and improved mass activity. In this joint theoretical-experimental study, theoretical calculations detail the impact of Versogen’s piperidinium functional group on the complex, kinetically limiting oxygen evolution reaction, finding that the functional group can act as a promoter of specific steps (O*/O 2 * formation; H 2 O/O 2 desorption with reaction enthalpies ranging between 0.2–0.6 eV at higher coverages of O x H y intermediates) on NiO and NiFeO x catalysts. In particular, Fe sites on the NiFeO x catalyst facilitate concerted mechanisms of O*/O 2 * formation and H 2 O desorption with a low enthalpy of 0.5 eV; O 2 desorption alone requires only 0.3 eV. In contrast, Versogen-IrO 2 results in stronger Ir–O bonds, where the enthalpies for bond breaking (Ir–OH 2 and Ir–O 2 ) are considerably higher (1.4 eV and 1.6 eV, respectively). Rotating disk electrode studies utilized commercially available NiO and IrO 2 and synthesized 7.5 wt % Fe in NiFeO x catalysts in combination with Versogen, a common AEM ionomer, and Nafion, an alternative binder. Electrochemical testing validated the impact of these mechanistic changes on ionomer-catalyst combinations, finding that Versogen particularly activates NiO and NiFeO x compared to IrO 2 . Following a 13.5 h hold at 1.8 V, mass activities and Tafel slopes improved to 34 ± 13 A g −1 and 79 ± 2 mV dec −1 (NiO) and 82 ± 4.9 A g −1 and 72 ± 2 mV dec −1 (NiFeO x ). In contrast, Versogen-IrO 2 only reached 17 ± 2.9 A g −1 and 81 ± 3 mV dec −1 . Optimization of the ionomer-catalyst can yield significant increases in performance from initial activity and after an electrochemical conditioning procedure: this enhancement to the mass activity resulted in a 200.9 ± 106.1% improvement for Versogen-NiFeO x and 1284.2 ± 260.5% for Versogen-NiO. In contrast, Nafion-NiFeO x and -NiO offered moderate improvements of 39.1 ± 30.5% and 120.9 ± 59.1%, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗