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DOE OSTI2020

Atomic-Scale Structural Mapping of Active Sites in Monolayer PGM-Free Catalysts by Low-Voltage 4D-STEM

Two-dimensional (2D) materials have attracted a large amount of attention in both basic and applied fields, and scanning transmission electron microscopy (STEM) is often uniquely well-suited for characterizing the atomic-scale structure of these materials [1-4]. As a result, STEM is poised to significantly impact progress on platinum group metal (PGM)-free catalysts, which are currently under intense development to enable low-cost, commercially viable hydrogen fuel cells [5]. While recent advancements have resulted in fuel cell performance comparable to Pt catalysts by some measures [6], cell durability remains a significant challenge, limiting practical applications [7]. Catalytically active sites in PGM-free materials are proposed to be FeN4 complexes embedded in a graphene lattice (Fig. 1b) within layered or other larger materials, but this is still under debate largely due to the range of potential actives sites predicted by computational methods and lack of methods for directly validating these models [5]. Fundamental insights into the atomic structure and resulting degradation pathways of proposed active sites are therefore needed to fully understand and control cell performance and durability [6].2D materials typically make ideal samples for STEM, but those within PGM-free catalysts present additional challenges since these materials are often defect-rich, with a high density of edges, dopant atoms, etc., which significantly increase susceptibility to beam damage at standard operating voltages. This makes analysis of potential FeN4 active sites particularly challenging, since a large proportion of Fe exists at edge sites where beam-induced atomic displacements can prohibit high-resolution structural characterization [6]. Conventional dark-field imaging compounds this problem by producing less signal for a given dose and being less sensitive to light elements than dose-efficient phase contrast imaging techniques such as those enabled by four-dimensional (4D)-STEM [8-10] (Fig. 1a). Consequently, active site structural analysis is often left to methods such as low-resolution imaging combined with quantum chemical calculations [6], which hinders accurate determination of reaction and degradation mechanisms.Here, we demonstrate direct atomic-scale structural mapping of FeN4 sites by performing low-voltage 4D-STEM on a model PGM-free catalyst system with many exposed monolayer regions. To accomplish this, we pair a 30 keV aberration-corrected probe with a fast pixelated detector that has optimal performance at low beam voltages [11]. This enables us to simultaneously image light and heavy elements with high signal-to-noise by center-of-mass analysis (Fig. 1c) while minimizing beam-induced atomic displacements at sensitive sites. The monolayer nature of these materials additionally allows for experimental validation by direct comparison with multislice simulations [12] of model structures (Fig. 1d-e). This work demonstrates how low-voltage 4D-STEM will provide new insights into the atomic-scale structure and degradation mechanisms of active sites in PGM-free catalysts, facilitating the development of low-cost hydrogen fuel cells and other energy conversion technologies in the future [13].

Zachman, Michael↗

DOE OSTI2021

Atomic-scale Imaging of PGM-free Catalyst Active Sites by 30 keV 4D-STEM

Platinum group metal (PGM)-free catalysts have attracted a large amount of attention due to their potential for enabling low-cost, commercially viable hydrogen fuel cells and electrolyzers [1]. Degradation of cell performance remains a significant challenge, however, currently limiting implementation of devices that utilize PGM-free materials [2]. Controlling degradation in these materials requires a better understanding of the atomic structure of active sites, thought to be FeN4 structures within a graphitic carbon lattice, which would enable more accurate prediction of the associated degradation pathways. The exact structural arrangement of active sites in these materials is still debated since a range of structures have been computationally predicted and methods to directly validate these models are still needed [1,3-5].While scanning transmission electron microscopy (STEM) has provided initial glimpses into the nature of the proposed active sites, detailed evaluation of the structure of these sites is challenging since they involve defects, edges, and nitrogen dopants in the graphitic lattice, which are susceptible to beam damage [6,7]. Conventional STEM imaging and spectroscopy methods exacerbate this problem with dose-inefficiency or nonideal contrast characteristics for imaging light and heavy elements simultaneously. A method that minimizes damage while generating dose-efficient, easily-interpretable contrast for both light and heavy elements is therefore needed to facilitate imaging of sensitive active site atomic structure.Here, we demonstrate direct atomic-scale imaging of PGM-free catalyst active sites by low-voltage four-dimensional (4D)-STEM. To accomplish this, we pair a 30 keV aberration-corrected probe, which minimizes knock-on damage, with a fast pixelated detector that has optimal performance at low beam energies [8]. We show how this setup enables relatively simple center-of-mass (CoM) techniques [9,10] to produce images with an increased signal-to-noise ratio (SNR) and light-element contrast over conventional imaging modes, allowing the entire active site structure to be imaged at the atomic scale. Moreover, we show how electron ptychography [11,12] enables images with further improved characteristics to be obtained, for example by minimizing residual aberrations, which provides a more accurate structural representation. The increased understanding that these low-voltage 4D-STEM techniques will provide about the atomic structure of PGM-free active sites and their associated degradation pathways will facilitate rational design of next-generation materials, promoting development of low-cost hydrogen fuel cells, electrolyzers, and other energy conversion devices [13]. References:[1] U Martinez et al., Adv. Mater. 31 (2019), p. 1806545.[2] Y Shao et al., Adv. Mater. 31 (2019), p. 1807615.[3] J Kneebone et al., J. Phys. Chem. C 121, (2017), p.16283.[4] T Mineva et al., ACS Catal. 9 (2019), p. 9359.[5] J Li et al., Nat. Catal. 4 (2021), p. 10.[6] T Susi et al., ACS Nano 6 (2012), p. 8837.[7] P Zelenay and DJ Myers, US Department of Energy Hydrogen and Fuel Cells Program 2017 Annual Merit Review and Peer Evaluation Meeting, Washington, DC (2017).[8] H Ryll et al., J. Inst. 11 (2016), p. P04006.[9] K Müller et al., Nat. Commun. 5 (2014), p. 5653.[10] I Lazic et al., Ultramicroscopy 160 (2016), p. 265.[11] H Yang et al., Nat. Commun. 7 (2016), p. 12532.[12] Y Jiang et al., Nature 559 (2018), p. 343. [13] Research sponsored by the Hydrogen and Fuel Cell Technologies Office, Office of Energy Efficiency and Renewable Energy, US Department of Energy (DOE). Research was conducted at the Center for Nanophase Materials Sciences, which is a DOE Office of Science User Facility.

Zachman, Michael↗

DOE OSTI2020

Use of Unmanned Aerial Systems for Post-closure Waste Site Maintenance and Surveillance - 20143

The P- and R-Area Reactor buildings, located at SRS near Aiken, SC, were in-situ decommissioned by grouting below-grade portions of the buildings and demolishing some above-grade structures to grade level. Other reactor building structures were left above-grade and sealed to prevent human or animal access. Because the above grade-structures are expected to continue in their present state for hundreds of years, the condition of the building roofs is critical to mitigate rainwater intrusion. For this reason, building roof areas were strengthened with high strength concrete to ensure the long-term integrity of the roof structure. Periodic inspections of the roof structures are required to ensure that the roofs are functioning properly and to identify damage areas. The traditional method of inspecting closed reactor buildings requires the use of a helicopter and photographer to generate photographs and videos for review. This method proved sufficient but lacked the resolution and clarity that is required for a thorough inspection of the building structure. Fortunately, the Savannah River National Laboratory (SRNL) has established a Small Unmanned Aircraft System (sUAS) program using commercially available and custom-built remote-controlled aircraft. EC and ACP contacted the SRNL program to evaluate whether the sUAS technology could be employed for periodic reactor building inspections. The sUAS can fly within a few meters of the reactor buildings and hover, allowing for a more thorough aerial inspection. The initial sUAS inspection of the P-Area Reactor building was completed in February 2018 and at the R-Area Reactor building in August 2018 and were successful in providing higher resolution photos and videos. The sUAS inspections also revealed that vegetation had begun to grow on the roofs that could potentially damage the structure integrity. SRNL partnered with Virginia Polytechnic Institute and State University to build a custom heavy lift sUAS that could be equipped with herbicides to remotely treat the vegetative growth. Herbicides were successfully applied to the R-Area Reactor building roof using the custom sUAS in September 2018. The use of unmanned aircraft systems at SRS to perform aerial inspections and herbicide treatment in otherwise inaccessible areas has proven to be an efficient and cost-effective technology that provides high value, increases knowledge of facility conditions, and provides for early detection of damage. Periodic inspections of the reactor building roofs using sUAS technology are performed safely, efficiently, and at a significant cost and schedule savings while reducing emissions, noise, and fossil fuel use. The use of sUAS equipment for building inspections and herbicide application at SRS is unique within the DOE complex. The goal of SRS is to apply this remote technology to other waste unit operations and maintenance activities in the future. (authors)

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DOE OSTI2022

Active Cancellation of Servo-Induced Noise on Stabilized Lasers via Feedforward

Many precision laser applications require active frequency stabilization. However, such stabilization loops operate by pushing noise to frequencies outside their bandwidth, leading to large “servo bumps” that can have deleterious effects for certain applications. The prevailing approach to filtering this noise is to pass the laser through a high-finesse optical cavity, which places constraints on the system design. Here, we propose and demonstrate a different approach where a frequency error signal is derived from a beat note between the laser and the light that passes through the reference cavity. The phase noise derived from this beat note is fed forward to an electro-optic modulator after the laser, carefully accounting for relative delay, for real-time frequency correction. With a hertz-line-width laser, we show ≳20 dB noise suppression at the peak of the servo bump (approximately 250 kHz) and a noise-suppression bandwidth of approximately 5 MHz—well beyond the servo bump. By simulating the Rabi dynamics of a two-level atom with our measured data, we demonstrate substantial improvements to the pulse fidelity over a wide range of Rabi frequencies. Here, our approach offers a simple and versatile method for obtaining a clean spectrum of a narrow-line-width laser, as required in many emerging applications of cold atoms, and is readily compatible with commercial systems that may even include wavelength conversion.

47 OTHER INSTRUMENTATION↗

DOE OSTI2026

Knowledge gaps for neuromorphic ionic computing

BACKGROUND Neuromorphic computing, inspired by the human brain’s ability to process information efficiently, represents a transformative approach to computation. In this Review, we explore the emerging field of neuromorphic ionic computing, which leverages ionic conduction and coupling to mimic neural processes, and identify critical knowledge gaps that must be addressed to realize its full potential. A central theme of the discussion is energy efficiency, a challenge that is both a limitation and an opportunity for this technology. Although complementary metal-oxide semiconductor (CMOS)–based neuromorphic technologies have made strides in scaling to billions of neurons and are increasingly applied in artificial intelligence and numerical computing, they remain orders of magnitude behind the human brain in terms of connectivity and energy efficiency. Neuromorphic ionic computing promises to overcome these limitations by leveraging the distinct architectural and operational principles of the brain. Our brains achieve this energy efficiency by combining several key features: using the same network elements to store and process information; using an incredibly complex and massively interconnected three-dimensional (3D) network of locally active elements that enables sparsity, robustness in the presence of noise, adaptation, and life-long learning; computing at comparatively low voltage and frequency; and last, taking advantage of a plethora of ions and small molecules as information carriers. Here, we propose that ionic computing systems can take advantage of similar features to achieve substantial gains in energy efficiency. ADVANCES Since the first reports of neuromorphic ionic behavior in nanofluidic channels, we have witnessed an explosion of reports that used ionic devices to produce synaptomimetic behaviors. However, achieving the goals of ionic computing requires not only implementation of much more sophisticated device functionality but also overcoming fundamental barriers in materials science, device architecture, and system integration. Current ionic devices, even those incorporating state-of-the-art materials, still suffer from limited functionality and stability, which restrict their performance and increase energy demands. Developing new materials with enhanced ionic properties is essential to overcome these limitations. Similarly, the design of neuromorphic devices must evolve to leverage the particular advantages of ionic processes. Existing architectures often follow a single-information-carrier logic of conventional electronics or are constructed of mesoscale fluidics, failing to capitalize on the energy-efficient mechanisms inherent to ionic systems or implement the multiple-information-carrier paradigm. Current neuromorphic chips focus on large-scale networks of analog memory elements based on mechanisms such as charge trap (flash), filamentary, phase change, or spin, which are built on top of a network of artificial CMOS neurons. Although such prototype networks have achieved impressive performance, it is difficult to envision how they can implement the key features such as massive connectivity, sophisticated plasticity, adaptability, sparsity, and “multichromatic” computing. Although small-scale devices have demonstrated promising results, integrating them, maintaining energy efficiency, and implementing temperature control as systems grow in complexity and size to computationally relevant scale remain major hurdles. Furthermore, interfacing neuromorphic ionic devices with existing computing technologies presents technical and conceptual challenges that will require innovative approaches that combine insights from neuroscience, materials science, and engineering. OUTLOOK Despite these challenges, the potential impact of neuromorphic ionic computing is profound with potential applications ranging from artificial intelligence to robotics and beyond. We also argue that neuromorphic ionic computing systems should not, at least in the beginning, compete with CMOS technologies but rather should focus on applications that require extreme energy efficiency with chemical and/or biological compatibility, such as biomedical applications (for example, brain-computer interfaces), environmental monitoring, and agricultural and food applications. Ultimately, this Review highlights the crucial role of interdisciplinary collaboration in advancing the field. Neuromorphic ionic computing is not merely a technological innovation; it represents a substantial step toward sustainable computation, aligning with the growing demand for energy-conscious solutions in a world that is increasingly reliant on data and computation.

Neuromorphic↗

DOE OSTI2026

Higher Efficiency, Demand Flexible Refrigerator with On-Demand Micro-Vibrational De-icing Technology

Refrigerator technology has advanced significantly over the last couple of decades. Today’s refrigerators use only about 25% of the energy that was required to power models built in 1975. Even as they continually improve efficiency to meet standards, refrigerators have increased in size by almost 20%, added energy-consuming features such as through-the-door ice, and provide more benefits than ever before. However, a few challenges and technology gaps are preventing further improvement of the demand responsiveness and efficiency of the refrigerators. One of the major technology gaps in existing refrigerators is their outdated de-icing process. When the evaporator generates frost, an old-fashioned resistive heating element melts the ice. Most refrigerators have a timed defrost cycle, rather than an active system that could monitor the state of the frost. In these systems, not only is the precious electricity used at its least efficient form of conversion (direct conversion of electricity to heat), but also all the latent heat associated with the ice is wasted during the melting process. On top of that, the refrigerator needs to work harder to pull the temperature down after defrosting, and, last but not least, the food quality is severely impacted by the temperature swings during the defrost cycle. According to a study, the EU alone wastes 89 million tons of food in the supply chain every year. Any temperature swing during defrosting (about 6F according to Emerson for low-temperature cases) can negatively impact the shelf life of meat and other products for multiple days. All these issues can happen during the peak demand time of the electric grid. Unlike the conventional systems, the proposed novel advanced micro-vibrational deicing process uses no heat for defrosting. Instead, it uses the micro vibrations generated by a piezoelectric or vibration-generating module to mechanically break ice from the heat exchanger almost instantaneously. The project titled “Higher Efficiency, Demand Flexible Refrigerator with On-Demand Micro-Vibrational De-icing Technology, performed by Ultrasonic Technology Solutions, LLC (UTS) of Knoxville, TN, in collaboration with Emerson (now Copeland), represents the final phase of a multi-year effort funded under the U.S. Department of Energy’s Building Technologies Office (BTO) BENEFIT FOA 2020. Initiated on October 1, 2021, and completed after a nine-month no-cost extension ending September 30, 2025, this project aimed to develop and validate a novel micro-vibrational mechanical defrosting system, achieving more than 25% improvement in defrosting energy efficiency over conventional baseline defrosting technologies. Over sixteen quarters, the project advanced from fundamental ice-mechanical characterization and prototype development to full-scale system integration and validation. Initial efforts established project management infrastructure and characterized ice adhesion properties, followed by the design and fabrication of early aluminum-based prototypes for resonance frequency testing. Subsequent quarters saw rapid technical progression, including the identification of optimal piezoelectric and motor-based vibration mechanisms, the demonstration of effective de-icing over 6x6-inch aluminum surfaces. The team achieved its Go/No-Go milestone by exceeding the 25% energy-efficiency improvement target—reaching up to 3,340% under optimized conditions—and later confirmed that motor-driven systems offered superior performance and energy efficiency compared to piezoelectric alternatives. Continued refinement led to the development of amplifier systems on printed circuit boards, improved control and instrumentation hardware, and integration into full-scale heat exchanger (HX) prototypes at both UTS and Copeland facilities. Multiple vibration-mounting studies and frost-growth experiments guided mechanical optimization and noise-mitigation strategies, achieving a 17.5 dB reduction in sound pressure level and verifying robust mechanical performance. Advanced analyses, including modal and harmonic simulations, established a quantitative understanding of vibrational behavior and de-icing efficiency across >1000 cm² systems. The final project phase successfully demonstrated scalable integration within reach-in and chest freezer prototypes, confirmed >25% efficiency improvements in large-area systems, and completed a comprehensive business model and scale-up strategy identifying electric defrost systems as the primary beachhead market. The culmination of this DOE-supported effort establishes micro-vibrational defrosting as a viable, high-efficiency, low-noise, and demand-flexible de-icing technology, paving the way for commercial deployment and broader application in next-generation refrigeration systems.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2020

Large Volume Airborne Contamination Monitoring To Support Nuclear Processes' Deactivation and Decommissioning

Current D and D operations at Hanford have demonstrated a flaw in the current state of the art capability of defining airborne contamination boundaries - Airborne particulate emissions of Pu-239 from CM2H operations on the Hanford Pu Finishing Plant were detected well beyond areas controlled for airborne Pu, putting numerous workers at risk for radiological assimilations - Current air samplers and CAM systems were surveying insufficient volumes of air to accurately predict where respiratory protection was required - Hanford is located in a high radon environment, making air monitoring for alpha emitting actinides challenging in high alpha radon induced backgrounds. - Inexpensive HEPA based home and industrial air purifiers filter significantly higher volumes of air than commercially available continuous-air monitoring (CAM) systems. - Inexpensive models capable of filtered air volumes exceeding 1000 times that of a CAM. - Detector system can be built to detect x-rays generated from actinide decay. - Branching ratios of x-rays are 4 orders of magnitude more intense from Plutonium decay than its gamma emissions. - Detector system can be a low resolution systems, as x-ray region of interest is not terribly congested. - Detection systems evaluated will be designed based on slabs of NaI or pixelated NaI or CsI panels. - Simple graphical user interface software will be developed to operate the detection system. - Concept is to deploy some of these air-purifying systems in nonradiological areas around SRNL to confirm radon can be rejected with confidence. - Generate some filters contaminated with plutonium via electroplated Pu or lab generated simulated particles. - then deploy units in known airborne radiological environments to establish systems ability to accurately measure actinide based hot particles Lab analyses will follow up the system analyses to ensure hot particles were correctly identified. Analysis by Scintillation: - Application of scintillation media to the surface of the filters is being explored. - Evaluating slabs of ZnS(Ag), application of powdered ZnS(Cu) and spray on Perkin Elmer Enhance. - Scintillation events would then be digitized with a digital camera and quantified. - Comparing against sensitivity of a PMT or SiPD readout. - Currently evaluating a Thorlabs 8 Megapixel Monochrome Scientific CCD Camera, hermetically sealed cooled package with a wide angle lens. - Wide angle lens allows complete view of HEPA filter from 7 inches away. - Images taken of glow in the dark paint, as well as plutonium-induced fluorescence. - Plutonium was flamed mounted on a 1 inch diameter stainless steel planchet, covered with a layer of mylar and a section of scintillating ZnS obtained from Eljon. - Currently working on reducing signal-to-noise levels to boost sensitivity. - Dark box to hold contaminated or electroplated source covered filters under fabrication. Analysis by x-ray Spectroscopy: - Branching ratios for x-ray emissions from Plutonium isotopes are orders of magnitude more intense than gamma-ray emissions. - The nuclear databases are incomplete on the branching ratios of some of the isotopes. - Evaluating some custom built SrI2 x-ray spectrometers vs a conventional windowed NaI detector. - SrI2 detectors are carbon-composite-windowed 51 mm x 51 mm. - MCNP calculations to establish self absorbance of filter media on 17 keV x-ray. Radon Rejection: - Activated charcoal pre-filter acts as a Radon trap. - Adding a time lapse feature to camera to aid in radon rejection. SRS Plutonium Fuel Form D and D Operations: Currently deploying air sampler to D and D operation of Pu-238 facility at SRS to generate some field samples to analyze.

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