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At least 19 records

Ballistic-Electron-Emission Microscopy Techniques for Nanometer-scale Characterization of Interfaces

Semiconductor interface properties are among the most important phenomena in materials science and technology. The study of metal/semiconductor Schottky barrier interfaces has been the primary focus of a large research and development community for decades. Throughout the long history of interface investigation, the study of interface defect electronic properties have been seriously hindered by the fundamental experimental difficulty of probing subsurface structures. A new method, Ballistic-Electron-Emission Microscopy (BEEM), has been developed which not only enables spectroscopic probing of subsurface interface properties, but also, provides nanometer-resolution imaging capabilities. BEEM employs Scanning Tunneling Microscopy (STM) and a unique spatially localized ballistic electron spectroscopy method...

Bell, L. D.↗

Synthesis‐Related Nanoscale Defects in Mo‐Based Janus Monolayers Revealed by Cross‐Correlated AFM and TERS Imaging

2D Janus transition metal dichalcogenides (TMDs) are promising candidates for various applications including non-linear optics, energy harvesting, and catalysis. These materials are usually synthesized via chemical conversion of pristine TMDs. Nanometer-scale characterization of the obtained Janus materials’ morphology and local composition is crucial for both the synthesis optimization and the future device applications. In this work, we present the results of cross-correlated atomic force microscopy (AFM) and tip-enhanced Raman spectroscopy (TERS) study of Janus monolayers synthesized by the hydrogen plasma-assisted chemical conversion of MoSe 2 and MoS 2 . We demonstrate that the choice of both the growth substrate and the starting TMD influences the residual strain, thereby shaping the nanoscale morphology of the resulting Janus material. Furthermore, by employing TERS imaging, we show the presence of nanoscale islands (≈20 nm across) of MoSe 2 - ${\mathrm{Mo}}_{{\mathrm{Se}}}^{\mathrm{S}}$ (MoS 2 -${\mathrm{Mo}}_{\mathrm{S}}^{{\mathrm{Se}}}$) vertical heterostructures originating from the bilayer nanoislands in the precursor monolayer crystals. The understanding of the origins of nanoscale defects in Janus TMDs revealed in this study can help with further optimization of the Janus conversion process towards uniform and wrinkle-/crack-free Janus materials. Moreover, this work shows that cross-correlated AFM and TERS imaging is a powerful and accessible method for studying nanoscale composition and defects in Janus TMD monolayers.

2D materials↗

Space Weathering Effects in Lunar Soils: The Roles of Surface Exposure Time and Bulk Chemical Composition

Space weathering effects on lunar soil grains result from both radiation-damaged and deposited layers on grain surfaces. Typically, solar wind irradiation forms an amorphous layer on regolith silicate grains, and induces the formation of surficial metallic Fe in Fe-bearing minerals [1,2]. Impacts into the lunar regolith generate high temperature melts and vapor. The vapor component is largely deposited on the surfaces of lunar soil grains [3] as is a fraction of the melt [4, this work]. Both the vapor-deposits and the deposited melt typically contain nanophase Fe metal particles (npFe0) as abundant inclusions. The development of these rims and the abundance of the npFe0 in lunar regolith, and thus the optical properties, vary with the soil mineralogy and the length of time the soil grains have been exposed to space weathering effects [5]. In this study, we used the density of solar flare particle tracks in soil grains to estimate exposure times for individual grains and then perform nanometer-scale characterization of the rims using transmission electron microscopy (TEM). The work involved study of lunar soil samples with different mineralogy (mare vs. highland) and different exposure times (mature vs. immature).

Zhang, Shouliang↗

Roadmap on advanced and / real-time characterisation of solid state materials and devices for energy applications

A strong societal and political drive is motivating the development and optimization of novel energy conversion and storage systems for decarbonization. The successful implementation of solid state devices such as fuel cells and secondary batteries depends, however, on achieving ambitious targets in terms of performance, reliability and cost competitiveness. Research and technology are addressing these needs through a holistic approach including exploration of new materials and nanoarchitectures, as well as system engineering. These significant efforts require the support of appropriate characterization tools capable of assessing nanometer-scale phenomena such as concentration profiles of ionic and electronic charges, local chemical compositions and their evolution over time across interfaces. This roadmap provides an overview of selected advanced characterization techniques for energy materials and devices. Specific focus is put on in situ/operando methods for probing electrochemical phenomena in real-time under realistic working conditions. Experts in the field provide an extensive review of the current state of the art in 2025 and the current and future challenges for the characterization of local chemistry and kinetics in the bulk of the material, in nanoarchitectures (e.g. thin films) and at the interfaces (e.g. grain boundaries, phase contacts, solid/liquid and solid/gas interfaces) . The aim is to provide a detailed guide to the techniques, describing opportunities and bottlenecks for their practical deployment and examples of successful applications.

25 ENERGY STORAGE↗

Fine-Grained, Spinel-Rich Ca-Al-Rich Inclusions From The Reduced CV3 Chondrite Efremovka: A Genetic Link To Wark-Lovering Rims?

Fine-grained, spinel-rich Ca-Al-rich inclusions (FGIs) in carbonaceous chondrites, mostly CV3 chondrites, are interpreted as aggregates of nebular gas-solid condensates that escaped significant melting [1]. Multiple lines of evidence suggest a condensation origin for FGIs, including their layered structures and irregular shapes and the fine grain size of numerous spinel-cored nodules [e.g., 2,3], and the distinctive volatility-fractionated group II rare earth element patterns of bulk inclusions and their mineral constituents [e.g., 4,5]. The origin and nature of FGIs are poorly constrained because of their fine grain sizes and intimate intergrowths of refractory phases, combined with their susceptibility to secondary parent body alteration processes, making detailed mineralogical and petrologic characterizations difficult using scanning electron microscope (SEM) and electron microprobe techniques. In this study, we present preliminary transmission electron microscope (TEM) analyses of pristine FGIs from the reduced CV3 chondrite Efremovka in order to provide the detailed characterization of their micrometer- to nanometer-scale textures and chemical compositions. Our goals are to better understand the formation processes and conditions of FGIs in the early solar nebula and to explore their possible genetic relationship with other early-formed refractory inclusions and their rims.

Keller, L. P.↗

Bio-Nanobattery Development and Characterization

A bio-nanobattery is an electrical energy storage device that utilizes organic materials and processes on an atomic, or nanometer-scale. The bio-nanobattery under development at NASA s Langley Research Center provides new capabilities for electrical power generation, storage, and distribution as compared to conventional power storage systems. Most currently available electronic systems and devices rely on a single, centralized power source to supply electrical power to a specified location in the circuit. As electronic devices and associated components continue to shrink in size towards the nanometer-scale, a single centralized power source becomes impractical. Small systems, such as these, will require distributed power elements to reduce Joule heating, to minimize wiring quantities, and to allow autonomous operation of the various functions performed by the circuit. Our research involves the development and characterization of a bio-nanobattery using ferritins reconstituted with both an iron core (Fe-ferritin) and a cobalt core (Co-ferritin). Synthesis and characterization of the Co-ferritin and Fe-ferritin electrodes were performed, including reducing capability and the half-cell electrical potentials. Electrical output of nearly 0.5 V for the battery cell was measured. Ferritin utilizing other metallic cores were also considered to increase the overall electrical output. Two dimensional ferritin arrays were produced on various substrates to demonstrate the feasibility of a thin-film nano-scaled power storage system for distributed power storage applications. The bio-nanobattery will be ideal for nanometerscaled electronic applications, due to the small size, high energy density, and flexible thin-film structure. A five-cell demonstration article was produced for concept verification and bio-nanobattery characterization. Challenges to be addressed include the development of a multi-layered thin-film, increasing the energy density, dry-cell bionanobattery development, and selection of ferritin core materials to allow the broadest range of applications. The potential applications for the distributed power system include autonomously-operating intelligent chips, flexible thin-film electronic circuits, nanoelectromechanical systems (NEMS), ultra-high density data storage devices, nanoelectromagnetics, quantum electronic devices, biochips, nanorobots for medical applications and mechanical nano-fabrication, etc.

King, Glen C.↗

Operando Infrared Nanospectroscopy of the Silicon/Electrolyte Interface during Initial Stages of Solid-Electrolyte-Interphase Layer Formation

The solid electrolyte interphase (SEI) is a critical component in Li-ion batteries; however, its nanoscale structure and composition and unstable nature make it difficult to characterize and ascertain primary functional mechanisms. We use operando nanoscale Fourier transform infrared spectroscopy (nano-FTIR) with a broadband synchrotron IR source to study the SEI formation on a thin-film Si electrode at nanometer-scale spatial resolution as a function of time and voltage. By probing the Si/carbonate electrolyte interface through a 25 nm-thick amorphous Si window/electrode, we detect molecular vibrational modes within a 10s of nanometers region adjacent to the Si surface and observe that PF6 – anions react to form LiF at 0.5 V. Spatially resolved nano-FTIR spectra showcase subtle nanoscale heterogeneities in the initial solid/liquid interface and the resulting deposited LiF. With its nanoscale resolution and high chemical specificity, operando nano-FTIR provides unique insights into the dynamics and heterogeneous formation of SEIs and opens opportunities for connecting nanoscale interfacial properties to bulk performance metrics.

Dopilka, Andrew↗

Carbon Nanotube Tip Probes: Stability and Lateral Resolution in Scanning Probe Microscopy and Application to Surface Science to Semiconductors

In this paper we present results on the stability and lateral resolution capability of carbon nanotube (CNT) scanning probes as applied to atomic force microscopy (AFM). Surface topography images of ultra-thin films (2-5 nm thickness) obtained with AFM are used to illustrate the lateral resolution capability of single-walled carbon nanotube probes. Images of metal films prepared by ion beam sputtering exhibit grain sizes ranging from greater than 10 nm to as small as approximately 2 nm for gold and iridium respectively. In addition, imaging stability and lifetime of multi-walled carbon nanotube scanning probes are studied on a relatively hard surface of silicon nitride (Si3N4). AFM images Of Si3N4 surface collected after more than 15 hrs of continuous scanning show no detectable degradation in lateral resolution. These results indicate the general feasibility of CNT tips and scanning probe microscopy for examining nanometer-scale surface features of deposited metals as well as non-conductive thin films. AFM coupled with CNT tips offers a simple and nondestructive technique for probing a variety of surfaces, and has immense potential as a surface characterization tool in integrated circuit manufacturing.

Nguyen, Cattien V.↗

Scintillating Quantum Dots for Imaging X-rays (SQDIX) for Aircraft Inspection

Scintillation is the process currently employed by conventional x-ray detectors to create x-ray images. Scintillating quantum dots or nano-crystals (StQDs) are a novel, nanometer-scale material that upon excitation by x-rays, re-emit the absorbed energy as visible light. StQDs theoretically have higher output efficiency than conventional scintillating materials and are more environmental friendly. This paper will present the characterization of several critical elements in the use of StQDs that have been performed along a path to the use of this technology in wide spread x-ray imaging. Initial work on the SQDIX system has shown great promise to create state-of-the-art sensors using StQDs as a sensor material. In addition, this work also demonstrates a high degree of promise using StQDs in microstructured fiber optics. Using the microstructured fiber as a light guide could greatly increase the capture efficiency a StQDs based imaging sensor.

Burke, Eric↗

Scintillating Quantum Dots for Imaging X-Rays (SQDIX) for Aircraft Inspection

Scintillation is the process currently employed by conventional X-ray detectors to create X-ray images. Scintillating quantum dots (StQDs) or nano-crystals are novel, nanometer-scale materials that upon excitation by X-rays, re-emit the absorbed energy as visible light. StQDs theoretically have higher output efficiency than conventional scintillating materials and are more environmentally friendly. This paper will present the characterization of several critical elements in the use of StQDs that have been performed along a path to the use of this technology in wide spread X-ray imaging. Initial work on the scintillating quantum dots for imaging X-rays (SQDIX) system has shown great promise to create state-of-the-art sensors using StQDs as a sensor material. In addition, this work also demonstrates a high degree of promise using StQDs in microstructured fiber optics. Using the microstructured fiber as a light guide could greatly increase the capture efficiency of a StQDs based imaging sensor.

Burke, E. R.↗

Topographic Characterization of Niobium Films on Copper for SRF Applications

Niobium films on copper substrates are being actively developed as a low-cost alternative to bulk niobium for superconducting radio-frequency (SRF) cavities, offering superior thermal conductivity, reduced material cost, and the potential for scalable cavity fabrication. The performance of such films can be limited by imperfect surfaces that reduce the peak achievable magnetic field. Nb films deposited under varied electron cyclotron resonance conditions were characterized via atomic force microscopy. The films exhibit a corrugated surface morphology which can be characterized by the depth of the corrugation, slope angle, and standard roughness parameters. The influence of this surface roughness on field limitations is examined within the framework of London theory. These measurements and models aid in understanding how ECR deposition conditions influence the nanometer-scale roughness of Nb films on Cu and its impact on high-field SRF cavity performance.

Redman, Brandi [Old Dominion Univ., Norfolk, VA (U↗

Time of Flight Secondary Ion Mass Spectrometry for Characterization of Pt-Coated Porous Transport Layers in PEM Water Electrolyzers

Titanium-based porous transport layers (PTLs) and iridium-based catalyst layers (CLs) are two main components of proton exchange membrane water electrolyzers (PEMWEs). PTLs are typically coated with platinum to minimize interfacial losses and to support long-term operation. Optimizing coatings and the PTL-CL interface requires comprehensive characterization. This study establishes time-of-flight secondary ion mass spectrometry (ToF-SIMS) as a valuable technique for PTL characterization, addressing capabilities and limitations related to PTL morphology. A methodology was developed that uses a Cs + sputter beam for dynamic depth profiling, with data collected in both positive-ion (MCs + ) and negative-ion modes to generate depth profiles, 2D ion maps, and 3D ion reconstructions. ToF-SIMS detected relative differences in platinum-layer thickness between samples; these trends were validated by cross-sectional scanning transmission electron microscope (STEM) measurements and flat-titanium substrate controls. Interfacial oxide layers are identified in both ion modes, with enhanced oxide sensitivity in negative mode. The technique’s high sensitivity enables detection of nanometer-scale coatings and trace impurities within the bulk PTL structure. These results provide a methodological framework for analyzing Pt-coated PTLs, with the potential to extend to other components in PEMWEs and other electrolyzer systems.

36 MATERIALS SCIENCE↗

Shock propagation in aerogel and TPP foams for inertial fusion energy target design

Achieving practical inertial fusion energy (IFE) requires the development of target designs with well-characterized microstructure and compression response. We measured shock dynamics in low-density (17.5–500 mg/cm 3 ) aerogel and two-photon polymerization (TPP) foams using x-ray phase contrast imaging (XPCI) methods and the Velocity Interferometer System for Any Reflector. By analyzing shock front evolution, we examined how target type and density influence shock propagation and energy dissipation. Talbot-XPCI shows that aerogels support a smooth, bowed shock front due to their homogeneous nanometer-scale pore network. In contrast, TPP foams exhibit irregular, stepwise propagation driven by interactions with their periodic micrometer-scale lattice. Shock velocity follows a power-law relation: aerogels deviate from classical ρ −1/2 scaling due to pore-collapse dissipation, while TPP foams follow the trend with larger uncertainties from density variations. Comparisons with xRAGE simulations reveal systematic underestimation of shock speeds. These results provide the first experimental constraints on shock propagation in TPP foams over a wide density range and highlight the influence of internal structure on anisotropic shock behavior. Our findings support improved benchmarking of EOS and hydrodynamic models and inform the design of foam architectures that promote implosion symmetry in IFE capsules.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Carbon Nanotube Scanning Probe for Surface Profiling of DUV and 193 nm Photoresist Pattern

The continual scaling down of semiconductors to 100 nm and below necessitates a characterization technique to resolve high aspect ratio features in the nanoscale regime. This paper reports the use of atomic force microscope coupled with high aspect ratio multi-walled carbon nanotube scanning probe tip for the purpose of imaging surface profile of photoresists. Multi-walled carbon nanotube tips used in this work are 5-10 nm in diameter and about a micron long. Their exceptional mechanical strength and ability to reversibly buckle enable to resolve steep, deep nanometer-scale features. Images of photoresist patterns generated by 257 nm interference lithography as well as 193 nm lithography are presented to demonstrate multi-walled carbon nanotube scanning probe tip for applications in metrology.

Nguyen, Cattien V.↗

Co-Design of Charge Transport Superhighways to Connect Catalytic Sites in Soft Photoelectrochemical Systems

Efficient photon-to-electron-to-molecule conversion requires multi-length scale control over charge transport pathways, where electronic charges are delivered to catalytic sites under high mass transport flux. A fundamental question is how can we co-design charge transport pathways to promote efficient charge transfer to/from catalytic sites in complex three-dimensional architectures? Soft conducting polymer systems offer exceptional promise to provide three-dimensional charge transport networks, where electrolyte (ion and solvent) can interdiffuse to promote long-lived charge carriers and the molecular nature allows for strategic synthetic design of catalytic sites. Herein we combine theoretical and experimental approaches to investigate the earliest stages of photoelectrochemical deposition of near-surface catalytic sites (Pt) on soft bulk heterojunction polymeric semiconductors composed of a prototype donor (PTB7-Th) and a prototype acceptor (N2200) as a model system towards better understanding molecular catalyst-polymer site interactions. We focus initially on photoelectrochemical deposition of low Pt loadings, nanoparticle sizes (formed by progressive nucleation) below 20 nm, for both density functional theory (DFT) modeling studies and for spectroscopic characterization using surface-sensitive X-ray and UV-photoemission (XPS/UPS). DFT modeling of “n-type” N2200 slabs reveal for the first time that sulfur atoms in the thiophene units serve as the lowest-energy adsorption sites for single Pt atoms, while larger Pt clusters engage more complexly with both thiophene and naphthalene diimide (NDI) core sites. Changes in chemical composition observed by X-ray photoelectron spectroscopy (XPS) support the DFT predictions, and the angle-resolved measurements reveal that Pt nucleation initiates at subsurface sites which appear to be localized active domains that promote charge transport/transfer and enable vertical growth toward the surface. These results suggest that light-activated Pt nanoparticle deposition decorates energetically distinct sites, where photoactivity is dictated by the local energetics of those sites, and the fact that they represent the termini of charge transport “super-highways” – a small percentage of the total volume of the donor/acceptor polymeric active layer which carries most of the photocurrent generated during both Pt deposition and photoelectrochemical HER. We posit that these initial studies provide a foundational strategy for design of catalytic sites in the near surface regions of complex polymeric materials and advancing soft semiconductor-based photoelectrochemical systems. Achieving a nanometer-scale understanding of catalyst deposition and the impact of local composition and energetics on that placement, should ultimately provide the design guidelines (co-design) for a broad array of catalysts at sites that optimize that efficiency and maximize platform durability.

14 SOLAR ENERGY↗

Advancing Dust Tolerant Mechanisms for a Sustained Exploration of the Moon

Introduction: “I think dust is probably one of our greatest inhibitors to a nominal operation on the Moon. I think we can overcome other physio-logical or physical or mechanical problems except dust.”– Gene Cernan, Apollo 17 Technical Debrief The Apollo missions revealed the impact of lu-nar dust on mechanisms. Lunar dust particles are jagged and electrostatically charged, giving them the ability to bind or damage mechanisms and alter thermal properties. Reports documented clogged equipment and jammed mechanisms in every mission, regardless of surface duration, as well as clogged mechanisms in the Extravehicular Mobility Suit (EMS), including zippers, wrist and hose locks, faceplates, and sunshades [1-2]. Several astronauts remarked they could not have sustained surface activity much longer because clogged joints would have frozen up completely [2]. Effective dust mitigation strategies are need-ed to support longer duration stays on the lunar surface [3-4]. State of the Art: Technology for mechanisms able to operate in dusty enviroments is advancing rapidly due to the needs of both Mars rovers and the Artemis program. Vacuum-tight connectors are essential for spacesuits and habitats, and their performance can be dependent on cleaning technologies, which have proven difficult on the lunar surface. Several TRL 3-5 technologies are undergoing tests with the expectation to reach TRL 6 within 1-2 years. Some mechanisms will be infused and tested on the VIPER (Volatiles Inves-tigating Polar Exploration Rover) mission planned for mid-2020s. NASA Funded Efforts: NASA has recognized the need for dust tolerant mechanisms, and has partnered with industry to advance the state-of-the-art. At NASA GRC, KSC, and JSC, the Dust Tolerant Mechanisms Project is working to devel-op advanced actuator seals for rotary joints and rotary bearing technologies for long-term sus-tained operation in lunar dust environments. An-other NASA project at NASA GRC, partnered with GSFC, JPL, and KSC is Motors for Dusty & Ex-treme Cold Environments (MDECE). MDECE is developing an unheated magnetically-geared mo-tor that can operate continuously for a long dura-tion at an ambient temperature of -243 ºC (33 K). NASA GRC has the capability to characterize the effects of dust on seals, mechanisms, and other mating surfaces and components under lunar conditions [5]. Through the SBIR/STTR program, NASA has funded several companies to advance dust toler-ant mechanisms via the Dust Tolerant Mecha-nisms sub-topic with applications in surface mobil-ity, spacesuits, connectors, joints, and more. LSIC and Community Efforts: The Lunar Surface Innovation Consortium (LSIC) Dust Miti-gation focus group has fostered collaborations across NASA, industry, and academia to develop solutions that minimizes the impact of lunar dust on robotic and human systems. Community ef-forts have included topical meetings on dust tol-erant mechanisms, featured technology presenta-tions, and feedback to NASA on potential gaps and needs. Testing: In 2021, NASA released NASA-STD-1008 [6]. This NASA Technical Standard estab-lishes minimum requirements and provides guid-ance for testing systems and hardware to be ex-posed to dust in planetary environments. The standard has specific sections dedicated to Mechanisms Testing (e.g. bearings, gears) as well as Seals and Mating Surfaces Testing (e.g. hatches, docking systems). Gaps and Needs: NASA is tracking dust tol-erant mechanisms as a gap in a cross-directorate analysis of capability areas needed to enable fu-ture human space-flight architectures. Two high-priority gap areas include additional facilities for testing mechanisms in lunar-surface conditions, and a better understanding of vulnerabilities to the smallest, nanometer-scale dust particles. Conclusion: Understanding and mitigating lu-nar dust is critical to successful, sustained opera-tions on the lunar surface – whether autonomous or otherwise. This presentation will discuss both the state-of-the-art and open needs in lunar dust tolerant mechanisms, technology impacts, mitiga-tion approaches, testing, LSIC community efforts, and more. References: [1] Gaier, J. R. (2020). The Im-pact of Dust on Lunar Surface Equipment During Apollo. Lunar Dust 2020. [2] GRC, & Gaier, J. R. (2005). The Effects of Lunar Dust on EVA Sys-tems During the Apollo Missions. [3] Johansen, M. R. (2020). An Update on NASA’s Lunar Dust Mitigation Strategy. Lunar Dust 2020. [4] ASI, CSA, ESA, JAXA, & NASA. (2016). Dust Mitiga-tion Gap Assessment Report. [5] Jimenez, N. et al (2022), LPSC Abstract 2572. [6] NASA-STD-1008, 2021.

J I Nunez↗