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DOE OSTI2025

Chemical Analysis of Tantalum Thin Films compared to Niobium Thin Films using SIMS and XPS

Superconducting qubits are a leading platform for quantum computation. These circuits are typically made from superconducting materials like aluminum or niobium. However, the amorphous niobium oxide and aluminum oxide on the surface of these circuits introduce considerable RF loss due to the presence of two-level systems (TLS), which limits the maximum coherence times T1 to ~100 μs. Capping the niobium qubits with a tantalum layer leads to a 3- 5x improvement [Bal et al., 2024]. But even in this case, tantalum forms an amorphous surface oxide that introduces loss. In an effort to devise strategies to eliminate the presence of this oxide, we present a comprehensive study on the nature of Ta oxide using x-ray photoemission spectroscopy (XPS) and secondary ion mass spectrometry (ToF-SIMS) as a function of heat treatment. The thin films were annealed in ultra-high vacuum conditions and analyzed in situ to characterize the composition and evolution of the native tantalum oxide layer and oxide-metal interface. Our analysis reveals two critical differences between tantalum and niobium oxides: Nb2O5 completely dissolves at 400°C, while Ta2O5 persists even at 800°C. Additionally, tantalum oxide contains only a single suboxide (TaO), in contrast to niobium's two suboxides (NbO and NbO2). The suboxide of tantalum contributes minimally to the total oxide content and shows a relative increase with temperature. Understanding the oxide’s behavior will open new pathways for optimizing coherence times in tantalum qubits.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

NASA NTRS1977

Method of forming metal hydride films

The substrate to be coated (which may be of metal, glass or the like) is cleaned, both chemically and by off-sputtering in a vacuum chamber. In an ultra-high vacuum system, vapor deposition by a sublimator or vaporizer coats a cooled shroud disposed around the substrate with a thin film of hydride forming metal which getters any contaminant gas molecules. A shutter is then opened to allow hydride forming metal to be deposited as a film or coating on the substrate. After the hydride forming metal coating is formed, deuterium or other hydrogen isotopes are bled into the vacuum system and diffused into the metal film or coating to form a hydride of metal film. Higher substrate temperatures and pressures may be used if various parameters are appropriately adjusted.

Steinberg, R.↗

DOE OSTI2024

Ultra-High Efficiency and Stable All-Perovskite Tandem Solar Cells

In the project period, the research team has fabricated more than 6,000 single-junction wide-bandgap (wide-E g ) and low-bandgap (low-E g ) perovskite solar cells (PSCs) and more than 2,000 all-perovskite tandem solar cells (APTSCs). The best-performing wide-E g and low-E g PSCs and APTSCs showed PCEs greater than 19%, 23%, and 30%, respectively. The average PCEs for wide-E g and low-E g PSCs and APTSCs fabricated by the benchmark processes are (18.5 ± 0.4)%, (21.9 ± 0.8)%, and (26.8 ± 2.1)%, respectively. We have demonstrated APTSCs with T 80 lifetime of more than 1,000 h, which were measured by maximum power point tracking (MPPT) under one sun operation in the air. The team has also utilized various advanced characterization techniques to study the optical and electrical properties of wide-E g and low-E g perovskite materials and devices, developing a better understanding of the unique working principle and degradation mechanism of APTSCs. The team has met most GNG decision criteria except for the stability goal of APTSCs under 85 °C/85 RH accelerated lifetime test (ALT). The shortfall of the device ALT stability is mainly limited by the intrinsic instability of Sn-Pb perovskites under illumination at elevated temperatures. The team discussed with stakeholders in the PV academic and industry about these durability concerns and concluded that this is the major technical barrier preventing the market entry of APTSCs. Future fundamental study and R&D work are needed to advance this promising technology.

14 SOLAR ENERGY↗

DOE OSTI2026

Evolution of size-selected Pt cluster catalysts on prototypical oxide supports

The current quest for new pathways into sustainable, efficient and durable energy conversion technologies makes the used for a fundamental understanding of the atomic-scale phenomena underlying catalytic processes ever more pressing. In this context, characterizing catalyst particles in situ provides valuable information about the evolution of their composition, structure, oxidation state and charge state during an ongoing process. To disentangle the influence of individual parameters – temperature, pressure, gas composition, cluster size, as well as support acidity, redox state and defect density – it is crucial to control them precisely and separately in experiments. At the example of size-selected Pt n clusters – i.e. sub-nm particles defined to the exact number of atoms – on flat oxide supports, we follow their rich evolution phenomena via (synchrotron-based) X-ray photoelectron spectroscopy (XPS) and scanning tunnelling microscopy (STM) during temperature ramps and in various gas environments. Here, we present our experience with these highly defined, yet complicated-to-create samples in ultra-high vacuum (UHV) and at mbar pressures. We discuss their stability during transport to synchrotrons and under reaction conditions on three prototypical oxide supports and show the various phenomena that can be disentangled. Ptn clusters on the non-reducible silicon dioxide, SiO 2 , remain size-selected and show remarkable stability. Doping strongly influences the size-dependent binding energy shifts and changes the Pt response to oxidative and reaction conditions, which we attribute to different cluster geometries: p-type doping leads to wetting, enhanced sinter resistance and a diminished response to oxidative environments, compared to clusters on n-type doped samples. We compare the system with our previous findings of a similar change in dimensionality for Pt 20 clusters on the reducible ceria, CeO 2 (111), support, induced by modulation of its O vacancy density. The Pt n /CeO 2 system is particularly interesting for strategies to stabilize and redisperse Pt clusters dynamically. Finally, we study the evolution of Pt n clusters on another reducible oxide support, magnetite, Fe 3 O 4 (001), in 0.1 mbar alternating redox conditions at RT and elevated temperature. In analogy to findings previously reported for Pt/TiO 2 (110), the clusters either become encapsulated by a thin oxide film via strong metal–support interaction (SMSI) or deeply buried in the magnetite. Overall, our approach of following the evolution of size-selected clusters on oxide supports leads to fundamental atomic-scale insights on nano-scale catalyst materials, on our path to sustainable, dynamic and self-repairing catalysts.

Falling, Lorenz J. [Technical Univ. of Munich (Ger↗

DOE OSTI2025

Particle balance of deuterium during deuterium shattered pellet injection shutdown in DIII-D

A particle balance analysis was conducted during a deuterium (D 2 ) shattered pellet injection-induced plasma shutdown on the DIII-D tokamak to determine why less than 20% of the pellet material is assimilated into the core plasma by the mid-current quench (CQ). Initially, most of the D 2 is injected as frozen shards and ionized upon entering the vessel. During the thermal quench, ionized particles move to the divertors and subsequently to the center post (CP) walls, where they rapidly recycle and partially accumulate as neutrals without assimilating into the core plasma. In contrast, the particle flux to the outer midplane walls is negligible, despite being accompanied by hot plasma with electron temperatures exceeding 100 eV. During mid-CQ, volume recombination effects, although not large enough to impact overall particle balance, were significant enough to require accounting for accurate interpretation of fast-framing camera D-alpha signals and the estimation of the CP wall particle flux. In addition, toroidal asymmetries, observed in measurements of toroidal electron density perturbations and the phase of magnetohydrodynamic modes, are present throughout the shutdown and can account for a discrepancy in the assimilation rate for up to 50% of the observed D 2 particle inventory. These sources and sinks of particles and fluxes were identified using absolutely calibrated D-alpha brightness and Langmuir probes.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2025

Ultra-high efficiency hydrogen production using a large-scale solid oxide electrolysis cell system

Efficient and cost-effective production of clean hydrogen is key to decarbonizing the production of hard-to-abate industries, such as chemicals, fuels, steel, cement and many other commodities that form the basis of modern societies. High-temperature steam electrolysis (HTSE) has recently become commercially available and offers opportunities for producing hydrogen at higher efficiency and lower cost than competing low temperature technologies. In this work, we report world record setting hydrogen production efficiency from large-scale prototype HTSE systems based on solid oxide electrolysis cell (SOEC) technology. Independent tests performed at Idaho National Laboratory (INL) employed a Bloom Energy 100 kW SOEC system to achieve a hydrogen production direct current specific electric energy consumption as low as 36.7 kWh per kilogram of hydrogen. Remarkably, similar high efficiencies in the range of 36–39 kW/kg-H2 were obtained over a wide range of hydrogen production rates and even during dynamic ramping as the hydrogen production and electric power consumption of the system were varied between 20 % and 100 % of nominal conditions. Furthermore, these test results validate previous projections that commercial SOEC systems can produce clean hydrogen at efficiencies approaching 100 % for less than 2 U S. dollars per kilogram when located near sources of inexpensive, low-grade heat and clean electricity.

08 HYDROGEN↗

DOE OSTI2025

Rapid tempering to enhance dynamic performance of high and ultra-high strength steels

This study employed rapid, short-time duration (1 s) tempering to improve the dynamic performance of high-strength steel (HSS) and ultra-high-strength steel (UHSS), compared to quenched and conventionally (1800 s) tempered microstructures. Rapid tempering significantly improved the Charpy toughness of both steels compared to the conventionally tempered condition at an equivalent tempering parameter (TP) or hardness level. For conventionally tempered conditions, tempered martensite embrittlement was observed within the tempering temperature range of 200–400 °C, whereas rapid tempering exhibited increased Charpy toughness with increasing tempering temperature across all tempering conditions. Dynamic compression experiments indicated that rapid tempering led to improved ductility compared to the conventionally tempered condition at an equivalent TP. This work shows that the same rapid tempering strategy used for HSS is directly transferable to a higher-carbon UHSS and provides the first systematic evidence of improved strength-ductility combinations and cracking resistance under dynamic compression, supported by Kolsky bar experiments.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Development of Transformative Preparation Methods to Push up High Q&G Performance of FRIB Spare HWR Cryomodule Cavities

The FRIB accelerator project construction, a top priority of US nuclear science, was completed in January 2022, and is now moving to user operation. The stable and reliable operation of the accelerating cryomodules is essential in achieving/fulfilling DOE and user expectations. So far, FRIB cryomodules meet all FRIB specifications for cavity performance. However, during the lifetime of machine operation, degradation of cryomodule performance is possible, as reported in similar operating facilities (CEBAF, SNS). If cryomodule degradation is observed at FRIB, the under-performing cryomodule will require replacement/maintenance. In effort to manage operational reliability, FRIB plans to construct a 0.53 half-wave cryomodule to serve as an active spare. In a parallel effort, FRIB will also work toward increasing operational Q and gradient of spare cryomodule cavities to gain an overall performance margin to support future operational reliability. The current FRIB cavity designs have a potential to operate at gradients higher than 8 MV/m, but are currently limited by field emission (FE) and/or high field Q slope (HFQS); known issue in buffered chemical polished (BCP) treated cavities. The proposal looks to develop transformative surface preparation treatments to improve the operational gradient of spare cryomodules higher than 10 MV/m while maintaining high Q. Thus, increasing operational margin by 30 - 50%. With the goal to improve operational reliability set, the proposal will investigate multiple objectives as possible paths forward to achieve an overall increase in cavity performance and gain a better understanding of SRF limiting mechanisms. The proposal will study the application of different chemical surface treatments to 0.53 half-wave cavities, with the addition of low temperature bakes (LTB), and measure their effects on accelerating performance. Proposed chemical treatments to be explored in this proposal include conventional EP acid mixtures, as well as innovated EP and BCP acid mixtures designed to simplify processing paths in migrating FE and HFQS. The proposed transformative treatment wet N-doping also has the potential to replicate recent advancements in SRF technology relating to nitrogen doping and high Q operation without the requirement for an ultra-high vacuum annealing furnace; currently being developed at FNAL and JLAB. In parallel, high Q performance relating to flux trapping will be investigated with the installation of a second layer of magnetic shielding in the vertical test Dewar. The research objectives presented in the proposal, and their corresponding effects on cavity performance, will provide essential knowledge and future guidance to the SRF community and provide possible paths for future SRF based projects and applications.

43 PARTICLE ACCELERATORS↗

DOE OSTI2025

Correlating Nb-SRF Surface Processing with Evolution of Surface Electronic States

The few nanometers of the surface exposed to RF field plays a major role in defining the RF performance of superconducting cavities. Over the past two decades, several pioneering surface treatment and processing methods have emerged, enabling remarkable improvements in cavity performance by simultaneously achieving high Q with increasing Eacc. These processing methods include: thermal treatment under ultra-high vacuum (UHV) conditions across lo¬¬¬¬¬¬¬w-, mid-, and high-temperature ranges and high temperature treatments under controlled N2 atmosphere. These processes also produce distinct surface oxide configurations with different valence states, thicknesses, and uniformity, as well as different oxygen concentration profiles in bulk Nb. In this work, we are trying to understand how do surface-processing methods and the resulting oxide/oxygen profiles affect the electronic structure of surface and the mechanism of superconductivity? With the help of Fermilab’s in-house X-ray photoemission facility and, in collaboration with the synchrotron-based angle-resolved photoemission (ARPES) facility at Argonne National Laboratory, we are investigating how the valence band structure and density of states (DoS) near the Fermi level modify with different surface treatments. Our observations show that different surface-processing methods lead to distinct evolutions of the valence-band states near the Fermi level during the superconducting transition. This behavior suggests variations in Nb-O orbital hybridizations and points towards the possibility of different underlying mechanisms of superconductivity governed by the surface chemistry and oxide configuration. We also correlate these distinct superconducting mechanisms with RF cavity performance, specifically focusing on measured surface resistance, the nature of the Q-slope, and quench fields observed in SRF measurements. These results will enable us to identify the potential limiting factors and relevant controllable parameters that can be further optimized to improve the performance of SRF cavities.

Tripathi, Malvika [Fermilab]↗

DOE OSTI2026

Correlating Surface Processing of Nb Superconducting RF Cavities with the Evolution of Surface Electronic States

Superconducting-radio frequency (RF) cavities provide an efficient way to accelerate particle beams with extremely high acceleration gradients while generating very small power dissipation. The few nanometers of the surface play a critical role in defining the RF performance of superconducting Nb based cavities. Over the past two decades, several pioneering surface treatment and processing methods have emerged, enabling remarkable improvements in superconducting cavity performance by simultaneously achieving high quality factors with increasing maximum acceleration gradients. These processing approaches include chemical polishing, distinct multi-step thermal treatments under ultra-high vacuum (UHV) conditions over low to high temperature regimes, as well as high-temperature treatments under controlled nitrogen atmospheres. Beyond their macroscopic impact on RF performance, these methods produce distinct surface oxide configurations characterized by different valence states, oxide thicknesses, chemical uniformity, and oxygen concentration profiles extending into the near-surface bulk of niobium. In this work, we are trying to understand how the surface-processing methods and the resulting oxide/oxygen profiles affect the electronic structure of surface and the mechanism of superconductivity. Using a combination of X-ray photoemission and X-ray absorption spectroscopies, we investigate how the valence-band structure and the electronic density of states (DoS) near the Fermi level evolve under different surface treatments. By employing tunable photon energies across multiple elemental absorption edges, we use resonant photoemission to disentangle and identify the elemental contributions to specific valence-band features. Our observations show that different surface-processing methods lead to distinct temperature evolutions of the DoS and valence-band states near the Fermi level. Our results suggest variations in different Nb-O orbital hybridizations in distinct processes and point towards the possibility of different underlying mechanisms of superconductivity governed by surface chemistry and oxide configuration. We also correlate these distinct superconducting mechanisms with RF cavity performance, specifically focusing on measured surface resistance, the nature of the Q-slope, and quench fields observed in superconducting RF measurements. These results will enable us to identify the potential limiting factors and relevant controllable parameters that can be further optimized to improve the performance of superconducting RF cavities.

Tripathi, Malvika [Fermilab] (ORCID:00000001989251↗

DOE OSTI2026

Ultra-High Vacuum Outgassing Characterization of Thermally Processed Low-Carbon Steel for Advanced Particle Accelerator and Gravitational Wave Detector Applications

This dissertation investigated AISI 1020 low-carbon steel as an alternative vacuum chamber material to conventional stainless steel for ultra-high vacuum (UHV) and extreme-high vacuum (XHV) applications. After a 400 °C/48 h bake, AISI 1020 tube chambers achieved a hydrogen outgassing rate of 2.4 × 10¿¹6 Torr·L·s¿¹·cm¿², approximately 2,300 times lower than the prebaked 316L stainless-steel comparator, among the lowest hydrogen outgassing rates ever reported for an uncoated metallic vacuum chamber. Bare and magnetite-coated AISI 1020 chambers were then compared using throughput and rate-of-rise methods. The magnetite coating yielded 5× lower water outgassing at room temperature, but this advantage disappeared after 80 °C baking. After full thermal conditioning (400 °C/48 h prebake followed by 150 °C/96 h and 200 °C/110 h), bare steel achieved 25× lower hydrogen outgassing than the magnetite-coated chamber (9.6 × 10¿¹6 Torr·L·s¿¹·cm¿²) and >99% H2 purity with carbon species below RGA detection. Monte Carlo molecular flow simulations of a CEBAF photogun beamline (96 scenarios) showed that replacing 304L stainless steel with AISI 1020 reduces equilibrium H2 pressure by a factor of 833; a single 304L electrode contributes 98.8% of the gas load despite occupying only 9.1% of the internal surface area. A 500-m Einstein Telescope beampipe screening showed that corrugated bellows contribute 18% of the gas load from only 0.7% of the surface area. A five-model adsorption isotherm framework applied to 22 pumpdown datasets (164 fits with AR(1)-GLS correction) established that the experimental protocol, not the material, controls isotherm identifiability: Dubinin–Radushkevich wins isothermal pipe pumpdowns; Langmuir wins thermally dominated chamber bakes. Cross-dataset joint fitting of the AISI 1020 pipe pumpdowns yielded an H2 diffusion activation energy Ed = 7.24 ± 1.28 kcal·mol¿¹, consistent with trap dominated diffusion in commercial low-carbon steels. Two companion innovations were developed: a Variable Conductance Device (VCD, patent pending IDF-00723) for XHV outgassing measurement, and VacuumDesignerPro (VDP), a MATLAB-based design tool validated against LIGO benchmarks.

Al-Allaq, Aiman H [Old Dominion University]↗

NASA NTRS1980

Directional solidification at ultra-high thermal gradient

A high gradient controlled solidification (HGC) furnace was designed and operated at gradients up to 1800 C/cm to continuously produce aluminum alloys. Rubber '0' rings for the water cooling chamber were eliminated, while still maintaining water cooling directly onto the solidified metal. An HGC unit for high temperature ferrous alloys was also designed. Successful runs were made with cast iron, at thermal gradients up to 500 C/cm.

Flemings, M. C.↗

NASA NTRS1982

A facility for the simulation of low orbit atmospheric oxygen bombardment

A molecular beam facility to simulate the space environment of a spacecraft at low orbit was designed with the intent of studying the effect on the properties of optical elements of oxygen atoms impacting at orbital velocity. The four-stage differentially pumped molecular beam facility includes a variety of oxygen atom beam sources which cover a wide range of velocities (1 km/sec to approximately 8 km/sec), in addition to the ultra-clean experimental environmental of an ultra-high vacuum chamber and an optical diagnostic set-up. The primary oxygen atom beam source used to obtain the 8 km/sec O atoms is an arc heated source. It consists of a modified commercially available plasma torch. The modifications include attachments which provide for a nozzle which is used to expand the atomic beam into the vacuum system, and exhaust channels to dispose of excess torch gas. The torch operates in the 'nontransferred' mode of operation, that is the electric arc is confined within the torch. A plasma is formed in helium by a dc arc. A small amount of O2 is injected downstream from the arc where it is thermally dissociated by the hot He into oxygen atoms. The high temperature and isentropic expansion give the oxygen atoms their velocity. Using seeded beam techniques, oxygen atom beams of approximately 3.5 and approximately 1.5 km/sec, respectively, are obtained.

Arnold, G. S.↗

NASA NTRS1981

On the distribution of noble gases in Allende - A differential oxidation study

The investigation makes use of an oxidizing technique which is based on methods widely employed in light stable isotope analysis. The utilization of closed-system differential combustion in molecular oxygen in an ultra-high vacuum system on-line with a spectrometer makes it possible to conduct precise abundance and isotopic measurements of all gases released in progressive oxidation and/or thermal outgassing of the host phases. Attention is given to the noble gases mobilized in progressive oxidation of a carbon-rich acid residue and a fine-grained matrix separate. The progressive oxidation of the Allende matrix is discussed. Release occurred over three distinct intervals, characterized by oxidation below 600 C, gas mobilization between 630 and 750 C, and high-temperature diffusive release.

Frick, U.↗

NASA NTRS1988

Advanced infrared astronomy

This task supports the application of infrared heterodyne and Fourier transform spectroscopy to ultra-high resolution studies of molecular constituents of planetary astomspheres and cometary comae. High spectral and spatial resolutions are especially useful for detection and study of localized, non-thermal phenomena in low temperature and low density regions, for detection of trace constituents and for measurement of winds and dynamical phenomena such as thermal tides. Measurement and analysis of individual spectial lines permits retrieval of atmospheric molecular abundances and temperatures and thus, information on local photochemical processes. Determination of absolute line positions to better than 10 to the minus eighth power permits direct measurements of gas velocity to a few meters/sec. Observations are made from ground based heterodyne spectrometers at the Kitt Peak McMath solar telescope and from the NASA infrared Telescope Facility on Mauna Kea, Hawaii. Wind velocities at 110km altitude on Venus were extracted approximately 1 m/sec from measurements of non-thermal emission cores of 10.3 micron CO2 lines. Results indicate a subsolar to antisolar circulationwith a small zonal retrograde component.

Kostiuk, T.↗

NASA NTRS1990

Structure and properties during aging of an ultra-high strength Al-Cu-Li-Ag-Mg alloy

The structure and properties of the strengthening phases formed during aging in an Al-Cu-Li-Ag-Mg alloy (Weldalite 049) were elulcidated, by following the development of the microstructure by means of TEM. The results of observations showed that the Weldalite 049 alloy has a series of unusual and technologically useful combinations of mechanical properties in different aging conditions, such as natural aging without prior cold work to produce high strengths, a reversion temper of lower yield strength and unusually high ductility, a room temperature reaging of the reversion temper eventually leading to the original T4 hardness, and ultrahigh-strength T6 properties.

Gayle, Frank W.↗

NASA NTRS1991

Advanced infrared astronomy

This task supports the application of infrared heterodyne spectroscopy and other high resolution techniques, as well as infrared arrays to ultra-high resolution studies of molecular constituents of planetary atmospheres. High spectral and spatial resolution measurement and analysis of individual spectral lines permits the retrieval of distributions of atmospheric molecular abundances and temperatures and thus, information on local photochemical processes. Determination of absolute line positions to better than 10(exp -8) permits direct measurement of gas velocities to a few m/sec and thus, the study of dynamics. Observations are made from ground based observatories.

Kostiuk, Theodor↗

NASA NTRS1993

Status of local oscillators for operating ultra-high resolution frequency discriminators as frequency standards

The operation of new improved frequency standards based on new ultra-high-resolution frequency discriminators requires high stability local, or 'flywheel' oscillators. We review the spectral density of phase fluctuations of existing flywheel oscillators and the related time domain frequency stability of new and proposed cryogenically cooled oscillators suitable for this application. Presently used devices include the quartz crystal oscillator, the room-temperature actively oscillating atomic hydrogen (H) maser, and the superconducting maser oscillator. Future devices include the cryogenic H-maser and other cryogenic devices using resonators of superconducting metal or solid crystalline sapphire. The relation of the phase spectral density of these devices to the characteristics of present and proposed frequency discriminators based on trapped cooled ions and cold atoms is discussed in terms of their operation as frequency standards.

Vessot, R. F. C.↗