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DOE OSTI2024

Systematic improvements in transmon qubit coherence enabled by niobium surface encapsulation

Abstract We present a transmon qubit fabrication technique that yields systematic improvements in T 1 relaxation times. We encapsulate the surface of niobium and prevent the formation of its lossy surface oxide. By maintaining the same superconducting metal and only varying the surface, this comparative investigation examining different capping materials, such as tantalum, aluminum, titanium nitride, and gold, as well as substrates across different qubit foundries demonstrates the detrimental impact that niobium oxides have on coherence times of superconducting qubits, compared to native oxides of tantalum, aluminum or titanium nitride. Our surface-encapsulated niobium qubit devices exhibit T 1 relaxation times 2–5 times longer than baseline qubit devices with native niobium oxides. When capping niobium with tantalum, we obtain median qubit lifetimes above 300 μs, with maximum values up to 600 μs. Our comparative structural and chemical analysis provides insight into why amorphous niobium oxides may induce higher losses compared to other amorphous oxides.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Hydrogen in disordered titania: connecting local chemistry, structure, and stoichiometry through accelerated exploration

Hydrogen incorporation in native surface oxides of metal alloys often controls the onset of metal hydriding, with implications for materials corrosion and hydrogen storage. A key representative example is titania, which forms as a passivating layer on a variety of titanium alloys for structural and functional applications. These oxides tend to be structurally diverse, featuring polymorphic phases, grain boundaries, and amorphous regions that generate a disparate set of unique local environments for hydrogen. Here, we introduce a workflow that can efficiently and accurately navigate this complexity. First, a machine learning force field, trained on ab initio molecular dynamics simulations, was used to generate amorphous configurations. Density functional theory calculations were then performed on these structures to identify local oxygen environments, which were compared against experimental observations. Second, to classify subtle differences across the disordered configuration space, we employ a graph-based sampling procedure. Finally, local hydrogen binding energies and hopping kinetics are computed using exhaustive density functional theory calculations on representative configurations. Here, we leverage this methodology to show that hydrogen binding energetics are described by local oxygen coordination, which in turn is affected by stoichiometry, and form the basis of hopping kinetics and diffusion. Together these results imply that hydrogen incorporation and transport in TiO x can be tailored through compositional engineering, with implications for improving the performance and durability of titanium-derived alloys in hydrogen environments.

36 MATERIALS SCIENCE↗

NASA NTRS2005

Oxide Ceramic Films Grown on 60 Nitinol for NASA and Department of Defense Applications

Both the NASA Glenn Research Center and the U.S. Army Research Laboratory, Development and Engineering Center (ARDEC) have worked to develop oxide ceramic films grown on 60 nitinol (60-wt% nickel and 40-wt% titanium) to decrease friction and increase wear resistance under unlubricated conditions. In general, oxide and nonoxide ceramic films have unique capabilities as mechanical-, chemical-, and thermal-barrier materials in diverse applications, including high-temperature bearings and gas bearings requiring low friction, wear resistance, and chemical stability. All oxide ceramic films grown on 60 nitinol were furnished by ARDEC, and materials and surface characterization and tribological experiments were conducted at Glenn.

Miyoshi, Kazuhisa↗

NASA NTRS1976

Material development aspects of an oxidation protection system for a reinforced carbon-carbon composite

The paper describes the procedures which led to selection of a diffusion-coated siliconized oxidation-resistant reinforced carbon-carbon composite as a candidate for use in the leading edge structure of the Space Shuttle for the purpose of providing thermal protection. Materials were evaluated on the basis of oxidation-inhibitor performance, strength properties, and fabricability. Compounds of titanium, tantalum, zirconium, silicon, hafnium, aluminum, and boron were compounded with the reinforced carbon-carbon material in two different processing techniques to discover an oxidation-inhibited system which provided multicycle protection at temperatures up to 4000 F. Details of the manufacture and testing of the reinforced carbon-carbon composites are provided.

Rogers, D. C.↗

NASA NTRS1990

Oxidation characteristics of Ti-25Al-10Nb-3V-1Mo intermetallic alloy

Static oxidation kinetics of the super-alpha 2 titanium-aluminide alloy Ti-25Al-10Nb-3V-1Mo (at. percent) were investigated in air over the temperature range of 650 to 1000 C using thermogravimetric analysis. The oxidation kinetics were complex at all exposure temperatures and displayed up to three distinct oxidation rates. Breakaway oxidation occurred after long exposure times at high temperatures. Oxidation products were determined using x ray diffraction techniques, electron microprobe analysis, and energy dispersive x ray analysis. Oxide scale morphology was examined by scanning electron microscopy of the surfaces and cross sections of oxidized specimens. The oxides during the parabolic stages were compact and multilayered, consisting primarily of TiO2 doped with Nb, a top layer of Al2O3, and a thin bottom layer of TiN. The transition between the second and third parabolic stage was found to be linked to the formation of a TiAl layer at the oxide-metal interface. Porosity was formed during the third stage, causing degradation of the oxide and the beginning of breakaway oxidation.

Wallace, Terryl A.↗

NASA NTRS1992

Oxidation characteristics of Ti-25Al-10Nb-3V-1Mo

Static oxidation kinetics of the super-alpha 2 titanium-aluminide alloy Ti-25Al-10Nb-3V-1Mo (at. percent) were investigated in air over the temperature range of 650 to 1000 C using thermogravimetric analysis. The oxidation kinetics were complex at all exposure temperatures and displayed up to three distinct oxidation rates. Breakaway oxidation occurred after long exposure times at high temperatures. Oxidation products were determined using X-ray diffraction techniques, electron microprobe analysis, and energy dispersive X-ray analysis. Oxide scale morphology was examined by scanning electron microscopy of the surfaces and cross sections of oxidized specimens. The oxides during the parabolic stages were compact and multilayered, consisting primarily of TiO2 doped with Nb, a top layer of Al2O3, and a thin bottom layer of TiN. The transition between the second and third parabolic stage was found to be linked to the formation of a TiAl layer at the oxide-metal interface. Porosity was formed during the third stage, causing degradation of the oxide and the beginning of breakaway oxidation.

Wallace, T. A.↗

DOE OSTI2021

Methods of producing a titanium alloy product

A method for producing a particulate titanium alloy product can include preparing a composite particulate oxide mixture with TiO2 powder and at least one alloying element powder. The composite particulate oxide mixture can be co-reduced using a metallic reducing agent under a hydrogen atmosphere at a reduction temperature for a reduction time sufficient to produce a hydrogenated titanium alloy product. The hydrogenated titanium alloy product can then be heat treated under a hydrogen atmosphere and a heat treating temperature to reduce pore size and specific surface area to form a heat treated hydrogenated titanium product. The heat treated hydrogenated titanium product can be deoxygenated to reduce residual oxygen to less than 0.2 wt % to form a deoxygenated hydrogenated titanium product as a particulate. The deoxygenated hydrogenated titanium product can optionally be dehydrogenated to form the titanium alloy product as a particulate.

Fang, Zhigang Zak↗

NASA NTRS1980

The role of oxidation in the fretting wear process

Fretting experiments were conducted on titanium, a series of Ni-Cr-Al alloys and on some high temperature turbine alloys at room temperature and at elevated temperatures in air and in various inert environments. It was found that, depending on temperature and environment, the fretting behavior of the materials examined could be classified according to four general types of behavior. Briefly, these types of behavior were: (1) the complete absence of oxidation, as in inert environments, generally leading to low rates of fretting wear but high fretting friction; (2) gradual attrition of surface oxide with each fretting stroke, found in these experiments to operate in concert with other dominating mechanisms; (3) rapid oxidation at surface fatigue damage sites, resulting in undermining and rapid disintegration of the load bearing surface; and (4) the formation of coherent, protective oxide film, resulting in low rates of fretting wear. An analytical model predicting conditions favorable to the fourth type of behavior was outlined.

Bill, R. C.↗

NASA NTRS1979

Adherence of sputtered titanium carbides

Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited, in practice, by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium based alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.

Brainard, W. A.↗

NASA NTRS1980

Improved adhesion of sputtered refractory carbides to metal substrates

Sputtered coatings of the refractory metal carbides are of great interest for applications where hard wear-resistant materials are desired. The usefulness of sputtered refractory carbides is often limited in practice by spalling or interfacial separation. In this work improvements in the adherence of refractory carbides on iron, nickel and titanium base alloys were obtained by using oxidation, reactive sputtering or sputtered interlayers to alter the coating-substrate interfacial region. X-ray photoelectron spectroscopy and argon ion etching were used to characterize the interfacial regions, and an attempt was made to correlate adherence as measured in wear tests with the chemical nature of the interface.

Wheeler, D. R.↗

NASA NTRS1980

Gas phase hydrogen permeation in alpha titanium and carbon steels

Commercially pure titanium and heats of Armco ingot iron and steels containing from 0.008-1.23 w/oC were annealed or normalized and machined into hollow cylinders. Coefficients of diffusion for alpha-Ti and alpha-Fe were determined by the lag-time technique. Steady state permeation experiments yield first power pressure dependence for alpha-Ti and Sievert's law square root dependence for Armco iron and carbon steels. As in the case of diffusion, permeation data confirm that alpha-titanium is subject to at least partial phase boundary reaction control while the steels are purely diffusion controlled. The permeation rate in steels also decreases as the carbon content increases. As a consequence of Sievert's law, the computed hydrogen solubility decreases as the carbon content increases. This decreases in explained in terms of hydrogen trapping at carbide interfaces. Oxidizing and nitriding the surfaces of alpha-titanium membranes result in a decrease in the permeation rate for such treatment on the gas inlet surfaces but resulted in a slight increase in the rate for such treatment on the gas outlet surfaces. This is explained in terms of a discontinuous TiH2 layer.

Johnson, D. L.↗

DOE OSTI2021

Understanding the TiH (2-x) /TiO y System at Elevated Temperature: A Literature Review

Titanium hydride of varying TiH stoichiometry is used in pyrotechnic compositions. In order to yield consistent performance, manufacturing processes must be developed to ensure precise and reproducible material properties, including composition and morphology. Legacy synthesis protocols are not comprehensive nor are the required apparatuses still available. To guide the development of novel production procedures, this report reviews literature on relevant chemical reactions and diffusion events occurring at elevated temperature in the TiH (2-x) /TiO y system. Titanium hydride exposed to air spontaneously forms a passivating oxide layer. Upon heating, significant hydrogen release, which is accompanied by changes to the surface oxide layer, is noted by 375–400°C. At higher temperatures (above about 500°C) the oxide layer is reported to be essentially nonexistent as a result of oxide-layer dissolution processes and, potentially, oxide-layer reduction due to water formation. Based on the reviewed literature, we hypothesize that, by 500°C, the surface layer consists of an oxyhydride phase, which is a solid solution of oxygen in titanium hydride. We believe that hydrogen release from titanium hydride is controlled by the kinetics of molecular hydrogen desorption on the oxyhydride surface. No literature data is available for corresponding activation energies of the dynamic desorption process, and the equilibrium phase diagram of this three-component system remains largely unexplored as well. These gaps in knowledge might be addressed through coordinated computational modeling and experimental efforts.

36 MATERIALS SCIENCE↗

NASA NTRS2003

Modeling of High-Strain-Rate Deformation, Fracture, and Impact Behavior of Advanced Gas Turbine Engine Materials at Low and Elevated Temperatures

Gamma titanium aluminides have received considerable attention over the last decade. These alloys are known to have low density, good high temperature strength retention, and good oxidation and corrosion resistance. However, poor ductility and low fracture toughness have been the key limiting factors in the full utilization of these alloys. More recently, Gamma-met PX has been developed by GKSS, Germany. These alloys have been observed to have superior strengths at elevated temperatures and quasi-static deformation rates and good oxidation resistance at elevated temperatures when compared with other gamma titanium aluminides. The present paper discusses results of a study to understand dynamic response of gamma-met PX in uniaxial compression. The experiments were conducted by using a modified split Hopkinson pressure bar between room temperature and 900 C and strain rates of up to 3500 per second. The Gamma met PX alloy showed superior strength when compared to nickel based superalloys and other gamma titanium aluminides at all test temperatures. It also showed strain and strain-rate hardening at all levels of strain rates and temperatures and without yield anomaly up to 900 C. After approximately 600 C, thermal softening is observed at all strain rates with the rate of thermal softening increasing dramatically between 800 and 900 C. However, these flow stress levels are comparatively higher in Gamma met PX than those observed for other TiAl alloys.

Shazly, Mostafa↗

DOE OSTI2025

Imaging and speciation of intracellular metallic implant debris using synchrotron-based X-ray fluorescence micro-spectroscopy: a study of two cases

Debris generated from total hip arthroplasty (THA) components made from metal alloys can cause, in some cases, inflammatory cell (e.g., macrophages) responses that lead to adverse local tissue reactions (ALTR) and implant failure. The lack of information on intracellular chemical alterations of metal debris has hindered the understanding of the pathogenesis of ALTR. The goal of this study was to characterize intracellular debris within macrophages using Synchrotron imaging and spectroscopy. We studied periprosthetic tissues of two retrieved THAs with (1) a metal-on-metal (MoM) articulation and (2) a metal-on-polyethylene (MoP) articulation exhibiting corrosion of the metal femoral head. The MoM-THA exhibited different valence states of chromium- and cobalt-containing debris, suggesting three different moieties: Cr 2 O 3 , CrPO 4 , and an alloy-oxide mixture. The findings further suggest that Cr 2 O 3 formed in the tribological interfaces of the implant, while CrPO 4 is a by-product of the phagocytosis process of cobalt alloy-containing debris. Titanium debris appeared to occur in a mixed crystalline/amorphous oxide state. It remains unclear if this chemical state results from the tribochemical processes at the implant surface or intracellular alterations. The MoP-THA specimen exhibited no intracellular particulate debris associated with macrohpages, indicating that the ALTR may be entirely triggered by metal ionic species in this case. A better understanding of in vivo chemical alteration of implant debris will aid in assessing the risk for ALTR during implant design and material choice. However, various techniques are needed to accurately determine the interaction between metal particles and the inta- and extra-cellular environment.

60 APPLIED LIFE SCIENCES↗

NASA NTRS1983

Residual mechanical properties of Ti-6Al-4V after simulated Space Shuttle reentry

Oxidation and embrittlement are concerns in use of titanium foils for shielding advanced space transportation system vehicles during Earth reentry. Ti-6Al-4V in 0.003 in. and 0.035 in. thicknesses were exposed to multiple cycles of simulated space transportation system ascent/reentry conditions at temperatures ranging from 1000 F to 1200 F. Residual mechanical tests and metallurgical analyses were made on the specimens after exposure. Results show that tensile elongation is the mechanical property most affected by the reentry environment. Results are presented to show a comparison of residual properties of foil specimens from static oxidation exposure and cyclic oxidation exposure.

Clark, R. K.↗

NASA NTRS1985

Residual mechanical properties of Ti-6Al-2Sn-4Zr-2Mo after simulated Space Shuttle reentry

Oxidation and embrittlement are concerns in use of titanium foils for shielding advanced space transportation system vehicles during earth reentry. Ti-6Al-4V in 0.003 in. and 0.035 in. thicknesses were exposed to multiple cycles of simulated space transportation system ascent/reentry conditions at temperatures ranging from 1000 F to 1200 F. Residual mechanical tests and metallurgical analyses were made on the specimens after exposure. Results show that tensile elongation is the mechanical property most affected by the reentry environment. Results are presented to show a comparison of residual properties of foil specimens from static oxidation exposure and cyclic oxidation exposure.

Clark, R. K.↗

DOE OSTI2026

High-throughput oxidation screening and down-selection of refractory high entropy alloys in the Al-Cr-Mo-Nb-Ta-Ti system

Rapid experimentation and characterization are ever-present needs in the discovery of high entropy alloys. High entropy alloy systems are difficult to survey with systematic composition sweeps using traditional synthesis methods. The number of distinct compositions in even a four-element system is experimentally intractable. Exploration of these, and higher-element systems, necessitates thermodynamic prediction coupled with an automated sample creation method and a rapid screening methodology to effectively down-select alloys with targeted properties. As a result, a high-throughput method for evaluating the oxidation performance of refractory high entropy alloys was developed and tested. The six-element system of aluminum, chromium, molybdenum, niobium, tantalum, and titanium was evaluated for single phase stability and short-duration oxidation resistance. Target compositions were initially determined via thermodynamic predictions of single-phase stability across a wide temperature range. A twenty-five-sample build plate was produced using directed energy deposition additive manufacturing. After fabrication, the twenty-five 1 cm 3 samples were heat treated and characterized for composition and phase identification. The build plate was exposed to a high temperature oxidizing environment at 1000 °C for three hours. After oxidation, the composition, morphology, and chemistry of the oxides formed were characterized. Of the twenty-five samples produced, nine exhibited a favorable oxidation response, from which a single-phase BCC alloy at a composition of Al 13 Cr 7 Mo 19 Nb 18 Ta 26 Ti 17 was identified as the alloy with the most protective oxidation coating with a thin, adherent oxide scale. Finally, the complete experimental down-selection—from machine setup to final alloy identification—required approximately 45 labor hours, demonstrating a rapid validation for alloy discovery.

Additive manufacturing↗

DOE OSTI2024

Acoustic and electrical properties of Fe-Ti oxides with application to the deep lunar mantle

The overturn of titanium-rich mantle cumulates has been invoked to explain the structure and dynamics of the Moon. These dense cumulates are stable at the core-mantle boundary (CMB) and could explain field observations inferred from geophysical studies. Here, we report acoustic and electrical experiments on natural ilmenite-rutile aggregates up to 4.5 GPa and 1920 K. Seismic velocities show a weak pressure and temperature dependence, with Vs ~ 4.2 (+/-0.2) km/s and Vp ~8.0 (+/-0.2) km/s at the CMB conditions. Conductivity increases by a factor of 10 4 from 373 to 1920 K and is >10(3) S/m above 1573 K. Seismic and electrical models for the lunar mantle based on our results, considering mixtures of Fe-Ti oxides and olivine, indicate that field velocity and conductivity estimates are reproduced satisfactorily with 3-16 vol.% Fe-Ti oxides and 20 vol.% melt. Interactions between a Ti-rich, melt-bearing layer and the adjacent core likely affect the cooling and magnetic history of the Moon.

58 GEOSCIENCES↗