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NASA NTRS1986

Outgassing measurement of the aluminum alloy UHV chamber

A large vacuum chamber (580 mm diameter) was fabricated from an aluminum alloy surface treated by a special process normally used on small chambers. The chamber was tested unbaked and baked at various temperatures, pressures, and holding periods. The chamber was filled with N2 gas, and the outgassing rate was measured after one hour. Then the ultimate pressure was measured. Outgassing rates for baked and unbaked groups were compared. It is concluded that the same surface treatment technique can be used on both large and small chambers produced by the same special extrusion process.

Miyamoto, M.↗

NASA NTRS1998

Flow Characteristics of UHV Nitrogen Arcjet

Flow characteristics in the nozzle of a nitrogen arcjet have been simulated by a model. Electrons, ions, and neutral atoms and molecules are represented as separate species. Dissociation, ionization, and recombination are treated as separate reactions. Thermal non-equilibrium is represented by a two-temperature model. Energy input to plasma from the arc is modeled as a source determined by local current and electrical conductivity. Momentum and energy losses and recombinations at the nozzle wall are included as source/sink determined by fluxes to the wall. The results show essentially frozen gas-phase reactions and thermal nonequilibrium due to Joule heating of electrons and in the expansion part of the nozzle. Wall interactions have strong effects on the results, indicating that they play important roles in the flow due to very high surface area relative to the volume of the plasma. For example, plasma velocity decreases from 6000 m per s without wall interactions to 3000 m per s with modest amount of wall interactions. These results also show reasonable agreement with optical emission measurements, which confirms that the arcjet plasma is far from LTE. The spectra suggest nitrogen dissociation levels of 0.3% - 9%, depending on nitrogen flow rate and arc plasma current, which also determine the relative amounts of excited atomic and molecular nitrogen. Langmuir probe studies of the source show that electron and ion fluxes increase with increasing power, and that the ion energy distribution shifts to lower energies. Typical ion fluxes were on the order of 4E-9 A/cm**2 with a maximum ion kinetic energy of 3.5eV. The median electron energy was 1eV, with a maximum of less than 4eV.

Chang, C. H.↗

DOE OSTI2021

Examining Perceptual Luminance Uniformity of Simulated Luminaire Patterns

Luminaire luminance uniformity is an important aspect that can affect perceived lighting quality, discomfort glare, and efficacy. While several metrics have been proposed to characterize luminance uniformity, previous studies have shown that current metrics such as Max:Min or Avg:Min luminance ratios can be insensitive to important differences in luminance gradient that may affect perceived uniformity. In an attempt to resolve this issue, previous studies incorporated a contrast sensitivity function for the human eye based on spatial frequency, such as in the UHVS metric; however, this metric has not been comprehensively studied in relation to perceived uniformity ratings. The study presented in this paper aimed to examine the relationship between the UHVS metric and perceived uniformity ratings. Specifically, the study used a web-based questionnaire that presented simulated luminance patterns and asked participants to assess uniformity using a two-alternative forced-choice procedure. Responses were collected and analyzed from 94 participants. The results showed a significant correlation and relationship between the UHVS metric and perceived uniformity. However, comparisons between patterns that had similar UHVS and between patterns that had larger differences in UHVS did not yield consistent results. These results suggest that the UHVS metric might be used for general guidance but may warrant further studies to better understand its sensitivity and improve its alignment with perceived uniformity ratings.

Abboushi, Belal K.↗

DOE OSTI2020

A modular ultra-high vacuum millikelvin scanning tunneling microscope

We describe the design, construction, and performance of an ultra-high vacuum (UHV) scanning tunneling microscope (STM) capable of imaging at dilution-refrigerator temperatures and equipped with a vector magnet. The primary objective of our design is to achieve a high level of modularity by partitioning the STM system into a set of easily separable, interchangeable components. This naturally segregates the UHV needs of STM instrumentation from the typically non-UHV construction of a dilution refrigerator, facilitating the usage of non-UHV materials while maintaining a fully bakeable UHV chamber that houses the STM. Here, the modular design also permits speedy removal of the microscope head from the rest of the system, allowing for repairs, modifications, and even replacement of the entire microscope head to be made at any time without warming the cryostat or compromising the vacuum. Without using cryogenic filters, we measured an electron temperature of 184 mK on a superconducting Al(100) single crystal.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

The stability of Cl-, Br-, and I-passivated Si(100)-(2 × 1) in ambient environments for atomically-precise pattern preservation

Abstract Atomic precision advanced manufacturing (APAM) leverages the highly reactive nature of Si dangling bonds relative to H- or Cl-passivated Si to selectively adsorb precursor molecules into lithographically defined areas with sub-nanometer resolution. Due to the high reactivity of dangling bonds, this process is confined to ultra-high vacuum (UHV) environments, which currently limits its commercialization and broad-based appeal. In this work, we explore the use of halogen adatoms to preserve APAM-derived lithographic patterns outside of UHV to enable facile transfer into real-world commercial processes. Specifically, we examine the stability of H-, Cl-, Br-, and I-passivated Si(100) in inert N 2 and ambient environments. Characterization with scanning tunneling microscopy and x-ray photoelectron spectroscopy (XPS) confirmed that each of the fully passivated surfaces were resistant to oxidation in 1 atm of N 2 for up to 44 h. Varying levels of surface degradation and contamination were observed upon exposure to the laboratory ambient environment. Characterization by ex situ XPS after ambient exposures ranging from 15 min to 8 h indicated the Br– and I–passivated Si surfaces were highly resistant to degradation, while Cl–passivated Si showed signs of oxidation within minutes of ambient exposure. As a proof-of-principle demonstration of pattern preservation, a H–passivated Si sample patterned and passivated with independent Cl, Br, I, and bare Si regions was shown to maintain its integrity in all but the bare Si region post-exposure to an N 2 environment. The successful demonstration of the preservation of APAM patterns outside of UHV environments opens new possibilities for transporting atomically-precise devices outside of UHV for integrating with non-UHV processes, such as other chemistries and commercial semiconductor device processes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

NASA NTRS1991

The Nickel(111)/Alkaline Electrolyte Interface

The electrochemical properties of Ni (111) prepared and characterized in ultra high vacuum, UHV, by surface analytical techniques have been examined in alkaline media by cyclic voltammetry using an UHV-electrochemical cell transfer system designed and built in this laboratory. Prior to the transfer, the Ni(111) surfaces were exposed to saturation coverages of CO in UHV in an attempt to protect the surface from possible contamination with other gases during the transfer. Temperature Programmed Desorption, TPD, of CO-dosed Ni (111) surfaces displaying sharp c(4x2), LEED patterns, subsequently exposed to water-saturated Ar at atmospheric pressure in an auxiliary UHV compatible chamber and finally transferred back to the main UHV chamber, yielded CO2 and water as the only detectable products. This indicates that the CO-dosed surfaces react with water and/or bicarbonate and hydroxide as the most likely products. Based on the integration of the TPD peaks, the combined amounts of H2O and CO2 were found to be on the order of a single monolayer. The reacted c(4x2)CO/Ni(111) layer seems to protect the surface from undergoing spontaneous oxidation in strongly alkaline solutions. This was evidenced by the fact that the open circuit potential observed immediately after contact with deaerated 0.1 M KOH was about 0.38 V vs. DHE, drifting slightly towards more negative values prior to initiating the voltametric scans. The average ratio of the integrated charge obtained in the first positive linear scan in the range of 0.35 to 1.5 V vs. DHE (initiated at the open circuit potential) and the first (and subsequent) linear negative scans in the same solution yielded for various independent runs a value of 3.5 +/- 0.3. Coulometric analysis of the cyclic voltammetry curves indicate that the electrochemically formed oxyhydroxide layer involves a charge equivalent to 3.2 +/- 0.4 layers of Ni metal.

Wang, Kuilong↗

NASA NTRS1989

Method for producing an atomic oxygen beam

A method for producing an atomic oxygen beam is provided by the present invention. First, a material 10' is provided which dissociates molecular oxygen and dissolves atomic oxygen into its bulk. Next, molecular oxygen is exposed to entrance surface 11' of material 10'. Next, material 10' is heated by heater 17' to facilitate the permeation of atomic oxygen through material 10' to the UHV side 12'. UHV side 12' is interfaced with an ultra-high vacuum (UHV) environment provided by UHV pump 15'. The atomic oxygen on the UHV side 12' is excited to a non-binding state by exciter 14' thus producing the release of atomic oxygen to form an atomic oxygen beam 35'.

Outlaw, Ronald A.↗

DOE OSTI2025

A rotor-based multileaf collimator for beam shaping

We introduce a new style of multileaf collimator which employs rotors with angularly dependent radius to control the masking aperture: a rotor-based multileaf collimator (RMLC). Using a padlock-inspired mechanism, a single motor can set dozens of rotors, i.e. leaves, independently. This is especially important for an ultra-high vacuum (UHV) compatible MLC, since this reduces the number of actuators and vacuum feedthroughs required by more than an order of magnitude. This new RMLC will complement previous work employing a UHV compatible MLC with an emittance exchange beamline to create arbitrarily shaped beams on demand. A feed-forward control system which abstracts away the complexity of the RMLC operation, and is adaptable to real beamline conditions, is discussed and demonstrated in simulation.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1996

Scanning Tunneling Microscopy Studies of Diamond Films and Optoelectronic Materials

We present a summary of the research, citations of publications resulting from the research and abstracts of such publications. We have made no inventions in the performance of the work in this project. The main goals of the project were to set up a Chemical Vapor Deposition (CVD) diamond growth system attached to an UltraHigh Vacuum (UHV) atomic resolution Scanning Tunneling Microscopy (STM) system and carry out experiments aimed at studying the properties and growth of diamond films using atomic resolution UHV STM. We successfully achieved these goals. We observed, for the first time, the atomic structure of the surface of CVD grown epitaxial diamond (100) films using UHV STM. We studied the effects of atomic hydrogen on the CVD diamond growth process. We studied the electronic properties of the diamond (100) (2x1) surface, and the effect of alkali metal adsorbates such as Cs on the work function of this surface using UHV STM spectroscopy techniques. We also studied, using STM, new electronic materials such as carbon nanotubes and gold nanostructures. This work resulted in four publications in refereed scientific journals and five publications in refereed conference proceedings.

Perez, Jose M.↗

DOE OSTI2026

Removal of deuterium retained in boron powder by oxygen or high-temperature bakeout

Fuel retention in dust accumulated in fusion devices is a potential operational hazard. Boronization is one of the leading wall-conditioning candidates for future fusion devices. Fuel retention characteristics of boron dust must be studied to accurately understand the potential hazards of boron dust in fusion devices. We evaluated the retention of deuterium (D) in commercially available boron powder as a proxy for tritium retention in boron dust. Diffuse reflectance infrared Fourier transform spectroscopy revealed that boron powder between 300 and 500 K exposed to neutral hydrogen (H 2 ) gas retains H via B-H bonding. We utilized D 2 exposures of 17,400 L on the boron powder, which led to retention on the order of 0.5 g D per 100 kg B or 1.2 g D per m 2 B, as estimated from temperature programmed desorption measurements. We evaluated how powder bakeouts under ultra-high vacuum (UHV), or in an oxygen (O 2 ) or H 2 gas backfilled environment can remove the retained fuel. Bakeouts below 523 K under UHV exhibited poor D removal, promoting recapture of D 2 present as background gas in the chamber. Higher temperature bakeouts led to the removal of over 80% of the retained D within 3 days (623 K) or 1 h (723 K). Bakeouts at 423 K under an O 2 gas environment removed ∼150% more retained D from the boron powder, when compared to bakeouts conducted under UHV. These results suggest that efficient fuel removal from boron dust can be achieved by high-temperature bakeout (>623 K) or by bakeouts at lower temperature (423 K) under an O 2 environment.

Bakeout↗

DOE OSTI2020

Characterizing Complex Gas–Solid Interfaces with in Situ Spectroscopy: Oxygen Adsorption Behavior on Fe–N–C Catalysts

Electrocatalysts for the oxygen reduction reaction within polymer electrolyte membrane fuel cells based on iron, nitrogen, and carbon elements (Fe–N–C) are receiving significant research attention as they offer an inexpensive alternative to catalysts based on platinum-group metals. Although both the performance and the fundamental understanding of Fe–N–C catalysts have improved over the past decade, there remains a need to differentiate the relative activity of different active sites. Toward this goal, our study is focused on characterizing the interactions between O 2 and a set of five structurally different Fe–N–C materials. Detailed characterization of the Fe speciation was performed with 57 Fe Mössbauer spectroscopy and soft X-ray absorption spectroscopy of the Fe L 3,2 -edge, whereas nitrogen chemical states were investigated with X-ray photoelectron spectroscopy (XPS). In addition to initial sXAS and XPS measurements performed in ultra-high vacuum (UHV), measurements were also performed (at the identical location) in an atmosphere of 100 mTorr of O 2 at 80 °C (O 2 -rich). XPS and sXAS results reveal the presence of several types of FeNxCy adsorption sites. FeNxCy sites that are proposed as the most active ones do not show significant change (based on the techniques used in this study) when their environment is changed from UHV to O 2 -rich. Correlation with Mössbauer and sXAS results suggests that this is most likely due to the persistence of strongly adsorbed O 2 molecules from their previous exposure to air. However, other species do show spectroscopic changes from UHV conditions to O 2 -rich. This implies that these sites have a weaker interaction with O 2 that results in their desorption in vacuum conditions and re-adsorption when exposed to the O 2 -rich environment. The nature of these weakly and strongly O 2 -adsorbing FeN x C y sites is discussed in the context of different synthetic and processing parameters employed to fabricate each of these five Fe–N–C materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Controlling Selective C–O and C–H Bond Scission of Methanol by Supporting Pt on TiN and Mo 2 N Model Surfaces and Powder Catalysts

Transition metal nitrides (TMNs) have been explored as effective supports for Pt due to their Pt-like electronic properties. However, there is a lack of fundamental understanding regarding the behavior of Pt on different TMNs (Pt/TMN). Herein two TMNs, Mo 2 N and TiN, were modified with Pt and compared using methanol decomposition as a probe reaction via both ultrahigh vacuum (UHV) studies on thin films and ambient-pressure batch reactor studies of powder catalysts. Temperature-programmed desorption (TPD) and high-resolution electron energy loss spectroscopy (HREELS) measurements were conducted under UHV conditions with Mo 2 N and TiN thin films. Mo 2 N was shown to favor C–H bond scission to form CO with a 56.2% selectivity, while TiN favored C–O bond scission to form CH 4 with a 74.5% selectivity. The addition of 0.9 monolayers (MLs) of Pt increased C–H bond scission selectivity to 89.7% and 49.2% for Mo 2 N and TiN respectively. Density functional theory (DFT) calculations on model surfaces revealed that the binding energy of O (BE *O ) was significantly reduced on Pt/TMNs, from −4.02 eV on Mo 2 N to −1.31 eV on Pt/Mo 2 N and −4.74 eV on TiN to −1.37 eV on Pt/TiN. As a result, C–O bond scission pathways were suppressed, leading to the preferential C–H bond scission that was observed experimentally. The C–O and C–H bond scission trends observed on thin films were then extended to powder catalysts, which demonstrated similar trends toward methanol decomposition. In conclusion, results from the current study establish that by combining UHV studies and DFT calculations over model surfaces, one can effectively predict the catalytic behavior of realistic TMN powder catalysts.

08 HYDROGEN↗

DOE OSTI2025

Pt Particles on a Dynamic TiO 2 Support in Near-Ambient Conditions−Disentangling Size, Pressure, and Support Effects

Platinum particles on reducible oxides are known to form complex and highly dynamic catalyst systems at elevated pressures and temperatures, often adopting active structures that differ from those found at room temperature and under ultrahigh vacuum (UHV). Here, we study the oxidation and structural evolution of subnanometer Pt clusters and nanoparticles supported on rutile TiO 2 (110) across an oxygen pressure range from UHV to 0.1 mbar, using near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS), scanning tunneling microscopy (STM) under UHV and NAP conditions, and low-energy ion scattering (LEIS). Our results reveal distinct differences in oxidation behavior and thermal stability between Pt nanoparticles and clusters, which are further modulated by the support stoichiometry and oxygen pressure. Small Pt clusters become oxidized even at room temperature but are susceptible to accelerated sintering in 0.1 mbar O 2 at elevated temperatures. In contrast, well-crystallized Pt nanoparticles on near-stoichiometric TiO 2 show weaker oxidation. On a reduced, defective TiO 2 support, Pt instead quickly becomes deeply buried by new titania layers, which are formed during support reoxidation. This process appears to result primarily from interactions of the support with the gas phase, unlike the classical, selflimited encapsulation that is induced by the strong metal−support interaction (SMSI). Finally, we address the full complexity of real catalysts in a direct side-by-side comparison of the single-crystalline model system with a Pt-loaded TiO 2 powder catalyst (P25). We conclude that the stoichiometry of the model supports must be carefully chosen and controlled to accurately reproduce the expected state of powder supports during redox reactions.

metal nanoparticles↗

DOE OSTI2024

Cryogen-free modular scanning tunneling microscope operating at 4-K in high magnetic field on a compact ultra-high vacuum platform

One of the daunting challenges in modern low temperature scanning tunneling microscopy (STM) is the difficulty of combining atomic resolution with cryogen-free cooling. Further functionality needs, such as ultra-high vacuum (UHV), high magnetic field (HF), and compatibility with μm-sized samples, pose additional challenges to an already ambitious build. We present the design, construction, and performance of a cryogen-free, UHV, low temperature, and high magnetic field system for modular STM operation. An internal vibration isolator reduces vibrations in this system, allowing for atomic resolution STM imaging while maintaining a low base temperature of ∼4 K and magnetic fields up to 9 T. Samples and tips can be conditioned in situ utilizing a heating stage, an ion sputtering gun, an e-beam evaporator, a tip treater, and sample exfoliation. In situ sample and tip exchange and alignment are performed in a connected UHV room temperature stage with optical access. Multisite operation without breaking vacuum is enabled by a unique quick-connect STM head design. A novel low-profile vertical transfer mechanism permits transferring the STM between room temperature and the low temperature cryostat.

Instruments & Instrumentation↗

DOE OSTI2024

Impact of metal diffusion, lattice distortions, native defects, and ambient on dielectric breakdown in Ni–Ga 2 O 3 Schottky diodes

Ga 2 O 3 unipolar devices are of high interest due to their ~8 MV/cm predicted breakdown fields, which have not yet been achieved due to premature device failure. Pre- and post-failure defect analysis of Ni–Ga 2 O 3 Schottky diodes in ultrahigh vacuum (UHV) and air were performed using depth-resolved cathodoluminescence, high angle annular dark field scanning transmission electron microscopy, and energy dispersive x-ray analysis to understand the physical mechanisms that precede premature breakdown. The breakdown voltage in UHV was dramatically reduced by nearly 40% compared with the breakdown in air. This reduction in the breakdown voltage correlated with post-breakdown differences in Ni distribution, indicating that the coordination and bonding of Ni contribute strongly to electrical behavior in Ni–Ga 2 O 3 Schottky diodes. Breakdown studies in UHV revealed that Ni diffuses away more from the metal–semiconductor interface than with air breakdown, where Ni localizes more near the interface, indicative of the preferential formation of a Ni oxide under O-poor conditions. These measurements also identified the formation of divacancy-interstitial complexes and their characteristic luminescence signature ~150 nm from the interface, the densities of which correlated with breakdown fields. These findings show that electric-field-induced degradation occurs via the rearrangement of native point defects, which act as an additional precursor to device failure. Macroscopically, they show the impact of both vacuum conditions and metal reactivity on Ga 2 O 3 device fabrication.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Deployable Element Ultra-High Vacuum Pump

Advancing Ultra High Vacuum (UHV) Pumping Technology: The deployable UHV pump team has designed a theoretical model to boost efficiency in high vacuum environments. Traditional systems face challenges with random molecular motion. The innovative windmill design, using titanium sublimation technology, reduces randomness by deploying a gettering surface that actively captures particles. This marks a notable advancement in UHV pumping technology.

43 PARTICLE ACCELERATORS↗

NASA NTRS1975

Surface friction of rock in terrestrial and simulated lunar environments

The conventional probe-on-the rotating-disk concept was used to determine the surface friction in mineral probe/specimen interfaces. Nine rocks or minerals and two stainless steels were tested in both new (NT) and same track (ST) tests under three different pressure environments-atmospheric, UHV, and dry nitrogen. Each environment was further subdivided into two testing conditions, that is, ambient and elevated (135 C) temperatures. In NT tests, friction was the lowest in an atmospheric pressure condition for all rock types and increased to the largest in UHV ambient condition except for pyroxene and stainless steel. Friction values measured in dry nitrogen ambient condition lie between the two extremes. Heating tends to increase friction in atmospheric and dry nitrogen environment but decreases in UHV environment with the exception of stainless steel, basalt, and pyroxene. In ST tests, friction was the lowest in the first run and increased in subsequent runs except for stainless steel where the reverse was true. The increases leveled off after a few runs ranging from the second to the seventh depending on rock types.

Roepke, W. W.↗

NASA NTRS1993

Hyperthermal-Atomic-Oxygen Generator

Small hyperthermal-atomic-oxygen generator (HAOG) compatible with ultrahigh vacuum (UHV) developed. Provides pure flux of ground-state oxygen atoms with mean kinetic energy of approximately 5 eV, accurately simulating conditions in low orbit around Earth, and mounted on any existing UHV processing or analysis system. HAOG clean and compatible with other UHV processing or diagnostic systems and relatively inexpensive and simple to operate. Valuable in studies involving atomic oxygen because added easily to existing systems.

Outlaw, R. A.↗