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At least 991 records · Page 55
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

An automatic multi-precursor flow-type atomic layer deposition system

Designs for two automated atomic layer deposition (ALD) flow reactors are presented, and their capabilities for coating additively manufactured (AM) metal prints are described. One instrument allows the coating of several AM parts in batches, while the other is useful for single part experiments. To demonstrate reactor capabilities, alumina (Al 2 O 3 ) was deposited onto AM 316L stainless steel by dosing with water (H 2 O) vapor and trimethylaluminum (TMA) and purging with nitrogen gas (N 2 ). Both instruments are controlled by custom-programmed LabVIEW software that enables in situ logging of temperature, total pressure, and film thickness using a quartz crystal microbalance. An initial result shows that 150 ALD cycles led to a film thickness of ~55 nm, which was verified with Rutherford backscattering spectroscopy. This indicates that the reactors were indeed depositing single atomic layers of Al 2 O 3 per ALD cycle, as intended.

47 OTHER INSTRUMENTATION↗
NASA NTRS1994

Metafusion: A breakthrough in metallurgy

The Metafuse Process is a patented development in the field of thin film coatings utilizing cold fusion which results in a true inter-dispersion of dissimilar materials along a gradual transition gradient through a boundary of several hundred atomic layers. The process is performed at ambient temperatures and pressures requiring relatively little energy and creating little or no heat. The process permits a remarkable range of material combinations and joining of materials which are normally incompatible. Initial applications include titanium carbide into and onto the copper resistance welding electrodes and tungsten carbide onto the cutting edges of tool steel blades. The process is achieved through application of an RF signal of low power and is based on the theory of vacancy fusion.

Joseph, Adrian A.↗
NASA NTRS2000

Scattering/Transmission of Energetic H+,He+, and O+ Through a Thin Composite Si/Lexan/C Foil

The need for a thin foil to serve both as an extreme ultraviolet (EUV) radiation attenuator and as a secondary electron generator for time-of-flight (TOF) instruments and energetic neutral atom (ENA) imagers has led us to test the scattering and transmission characteristics of a layered foil of nominal aerial thicknesses of 5 micrograms (raised dot) per square centimeter Si, 4 micrograms (raised dot) per square centimeter Lexan (C16H14O3), and 1 microgram (raised dot) per square centimeter C. We report the scattering/transmission results of subjecting this foil to H(+), He(+), and O(+) beams of energies less than or equal to 120 keV. The scattering of these particles, defined by the half-angular-width at half-maximum (HWHM), decreases with increasing energy and found to be 10 degrees for 10 keV H(+), 22 keV for He(+), and 100 keV for O(+). The 50% transmission threshold for these particles was found to be 3.9 keV for H(+), 8.6 keV for He(+), and 49.5 keV for O(+). Computer simulations of H(+)-foil interactions using SRIM96 agree well with the H(+) data, while yielding less scattering and higher transmission than indicated by the O(+) data.

Adrian, M. L.↗
NASA NTRS2000

Scattering/Transmission of Energetic H(sup +), He(sup +), and O(sup +) Through a Thin Composite Si/Lexan/C Foil

The need for a thin foil to serve both as an extreme ultraviolet (EUV) radiation attenuator and as a secondary electron generator for time-of-flight (TOF) instruments and energetic neutral atom (ENA) imagers has led us to test the scattering and transmission characteristics of a layered foil of nominal aerial thicknesses of 5 microns/sq cm Si, 4 microns/sq.cm Lexan ((C16)H(14)O3), and 1 micron/sq.cm C. We report the scattering and transmission results of subjecting this foil to H(sup +), He(sup +), and O(sup +) beams of energy less than 120 keV. The scattering of these particles, defined by the half-angular-width at half-maximum (HWHM), decreases with increasing energy and is found to be 10 deg for 10 keV H(sup +), 22 keV for He(sup +), and 100 keV for O(sup +). The 50% transmission threshold for these particles was found to be 3.9 keV for H(sup +), 8.6 keV for He(sup +), and 49.5 keV for O(sup +). Additionally, ion transmission shows evidence of resonance scattering from a rectangular potential independent of incident ion mass. Particularly evident is a local transmission minimum at 70 keV possessing a Gaussian-width of 20 keV. For incident energies below 50 keV, computer simulations of H+-foil interactions using SRIM96 agree well with the H(sup +) data, while yielding less scattering and higher transmission than indicated by the O(sup +) data.

Adrian, M. L.↗
NASA NTRS1996

Transparent, Conductive Coatings Developed for Arc-Proof Solar Arrays

Transparent, conductive thin-film coatings have many potential applications where a surface must be able to dissipate electrical charges without sacrificing its optical properties. Such applications include automotive and aircraft windows, heat mirrors, optoelectronic devices, gas sensors, and solar cell array surfaces for space applications. Many spacecraft missions require that solar cell array surfaces dissipate charges in order to avoid damage such as electronic upsets, formation of pinholes in the protective coatings on solar array blankets, and contamination due to deposition of sputtered products. In tests at the NASA Lewis Research Center, mixed thin-films of sputter-deposited indium tin oxide (ITO) and magnesium fluoride (MgF2) that could be tailored to the desired sheet resistivity, showed transmittance values of greater than 90 percent. The samples evaluated were composed of mixed, thin-film ITO/MgF2 coatings, with a nominal thickness of 650 angstroms, deposited onto glass substrates. Preliminary results indicated that these coatings were durable to vacuum ultraviolet radiation and atomic oxygen. These coatings show promise for use on solar array surfaces in polar low-Earth-orbit environments, where a sheet resistivity of less than 10(exp 8)/square is required, and in geosynchronous orbit environments, where a resistivity of less than 10(exp 9)/square is required.

Source record↗
DOE OSTI2023

Copper alloys for interconnectors and methods for making the same

Metallic alloy interconnects (which can comprise copper) with low electrical resistivity and methods for making the same are disclosed. The electrical resistivity of thin film copper alloys was reduced by 36% with niobium solute and by 51% with iron solute compared to pure copper counterpart in dilute solute regimes (0-1.5 atomic %). The fabrication method is operated at room temperature, and does not require a high temperature annealing step.

Gianola, Daniel S.↗
DOE OSTI2021

Chemical Passivation of Crystalline Si by Al 2 O 3 Deposited Using Atomic Layer Deposition: Implications for Solar Cells

The atomistic-level mechanism for the chemical passivation of the monocrystalline Si (c-Si) surface with thermally annealed Al 2 O 3 was studied using in situ infrared spectroscopy and photoconductance decay measurements. Al 2 O 3 was deposited on high-lifetime, float-zone c-Si substrates using atomic layer deposition (ALD) from trimethylaluminum (TMA), and H 2 O or O 3 . Surface-sensitive attenuated total reflection Fourier transform infrared spectroscopy was used to monitor the c-Si/Al 2 O 3 interface, as well as the bulk of the Al 2 O 3 film during the entire process. Our results show that some surface Si–H bonds are preserved after the ALD of Al 2 O 3 on H-terminated Si. During the annealing step at 400 °C, restructuring occurs at the c-Si/Al 2 O 3 interface to form interfacial SiO x . Isotope labeling was used to differentiate interfacial SiD bonds on the c-Si surface from H incorporated in Al 2 O 3 . Within the sensitivity of our infrared setup (~10 13 cm –2 ), we did not observe any net migration of atomic H or D from Al 2 O 3 to the c-Si/Al 2 O 3 interface. To isolate the effects of chemical and field-effect passivation of Al 2 O 3 thin films, we carried out surface passivation studies on c-Si/SiO 2 /Al 2 O 3 stacks. We also annealed these stacks in different atmospheres to test the influence of annealing atmospheres on the chemical passivation of c-Si by Al 2 O 3 and observed that O 2 -containing atmosphere led to the best surface chemical passivation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

Ultrafast electron dynamics in platinum and gold thin films driven by optical and terahertz fields

Here, we investigate the ultrafast electron dynamics triggered by terahertz and optical pulses in thin platinum and gold films by probing their transient optical reflectivity. The response of the platinum film to an intense terahertz pulse is similar to the optically induced one and can be described by a two-temperature model with a 20% larger electron–phonon coupling for the terahertz-driven dynamics compared to the optically induced one, ascribed to an additional nonthermal electron–phonon coupling contribution. Surprisingly, gold films exhibit a much smaller terahertz pulse-induced reflectivity change and with a sign opposite to the optical case. Additionally we explain this remarkable observation with field emission of electrons due to Fowler–Nordheim tunneling, enabled in samples with thicknesses below the structural percolation threshold, where nanostructuring promotes near-field enhancement. Our results provide a fundamental insight into the ultrafast processes relevant to modern electro- and magneto-optical applications.

74 ATOMIC AND MOLECULAR PHYSICS↗
NASA NTRS1995

Changes in chemical and optical properties of thin film metal mirrors on LDEF

Thin films of the metals Cu, Ni, Pt, Au, Sn, Mo, and W deposited on fused silica flats were exposed at ambient temperature on the leading and trailing faces of the LDEF. Reflectances of these films were measured from 250 to 2500 nm and compared with controls. The exposed films were subjected to the LDEF external environment including atomic oxygen, molecular contamination, and solar ultraviolet. Major changes in optical and infrared reflectance were seen for Cu, Mo, Ni, and W films on the leading face of LDEF and are attributed to partial conversion of metal to metal oxide. Smaller changes in optical properties are seen on all films and are probably caused by thin contaminant films deposited on top of the metal. The optical measurements are correlated with film thickness measurements, x-ray photoelectron spectroscopy, optical calculations, and, in the case of Cu, with x-ray diffraction measurements. In a few cases, comparisons with results from a similar UAH experiment on STS-8 have been drawn.

Peters, Palmer N.↗
DOE OSTI2022

Machine learning and atomic layer deposition: Predicting saturation times from reactor growth profiles using artificial neural networks

In this work, we explore the application of deep neural networks to the optimization of atomic layer deposition (ALD) processes. In particular, we focus on a one-shot optimization problem, where we try to predict the optimal dose time that leads to saturation everywhere in the reactor based on thickness values measured at different points of an ALD reactor after a single trial growth. In order to tackle this problem, we introduce a dataset designed to train neural networks to predict saturation times based on these inputs for a cross-flow ALD reactor. Here, we then explore the predictive ability of artificial neural networks of different depths and sizes using a separate testing dataset to evaluate their accuracies. The results obtained show that networks trained using stochastic gradient descent methods can accurately predict saturation times without requiring any additional information on the surface kinetics. This provides a viable approach to minimize the number of experiments required to optimize new ALD processes in a known reactor, and it highlights the way machine learning can be leveraged for thin film growth and manufacturing. While the datasets and training procedure depend on the reactor geometry, the trained neural networks provide a general surrogate model connecting thickness values and trial dose times with optimal saturation times that can be reused for different ALD processes within the same reactor.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Intrinsic (Trap‐Free) Transistors Based on Epitaxial Single‐Crystal Perovskites

Abstract The first experimental realization of the intrinsic (not dominated by defects) charge conduction regime in lead‐halide perovskite field‐effect transistors (FETs) is reported. The advance is enabled by: i) a new vapor‐phase epitaxy technique that results in large‐area single‐crystalline cesium lead bromide (CsPbBr 3 ) films with excellent structural and surface properties, including atomically flat surface morphology, essentially free from defects and traps at the level relevant to device operation; ii) an extensive materials analysis of these films using a variety of thin‐film and surface probes certifying the chemical and structural quality of the material; and iii) the fabrication of nearly ideal (trap‐free) FETs with characteristics superior to any reported to date. These devices allow the investigation of the intrinsic FET and (gated) Hall‐effect carrier mobilities as functions of temperature. The intrinsic mobility is found to increase on cooling from ≈30 cm 2 V −1 s −1 at room temperature to ≈250 cm 2 V −1 s −1 at 50 K, revealing a band transport limited by phonon scattering. Establishing the intrinsic (phonon‐limited) mobility provides a solid test for theoretical descriptions of carrier transport in perovskites, reveals basic limits to the technology, and points to a path for future high‐performance perovskite electronic devices.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Current Status on the Manufacturing of Nanomaterials for Proton Exchange Membrane Energy Systems by Vapor-Based Processes

Development of novel technologies for catalyst synthesis and membrane electrode assembly (MEA) fabrication is of primary importance for further improvement of the performance and economics of proton exchange membrane fuel cells (PEMFCs) and proton exchange membrane water electrolyzers (PEMWEs). While the traditional manufacturing methods are time-consuming, energy intensive, and require many processing steps, the new vapor-based methods provide many benefits including the development of improved catalysts and catalyst supports, deposition of uniform thin films, reduction of catalyst loading, and minimizing the number of manufacturing steps. Recent publications in the field identified spray pyrolysis, reactive spray deposition technology, chemical vapor deposition, and atomic layer deposition as advanced vapor-based catalyst synthesis and deposition methods used for fabrication of MEAs for PEMFCs and PEMWEs. Here, the MEAs fabricated via vapor-based processes have shown significant performance improvements in comparison to the state-of-the-art MEAs, which are attributed to better catalyst distribution, improved catalyst supports, and controlled, uniform catalyst layer microstructures. This review provides an overview of the vapor-based synthesis and deposition methods currently being used for the development of PEM-based devices. The advantages and disadvantages of these methods are critically compared and discussed while the outlook for future development is provided.

25 ENERGY STORAGE↗
DOE OSTI2021

Designing Anion-Exchange Ionomers with Oriented Nanoscale Phase Separation at a Silver Interface

We report performance of polymer electrolyte-based energy systems is significantly impacted by transport within the electrode catalyst layer, where ionomer thin films coat catalyst particles. Proton exchange ionomer thin films have been thoroughly characterized, but few studies have critically examined anion-exchange ionomer (AEI) thin films. Further, none have reported nanoscale phase separation for hydrocarbon AEIs, which is critical to mitigate transport resistances. In this work, a set of hydrocarbon-based AEIs with nanoscale phase separation are developed from tunable block copolymer systems composed of polyisoprene (PIp) and polychloromethylstyrene (PCMS). The effect of the PIp/PCMS ratio, architecture, and thickness on the thin-film morphology of the neutral block copolymer precursors on silicon and silver substrates is investigated using grazing-incidence small-angle X-ray scattering (GISAXS) and atomic force microscopy (AFM). AEIs are prepared by quaternizing with trimethylamine or methylpiperidine and their cation-dependent morphology is characterized at 60 °C and 95% RH. A perpendicularly aligned morphology is observed on silver, while no phase separation is observed on silicon, indicating that silver-polymer interfacial interactions drive phase separation. After quaternization, dipole-dipole interactions induce some disorder, but nanoscale phase separation is still maintained. GISAXS patterns are modeled using a Unified Fit approach to understand water uptake and swelling, and recommendations for AEI design are presented.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Ultrafast Optically Induced Perturbation of Oxygen Octahedral Rotations in Multiferroic BiFeO 3 Thin Films

The functional properties of complex oxides, including magnetism and ferroelectricity, are closely linked to subtle structural distortions. Ultrafast optical excitations provide the means to manipulate structural features and ultimately to affect the functional properties of complex oxides with picosecond-scale precision. Here, we report that the lattice expansion of multiferroic BiFeO 3 following above-bandgap optical excitation leads to distortion of the oxygen octahedral rotation (OOR) pattern. The continuous coupling between OOR and strain was probed using time-resolved X-ray free-electron laser diffraction with femtosecond time resolution. Density functional theory calculations predict a relationship between the OOR and the elastic strain consistent with the experiment, demonstrating a route to employing this approach in a wider range of systems. Ultrafast control of the functional properties of BiFeO 3 thin films is enabled by this approach because the OOR phenomena are related to ferroelectricity, and via the Fe-O-Fe bond angles, the superexchange interaction between Fe atoms.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Eliminating chemo-mechanical degradation of lithium solid-state battery cathodes during >4.5 V cycling using amorphous Nb2O5 coatings

Abstract Lithium solid-state batteries offer improved safety and energy density. However, the limited stability of solid electrolytes (SEs), as well as irreversible structural and chemical changes in the cathode active material, can result in inferior electrochemical performance, particularly during high-voltage cycling (>4.3 V vs Li/Li + ). Therefore, new materials and strategies are needed to stabilize the cathode/SE interface and preserve the cathode material structure during high-voltage cycling. Here, we introduce a thin (~5 nm) conformal coating of amorphous Nb 2 O 5 on single-crystal LiNi 0.5 Mn 0.3 Co 0.2 O 2 cathode particles using rotary-bed atomic layer deposition (ALD). Full cells with Li 4 Ti 5 O 12 anodes and Nb 2 O 5 -coated cathodes demonstrate a higher initial Coulombic efficiency of 91.6% ± 0.5% compared to 82.2% ± 0.3% for the uncoated samples, along with improved rate capability (10x higher accessible capacity at 2C rate) and remarkable capacity retention during extended cycling (99.4% after 500 cycles at 4.7 V vs Li/Li + ). These improvements are associated with reduced cell polarization and interfacial impedance for the coated samples. Post-cycling electron microscopy analysis reveals that the Nb 2 O 5 coating remains intact and prevents the formation of spinel and rock-salt phases, which eliminates intra-particle cracking of the single-crystal cathode material. These findings demonstrate a potential pathway towards stable and high-performance solid-state batteries during high-voltage operation.

Science & Technology - Other Topics↗
NASA NTRS1992

The spectrum of the tropical oxygen nightglow observed at 3 A resolution with the Hopkins Ultraviolet Telescope

Ultraviolet spectra of the tropical oxygen nightglow in the range of 830 to 1850 A (in first order) at 3 A resolution were obtained with the Hopkins Ultraviolet Telescope in December 1990. The data are presented which were obtained on a setting celestial target as the zenith angle of the line-of-sight varied from 77 to 95 deg. The dominant features in the spectrum (other than geocoronal hydrogen) are O I 1304 and 1356 and the radiative recombination continuum near 911 A. The continuum is resolved and found to be consistent with an electron temperature in the range 1000-1250 K. The observed ratio of the brightness of O I 1356 to the continuum suggests that O(+)-O(-) mutual neutralization contributes about 40 percent to the 1356 A emission. The dependence of the optically thin emissions on zenith angle is consistent with a simple ionospheric model. Weak O I 989 emission is also detected, but there is no evidence for any similarly produced atomic nitrogen emissions.

Feldman, P. D.↗
NASA NTRS2004

Gear Performance Improved by Coating

Gears, bearings, and other mechanical elements transmit loads through contacting surfaces. Even if properly designed, manufactured, installed, and maintained, gears and bearings will eventually fail because of the fatigue of the working surfaces. Economical means for extending the fatigue lives of gears and bearings are highly desired, and coatings offer the opportunity to engineer surfaces to extend the fatigue lives of mechanical components. A tungsten-containing diamondlike-carbon coating exhibiting high hardness, low friction, and good toughness was evaluated for application to spur gears. Fatigue testing was done at the NASA Glenn Research Center on both uncoated and coated spur gears. The results showed that the coating extended the surface fatigue lives of the gears by a factor of about 5 relative to the uncoated gears. For the experiments, a lot of spur test gears made from AISI 9310 gear steel were case-carburized and ground to aerospace specifications. The geometries of the 28-tooth, 8-pitch gears were verified as meeting American Gear Manufacturing Association (AGMA) quality class 12. One-half of the gears were randomly selected for coating. The method of coating was selected to achieve desired adherence, toughness, hardness, and low-friction characteristics. First the gears to be coated were prepared by blasting (vapor honing) with Al2O3 particles and cleaning. Then, the gears were provided with a thin adhesion layer of elemental chromium followed by magnetron sputtering of the outer coating consisting of carbon (70 at.%), hydrogen (15 at.%), tungsten (12 at.%), and nickel (3 at.%) (atomic percent at the surface). In total, the coating thickness was about 2.5 to 3 microns. As compared with the steel substrate, the coated surface was harder by a factor of about 2 and had a smaller elastic modulus. All gears were tested using a 5-centistoke synthetic oil, a 10,000-rpm rotation speed, and a hertzian contact stress of at least 1.7 GPa (250 ksi). Tests were run until either surface fatigue occurred or 300 million stress cycles were completed. Tests were run using either a pair of uncoated gears or a pair of coated gears (coated gears mated with uncoated gears were not evaluated). The fatigue test results, shown on Weibull coordinates in the graph, demonstrate that the coating provided substantially longer fatigue lives even though some of the coated gears endured larger stresses. The increase in fatigue life was a factor of about 5 and the statistical confidence for the improvement is high (greater than 99 percent). Examination of the tested gears revealed substantial reductions of total wear for coated gears in comparison to uncoated gears. The coated gear surface topography changed with running, with localized areas of the tooth surface becoming smoother with running. Theories explaining how coatings can extend gear fatigue lives are research topics for coating, tribology, and fatigue specialists. This work was done as a partnership between NASA, the U.S. Army Research Laboratory, United Technologies Research Corporation, and Sikorsky Aircraft.

Krantz, Timothy L.↗
DOE OSTI2023

Tailoring Growth Interfaces of Virtual Substrates for Power Electronics

Power electronics materials are poised to play a critical role in fulfilling next generation energy needs, with up to 90% of future energy demand predicted to flow through power electronics at some point.[1] Among a number of candidate materials, AlxGa1-xN is the strongest, having bipolar dopability, thermal and chemical stability, an ultra-wide bandgap, and demonstrated experimental feasibility. However, AlGaN growth is limited by a lack of lattice-matched substrates, ultimately stunting material quality at higher thicknesses needed for power electronics applications. Further, high power applications increasingly call for fully vertical device structures, necessitating a conductive substrate. [1] Recently our group identified the (111) plane of TaC as a conductive surface lattice-matched to Al0.55Ga0.45N, taking inspiration from prior work of AlN and GaN binaries on carbide and boride substrates. [2,3,4] In this talk we demonstrate the growth of (111)-oriented TaC by RF sputtering. We investigate the interface of TaC with sapphire and SiC substrates and identify means to suppress competing Ta2C nucleation in order to stabilize (111)-oriented TaC. Potential stacking sequences are identified with respect to crystal structure and observed twinning in the TaC films. We next assess structural changes and film recrystallization that results from face-to-face annealing of TaC thin films at high temperatures above 1500 degrees Celsius. Changes to grain structure and domain size are assessed by x-ray diffraction and surface morphology is explored using atomic force microscopy. Figure 1 shows significant improvements to in- and out-of-plane strain following annealing along with the formation of terraced step edges at the film surface. Strain as a function of material composition and thickness is considered, as this may play a major role in future nucleation of AlGaN layers.

CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND SU↗