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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

A high-temperature Rutherford Backscattering Spectrometry apparatus for in situ material characterization

A new methodology for high-temperature Rutherford Backscattering Spectrometry (HT-RBS) has been developed to enable in situ material characterization at elevated temperatures. A 3.5 MeV proton beam penetrates a 10-µm-thick 316L stainless steel foil mounted on a graphite substrate, with backscattered signals detected using an HT-RBS system. Conventional semiconductor detectors, primarily based on silicon, suffer significant performance degradation at temperatures higher than ~ 60 °C due to increased leakage current and noise, leading to signal distortion and failure. Here, to preserve spectral quality, a 5 µm aluminum foil shields the detector from thermal radiation, allowing reliable operation up to 900 °C at the target. A rotatable shutter provides additional thermal isolation during data collection pauses. In situ measurements of areal density changes of 316L stainless steel were conducted to validate the technique, revealing consistency with the known thermal expansion coefficient. The method facilitates seamless switching between irradiation and analysis, enabling continuous studies. This approach supports in situ investigations of diffusion, void swelling, creep, and corrosion, offering a versatile tool for advanced materials research.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Sputtering Erosion in the Ion Thruster

During the first phase of this research, the sputtering yields of molybdenum by low energy (100 eV and higher) xenon ions were measured by using the methods of secondary neutral mass spectrometry (SNMS) and Rutherford backscattering spectrometry (RBS). However, the measured sputtering yields were found to be far too low to explain the sputtering erosions observed in the long-duration tests of ion thrusters. The only difference between the sputtering yield measurement experiments and the ion thruster tests was that the later are conducted at high ion fluences. Hence, a study was initiated to investigate if any linkage exists between high ion fluence and an enhanced sputtering yield. The objective of this research is to gain an understanding of the causes of the discrepancies between the sputtering rates of molybdenum grids in an ion thruster and those measured from our experiments. We are developing a molecular dynamics simulation technique for studying low-energy xenon ion interactions with molybdenum. It is difficult to determine collision sequences analytically for primary ions below the 200 eV energy range where the ion energy is too low to be able to employ a random cascade model with confidence and it is too high to have to consider only single collision at or near the surface. At these low energies, the range of primary ions is about 1 to 2 nm from the surface and it takes less than 4 collisions on the average to get an ion to degrade to such an energy that it can no longer migrate. The fine details of atomic motion during the sputtering process are revealed through computer simulation schemes. By using an appropriate interatomic potential, the positions and velocities of the incident ion together with a sufficient number of target atoms are determined in small time steps. Hence, it allows one to study the evolution of damages in the target and its effect on the sputtering yield. We are at the preliminary stages of setting up the simulation program.

Ray, Pradosh K.↗
DOE OSTI2025

Molecular beam epitaxy growth and optoelectronic properties of droplet-free lattice-matched GaInAsSbBi on GaSb with wavelength extension exceeding 5 μ m

GaInAsSbBi alloys are grown lattice-matched on GaSb by molecular beam epitaxy demonstrating smooth surface morphologies, >5 μm wavelength photoluminescence emission, and minority carrier lifetimes >1 μs. At a growth temperature of 400 °C, the Ga flux is systematically increased and the Bi flux systematically decreased to identify GaInAsSbBi growth conditions that yield smooth droplet-free surface morphologies. The minority carrier lifetime is evaluated using time-resolved photoluminescence, where it is observed that GaInAsSbBi samples exhibit minority carrier lifetimes comparable to their Bi-free GaInAsSb counterparts, on the order of 1.5–2 μs. The bandgap and Urbach energy are evaluated from steady-state photoluminescence to gain insight into the impact of the incorporated Bi. Coupled with Rutherford backscattering spectrometry measurements of the Bi mole fraction, bandgap reduction rates of 97 meV/% Bi in InAsSbBi and 150 meV/% Bi in GaInAsSbBi are observed, significantly higher than previous evaluations in InAsSbBi (35–55 meV/% Bi). Detailed comparisons of the Bi mole fraction, bandgap energy, and Urbach energy indicate that the bandgap reduction potential in this alloy system is inhibited by the formation of Bi clusters; however, the inclusion of Ga in the quinary alloy is effective in suppressing Bi's tendency to incorporate in clusters for Ga mole fractions >9%, maximizing the bandgap reduction per unit Bi and overall optoelectronic quality.

Atomic force microscopy↗
DOE OSTI2026

Expanding the Zinc Precursor Toolbox: A Comparative Study of Precursors for Thermal ALD of ZnO Thin Films

Atomic layer deposition (ALD) of zinc oxide (ZnO) has been widely researched using diethyl zinc (DEZ)-based methods. The significant importance of thin films of ZnO as transparent conductive oxides (TCO) in optoelectronic devices and photovoltaics warrants examining alternative Zn precursors for ZnO ALD as potential replacements for the pyrophoric DEZ. In this study, we investigated three alternative Zn precursors: Zn(EEKI)2, Zn(DMP)2, ZnEt(HMDS), in the process development for high-quality ZnO thin films and compared them to DEZ. The ALD processes were studied using in situ spectroscopic ellipsometry. The properties of the ALD ZnO films were characterized using ex situ X-ray photoelectron spectroscopy (XPS), Rutherford backscattering spectrometry and nuclear reaction analysis (RBS/NRA), X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), and ultraviolet-visible (UV/Vis) spectrophotometry. These measurements confirmed the formation of pure, stoichiometric, and polycrystalline ZnO films using all four Zn precursors. Although the selected precursors are chemically diverse Zn compounds, they all yielded saturating ALD processes and high-quality ZnO thin films at 200 °C. This study highlights the potential benefits of alternative zinc precursors in designing ALD processes for ZnO thin films.

Obenlüneschloß, Jorit↗
DOE OSTI2025

A15 phase Ta 3⁢ Sb thin films: Direct synthesis, charge transport, and spin-orbit torque

Ta 3 ⁢Sb is one of the A15 compounds that have been predicted to have giant spin Hall conductivities due to the gapped Dirac-like band crossings in their electronic structures. We use co-sputtering to directly synthesize thin films of Ta 3 ⁢Sb and identify a large window of Ta:Sb flux ratio that permits the formation of single-phase A15 structure. These sputtered films have an actual Ta:Sb atomic ratio of 4:1, as determined from Rutherford backscattering spectrometry. Their high resistivity, at the Mott-Ioffe-Regel limit, suggests that the electron mean free path is comparable to interatomic distances. From harmonic Hall and spin-torque ferromagnetic resonance measurements, the intrinsic spin Hall conductivity of thin film Ta 3 ⁢Sb is estimated to be in the range of −526 to −1230⁢(ℏ/𝑒)S/cm at 300 K, lower in magnitude than the predicted value of −1400⁢(ℏ/𝑒)S/cm . Here, first-principles calculations of the electronic structure show that the discrepancy is consistent with an increase of the Fermi level due to the nonideal stoichiometry needed to stabilize the A15 structure.

Density functional theory↗
DOE OSTI2024

In-Situ Characterization Tools for Evaluating Radiation Tolerance and Elemental Migration in Perovskites

This paper discusses the in-situ characterization tools designed to assess radiation tolerance and elemental migration in perovskite materials. With the increasing use of perovskites in various technological applications, understanding their response to radiation exposure is paramount. Ion Beam Induced Charge (IBIC) emerges as a powerful tool for investigating the radiation tolerance of perovskites at the microscale. By employing focused ion beams, IBIC allows for the spatial mapping of charge carriers, offering insights into the material's electronic response to radiation-induced defects. This technique enables researchers to pinpoint areas of enhanced or suppressed charge collection, providing valuable information on the perovskite's intrinsic properties under irradiation. Rutherford Backscattering Spectrometry (RBS) complements the study by offering a quantitative analysis of elemental migration in perovskite materials. Through the precise measurement of backscattered ions, RBS provides a detailed understanding of the elemental composition and distribution within the perovskite lattice after radiation exposure. The integration of IBIC and RBS techniques in in-situ experiments enhances the comprehensive characterization of radiation effects on perovskites.

ion beams↗
DOE OSTI2025

Transformation of TiN to TiNO Films via In-Situ Temperature-Dependent Oxygen Diffusion Process and Their Electrochemical Behavior

Titanium oxynitride (TiNO) thin films represent a multifaceted material system applicable in diverse fields, including energy storage, solar cells, sensors, protective coatings, and electrocatalysis. This study reports the synthesis of TiNO thin films grown at different substrate temperatures using pulsed laser deposition. A comprehensive structural investigation was conducted by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Non-Rutherford backscattering spectrometry (N-RBS), and X-ray absorption spectroscopy (XAS), which facilitated a detailed analysis that determined the phase, composition, and crystallinity of the films. Structural control was achieved via temperature-dependent oxygen in-diffusion, nitrogen out-diffusion, and the nucleation growth process related to adatom mobility. The XPS analysis indicates that the TiNO films consist of heterogeneous mixtures of TiN, TiNO, and TiO2 phases with temperature-dependent relative abundances. The correlation between the structure and electrochemical behavior of the thin films was examined. The TiNO films with relatively higher N/O ratio, meaning less oxidized, were more electrochemically active than the films with lower N/O ratio, i.e., more oxidized films. Films with higher oxidation levels demonstrated enhanced crystallinity and greater stability under electrochemical polarization. These findings demonstrate the importance of substrate temperature control in tailoring the properties of TiNO film, which is a fundamental part of designing and optimizing an efficient electrode material.

Cherono, Sheilah↗
NASA NTRS1985

Palladium silicide formation under the influence of nitrogen and oxygen impurities

The effect of impurities on the growth of the Pd2Si layer upon thermal annealing of a Pd film on 100 line-type and amorphous Si substrates is investigated. Nitrogen and oxygen impurities are introduced into either Pd or Si which are subsequently annealed to form Pd2Si. The complementary techniques of Rutherford backscattering spectrometry, and N-15(p, alpha)C-12 or O-18(p, alpha)N-15 nuclear reaction, are used to investigate the behavior of nitrogen or oxygen and the alterations each creates during silicide formation. Both nitrogen and oxygen retard the silicide growth rate if initially present in Si. When they are initially in Pd, there is no significant retardation; instead, an interesting snow-plowing effect of N or O by the reaction interface of Pd2Si is observed. By using N implanted into Si as a marker, Pd and Si appear to trade roles as the moving species when the silicide front reaches the nitrogen-rich region.

Ho, K. T.↗
NASA NTRS1987

Theoretical approach to oxygen atom degradation of silver

Based on available Rutherford backscattering spectrometry (RBS), proton induced X-ray emission (PIXE) and ellipsometry data obtained on silver specimens subjected to atomic oxygen attack in low Earth orbit STS flight 41-G, a theory was developed to model the oxygen atom degradation of silver. The diffusion of atomic oxygen in a microscopically nonuniform medium is an essential constituent of the theory. The driving force for diffusion is the macroscopic electrochemical potential gradient developed between the specimen surface exposed to the ambient and the bulk of the silver specimen. The longitudinal electric effect developed parallel to the gradient is modified by space charge of the diffusing charged species. Lateral electric fields and concentration differences also exist due to the nonuniform nature of the medium. The lateral concentration differences are found to be more important than the lateral electric fields in modifying the diffusion rate. The model was evaluated numerically. Qualitative agreement exists between the kinetics predicted by the theory and kinetic data taken in ground-based experiments utilizing a plasma asher.

Fromhold, Albert T., Jr.↗
NASA NTRS1993

Evaluation of chemical conversion material (protective coating) exposed to space environmental conditions

This report focuses on the development of an operational Rutherford backscattering spectrometry (RBS) system and shows the application of such a system on a space environmental test. Thin films of aluminum and tantalum were deposited on diamond substrates. These films were anodized and preexposure characterization spectra obtained using RBS and total hemispherical reflectance. The samples were exposed to energetic protons then postexposure characterization spectra was obtained using the same techniques. Conclusions based on the comparison of preexposure and postexposure spectra are presented. RBS comparison spectra show no change in the metal/metal oxide interface, while the comparison reflectance data indicate change. Explanations for this reflectance change are presented in this report.

Edwards, D. L.↗
NASA NTRS1999

Low-Energy Sputtering Research

An experimental study is described to measure low-energy (less than 600 eV) sputtering yields of molybdenum with xenon ions using Rutherford backscattering spectroscopy (RBS) and secondary neutral mass spectroscopy (SNMS). An ion gun was used to generate the ion beam. The ion current density at the target surface was approximately 30 (micro)A/sq cm. For RBS measurements, the sputtered material was collected on a thin aluminum strip which was mounted on a semi-circular collector plate. The target was bombarded with 200 and 500 eV xenon ions at normal incidence. The differential sputtering yields were measured using the RBS method with 1 MeV helium ions. The differential yields were fitted with a cosine fitting function and integrated with respect to the solid angle to provide the total sputtering yields. The sputtering yields obtained using the RBS method are in reasonable agreement with those measured by other researchers using different techniques. For the SNMS measurements, 150 to 600 eV xenon ions were used at 50deg angle of incidence. The SNMS spectra were converted to sputtering yields for perpendicular incidence by normalizing SNMS spectral data at 500 eV with the yield measured by Rutherford backscattering spectrometry. Sputtering yields as well as the shape of the yield-energy curve obtained in this manner are in reasonable agreement with those measured by other researchers using different techniques. Sputtering yields calculated by using two semi-spherical formulations agree reasonably well with measured data. The isotopic composition of secondary ions were measured by bombarding copper with xenon ions at energies ranging from 100 eV to 1.5 keV. The secondary ion flux was found to be enriched in heavy isotopes at low incident ion energies. The heavy isotope enrichment was observed to decrease with increasing impact energy. Beyond 700 eV, light isotopes were sputtered preferentially with the enrichment remaining nearly constant.

Ray, P. K.↗
NASA NTRS1999

Epitaxial Ferroelectric Ba(0.5)Sr(0.5)TiO3 Thin Films for Room-Temperature High-Frequency Tunable Element Applications

Perovskite Ba(0.5)SR(0.5)TiO3 thin films have been synthesized on (001) LaAl03 substrates by pulsed laser ablation. Extensive X-ray diffraction, rocking curve, and pole-figure studies suggest that the films are c-axis oriented and exhibit good in-plane relationship of <100>(sub BSTO)//<100>(sub LAO). Rutherford Backscattering Spectrometry studies indicate that the epitaxial films have excellent crystalline quality with an ion beam minimum yield chi(sub min) Of only 2.6 %. The dielectric property measurements by the interdigital technique at 1 MHz show room temperature values of the relative dielectric constant, epsilon(sub r), and loss tangent, tan(sub delta), of 1430 and 0.007 with no bias, and 960 and 0.001 with 35 V bias, respectively. The obtained data suggest that the as-grown Ba(0.5)SR(0.5)TiO3 films can be used for development of room-temperature high-frequency tunable elements.

Chen, C. L.↗
NASA NTRS2002

Study of Lightweight Ni-Co Alloy Mirrors Obtained by Electroforming Techniques

One contribution in reducing the costs of optics in space can be provided by production of ultralight mirrors. The decrease in the weight of the primary mirror of a telescope is anticipated to lead to the possibility of increasing the size of the telescopes, therefore increasing the amount and distance from which information is received. An electroplating process of ultralight replica mirrors from nickel sulfamate solution will be described. Based on an experimental setup with cylindrical symmetry, flat mirrors with a diameter of 7 inches and thickness of 1.5 mm are made from a Ni-Co alloy. The composition of the resulting deposit is analyzed using Rutherford Backscattering Spectrometry (RBS) and Proton Induced X-ray Emission (PIXE). In order to resolve Ni and Co, 10 MeV nitrogen ions are used as projectiles in the RBS measurements. Solution parameters monitored during the deposition process using optical absorption and polarography will be correlated with the final concentration of Ni and Co in the deposit. Bath parameters like temperature, current density, agitation level and acidity are chosen at certain values and maintained constant from one sample to another throughout the deposition process. The purpose of the experiment is to obtain mirrors with near zero stress, and predetermined composition and hardness. This study is an intermediate step in obtaining through the same process, but with a larger scale setup, ultralight large aperture replica mirrors.

Jones, Ruth↗
NASA NTRS2004

In situ Pulsed Laser Deposition of C-Axis Oriented MgB2 Films and Their Characterization

The recent discovery of an intermetallic superconductor MgB2 has renewed interest in the area of superconductivity not only because of fundamental understanding of superconductivity but also due to its potential applicability in devices such as thermal detectors. Considerable amount of research has been devoted to obtain MgB2 films by an all in situ growth technique. We have grown MgB2 thin films by an all in situ pulsed laser deposition process from pure B and Mg targets. Ultrathin layers of B and Mg were deposited in a multilayer configuration. Hundreds of such Mg-B bilayers with a capping Mg layer on the top were deposited on sapphire substrate. These depositions were done in high vacuum (approx. 10(exp -7) Torr) and at room temperature. After deposition, such a configuration was annealed at high temperature for a short time in a forming gas (4% H2 in Ar). The best films, obtained by this procedure, showed superconducting transition temperature approx. 30 K. These films have been characterized by x-ray diffraction, Rutherford Backscattering Spectrometry, AC susceptibility-, resistivity- (with and without magnetic field) and 1/f noise-measurements. The physical properties of these films will be presented and discussed.

Shinde, Sanjay↗
NASA NTRS2005

Growth of periodic nano-layers of nano-crystals of Au, Ag, Cu by ion beam

Multilayered thin films of SiO2/AU+ SiO2/, SiO2/Ag+ SiO2/, and SiO2/Cu+ SiO2/, were grown by deposition. We have previously shown that MeV ion Bombardment of multi-nano-layers of SiO2/AU+ SiO2/ produces Au nanocrystals in the AU+ SiO2 layers. An increased number of nano-layers followed by MeV ion bombardment produces a wide optical absorption band, of which its FWHM depends on the number of nano-layers of SiO2/AU+ SiO2/. We have successfully repeated this process for nano-layers of SiO2/Ag+ SiO2/, and SiO2/Cu+ SiO2/. In this work we used 5 MeV Si as the post deposition bombardment ion and monitored the location as well as the optical absorption's FWHM for each layered structure using Optical Absorption Photospectrometry. The concentration and location of the metal nano-crystals were measured by Rutherford Backscattering Spectrometry. We will report on the results obtained for nano-layered structures produced by post deposition bombardment of SiO2/AU+ SiO2/, SiO2/Ag+ SiO2/, and SiO2/Cu+ SiO2/ layered systems as well as the results obtained from a system containing a periodic combination of SiO2/AU+ SiO2/, SiO2/Ag+ SiO2/, and SiO2/Cu+ SiO2/.

Smith, Cydale C.↗
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 NTRS1980

Ion-implanted laser annealed silicon solar cells

Development of low cost solar cells fabrication technology is being sponsored by NASA JPL as part of the Low Cost Solar Array Project (LSA). In conformance to Project requirements ion implantation and laser annealing were evaluated as junction formation techniques offering low cost-high throughput potential. Properties of cells fabricated utilizing this technology were analyzed by electrical, transmission electron microscopy, Rutherford backscattering and secondary ion mass spectrometry techniques. Tests indicated the laser annealed substrates to be damage free and electrically active. Similar analysis of ion implanted furnace annealed substrates revealed the presence of residual defects in the form of dislocation lines and loops with substantial impurity redistribution evident for some anneal temperature/time regimes. Fabricated laser annealed cells exhibited improved spectral response and conversion efficiency in comparison to furnace annealed cells. An economic projection for LSA indicates a potential for considerable savings from laser annealing technology.

Katzeff, J. S.↗