Search NASA⌕ Search

SEARCH · Search NASA

Results for “spectroscopic ellipsometry”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
NASA NTRS2011

O-6 Optical Property Degradation of the Hubble Space Telescope's Wide Field Camera-2 Pick Off Mirror

Degradation in the performance of optical components can be greatly affected by exposure to the space environment. Many factors can contribute to such degradation including surface contaminants; outgassing; vacuum, UV, and atomic oxygen exposure; temperature cycling; or combinations of parameters. In-situ observations give important clues to degradation processes, but there are relatively few opportunities to correlate those observations with post-flight ground analyses. The return of instruments from the Hubble Space Telescope (HST) after its final servicing mission in May 2009 provided such an opportunity. Among the instruments returned from HST was the Wide-Field Planetary Camera-2 (WFPC-2), which had been exposed to the space environment for 16 years. This work focuses on the identifying the sources of degradation in the performance of the Pick-off mirror (POM) from WFPC-2. Techniques including surface reflectivity measurements, spectroscopic ellipsometry, FTIR (and ATR-FTIR) analyses, SEM/EDS, X-ray photoelectron spectroscopy (XPS) with and without ion milling, and wet and dry physical surface sampling were performed. Destructive and contact analyses took place only after completion of the non-destructive measurements. Spectroscopic ellipsometry was then repeated to determine the extent of contaminant removal by the destructive techniques, providing insight into the nature and extent of polymerization of the contaminant layer.

McNamara, Karen M.↗
DOE OSTI2021

Mixed Tin-Titanium Oxides by Atomic Layer Deposition on Planar Substrates: Physical and Electronic Structure

Ternary atomic layer deposition of Sn-doped TiO x (Sn:TiO x ) and Ti-doped SnO x (Ti:SnO x ) was performed using tetrakisdimethylamidotitanium (IV) and tin(IV) with water at 150 °C on (1 0 0) Si and quartz substrates. The physical structure of the films was investigated using scanning electron, atomic force, and Kelvin probe force microscopies as well as spectroscopic ellipsometry, Raman spectroscopy, and X-ray diffraction. All as-deposited films are amorphous and possessed flat and conformal topographies with low surface roughness (<1 nm). Annealed Sn:TiO x and Ti:SnO x crystallize into the tetragonal anatase TiO 2 and cassiterite SnO 2 structures, respectively, without large variations to the film topography. The chemical composition of the as-deposited and annealed films was investigated through X-ray photoelectron spectroscopy. While dopants are homogenously mixed, the ternary ALD to form Sn:TiO x and Ti:SnO x surprisingly does not follow the rule of mixtures, despite similarities in both the growth rates of binary SnO x and TiO x and the precursors used. This finding is also supported by spectroscopic ellipsometry. Here, we postulate the deviation from the rule of mixtures is due to non-ideal surface chemistry of the binary ALD of SnO x . The optical bandgap of all films was quantified by the Tauc analysis and the valence band position was investigated by valence band X-ray photoelectron spectroscopy. Intra-bandgap states above the valence band maximum were observed for as-deposited Ti:SnO x and Sn:TiO x and ascribed to 5 s states from Sn 2+ ions. The presence of these intra-bandgap states induces enhanced visible absorption and bathochromic shifts to the apparent bandgap for all as-deposited films. Annealing the films removes the intra-bandgap states and increases the optical bandgap. Simplified band diagrams created using the data available demonstrated that the conduction and valence band positions did not vary between the positions of pure TiO 2 or SnO 2 with monotonic increases to the dopant incorporation.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Deriving the Infrared Complex Refractive Indices of Organic Powders for Optical Modeling: Comparison of Methods

Identification of solids via infrared reflection spectroscopy requires a spectral library of all solids likely to be encountered. A confounding factor in populating such a spectral library is that the reflectance spectra of solids vary with their form, including particle size, film thickness, and substrate. To reduce the efforts of experimentally constructing such a library, an alternate strategy is to use the wavelength-dependent optical constants, n and k, of a solid to calculate a series of reflectance spectra corresponding to each scenario or morphology. Because most n/k measurements are best performed on mm-sized crystals, however, the challenge of determining the optical constants increases when a solid is only readily available as a powder, as is often the case. Some organic solids, such as caffeine, are both unavailable in large crystals and difficult to press into pellets. In this study, the infrared optical constants, or complex refractive indices, of caffeine were determined using three different methods: single-angle reflectance, infrared spectroscopic ellipsometry, and quantitative absorbance measurements of KBr pellets. The n and k values derived through each method were used to model the hyperspectral imaging reflectance spectrum of a caffeine film on a steel planchet. Over 1,110 – 870 cm-1, the single-angle reflectance-derived n and k had the best correlation with the experimental spectrum. These results suggest different organic solids may require different methods to determine the most accurate infrared complex refractive indices for synthetic spectral libraries.

FTIR, hyperspectral imaging, infrared, infrared (I↗
DOE OSTI2021

Impact of Humidity and Temperature on the Stability of the Optical Properties and Structure of MAPbI3, MA0.7FA0.3PbI3 and (FAPbI3)0.95(MAPbBr3)0.05 Perovskite Thin Films

In situ real-time spectroscopic ellipsometry (RTSE) measurements have been conducted on MAPbI3, MA0.7FA0.3PbI3, and (FAPbI3)0.95(MAPbBr3)0.05 perovskite thin films when exposed to different levels of relative humidity at given temperatures over time. Analysis of RTSE measurements track changes in the complex dielectric function spectra and structure, which indicate variations in stability influenced by the underlying material, preparation method, and perovskite composition. MAPbI3 and MA0.7FA0.3PbI3 films deposited on commercial fluorine-doped tin oxide coated glass are more stable than corresponding films deposited on soda lime glass directly. (FAPbI3)0.95(MAPbBr3)0.05 films on soda lime glass showed improved stability over the other compositions regardless of the substrate, and this is attributed to the preparation method as well as the final composition.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Optical and Electronic Losses Arising from Physically Mixed Interfacial Layers in Perovskite Solar Cells

Perovskite solar cell device performance is affected by optical and electronic losses. To minimize these losses in solar cells, it is important to identify their sources. Here, we report the optical and electronic losses arising from physically mixed interfacial layers between the adjacent component materials in highly efficient two terminal (2T) all-perovskite tandem, single junction wide-bandgap, and single junction narrow-bandgap perovskite-based solar cells. Physically mixed interfacial layers as the sources of optical and electronic losses are identified from spectroscopic ellipsometry measurements and data analysis followed by comparisons of simulated and measured external quantum efficiency spectra. Parasitic absorbance in the physically mixed regions between silver metal electrical contacts and electron transport layers (ETLs) near the back contact and a physical mixture of commercial indium tin oxide and hole transport layers (HTL) near the front electrical contact lead to substantial optical loss. Here, a lower-density void + perovskite nucleation layer formed during perovskite deposition at the interface between the perovskite absorber layer and the HTL causes electronic losses due to incomplete collection of photogenerated carriers likely originating from poor coverage and passivation of the initially nucleating grains.

14 SOLAR ENERGY↗
DOE OSTI2024

Development of an Optical Library for Coevaporated CdSe x Te 1– x

The conversion efficiency of CdTe solar cells may be improved by bandgap engineering, i.e., changing the bandgap value through the addition of Se in the absorber. The Se alloying enables a short-circuit current density improvement, as it leads to a bandgap energy value decrease. Furthermore, it has been associated with increased minority carrier lifetimes, assuring high open-circuit voltage values. An Se gradient profile control can further optimize the solar cell performance. Thus, an optical model baseline of the CdSe x Te 1–x (CST) compound was developed. Spectroscopic ellipsometry measurements were conducted to accurately extract the optical constants of ten CST layers deposited through coevaporation with x varying from 0 to 1. Using the measured dielectric function spectra from the discrete CST layers with varying x, and considering the composition-induced shift in the critical point energies, an energy-shift model was employed to develop the accurate optical library for the CST compound for any x value to provide data for future modeling and optimization. Furthermore, the library accuracy was validated through optical simulations of the quantum efficiency of a graded CST solar cell using the finite-difference time-domain method by replicating the Se profile in the absorber layer measured through secondary ion mass spectrometry.

14 SOLAR ENERGY↗
DOE OSTI2022

Methods for Determining the Infrared Complex Refractive Indices n (λ) and k (λ) from Organic Solid Powders: Comparison of a Sucrose Single Crystal and a Pressed Pellet

There exists a need to measure optical constants n and k for many materials, especially organic solids in the infrared spectral region, but at present, there are only two established methods for making such measurements: single-angle (SA) reflectance and infrared spectroscopic ellipsometry (IRSE). The former derives the n/k vectors via measurement of the change in the amplitude of light reflected from the sample and then uses the Kramers–Kronig transform, while the latter measures the change in polarization of the reflected light from the sample to derive n/k. Here we make a direct comparison between the n/k vectors derived from SA measurements of a sucrose single crystal and the n/k values obtained after the crystal had been crushed, ground to powder, and pressed into a pellet form. The pellet was measured not only by SA but also via the IRSE method, and we found that pressing specular-quality pellets was critical, especially for the SA data. The n/k values of this typical organic molecule all agree to within 0.04 root-mean-square error, confirming that a pressed pellet can be used instead of a crystal to derive the intrinsic n/k vectors. In conclusion, this result is important for the many organic materials that, unlike sugar, do not have centimeter-sized crystals readily available.

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

Correlating electronic properties with M-site composition in solid solution Ti y Nb 2- y CT x MXenes

High electrical conductivity is desired in MXene films for applications such as electromagnetic interference shielding, antennas, and electrodes for electrochemical energy storage and conversion applications. Due to the acid etching-based synthesis method, it is challenging to deconvolute the relative importance that factors such as chemical composition and flake size contribute to resistivity. To understand the intrinsic and extrinsic contributions to the macroscopic electronic transport properties, a systematic study controlling compositional and structural parameters was conducted with eight solid solutions in the Ti y Nb 2-y CT x system. Here, in particular, we investigated the different roles played by metal (M)-site composition, flake size, and d-spacing on macroscopic transport. Hard x-ray photoemission spectroscopy and spectroscopic ellipsometry revealed changes to electronic structure induced by the M-site alloying. Consistent with the spectroscopic results, the low- and room-temperature conductivities and effective carrier mobility are correlated with the Ti content, while the impact of flake size and d-spacing is most prominent in low-temperature transport. The results provide guidance for designing and engineering MXenes with a wide range of conductivities.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Observation of the surface layer of lithium metal using in situ spectroscopy

In this work, we have investigated the surface of lithium metal using x-ray photoemission spectroscopy and optical spectroscopic ellipsometry. Even if we prepare the surface of lithium metal rigorously by chemical cleaning and mechanical polishing inside a glovebox, both spectroscopic investigations show the existence of a few tens of nanometer-thick surface layers, consisting of lithium oxides and lithium carbonates. When lithium metal is exposed to room air (~50% moisture), in situ real-time monitoring of optical spectra indicates that the surface layer grows at a rate of approximately 24 nm/min, presumably driven by an interface-controlled process. Our results hint that surface-layer-free lithium metals are formidable to achieve by a simple cleaning/polishing method, suggesting that the initial interface between lithium metal electrodes and solid-state electrolytes in fabricated lithium metal batteries can differ from an ideal lithium/electrolyte contact.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Assessing atomically thin delta-doping of silicon using mid-infrared ellipsometry

Hydrogen lithography has been used to template phosphine-based surface chemistry to fabricate atomic-scale devices, a process we abbreviate as atomic precision advanced manufacturing (APAM). In this work, we use mid-infrared variable angle spectroscopic ellipsometry (IR-VASE) to characterize single-nanometer thickness phosphorus dopant layers (δ-layers) in silicon made using APAM compatible processes. A large Drude response is directly attributable to theδ-layer and can be used for nondestructive monitoring of the condition of the APAM layer when integrating additional processing steps. Furthermore, the carrier density and mobility extracted from our room temperature IR-VASE measurements are consistent with cryogenic magneto-transport measurements, showing that APAM δ-layers function at room temperature. Finally, the permittivity extracted from these measurements shows that the doping in the APAM δ-layers is so large that their low-frequency in-plane response is reminiscent of a silicide. However, there is no indication of a plasma resonance, likely due to reduced dimensionality and/or low scattering lifetime.

2D material↗
NASA NTRS2017

Jet Fuel Thermal Stability Investigations Using Ellipsometry

Jet fuels are typically used for endothermic cooling in practical engines where their thermal stability is very important. In this work the thermal stability of Sasol IPK (a synthetic jet fuel) with varying levels of naphthalene has been studied on stainless steel substrates using spectroscopic ellipsometry in the temperature range 385-400 K. Ellipsometry is an optical technique that measures the changes in a light beam’s polarization and intensity after it reflects off of a thin film to determine the film’s thickness and optical properties. All of the tubes used were rated as thermally unstable by the color standard portion of the Jet Fuel Thermal Oxidation Test, and this was confirmed by the deposit thicknesses observed using ellipsometry. A new amorphous model on a stainless steel substrate was used to model the data and obtain the results. It was observed that, as would be expected, increasing the temperature of the tube increased the overall deposit amount for a constant concentration of naphthalene. The repeatability of these measurements was assessed using multiple trials of the same fuel at 385 K. Lastly, the effect of increasing the naphthalene concentration in the fuel at a constant temperature was found to increase the deposit thickness.In conclusion, ellipsometry was used to investigate the thermal stability of jet fuels on stainless steel substrate. The effects of increasing temperature and addition of naphthalene on stainless steel tubes with Sasol IPK fuel were investigated. It was found, as expected, that increasing temperature lead to an increase in deposit thickness. It wasAmerican Institute of Aeronautics and Astronautics6also found that increasing amounts of naphthalene increased the maximum deposit thickness. The repeatability of these measurements was investigated using multiple tests at the same conditions. The present work provides as a better quantitative tool compared to the widely used JFTOT technique. Future work will expand on the fuel types, temperature, and substrate materials.

thermal stability↗
NASA NTRS2006

Modeling Ellipsometry Measurements of Molecular Thin-Film Contamination on Genesis Array Samples

The discovery of a molecular thin-film contamination on Genesis flown array samples changed the course of preliminary assessment strategies. Analytical techniques developed to measure solar wind elemental abundances must now compensate for a thin-film contamination. Currently, this is done either by experimental cleaning before analyses or by depth-profiling techniques that bypass the surface contamination. Inside Johnson Space Center s Genesis dedicated ISO Class 4 (Class 10) cleanroom laboratory, the selection of collector array fragments allocated for solar wind analyses are based on the documentation of overall surface quality, visible surface particle contamination greater than 1 m, and the amount of thin film contamination measured by spectroscopic ellipsometry. Documenting the exact thickness, surface topography, and chemical composition of these contaminates is also critical for developing accurate cleaning methods. However, the first step in characterization of the molecular film is to develop accurate ellipsometry models that will determine an accurate thickness measurement of the contamination film.

Calaway, Michael J.↗
NASA NTRS1989

Ellipsometric study of Al2O3/Ag/Si and SiO2/Ag/quartz ashed in an oxygen plasma

The growth of silver oxide (proposed as a potentially useful protective coating for space environment) on a silver mirror coated with an Al2O3 or a SiO2 protective layer was investigated using the monolayer-sensitive variable angle of incidence spectroscopic ellipsometry technique. The samples were exposed to a pure oxygen plasma in a plasma asher, and the silver oxide growth was monitored as a function of the exposure time. It was found that atomic oxygen in the asher penetrated through the SiO2 or Al2O3 coatings to convert the silver underneath to silver oxide, and that the quantity of the silver oxide formed was proportional to the ashing time. The band gap of silver oxide was determined to be 1.3 eV. A schematic diagram of the variable angle of incidence spectroscopic ellipsometer is included.

De, Bhola N.↗
DOE OSTI2022

Impact of aqueous solution pH on network structure of corrosion–induced surface layers of boroaluminosilicate glass

Understanding of the long-term stability of vitrified nuclear waste glass is critical to its safe storage, but knowledge gaps remain regarding the corrosion mechanism, especially with respect to surface alteration layers whose presence changes the observed corrosion rates. Here, we report the aqueous corrosion of a model boroaluminosilicate glass at ground water relevant pHs as investigated by vibrational spectroscopy to understand the network structure of the alteration layer that we hypothesize controls the corrosion rates. Both specular reflection infrared spectroscopy and infrared variable angle spectroscopic ellipsometry were used to elucidate details of the structure of the alteration layers formed at pH 7 and pH 9. After 2312 days, the thickness of the alteration layer is found to be ~2000 nm for corrosion at pH 7 and ~300 nm for corrosion at pH 9. Here, the interpretation of the vibrational spectra suggests that alteration layers formed at pH 7 and pH 9 both exhibit a porous network with "silica-like" structures, but with differences in the bond lengths and bond angles in the glass network. Moreover, the relative abundance of the hydrous species within the porous network appears to be dependent on pH. Additionally, the spectroscopic data suggest that the B and Ca trapped in the alteration layer during the secondary corrosion of the pH 9 pre-corroded sample in pH 3 solution are hydrated within the nano-porous layer and not bound to the silicate network. However, the precise chemical form remains to be determined. Based on these findings, we propose that the combination of the network structure of the alteration layer and the relative abundance of hydrous species within the alteration layer act to control the transport of ionic species dissolved from the reaction front to the aqueous solution outside the glass.

36 MATERIALS SCIENCE↗
NASA NTRS2007

Genesis Silicon Carbide Concentrator Target 60003 Preliminary Ellipsometry Mapping Results

The Genesis concentrator was custom designed to focus solar wind ions primarily for terrestrial isotopic analysis of O-17/O-16 and O-18/O-16 to +/-1%, N-15/N-14 to +/-1%, and secondarily to conduct elemental and isotopic analysis of Li, Be, and B. The circular 6.2 cm diameter concentrator target holder was comprised of four quadrants of highly pure semiconductor materials that included one amorphous diamond-like carbon, one C-13 diamond, and two silicon carbide (SiC). The amorphous diamond-like carbon quadrant was fractured upon impact at Utah Test and Training Range (UTTR), but the remaining three quadrants survived fully intact and all four quadrants hold an important collection of solar wind. The quadrants were removed from the target holder at NASA Johnso n Space Center Genesis Curation Laboratory in April 2005, and have been housed in stainless steel containers under continual nitrogen purge since time of disintegration. In preparation for allocation of a silicon carbide target for oxygen isotope analyses at UCLA, the two SiC targets were photographed for preliminary inspection of macro particle contamination from the hard non-nominal landing as well as characterized by spectroscopic ellipsometry to evaluate thin film contamination. This report is focused on Genesis SiC target sample number 60003.

Calaway, M. J.↗
DOE OSTI2021

Anion Exchange Ionomers: Impact of Chemistry on Thin-Film Properties

Ionomer thin-films (i.e., 20–100 nm) on supports serve as model systems to understand ionomer-catalyst interfacial behavior as well as the confinement-driven deviation in properties from bulk membranes. While ionomer thin-films have been examined for proton exchange ionomers, the thin-film properties of anion exchange ionomers (AEIs) remain largely unexplored. More importantly, delineating the convoluted impact of chemistry and confinement on thin-film morphology and hydration is of interest to advancing the field on functional ionic interfaces. In this work, these aspects are studied by using AEIs of different backbones (perfluorinated, aliphatic, and aromatic) and side chains (various lengths, and single versus dual functional groups). Quartz-crystal microbalance and spectroscopic ellipsometry are used to analyze density and coupled with calculated free volume fraction of thin-films to provide insights on their gas transport properties. AEI side-chain's chemical character plays a key role in how confinement modulates hydration (in thin-film versus bulk). Overall, the results elucidate the effects of backbone, side-chain chemistry versus anion/cation type in the confinement-driven changes in thin-film morphology and swelling. This study also provides new insights for tuning AEI transport functionalities at interfaces via chemistry, which can benefit the design and development of electrode-ionomers for alkaline membrane-based energy systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

The Role of Optical Phonon Confinement in the Infrared Dielectric Response of III–V Superlattices

Polar dielectrics are key materials of interest for infrared (IR) nanophotonic applications due to their ability to host phonon-polaritons that allow for low-loss, subdiffractional control of light. The properties of phonon-polaritons are limited by the characteristics of optical phonons, which are nominally fixed for most “bulk” materials. Superlattices composed of alternating atomically thin materials offer control over crystal anisotropy through changes in composition, optical phonon confinement, and the emergence of new modes. In particular, the modified optical phonons in superlattices offer the potential for so-called crystalline hybrids whose IR properties cannot be described as a simple mixture of the bulk constituents. To date, however, studies have primarily focused on identifying the presence of new or modified optical phonon modes rather than assessing their impact on the IR response. Here, this study focuses on assessing the impact of confined optical phonon modes on the hybrid IR dielectric function in superlattices of GaSb and AlSb. Using a combination of first principles theory, Raman, FTIR, and spectroscopic ellipsometry, the hybrid dielectric function is found to track the confinement of optical phonons, leading to optical phonon spectral shifts of up to 20 cm -1 . These results provide an alternative pathway toward designer IR optical materials.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Stoichiometric Control and Optical Properties of BaTiO 3 Thin Films Grown by Hybrid MBE

BaTiO 3 is a technologically relevant material in the perovskite oxide class with above-room-temperature ferroelectricity and a very large electro-optical coefficient, making it highly suitable for emerging electronic and photonic devices. An easy, robust, straightforward, and scalable growth method is required to synthesize epitaxial BaTiO 3 thin films with sufficient control over the film's stoichiometry to achieve reproducible thin film properties. Here the growth of BaTiO 3 thin films by hybrid molecular beam epitaxy is reported. A self-regulated growth window is identified using complementary information obtained from reflection high energy electron diffraction, the intrinsic film lattice parameter, film surface morphology, and scanning transmission electron microscopy. Subsequent optical characterization of the BaTiO 3 films by spectroscopic ellipsometry revealed refractive index and extinction coefficient values closely resembling those of stoichiometric bulk BaTiO 3 crystals for films grown inside the growth window. Even in the absence of a lattice parameter change of BaTiO 3 thin films, degradation of optical properties is observed, accompanied by the appearance of a wide optical absorption peak in the IR spectrum, attributed to optical transitions involving defect states present. Therefore, the optical properties of BaTiO 3 can be utilized as a much finer and more straightforward probe to determine the stoichiometry level present in BaTiO 3 films.

36 MATERIALS SCIENCE↗