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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.

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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Chemical abrasion: the mechanics of zircon dissolution

Chemical abrasion is a technique that combines thermal annealing and partial dissolution in hydrofluoric acid (HF) to selectively remove radiation-damaged portions of zircon crystals prior to U–Pb isotopic analysis, and it is applied ubiquitously to zircon prior to U–Pb isotope dilution thermal ionization mass spectrometry (ID-TIMS). The mechanics of zircon dissolution in HF and the impact of different leaching conditions on the zircon structure, however, are poorly resolved. We present a microstructural investigation that integrates microscale X-ray computed tomography (µCT), scanning electron microscopy, and Raman spectroscopy to evaluate zircon dissolution in HF. We show that µCT is an effective tool for imaging metamictization and complex dissolution networks in three dimensions. Acid frequently reaches crystal interiors via fractures spatially associated with radiation damage zoning and inclusions to dissolve soluble high-U zones, some inclusions, and material around fractures, leaving behind a more crystalline zircon residue. Other acid paths to crystal cores include the dissolution of surface-reaching inclusions and the percolation of acid across zones with high defect densities. In highly crystalline samples dissolution is crystallographically controlled with dissolution proceeding almost exclusively along the c axis. Increasing the leaching temperature from 180 to 210 °C results in deeper etching textures, wider acid paths, more complex internal dissolution networks, and greater volume losses. How a grain dissolves strongly depends on its initial radiation damage content and defect distribution as well as the size and position of inclusions. As such, the effectiveness of any chemical abrasion protocol for ID-TIMS U–Pb geochronology is likely sample-dependent. We also briefly discuss the implications of our findings for deep-time (U-Th)/He thermochronology.

58 GEOSCIENCES↗
NASA NTRS1981

Highlights of 10th plasma chemistry meeting

The chemical structure is given of a film formed by plasma polymerization from pyridine monomers. The film has a hydrophilic chemical structure, its molecular weight is 900, and the molecular system is C55H50N10O3. The electrical characteristics of a plasma polymerized film are described. The film has good insulating properties and was successfully applied as video disc coating. Etching resistance properties make it possible to use the film as a resist in etching. The characteristics of plasma polymer formed from monomers containing tetramethyltin are discussed. The polymer is in film form, displays good adhesiveness, is similar to UV film UV 35 in light absorption and is highly insulating.

Kitamura, K.↗
DOE OSTI2025

Si–Cl 2 –Ar + Atomic Layer Etching Window: A Fundamental Study Using Molecular Dynamics Simulations and a Reduced Order Model

Silicon (Si) atomic layer etching (ALE) by alternating exposure to chlorine gas (Cl 2 ) and argon ions (Ar + ) is studied by using molecular dynamics (MD) simulations and a reduced order model (ROM). Here, the purpose of this study is to elucidate the properties of the ALE window, a range of ion energies where the amount of Si etched over a series of cycles is nonzero and nearly independent of ion energy. Experimental studies of the Si–Cl 2 –Ar + ALE system report contradictory results related to the ALE window’s ion energy range. Both MD simulations and the ROM show that there is an ALE window present from approximately 15 to 20 eV for normal incidence argon ions. The Si–Cl 2 –Ar + system, therefore, exhibits a narrow ALE window. The amount of Si etched per cycle is less than one atomic layer because of the higher etch yield of Cl atoms relative to atomic Si and silicon chlorides. A modified version of the ROM with an artificially increased Si physical sputtering threshold energy expands the ALE window, illustrating the importance of the difference in chemical and physical sputtering threshold energies in the ALE window energy range. The ROM is also used to examine the dependence of the EPC on the Ar + ion fluence.

energy↗
NASA NTRS1993

Method for producing a hybridization of detector array and integrated circuit for readout

A process is explained for fabricating a detector array in a layer of semiconductor material on one substrate and an integrated readout circuit in a layer of semiconductor material on a separate substrate in order to select semiconductor material for optimum performance of each structure, such as GaAs for the detector array and Si for the integrated readout circuit. The detector array layer is lifted off its substrate, laminated on the metallized surface on the integrated surface, etched with reticulating channels to the surface of the integrated circuit, and provided with interconnections between the detector array pixels and the integrated readout circuit through the channels. The adhesive material for the lamination is selected to be chemically stable to provide electrical and thermal insulation and to provide stress release between the two structures fabricated in semiconductor materials that may have different coefficients of thermal expansion.

Fossum, Eric R.↗
DOE OSTI2022

Unveiling the Degradation Mechanism of High-Temperature Superconductor Bi 2 Sr 2 CaCu 2 O 8+δ in Water-Bearing Environments

We report the physical properties of copper oxide high-temperature superconductors have been studied extensively, such as its band structure, and doping effects of Bi 2 Sr 2 CaCu 2 O 8+δ (Bi-2212). However, some chemical-related properties of these superconductors are rarely reported, such as their stability in air. Here, we report experiments combined with ab initio calculations that address the effects of water in contact with Bi-2212. The evolution of Bi-2212 flake with exposure to water for different time intervals were tested and characterized by optical microscopy (OM), atomic force microscopy (AFM), Raman spectroscopy, transmission electron microscopy (TEM) and electrical measurements. The thickness of Bi-2212 flakes is gradually decreased in water, and some thin flakes can be completely etched away after a few days. The stability of Bi-2212 in other solvents is also evaluated, including alcohol, acetone, HCl and KOH. The morphology of Bi-2212 flakes is relatively stable in organic solvents. However, the flakes are etched relatively quick in HCl and KOH, especially in acidic environment. Our results imply that hydrogen ion is primarily responsible for the deterioration of their properties. Both TEM and calculation results demonstrate that the atoms in Bi-O plane is relatively stable when compared to the inner atoms in Sr-O, Ca-O and Cu-O planes. This work contributes towards understanding the chemical stability of Bi-2212 superconducting device in environmental medium, which is important for both fundamental studies and practical applications of copper oxide high-temperature superconductors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRS1991

The interactions of atmospheric cosmogenic radionuclides with spacecraft surfaces

The discovery of the cosmogenic radionuclide Be-7 on the front surface (and the front surface only) of the Long Duration Exposure Facility (LDEF) spacecraft has opened opportunities to investigate new phenomena in several disciplines of space science. The experiments performed for this work show that the Be-7 results only if the source of the isotope is the atmosphere through which the spacecraft passed. We should expect that the uptake of beryllium in such circumstances will depend on the chemical form of the Be and the chemical nature of the substrate. It was found that the observed concentration of Be-7 does, in fact, differ between metal surfaces and organic surfaces such as PTFE (teflon). It is noted, however, that: (1) organic surfaces, even PTFE, are etched by the atomic oxygen found under these orbital conditions, and (2) the relative velocity of the species is 8 km(exp -1)s relative to the surface and the interaction chemistry and physics may differ from the norm. The Be-7 is formed by spallation of O and N nuclei under cosmic ray proton bombardment. The principal source region is at altitudes of 12-15 km. While very small quantities are produced above 300 km, the amount measured on the LDEF was 3 to 4 orders of magnitude higher than expected from production at orbital attitude. The most reasonable explanation is that Be-7 is rapidly transported from low altitudes by some unknown mechanism. The process must take place on a time scale similar to the half-life of the isotope (53 days). Many other isotopes are produced by cosmic ray reactions, and some of these are suited to measurement by the extremely sensitive methods of accelerator mass spectrometry. A program was initiated to search for these isotopes and it is hoped that such studies will provide new methods for studying mixing in the upper atmosphere.

Gregory, John C.↗
NASA NTRS1992

The interactions of atmospheric cosmogenic radionuclides with spacecraft surfaces

The discovery of the cosmogenic radionuclide Be-7 on the front surface of the Long Duration Exposure Facility (LDEF) spacecraft has opened opportunities to investigate new phenomena in several disciplines of space science. The experiments performed for this work show that the Be-7 results only if the source of the isotope is the atmosphere through which the spacecraft passed. We should expect that the uptake of beryllium in such circumstances will depend on the chemical form of the Be and the chemical nature of the substrate. It was found that the observed concentration of Be-7 does, in fact, differ between metal surfaces and organic surfaces such as PTFE (teflon). It is noted, however, that: (1) organic surfaces, even PTFE, are etched by the atomic oxygen found under these orbital conditions, and (2) the relative velocity of the species is 8 km(exp -1)s relative to the surface and the interaction chemistry and physics may differ from the norm. The Be-7 is formed by spallation of O and N nuclei under cosmic ray proton bombardment. The principal source region is at altitudes of 12-15 km. While very small quantities are produced above 300 km, the amount measured on the LDEF was 3 to 4 orders of magnitude higher than expected from production at orbital altitude. The most reasonable explanation is that Be-7 is rapidly transported from low altitudes by some unknown mechanism. The process must take place on a time scale similar to the half-life of the isotope (53 days). Many other isotopes are produced by cosmic ray reactions, and some of these are suited to measurement by the extremely sensitive methods of accelerator mass spectrometry. A program was initiated to search for these isotopes and it is hoped that such studies will provide new methods for studying mixing in the upper atmosphere.

Gregory, J. C.↗
DOE OSTI2024

Formation and Microwave Losses of Hydrides in Superconducting Niobium Thin Films Resulting from Fluoride Chemical Processing

Abstract Superconducting niobium (Nb) thin films have recently attracted significant attention due to their utility for quantum information technologies. In the processing of Nb thin films, fluoride‐based chemical etchants are commonly used to remove surface oxides that are known to affect superconducting quantum devices adversely. However, these same etchants can also introduce hydrogen to form Nb hydrides, potentially negatively impacting microwave loss performance. Here, comprehensive materials characterization of Nb hydrides formed in Nb thin films as a function of fluoride chemical treatments is presented. In particular, secondary‐ion mass spectrometry, X‐ray scattering, and transmission electron microscopy reveal the spatial distribution and phase transformation of Nb hydrides. The rate of hydride formation is determined by the fluoride solution acidity and the etch rate of Nb 2 O 5, which acts as a diffusion barrier for hydrogen into Nb. The resulting Nb hydrides are detrimental to Nb superconducting properties and lead to increased power‐independent microwave loss in coplanar waveguide resonators. However, Nb hydrides do not correlate with two‐level system loss or device aging mechanisms. Overall, this work provides insight into the formation of Nb hydrides and their role in microwave loss, thus guiding ongoing efforts to maximize coherence time in superconducting quantum devices.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of fabrication processes on BaTiO 3 capacitor properties

There is an increasing desire to utilize complex functional electronic materials such as ferroelectrics in next-generation microelectronics. As new materials are considered or introduced in this capacity, an understanding of how we can process these materials into those devices must be developed. Here, the effect of different fabrication processes on the ferroelectric and related properties of prototypical metal oxide (SrRuO 3 )/ferroelectric (BaTiO 3 )/metal oxide (SrRuO 3 ) heterostructures is explored. Two different types of etching processes are studied, namely, wet etching of the top SrRuO 3 using a NaIO 4 solution and dry etching using an Ar + -ion beam (i.e., ion milling). Polarization-electric-field hysteresis loops for capacitors produced using both methods are compared. For the ion-milling process, it is found that the Ar + beam can introduce defects into the SrRuO 3 /BaTiO 3 /SrRuO 3 devices and that the milling depth strongly influences the defect level and can induce a voltage imprint on the function. Realizing that such processing approaches may be necessary, work is performed to ameliorate the imprint of the hysteresis loops via ex situ “healing” of the process-induced defects by annealing the ferroelectric material in a barium-and-oxygen-rich environment via a chemical-vapor-deposition-style process. This work provides a pathway for the nanoscale fabrication of these candidate materials for next-generation memory and logic applications.

36 MATERIALS SCIENCE↗
NASA NTRS1990

Chemical removal of contaminants from thin film Bi4Sr3Ca3Cu4O(16 + x) surfaces

A solution of Br in absolute ethanol, previously shown to be effective in removing nonsuperconducting species from Y-Ba-Cu-O thin film surfaces, is shown also to be effective in treating Bi-Sr-Ca-Cu-O thin film surfaces. X-ray photoelectron spectra obtained after etching are consistent with previously reported results obtained from samples cleaved or scraped in vacuum.

Vasquez, R. P.↗
DOE OSTI2021

Reactivity of CO 2 with Utica, Marcellus, Barnett, and Eagle Ford Shales and Impact on Permeability

We report that in order to reduce greenhouse gas emissions while recovering hydrocarbons from unconventional shale formations, processes that make use of carbon dioxide to enhance oil recovery while storing carbon dioxide (CO 2 ) should be considered. Here, we examine samples from three shale basins across the United States (Utica and Marcellus Shales in the Appalachian Basin, Barnett Shale in the Bend Arch-Ft. Worth Basin, and Eagle Ford in the Western Gulf Basin) to address the following questions: (1) do changes from reaction with CO 2 and fluids at the micrometer and nanometer scale alter flow pathways and, in turn, impact hydrocarbon production, CO 2 storage, and seal integrity and (2) can CO 2 or fluid reactivity be predicted based on physical or chemical properties of shale formations? Experiments were conducted at 40 °C and 10.3 MPa to characterize the interaction between CO 2 and shale using X-ray diffraction (XRD), carbon and sulfur analysis, in situ Fourier transform infrared spectroscopy (FT-IR), feature relocation scanning electron microscopy coupled with energy-dispersive spectroscopy (SEM-EDS), mercury (Hg) intrusion porosimetry, and Brunauer-Emmett-Teller (BET) surface area and pore size analysis coupled with density functional theory (DFT) methods. Changes in mechanical, physical, and flow properties of shale cores due to CO 2 exposure were addressed using a New England Research Autolab 1500 and Xenon X-ray computed tomography (CT) scanning. Results showed that CO 2 did not promote significant reactivity with the shale if water was not present; only shales with swelling clays or residual interstitial pore water reacted with dry CO 2 to promote reactivity in shale. When water was added as a reactant, CO 2 formed carbonic acid and reacted with the shale to dissolve carbonate pockets, etched and pitted the shale matrix surfaces, and increased the microporosity and decreased nanoporosity. Porosity and permeability increased appreciably in core shale samples after exposure to CO 2 saturated fluid due to dissolution of carbonate. Shale mechanical properties were not altered. Trends were not observed that could tie CO 2 or fluid reactivity to physical or chemical properties of the shale formations at the basin scale from the samples we examined. However, if the shale contained significant amounts of carbonate and water was available to react with the CO 2 , pore sizes were altered in the matrix and permeability and porosity increased.

04 OIL SHALES AND TAR SANDS↗
DOE OSTI2020

Reaction of Hydrazine with Solution- and Vacuum-Prepared Selectively Terminated Si(100) Surfaces: Pathways to the Formation of Direct Si–N Bonds

Here, the reactivity of liquid hydrazine (N 2 H 4 ) with respect to H-, Cl-, and Br-terminated Si(100) surfaces was investigated to uncover the principles of nitrogen incorporation into the interface. This process has important implications in a wide variety of applications, including semiconductor surface passivation and functionalization, nitride growth, and many others. The use of hydrazine as a precursor allows for reactions that exclude carbon and oxygen, the primary sources of contamination in processing. In this work, the reactivity of N 2 H 4 with H- and Cl-terminated surfaces prepared by traditional solvent-based methods and with a Br-terminated Si(100) prepared in ultrahigh vacuum was compared. The reactions were studied with X-ray photoelectron spectroscopy, atomic force microscopy, and scanning tunneling microscopy, and the observations were supported by computational investigations. The H-terminated surface led to the highest level of nitrogen incorporation; however, the process proceeds with increasing surface roughness, suggesting possible etching or replacement reactions. In the case of Cl-terminated (predominantly dichloride) and Br-terminated (monobromide) surfaces, the amount of nitrogen incorporation on both surfaces after the reaction with hydrazine was very similar despite the differences in preparation, initial structure, and chemical composition. Density functional theory was used to propose the possible surface structures and to analyze surface reactivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Effect of Networking Density on the Patterning Performance of Molecular Layer Deposited Alucone Electron Beam/EUV Resists

One of the main barriers to continued device scaling in the era of extreme ultraviolet (EUV) lithography is the need for improved photoresist chemistries to address challenges such as poor EUV sensitivity, inadequate etch resistance, and pattern collapse. Metal-organic photoresists are a promising class of materials that can address many of these challenges, and among them, resists deposited via hybrid molecular layer deposition (MLD) have attracted interest for their unique advantages in thickness control, chemical homogeneity, and compatibility with vacuum processing. However, despite many successful demonstrations of patterning, little is known about how the molecular design of hybrid MLD resists affects their lithographic performance. In this work, we study the effect of the network structure, a common feature among all hybrid MLD resists, via a series of aluminum alkoxide ("alucone") negative tone resists with varying networking density. Their patterning mechanism is investigated via electron beam lithography (EBL)─a common proxy for EUV─and compared to their EUV-induced reactions studied via flood exposure and in situ characterization. In conclusion, we show that the resist with the least networking density demonstrates the best sensitivity and resolution, with the ability to resolve dense line/space gratings as small as 14 nm half pitch via EBL.

electron beam lithography↗
NASA NTRS1972

TiO2 film properties as a function of processing temperature, volume 3

Thin film TiO2 was produced at 150 C by chemical vapor deposition using hydrolysis of tetraisopropyl titanate. Films were amorphous as grown, but annealing in air caused crystallization, with anatase formed beginning at 350 C and rutile at 700 C. Density and index of refraction increased substantially with increasing anneal temperature, while etch susceptibility in HF and H2SO4 decreased. Comparison with literature data showed two groups of processes. One group yields films having properties that gradually approach those of rutile with increasing process temperature. The other group gives rutile directly at moderate temperatures. Deposition of amorphous film followed by etching and annealing is suggested as a means for pattern definition.

Fitzgibbons, E. T.↗
NASA NTRS1982

Long term compatibility of nitrogen tetroxide with metals - Results at the ten-year milestone

Analyses and results are reported of a test program to establish the effects of long-term (10 years or more) contact of materials with nitrogen textroxide MON-1 for the purpose of designing chemical propulsion system components which can be used for current as well as future planetary spacecraft. The test materials included aluminum alloy, corrosion-resistant steel, titanium alloy, and nickel. The weight and appearance of each specimen were observed, including the presence of deposits, etching, pitting, and cracking. Aluminum alloy and steel were rated satisfactory with minor reservations, titanium alloy was satisfactory, and nickel was unsatisfactory. Criteria for ratings are shown.

Moran, C. M.↗
NASA NTRS2005

Photochemically Etched Construction Technology Developed for Digital Xenon Feed Systems

Electric propulsion systems are quickly emerging as attractive options for primary propulsion in low Earth orbit, in geosynchronous orbit, and on interplanetary spacecraft. The driving force behind the acceptance of these systems is the substantial reduction in the propellant mass that can be realized. Unfortunately, system designers are often forced to utilize components designed for chemical propellants in their electric systems. Although functionally acceptable, these relatively large, heavy components are designed for the higher pressures and mass flow rates required by chemical systems. To fully realize the benefits of electric propulsion, researchers must develop components that are optimized for the low flow rates, critical leakage needs, low pressures, and limited budgets of these emerging systems.

Otsap, Ben↗
DOE OSTI2023

Corrosion characteristics of monolithic SiC materials in beryllium-bearing molten fluoride salt

In this work, chemical vapor deposited SiC single crystal and polycrystals were exposed to a static beryllium-bearing molten fluoride salt, 2LiF–BeF 2 for 500 and 1000 h at 750 °C. Overall, the single crystal and polycrystalline SiC materials experienced slight weight loss and nominal surface etching regardless of the material type. Localized pitting and nonuniform Si removal from surface regions were associated with trace metal impurities and oxygen. Cross-sectional observation revealed minimal subsurface changes in the microstructure. The corrosion damage processes were similar to those reported for molten LiF–KF–NaF salt with trace impurities, indicating that the impurities significantly affect SiC corrosion.

36 MATERIALS SCIENCE↗
NASA NTRS1989

Nonaqueous chemical depth profiling of YBa2Cu3O(7-x)

A nonaqueous solution of Br in absolute ethanol (EtOH) has recently been reported to be effective at removing nonsuperconducting surface species from YBa2Cu3O(7-x) films, leaving the surface close to the ideal stoichiometry. This same etchant is shown here to be an effective bulk etchant in chemical depth profiling through 1-micron-thick films. The Cu remains in the 2 + oxidation state and the stoichiometry, as determined by X-ray photoelectron spectroscopy, is close to ideal and nearly constant throughout the profile, indicating the absence of any large preferential etching effects. The reaction of YBa2Cu3O(7-x) films with HF/EtOH, HCl/EtOH, and I/EtOH solutions is also reported.

Vasquez, R. P.↗