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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 739 records · Page 41
All sourcesNASA NTRSDOE OSTI
DOE OSTI2015

Impact of x-ray dose on track formation and data analysis for CR-39-based proton diagnostics

The nuclear track detector CR-39 is used extensively for charged particle diagnosis, in particular proton spectroscopy, at inertial confinement fusion facilities. These detectors can absorb x-ray doses from the experiments in the order of 1–100 Gy, the effects of which are not accounted for in the previous detector calibrations. X-ray dose absorbed in the CR-39 has previously been shown to affect the track size of alpha particles in the detector, primarily due to a measured reduction in the material bulk etch rate [Rojas-Herrera et al., Rev. Sci. Instrum. 86, 033501 (2015)]. Similar to the previous findings for alpha particles, protons with energies in the range 0.5–9.1 MeV are shown to produce tracks that are systematically smaller as a function of the absorbed x-ray dose in the CR-39. The reduction of track size due to x-ray dose is found to diminish with time between exposure and etching if the CR-39 is stored at ambient temperature, and complete recovery is observed after two weeks. Lastly, the impact of this effect on the analysis of data from existing CR-39-based proton diagnostics on OMEGA and the National Ignition Facility is evaluated and best practices are proposed for cases in which the effect of x rays is significant.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2018

Twin-Slot Antenna-Coupled Superconducting Ti Transition-Edge Sensor at 350 GHz

We have developed four-leg-supported superconducting Ti transition-edge sensors (TES) formed by KOH wet etching. Energy relaxation mechanism is changed from electron–phonon coupling to diffusive phonon after wet etching. The current–voltage curves of the same TES device were measured before and after wet etching. After wet etching, its thermal conductance (G) is reduced to 500 pW/K from 8950 pW/K. The measured effective response time (τ{sub eff}) is 143 μs, about 30 times larger. In addition, we have studied the optical noise equivalent power (NEP) with a cryogenic blackbody in combination with metal-mesh filters to define the radiation bandwidth. The obtained optical NEP is 5 × 10{sup −16} W/√Hz, which is suitable for ground-based astronomical applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2020

Evaluation and mitigation of trace 210Pb contamination on copper surfaces

Clean materials are required to construct and operate many low-background physics experiments. High-purity copper has found broad use because of its physical properties and availability. In this paper, we describe methods to assay and mitigate Pb-210 contamination on copper surfaces, such as from exposure to environmental radon or coming from bulk impurities. We evaluated the efficacy of wet etching on commercial samples and observed that Po-210 contamination from the copper bulk does not readily pass into solution. During the etch, the polonium appears to trap at the copper-etchant boundary, such that it is effectively concentrated at the copper surface. We observed a different behavior for Pb-210; high-sensitivity measurements of the alpha emissivity versus time indicate the lowest level of Pb-210 contamination ever reported for a commercial copper surface: 0 +/- 12 nBq/cm2 (1-sigma). Additionally, we have demonstrated the effectiveness of mitigating trace Pb-210 and Po-210 surface backgrounds using custom, high-purity electroplating techniques. These approaches were evaluated utilizing assays performed with an XIA UltraLo-1800 alpha spectrometer.

radon, copper, copper cleaning, dark matter, Pb-21↗
DOE OSTI2017

Deterministic Placement of Quantum-Size Controlled Quantum Dots for Seamless Top-Down Integration

We demonstrate a new route toward the integration and deterministic placement of quantum dots (QDs) within prepatterned nanostructures. Using standard electron-beam lithography (EBL) and inductively coupled plasma reactive-ion etching (ICP-RIE), we fabricate arrays of nanowires on a III-nitride platform. Next, we integrate QDs of controlled size within the prepatterned nanowires using a bandgap-selective, wet-etching technique: quantum-size-controlled photoelectrochemical (QSC-PEC) etching. Low-temperature microphotoluminescence (μ-PL) measurements of individual nanowires reveal sharp spectral signatures, indicative of QD formation. Further, internal quantum efficiency (IQE) measurements reveal a near order of magnitude improvement in emitter efficiency following QSC-PEC etching. Finally, second-order cross-correlation (g(2)(0)) measurements of individual QDs directly confirm nonclassical, antibunching behavior. Lastly, our results illustrate an exciting approach toward the top-down integration of nonclassical light sources within nanophotonic platforms.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Removal of {sup 222}Rn daughters from metal surfaces

Removal of the long-lived {sup 222}Rn daughters ({sup 210}Pb, {sup 210}Bi and {sup 210}Po) from copper, stainless steel and germanium surfaces was investigated. As cleaning techniques etching and electro-polishing was applied to samples in a form of discs exposed earlier to a strong radon source. Reduction of the {sup 210}Pb activity was tested using a HPGe spectrometer, for {sup 210}Bi a beta spectrometer and for {sup 210}Po an alpha spectrometer was used. According to the conducted measurements electro-polishing was always more efficient compared to etching and in case of copper the activity reduction factors for {sup 210}Pb, {sup 210}Bi and {sup 210}Po were between 200 and 400. Etching does not remove {sup 210}Po from copper but works very efficiently from germanium. Results obtained for {sup 210}Pb and {sup 210}Bi for etched stainless steel were worse but still slightly better than those achieved for copper.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Superluminescent light emitting diodes on naturally survived InGaN/GaN lateral nanowires

We demonstrate a method for nanowire formation by natural selection during wet anisotropic chemical etching in boiling phosphoric acid. Nanowires of sub-10 nm lateral dimensions and lengths of 700 nm or more are naturally formed during the wet etching due to the convergence of the nearby crystallographic hexagonal etch pits. These nanowires are site controlled when formed in augmentation with dry etching. Temperature and power dependent photoluminescence characterizations confirm excitonic transitions up to room temperature. The exciton confinement is enhanced by using two-dimensional confinement whereby enforcing greater overlap of the electron-hole wave-functions. The surviving nanowires have less defects and a small temperature variation of the output electroluminescent light. We have observed superluminescent behaviour of the light emitting diodes formed on these nanowires. There is no observable efficiency roll off for current densities up to 400 A/cm{sup 2}.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Al capping layers for nondestructive x-ray photoelectron spectroscopy analyses of transition-metal nitride thin films

X-ray photoelectron spectroscopy (XPS) compositional analyses of materials that have been air exposed typically require ion etching in order to remove contaminated surface layers. However, the etching step can lead to changes in sample surface and near-surface compositions due to preferential elemental sputter ejection and forward recoil implantation; this is a particular problem for metal/gas compounds and alloys such as nitrides and oxides. Here, the authors use TiN as a model system and compare XPS analysis results from three sets of polycrystalline TiN/Si(001) films deposited by reactive magnetron sputtering in a separate vacuum chamber. The films are either (1) air-exposed for ≤10 min prior to insertion into the ultrahigh-vacuum (UHV) XPS system; (2) air-exposed and subject to ion etching, using different ion energies and beam incidence angles, in the XPS chamber prior to analysis; or (3) Al-capped in-situ in the deposition system prior to air-exposure and loading into the XPS instrument. The authors show that thin, 1.5–6.0 nm, Al capping layers provide effective barriers to oxidation and contamination of TiN surfaces, thus allowing nondestructive acquisition of high-resolution core-level spectra representative of clean samples, and, hence, correct bonding assignments. The Ti 2p and N 1s satellite features, which are sensitive to ion bombardment, exhibit high intensities comparable to those obtained from single-crystal TiN/MgO(001) films grown and analyzed in-situ in a UHV XPS system and there is no indication of Al/TiN interfacial reactions. XPS-determined N/Ti concentrations acquired from Al/TiN samples agree very well with Rutherford backscattering and elastic recoil analysis results while ion-etched air-exposed samples exhibit strong N loss due to preferential resputtering. The intensities and shapes of the Ti 2p and N 1s core level signals from Al/TiN/Si(001) samples do not change following long-term (up to 70 days) exposure to ambient conditions, indicating that the thin Al capping layers provide stable surface passivation without spallation.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Chamber wall interactions with HBr/Cl{sub 2}/O{sub 2} plasmas

The authors have studied the interaction of HBr/Cl{sub 2}/O{sub 2} inductively coupled plasmas with reactor chamber wall deposits, with and without Si etching, using the “spinning wall” technique. The spinning wall is part of the reactor chamber walls, allowing near-real-time analysis of the composition of surface layers via Auger electron spectrometry and determination of species desorbing off the walls by mass spectrometry. In HBr plasmas with no bias voltage on the Si substrate, and hence no Si etching, HBr is ∼30% dissociated, and H{sub 2} and Br{sub 2} form in the plasma. Layers deposited on the reactor chamber contained little if any Br under these conditions. Adding O{sub 2} to an HBr plasma leads to formation of H{sub 2}O and increased Br{sub 2} (compared to a pure HBr plasma) products that desorb from the spinning wall. H{sub 2}O has a very long residence time on the surface. With bias voltage applied to the Si substrate in an HBr plasma, mass spectrometer signals are prominent for SiBr and SiBr{sub 3}, and weaker for SiBr{sub 2}, SiBr{sub 4}, Si{sub 2}Br{sub 4}, Si{sub 2}Br{sub 5}, and Si{sub 2}OBr{sub 5}. Under these conditions, a SiO{sub x}Br{sub y} layer deposits on the spinning wall. Adding 20% O{sub 2} to HBr stops etching and eliminates Br from the surface layer, indicating that Br on the reactor walls is a result of SiBr{sub x} impingement and not from bromination by impinging Br. With HBr/Cl{sub 2} plasmas and no bias on the stage, a SiO{sub x}Cl{sub y} layer deposits, and no Br is detected. HCl, BrCl, and Br{sub 2} were detected in the line-of-sight leak, around the spinning wall, of a HBr/Cl{sub 2} (1:1) gas mixture in the absence of a plasma. Residence time analysis of species in the chamber and a change in the product distribution with a change in the composition of the layer deposited on the chamber wall suggest that reactions forming these products in the absence of a plasma occur on the reactor walls. With a plasma and bias on the Si substrate, both Br and Cl incorporate in the layer, and a rich spectrum with numerous SiCl{sub x}Br{sub y} peaks was observed up to at least 500 amu. The spectrum does not change with the addition of 6% O{sub 2}. Adding 20% O{sub 2} suppresses Br adsorption, but Cl still adsorbs. In 40% O{sub 2}/HBr/Cl{sub 2} plasmas with stage bias, Cl adsorption also ceases and no etching products are observed in the mass spectrum.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Fabrication of high aspect ratio TiO{sub 2} and Al{sub 2}O{sub 3} nanogratings by atomic layer deposition

The authors report on the fabrication of TiO{sub 2} and Al{sub 2}O{sub 3} nanostructured gratings with an aspect ratio of up to 50. The gratings were made by a combination of atomic layer deposition (ALD) and dry etch techniques. The workflow included fabrication of a Si template using deep reactive ion etching followed by ALD of TiO{sub 2} or Al{sub 2}O{sub 3}. Then, the template was etched away using SF{sub 6} in an inductively coupled plasma tool, which resulted in the formation of isolated ALD coatings, thereby achieving high aspect ratio grating structures. SF{sub 6} plasma removes silicon selectively without any observable influence on TiO{sub 2} or Al{sub 2}O{sub 3}, thus revealing high selectivity throughout the fabrication. Scanning electron microscopy was used to analyze every fabrication step. Due to nonreleased stress in the ALD coatings, the top parts of the gratings were observed to bend inward as the Si template was removed, thus resulting in a gradual change in the pitch value of the structures. The pitch on top of the gratings is 400 nm, and it gradually reduces to 200 nm at the bottom. The form of the bending can be reshaped by Ar{sup +} ion beam etching. The chemical purity of the ALD grown materials was analyzed by x-ray photoelectron spectroscopy. The approach presented opens the possibility to fabricate high quality optical metamaterials and functional nanostructures.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Characteristic properties of macroporous silicon sintering in an argon atmosphere

The temperature and time dependences of the sintering of macroporous silicon in Ar or Ar + 3% H{sub 2} are studied. The contribution of various mechanisms governing this process is determined. The specific features of the sintering of macroporous silicon are examined by means of isochronous and isothermal annealing of the samples with ordered and random macropores in the temperature range 1000–1225°C. It is found that the sintering of macroporous silicon under atmospheric pressure in an inert gas flow containing 2 × 10–4% O{sub 2} is greatly affected by thermal etching. Thermal etching competes with the substance-transfer processes characteristic of sintering and hinders the formation of a defect-free surface crust. The reason for etching consists in that gaseous silicon monoxide is generated and then carried away by the gas flow. The etching effect is dominant in the low-temperature range and is independent of whether H{sub 2} is added. The values obtained for the activation energy of the silicon diffusion coefficient, E{sub a} = 2.57 eV, and for the exponent n = 3.31–3.74 in the time dependence of the pore radius, r ~ t{sup 1/n} are indicative of a mixed substance-transfer mechanism via the surface and volume diffusion of silicon atoms.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Investigation of differential surface removal due to electropolishing at JLab

Surface chemistry carried out for Superconducting Radio Frequency (SRF) cavities such as Buffered Chemical Polishing (BCP) and Electropolishing (EP) aims to uniformly remove the internal surface of a cavity along the entire structure and within each cell from equator to iris in order to obtain an equally etched surface. A uniform removal, however, is not readily achievable due to the complex fluid flow and varying temperatures of the acid mixture, which can lead to differential etching. This needs to be considered when envisaging a certain surface damage removal throughout the interior. The process-specific differential etching influences the target frequency set at the manufacturing stage as well as the field flatness and length of the as-built cavity. We report on analyses of JLab's present EP system using experimental data for six nine-cell cavities that have been processed recently in the frame of the LCLS-II high-Q development plan. In conjunction with numerical simulations, the differential etching and the impact on field flatness is assessed.

43 PARTICLE ACCELERATORS↗
DOE OSTI2023

Vapor‐Phase Infiltrated Organic–Inorganic Positive‐Tone Hybrid Photoresist for Extreme UV Lithography

Abstract Continuing extreme downscaling of semiconductor devices, essential for high performance and energy efficiency of future microelectronics, hinges on extreme ultraviolet lithography (EUVL) and addressing associated challenges. One of such challenges is a need for improved EUV photoresists featuring simultaneously high sensitivity, resolution, and etch selectivity. Here, a new, positive‐tone, organic–inorganic hybrid EUV photoresist is demonstrated that delivers a high‐resolution EUVL and electron‐beam lithography (EBL) patterning capability combined with high sensitivity and etch resistance. The new resist, poly(methyl methacrylate) infiltrated with indium oxide (PMMA‐InO x ), is synthesized via vapor‐phase infiltration (VPI), a material hybridization technique derived from atomic layer deposition. The weak binding of the gaseous indium precursor, trimethylindium, to the carbonyl group in PMMA allows the synthesis of hybrids with inorganic content distributed uniformly in the resist, enabling high EUVL and EBL sensitivities (18 mJ cm −2 and 300 µC cm −2 , respectively) and high‐resolution positive‐tone EUVL patterning (e.g., 40 nm half‐pitch line‐space and 50 nm diameter contact hole patterns) with high Si etch selectivity (>30–40). The low exposure doses required to pattern the PMMA‐InO x hybrid resist, high etch resistance, and processing strategies, which are developed, can pave the way for using infiltration‐synthesized hybrid thin films as reliable positive‐tone EUV photoresists for future semiconductor patterning.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Evolution of photoresist layer structure and surface morphology under fluorocarbon‐based plasma exposure

Abstract Ion bombardment of photoresist materials during plasma etching results in the formation of a surface dense amorphous carbon (DAC) layer that contributes to both etch resistance and the development of surface roughness. Real‐time ellipsometric measurements/analysis reveals that a C 4 F 8 ‐containing plasma interacts with an Ar‐plasma‐formed DAC layer to produce a modified DAC/fluorocarbon (FC) layer by FC deposition/diffusion of fluorine into the surface. The depletion of the DAC layer via modification and ion bombardment causes the etch rate of the bulk layer to increase. As the modified surface layer is formed, a noticeable decrease in surface roughness decrease is observed. These findings provide an understanding of the mechanisms of atomic layer etching processes in photoresist materials.

Pranda, Adam↗
DOE OSTI2020

Large-Scale Plasmonic Hybrid Framework with Built-In Nanohole Array as Multifunctional Optical Sensing Platforms

Light coupling with patterned subwavelength hole arrays induces enhanced transmission supported by the strong surface plasmon mode. In this work, a nanostructured plasmonic framework with vertically built-in nanohole arrays at deep-subwavelength scale (6 nm) is demonstrated using a two-step fabrication method. The nanohole arrays are formed first by the growth of a high-quality two-phase (i.e., Au–TiN) vertically aligned nanocomposite template, followed by selective wet-etching of the metal (Au). Such a plasmonic nanohole film owns high epitaxial quality with large surface coverage and the structure can be tailored as either fully etched or half-way etched nanoholes via careful control of the etching process. The chemically inert and plasmonic TiN plays a role in maintaining sharp hole boundary and preventing lattice distortion. Optical properties such as enhanced transmittance and anisotropic dielectric function in the visible regime are demonstrated. Numerical simulation suggests an extended surface plasmon mode and strong field enhancement at the hole edges. Furthermore, two demonstrations, including the enhanced and modulated photoluminescence by surface coupling with 2D perovskite nanoplates and the refractive index sensing by infiltrating immersion liquids, suggest the great potential of such plasmonic nanohole array for reusable surface plasmon-enhanced sensing applications.

42 ENGINEERING↗
DOE OSTI2021

Surfactant inhibition mechanisms of carbonate mineral dissolution in shale

Surfactants are common additives to hydraulic fracturing and enhanced oil recovery (EOR) fluids, and are under consideration for amendment to supercritical carbon dioxide for geological carbon sequestration (GCS). The effect of a common anionic surfactant, internal olefin sulfonate (IOS), on mineral dissolution from shale into brine was evaluated. When added to brine at concentrations exceeding the critical micelle concentration (94 mg/L), IOS inhibited carbonate mineral dissolution in an Eagle Ford shale, as well as dissolution of optical quality calcite (the dominant carbonate in the shale). Laser profilometry images provide spatial resolution across > 3 orders of magnitude, and indicate that IOS addition to brine both enhances the formation of new etch pits in calcite, and impedes their further growth. Time-of-flight secondary ion mass spectrometry surface profiles show for the first time that IOS preferentially adsorbs at calcite pit edges versus flat calcite surfaces (i.e., terraces). Surface pressure calculations, sulfur K-edge near edge X-ray absorption fine structure (NEXAFS) spectroscopy results, and density functional theory (DFT) calculations support this observation; the DFT results indicate that the sulfonate head group of the IOS molecule binds strongly to the calcite step site as compared to the terrace site. The S K-edge NEXAFS results indicate that IOS adsorbed more to etched calcite surfaces compared to smooth calcite surfaces. Overall, the results indicate that weak adsorption on flat calcite surfaces (i.e., terraces) disrupts water structure and enhances mass transfer of dissolution, while strong adsorption on calcite pit edges displaces adsorbed water and inhibits further etch pit growth. This work provides the first direct evidence of preferential adsorption of IOS to etched calcite surfaces and links it to macroscopic dissolution kinetics. Finally, this work has implications for surfactant-containing fluids used in hydraulic fracturing, EOR and potentially GCS for subsurface injection into carbonate rich reservoirs.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Characterization of surface layers formed on DU10Mo ingots after processing steps and high humidity exposure

The design of monolithic U-Mo fuel elements fabricated from low-enriched uranium for use in high-power research reactors requires bonding of the fuel foil to either Al cladding or a Zr barrier layer. Processing of the U-Mo ingot to final foil form has the potential to generate surface layers on the foil that differ from the bulk, metallic U-Mo. The interfacial properties between the U-Mo and Zr or Al cladding layers will then be determined by these surface layers. We use x-ray photoelectron spectroscopy, cross-sectional scanning electron microscopy, and atomic force microscopy to characterize the composition, oxidation state, and morphology of the surface layers that form after hot rolling and cold rolling depleted U–10 wt% Mo alloy (DU10Mo). A thick uranium nitride layer is observed after hot rolling, although its origin is likely from a previous processing step. The surface composition of cold-rolled DU10Mo varied significantly between two foils, with a strongly Mo-depleted surface oxide layer observed on one foil but nominal Mo composition observed on the other. The efficacy of acid etching in HNO 3 is compared to that of electropolishing in H 2 SO 4 to remove the surface layers, and both methods are found to be similarly effective. Both laboratory (low humidity) air exposure and longer rinse times in water are shown to promote the formation of surface oxide layers. Exposure of both acid-etched and electropolished DU10Mo foils to humid air (97% relative humidity) for six weeks results in formation of a thick oxide layer due to corrosion. The oxide layer on the acid-etched foil is thicker and more highly oxidized than the oxide layer that forms on the electropolished foil, and these differences in oxidation behavior are attributed to higher surface roughness on the acid-etched foil. In general, Mo is found to play a role as a sacrificial element, typically exhibiting a larger ratio of Mo 6+ / Mo 4+ than U 6+ / U 4+ . This is unexpected, given the greater thermodynamic driving force to form U oxides than Mo oxides.

Kaspar, Tiffany C. (ORCID:0000000328167569)↗
DOE OSTI2022

Fabrication methods for high reflectance dielectric-metal point contact rear mirror for optoelectronic devices

The patterned dielectric back contact (PDBC) structure can be used to form a point-contact architecture that features a dielectric spacer with spatially distributed, reduced-area metal point contacts between the semiconductor back not recognized contact layer and the metal back contact. In this structure, the dielectric-metal region provides higher reflectance and is electrically insulating. Reduced-area metal point contacts provide electrical conduction for the back contact but typically have lower reflectance. The fabrication methods discussed in this article were developed for thermophotovoltaic cells, but they apply to any III-V optoelectronic device requiring the use of a conductive and highly reflective back contact. Patterned dielectric back contacts may be used for enhanced sub-bandgap reflectance, for enhanced photon recycling near the bandgap energy, or both depending on the optoelectronic application. The following fabrication methods are discussed in the article: PDBC fabrication procedures for spin-on dielectrics and commonly evaporated dielectrics to form the spacer layer; methods to selectively etch a parasitically absorbing back contact layer using metal point contacts as an etch mask; methods incorporating a dielectric etch through different process techniques such as reactive ion and wet etching.

14 SOLAR ENERGY↗