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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 253 records · Page 14
All sourcesNASA NTRSDOE OSTI
NASA NTRS1982

Pre- and post-annealing of mechanical damage in silicon wafers

Basic properties of mechanical damage in silicon consisting of cracks and abrasion were studied using transmission electron microscopy. The crystallographic structure of mechanical damage was determined before and after high temperature annealing. The main findings include that stresses in silicon around crack tips are not plastically relieved at room temperature and that abrasion at room temperature introduces shear loops into the silicon. It was also found that cracks of micron size can be annealed out, specifically, if cleavage occurs on 111 planes. The healing products of such cracks are 60 deg and 90 deg dislocations. Submicron cracks transform into stacking faults during annealing. Likewise high concentrations of shear loops due abrasion were found to anneal into stacking faults. A one to one correlation between surface areas containing small cracks and stacking faults was made. Measurements of damage removal on silicon surfaces through chemical-mechanical etching techniques are presented. It is shown that silicon dioxide repolishes damaged silicon surfaces most effectively.

Schwottke, G. H.↗
NASA NTRS2003

The Evaluation of High Temperature Adhesive Bonding Processes for Rocket Engine Combustion Chamber Applications

NASA Glenn Research Center is currently evaluating the possibility of using high- temperature polymer matrix composites to reinforce the combustion chamber of a rocket engine. One potential design utilizes a honeycomb structure composed of a PMR-II- 50/M40J 4HS composite facesheet and titanium honeycomb core to reinforce a stainless steel shell. In order to properly fabricate this structure, adhesive bond PMR-II-50 composite. Proper prebond surface preparation is critical in order to obtain an acceptable adhesive bond. Improperly treated surfaces will exhibit decreased bond strength and durability, especially in metallic bonds where interface are susceptible to degradation due to heat and moisture. Most treatments for titanium and stainless steel alloys require the use of strong chemicals to etch and clean the surface. This processes are difficult to perform due to limited processing facilities as well as safety and environmental risks and they do not consistently yield optimum bond durability. Boeing Phantom Works previously developed sol-gel surface preparations for titanium alloys using a PETI-5 based polyimide adhesive. In support of part of NASA Glenn Research Center, UDRI and Boeing Phantom Works evaluated variations of this high temperature sol-gel surface preparation, primer type, and primer cure conditions on the adhesion performance of titanium and stainless steel using Cytec FM 680-1 polyimide adhesive. It was also found that a modified cure cycle of the FM 680-1 adhesive, i.e., 4 hrs at 370 F in vacuum + post cure, significantly increased the adhesion strength compared to the manufacturer's suggested cure cycle. In addition, the surface preparation of the PMR-II-50 composite was evaluated in terms of surface cleanness and roughness. This presentation will discuss the results of strength and durability testing conducted on titanium, stainless steel, and PMR-II-50 composite adherends to evaluate possible bonding processes.

McCray, Daniel↗
NASA NTRS2011

Tissue Photolithography

Tissue lithography will enable physicians and researchers to obtain macromolecules with high purity (greater than 90 percent) from desired cells in conventionally processed, clinical tissues by simply annotating the desired cells on a computer screen. After identifying the desired cells, a suitable lithography mask will be generated to protect the contents of the desired cells while allowing destruction of all undesired cells by irradiation with ultraviolet light. The DNA from the protected cells can be used in a number of downstream applications including DNA sequencing. The purity (i.e., macromolecules isolated form specific cell types) of such specimens will greatly enhance the value and information of downstream applications. In this method, the specific cells are isolated on a microscope slide using photolithography, which will be faster, more specific, and less expensive than current methods. It relies on the fact that many biological molecules such as DNA are photosensitive and can be destroyed by ultraviolet irradiation. Therefore, it is possible to protect the contents of desired cells, yet destroy undesired cells. This approach leverages the technologies of the microelectronics industry, which can make features smaller than 1 micrometer with photolithography. A variety of ways has been created to achieve identification of the desired cell, and also to designate the other cells for destruction. This can be accomplished through chrome masks, direct laser writing, and also active masking using dynamic arrays. Image recognition is envisioned as one method for identifying cell nuclei and cell membranes. The pathologist can identify the cells of interest using a microscopic computerized image of the slide, and appropriate custom software. In one of the approaches described in this work, the software converts the selection into a digital mask that can be fed into a direct laser writer, e.g. the Heidelberg DWL66. Such a machine uses a metalized glass plate (with chrome metallization) on which there is a thin layer of photoresist. The laser transfers the digital mask onto the photoresist by direct writing, with typical best resolution of 2 micrometers. The plate is then developed to remove the exposed photoresist, which leaves the exposed areas susceptible to chemical chrome etch. The etch removes the unprotected chrome. The rest of the photoresist is then removed, by either ultraviolet organic solvent or over-development. The remaining chrome pattern is quickly oxidized by atmospheric exposure (typically within 30 seconds). The ready chrome mask is now applied to the tissue slide and aligned manually, or using automatic software and pre-designed alignment marks. The slide plate sandwich is then exposed to UV to destroy the DNA of the unwanted cells. The slide and plate are separated and the slide is processed in a standard way to prepare for polymerase chain reaction (PCR) and potential identification of cancer sequences.

Wade, Lawrence A.↗
DOE OSTI2020

ScAIN etch mask for highly selective etching

A fabrication process employing the use of ScAlN as an etch mask is disclosed. The ScAlN etch mask is chemically nonvolatile in fluorine-based etch chemistries and has a low sputter yield, resulting in greater etch mask selectivity and reduced surface roughness for silicon and other semiconductor materials. The ScAlN etch mask has an etch mask selectivity of greater than 200,000:1 relative to silicon compared to an etch mask selectivity of less than 40,000:1 for a prior art AlN etch mask relative to silicon. Further, due to reduced sputtering of the ScAlN etch mask, and thus reduced micromasking, the ScAlN etch mask yielded a surface roughness of 0.6 μm compared to a surface roughness of 2.8 μm for an AlN etch mask.

36 MATERIALS SCIENCE↗
NASA NTRS2005

Structures Self-Assembled Through Directional Solidification

Nanotechnology has created a demand for new fabrication methods with an emphasis on simple, low-cost techniques. Directional solidification of eutectics (DSE) is an unconventional approach in comparison to low-temperature biomimetic approaches. A technical challenge for DSE is producing microstructural architectures on the nanometer scale. In both processes, the driving force is the minimization of Gibb's free energy. Selfassembly by biomimetic approaches depends on weak interaction forces between organic molecules to define the architectural structure. The architectural structure for solidification depends on strong chemical bonding between atoms. Constituents partition into atomic-level arrangements at the liquid-solid interface to form polyphase structures, and this atomic-level arrangement at the liquid-solid interface is controlled by atomic diffusion and total undercooling due to composition (diffusion), kinetics, and curvature of the boundary phases. Judicious selection of the materials system and control of the total undercooling are the keys to producing structures on the nanometer scale. The silicon-titanium silicide (Si-TiSi2) eutectic forms a rod structure under isothermal cooling conditions. At the NASA Glenn Research Center, directional solidification was employed along with a thermal gradient to promote uniform rods oriented with the thermal gradient. The preceding photomicrograph shows the typical transverse microstructure of a solidified Si-TiSi2 eutectic composition. The dark and light gray regions are Si and TiSi2, respectively. Preferred rod orientation along the thermal gradient was poor. The ordered TiSi2 rods have a narrow distribution in diameter of 2 to 3 m, as shown. The rod diameter showed a weak dependence on process conditions. Anisotropic etch behavior between different phases provides the opportunity to fabricate structures with high aspect ratios. The photomicrographs show the resulting microstructure after a wet chemical etch and a dry plasma etch. The wet chemical etches the silicon away, exposing the TiSi2 rods, whereas plasma etching preferentially etches the Si-TiSi2 interface to form a crater. The porous architectures are applicable to fabricating microdevices or creating templates for part fabrication. The porous rod structure can serve as a platform for fabricating microplasma devices for propulsion or microheat exchangers and for fabricating microfilters for miniatured chemical reactors. Although more work is required, self-assembly from DSE can have a role in microdevice fabrication.

Dynys, Frederick W.↗
DOE OSTI2021

Highly efficient ultra-low blaze angle multilayer grating

We have developed an advanced process for blaze angle reduction of x-ray gratings for the soft, tender, and EUV spectral ranges. The process is based on planarization of an anisotropically etched Si blazed grating followed by a chemically selective plasma etch. This provides a way to adjust the blaze angle to any lower value with high accuracy. Here we demonstrate the reduction of the blaze angle to an extremely low value of 0.04°±0.004°. For a 100 lines/mm grating with a Mo/Si multilayer coating, the grating exhibits diffraction efficiency of 58% in the 1 st diffraction order at a wavelength of 13.3 nm. This technique will be applicable to a wide range of uses of high efficiency gratings for synchrotron sources, as well as for Free Electron Lasers (FEL).

42 ENGINEERING↗
DOE OSTI2023

Enhanced internal condensation of R1233zd(E) on micro- and nanostructured copper and aluminum surfaces

In-tube condensation of refrigerants is an important process which affects thermal efficiency in many applications, ranging from refrigeration and air conditioning to electronics thermal management. In-tube heat transfer and pressure drop are important to heat exchanger sizing and design. Here, in this work, micro- and nanostructured surfaces are applied to the internal wetted areas of copper and aluminum mini-channels to enhance the condensation heat transfer coefficient of hydrofluorocarbon R1233zd(E) refrigerant. To achieve scalable nanomanufacturing, surfaces were uniformly structured by relying on hydrochloric acid etching of aluminum and chemical oxidation of copper. The etched aluminum surfaces exhibited a 150% increase in heat transfer coefficient compared to smooth aluminum channels at specific qualities, with a 66% heat transfer coefficient improvement for complete phase change from saturated vapor to saturated liquid. Copper oxide structures showed no discernable difference in thermal-hydraulic performance when compared to smooth copper channels. Critical dimensionless parameters governing the heat transfer enhancement were identified by varying the tube internal diameter (2.3 mm to 4.7 mm), refrigerant mass flux (50 to 300 kg/(m 2 ·s)), and refrigerant quality (0 to 1). The dimensionless parameters include the Bond number normalized to the condensate film thickness, and the Weber number modified by the vapor friction factor. The relatively small increase in pressure drop (< 10%) associated with these surface enhancements further supports the promise of this method. The scalable and cost-effective techniques used to create these aluminum microstructures may reduce manufacturing cost when compared with current enhancement approaches such as extrusion, drawing, and welding.

42 ENGINEERING↗
NASA NTRS1989

Process For Patterning Dispenser-Cathode Surfaces

Several microfabrication techniques combined into process cutting slots 100 micrometer long and 1 to 5 micrometer wide into tungsten dispenser cathodes for traveling-wave tubes. Patterned photoresist serves as mask for etching underlying aluminum. Chemically-assisted ion-beam etching with chlorine removes exposed parts of aluminum layer. Etching with fluorine or chlorine trifluoride removes tungsten not masked by aluminum layer. Slots enable more-uniform low-work function coating dispensed to electron-emitting surface. Emission of electrons therefore becomes more uniform over cathode surface.

Garner, Charles E.↗
DOE OSTI2022

Multimodal analysis and characterization of the boehmite layer formed on AA6061 before and after alkaline etching

Low-enriched uranium (LEU) alloyed with 10% Mo (U-10Mo) is being considered as a promising alternative to oxide-based dispersion fuel with high-enriched uranium for use in research reactors. The configuration of this proposed LEU monolithic LEU fuel plate consists of a U-10Mo plate-type fuel foil with a 25 µm zirconium interlayer barrier clad with an aluminum alloy (AA6061). In certain research reactors, the clad AA6061 is coated with a boehmite layer to prevent corrosion. The boehmite layer has a high-pH passivation range, which makes it resistant to oxidation. Boehmite is usually formed on the AA6061 surface by autoclave processing. Before the boehmite layer is added, the surface of the AA6061 is cleaned using techniques such as polishing and wet etching. In this study, we use multimodal analysis to examine how pretreatment of AA6061 using polishing followed by alkaline etching affects the chemical composition of the boehmite layer. X-ray photoelectron microscopy (XPS), transmission electron microscopy (TEM), and x-ray diffraction (XRD) were used to study the chemical changes in the boehmite layer caused by alkaline etching pretreatment. XPS provides quantitative analysis for the Al:O ratio as well as oxidation states present on the surface, which suggests slight oxidation of the boehmite surface after alkaline etching of the AA6061 surface. We further explored this suggested oxidation of the boehmite surface using high-resolution transmission electron microscopy with selected area electron diffraction (SAED) and grazing incidence x-ray diffraction (GI-XRD), which suggested only a small amount of aluminum oxide at the surface. The multimodal analysis and imaging yielded new insights for optimizing boehmite growth on AA6061 for research reactors.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Alloy selective optical sorting of mixed post-consumer aluminum scrap streams

Shredded post-consumer non-ferrous scrap stream, also known as Zorba, contains a mixture of cast and wrought aluminum pieces with very different compositions. Cast Al pieces, with their high Si, Cu and Fe content, are a major contaminant in wrought scrap fraction, which results in downcycling of the mixed cast + wrought scrap into non-structural cast Al alloys and parts. Here, in this paper, we introduce a chemical treatment method to color-code scrap aluminum pieces by alloy family and demonstrate low-cost optical sorting of cast from wrought pieces to upgrade the scrap stream. We utilized non-acidic chemical solutions that react with (i.e., etch) the scrap pieces to produce colors based on the Al alloy chemistry of a given piece. Cast pieces with high Si and Cu fractions turned black, whereas the much leaner wrought pieces remained unreacted. We showed > 95% sorting efficiency of mixed cast and wrought pieces using a repurposed low-cost optical sorter originally designed for food sorting. We also colored wrought Al pieces by alloy families, such as 5xxx and 6xxx, using a two-step chemical etching technique, which has the potential to create a circular supply chain in which wrought aluminum alloys are sorted from the mixed scrap stream and recycled back to high-value wrought products such as sheets, extrusions, and forgings with minimal contamination from cast scrap.

Aluminum↗
NASA NTRS2005

Chemical Sensors Based on Optical Ring Resonators

Chemical sensors based on optical ring resonators are undergoing development. A ring resonator according to this concept is a closed-circuit dielectric optical waveguide. The outermost layer of this waveguide, analogous to the optical cladding layer on an optical fiber, is a made of a polymer that (1) has an index of refraction lower than that of the waveguide core and (2) absorbs chemicals from the surrounding air. The index of refraction of the polymer changes with the concentration of absorbed chemical( s). The resonator is designed to operate with relatively strong evanescent-wave coupling between the outer polymer layer and the electromagnetic field propagating along the waveguide core. By virtue of this coupling, the chemically induced change in index of refraction of the polymer causes a measurable shift in the resonance peaks of the ring. In a prototype that has been used to demonstrate the feasibility of this sensor concept, the ring resonator is a dielectric optical waveguide laid out along a closed path resembling a racetrack (see Figure 1). The prototype was fabricated on a silicon substrate by use of standard techniques of thermal oxidation, chemical vapor deposition, photolithography, etching, and spin coating. The prototype resonator waveguide features an inner cladding of SiO2, a core of SixNy, and a chemical-sensing outer cladding of ethyl cellulose. In addition to the ring Chemical sensors based on optical ring resonators are undergoing development. A ring resonator according to this concept is a closed-circuit dielectric optical waveguide. The outermost layer of this waveguide, analogous to the optical cladding layer on an optical fiber, is a made of a polymer that (1) has an index of refraction lower than that of the waveguide core and (2) absorbs chemicals from the surrounding air. The index of refraction of the polymer changes with the concentration of absorbed chemical( s). The resonator is designed to operate with relatively strong evanescent-wave coupling between the outer polymer layer and the electromagnetic field propagating along the waveguide core. By virtue of this coupling, the chemically induced change in index of refraction of the polymer causes a measurable shift in the resonance peaks of the ring. In a prototype that has been used to demonstrate the feasibility of this sensor concept, the ring resonator is a dielectric optical waveguide laid out along a closed path resembling a racetrack (see Figure 1). The prototype was fabricated on a silicon substrate by use of standard techniques of thermal oxidation, chemical vapor deposition, photolithography, etching, and spin coating. The prototype resonator waveguide features an inner cladding of SiO2, a core of SixNy, and a chemical-sensing outer cladding of ethyl cellulose. In addition to the ring res

Homer, Margie↗
NASA NTRS1999

Computational Study of Field Initiated Surface Reactions for Synthesis of Diamond and Silicon

This project involves using quantum chemistry to simulate surface chemical reactions in the presence of an electric field for nanofabrication of diamond and silicon. A field delivered by a scanning tunneling microscope (STM) to a nanometer scale region of a surface affects chemical reaction potential energy surfaces (PES) to direct atomic scale surface modification to fabricate sub-nanometer structures. Our original hypothesis is that the applied voltage polarizes the charge distribution of the valence electrons and that these distorted molecular orbitals can be manipulated with the STM so as to change the relative stabilities of the electronic configurations over the reaction coordinates and thus the topology of the PES and reaction kinetics. Our objective is to investigate the effect of applied bias on surface reactions and the extent to which STM delivered fields can be used to direct surface chemical reactions on an atomic scale on diamond and silicon. To analyze the fundamentals of field induced chemistry and to investigate the application of this technique for the fabrication of nanostructures, we have employed methods capable of accurately describing molecular electronic structure. The methods we employ are density functional theory (DFT) quantum chemical (QC) methods. To determine the effect of applied bias on surface reactions we have calculated the QC PESs in various applied external fields for various reaction steps for depositing or etching diamond and silicon. We have chosen reactions which are thought to play a role in etching and the chemical vapor deposition growth of Si and diamond. The PESs of the elementary reaction steps involved are then calculated under the applied fields, which we vary in magnitude and configuration. We pay special attention to the change in the reaction barriers, and transition state locations, and search for low energy reaction channels which were inaccessible without the applied bias.

Musgrave, Charles Bruce↗
DOE OSTI2022

ICP etching of GaN microstructures in a Cl 2 –Ar plasma with subnanometer-scale sidewall surface roughness

In this work, substrate temperature, RF power, and ICP power were investigated for their effects on GaN micropillar sidewall roughness and etch characteristics. Elevated substrate temperature was shown to improve the sidewall etch morphology at low RF powers (reduced physical bombardment) and low ICP powers (lower plasma densities). Increased lateral etching is observed with both increased ICP power and substrate temperature, which both act to increase the chemical component of the etch. Etch conditions with a high chemical driving force resulted in faceting along the a-plane on the sidewalls. This faceting produced extremely smooth surfaces with root-meansquare roughness (R q ) as low as 0.20 nm which is comparable to typical epitaxy-ready surfaces and smaller than the a-plane lattice spacing of 0.3186 nm. The smooth surfaces produced in this study enable possibilities for laser facets or for new device structures that require high quality surfaces for GaN regrowth.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Evidence for anti-synergism between ion-assisted etching and in-plasma photoassisted etching of silicon in a high-density chlorine plasma

Etching of p-Si in 60 mTorr 10%Cl2/90%Ar Faraday-shielded inductively coupled high density plasmas was investigated under both ionassisted etching (IAE) and photoassisted etching (PAE) conditions. Real-time etching rates and after-etching Si surface chemical compositions were obtained by laser interferometry and vacuum-transfer x-ray photoelectron spectroscopy (XPS), respectively. Precisely controlled ion energy distributions (IEDs) were generated by applying pulsed negative DC bias on the conductive sample stage. Above a 36 eV threshold at a total flow rate of 250 SCCM, the IAE rate increased with the square root of the ion energy. In contrast to the DC bias, etching under RF bias did not exhibit a threshold ion energy because of the wide IED. XPS spectra revealed that the surface layer under PAE conditions had a significantly lower chlorine content, composed of only SiCl. Under IAE conditions, however, silicon dangling bonds (Si•), SiCl 2 , and SiCl 3 were found on the surface, in addition to SiCl, with a relative abundance of SiCl > SiCl 2 , and SiCl 3 . The absence of higher chlorides and Si• under PAE conditions suggested that vacuum ultraviolet photons and above threshold-energy ions interact with the surface very differently. By varying the duty cycle of the pulsed DC bias, it was found that the IAE rate scaled with the energetic ion dose, but only for low duty cycles. For higher duty cycles, the apparent IAE yield fell off with an increasing Cl coverage on the surface, as the duty cycle went up, which pointed to a negative synergy (antisynergism) between PAE and IAE as the explanation. This antisynergism was further supported by the observed decrease of the total etching rate with an increasing period of the pulsed DC bias. A plausible mechanism is that increasing the pulsing period causes more near-surface damage, creating more recombination centers that lead to a higher loss rate of electron-hole pairs through recombination, thereby reducing the PAE rate.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
NASA NTRS1990

Single-ended output GaAs/AlGaAs single quantum well laser with a dry-etched corner reflector

GaAs/AlGaAs single quantum well lasers with integrated corner reflectors have been fabricated using chemically assisted ion beam etching. The air-GaAs interface is internally totally reflecting, and no coherent radiation is transmitted through the corner reflector. The corner reflector laser was compared with a conventional Fabry-Perot laser cleaved from the same wafer. An 11-percent reduction in threshold current and a reduction of the far-field angle from 4.4 deg to 0.7 deg was measured.

Hagberg, M.↗
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↗