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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 55 records · Page 3

Reduction of Defects in Germanium-Silicon

Crystals grown without contact with a container have far superior quality to otherwise similar crystals grown in direct contact with a container. In addition to float-zone processing, detached- Bridgman growth is a promising tool to improve crystal quality, without the limitations of float zoning or the defects introduced by normal Bridgman growth. Goals of this project include the development of the detached Bridgman process to be reproducible and well understood and to quantitatively compare the defect and impurity levels in crystals grown by these three methods. Germanium (Ge) and germanium-silicon (Ge-Si) alloys are being used. At MSFC, we are responsible for the detached Bridgman experiments intended to differentiate among proposed mechanisms of detachment, and to confirm or refine our understanding of detachment. Because the contact angle is critical to determining the conditions for detachment, the sessile drop method was used to measure the contact angles as a function of temperature and composition for a large number of substrates made of potential ampoule materials. Growth experiments have used pyrolytic boron nitride (pBN) and fused silica ampoules with the majority of the detached results occurring predictably in the pBN. Etch pit density (EPD) measurements of normal and detached Bridgman-grown Ge samples show a two order of magnitude improvement in the detached-grown samples. The nature and extent of detachment is determined by using profilometry in conjunction with optical and electron microscopy. The stability of detachment has been analyzed, and an empirical model for the conditions necessary to achieve sufficient stability to maintain detached growth for extended periods has been developed. We have investigated the effects on detachment of ampoule material, pressure difference above and below the melt, and Si concentration; samples that are nearly completely detached can be grown repeatedly in pBN. Current work is concentrated on developing a method to make in situ pressure measurements in the growth ampoules.

Source record↗

New Technology-Large-Area Three- Dimensional Surface Profiling Using Only Focused Air-Coupled Ultrasound-Given 1999 R&D 100 Award

Surface topography, which significantly affects the performance of many industrial components, is normally measured with diamond-tip profilometry over small areas or with optical scattering methods over larger areas. To develop air-coupled surface profilometry, the NASA Glenn Research Center at Lewis Field initiated a Space Act Agreement with Sonix, Inc., through two Glenn programs, the Advanced High Temperature Engine Materials Program (HITEMP) and COMMTECH. The work resulted in quantitative surface topography profiles obtained using only high-frequency, focused ultrasonic pulses in air. The method is nondestructive, noninvasive, and noncontact, and it does not require light-reflective surfaces. Air surface profiling may be desirable when diamond-tip or laserbased methods are impractical, such as over large areas, when a significant depth range is required, or for curved surfaces. When the configuration is optimized, the method is reasonably rapid and all the quantitative analysis facilities are online, including two- and three-dimensional visualization, extreme value filtering (for faulty data), and leveling.

Roth, Don J.↗

MAB Phase Ceramics for Lunar Applications

During the ten-week internship my work focused on designing characterization protocol for 3D printed MAB phase ceramics on steel and Tiplates. I was mentored by Dr. Samuel Hocker of NASA and advised by Dr. Gupta from University of North Dakota. I also collaborated with Mackenzie Short from the University of North Dakota. The characterization protocol was divided into following steps; initially, we performed visual inspection of the plates. During this process, the coatings which spalled or delaminated were discarded for further evaluation. During the next step, we performed optical microscopy to discern and document surface features and porosities of the samples. We also noted some decomposition under the optical microscope as well. Thereafter, profilometry analysis was performed to understand the effect of power density on the surface roughness. Due to the deposited powder over the samples, the profilometry was inconclusive. We then cleaned the samples on the steel plate using ethanol and cotton swabs to wipe up the loose powder covering the samples. Detailed SEM analysis was then performed on the cleaned specimens. In parallel, the 3D printed samples on the Tiplate were cleaned by using an ultrasonic bath for 1h. Optical imaging showed that this cleaning process was more effective for cleaning except that small cracks propagated through the layered ceramics. The profilometry data gathered on the titanium plate after cleaning was more conclusive. The SEM data on the steel plate showed that there is decomposition at all wattages although at 100 W the extent of decomposition was lower. We are planning to characterize the steel samples after cleaning in ultrasonic bath for 5-10 min to minimize cracking during the cleaning process. In addition, we are also planning to study the fractured surface by SEM analysis.

Additive Manufacturing, Laser Powder Bed Fusion, S↗

Thin film processing of photorefractive BaTiO3

During the period covered by this report, October 11, 1991 through October 10, 1992, the research has progressed in a number of different areas. The sol-gel technique was initially studied and experimentally evaluated for depositing films of BaTiO3. The difficulties with the precursors and the poor quality of the films deposited lead to the investigation of pulsed laser deposition as an alternative approach. The development of the pulsed laser deposition technique has resulted in continuous improvements to the quality of deposited films of BaTiO3. The initial depositions of BaTiO3 resulted in amorphous films, however, as the pulsed laser deposition technique continued to evolve, films were deposited in the polycrystalline state, then the textured polycrystalline state, and most recently heteroepitaxial films have also been successfully deposited on cubic (100) oriented SrTiO3 substrates. A technique for poling samples at room temperature and in air is also undergoing development with some very preliminary but positive results. The analytical techniques, which include x-ray diffraction, ferroelectric analysis, UV-Vis spectrophotometry, scanning electron microscopy with x-ray compositional analysis, optical and polarized light microscopy, and surface profilometry have been enhanced to allow for more detailed evaluation of the samples. In the area of optical characterization, a pulsed Nd:YAG laser has been incorporated into the experimental configuration. Now data can also be acquired within various temporal domains resulting in more detailed information on the optical response of the samples and on their photorefractive sensitivity. The recent establishment of collaborative efforts with two departments at Johns Hopkins University and the Army Research Lab at Fort Belvoir has also produced preliminary results using the metallo-organic decomposition technique as an alternative method for thin film processing of BaTiO3. RF and DC sputtering is another film deposition approach that should be initiated in the near future. Other techniques for optical characterization, which may even allow for intragrannular (within single grains) investigations, are also being considered.

Schuster, Paul R.↗

FAST Irradiations, Postirradiation Examinations, and Modeling of U-Mo for Light Water Reactor Applications

Many next generation light water reactor (LWR) concepts, such as mobile small modular reactors, are seeking to use smaller core dimensions than conventional reactor types. Smaller reactor cores require an increase in fissile material to maintain reactivity. For non-proliferation purposes, enrichment increases are limited to less than 20% (high assay low enriched uranium, [HALEU]) and so higher uranium density fuels than UO 2 must be considered. To this end, uranium-molybdenum alloys were tested using the Fission Accelerated Steady-state Test (FAST) approach. The experiment test matrix is focused on identifying the temperature transition between low swelling and high fission gas retention to break away swelling and low fission gas retention. This paper documents the results of irradiation tests and post-irradiation examinations (PIE) including neutron radiography, rodlet profilometry, fission gas collection analysis, and optical metallography. The results of these tests showed that unconstrained U-Mo fuels (solid, Na-bonded rodlets) have a swelling threshold between 400-450°C with minimal fission gas release below this point. Higher temperature solid fuel showed microstructural zoning with small pore networks while lower temperature solid fuels have a uniform microstructure with large pore networks. U-Annular Mo fuels where swelling had some self-constraint imposed upon it, were shown to have much reduced swelling compared to their solid counterparts as well as very low fission gas release for irradiation temperatures up to 500°C. These initial results show that the use of U-Mo in constrained fuel geometries could be used as a high uranium density HALEU fuel for LWRs.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

3-D Surface Depression Profiling Using High Frequency Focused Air-Coupled Ultrasonic Pulses

Surface topography is an important variable in the performance of many industrial components and is normally measured with diamond-tip profilometry over a small area or using optical scattering methods for larger area measurement. This article shows quantitative surface topography profiles as obtained using only high-frequency focused air-coupled ultrasonic pulses. The profiles were obtained using a profiling system developed by NASA Glenn Research Center and Sonix, Inc (via a formal cooperative agreement). (The air transducers are available as off-the-shelf items from several companies.) The method is simple and reproducible because it relies mainly on knowledge and constancy of the sound velocity through the air. The air transducer is scanned across the surface and sends pulses to the sample surface where they are reflected back from the surface along the same path as the incident wave. Time-of-flight images of the sample surface are acquired and converted to depth/surface profile images using the simple relation (d = V*t/2) between distance (d), time-of-flight (t), and the velocity of sound in air (V). The system has the ability to resolve surface depression variations as small as 25 microns, is useable over a 1.4 mm vertical depth range, and can profile large areas only limited by the scan limits of the particular ultrasonic system. (Best-case depth resolution is 0.25 microns which may be achievable with improved isolation from vibration and air currents.) The method using an optimized configuration is reasonably rapid and has all quantitative analysis facilities on-line including 2-D and 3-D visualization capability, extreme value filtering (for faulty data), and leveling capability. Air-coupled surface profilometry is applicable to plate-like and curved samples. In this article, results are shown for several proof-of-concept samples, plastic samples burned in microgravity on the STS-54 space shuttle mission, and a partially-coated cylindrical ceramic composite sample. Impressive results were obtained for all samples when compared with diamond-tip profiles and measurements from micrometers. The method is completely nondestructive, noninvasive, non-contact and does not require light-reflective surfaces.

Roth, Don J.↗

Growth and characterization of cubic SiC single-crystal films on Si

Morphological and electrical characterization results are presented for cubic SiC films grown by chemical vapor deposition on single-crystal Si substrates. The films, up to 40 microns thick, were characterized by optical microscopy, (SEM), (TEM), electron channeling, surface profilometry, and Hall measurements. A variety of morphological features observed on the SiC films are described. Electrical measurements showed a decrease in the electron mobility with increasing electron carrier concentration, similar to that observed in Si. Room-temperature electron mobilities up to 520 sq cm/V-s (at an electron carrier concentration of 5 x 10 to the 16th/cu cm) were measured. Finally, a number of parameters believed to be important in the growth process were investigated, and some discussion is given of their possible effects on the film characteristics.

Powell, J. Anthony↗

Using High Frequency Focused Water-Coupled Ultrasound for 3-D Surface Depression Profiling

Surface topography is an important variable in the performance of many industrial components and is normally measured with diamond-tip profilometry over a small area or using optical scattering methods for larger area measurement. A prior study was performed demonstrating that focused air-coupled ultrasound at 1 MHz was capable of profiling surfaces with 25 micron depth resolution and 400 micron lateral resolution over a 1.4 mm depth range. In this article, the question of whether higher-frequency focused water-coupled ultrasound can improve on these specifications is addressed. 10 and 25 MHz focused ultrasonic transducers were employed in the water-coupled mode. Time-of-flight images of the sample surface were acquired and converted to depth / surface profile images using the simple relation (d = V*t/2) between distance (d), time-of-flight (t), and the velocity of sound in water (V). Results are compared for the two frequencies used and with those from the 1 MHz air-coupled configuration.

Roth, Don J.↗

Analysis of surfaces from the LDEF A0114, phase 2

During the reporting period, work continued on profilometry measurements of eroded and corroded sample surfaces, optical transmission measurements, analysis of the pinhole camera, and x-ray photoelectron spectroscopy (XPS) analysis of some samples. Among metal samples, copper showed some interesting new results. There were two forms of copper samples: a thin film sputter-coated on fused silica and a solid piece of OFHC copper. They were characterized by x-ray and Auger electron spectroscopies, x-ray diffraction, and high resolution profilometry. Cu 2p core level spectra were used to demonstrate the presence of Cu2O and CuO and to determine the oxidation states.

Gregory, John C.↗

Analysis of surfaces from the LDEF A0114, phase 4

Progress made from 1 Mar. to 31 Aug. 1991 is presented. The work concentrated on profilometry measurements of eroded and corroded sample surfaces, optical transmission measurements, analysis of the pinhole camera, and x-ray photoelectron spectroscopic (XPS) analysis of some samples. The following papers are presented: (1) observation of Be-7 on the surface of the Long Duration Exposure Facility (LDEF) Spacecraft; (2) measurement of the passive attitude control performance of a recovered spacecraft; (3) effects on LDEF exposed copper flim and bulk; (4) measurements of erosion characteristics for metal and polymer surfaces using profilometry; (5) the interactions of atmospheric cosmogenic radionuclides with spacecraft surfaces; (6) pinhole cameras as sensors for atomic oxygen in orbit; and (7) interaction of atomic oxygen with solid surfaces in low earth orbit- results from LDEF experiment A0114.

Gregory, John C.↗

Analysis of surfaces from the LDEF A0114, phase 2

Analysis of surfaces from the Long Duration Exposure Facility (LDEF) continued during the reporting period. Work has continued on profilometry measurements of eroded and corroded sample surfaces, optical transmission measurements, analysis of the pinhole camera, and x-ray photoelectron spectroscopy (XPS) analysis of some samples. Papers that have appeared or have been accepted for publications are listed. Several of these papers and an abstact are included.

Gregory, John C.↗

Report on twisted nematic and supertwisted nematic device characterization program

In this study we measured the optical characteristics of normally white twisted nematic (NWTN) and super twisted nematic (STN ) cells. Though no dynamic computer model was available, the static observations were compared with computer simulated behavior. The measurements were taken as a function of both viewing angle and applied voltage and included in the static case not only luminance but also contrast ratio and chromaticity . We employed the computer model Twist Cell Optics, developed at Kent State in conjunction with this study, and whose optical modeling foundation, Iike the ViDEOS program, is the 4 x 4 matrix method of Berreman. In order to resolve discrepancies between the experimental and modeled data the optical parameters of the individual cell components, where not known, were determined using refractometry, profilometry, and various forms of ellipsometry. The resulting agreement between experiment and model is quite good due primarily to a better understanding of the structure and optics of dichroic sheet polarizers. A description of the model and test cells employed are given in section 2. Section 3 contains the experimental data gathered and section 4 gives examples of the fit between model and experiment. Also included with this report are a pair of papers which resulted from the research and which detail the polarizer properties and some of the cell characterization methods.

Source record↗

Qualification of a Null Lens Using Image-Based Phase Retrieval

In measuring the figure error of an aspheric optic using a null lens, the wavefront contribution from the null lens must be independently and accurately characterized in order to isolate the optical performance of the aspheric optic alone. Various techniques can be used to characterize such a null lens, including interferometry, profilometry and image-based methods. Only image-based methods, such as phase retrieval, can measure the null-lens wavefront in situ - in single-pass, and at the same conjugates and in the same alignment state in which the null lens will ultimately be used - with no additional optical components. Due to the intended purpose of a Dull lens (e.g., to null a large aspheric wavefront with a near-equal-but-opposite spherical wavefront), characterizing a null-lens wavefront presents several challenges to image-based phase retrieval: Large wavefront slopes and high-dynamic-range data decrease the capture range of phase-retrieval algorithms, increase the requirements on the fidelity of the forward model of the optical system, and make it difficult to extract diagnostic information (e.g., the system F/#) from the image data. In this paper, we present a study of these effects on phase-retrieval algorithms in the context of a null lens used in component development for the Climate Absolute Radiance and Refractivity Observatory (CLARREO) mission. Approaches for mitigation are also discussed.

Bolcar, Matthew R.↗

Measurements of erosion characteristics for metal and polymer surfaces using profilometry

The surfaces of many materials exposed in low earth orbit are modified due to interaction with atomic oxygen. Chemical changes and surface roughening effects can occur which alter optical and other properties. The experiment A0114 contained 128 solid surface samples, half of which were exposed on the front and half on the rear of LDEF. Each sample has been subjected to many analyses, but only the methods and techniques used to measure the changes in roughness, erosion depths, and material growth using profilometry are described.

Christl, Ligia C.↗

Measurements of erosion characteristics for metal and polymer surfaces using profilometry

The surfaces of many materials exposed in low earth orbit are modified due to interaction with atomic oxygen. Chemical changes and surface roughening effects can occur which alter optical and other properties. The experiment A0114 contained 128 solid surface samples, half of which were exposed on the front and half on the rear of Long Duration Exposure Facility. Each sample was subjected to many analyses, but only the methods and techniques are described which were used to measure the changes in roughness, erosion depths, and material growth using profilometry.

Christl, Ligia C.↗

Mach 5 electroformed nickel nozzle refurbishment FNAS investigation of ultra-smooth surfaces

This task is in support of the Quiet Hypersonic Wind Tunnel effort currently in effect at NASA Langley Research Center, VA. A laminar flow wind tunnel nozzle has been previously fabricated by electroforming pure nickel over a machined and polished two piece stainless steel mandrel. The mandrel was removed leaving the replicate nozzle surface. The nozzle was then pressed into a heavy stainless steel jacket for mounting features and rigidity. The original nickel surface was a replication of the polished mandrel but had degraded due to oxidation. The inside surface requirements are very stringent in order to achieve laminar or quiet flow at the desired pressure and temperature for the specific design of Mach 5. The throat area of the axisymmetric device must have a surface finish with no defects greater than 16 microinches. This requires an rms average background of about four microinches or better for inspection purposes. A coating of nickel-phosphorous alloy was applied by catalytic deposition and then the inside of the nozzle was polished retaining dimensional and surface finish tolerances as specified per drawings supplied. Since the unit is not an optical component, conventional optical inspection methods for surface finish and figure are not readily achieved. Measurements were made using surface profilometry.

Rood, Robert↗

Understanding the Feasibility of MAB Phase Structures for Lunar Applications

During the ten-week internship, my work focused on synthesis, characterization, and tailoring the flowability of the MAB phase powders for improving the surface finish and decreasing porosity of 3D-printed MAB phase structures. My mentor for the project was Dr. Samuel Hocker from NASA Langley and my faculty advisor was Dr. Surojit Gupta from the University of North Dakota. I also collaborated with Daniel Trieff from the University of North Dakota in developing characterization paradigm of 3D printed samples. The microencapsulation was performed via novel solvent casting-based microencapsulation process pioneered in UND, wherein a polymer (PLA, PHA) was dissolved into dichloromethane and precipitated onto the surface of the MoAlB particles. Two 100mL samples of microencapsulated powder was outsourced to Particle Technology Labs for flowability testing along with a 100mL control sample to determine if microencapsulation is a valid method for improving the flowability. The microencapsulated powders were characterized using SEM, Differential Scanning Calorimetry, and optical microscopy. The SEM images showed no change between the pure and microencapsulated powders. The optical microscopy analysis indicated a reduction in reflectivity for the PLA microencapsulated powders as well as hydrophobic properties. Both results suggest that microencapsulation was successful as PLA is a hydrophobic polymer and the change in reflectivity could be a result of the light being dispersed through the polymer coating. A reflectivity analysis will be done to bring more perspective to these observations. If powder flowability is improved, then the project will move forward with testing the printability of the microencapsulated powders and characterizing the structures using the designed characterization protocol. We are waiting for the DSC results. The characterization protocol for the 3D-printed MAB structures included a visual inspection of the plates to rule out any samples that had spalled or delaminated, optical microscopy to document surface features, porosity, and decomposition, and cleaning of the plates using an ultrasonic bath in preparation for SEM, EDS, and profilometry analyses.

MAB Phase↗

Pre-Transient Characterization of Historic EBR-II Pins for Transient Testing

Current interest in sodium-cooled fast reactor (SFR) designs, such as TerraPower’s Natrium Reactor, has highlighted the need for advanced reactor fuel technology development. Modern U-Zr and U- Pu-Zr pin designs are primary candidates to fuel SFRs and boast high fuel utilization capacity, increased fuel-cladding compatibility, and improved safety through inherent feedback mechanisms. Despite over 60 years of metallic fuel irradiation, uncertainties exist in the performance of the fuel system, particularly under transient overpower (TOP) and loss of flow (LOF) scenarios. Throughout historical testing within the Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF), fuel behavior has demonstrated benign response to transient reactor conditions; however, accurate predictions of failure thresholds to inform operational limitations rely heavily on fuel composition, burnup, and irradiation history. In expanding TOP and LOF testing, the Transient Heat sink Overpower Response (THOR) Capsule will be used to test modern fuel technologies in a static sodium environment in the Transient Reactor Test (TREAT) Facility. The THOR capsule is highly instrumented and will provide time-dependent thermal behavior of SFR fuel pins subjected to accident conditions within TREAT. The THOR-Metallic (THOR- M) campaign aims to validate and expand historical TOP and LOF testing on high burnup U-Zr and U-Pu- Zr fuel alloys previously irradiated in EBR-II by running the rods to failure. This contribution focuses primarily on the pre-transient engineering-scale destructive and non- destructive characterization that has been conducted on both the test and sibling pins used for the TOP and LOF tests. All pins underwent visual examination, neutron radiography, element contact profilometry, and precise gamma scan. The sibling pins used for each test were further analyzed using gas assay, sampling, and recharge analysis (GASR), and optical microscopy. The results from each technique confirmed that the fuel pins were intact and devoid of any atypical developments when compared to historical data. Additionally, the analyzed measurements establish a baseline for comparison to post-transient analysis. Key fuel behaviors quanitifed include axial elongation of the fuel column, diametral strain of the pin, patterns in fluff structure geometry, changes in axial isotope distribution, evolution of constituent redistribution, porosity, and fission gas release. The pre-transient measurements and changes attributed to transient behavior from post-transient measurement will be compared to historical data to capture the behavioral dependence on composition, burnup, and irradiation history. Results from this work advance the initiatives of the THOR-M campaign, which aid in informing fuel performance models and establishing safety criteria for SFR operational limits. The novel combination of test environment, in-situ instrumentation, and comprehensive suite of characterization methods provides greater understanding of transient fuel behavior. Overall, information on the time and condition of pin failure for high burnup U-Pu-Zr will greatly expand the limited existing TOP and LOF test data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗