Roughness measurements across topographically varied additively manufactured metal surfaces
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36 MATERIALS SCIENCE↗
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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↗
Influence of Realistic, Cyclic Atmospheric Cycles on the Pitting Corrosion of Austenitic Stainless Steels
Pitting corrosion was evaluated on stainless steels 304H, 304, and 316L the surfaces of which had ASTM seawater printed on them as a function of surface roughness after exposure to an exemplar realistic atmospheric diurnal cycle for up to one year. Methods to evaluate pitting damage included optical imaging, scanning electron microscopy imaging, profilometry analysis, and polarization scans. The developed cyclic exposure environment did not significantly influence pitting morphology nor depth in comparison to prior static exposure environments. Cross-hatching was observed in a majority of pits for all material compositions with the roughest surface finish (#4 finish) and in all surface finishes for the 304H composition. Evidence is provided that cross-hatched pit morphologies are caused by slip bands produced during the grinding process for the #4 finish or by material processing. Additionally, micro-cracking was observed in pits formed on samples with the #4 surface finish and was greatly reduced or absent for pits formed on samples with smooth surface finishes. This suggests that both a low RH leading to an MgCl 2 -dominated environment and a rough surface containing significant residual stress are necessary for micro-cracking. Finally, the use of various characterization techniques and cross sectioning was employed to both qualitatively and quantitatively assess pitting damage across all SS compositions and surface finishes.
36 MATERIALS SCIENCE↗
Micro Fourier Transform Profilometry (μFTP): 3D shape measurement at 10,000 frames per second
We report that fringe projection profilometry is a well-established technique for optical 3D shape measurement. However, in many applications, it is desirable to make 3D measurements at very high speed, especially with fast moving or shape changing objects. In this work, we demonstrate a new 3D dynamic imaging technique, Micro Fourier Transform Profilometry (μFTP), which can realize an acquisition rate up to 10,000 3D frame per second (fps). The high measurement speed is achieved by the number of patterns reduction as well as high-speed fringe projection hardware. In order to capture 3D information in such a short period of time, we focus on the improvement of the phase recovery, phase unwrapping, and error compensation algorithms, allowing to reconstruct an accurate, unambiguous, and distortion-free 3D point cloud with every two projected patterns. We also develop a high-frame-rate fringe projection hardware by pairing a high-speed camera and a DLP projector, enabling binary pattern switching and precisely synchronized image capture at a frame rate up to 20,000 fps. Lastly, based on this system, we demonstrate high-quality textured 3D imaging of 4 transient scenes: vibrating cantilevers, rotating fan blades, flying bullet, and bursting balloon, which were previously difficult or even unable to be captured with conventional approaches.
3D shape measurement↗
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.↗
Experimental study of crack initiation and propagation in high- and gigacycle fatigue in titanium alloys
Fatigue (high- and gigacycle) crack initiation and its propagation in titanium alloys with coarse and fine grain structure are studied by fractography analysis of fracture surface. Fractured specimens were analyzed by interferometer microscope and SEM to improve methods of monitoring of damage accumulation during fatigue test and to verify the models for fatigue crack kinetics. Fatigue strength was estimated for high cycle fatigue regime using the Luong method [1] by “in-situ” infrared scanning of the sample surface for the step-wise loading history for different grain size metals. Fine grain alloys demonstrated higher fatigue resistance for both high cycle fatigue and gigacycle fatigue regimes. Fracture surface analysis for plane and cylindrical samples was carried out using optical and electronic microscopy method. High resolution profilometry (interferometer-profiler New View 5010) data of fracture surface roughness allowed us to estimate scale invariance (the Hurst exponent) and to establish the existence of two characteristic areas of damage localization (different values of the Hurst exponent). Area 1 with diameter ∼300 μm has the pronounced roughness and is associated with damage localization hotspot. Area 2 shows less amplitude roughness, occupies the rest fracture surface and considered as the trace of the fatigue crack path corresponding to the Paris kinetics.
36 MATERIALS SCIENCE↗
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↗
High Quality, Low Cost Bulk Gallium Nitride Substrates Grown by the Electrochemical Solution Growth Method
The objective of this project was to develop the Electrochemical Solution Growth (ESG) method conceived / patented at Sandia National Laboratory into a commercially viable bulk gallium nitride (GaN) growth process that can be scaled to low cost, high quality, and large area GaN wafer substrate manufacturing. The goal was to advance the ESG growth technology by demonstrating rotating seed growth at the lab scale and then transitioning process to prototype commercial system, while validating the GaN material and electronic / optical device quality. The desired outcome of the project is a prototype commercial process for US-based manufacturing of high quality, large area, and lower cost GaN substrates that can drive widespread deployment of energy efficient GaN-based power electronic and optical devices. In year 1 of the project (Sept 2012 – Dec 2013) the overall objective was to demonstrate crystalline GaN growth > 100um on a GaN seed crystal. The development plan included tasks to demonstrate and implement a method for purifying reagent grade salts, develop the reactor 1 process for rotating seed Electrochemical Solution Growth (ESG) of GaN, grow and characterize ESG GaN films, develop a fluid flow and reaction chemistry model for GaN film growth, and design / build an improved growth reactor capable of scaling to 50mm seed diameter. The first year’s project objectives were met in some task areas including salt purification, film characterization, modeling, and reactor 2 design / fabrication. However, the key project objective of the growth of a crystalline GaN film on the seed template was not achieved. Amorphous film growth on the order of a few tenths of a micron has been detected with a film composition including Ga and N, plus several other impurities originating from the process solution and hardware. The presence of these impurities, particularly the oxygen, has inhibited the demonstration of crystalline GaN film growth on the seed template. However, the presence of both Ga and N at the growth surface indicates that the reactor hardware physics is all functioning properly; achieving film growth is a matter of controlling the chemistry at the interface. The impurities originating from the hardware are expected to be straightforward to eliminate. Activities were defined for an extension of budget period 1 to eliminate the undesired impurities originating from the reactor hardware and interfering with crystalline GaN film growth. The budget period 1 extension was negotiated during the 1st half of 2014. The budget period 1 extension spanned approximately from August 2014 to August 2015. The project objective for this extension period was to demonstrate at least 0.5um crystalline GaN film on a GaN seed in the lab scale reactor. The focus of the budget 1 extension period from August 2014 to August 2015 was to eliminate oxygen contamination interference with GaN film growth. The team procured the highest purity lowest oxygen salt for testing. Low oxygen crucible materials such as silicon carbide were installed and evaluated in the laboratory reactor. Growth experiments were performed with high purity salt, high purity hardware, and optimized oxide removal from the seed surface. Experiments were characterized with methods including UV inspection, profilometry, x-ray diffraction (XRD) to determine crystalline structure, optical and scanning electron microscopy, photoluminescence, x-ray photon spectroscopy (XPS), transmission electron microscopy (TEM), and secondary ion mass spectroscopy (SIMS). Despite successfully integrating the low oxygen materials in the laboratory reactor, the goal of depositing 0.5um of crystalline GaN on the MOCVD GaN seed was not met. Very thin (ca. 10nm) cubic phase GaN deposition was observed on the hexagonal MOCVD GaN seeds. But there was a competing etching reaction which was also observed and thought to be related to the presence of metallic lithium, a byproduct of the LiCl-KCl salt used as the process medium. The etching reaction could potentially be addressed by alternate salts not containing lithium, but would necessitate starting all over on the reactor and process design. Further, controlling the reaction of Ga and N in the bulk salt to favor deposition on the seed has proved to be very difficult and unlikely to be solved within the scope of this project in a manner consistent with the original objective for wafer or crystal scale thickness for GaN deposition on a GaN seed. Upon completion of the budget 1 extension period in August 2015 the project partners and DOE agreed to stop work on the project.
32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
Control of waveguide properties by tuning femtosecond laser induced compositional changes
Local compositional changes induced by high repetition rate fs-laser irradiation can be used to produce high performance optical waveguides in phosphate-based glasses. The waveguide refractive index contrast is determined by the local concentration of La, which can be changed by the action of the writing laser pulses. In this work, we have investigated the degree of control that can be exerted using this waveguide writing mechanism over the cross-section of the guiding region, and the local refractive index and compositional changes induced. These variables can be smoothly controlled via processing parameters using the slit shaping technique with moderate Numerical Aperture (NA 0.68) writing optics. The combined use of X-ray microanalysis and near field refractive index profilometry evidences a neat linear correlation between local La content and refractive index increase over a broad Δn interval (>3 × 10{sup −2}). This result further confirms the feasibility of generating efficient, integrated optics elements via spatially selective modification of the glass composition.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
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↗
Investigation on lateral resolution of surface slope profilers
Here, we investigate and compare the spatial (lateral) resolution, or more generally, the optical/instrumental transfer function (OTF/ITF) of surface slope measuring profilometers of two different types that are commonly used for high accuracy characterization of x-ray optics at the long-spatial-wavelength range. These are an autocollimator based profiler, Optical Surface Measuring System (OSMS), and a long trace profiler, LTP-II, both available at the Advanced Light Source (ALS) X-Ray Optics Lab (XROL). In the OSMS, an ELCOMAT-3000 electronic auto-collimator, vertically mounted to the translation carriage and equipped with an aperture of 2.5 mm diameter, is scanned along the surface under test. The LTP-II OTF has been measured for two different configurations, a classical two-beam pencil-beam-interferometry and a single-Gaussian-beam deflectometry. For the ITF calibration, we apply a recently developed method based on test surfaces with one-dimensional (1D) linear chirped height profiles of constant slope amplitude. Analytical expressions for the OTFs, empirically deduced based on the experimental results, are presented. We also discuss the application of the results of the ITF measurements and modeling to improve the surface slope metrology with state-of-the-art x-ray mirrors.
42 ENGINEERING↗
Characterization of Mk-IV and EBR-II X441A Metallic Fuel Pins for the THOR-C-2 and THOR-M-TOP-1 Experiments: Results from Post-Transient Neutron Tomography of THOR-C-2 Capsule and Pre-transient Non-Destructive and Destructive Examination of DP 36 and DP 40 (Rev.1)
Current interest in sodium-cooled fast reactor designs, such as TerraPower’s Natrium Reactor, has highlighted the need for advanced-reactor fuel technology development. A Fuel Safety Research and Development (FSRD) program for metallic fast reactor fuels has been created to achieve comprehensive safety testing within the re-commissioned Transient Reactor Test (TREAT) facility at the Idaho National Laboratory. Despite over 60 years of metallic fuel irradiation, uncertainties exist in the performance of the fuel system, particularly under anticipated operational occurrences and severe accident scenarios. Throughout historical testing within the Experimental Breeder Reactor (EBR)-II and the Fast Flux Test Facility, fuel behavior has demonstrated benign response to transient reactor conditions; however, accurate predictions of failure thresholds rely heavily on fuel composition and irradiation history. In advancing the FSRD program, two planned transient heating experiments are at various stages of completion. The Temperature Heat sink Overpower Response (THOR)-C-2, fueled with an unirradiated Mk IV U-10Zr pin, has undergone transient irradiation in TREAT and post-transient three-dimensional neutron tomography. Additionally, pre-transient characterization of test and sibling U-19Pu-10Zr pins for THOR-M-TOP-1 was evaluated by both non-destructive and destructive methods. The test and sibling pins were selected from previously irradiated EBR-II experiment X441A. Both pins underwent visual examination, precise gamma spectrometry, two-dimensional neutron radiography, and element contact profilometry while the sibling pin was additionally subjected to sectioning and optical microscopy. THOR-C-2 radiography captured the fuel and cladding relocation during the intermediate transient at the top and bottom of the THOR capsule, allowing key features to be linked to the pin’s measured thermal response. For THOR M TOP 1, a solid baseline for steady-state behavior has been established. No anomalous features were identified in either the test or sibling pin. Defining characteristics and features were recorded for further comparisons.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
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.↗