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At least 1,099 records · Page 61
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Analysis of Defects in Metal Additive Manufacturing with Augmented Data Generation

Laser powder bed fusion (LPBF) is a method of additive manufacturing (AM) that selectively melts and fuses together microscopic metallic powder. LPBF offers the benefit of producing custom structures out of high strength metals that can be difficult to fabricate with conventional methods. The challenge of LPBF is that 3D printed structures often have internal pores due to process flaws. Pulsed thermal tomography (PTT) is a method for reconstructing the depth profile of materials, allowing the visualization internal voids in solids. In prior work, we developed a convolutional neural network (CNN) which, having been trained on simulated 2D PTT images of subsurface elliptical defects, was able to classify the semi-major radii, semi-minor radii, and angular orientation of the best-fit ellipses in previously unseen PTT images. The unseen PTT images contained subsurface irregular defect shapes imported from scanning electron microscopy (SEM) images of metallic LPBF-printed specimens. Training the CNN on irregular defect shapes instead of on elliptical shapes would make the resulting classifications more descriptive of actual defect shapes. However, this requires a much higher volume of SEM images of material defects, which are difficult to obtain because of random occurrence of defects in LPBF. To address this challenge, we developed a generative adversarial network (GAN) to augment the existing dataset of SEM defect images. The GAN model is demonstrated to create novel yet realistic defect shapes that can be used as input for simulated PTT images to train CNN.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Microscopic analysis of irradiated UN–Mo–W for space nuclear propulsion

Nuclear propulsion is an effective method of providing thrust in deep space, allowing for shorter mission duration for long-term surface missions to Mars. The fuel for nuclear propulsion systems must exhibit superior mechanical and thermal properties, to decrease the possibility of fuel failure and to increase reactor efficiency. Here, the objective of the Sirius project is to fabricate and irradiate cermet fuels at the Idaho National Laboratory Transient Reactor Facility to determine the properties of the fuel after irradiation at prototypical nuclear propulsion start-up conditions. The Sirius project featured 3 test capsules, Sirius-1 featured uranium nitride fuel dispersed in a matrix of tungsten and rhenium, while Sirius-2A and -2B featured uranium nitride-molybdenum-tungsten fuel (UN-Mo-W). The fuel samples from the Sirius-2A and -2B capsules were examined after irradiation using optical microscopy, scanning electron microscopy, and X-ray diffraction analyses. The mechanical properties of the fuel from Sirius-2A and -2B are discussed in a previous work. In this study, the results of the optical microscopy, scanning electron microscopy, and X-ray diffraction analyses are discussed.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

In-situ TEM Holder for Ultrafast, Multimodal Imaging

This project developed a prototype in-situ specimen holder product to transmission electron microscope (TEM) users that drastically expand the usability of TEM by combining nanoscale laser excitation and optical signal collection. A commercial prototype has been constructed and a few nanoscale materials characterization experiments have been performed to validate its performance and demonstrate its utility in real scientific studies, for example, in-situ characterization and mapping of defects in the synthesis of nanostructures.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

Performance of Pulsed Thermal Tomography Imaging with Machine Learning-Based Classification of Defects in Additively Manufactured Structures

Additive manufacturing (AM) is an emerging method for cost-efficient fabrication of complex topology nuclear reactor parts from high-strength corrosion resistance alloys, such as stainless steel and Inconel. AM of metallic structures for nuclear energy applications is currently based on laser powder bed fusion (LPBF) process. Some of the challenges with using LPBF method for nuclear manufacturing include the possibility of introducing pores into metallic structures. Integrity of AM structures needs to be evaluated nondestructively because material flaws could lead to premature failures in high temperature nuclear reactor environment. Currently, there exist limited capabilities to evaluate actual AM structures non-destructively. Pulsed Thermal Tomography Imaging (PTT) provides a capability for non-destructive evaluation (NDE) of subsurface defects in arbitrary size structures. The PTT method is based on recording material surface temperature transients with infrared (IR) camera following thermal pulse delivered on material surface with flash light. The PTT method has advantages for NDE of actual AM structures because the method involves one-sided non-contact measurements and fast processing of large sample areas captured in one image. Following initial qualification of an AM component for deployment in a nuclear reactor, a PTT system can also be used for in-service nondestructive evaluation (NDE) applications. In this report, we describe recent progress in enhancing PTT capabilities in detecting and visualizing microscopic defects in metallic specimens. The thermal tomography (TT) algorithm obtains depth reconstructions of spatial effusivity from the data cube of sequentially recorded surface temperatures. However, interpretation of TT images is non-trivial because of blurring of images with increasing depth. To address this challenge, we have developed a deep learning convolutional neural network (CNN) to classify size and orientation subsurface defects in simulated TT images. CNN is trained on a database of TT images created for a set of simulated metallic structures with elliptical subsurface voids. Test of CNN performance demonstrate the ability to classify radii and angular orientation of subsurface defects in TT images. In addition, we have shown that CNN trained on elliptical defects is capable of classifying irregular-shaped defects obtained from scanning electron microscopy (SEM) of stainless steel sections printed with LPBF.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

Ultrafast state-selective tunneling in two-dimensional semiconductors with a phase- and amplitude-controlled THz-scanning tunneling microscope

THz-pulse driven scanning tunneling microscopy (THz-STM) enables access to the ultrafast quantum dynamics of low-dimensional material systems at simultaneous ultrafast temporal and atomic spatial resolution. State-selective tunneling requires precise amplitude and phase control of the THz pulses combined with quantitative near-field waveform characterization. Here, we employ our state-of-the-art THz-STM with multi-MHz repetition rates, efficient THz generation, and precisely tunable THz waveforms to investigate a single sulfur vacancy in monolayer MoS2. We demonstrate that 2D transition metal dichalcogenides (TMDs) are an ideal platform for near-field waveform sampling by THz cross-correlation. Furthermore, we determine the THz voltage via QEV scans, which measure the THz rectified charge Q as a function of THz field amplitude E and dc bias Vdc. Mapping the complex energy landscape of localized states with a resolution down to 0.01 electrons per pulse facilitates state-selective tunneling to the HOMO and LUMO orbitals of a charged sulfur vacancy.

Materials Science↗
NASA NTRS2014

X-Ray Absorption near Edge Structure Spectroscopic Study of Hayabusa Category 3 Carbonaceous Particles

Analyses with a scanning transmission x-ray microscope (STXM) using x-ray absorption near edge structure (XANES) spectroscopy were applied for the molecular characterization of two kinds of carbonaceous particles of unknown origin, termed category 3, which were collected from the Hayabusa spacecraft sample catcher. Carbon-XANES spectra of the category 3 particles displayed typical spectral patterns of heterogeneous organic macromolecules; peaks corresponding to aromatic/olefinic carbon, heterocyclic nitrogen and/or nitrile, and carboxyl carbon were all detected. Nitrogen-XANES spectra of the particles showed the presence of N-functional groups such as imine, nitrile, aromatic nitrogen, amide, pyrrole, and amine. An oxygen-XANES spectrum of one of the particles showed a ketone group. Differences in carbon- and nitrogen-XANES spectra of the category 3 particles before and after transmission electron microscopic (TEM) observations were observed, which demonstrates that the carbonaceous materials are electron beam sensitive. Calcium-XANES spectroscopy and elemental contrast mapping identified a calcium carbonate grain from one of the category 3 particles. No fluorine-containing molecular species were detected in fluorine-XANES spectra of the particles. The organic macromolecular features of the category 3 particles were distinct from commercial and/or biological ‘fresh (non-degraded)’ polymers, but the category 3 molecular features could possibly reflect degradation of contaminant polymer materials or polymer materials used on the Hayabusa spacecraft. However, an extraterrestrial origin for these materials cannot currently be ruled out.

Asteroides↗
DOE OSTI2021

Algorithm-Driven Advances for Scientific CT Instruments: From model-based to deep learning-based approaches

Multiscale 3D characterization is widely used by materials scientists to further their understanding of the relationships between microscopic structure and macroscopic function. Scientific computed tomography (SCT) instruments are one of the most popular choices for 3D nondestructive characterization of materials at length scales ranging from the angstrom scale to the micron scale. These instruments typically have a source of radiation (such as electrons, X-rays, or neutrons) that interacts with the sample to be studied and a detector assembly to capture the result of this interaction (see Figure 1 ). A collection of such high-resolution measurements is made by reorienting the sample, which is mounted on a specially designed stage/holder after which reconstruction algorithms are used to produce the final 3D volume of interest. The specific choice of which instrument to use depends on the desired resolution and properties of the materials being imaged. Additionally, the end goal of SCT scans includes determining the morphology, chemical composition, or dynamic behavior of materials when subjected to external stimuli. In summary, SCT instruments are powerful tools that enable 3D characterization across multiple length scales and play a critical role in furthering the understanding of the structure–function relationships of different materials.

42 ENGINEERING↗
DOE OSTI2025

Mapping causal patterns in crystalline solids

The evolution of the atomic structures of the combinatorial library of Sm-substituted thin film BiFeO 3 along the phase transition boundary from the ferroelectric rhombohedral phase to the non-ferroelectric orthorhombic phase is explored using scanning transmission electron microscopy. Localized properties, including polarization, lattice parameter, and chemical composition, are parameterized from atomic-scale imaging, and their causal relationships are reconstructed using a linear non-Gaussian acyclic model. This approach is further extended to explore the spatial variability of the causal coupling using the sliding window transform method, which revealed that new causal relationships emerged at both the expected locations, such as domain walls and interfaces, and at additional regions forming clusters in the vicinity of the walls or spatially distributed features. While the exact physical origins of these relationships are unclear, they likely represent nanophase-separated regions in the morphotropic phase boundaries. Overall, we posit that an in-depth understanding of complex disordered materials away from thermodynamic equilibrium necessitates understanding not only the generative processes that can lead to observed microscopic states but also the causal links between multiple interacting subsystems.

Causal inference↗
DOE OSTI2019

Microscopic subsurface characterization of layered magnetic materials using magnetic resonance force microscopy

This project resulted in the following accomplishments: 1) The invention of scanned probe ferromagnetic resonance microscopy. Upon implementation and refinement this approach was used to measure static and dynamic magnetic resonance properties of ferromagnets with an unprecedented combination of spectral and spatial resolution. 2) Demonstration and study of spin pumping in a pristine ferromagnet across a boundary defined entirely by a magnetic field gradient, and so free of materials discontinuities. 3) First demonstrated highly efficient dynamic spin injection from Y 3 Fe 5 O 12 (YIG) into NiO, an antiferromagnetic (AF) insulator and robust spin propagation in AF NiO over distances up to 100-nm thickness; both spin injection and spin transport are mediated by the AF spin correlations. 4) Demonstration of exceptionally high efficiency conversion of spin current to charge current achieved in spin pumping from the dynamic magnetization of a ferromagnetic insulator into a variety of adjacent metal films. 5) Seminal study of the nature of spin-orbit coupling in d-electron metals that revealed the dominant sensitivity of the d-orbital moment to the d-electron count and revealing the important roles of both d-electron configuration and atomic number in the physics of the spin Hall effect. 6) Demonstration of observation of FMR by means of optically-detected NV diamond relaxometry that provided a highly sensitive, spatially resolved FMR detection method and revealed spin pumping across 100-nm length scales by means of dipolar coupling. 7) Using magnetic field localization, developed for FMR imaging, demonstrated a novel approach to discretizing spin wave modes to improve the characteristics of auto-oscillators driven by pure spin currents produced by the spin Hall effect. 8) We demonstrated large spin pumping signals from propagating high wavevector spinwaves in thin film YIG find that the spin pumping efficiency was insensitive to wavevector thus emphasizing the promise of thin YIG films for spinwave-based spintronics by allowing for predictable down-scaling of device dimensions and enabling a broad range of operational frequencies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Compact single-shot soft X-ray photon spectrometer for free-electron laser diagnostics

The photon spectrum from free-electron laser (FEL) light sources offers valuable information in time-resolved experiments and machine optimization in the spectral and temporal domains. We have developed a compact single-shot photon spectrometer to diagnose soft X-ray spectra. The spectrometer consists of an array of off-axis Fresnel zone plates (FZP) that act as transmission-imaging gratings, a Ce:YAG scintillator, and a microscope objective to image the scintillation target onto a two-dimensional imaging detector. This spectrometer operates in segmented energy ranges which covers tens of electronvolts for each absorption edge associated with several atomic constituents: carbon, nitrogen, oxygen, and neon. The spectrometer’s performance is demonstrated at a repetition rate of 120 Hz, but our detection scheme can be easily extended to 200 kHz spectral collection by employing a fast complementary metal oxide semiconductor (CMOS) line-scan camera to detect the light from the scintillator. This compact photon spectrometer provides an opportunity for monitoring the spectrum downstream of an endstation in a limited space environment with sub-electronvolt energy resolution.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2024

Power Electronics Materials and Bonded Interfaces - Reliability and Lifetime

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronic modules, especially in operating temperatures greater than 150 degrees Celsius. In this paper, we investigate the thermomechanical performance of sintered copper (Cu) as a large-area attachment, bonded between Cu baseplates and active-metal-bonded substrates, under accelerated thermal shock (-40 degrees Celsius to 200 degrees Celsius) conditions. In the fabrication phase of the samples, we used different stencil patterns and found out that the grid and stripe patterns resulted in a better outgassing of the residual organics during the sintering process, thereby ensuring a substantially improved bond quality than a full-area print. The paste consisted of Cu microflakes and we performed sintering using a Budatec SP300 sintering press at 275 degrees Celsius with 15 MPa of bonding pressure for 5 minutes in a nitrogen atmosphere. Under accelerated experiments, we monitored the degradation of the sintered Cu bond in the samples through C-mode scanning acoustic microscope (C-SAM) images. To quantify the defect percentage in C-SAM images, we investigated image denoising techniques to exclude the pattern prints. Finally, we cross-sectioned a sample and obtained digital microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS↗
NASA NTRS1995

ZnO Films on {001}-Cut <110>-Propagating GaAs Substrates for Surface Acoustic Wave Device Applications

A potential application for piezoelectric films on GaAs substrates is the monolithic integration of surface acoustic wave (SAW) devices with GaAs electronics. Knowledge of the SAW properties of the layered structure is critical for the optimum and accurate design of such devices. The acoustic properties of ZnO films sputtered on {001}-cut <110> -propagating GaAs substrates are investigated in this article, including SAW Velocity effective piezoelectric coupling constant, propagation loss. diffraction, velocity surface, and reflectivity of shorted and open metallic gratings. The measurements of these essential SAW properties for the frequency range between 180 and 360 MHz have been performed using a knife-edge laser probe for film thicknesses over the range of 1.6-4 micron and with films or different grain sizes. The high quality of dc triode sputtered films was observed as evidenced by high K(exp 2) and low attenuation. The measurements of the velocity surface, which directly affects the SAW diffraction, on the bare and metalized ZnO on SiO2, or Si3N4 on {001}-cut GaAs samples are reported using two different techniques: 1) knife-edge laser probe, 2) line-focus-beam scanning acoustic microscope. It was found that near the <110> propagation direction, the focusing SAW property of the bare GaAs changes into a nonfocusing one for the layered structure, but a reversed phenomenon exists near the <100> direction. Furthermore, to some extent the diffraction of the substrate can be controlled with the film thickness. The reflectivity of shorted and open gratings are also analyzed and measured. Zero reflectivity is observed for a shorted grating. There is good agreement between the measured data and theoretical values.

Kim, Yoonkee↗
DOE OSTI2025

Growth and structure of alpha-Ta films for quantum circuit integration

Tantalum films incorporated into superconducting circuits have exhibited low surface losses, resulting in long-lived qubit states. The remaining loss pathways originate in microscopic defects that manifest as two level systems (TLSs) at low temperatures. These defects limit performance, so careful attention to tantalum film structures is critical for optimal use in quantum devices. In this work, we investigate the growth of tantalum using magnetron sputtering on sapphire, Si, and photoresist substrates. In the case of sapphire, we present procedures for the growth of fully-oriented films with α-Ta [1 1 1]//Al2O3 [0 0 0 1] and α-Ta [1 −1 0]//Al2O3 [1 0 −1 0] orientational relationships and having residual resistivity ratio (RRR) ∼ 60 for 220 nm thick films. On Si, we find a complex grain texturing with Ta [1 1 0] normal to the substrate and RRR ∼ 30. We further demonstrate airbridge fabrication using Nb to nucleate α-Ta on photoresist surfaces. For the films on sapphire, resonators show TLS-limited quality factors of 1.3 ± 0.3 × 106 at 10 mK (for a waveguide gap and conductor width of 3 and 6 μm, respectively). Structural characterization using scanning electron microscopy, x-ray diffraction, low temperature transport, secondary ion mass spectrometry, and transmission electron microscopy reveal the dependence of residual impurities and screw dislocation density on processing conditions. The results provide practical insights into the fabrication of advanced superconducting devices including qubit arrays and guide future works on crystallographically deterministic qubit fabrication.

42 ENGINEERING↗
NASA NTRS1995

ZnO films on /001/-cut (110)-propagating GaAs substrates for surface acoustic wave device applications

A potential application for piezoelectric films substrates is the monolithic integration of surface acoustic wave (SAW) devices with GaAs electronics. Knowledge of the SAW properties of the layered structure is critical for the optimum and accurate design of such devices. The acoustic properties of ZnO films sputtered on /001/-cut group of (110) zone axes-propagating GaAs substrates are investigated in this article, including SAW velocity, effective piezoelectric coupling constant, propagation loss, diffraction, velocity surface, and reflectivity of shorted and open metallic gratings. The measurements of these essential SAW properties for the frequency range between 180 and 360 MHz have been performed using a knife-edge laser probe for film thicknesses over the range of 1.6-4 micron and with films of different grain sizes. The high quality of dc triode sputtered films was observed as evidenced by high K(sup 2) and low attenuation. The measurements of the velocity surface, which directly affects the SAW diffraction, on the bare and metalized ZnO on SiO2 or Si3N4 on /001/-cut GaAs samples are reported using two different techniques: (1) knife-edge laser probe, (2) line-focus-beam scanning acoustic microscope. It was found that near the group of (110) zone axes propagation direction, the focusing SAW property of the bare GaAs changes into a nonfocusing one for the layered structure, but a reversed phenomenon exists near the (100) direction. Furthermore, to some extent the diffraction of the substrate can be controlled with the film thickness. The reflectivity of shorted and open gratings are also analyzed and measured. Zero reflectivity is observed for a shorted grating. There is good agreement between the measured data and theoretical values.

Hickernell, Frederick S.↗
NASA NTRS2000

Microscopic physical biomarkers in carbonate hot springs: implications in the search for life on Mars

Physical evidence of life (physical biomarkers) from the deposits of carbonate hot springs were documented at the scale of microorganisms--submillimeter to submicrometer. The four moderate-temperature (57 to 72 degrees C), neutral pH springs reported on in this study, support diverse communities of bacteria adapted to specific physical and chemical conditions. Some of the microbes coexist with travertine deposits in endolithic communities. In other cases, the microbes are rapidly coated and destroyed by precipitates but leave distinctive mineral fabrics. Some microbes adapted to carbonate hot springs produce an extracellular polymeric substance which forms a three-dimensional matrix with living cells and cell remains, known as a biofilm. Silicon and iron oxides often coat the biofilm, leading to long-term preservation. Submicrometer mineralized spheres composed of calcium fluoride or silica are common in carbonate hot spring deposits. Sphere formation is biologically mediated, but the spheres themselves are apparently not fossils or microbes. Additionally, some microbes selectively weather mineral surfaces in distinctive patterns. Hot spring deposits have been cited as prime locations for exobiological exploration of Mars. The presence of preserved microscopic physical biomarkers at all four sites supports a strategy of searching for evidence of life in hot spring deposits on Mars.

NASA Center JSC↗
DOE OSTI2020

Open Source Platform for Live Processing of High Data Rate Electron Microscopy (SBIR Phase I Award Topic 15, Subtopic B, Final Scientific / Technical Report)

4D scanning transmission electron microscopy (STEM) is experiencing a revolution both in terms of data size, and data veracity, as are many other areas of experimental data acquisition. This presents enormous opportunities to make new scientific discoveries, but is also hamstrung by aging software that is no longer fit for purpose. Experimental data acquisition platforms must make the same investments in software infrastructure that the simulation community made decades ago to take advantage of high-performance computing (HPC) if they hope to realize the full potential of the latest advances made in detector technology. This requires rethinking the design and deployment of hardware, moving away from small, fixed commodity computing capabilities with closed interfaces to open, modular, scalable systems designed for parallelism and throughput. The technical approach will leverage best-in-class open source technologies, and develop new approaches strategically to build an open source platform for experimental data acquisition targeting high data rate electron microscopy. The project will develop a software platform that uses the power and performance of modern HPC resources to ingest the large volume of data produced by electron microscopes using direct electron detectors. A set of configurable pipelines will be used to enable the processing to be tailored to the problem being investigated with builtin visualization of data at interactive rates. This project will leverage investments made by the DOE and other agencies to provide a powerful software platform for the experimental data community working with most powerful electron microscopes, such as 4D STEM detectors. It will create a platform that serves as a reference for the community. Permissive open source licensing will make the platform available to all, with a simple deployment strategy offering the ability to keep data close to where it is generated. This advanced software platform will require customization for each deployment, creating opportunities for software services that are typically offered to extend open source software platforms.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2024

Core/Shell-Like Localized Emission at Atomically Thin Semiconductor–Au Interface

Localized emission in atomically thin semiconductors has sparked significant interest as single-photon sources. Despite comprehensive studies into the correlation between localized strain and exciton emission, the impacts of charge transfer on nanobubble emission remains elusive. Here, in this paper, we report the observation of core/shell-like localized emission from monolayer WSe 2 nanobubbles at room temperature through near-field studies. By altering the electronic junction between monolayer WSe 2 and the Au substrate, one can effectively adjust the semiconductor to metal junction from a Schottky to an Ohmic junction. Through concurrent analysis of topography, potential, tip-enhanced photoluminescence, and a piezo response force microscope, we attribute the core/shell-like emissions to strong piezoelectric potential aided by induced polarity at the WSe 2 –Au Schottky interface which results in spatial confinement of the excitons. Our findings present a new approach for manipulating charge confinement and engineering localized emission within atomically thin semiconductor nanobubbles. These insights hold implications for advancing the nano and quantum photonics with low-dimensional semiconductors.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS2004

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

McDaniels, Steven J.↗