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At least 181 records · Page 10

FY24 Progress Report: SRNL Analysis of ICCWR LCM and WAMS data for Corrosion and Cracking

Algorithms for Machine Learning (ML) and data analysis for the 3013 Surveillance Program have been developed in an ongoing collaborative effort by the Savannah River National Laboratory (SRNL) and the University of South Carolina (USC). The objective of the algorithms is to automate the identification of corrosion and crack formation in the Inner Container Closure Weld Region (ICCWR) of the canister system used to store Pu-bearing material. Data for corrosion and cracking is collected from large binary files generated by a Laser Confocal Microscope (LCM), the Wide Area 3D Measurement System (WAMS), or,in a recent proposal, by a Scanning Electron Microscope (SEM). The ML software uses the physical attributes in the data files (e.g., one or more of: height, color, and 16-bit grayscale values as functions of position in a plane projection) to detect signs of surface corrosion and cracking after being trained on similar data, with the features to be detected. Although the initial scope included screening for broader indicators of corrosion, e.g., pitting, identification of potential cracks was prioritized for the past several years at the request of program leadership. Labeled training data is essential to developing the ML algorithm, and enhancements to data labeling capability have been developed to address this essential precursor to application of ML routines. Efficient labeling is particularly important in view of the large volume of data required to train ML algorithms and the relative rarity of cracks in the ICCWR data set. The updated program will read binary data from either LCM, WAMS or SEM files, interrogate data attributes, facilitate user labeling of data for training ML algorithms, execute ML algorithms, output parameters from trained ML algorithms, report ML model accuracy with respect to labeled data, and generate graphical representations for various analyses. In FY24, hourglass neural networks (HNNs) that were initiated in FY22 were further developed and tested using available LCM data, and their performance was tested against that of the alternative U-Net Neural Network algorithm structure. HNNs along with previously developed Convolutional Neural Networks (CNNs) and Deep Neural Networks (DNNs) comprise a suite of ML tools for identification of cracks in the ICCWR

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

FY25 Progress Report: SRNL Analysis of ICCWR LCM and WAMS data for Corrosion and Cracking

Algorithms for Machine Learning (ML) and image analysis for the 3013 Surveillance Program have been developed in an ongoing collaborative effort by the Savannah River National Laboratory (SRNL) and the University of South Carolina (USC). The objective of the algorithms is to automate the identification of corrosion and cracks in the Inner Container Closure Weld Region (ICCWR) of the canister system used to store Pu-bearing material. Data for corrosion and cracking is collected from large binary files generated by a Laser Confocal Microscope (LCM), the Wide Area 3D Measurement System (WAMS), or, in a recent proposal, by a Scanning Electron Microscope (SEM). The ML software uses the physical attributes in the data files (e.g., one or more of: height, color, and 16-bit grayscale values as functions of position in a plane projection) to detect signs of surface corrosion and cracking after being trained on similar data with the features to be detected. Although the initial scope included screening for broader indicators of corrosion, e.g., pitting, the identification of potential cracks was prioritized for the past several years at the request of program leadership.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Plasma sprayed Fe(76)Nd(16)B(8) permanent magnets

Thin coatings (0.16 mm) and thick coatings (0.50 mm) of Fe(76)Nd(16)B(8) were deposited on stainless-steel substrates by low pressure plasma spraying. Microscopic examination of the coatings in a light microscope revealed excessive porosity, but good bonding to the substrate. Fracture cross sections examined in a scanning electron microscope showed the grains to be equiaxed and approximately 1 micron or less in diameter in the as-sprayed condition. The intrinsic coercivities of the as-sprayed coatings varied from 5.8 to 10.9 kOe. The effects of postspray heat treatments on the intrinsic coercivity are also given.

Overfelt, R. A.↗

Space Shuttle Columbia Aging Wiring Failure Analysis

A Space Shuttle Columbia main engine controller 14 AWG wire short circuited during the launch of STS-93. Post-flight examination divulged that the wire had electrically arced against the head of a nearby bolt. More extensive inspection revealed additional damage to the subject wire, and to other wires as well from the mid-body of Columbia. The shorted wire was to have been constructed from nickel-plated copper conductors surrounded by the polyimide insulation Kapton, top-coated with an aromatic polyimide resin. The wires were analyzed via scanning electron microscope (SEM), energy dispersive X-Ray spectroscopy (EDX), and electron spectroscopy for chemical analysis (ESCA); differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA) were performed on the polyimide. Exemplar testing under laboratory conditions was performed to replicate the mechanical damage characteristics evident on the failed wires. The exemplar testing included a step test, where, as the name implies, a person stepped on a simulated wire bundle that rested upon a bolt head. Likewise, a shear test that forced a bolt head and a torque tip against a wire was performed to attempt to damage the insulation and conductor. Additionally, a vibration test was performed to determine if a wire bundle would abrade when vibrated against the head of a bolt. Also, an abrasion test was undertaken to determine if the polyimide of the wire could be damaged by rubbing against convolex helical tubing. Finally, an impact test was performed to ascertain if the use of the tubing would protect the wire from the strike of a foreign object.

McDaniels, Steven J.↗

Computer image analysis of etched tracks from ionizing radiation

I proposed to continue a cooperative research project with Dr. David S. McKay concerning image analysis of tracks. Last summer we showed that we could measure track densities using the Oxford Instruments eXL computer and software that is attached to an ISI scanning electron microscope (SEM) located in building 31 at JSC. To reduce the dependence on JSC equipment, we proposed to transfer the SEM images to UHCL for analysis. Last summer we developed techniques to use digitized scanning electron micrographs and computer image analysis programs to measure track densities in lunar soil grains. Tracks were formed by highly ionizing solar energetic particles and cosmic rays during near surface exposure on the Moon. The track densities are related to the exposure conditions (depth and time). Distributions of the number of grains as a function of their track densities can reveal the modality of soil maturation. As part of a consortium effort to better understand the maturation of lunar soil and its relation to its infrared reflectance properties, we worked on lunar samples 67701,205 and 61221,134. These samples were etched for a shorter time (6 hours) than last summer's sample and this difference has presented problems for establishing the correct analysis conditions. We used computer counting and measurement of area to obtain preliminary track densities and a track density distribution that we could interpret for sample 67701,205. This sample is a submature soil consisting of approximately 85 percent mature soil mixed with approximately 15 percent immature, but not pristine, soil.

Blanford, George E.↗

Thermomechanical Degradation of Sintered Copper Under High-Temperature Thermal Shock

The need for reliable bonded interface materials is critical to realize the performance benefits of wide-bandgap devices in power electronics modules, especially in operating temperatures greater than 150 degrees C. 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 C to 200 degrees C) conditions. In the fabrication phase of the samples, we used different stencil patterns and found 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 compared to a full-area print. The paste consisted of Cu microflakes, and we performed sintering using a Budatec SP300 sintering press at 275 degrees C 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 scanning electron microscope images, which revealed adhesive fracture as the dominant failure mechanism.

ADVANCED PROPULSION SYSTEMS,INORGANIC, ORGANIC, PH↗

Machine Learning-Enabled Quantitative Analysis of Optically Obscure Scratches on Nickel-Plated Additively Manufactured (AM) Samples

Additively manufactured metal components often have rough and uneven surfaces, necessitating post-processing and surface polishing. Hardness is a critical characteristic that affects overall component properties, including wear. This study employed K-means unsupervised machine learning to explore the relationship between the relative surface hardness and scratch width of electroless nickel plating on additively manufactured composite components. The Taguchi design of experiment (TDOE) L9 orthogonal array facilitated experimentation with various factors and levels. Initially, a digital light microscope was used for 3D surface mapping and scratch width quantification. However, the microscope struggled with the reflections from the shiny Ni-plating and scatter from small scratches. To overcome this, a scanning electron microscope (SEM) generated grayscale images and 3D height maps of the scratched Ni-plating, thus enabling the precise characterization of scratch widths. Optical identification of the scratch regions and quantification were accomplished using Python code with a K-means machine-learning clustering algorithm. The TDOE yielded distinct Ni-plating hardness levels for the nine samples, while an increased scratch force showed a non-linear impact on scratch widths. The enhanced surface quality resulting from Ni coatings will have significant implications in various industrial applications, and it will play a pivotal role in future metal and alloy surface engineering.

36 MATERIALS SCIENCE↗

Results of examination of the returned Surveyor 3 samples for particulate impacts

The television housing and a section of the strut of the radar altimeter and Doppler velocity sensor were examined optically and with a scanning electron microscope for particulate impacts. The white surface of the camera was discolored during the months the Surveyor 3 was on the moon; however, most of the craters must have occurred as a result of lunar dust sandblasted by the LM exhaust. The polished section of the strut exhibits contamination which appears brown and seems to be partially composed of crystals. Electron microscopic analysis of the strut section indicated no craters of hypervelocity impact origin, confirmed pitting density results of the optical scans, and indicated that material in the craters is of lunar origin. No meteorite impacts larger than 25 microns were detected on the tubing section.

Cour-Palais, B. G.↗

Effect of matrix resin on the impact fracture characteristics of graphite-epoxy laminates

The effect of resin chemistry on basic impact energy absorbent mechanisms exibited by graphite-epoxy composites was investigated. Impact fracture modes and microscopic resin deformation characteristics were examined for 26 NASA-impacted graphite epoxy laminates with different resin chemistries. Discrete specimen fracture modes were identified through cross sectional examination after impact, and subsequently compared with measured glass transition temperatures, cure cycles, and residual impact capabilities. Microscopic resin deformation mechanisms and their overall relationship to impact loading conditions, voids, and resin content were also characterized through scanning electron microscopic examination of separated fracture surfaces.

Hertzberg, P. E.↗

Minority carrier diffusion length and edge surface-recombination velocity in InP

A scanning electron microscope was used to obtain the electron-beam-induced current (EBIC) profiles in InP specimens containing a Schottky barrier perpendicular to the scanned (edge) surface. An independent technique was used to measure the edge surface-recombination velocity. These values were used in a fit of the experimental EBIC data with a theoretical expression for normalized EBIC (Donolato, 1982) to obtain the electron (minority carrier) diffusion length.

Hakimzadeh, Roshanak↗

Automated Weld Characterization Using the Thermoelectric Method

The effective assessment of the integrity of welds is a complicated NDE problem that continues to be a challenge. To be able to completely characterize a weld, detailed knowledge of its tensile strength, ductility, hardness, microstructure, macrostructure, and chemical composition is needed. NDE techniques which can provide information on any of these features are extremely important. In this paper, we examine a seldom used approach based on the thermoelectric (TE) effect for characterizing welds and their associated heat affected zone (HAZ). The thermoelectric method monitors the thermoelectric power which is sensitive to small changes in the kinetics of the conduction electrons near the Fermi surface that can be caused by changes in the local microstructure. The technique has been applied to metal sorting, quality testing, flaw detection, thickness gauging of layers, and microscopic structural analysis. To demonstrate the effectiveness of the technique for characterizing welds, a series of tungsten-inert-gas welded Inconel-718 samples were scanned with a computer controlled TE probe. The samples were then analyzed using a scanning electron microscope and Rockwell hardness tests to characterize the weld and the associated HAZ. We then correlated the results with the TE measurements to provide quantitative information on the size of the HAZ and the degree of hardness of the material in the weld region. This provides potentially valuable information on the strength and fatigue life of the weld. We begin the paper by providing a brief review of the TE technique and then highlight some of the factors that can effect the measurements. Next, we provide an overview of the experimental procedure and discuss the results. Finally, we summarize our findings and consider areas for future research.

Fulton, J. P.↗

Residual strength of five boron/aluminum laminates with crack-like notches after fatigue loading

Boron/aluminum specimens were made with crack-like slits in the center and with various proportions of 0 and + or - 45 deg plies. They were fatigue loaded and then fractured to determine their residual strengths. The fatigue loads were generally in the range of 60 to 80 percent of the static tensile strength of the specimen as determined from a previous study, and the stress ratio was .05. For virtually all of the specimens the fatigue loading was continued for 100,000 cycles. The specimens were radiographed after the fatigue loading to determine the nature of the fatigue damage. A few specimens were sectioned and examined in a scanning electron microscope after being radiographed in order to verify the interpretation of the radiographs and also to get a better insight into the nature of the fatigue damage. The results indicate that the fatiguing does not significantly affect the strength of the specimens tested. The results of the radiography and of the scanning electron microscopy indicate that the 45 deg plies suffer extensive damage in the form of split and broken fibers and matrix cracking in the vicinity of the ends of the split. By contrast, the only significant damage to the 0 deg plies was a single 0 deg matric crack growing from the ends of the slit and between the 0 deg fibers.

Simonds, R. A.↗

Residual strength of five boron/aluminum laminates with crack-like notches after fatigue loading

Boron/aluminum specimens were made with crack-like slits in the center and with various proportions of 0 and + or - 45 deg plies. They were fatigue loaded and then fractured to determine their residual strengths. The fatigue loads were generally in the range of 60 to 80 percent of the static tensile strength of the specimen as determined from a previous study, and the stress ratio was .05. For virtually all of the specimens the fatigue loading was continued for 100,000 cycles. The specimens were radiographed after the fatigue loading to determine the nature of the fatigue damage. A few specimens were sectioned and examined in a scanning electron microscope after being radiographed in order to verify the interpretation of the radiographs and also to get a better insight into the nature of the fatigue damage. The results indicate that the fatiguing does not significantly affect the strength of the specimens tested. The results of the radiography and of the scanning electron microscopy indicate that the 45 deg plies suffer extensive damage in the form of split and broken fibers and matrix cracking in the vicinity of the ends of the split. By contrast, the only significant damage to the 0 deg plies was a single 0 deg matric crack growing from the ends of the slit and between the 0 deg fibers.

Simonds, R. A.↗

A digital holography ex situ measurement characterization of plasma-exposed surface erosion from an electrothermal arc source

Digital holography has been proposed to fulfill a need for an imaging diagnostic capable of in situ monitoring of surface erosion caused by plasma–material interaction in nuclear fusion devices. A digital holography diagnostic for 3D surface erosion measurement has been developed at Oak Ridge National Laboratory with the goal of deployment on a plasma device. A proof-of-concept in situ demonstration is planned which would involve measurement of plasma erosion on targets exposed to an electrothermal arc source. This work presents the results of an ex situ characterization of the capability and limitations of holographic imaging of targets exposed to the arc source. Targets were designed to provide a fiducial for comparison of deformed and unaffected areas. The results indicated that the average net erosion was ~150 nm/plasma exposure, which is expected to be within the diagnostic’s measurement capacity. Surface roughness averages determined by holographic image analysis showed good agreement with measurements taken with a profilometer. Finally, the limit of the holography diagnostic’s x–y spatial resolution was characterized by comparison with scanning electron microscope imaging.

47 OTHER INSTRUMENTATION↗

Analysis of the electron-beam-induced current of a polycrystalline p-n junction when the diffusion lengths of the material on either side of a grain boundary differ

The short circuit current generated by the electron beam of a scanning electron microscope in p-n junctions is reduced by enhanced recombination at grain boundaries in polycrystalline material. Frequently, grain boundaries separate the semiconductor into regions possessing different minority carrier life times. This markedly affects the short circuit current I(sc) as a function of scanning distance from the grain boundary. It will be shown theoretically that (1) the minimum of the I(sc) in crossing the grain boundary with the scanning electron beam is shifted away from the grain boundary toward the region with smaller life time (shorter diffusion length), (2) the magnitude of the minimum differs markedly from those calculated under the assumption of equal diffusion lengths on either side of the grain boundary, and (3) the minimum disappears altogether for small surface recombination velocities (s less than 10,000 cm/s). These effects become negligible, however, for large recombination velocities s at grain boundaries. For p-type silicon this happens for s not less than 100,000 cm/s.

Von Roos, O.↗

Quantitative Specifications to Avoid Degradation during E-Beam and Induced Current Microscopy of Halide Perovskite Devices

Degradation due to electron beam exposure has posed a challenge in the use of electron microscopy to probe halide perovskite materials and devices. Herein, the interaction between the electron beam and the perovskite across acceleration voltages and at low probe currents is investigated in a scanning electron microscope (SEM) by monitoring the electron-beaminduced current (EBIC) response in perovskite solar cells in a planview configuration. SEM probe conditions are identified where dozens of repeated scans over a single region of the perovskite solar cell induce minimal electronic degradation. Overall, the induced current response of the perovskite device is found to strongly depend upon the beam condition: rapid decay occurs at high beam powers, the current activates at the lowest beam powers, and a newfound quasi-steady response is revealed at intermediate beam conditions. A quantitative window for the successful conduction of e-beam studies with minimal electronic degradation is revealed by evaluating induced current response over a wide range of perovskite devices, which invites broader use of SEM-based characterization techniques, including EBIC, as powerful techniques for correlative microscopy investigations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A microscopic study of crack initiation mechanisms in 7075 aluminum alloy sheets.

A study of the opening mode of crack initiation in 7075-T6 aluminum alloy sheets has been conducted with the aid of a scanning electron microscope. Observations were made from several orientations, including the top view of the specimen which showed the notch profile and the edge view of the specimen which showed the entire notch front along the specimen thickness. It was found that the edge view exhibited the first signs of permanent deformation at about 55% of the breaking strength. These changes took the form of deformation bands which were aligned in the direction of the tensile axis and apparently defined limiting regions of homogeneous slip. It is felt that the appearance of microcracks at loads approaching the breaking strength was of fundamental importance in the formation of the final fracture surface. Many of these microcraks were initiated at intermetallic particles and other metallurgically weak regions on the notch surface. It was also possible to correlate the strain in the notch with the stress intensity factor for the various loads. Very large plastic strains were observed on the notch tip as compared to published values of elongation at fracture for unnotched specimens.

Jones, D. L.↗