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At least 37 records · Page 2

Synchrotron-based Infrared Microspectroscopy as a Useful Tool to Study Hydration States of Meteorite Constituents

The meteorites Dho 225 and Dho 735 were recently found in Oman. Studies of their mineralogical and chemical composition suggest that these unusual meteorites are thermally metamorphosed CM2 chondrites [1,2,3]. Similar to Antarctic metamorphosed carbonaceous chondrites, the Dho 225 and Dho 735 are enriched in heavy oxygen compared to normal CMs [1,2]. However, IR studies indicating dehydration of matrix phyllosilicates are needed to confirm that the two new meteorites from Oman are thermally metamorphosed [4]. Synchrotron-based IR microspectroscopy is a new promising technique which allows the acquisition of IR spectra from extremely small samples. Here we demonstrate that this non-destructive technique is a useful tool to study hydration states of carbonaceous chondrites in situ. In addition, we acquired reflectance spectra of bulk powders of the Dho 225 and Dho 735 in the range of 0.3-50 microns.

Moroz, L. V.↗

Optimizing performance and yield of vertical GaN diodes using wafer scale optical techniques

Abstract To improve the manufacturing of vertical GaN devices for power electronics applications, the effects of defects in GaN substrates need to be better understood. Many non-destructive techniques including photoluminescence, Raman spectroscopy and optical profilometry, can be used to detect defects in the substrate and epitaxial layers. Raman spectroscopy was used to identify points of high crystal stress and non-uniform conductivity in a substrate, while optical profilometry was used to identify bumps and pits in a substrate which could cause catastrophic device failures. The effect of the defects was studied using vertical P-i-N diodes with a single zone junction termination extention (JTE) edge termination and isolation, which were formed via nitrogen implantation. Diodes were fabricated on and off of sample abnormalities to study their effects. From electrical measurements, it was discovered that the devices could consistently block voltages over 1000 V (near the theoretical value of the epitaxial layer design), and the forward bias behavior could consistently produce on-resistance below 2 mΩ cm 2 , which is an excellent value considering DC biasing was used and no substrate thinning was performed. It was found that high crystal stress increased the probability of device failure from 6 to 20%, while an inhomogeneous carrier concentration had little effect on reverse bias behavior, and slightly (~ 3%) increased the on-resistance (R on ). Optical profilometry was able to detect regions of high surface roughness, bumps, and pits; in which, the majority of the defects detected were benign. However a large bump in the termination region of the JTE or a deep pit can induce a low voltage catastrophic failure, and increased crystal stress detected by the Raman correlated to the optical profilometry with associated surface topography.

42 ENGINEERING↗

High Resolution X-Ray Diffraction of Macromolecules with Synchrotron Radiation

We recently combined synchrotron-based monochromatic X-ray diffraction topography methods with triple axis diffractometry and rocking curve measurements: high resolution X-ray diffraction imaging techniques, to better understand the quality of protein crystals. We discuss these methods in the light of results obtained on crystals grown under different conditions. These non destructive techniques are powerful tools in the characterization of the protein crystals and ultimately will allow to improve, develop, and understand protein crystal growth. High resolution X-ray diffraction imaging methods will be discussed in detail in light of recent results obtained on Hen Egg White Lysozyme crystals and other proteins.

Stojanoff, Vivian↗

Electrochemical reduction of per- and polyfluorinated alkyl substances (PFAS): is it possible? Applying experimental and quantum mechanical insights from the reductive defluorination literature

Remediation of per- and polyfluorinated alkyl substances (PFAS) in global water systems is a critical human and environmental health challenge facing society. PFAS consumption is associated with a litany of adverse health effects, and our knowledge of these dangers is still evolving. Current techniques to remove PFAS from water include adsorption to media (e.g. granular activated carbon, ion-exchange resin), nanofiltration, and reverse osmosis. However, these processes create a concentrated PFAS residual that requires further management. Destructive techniques are therefore needed to detoxify these residuals. Oxidative techniques have garnered the most attention (e.g. supercritical water oxidation, electrochemical oxidation) but are energy intensive and potentially form toxic by-products. As an alternative, several groups have researched advanced reduction processes that form aqueous electrons, but these processes are still chemical and energy intensive (e.g. ultraviolet/SO 3 2− , electron beam). This concise review therefore focuses on whether electrochemical reduction — a chemical-free, modular process — could be technically feasible for PFAS destruction.

King, Jacob F.↗

Residual stress determination in oxide layers at different length scales combining Raman spectroscopy and X-ray diffraction: Application to chromia-forming metallic alloys

In oxidizing environments, the protection of metals and alloys against further oxidation at high temperature is provided by the oxide film itself. This protection is efficient only if the formed film adheres well to the metal (substrate), i.e., without microcracks and spalls induced by thermomechanical stresses. In this study, the residual stresses at both macroscopic and microscopic scales in the oxide film adhering to the substrate and over the damaged areas have been rigorously determined on the same samples for both techniques. Ni-30Cr and Fe-47Cr alloys have been oxidized together at 900 and 1000 °C, respectively, to create films with a thickness of a few microns. A multi-scale approach was adopted: macroscopic stress was determined by conventional X-ray diffraction and Raman spectroscopy, while microscopic residual stress mappings were performed over different types of bucklings using Raman micro-spectroscopy and synchrotron micro-diffraction. A very good agreement is found at macro- and microscales between the residual stress values obtained with both techniques, giving confidence on the reliability of the measurements. In addition, relevant structural information at the interface between the metallic substrate and the oxide layer was collected by micro-diffraction, a non-destructive technique that allows mapping through the oxide layer, and both the grain size and the crystallographic orientation of the supporting polycrystalline metal located either under a buckling or not were measured.

36 MATERIALS SCIENCE↗

O-6 Optical Property Degradation of the Hubble Space Telescope's Wide Field Camera-2 Pick Off Mirror

Degradation in the performance of optical components can be greatly affected by exposure to the space environment. Many factors can contribute to such degradation including surface contaminants; outgassing; vacuum, UV, and atomic oxygen exposure; temperature cycling; or combinations of parameters. In-situ observations give important clues to degradation processes, but there are relatively few opportunities to correlate those observations with post-flight ground analyses. The return of instruments from the Hubble Space Telescope (HST) after its final servicing mission in May 2009 provided such an opportunity. Among the instruments returned from HST was the Wide-Field Planetary Camera-2 (WFPC-2), which had been exposed to the space environment for 16 years. This work focuses on the identifying the sources of degradation in the performance of the Pick-off mirror (POM) from WFPC-2. Techniques including surface reflectivity measurements, spectroscopic ellipsometry, FTIR (and ATR-FTIR) analyses, SEM/EDS, X-ray photoelectron spectroscopy (XPS) with and without ion milling, and wet and dry physical surface sampling were performed. Destructive and contact analyses took place only after completion of the non-destructive measurements. Spectroscopic ellipsometry was then repeated to determine the extent of contaminant removal by the destructive techniques, providing insight into the nature and extent of polymerization of the contaminant layer.

McNamara, Karen M.↗

Root growth and development in response to CO2 enrichment

A non-destructive technique (minirhizotron observation tubes) was used to assess the effects of CO2 enrichment on root growth and development in experimental plots in a scrub oak-palmetto community at the Kennedy Space Center. Potential effects of CO2 enrichment on plants have a global significance in light of concerns over increasing CO2 concentrations in the Earth's atmosphere. The study at Kennedy Space Center focused on aboveground physiological responses (photosynthetic efficiency and water use efficiency), effects on process rates (litter decomposition and nutrient turnover), and belowground responses of the plants. Belowground dynamics are an exceptionally important component of total plant response but are frequently ignored due to methodological difficulties. Most methods used to examine root growth and development are destructive and, therefore, severely compromise results. Minirhizotrons allow nondestructive observation and quantification of the same soil volume and roots through time. Root length density and root phenology were evaluated for CO2 effects with this nondestructive technique.

Day, Frank P., Jr.↗

Identification of New Lithic Clasts in Lunar Breccia 14305 by Micro-CT and Micro-XRF Analysis

From 1969 to 1972, Apollo astronauts collected 382 kg of rocks, soils, and core samples from six locations on the surface of the Moon. The samples were initially characterized, largely by binocular examination, in a custom-built facility at Johnson Space Center (JSC), and the samples have been curated at JSC ever since. Despite over 40 years of study, demand for samples remains high (~500 subsamples per year are allocated to scientists around the world), particularly for plutonic (e.g., anorthosites, norites, etc.) and evolved (e.g., granites, KREEP basalts) lithologies. The reason for the prolonged interest is that as new scientists and new techniques examine the samples, our understanding of how the Moon, Earth, and other inner Solar System bodies formed and evolved continues to grow. Scientists continually clamor for new samples to test their emerging hypotheses. Although all of the large Apollo samples that are igneous rocks have been classified, many Apollo samples are complex polymict breccias that have previously yielded large (cm-sized) igneous clasts. In this work we present the initial efforts to use the non-destructive techniques of micro-computed tomography (micro-CT) and micro x-ray fluorescence (micro-XRF) to identify large lithic clasts in Apollo 14 polymict breccia sample 14305. The sample in this study is 14305,483, a 150 g slab of regolith breccia 14305 measuring 10x6x2 cm (Figure 1a). The sample was scanned at the University of Texas High-Resolution X-ray CT Facility on an Xradia MicroXCT scanner. Two adjacent overlapping volumes were acquired at 49.2 micrometer resolution and stitched together, resulting in 1766 slices. Each volume was acquired at 100 kV accelerating voltage and 98 mA beam current with a 1 mm CaF2 filter, with 2161 views gathered over 360deg at 3 seconds acquisition time per view. Micro-XRF analyses were done at Washington University in St. Louis, Missouri on an EDAX Orbis PC micro-XRF instrument. Multiple scans were made at 40 kV accelerating voltage, 800 mA beam current, 30 μm beam diameter, and a beam spacing of 30-120 micrometer. The micro-CT scan of 14305,483 (Figure 2) was able to identify several large lithic clasts (approx. 1 cm) within the interior of the slab. These clasts will be exposed by band-sawing or chipping of the slab, and their composition more fully characterized by subsequent micro-XRF analysis. In addition to lithic clasts, the micro-CT scans identified numerous mineral clasts, including many FeNi metal grains, as well as the prominent fractures within the slab. The micro-XRF analyses (Figure 1b,c) of the slab surfaces revealed the bulk chemical compositions (qualitative) of the different clast types observed. In particular, by looking at the ratios of major elements (e.g. Ca:Mg:Fe), differences among the many observed clast types are readily observed. Moreover, several clasts not apparent to the naked eye were revealed in the K:Al:Si ratio map. The scans are also able to identify small grains of Zr- and P-rich minerals (not shown), which could in turn yield important age dates for the samples.

Zeigler, Ryan A.↗

Advanced Characterization Capabilities for Nuclear Materials via Nuclear Science User Facilities (NSUF)

Advanced post-irradiation examination (PIE) techniques are required to design new or improved nuclear materials, characterize, and understand in-core behavior of fuel and materials, and support the qualification of new reactor materials. The Nuclear Science User Facilities (NSUF) is the U.S. Department of Energy Office of Nuclear Energy's only designated nuclear science user facility. NSUF provides researchers access to PIE capabilities at Idaho National Laboratory and at a diverse mix of university, national laboratory and industrial partner institutions. The PIE capabilities include novel destructive and non-destructive techniques for radiation damage characterization, such as advanced diffraction techniques (X-ray, electron, or neutron) coupled to extreme environments; in-situ observation of microstructural evolution under irradiation; in-situ irradiation to monitor corrosive attack in coolant environments; in-situ irradiation and mechanical testing; and test methods for synergistic effects of superimposed extreme environments (temperature, irradiation, stress, corrosion) on materials behaviors. This talk will provide an overview of NSUF PIE capabilities.

36 MATERIALS SCIENCE↗

AE (Acoustic Emission) for Flip-Chip CGA/FCBGA Defect Detection

C-mode scanning acoustic microscopy (C-SAM) is a nondestructive inspection technique that uses ultrasound to show the internal feature of a specimen. A very high or ultra-high-frequency ultrasound passes through a specimen to produce a visible acoustic microimage (AMI) of its inner features. As ultrasound travels into a specimen, the wave is absorbed, scattered or reflected. The response is highly sensitive to the elastic properties of the materials and is especially sensitive to air gaps. This specific characteristic makes AMI the preferred method for finding "air gaps" such as delamination, cracks, voids, and porosity. C-SAM analysis, which is a type of AMI, was widely used in the past for evaluation of plastic microelectronic circuits, especially for detecting delamination of direct die bonding. With the introduction of the flip-chip die attachment in a package; its use has been expanded to nondestructive characterization of the flip-chip solder bumps and underfill. Figure 1.1 compares visual and C-SAM inspection approaches for defect detection, especially for solder joint interconnections and hidden defects. C-SAM is specifically useful for package features like internal cracks and delamination. C-SAM not only allows for the visualization of the interior features, it has the ability to produce images on layer-by-layer basis. Visual inspection; however, is only superior to C-SAM for the exposed features including solder dewetting, microcracks, and contamination. Ideally, a combination of various inspection techniques - visual, optical and SEM microscopy, C-SAM, and X-ray - need to be performed in order to assure quality at part, package, and system levels. This reports presents evaluations performed on various advanced packages/assemblies, especially the flip-chip die version of ball grid array/column grid array (BGA/CGA) using C-SAM equipment. Both external and internal equipment was used for evaluation. The outside facility provided images of the key features that could be detected using the most advanced C-SAM equipment with a skilled operator. Investigation continued using in-house equipment with its limitations. For comparison, representative X-rays of the assemblies were also gathered to show key defect detection features of these non-destructive techniques. Key images gathered and compared are: Compared the images of 2D X-ray and C-SAM for a plastic LGA assembly showing features that could be detected by either NDE technique. For this specific case, X-ray was a clear winner. Evaluated flip-chip CGA and FCBGA assemblies with and without heat sink by C-SAM. Only the FCCGA package that had no heat sink could be fully analyzed for underfill and bump quality. Cross-sectional microscopy did not revealed peripheral delamination features detected by C-SAM. Analyzed a number of fine pitch PBGA assemblies by C-SAM. Even though the internal features of the package assemblies could be detected, C-SAM was unable to detect solder joint failure at either the package or board level. Twenty times touch ups by solder iron with 700degF tip temperature, each with about 5 second duration, did not induce defects to be detected by C-SAM images. Other techniques need to be considered to induce known defects for characterization. Given NASA's emphasis on the use of microelectronic packages and assemblies and quality assurance on workmanship defect detection, understanding key features of various inspection systems that detect defects in the early stages of package and assembly is critical to developing approaches that will minimize future failures. Additional specific, tailored non-destructive inspection approaches could enable low-risk insertion of these advanced electronic packages having hidden and fine features.

Ghaffarian, Reza↗

Correlating energy density induced residual stress, porosity, and mechanical property variations in directed energy deposition using neutron diffraction and imaging techniques

In a directed energy deposition (DED) process, the energy density deposited into the materials drives the structure and properties. The energy density is influenced by several printing parameters, such as laser power, hatch spacing, scanning speed, etc. In this study, 316L stainless steels samples were fabricated with varying hatch spacing aiming to induce variations in sample microstructure and properties. A combination of techniques including engineering neutron diffraction, neutron computed tomography, and tensile testing, were employed to correlate the structure and macroscopic properties. Porosity was predominantly observed at the bottom of the deposited materials and was effectively reduced by decreased hatch spacing. Correlatively, compressive residual stress was observed at the bottom of the specimens, while internal stress is largely determined by the hatch spacing. The residual stress in general decreases as the hatch spacing decreases. The maximum ultimate tensile strength (UTS) was found to increase from 517.4 to 528.6 MPa with a strain increased from 0.847 to 0.897 as the hatch spacing decreased from 0.45 to 0.42 mm. However, further increase in energy density by reducing the hatch spacing resulted in a significant decrease in UTS (as low as 452 MPa). This work provides new insights from bulk non-destructive techniques into correlating energy density induced residual stress, porosity, and mechanical property variations in directed energy deposition.

316L stainless steel↗

Manufacturing and characterization of continuous fiber-reinforced thermoplastic tape overmolded long fiber thermoplastic

Light-weight construction, design freedom, integration of functions, and compelling cost element are desired by Original Equipment Manufacturers (OEMs) and their suppliers. The emergence of overmolding of continuous-discontinuous reinforcement enables design freedom and ability to tailor stiffness, strength, and damage tolerance for structural applications. In this work, long fiber thermoplastics (LFT) are overmolded with continuous fiber-reinforced thermoplastic (CFRTP) tape are combined using extrusion compression molding process to evaluate the structural performance. The CFRTP tape overmolded LFT samples were characterized using nondestructive and destructive techniques to track fiber alignment, fiber distribution, manufacturing defects, interfacial bonding of the tape – LFT and effect of CFRTP tape on LFT. Mode 1 fracture toughness, G 1c for tape overmolded LFT was higher by 25–30% compared to literature reported G 1c . This response was attributed to excellent fiber distribution, good fiber wetting, and absence of voids at the interface. Three-point bend test indicated that CFRTP tape overmolded LFT composites were better able to resist damage under the bending load compared to constituent LFT composite. Flexural strength of the overmolded composite was higher by 119–142%, and modulus higher by 77–65% compared to constituent LFT composite. Simulated flexural results accurately represents the mechanical behavior of composites. Here, the penetration energy of tape overmolded LFT composites determined by LVI test was in the range of 27.66–30.15 J, which is significantly higher than constituent LFT composite, 7.76 J. CFRTP tape overmolded LFT composite exhibits progressive fiber fracture, matrix cracking, and interfacial debonding failure, whereas, constituent LFT composite showed catastrophic fiber fracture.

42 ENGINEERING↗

A scoping review of non-destructive testing (NDT) techniques in building performance diagnostic inspections

Understanding building envelope thermodynamics is an essential foundation of building sciences, mainly due to the envelope’s role as a boundary layer for exterior environments, as well as a container and regulator of internal microclimates. This paper presents a scoping literature review of select Non-destructive Testing (NDT) techniques for building envelope scanning and surveying for thermodynamic diagnostics. The investigation focuses specifically on reviewing six NDT techniques: Ground Penetrating Radar (GPR), Light Detection and Ranging (LiDAR)/Laser Scanning, Thermography, Ultrasound, Close-Range Photogrammetry and Through Wall Imaging Radar (TWIR). The aim is to identify knowledge gaps in terms of their use in accurately characterizing envelope compositions for further integration in Building Energy Modeling (BEM). Each technique was evaluated according to set categories imbibed from the American Society of Heating, Refrigerating, and Air Conditioning Engineering (ASHRAE) Standard 211P that showcase the technique’s ability to extract various relevant information. A framework is then developed to inform users on how to use hybrid NDT-based workflows applied in building envelope energy audits. The study concludes by discussing possibilities of utilizing NDT in large-scale audit automation, BEM integration, and developing built environment policies focusing on increasing existing building performance through retrofitting design.

36 MATERIALS SCIENCE↗

Unraveling the Correlation between Raman and Photoluminescence in Monolayer MoS 2 through Machine‐Learning Models

Abstract 2D transition metal dichalcogenides (TMDCs) with intense and tunable photoluminescence (PL) have opened up new opportunities for optoelectronic and photonic applications such as light‐emitting diodes, photodetectors, and single‐photon emitters. Among the standard characterization tools for 2D materials, Raman spectroscopy stands out as a fast and non‐destructive technique capable of probing material's crystallinity and perturbations such as doping and strain. However, a comprehensive understanding of the correlation between photoluminescence and Raman spectra in monolayer MoS 2 remains elusive due to its highly nonlinear nature. Here, the connections between PL signatures and Raman modes are systematically explored, providing comprehensive insights into the physical mechanisms correlating PL and Raman features. This study's analysis further disentangles the strain and doping contributions from the Raman spectra through machine‐learning models. First, a dense convolutional network (DenseNet) to predict PL maps by spatial Raman maps is deployed. Moreover, a gradient boosted trees model (XGBoost) with Shapley additive explanation (SHAP) to bridge the impact of individual Raman features in PL features is applied. Last, a support vector machine (SVM) to project PL features on Raman frequencies is adopted. This work may serve as a methodology for applying machine learning to characterizations of 2D materials.

Lu, Ang‐Yu↗

High-gradient magnetic filtration of UO 2 colloids from aqueous suspensions

Environmental samples often contain innocuous components that make trace actinide analysis difficult and expensive. Therefore, it is expedient to separate these materials from actinide particles. One characteristic of many actinides is that they are paramagnetic. High-gradient magnetic filtration (HGMF) is a non-destructive technique that selectively captures magnetic constituents from a matrix containing non-magnetic species. Here, in this work, a novel HGMF device made of a permanent magnet array was used to effectively separate UO 2 particles from undesirable soil species. Up to 88% of the UO 2 particles present in suspensions were effectively captured by HGMF, resulting in their enrichment and a substantial reduction in the concentrations of other constituents.

Actinide separations↗

Influence of Exposure to Multiple Brazing Cycles on the Integrity of OFE Copper Brazed Joints

A 10 MeV, 5 kW S-band travelling wave electron linear accelerator has been developed at Raja Ramanna Centre for Advanced Technology for industrial applications. The electron accelerating structure is made of oxygen-free electronic (OFE) copper and comprises of fifty-six brazed joints and is fabricated in multiple stages, as per the process and testing requirements. The accelerating structure is often required to be repaired through an additional brazing cycle with the same filler. The present study evaluates possible microstructural and mechanical property degradation of OFE copper brazed joints, as a result of its exposure to multiple brazing cycles. The study was performed on an OFE copper cavity stack brazed assembly, made through a four-stage brazing using BVAg-8 as braze filler. The resultant brazed assembly did not exhibit any leak at a sensitivity of 1 × 10{sup −10} mbar.L/s. The results of the study demonstrate that OFE copper brazements can be safely subjected to an additional brazing cycle without causing significant degradation in its microstructure and strength. However, brazed joint’s exposure to any additional brazing cycles results in the formation of voids and cracks due to intergranular penetration of silver, with associated drop in tensile strength from about 210 MPa to about 150-180 MPa. Based on the results of study, it is recommended to qualify the accelerating structure, fabricated through multiple brazing cycles, by a suitable non-destructive technique. The results of the study are important for design, fabrication and maintenance of electron linear accelerator components.

36 MATERIALS SCIENCE↗

Application of neutron imaging to investigate fundamental aspects of durability of cement-based materials: A review

Service life and durability of reinforced concrete structures have become crucial issues in all industrialized countries because of their economic and ecological relevance. Limited durability is frequently due to deterioration of steel and cement-based materials, such as mortar and concrete, by interactions with water and aggressive aqueous solutions. Neutron imaging has proved to be a powerful non-destructive technique to study quantitatively water content and water movement in porous materials. A neutron beam is much more attenuated by hydrogen in water than by most other elements present in cement-based materials. In this review, focus is placed on applications of both two-dimensional neutron radiography and three-dimensional neutron tomography to investigate specific aspects of durability and deterioration of cement-based materials. Examples of results obtained by qualitative and quantitative investigations of moisture movement in cracked and uncracked cement-based materials are presented. Self-healing, efficiency of water repellent treatment, internal curing, frost damage, fire spalling, ettringite formation and observations of various reinforced concrete components are addressed. The results obtained by neutron imaging provide a solid basis for better understanding of deterioration mechanisms of cement-based materials. Recent improvements of neutron imaging facilities have allowed unexpected possibilities to study complex processes in cement-based materials. The potential for further research based on this promising technology is outlined and discussed.

36 MATERIALS SCIENCE↗

Joint inversion of electromagnetic measurements for the determination of water saturation profiles in concrete structures

Highlights: • DC-electrical and dielectric data are combined to estimate concrete saturation degree. • A joint inversion approach of the electromagnetic measurements is proposed. • The sensitivity of the measurements to the saturation model parameters is analysed. • The new joint approach was developed and is applied to synthetic and real data. • The benefits of the joint approach over the inversion of one data type are highlighted. Water saturation profiles in concrete are essential to assess its durability and can be determined using non-destructive techniques, especially the electric and the capacitive methods. In this paper, we propose a new inversion scheme where both resistivity and permittivity measurements are inverted jointly to retrieve the saturation profile. The finite element method is used to model the measurements in 3D, the concrete having a saturation profile with depth, represented by a continuous model taking the form of a Weibull curve with four parameters. A non-linear least-squares optimization based on the Levenberg-Marquardt scheme is developed for the inversion of measurements. Results show that information gathered from both measurements enriches the reconstructed profile, leading to a more reliable estimation of saturation profiles. We believe that the joint inversion method herein developed could lead to the study of more complex phenomena, such as the coupled water-chloride ingress.

36 MATERIALS SCIENCE↗