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At least 217 records · Page 12

In-situ investigation of incipient melting in a 319 type Al alloy using laser scanning confocal microscopy

Highlights: • In-situ analysis of incipient melting of ternary eutectic in Al alloy. • Incipient melting occurred in three distinct stages in the eutectic. • Increased heating rate increase rate of liquid film propagation. • Incipient melting transformed initial eutectic structure and caused oxidation. • Study determined incipient melting mechanism for eutectic structures. - Abstract: The modified 319 Al alloy system has been used extensively in precision sand casting of automotive powertrain applications such as engine blocks and cylinder heads, with significant improvement in vehicle fuel efficiency. However, a concern in elevated temperature processing of Al alloys, such as heat treatment and hot working processes, is incipient melting of secondary phases, which is deleterious to mechanical properties. In this study, the laser scanning confocal microscopy (LSCM) technique was used in the analysis of in-situ changes in microstructure as a result of incipient melting. Microstructural analysis was carried out prior to and following elevated temperature exposure in the LSCM using optical microscopy, SEM and EDX. The results suggest that incipient melting of the Al-Al{sub 2}Cu-Al{sub 5}Mg{sub 8}Cu{sub 2}Si{sub 6} ternary eutectic clusters was initiated by the formation of a liquid film which propagated rapidly from the eutectic clusters, coating the Al dendrites in regions adjacent to the eutectic clusters. Following film formation, the ternary eutectic clusters melted completely. Incipient melting also resulted in a localized change in composition in the interdendritic channels as supported by a change in cluster morphology from eutectic to a combination of coarse blocky Al-Cu-Ni and Si particles, and ultra-fine eutectic.

36 MATERIALS SCIENCE↗

Spatial filter based light-sheet laser interference technique for three-dimensional nanolithography

We propose a laser interference technique for the fabrication of 3D nano-structures. This is possible with the introduction of specialized spatial filter in a 2π cylindrical lens system (consists of two opposing cylindrical lens sharing a common geometrical focus). The spatial filter at the back-aperture of a cylindrical lens gives rise to multiple light-sheet patterns. Two such interfering counter-propagating light-sheet pattern result in periodic 3D nano-pillar structure. This technique overcomes the existing slow point-by-point scanning, and has the ability to pattern selectively over a large volume. The proposed technique allows large-scale fabrication of periodic structures. Computational study shows a field-of-view (patterning volume) of approximately 12.2 mm{sup 3} with the pillar-size of 80 nm and inter-pillar separation of 180 nm. Applications are in nano-waveguides, 3D nano-electronics, photonic crystals, and optical microscopy.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

AGR-1 Compact 4-1-1 Post-Irradiation Examination Results

Destructive post-irradiation examination was performed on AGR-1 fuel Compact 4-1-1, which was irradiated to a final compact-average burnup of 19.4% FIMA (fissions per initial metal atom) and a time-average, volume-average temperature of 1072°C. The analysis of this compact focused on characterizing the extent of fission product release from the particles and examining particles to determine the condition of the kernels and coating layers. The work included deconsolidation of the compact and leach-burn-leach analysis, visual inspection and gamma counting of individual particles, metallurgical preparation of selected particles, and examination of particle cross-sections with optical microscopy, electron microscopy, and elemental analysis. Deconsolidation-leach-burn-leach (DLBL) analysis revealed no particles with failed TRISO or failed SiC layers (as indicated by very low uranium inventory in all of the leach solutions). The total fractions of the predicted compact inventories of fission products Ce-144, Cs-134, Cs-137, and Sr-90 that were present in the compact outside of the SiC layers were <2×10 -6 , based on DLBL data. The Ag-110m fraction in the compact outside the SiC layers was 3.3×10 -2 , indicating appreciable release of silver through the intact coatings and subsequent retention in the OPyC layers or matrix. The Eu-154 fraction was 2.4×10 -4 , which is equivalent to the inventory in one average particle, and indicates a small but measurable level of release from the intact coatings. Gamma counting of 61 individual particles indicated no particles with anomalously low fission product retention. The average ratio of measured inventory to calculated inventory was close to a value of 1.0 for several fission product isotopes (Ce-144, Cs-134, and Cs-137), indicating good retention and reasonably good agreement with the predicted inventories. Measured-to-calculated (M/C) activity ratios for fission products Eu-154, Eu-155, Ru-106, Sb-125, and Zr-95 were significantly less than 1.0. However, as no significant release of these fission products from compacts was noted during previous analysis of the AGR-1 capsule components, the low M/C ratios are most likely an indication of a bias in the inventories predicted by physics simulations of the AGR-1 experiment. The distribution of Ag-110m M/C ratios was centered on a value of 1.02 and was fairly broad (standard deviation of 0.18, with values as high as 1.42 and as low as 0.68). Based on all data gathered to date, it is believed that silver retention in the particles was on average relatively high, but that the broad distribution in values among the particles represents significant variation in the inventory of Ag-110m generated in the particles. Ceramographic analysis of particle cross-sections revealed many of the characteristic microstructures often observed in irradiated AGR-1 particles from other fuel compacts. Palladium-rich fission product clusters were observed in the IPyC and SiC layers near the IPyC-SiC interface of three Compact 4-1-1 particle cross-sections. In spite of the presence of fission product clusters in the SiC layer, no significant corrosion or degradation of the layer was observed in any of the particles examined.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Polaritonic Probe of an Emergent 2D Dipole Interface

The use of work-function-mediated charge transfer has recently emerged as a reliable route toward nanoscale electrostatic control of individual atomic layers. Using α-RuCl 3 as a 2D electron acceptor, we are able to induce emergent nano-optical behavior in hexagonal boron nitride (hBN) that arises due to interlayer charge polarization. Using scattering-type scanning near-field optical microscopy (s-SNOM), we find that a thin layer of α-RuCl 3 adjacent to an hBN slab reduces the propagation length of hBN phonon polaritons (PhPs) in significant excess of what can be attributed to intrinsic optical losses. Concomitant nano-optical spectroscopy experiments reveal a novel resonance that aligns energetically with the region of excess PhP losses. These experimental observations are elucidated by first-principles density-functional theory and near-field model calculations, which show that the formation of a large interfacial dipole suppresses out-of-plane PhP propagation. Finally, our results demonstrate the potential utility of charge-transfer heterostructures for tailoring optoelectronic properties of 2D insulators.

36 MATERIALS SCIENCE↗

Phase control of austenitic chrome-nickel steel

The paper presents the results of the comparative study of the possibilities of different structural and magnetic methods for detection and visualization of the strain-induced martensitic phase in low carbon austenitic chromium-nickel steel. Results of TEM, SEM, optical microscopy, atomic and magnetic force microscopy, and magnetic measurements are presented. Amount of the magnetic strain-induced martensite was estimated. We pioneered magnetic force microscopic images of the single domain cluster distribution of the strain-induced martensite in austenite-ferrite materials.

36 MATERIALS SCIENCE↗

The effect of hydrogen on the parameters of plastic deformation localization in low carbon steel

In the present study, the effect of interstitial hydrogen atoms on the mechanical properties and plastic strain localization patterns in tensile tested polycrystals of low-carbon steel Fe-0.07%C has been studied using double exposure speckle photography technique. The main parameters of plastic flow localization at various stages of deformation hardening have been determined in polycrystals of steel electrolytically saturated with hydrogen in a three-electrode electrochemical cell at a controlled constant cathode potential. Also, the effect of hydrogen on changing of microstructure by using optical microscopy has been demonstrated.

36 MATERIALS SCIENCE↗

Characterization of Pu-238 Heat Source Granule Containment

The Milliwatt Radioisotopic Themoelectric Generator (RTG) provides power for permissive-action links. Essentially these are nuclear batteries that convert thermal energy to electrical energy using a doped silicon-germanium thermopile. The thermal energy is provided by a heat source made of 238 Pu, in the form of 238 PuO 2 granules. The granules are contained by 3 layers of encapsulation. A thin T-111 liner surrounds the 238 PuO 2 granules and protects the second layer (strength member) from exposure to the fuel granules. An outer layer of Hastalloy-C protects the T-111 from oxygen embrittlement. The T-111 strength member is considered the critical component in this 238 PuO 2 containment system. Any compromise in the strength member seen during destructive testing required by the RTG surveillance program is characterized. The T-111 strength member is characterized through Scanning Electron Microscopy (SEM), and Metallography. SEM is used in the Secondary Electron mode to reveal possible grain boundary deformation and/or cracking in the region of the strength member weld. Deformation and cracking uncovered by SEM are further characterized by Metallography. Metallography sections are mounted and polished, observed using optical microscopy, then documented in the form of microphotographs. SEM mat further be used to examine polished Metallography mounts to characterize elements using the SEM mode of Energy Dispersive X-ray spectroscopy (EDS).

07 ISOTOPE AND RADIATION SOURCES↗

Characterization of Oxide + TiN Inclusions in Fe-16 Mass Pct Cr Ferritic Alloy Using Automatic SEM-EDS Analysis

The assessment of automatic SEM-EDS results is significant to reveal the possible inaccuracy of the results and the limitation of this characterization technique in analyzing inclusions. In current research, the oxide + TiN inclusion in Fe-16 mass pct Cr ferritic alloy is characterized by emphasizing the effects of Mg addition and N content on the composition, morphology, homogeneity of dispersion, and size distribution of inclusions; the assessment of automatic SEM-EDS results in rapid analysis concerning its limitation and the utilization of its advantage to clarify the formation mechanism of inclusions are conducted. The nature of inclusions is revealed. Mg addition makes the number density of inclusions larger and the size of inclusions finer. The effect of N content on the size of oxde + TiN was not obvious. Automatic SEM-EDS analysis is deficient in detecting light elements and low content elements in the inclusions and distinguishing between TiN and oxide + TiN. Optimizing the experimental design and combining automatic SEM-EDS results with manual SEM-EDS and optical microscopy results can contribute to delivering accurate and speedy results.

36 MATERIALS SCIENCE↗

Thermal Inspection for the Assessment of Adhesively Bonded Metal Adherents

Certification of adhesively bonded structures is currently a challenge for aircraft manufacturers. The ability to certify bonds in primary structure can reduce dependence on fasteners and this will enable more efficient manufacturing. For example, drilling holes and installing fasteners in bonded joints can be a potentially significant bottleneck in airframe manufacturing. In addition, fasteners increase the airframe weight and can add stress concentration areas. Reducing fastener count can accelerate manufacturing and improve aircraft performance. NASA is currently investigating nondestructive evaluation (NDE) techniques to assess bond integrity. For example, bond thickness influences bond strength and therefore NDE techniques are being investigated to determine bond thickness. For bonded metal structures, there is a large difference in the thermal diffusivity between the 7075 aluminum alloy metal adherends and aircraft grade adhesive. Multi-layered thermal models show a large variation in the thermal response for bondline adhesive thicknesses that vary from 100 to 300 microns for adherend thicknesses of 0.163 cm. Experimental through-transmission thermal measurements reveal promise to quantitatively characterize the bondline thickness. Results were validated with X-ray computed tomography and optical microscopy measurements, and influence of porosity on the thermal model and measurements are investigated.

bondline thickness↗

Microstructural Characterization and High Strain Rate Plastic Flow Behavior of SMAW Armox500T Steel Joints from Spherical Indentation Experiments

Static indentation and uniaxial compression tests have been conducted on Armox500T steel and its weldments to predict the constraint factor (CF), i.e., ratio of Meyer’s hardness to uniaxial flow stress. Series of dynamic indentation experiments were carried out at impact velocities ranging from 5 to 300 m/s to estimate dynamic hardness as a function of average strain. Subsequently, dynamic indentation (DI) test data and CF determined under static indentation conditions have been used to study the high strain rate plastic flow behavior of Armox500T weldments in comparison with the base metal. It was observed that flow stress for Armox500T and its weldments under dynamic loading conditions (10{sup 4} s{sup −1}) are significantly higher than flow stress measured under static loading conditions (10{sup −3} s{sup −1}). The plastic flow behavior computed from DI is in good agreement with the data evaluated through conventional split Hopkinson pressure bar technique. Further, the study of the microstructure of base metal and weldments by optical microscopy and SEM revealed a considerable variation in the microstructure.

36 MATERIALS SCIENCE↗

Fabrication and Characterization of A5083-WC-Al{sub 2}O{sub 3} Surface Composite by Friction Stir Processing

In this study, WC-Al{sub 2}O{sub 3} ceramic composite was incorporated into Al5083 to produce a surface composite by friction stir processing (FSP), and the microstructure, hardness and wear properties of Al5083-WC-Al{sub 2}O{sub 3} surface composite were evaluated. Optical microscopy of FSPed samples showed grain refinement in the stir zone. The addition of WC-Al{sub 2}O{sub 3} particles as well as increase in FSP pass number had a considerable effect on grain refinement, and the grain size of Al5083 base metal of 36 µm reduced to 11 µm for Al5083-WC-Al{sub 2}O{sub 3} surface composite after four passes. The SEM observation of the surface composite revealed that the WC-Al{sub 2}O{sub 3} particles distributed homogenously in the matrix and by increasing the FSP passes, the initial agglomerates of mechanochemically synthesized WC-Al{sub 2}O{sub 3} powders could be fractured. Microhardness evaluation showed a substantial improvement by adding WC-Al{sub 2}O{sub 3} particles and increase in FSP pass number. The maximum microhardness value of 101 HV belonged to surface composite after four passes, while the microhardness of the base metal was 65 HV. Wear test results revealed enhanced tribological behavior with a similar trend of microhardness values. Scanning electron microscopy tests revealed both adhesive and abrasive wear mechanisms on the surface of the wear test specimens.

36 MATERIALS SCIENCE↗

Narrow-band near-field nanoscopy in the spectral range from 1.3 to 8.5 THz

Nano-spectroscopy in the terahertz frequency range remains challenging despite recent technological progress in developing both THz emitter sources and near-field optical microscopy (SNOM). Here, we combine scattering-type SNOM with a free-electron laser light source, to tune into the 1.3–8.5 THz range. A significant portion of this range, namely, the frequencies above ∼3 THz, is not covered by previously reported near-field microscopy systems. However, it constitutes an indispensable regime where many elementary processes in solids including collective lattice excitations, charge, and spin transport occur. Our approach of nano-spectroscopy and nano-imaging provides a versatile analysis of nanostructures as small as 50 nm, hence beating the optical diffraction limit by λ/4600.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Generation of cylindrically polarized vector vortex beams with digital micromirror device

We propose a novel technique to directly transform a linearly polarized Gaussian beam into vector-vortex beams with various spatial patterns. Full high-quality control of amplitude and phase is implemented via a Digital Micro-mirror Device (DMD) binary holography for generating Laguerre-Gaussian, Bessel-Gaussian, and helical Mathieu–Gaussian modes, while a radial polarization converter (S-waveplate) is employed to effectively convert the optical vortices into cylindrically polarized vortex beams. Additionally, the generated vector-vortex beams maintain their polarization symmetry after arbitrary polarization manipulation. Due to the high frame rates of DMD, rapid switching among a series of vector modes carrying different orbital angular momenta paves the way for optical microscopy, trapping, and communication.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Large Photothermal Effect in Sub-40 nm h-BN Nanostructures Patterned Via High-Resolution Ion Beam

The controlled nanoscale patterning of 2D materials is a promising approach for engineering the optoelectronic, thermal, and mechanical properties of these materials to achieve novel functionalities and devices. Herein, high-resolution patterning of hexagonal boron nitride (h-BN) is demonstrated via both helium and neon ion beams and an optimal dosage range for both ions that serve as a baseline for insulating 2D materials is identified. Through this nanofabrication approach, a grating with a 35 nm pitch, individual structure sizes down to 20 nm, and additional nanostructures created by patterning crystal step edges are demonstrated. Raman spectroscopy is used to study the defects induced by the ion beam patterning and is correlated to scanning probe microscopy. Photothermal and scanning near-field optical microscopy measure the resulting near-field absorption and scattering of the nanostructures. These measurements reveal a large photothermal expansion of nanostructured h-BN that is dependent on the height to width aspect ratio of the nanostructures. This effect is attributed to the large anisotropy of the thermal expansion coefficients of h-BN and the nanostructuring implemented. Finally, the photothermal expansion should be present in other van der Waals materials with large anisotropy and can lead to applications such as nanomechanical switches driven by light.

2D materials↗

Methods of chemical and phase composition analysis of gallstones

This review presents the instrumental methods used for chemical and phase composition investigation of gallstones. A great body of data has been collected in the literature on the presence of elements and their concentrations, obtained by fluorescence microscopy, X-ray fluorescence spectroscopy, neutron activation analysis, proton (particle) induced X-ray emission, atomic absorption spectroscopy, high-resolution gamma-ray spectrometry, electron paramagnetic resonance. Structural methods—powder X-ray diffraction, infrared spectroscopy, Raman spectroscopy—provide information about organic and inorganic phases in gallstones. Stone morphology was studied at the macrolevel with optical microscopy. Results obtained by analytical scanning and transmission electron microscopy with X-ray energy dispersive spectrometry are discussed. The chemical composition and structure of gallstones determine the strategy of removing stone from the body and treatment of patients: surgery or dissolution in the body. Therefore one chapter of the review describes the potential of dissolution methods. Early diagnosis and appropriate treatment of the disease depend on the development of clinical methods for in vivo investigation, which gave grounds to present the main characteristics and potential of ultrasonography (ultrasound scanning), magnetic resonance imaging, and X-ray computed tomography.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Enhancing Nanoparticle Detection in Interferometric Scattering (iSCAT) Microscopy Using a Mask R-CNN

Interferometric scattering microscopy (iSCAT) is a label-free optical microscopy technique that enables imaging of individual nano-objects such as nanoparticles, viruses, and proteins. Essential to this technique is the suppression of background scattering and identification of signals from nano-objects. In the presence of substrates with high roughness, scattering heterogeneities in the background, when coupled with tiny stage movements, cause features in the background to be manifested in background-suppressed iSCAT images. Traditional computer vision algorithms detect these background features as particles, limiting the accuracy of object detection in iSCAT experiments. Here, in this paper, we present a pathway to improve particle detection in such situations using supervised machine learning via a mask region-based convolutional neural network (mask R-CNN). Using a model iSCAT experiment of 19.2 nm gold nanoparticles adsorbing to a rough layer-by-layer polyelectrolyte film, we develop a method to generate labeled datasets using experimental background images and simulated particle signals and train the mask R-CNN using limited computational resources via transfer learning. We then compare the performance of the mask R-CNN trained with and without inclusion of experimental backgrounds in the dataset against that of a traditional computer vision object detection algorithm, Haar-like feature detection, by analyzing data from the model experiment. Results demonstrate that including representative backgrounds in training datasets improved the mask R-CNN in differentiating between background and particle signals and elevated performance by markedly reducing false positives. The methodology for creating a labeled dataset with representative experimental backgrounds and simulated signals facilitates the application of machine learning in iSCAT experiments with strong background scattering and thus provides a useful workflow for future researchers to improve their image processing capabilities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Oxidation and alpha-case formation in Ti–6Al–2Sn–4Zr–2Mo alloy

Isothermal heat treatments in ambient air were performed on wrought Ti–6Al–2Sn–4Zr–2Mo (Ti-6242) material at 500, 593 and 700°C for times up to 500 h. In the presence of oxygen at elevated temperatures simultaneous reactions occurred in Ti-6242 alloy, which resulted in the formation of an oxide scale and a layer with higher oxygen concentration (termed as alpha-case). Total weight gain analysis showed that there was a transition in the oxidation kinetics. At 500°C, the oxidation kinetics obeyed a cubic relationship up to 200 h and thereafter changed to parabolic at prolonged exposure times. At 593°C, it followed a parabolic relationship. After heat treatment at 700°C, the oxidation obeyed a parabolic relationship up to 200 h and thereafter changed to linear at prolonged exposure times. The observed transition is believed to be due to the differences observed in the oxide scale. The activation energy for parabolic oxidation was estimated to be 157 kJ/mol. In addition, alpha-case layer was evaluated using optical microscope, electron probe micro-analyser and microhardness tester. The thickness of the alpha-case layer was found to be a function of temperature and time, increasing proportionally, and following a parabolic relationship. The activation energy for the formation of alpha-case layer was estimated to be 153 kJ/mol. - Highlights: • Transition in oxidation kinetics was observed in Ti–6Al–2Sn–4Zr–2Mo alloy in the temperature range 500–700°C. • The activation energy for parabolic oxidation and for alpha-case formation is about 157 kJ/mol and 153 kJ/mol. • Thickness of alpha-case layer estimated by optical microscopy and electron probe microanalysis is comparable.

36 MATERIALS SCIENCE↗

Validation of process simulation workflow for thermosetting prepreg platelet molding compounds

Continuous carbon fiber prepreg slit and cut into rectangular platelets has proven to be a useful material for net shape molding of semi-structural and structural components in the aerospace and automotive industries. Furthermore, to assist the designer in use of these prepreg platelet molding compounds, sometimes called carbon fiber sheet molding compounds, simulation tools are required that can predict the as-manufactured fiber orientation state which has a significant impact on the resulting performance. Herein, an analysis workflow for design-enabling predictions is demonstrated for a double dome geometry with two different initial charge configurations. Here, the workflow is validated through comparison with experimental short shots, orientation state, and stiffness trends. Significantly, to complete the validation, a method is proposed for determining the confidence bounds on measured orientation state enhancing the results of optical microscopy which can only produce a small sample of platelet orientations.

36 MATERIALS SCIENCE↗