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At least 505 records · Page 28

Shielded magnetic small-angle neutron scattering for characterization of radioactive samples

The development of a Pb-shielded fixture for the execution of a small-angle neutron scattering (SANS)-based workflow for interrogation of highly irradiated nuclear materials has been explored. The Pb shielding was specially designed to reduce the detected radioactivity from the specimen during SANS experiments, and the overall configuration is termed shielded magnetic SANS (SM-SANS). Two FeCrAl-based alloys, C35M and 125YF, were examined with the SM-SANS technique using a free-form size distribution locally monodisperse model in both the as-received and irradiated states. Quantitative values derived from the free-form size distribution were compared with atom probe tomography experiments. Microstructural and compositional parameters determined using the two characterization techniques were complements of each other. The results demonstrate that the SM-SANS technique is an effective means of characterizing nanoscale clustering in irradiated material systems and provides new avenues for investigating radioactive material microstructures.

FeCrAl↗

Neutron Diffraction Residual Stress Characterization of Large-Scale Components by WA-DED

Two large scale 316L stainless steel cylindrical shells were fabricated by wire arc directed energy deposition (WA DED). Residual stresses were measured by neutron diffraction, and the microstructure and mechanical properties of the printed material were characterized. Longitudinal and transverse residual stresses were compressive at the inner diameter, near neutral at mid wall, and tensile at the outer diameter; radial (through thickness) residual stresses were relatively low in magnitude, and peak tensile residual stresses occurred at the outer diameter surface along the longitudinal direction. The printed 316L SS exhibited a heterogeneous microstructure with finely dispersed δ ferrite, and demonstrated high yield and tensile strengths with large elongation and ductile fracture at ambient temperature and at 250 °C. These results indicate that the outer diameter surface and near surface regions—where tensile residual stress is highest—are the most vulnerable to residual stress–sensitive failure modes, such as stress corrosion cracking and fatigue.

36 MATERIALS SCIENCE↗

Novel Materials R&D for Next-Generation Accelerator Target Facilities

High-Entropy Alloys and Electrospun Nanofiber materials are two classes of novel materials that can offer improved resistance to beam-induced radiation damage and thermal shock. Research to develop these new materials specifically for multi-megawatt accelerator target applications, such as beam windows and particle-production targets, are ongoing at Fermilab within the scope of a DOE Early Career Research Program. The research program combines in-beam experiments with complementary simulations to tailor the microstructures of these novel materials for use in next-generation accelerator target facilities. Iterative simulations to optimize the material composition, physics performance, and beam-induced thermomechanical response will guide the material design and fabrication processes based on established figures of merit. This will be followed by material irradiation experiments using low-energy ions and prototypic high-energy protons with extensive post-irradiation material characterization to assess and qualify the selected novel materials. This talk will describe the alloy design and synthesis, microstructural pre-characterization of the alloys, and plans for the eventual down selection following low-energy ion irradiation studies.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Microscale Characterization of Damage Accumulation in CMCs

The developing roles of damage mechanisms in the failure response of SiC/SiC minicomposites was investigated by the characterization of microscale damage accumulation with respect to microstructure. A multi-modal approach combining spatially resolved acoustic emission (AE) with tensile testing in-SEM (scanning electron microscope) was used to simultaneously examine surface (observed in-SEM) and bulk damage (monitored via AE). Strong agreement was shown between the evolving crack density estimated by AE and in-SEM measurements. The following were observed: (i) in-plane matrix content and distribution impacted crack growth; (ii) spatially-distributed matrix cracks generated varying stress-dependent AE; and (iii) certain individual cracks became more probable failure locations due to unique combinations of damage mechanisms that drove their growth. This approach enabled characterizing potential failure determinants and suggests that early damage behavior is related to certain microstructural features (e.g. surface flaws), while subsequent damage behavior is coupled to interactions of local mechanisms evolving with stress.

ceramic matrix composites↗

Nondestructive ultrasonic characterization of a triple-weld-bead wire arc additively manufactured ER70S-6 S-curved wall

Understanding build-scale microstructural variation in wire arc additive manufacturing (WAAM) of low-carbon steels is essential for ensuring consistent structure–property relationships throughout large components. Conventional destructive characterization techniques, such as scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), are time-intensive and limited to localized regions, making comprehensive evaluation of large WAAM structures challenging. In this study, a nondestructive ultrasonic approach was employed to characterize a 252 mm tall ER70S-6 S-curved WAAM wall produced using a triple-bead deposition strategy. Optical and SEM analysis revealed a repeating dual-region microstructure consisting of uniform polygonal ferrite at melt pool centers and heterogeneous ferrite with coarse and fine grains near melt pool boundaries, attributed to cyclic thermal conditions. Longitudinal ultrasonic backscatter imaging was used to evaluate the continuity of this periodicity along the full build height. The ultrasonic response exhibited a consistent repeating pattern that correlated with the observed layer-wise microstructural variation. X-ray computed tomography confirmed the absence of detectable porosity, indicating that ultrasonic contrast is primarily governed by grain morphology. Overall, the results indicate that longitudinal backscatter ultrasound is a promising nondestructive characterization technique for validating microstructural variations along the s-curved WAAM wall, with significant potential for microstructure optimization and process control.

36 MATERIALS SCIENCE↗

Process-Microstructure-Property Relationships in Low Heat Input Wire-Arc Additive Manufacturing (WAAM) of Ni-Based Superalloy Haynes 282

Conference presentation on WAAM process optimization on Ni-based superalloy Haynes® 282®. This alloy is targeted for advanced power generation systems for its superior high temperature mechanical properties. Wire-arc additive manufacturing (WAAM) offers attractive cost and materials savings with high deposition rates. Based on initial build process optimization, WAAM blocks were made, and screened for defects using high-throughput CT scanning. The microstructural evolution in arc energy range of 250-700 J/mm was characterized in the as-built and aged conditions, using electron microscopy. Results showed self-consistent microstructure across conditions, with grain size dependence on arc energy, MC and M6C carbides in as-built, and blocky grain boundary M23C6 in as-heat-treated condition. Further reductions in as-built porosity were explored through 20+ combinations of H2 and CO2 additions to shielding gas. Initial results show improved wetting behavior, and bead overlap with up to 1% H2 and up to 0.25% CO2. Combination of experimentally determined datasets provided comprehensive understanding of process-structure-property relationships in WAAM Haynes 282.

Haynes 282↗

Impact-Induced Chondrule Deformation and Aqueous Alteration of CM2 Murchison

Deformed chondrules in CM2 Murchison have been found to define a prominent foliation [1,2] and lineation [3] in 3D using X-ray computed tomography (XCT). It has been hypothesized that chondrules in foliated chondrites deform by "squeezing" into surrounding pore space [4,5], a process that also likely removes primary porosity [6]. However, shock stage classification based on olivine extinction in Murchison is consistently low (S1-S2) [4-5,7] implying that significant intracrystalline plastic deformation of olivine has not occurred. One objective of our study is therefore to determine the microstructural mechanisms and phases that are accommodating the impact stress and resulting in relative displacements within the chondrules. Another question regarding impact deformation in Murchison is whether it facilitated aqueous alteration as has been proposed for the CMs which generally show a positive correlation between degree of alteration and petrofabric strength [7,2]. As pointed out by [2], CM Murchison represents a unique counterpoint to this correlation: it has a strong petrofabric but a relatively low degree of aqueous alteration. However, Murchison may not represent an inconsistency to the proposed causal relationship between impact and alteration, if it can be established that the incipient aqueous alteration post-dated chondrule deformation. Methods: Two thin sections from Murchison sample USNM 5487 were cut approximately perpendicular to the foliation and parallel to lineation determined by XCT [1,3] and one section was additionally polished for EBSD. Using a combination of optical petrography, SEM, EDS, and EBSD several chondrules were characterized in detail to: determine phases, find microstructures indicative of strain, document the geometric relationships between grain-scale microstructures and the foliation and lineation direction, and look for textural relationships of alteration minerals (tochilinite and Mg-Fe serpentine) that indicate timing of their formation relative to deformation event(s). Preliminary Results: Deformed chondrules are dominated by forsterite and clinoenstatite with lesser amounts of Fe-Mg serpentine, sulfides, and low calcium pyroxene. Olivine grains are commonly fractured but generally show sharp optical extinction. The pyroxene, in contrast, is not only fractured but also often displays undulose extinction. In addition, the clinoenstatite is frequently twinned but it is unclear whether the twins are the result of mechanical deformation or inversion from protoenstatite [8]. EBSD work is currently ongoing to determine if areas of higher crystallographic strain can be imaged and mapped, and to determine the pyroxene twin orientations. In regards to alteration, we have found evidence for post-deformation formation of tochilinite and Mg-Fe serpentine indicating that aqueous alteration has indeed post-dated the deformation of the chondrules.

Hanna, R. D.↗

Characterization of Carbon Foam Products Made from Coal at Atmospheric Pressure

Carbon foam products are currently manufactured on a commercial scale utilizing a high-pressure autoclave in batch mode. In an effort to increase manufacturing speed and reduce cost, carbon foam products (both panels and aggregates) were produced at atmospheric pressure in a continuous belt kiln. Here, the microstructure, properties, and performance of these materials were characterized and assessed in various applications. Lightweight aggregate was explored for use as a proppant, as well as it use in concrete and asphalt. The thermal conductivity, water permeability, and fire resistance of panels were evaluated, and its performance with respect to screw pullout was compared against conventional building materials. Some interesting performance aspects and potential for future work was revealed. This work was supported by a cooperative agreement with the Department of Energy – National Energy Technology Laboratory (DE-FOA-0002185, Area of Interest 4: Coal-Derived Carbon Foam Produced via a Continuous Process, award number DE-FE-0031992).

01 COAL, LIGNITE, AND PEAT↗

Postweld Heat Treatment on Toughness of Electric- Resistance Welded X70 Steel

In this report the effect of postweld heat treatment (PWHT) on Charpy V-notch impact toughness of a highfrequency electric-resistance welded (HF-ERW) grade X70 pipeline steel is investigated. PWHT thermal cycles are simulated using the Gleeble on the as-welded specimens. Microstructure, along with crystallographic texture and microhardness, is characterized in specimens that are impact tested at –5°C (23°F), –30°C (–22°F), and –45°C (–49°F). The impact toughness values show a wide scatter band and decrease with the increasing peak temperature of the PWHT. For higher peak temperatures, the microstructure of the heat-affected zone (HAZ) gradually changed from equiaxed ferrite to bainitic ferrite. Furthermore, the prior austenite grain size (PAGS) increases with the increasing peak temperature. The density of high-angle grain boundaries decreases, and the fraction of cleavage planes {100} parallel to the impact fracture plane increases for higher peak temperatures of the PWHT

36 MATERIALS SCIENCE↗

Status Report on Characterization of High Burnup Fuel with Advanced Nondestructive Pulsed Neutron PIE

Characterizing irradiated or spent nuclear fuels with pulsed neutron techniques provides microstructural data such as phase fractions as well as crystallographic data, e.g. lattice parameters, from diffraction analysis. Diffraction characterization is complemented by spatially resolved mapping of isotope densities from energy-resolved neutron imaging, in particular neutron absorption resonance imaging, and overall bulk isotope assay with better sensitivity for minority isotopes from neutron absorption resonance spectroscopy without spatial resolution. Furthermore, after characterization at ambient condition, heating of irradiated or spent fuel will allow to characterize differences of e.g. lattice thermal expansion or phase transition temperature and kinetics compared to fresh fuel as well as enable the study of disappearance of irradiation defects. This data enables benchmarking of predictions of properties of irradiated fuels for which otherwise experimental data is sparse. The effort described here strives to characterize a section cut from a high-burnup fuel. Volumes smaller than entire fuel pellets or rodlets as proposed here, e.g. sections cut from a fuel pellet, to pave the way to characterize entire pellets or rodlets in the future.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Defects in electro-optically active polymer solids

There is considerable current interest in the application of organic and polymeric materials for electronic and photonic devices. The rapid, non-linear optical (NLO) response of these materials makes them attractive candidates for waveguides, interferometers, and frequency doublers. In order to realize the full potential of these systems, it is necessary to develop processing schemes which can fabricate these molecules into ordered arrangements. There is enormous potential for introducing well-defined, local variations in microstructure to control the photonic properties of organic materials by rational 'defect engineering.' This effort may eventually become as technologically important as the manipulation of the electronic structure of solid-state silicon based devices is at present. The success of this endeavor will require complimentary efforts in the synthesis, processing, and characterization of new materials. Detailed information about local microstructure will be necessary to understand the influence of symmetry breaking of the solid phases near point, line, and planar defects. In metallic and inorganic polycrystalline materials, defects play an important role in modifying macroscopic properties. To understand the influence of particular defects on the properties of materials, it has proven useful to isolate the defect by creating bicrystals between two-component single crystals. In this way the geometry of a grain boundary defect and its effect on macroscopic properties can be determined unambiguously. In crystalline polymers it would be valuable to establish a similar depth of understanding about the relationship between defect structure and macroscopic properties. Conventionally processed crystalline polymers have small crystallites (10-20 nm), which implies a large defect density in the solid state. Although this means that defects may play an important or even dominant role in crystalline or liquid crystalline polymer systems, it also makes it difficult to isolate the effect of a particular boundary on a macroscopically observed property. However, the development of solid-state and thin-film polymerization mechanisms have facilitated the synthesis of highly organized and ordered polymers. These systems provide a unique opportunity to isolate and investigate in detail the structure of covalently bonded solids near defects and the effect of these defects on the properties of the material. The study of defects in solid polymers has been the subject of a recent review (Martin, 1993).

Martin, David C.↗

Corrosion of 316 L stainless steel under the natural circulation of molten NaCl-MgCl 2 salt

The corrosion behavior of 316 L stainless steel (SS) was studied via the natural circulation of molten eutectic NaCl-MgCl 2 salt through a microloop. The post-corrosion tested 316 L SS microloop sections were characterized with microscopy techniques to determine the microstructural and microchemical changes that occurred at the alloy/salt interface. It was found that 316 L SS showed heterogeneous dissolution at the hot-leg, whereas deposition of corrosion products occurred at the cold-leg. For the first time, experimentally obtained molten salt flow-induced corrosion of 316 L SS results were combined with computational thermodynamic-kinetic models to validate the dissolution and deposition in terms of elemental compositional changes at the alloy/salt interface. The thermodynamic-kinetic modeling predicted that the heterogeneous dissolution of Cr and Fe from the hot-leg section of 316 L SS persisted throughout the salt circulation. The model also estimated that, despite Cr deposition starting earlier than Fe, the total redeposition of Fe is expected to be significantly greater than that of Cr over the circulation of salt. Furthermore, the modeling accurately predicted the subsurface enrichment of Mo which is attributed to the reduced Cr activity and the relatively higher diffusion rate of Mo within the alloy matrix. Here, the agreement between modeling and experimental results confirms that Fe chlorides dissolve at the hot-leg and subsequently deposit at the cold-leg due to activity changes driven by the thermal gradient. By contrast, Cr was not detected in the cold-leg deposits, which is attributed to its weaker temperature dependence on activity, limiting its redeposition under these conditions.

36 - MATERIALS SCIENCE↗

Irradiation-Induced Structural Disorder and Its Influence on the Mechanical Response of Polycrystalline MoS2

Molybdenum disulfide (MoS2) thin films are widely used as dry-film lubricants and protective coatings in aerospace and other radiation-exposed environments. Conventional synthesis routes produce polycrystalline films whose grain boundaries and other native defects cause their mechanical and tribological behavior to differ substantially from that of ideal single crystals. Under irradiation, these films progressively evolve from polycrystalline structures, composed of layered MoS2 grains, into highly disordered and eventually amorphous structures, altering both their tribological performance and mechanical integrity. Here, we employ reactive atomistic simulations to investigate irradiation-driven structural evolution in bulk polycrystalline MoS2. Using controlled primary knock-on atom (PKA) events, we characterize the progressive transition from a polycrystalline microstructure to an amorphous network by tracking defect accumulation and structural disorder. We then establish how this transition modifies the dominant deformation mechanisms and the temperature-dependent tensile response. Specifically, irradiation suppresses interlayer sliding and delamination, mechanisms which facilitate the deformation of the pristine polycrystal, resulting in defect-induced hardening. Broadly, our results establish direct process–structure–property relationships linking irradiation-induced defect accumulation, microstructural evolution, deformation mechanisms, and mechanical behavior, providing an atomistic framework for understanding the structural integrity and long-term reliability of irradiated MoS2 coatings.

Moore, Daniel [Sandia National Laboratories (SNL)]↗

Electrodeposited Mo x S y O z /Ni Tribological Coatings

Deposition of molybdenum disulfide (MoS 2 ) coatings using physical vapor deposition (PVD) and mechanical burnishing has been widely assessed for solid lubricants in space applications but still suffers from line-of-sight constraints on complex geometries. Here, we highlight one of the first demonstrations of electrodeposited Mo x S y O z and Mo x S y O z /Ni thin-film coatings from aqueous solutions of ammonium tetrathiomolybdate for solid lubricant applications and their remarkable ability to provide low coefficients of friction and high wear resistance. Characterization of the coating morphology shows amorphous microstructures with a high oxygen content and cracking upon drying. Even so, electrodeposited Mo x S y O z can achieve low steady-state coefficients of friction (μ ∼ 0.05–0.06) and wear rates (2.6 × 10 –7 mm 3 /(N m)) approaching those of physical vapor deposited coatings (2.3 × 10 –7 mm 3 /(N m)). Additionally, we show that adding dopants such as nickel increased the wear rate (7.5 × 10 –7 mm 3 /(N m)) and initial coefficient of friction (μ i = 0.23) due to compositional modifications such as dramatic sub-stoichiometry (S/Mo ∼ 1) and expression of a NiO x surface layer, although doping did reduce the degree of cracking upon drying.

Babuska, Tomas F.↗

Three-dimensional photoluminescence imaging of threading dislocations in GaN by sub-band optical excitation

GaN is rapidly gaining attention for implementation in power electronics but is still impacted by its high density of threading dislocations (TDs), which have been shown to facilitate current leakage through devices limiting their performance and reliability. Here, we discuss a novel implementation of photoluminescence (PL) imaging to study TDs in regions within vertically structured p-i-n GaN (PIN) diodes consisting of metalorganic chemical vapor deposition (MOCVD) epitaxial layers grown on ammonothermal GaN (am-GaN) substrates. PL imaging with a sub-bandgap excitation energy (3.1 eV) reveals TDs with excellent clarity in three dimensions within the am-GaN substrate. Galvanometric-driven PL imaging allows the microstructure of hundreds of devices to be characterized in a single session, enhancing the screening process through the addition of device specific TD location tracking and density mapping. The visibility, structural characteristics, luminescent nature and evolution of TDs through the GaN growth process are described, potentially providing the ability to define TD structures associated with leakage current.

36 MATERIALS SCIENCE↗

Final Report on Characterization of Irradiated Sensors and Coupling Adhesive Bonds

This report summarizes characterization via scanning/transmission electron microscopy of the microstructures of the unirradiated and irradiated piezoelectric ultrasonic sensor/aluminum substrate assemblies using four commercially available inorganic coupling adhesives to bond two types of piezoelectric crystals to the substrates. The sample assemblies were irradiated in the PULSTAR reactor at NC State University and ultrasonic data was collected in-situ. ORNL LAMDA Laboratory capabilities were utilized to perform pre- and post-irradiation examination of the sensor assemblies. This document summarizes the PIE performed at the ORNL LAMDA laboratory. The results of the PIE described in this report are consistent with the ultrasonic data collected during irradiation – in particular, high temperature epoxy adhesive seemed to provide the best coupling as compared to the refractory ceramic adhesives. It was determined that the quality of the sensor-adhesive-substrates governed the ultrasonic performance of the sensors. It was also apparent that irradiation did not significantly affect bond quality, which is also supported by the ultrasonic data collected during irradiation. A more comprehensive DOE NSUF Final Report including details of materials selection, sample fabrication, initial ultrasonic testing, irradiation and in-situ ultrasonic testing, positron annihilation lifetime spectroscopy and doppler broadening spectroscopy performed at EPRI and NC State University will be published at the conclusion of the project.

36 MATERIALS SCIENCE↗

Microstructure and mechanical properties of a single crystal NiAl alloy with Zr or Hf rich G-phase precipitates

The possibility of producing NiAl reinforced with the G-phase (Ni16X6Si7), where X is Zr or Hf, has been investigated. The microstructure of these NiAl alloys have been characterized in the as-cast and annealed conditions. The G-phases are present as fine cuboidal precipitates (10 to 40 nm) and have lattice parameters almost four times that of NiAl. They are coherent with the matrix and fairly resistant to coarsening during annealing heat treatments. Segregation and nonuniform precipitate distribution observed in as-cast materials were eliminated by homogenization at temperatures near 1600 K. Slow cooling from these temperatures resulted in large plate shaped precipitates, denuded zones, and a loss of coherency in some of the large particles. Faster cooling produced a homogeneous fine distribution of cuboidal G-phase particles in the matrix. Preliminary mechanical properties for the Zr-doped alloy are presented and compared to binary single crystal NiAl. The presence of these precipitates appears to have an important strengthening effect at temperatures not less than 1000 K compared to binary NiAl single crystals.

Locci, I. E.↗

Thermomechanical Fatigue Damage/Failure Mechanisms in SCS-6/Timetal 21S [0/90](Sub S) Composite

The thermomechanical fatigue (TMF) deformation, damage, and life behaviors of SCS6/Timetal 21S (0/90)s were investigated under zero-tension conditions. In-phase (IP) and out-of-phase (OP) loadings were investigated with a temperature cycle from 150 to 650 deg C. An advanced TMF test technique was used to quantify mechanically damage progression. The technique incorporated explicit measurements of the macroscopic (1) isothermal static moduli at the temperature extremes of the TMF cycle and (2) coefficient of thermal expansion (CTE) as functions of the TMF cycles. The importance of thermal property degradation and its relevance to accurate post-test data analysis and interpretation is briefly addressed. Extensive fractography and metallography were conducted on specimens from failed and interrupted tests to characterize the extent of damage at the microstructure level. Fatigue life results indicated trends analogous to those established for similar unidirectional(0) reinforced titanium matrix composite systems. High stress IP and mid to low stress OP loading conditions were life-limiting in comparison to maximum temperature isothermal conditions. Dominant damage mechanisms changed with cycle type. Damage resulting from IP TMF conditions produced measurable decreases in static moduli but only minimal changes in the CTE. Metallography on interrupted and failed specimens revealed extensive (0) fiber cracking with sparse matrix damage. No surface initiated matrix cracks were present. Comparable OP TMF conditions initiated environment enhanced surface cracking and matrix cracking initiated at (90) fiber/matrix (F/M) interfaces. Notable static moduli and CTE degradations were measured. Fractography and metallography revealed that the transverse cracks originating from the surface and (90) F/M interfaces tended to converge and coalesce at the (0) fibers.

Castelli, Michael G.↗