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At least 433 records · Page 24

Development of a pulsed, variable-energy positron beam for atomic scale defect studies

Positron annihilation spectroscopy provides a sensitive means of non-destructive characterization of materials, capable of probing single atom vacancies in solids with 10 –7 sensitivity. Here, in this work, we detail the development of a magnetically guided, variable energy, pulsed positron beam designed to conduct depth-dependent defect studies in metals, semiconductors, and dielectrics, which will be the first of its kind in the United States. The design of the target stage provides capabilities for measurements during in situ annealing up to 800 °C and incorporates a new approach to minimize the background due to energetic backscattered positrons. The developed beam at Bowling Green State University provides a powerful tool for characterization of thin films, devices, and ion irradiated materials.

47 OTHER INSTRUMENTATION↗

Boundary characterization using 3D mapping of geometrically necessary dislocations in AM Ta microstructure

Additive manufacturing (AM) of high strength metallic materials produces microstructures and defects that deviate substantially from those created through conventional manufacturing methods. It has recently been demonstrated that with application of extreme energy densities, a high-temperature refractory metal, tantalum (Ta), can be printed to a fully dense state with exceptionally low porosity. Here we employ a combination of three-dimensional electron backscattered diffraction (EBSD) TriBeam technology and crystallographic geometrically necessary dislocation (GND) theory to characterize the microstructure and defect boundaries of this unusual AM product. Two-dimensional (2D) EBSD and these three-dimensional (3D) measurements indicate that the microstructure of AM Ta is highly oriented <111> along the build direction, yet at the same time contains large crystallographic orientation gradients that span mm’s across the build. Crystallographic GND density analysis of the 3D microstructure reveals that highly misoriented subboundaries exist within this strongly textured microstructure that have large dislocation densities of 1×10 16 m –2 , just as large as those comprising the high-angle grain boundaries (HAGBs) in the same material. The 3D crystallographic GND density mapping reveals these subboundaries are part of a complex, finely spaced network that extends throughout the entire microstructure. Here, the orientation of these boundaries can be related to the scan strategy used during printing. TEM measurements corroborate an extremely high dislocation density at the microscale and indicate a cell-like dislocation network structure existing in the AM Ta at the sub-μm scale.

36 MATERIALS SCIENCE↗

Coupled phase field damage and crystal plasticity analysis of intragranular fracture: The role of crystallographic orientation and voids

Damage evolution in engineering metal alloys at the grain scale exhibits significant microstructural heterogeneity and anisotropy. These heterogeneities create local hotspots for stress and strain localization, leading to void nucleation. Crystal orientation influences the active slip systems around voids, affecting lattice rotation and potentially forming discontinuities. At low triaxiality, voids may change shape due to lower stress, rotation, elongation, and coalescence. At high triaxiality, the correlation between crystal orientation and void growth rate becomes stronger, resembling the behavior observed in isolated single crystals. Therefore, understanding the effects of crystal orientation, heterogeneous strain, and defect evolution is crucial for single crystal fracture characterization. Here, in this work, a coupled phase-field damage (PFD) and crystal plasticity (CP) model is implemented within a finite element framework to analyze crystal deformation and failure. The CP method employs a dislocation density-based constitutive model, while intragranular failure is modeled using an anisotropic PFD method. The PFD model considers both the stored energy due to elastic stretching and the energy release due to defect formation and crack formation. A single crystal Al2219 with an intracrystalline spherical void is chosen to analyze fracture. The study finds that fracture propagation is strongly correlated with crystal orientations. This coupled CP-PFD model provides accurate failure prediction in crystalline materials by incorporating the effects of crystal orientations and existing voids. This study demonstrates how the local microstructure and defects influence plastic deformation and failure mechanisms in metal alloys.

Aluminum alloy↗

Radiative properties of quantum emitters in boron nitride from excited state calculations and Bayesian analysis

Abstract Point defects in hexagonal boron nitride (hBN) have attracted growing attention as bright single-photon emitters. However, understanding of their atomic structure and radiative properties remains incomplete. Here we study the excited states and radiative lifetimes of over 20 native defects and carbon or oxygen impurities in hBN using ab initio density functional theory and GW plus Bethe-Salpeter equation calculations, generating a large data set of their emission energy, polarization and lifetime. We find a wide variability across quantum emitters, with exciton energies ranging from 0.3 to 4 eV and radiative lifetimes from ns to ms for different defect structures. Through a Bayesian statistical analysis, we identify various high-likelihood charge-neutral defect emitters, among which the native V N N B defect is predicted to possess emission energy and radiative lifetime in agreement with experiments. Our work advances the microscopic understanding of hBN single-photon emitters and introduces a computational framework to characterize and identify quantum emitters in 2D materials.

Chemistry↗

The Convolutional Multiple Whole Profile (CMWP) Fitting Method, a Global Optimization Procedure for Microstructure Determination

The analysis of line broadening in X-ray and neutron diffraction patterns using profile functions constructed on the basis of well-established physical principles and TEM observations of lattice defects has proven to be a powerful tool for characterizing microstructures in crystalline materials. These principles are applied in the convolutional multiple-whole-profile (CMWP) procedure to determine dislocation densities, crystallite size, stacking fault and twin boundary densities, and intergranular strains. The different lattice defect contributions to line broadening are separated by considering the hkl dependence of strain anisotropy, planar defect broadening and peak shifts, and the defect dependent profile shapes. The Levenberg–Marquardt (LM) peak fitting procedure can be used successfully to determine crystal defect types and densities as long as the diffraction patterns are relatively simple. However, in more complicated cases like hexagonal materials or multiple-phase patterns, using the LM procedure alone may cause uncertainties. Here, we extended the CMWP procedure by including a Monte Carlo statistical method where the LM and a Monte Carlo algorithm were combined in an alternating manner. The updated CMWP procedure eliminated uncertainties and provided global optimized parameters of the microstructure in good correlation with electron microscopy methods.

36 MATERIALS SCIENCE↗

Excited States of Crystalline Point Defects with Multireference Density Matrix Embedding Theory

Accurate and affordable methods to characterize the electronic structure of solids are important for targeted materials design. Embedding-based methods provide an appealing balance in the trade-off between cost and accuracy-particularly when studying localized phenomena. Here, we use the density matrix embedding theory (DMET) algorithm to study the electronic excitations in solid-state defects with a restricted open-shell Hartree-Fock (ROHF) bath and multireference impurity solvers, specifically, complete active space self-consistent field (CASSCF) and n-electron valence state second-order perturbation theory (NEVPT2). In this work, we apply the method to investigate the electronic excitations in an oxygen vacancy (OV) on a MgO(100) surface and find absolute deviations within 0.05 eV between DMET using the CASSCF/NEVPT2 solver, denoted as CAS-DMET/NEVPT2-DMET, and the nonembedded CASSCF/NEVPT2 approach. Next, we establish the practicality of DMET by extending it to larger supercells for the OV defect and a neutral silicon vacancy in diamond where the use of nonembedded CASSCF/NEVPT2 is extremely expensive.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Complex defect chemistry of hydrothermally-synthesized Nb-substituted β$'$-LiVOPO 4

Lithium vanadyl phosphate (LiVOPO 4 ) is a next-generation multielectron battery cathode that can intercalate up to two Li-ions per V-ion through the redox couples of V 4+ /V 3+ and V 5+ /V 4+ . However, its rate capacity is undermined by the sluggish Li-ion diffusion in the high-voltage region (4 V for V 5+ /V 4+ redox). Nb substitution was used to expand the crystal lattice to facilitate Li-ion diffusion. Here, in this work, Nb substitution was achieved via hydrothermal synthesis, which resulted in a new, lower symmetry β'-LiVOPO 4 phase with preferential Nb occupation of one of the two V sites. This phase presents complex defect chemistries, including cation vacancies and hydrogen interstitials, characterized by a combination of X-ray and neutron diffraction, elemental and thermogravimetric analyses, X-ray absorption spectroscopy, and magnetic susceptibility measurements. The Nb-substituted samples demonstrated improved capacity retention and rate capabilities in the high-voltage region, albeit an enlarged voltage hysteresis related to a partial V 4+ /V 3+ redox reaction, as evidenced by ex situ X-ray absorption spectroscopy and pair distribution function analysis. This work highlights the importance of understanding the complex defect chemistry and its consequence on electrochemistry in polyanionic intercalation compounds.

36 MATERIALS SCIENCE↗

Interface stability of ultrasonic additively manufactured Zircaloy-4 during hydrothermal corrosion

Simulated pressurized water reactor conditions (330 °C, 15.6 MPa, ~20 ppb oxygen) without irradiation were used to investigate the hydrothermal corrosion behavior of ultrasonic additively manufactured Zircaloy-4 up to 1000 h. X-ray computed tomography allowed for visualization of defects from processing and their progression after corrosion experiments. The specimens were found to have clear variability in the mass change data, compared to typical wrought Zircaloy-4 specimens. The variation in the mass change after exposure was attributed to weld defects connected to the specimen surface which allowed ingress of oxidant into the samples. Defects visualized by computed tomography were found via metallography and characterized. In conclusion, ultrasonic additively manufactured Zircaloy-4 was found to have comparable corrosion behavior as wrought Zircaloy-4 for specimens which did not have clear surface defects along weld interfaces.

36 MATERIALS SCIENCE↗

Point and extended defects in heteroepitaxial 𝛽−G⁡a 2 ⁢O 3 films

G⁡a 2 ⁢O 3 is emerging as an excellent potential semiconductor for high power and optoelectronic devices. However, the successful development of G⁡a 2⁢ O 3 in a wide range of applications requires a full understanding of the role and nature of its point and extended defects. Here, in this work, high quality epitaxial G⁡a 2 ⁢O 3 films were grown on sapphire substrates by metal-organic chemical vapor deposition and fully characterized in terms of structural, optical, and electrical properties. Then defects in the films were investigated by a combination of depth-resolved Doppler broadening and lifetime of positron annihilation spectroscopies and thermally stimulated emission (TSE). Positron annihilation techniques can provide information about the nature and concentration of defects in the films, while TSE reveals the energy level of defects in the bandgap. Despite very good structural properties, the films exhibit short positron diffusion length, which is an indication of high defect density and long positron lifetime, a sign for the formation of Ga vacancy related defects and large vacancy clusters. These defects act as deep and shallow traps for charge carriers as revealed from TSE, which explains the reason behind the difficulty of developing conductive G⁡a 2 ⁢O 3 films on non-native substrates. Positron lifetime measurements also show nonuniform distribution of vacancy clusters throughout the film depth. Further, the work investigates the modification of defect nature and properties through thermal treatment in various environments. It demonstrates the sensitivity of G⁡a 2 ⁢O 3 microstructures to the growth and thermal treatment environments and the significant effect of modifying defect structure on the bandgap and optical and electrical properties of G⁡a 2 ⁢O 3 .

defects↗

Light-activated microtubule-based two-dimensional active nematic

We assess the ability of two light responsive kinesin motor clusters to drive dynamics of microtubule-based active nematics: opto-K401, a processive motor, and opto-K365, a non-processive motor. Measurements reveal an order of magnitude improvement in the contrast of nematic flow speeds between maximally- and minimally-illuminated states for opto-K365 motors when compared to opto-K401 construct. For opto-K365 nematics, we characterize both the steady-state flow and defect density as a function of applied light. We also examine the transient behavior as the system switches between steady-states upon changes in light intensities. Although nematic flows reach a steady state within tens of seconds, the defect density exhibits transient behavior for up to 10 minutes, showing a separation between small-scale active flows and system-scale structural states. Furthermore, our work establishes an experimental platform that can exploit spatiotemporally-heterogeneous patterns of activity to generate targeted dynamical states.

42 ENGINEERING↗

Engineering Nanostructured Interfaces of Hexagonal Boron Nitride-Based Materials for Enhanced Catalysis

Hexagonal boron nitrides (h-BNs) are attractive two-dimensional (2D) nanomaterials that consist of alternating B and N atoms and layered honeycomb-like structures similar to graphene. They have exhibited unique properties and promising application potentials in the field of energy storage and transformation. Recent advances in utilizing h-BN as a metal-free catalyst in the oxidative dehydrogenation of propane have triggered broad interests in exploring h-BN in catalysis. However, h-BN-based materials as robust nanocatalysts in heterogeneous catalysis are still underexplored because of the limited methodologies capable of affording h-BN with controllable crystallinity, abundant porosity, high purity, and defect engineering, which played important roles in tuning their catalytic performance. Here, in this account, our recent progress in addressing the above issues will be highlighted, including the synthesis of high-quality h-BN-based nanomaterials via both bottom-up and top-down pathways and their catalytic utilization as metal-free catalysts or as supports to tune the interfacial electronic properties on the metal nanoparticles (NPs). First, we will focus on the large-scale fabrication of h-BN nanosheets (h-BNNSs) with high crystallinity, improved surface area, satisfactory purity, and tunable defects. h-BN derived from the traditional approaches using boron trioxide and urea as the starting materials generally contains carbon/oxygen impurities and has low crystallinity. Several new strategies were developed to address the issues. Using bulk h-BN as the precursor via gas exfoliation in liquid nitrogen, single- or few-layered h-BNNS with abundant defects could be generated. Amorphous h-BN precursors could be converted to h-BN nanosheets with high crystallinity assisted by a magnesium metallic flux via a successive dissolution/precipitation/crystallization procedure. The as-fabricated h-BNNS featured high crystallinity and purity as well as abundant porosity. An ionothermal metathesis procedure was developed using inorganic molten salts (NaNH 2 and NaBH 4 ) as the precursors. The h-BN scaffolds could be produced on a large scale with high yield, and the as-afforded materials possessed high purity and crystallinity. Second, utilization of the as-prepared h-BN library as metal-free catalysts in dehydrogenation and hydrogenation reactions will be summarized, in which they exhibited enhanced catalytic activity over the counterparts from the previous synthesis method. Third, the interface modulation between metal NPs with the as-prepared defects’ abundant h-BN support will be highlighted. The h-BN-based strong metal–support interaction (SMSI) nanocatalysts were constructed without involving reducible metal oxides via the ionothermal procedure we developed by deploying specific inorganic metal salts, acting as robust nanocatalysts in CO oxidation. Under conditions simulated for practical exhaust systems, promising catalytic efficiency together with high thermal stability and sintering resistance was achieved. Across all of these examples, unique insights into structures, defects, and interfaces that emerge from in-depth characterization through microscopy, spectroscopy, and diffraction will be highlighted.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

3D‐Mapping and Manipulation of Photocurrent in an Optoelectronic Diamond Device

Abstract Establishing connections between material impurities and charge transport properties in emerging electronic and quantum materials, such as wide‐bandgap semiconductors, demands new diagnostic methods tailored to these unique systems. Many such materials host optically‐active defect centers which offer a powerful in situ characterization system, but one that typically relies on the weak spin‐electric field coupling to measure electronic phenomena. In this work, charge‐state sensitive optical microscopy is combined with photoelectric detection of an array of nitrogen‐vacancy (NV) centers to directly image the flow of charge carriers inside a diamond optoelectronic device, in 3D and with temporal resolution. Optical control is used to change the charge state of background impurities inside the diamond on‐demand, resulting in drastically different current flow such as filamentary channels nucleating from specific, defective regions of the device. Conducting channels that control carrier flow, key steps toward optically reconfigurable, wide‐bandgap optoelectronics are then engineered using light. This work might be extended to probe other wide‐bandgap semiconductors (SiC, GaN) relevant to present and emerging electronic and quantum technologies.

Wood, Alexander A.↗

Thermal conductivity measurement of U-Mo and U-Mo/Al interaction layers generated from in-pile irradiation using the suspended-bridge method

Here, this study presents the first measurement of the individual thermal conductivity of U-7wt.%Mo fuel particles and U-Mo/Al interaction layers (ILs) from in-pile irradiated dispersion fuel plates, using the suspended-bridge method. Nanorods of U-7wt.%Mo fuel and U-Mo/Al ILs were extracted by focused ion beam (FIB), and their microstructures were characterized with transmission electron microscopy (TEM). TEM revealed finely distributed nanobubbles in the U-7wt.%Mo matrix, along with an amorphous structure in the ILs. The thermal conductivity of in-pile irradiated U-7wt.%Mo was approximately 30% lower than that of the unirradiated material, ranging from 6.7 W/m·K at 300 K to 8.5 W/m·K at 380 K. The ILs exhibited even lower thermal conductivity, from 2.1 W/m·K at 300 K to 2.7 W/m·K at 380 K. These reductions, attributed to nanobubbles, fission products, and irradiation-induced point defects, were analyzed through a combination of microstructural characterization and literature-based transport models, which successfully reproduced the observed degradation trends.

42 - ENGINEERING↗

New perspectives on materials and device dynamics using time-resolved full-field diffraction X-ray imaging

Understanding how materials evolve during synthesis, processing, or device operation requires experimental access to structural dynamics across wide ranges of length and time scales, often in bulk samples or even within packaged devices. Time-resolved full-field diffraction X-ray microscopy has recently emerged as a powerful way to meet this need by combining the penetration and structural sensitivity of X-ray diffraction with objective-lens-based magnification, sensitive high-resolution X-ray imaging detectors, and pump-probe and real-time imaging strategies. Advances in full-field X-ray diffraction microscopy, often termed dark-field X-ray microscopy (DFXM), enable simultaneous imaging of extended fields of view while retaining crystallographic selectivity. Time-resolved DFXM promises to enable advances in materials processing and dynamics, electrochemical and photochemical processes, and the design of electronic devices. This Perspective summarizes the key instrumental concepts that define the performance of these methods, including the choice of imaging optics, detector considerations, and the impact of source time structure at synchrotron light sources and X-ray free-electron lasers (XFELs). We discuss the simultaneous use of complementary imaging modes that are increasingly used in practice. The early demonstrations of the potential of time-resolved DFXM include real-time defect and grain-boundary dynamics during metal annealing, stroboscopic imaging of functional devices with high strain sensitivity, and ultrafast pump-probe implementations at XFELs that directly visualize acoustic-wave propagation and energy dissipation in bulk crystals.

Dark-field X-ray microscopy↗

Oxygen Defect Configurations in Single-Phase UO 2.15

Hyperstoichiometric UO 2.15 was characterized by neutron total scattering at high temperature in the single-phase UO 2+x region of the U/O phase diagram. The diffraction data confirmed a single-phase fluorite structure at high temperature. Analysis of the short-range data showed that the same structural model does not fit the pair distribution functions well. Instead, structural models containing specific configurations of oxygen defect clusters best represent the local atomic arrangement. In conclusion, prevalent defect clusters previously proposed were fit to the experimental data, and moderately distorted oxygen cuboctahedra hypothesized by recent molecular dynamics simulations fit the data most accurately.

neutron pair-distribution function analysis↗

L-PBF High-Throughput Data Pipeline Approach for Multi-modal Integration

Abstract Metal-based additive manufacturing requires active monitoring solutions for assessing part quality. Multiple sensors and data streams, however, generate large heterogeneous data sets that are impractical for manual assessment and characterization. In this work, an automated pipeline is developed that enables feature extraction from high-speed camera video and multi-modal data analysis. The framework removes the need for manual assessment through the utilization of deep learning techniques and training models in a weakly supervised paradigm. We demonstrate this pipeline’s capability over 700,000 high-speed camera frames. The pipeline successfully extracts melt pool and spatter geometries and links them to corresponding pyrometry, radiography, and processparameter information. 715 individual prints are examined to reveal melt pool areas that exceeds 0.07 mm 2 and pyrometry signal over a threshold (375 pyrometry units) were more likely to have defects. These automated processes enable massive throughput of characterization techniques.

36 MATERIALS SCIENCE↗

Crystallographic and TEM Features of a TBC/Ti2AlC MAX Phase Interface after 1300°C Burner Rig Oxidation

A FIB/STEM interfacial study was performed on a TBC/Ti 2 AlC MAX phase system, oxidized in an aggressive burner rig test (Mach 0.3 at 1300 °C for 500 h). The 7YSZ TBC, α-Al 2 O 3 TGO, and MAXthal 211 TM Ti 2 AlC base were variously characterized by TEM/STEM, EDS, SADP, and HRTEM. The YSZ was a mix of “clean” featureless and “faulted” high contrast grains. The latter exhibited ferro-elastic domains of high Y content tetragonal t″ variants. No martensite was observed. The TGO was essentially a duplex α-Al 2 O 3 structure of inner columnar plus outer equiaxed grains. It maintained a perfectly intact, clean interface with the Ti 2 AlC substrate. The Ti 2 AlC substrate exhibited no interfacial Al-depletion zone but, rather, numerous faults along the basal plane of the hexagonal structure. These are believed to offer a means of depleting Al by forming crystallographic, low-Al planar defects, proposed as Ti 2.5 AlC 1.5 . These characterizations support and augment prior optical, SEM, and XRD findings that demonstrated remarkable durability for the YSZ/Ti 2 AlC MAX phase system in aggressive burner tests.

TI2AlC↗

Quantifying the dislocation content of atomically resolved grain boundary line defects using the Nye tensor

The Nye tensor, which quantifies the density of Burgers vector for a given dislocation line direction, can be effectively used to characterize dislocation content in bulk crystals from atomic-resolution transmission electron microscopy images. The Nye tensor can be calculated from these images, in part because the reference state is simply defined by the lattice of the perfect crystal. The application of the Nye tensor to interfacial line defects, for which the natural reference state is the dichromatic pattern of the two grains in their reference orientation, poses additional challenges. In this work, we present a method that employs the Nye tensor to characterize the edge dislocation content of line defects at grain boundaries from atomic-resolution images. This approach enables us to rapidly characterize all edge dislocation content along a grain boundary. Additionally, the Nye tensor provides information about line defect core structure. Finally, we demonstrate this method on two exemplar defects: a twin boundary disconnection and a facet junction in face-centered cubic Au.

Crystallographic defects↗