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Results for “defect microscopy”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 271 records · Page 15
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Impact of Low-Temperature Neutron Irradiation on Tensile Behavior of Base Metal and Electron-Beam Welded 316L Stainless Steel

Here, a study of 316L type stainless steel in its base metal and electron-beam (e-beam) welded conditions was performed to observe the effects of low-temperature (60 °C to 100 °C) neutron irradiation on the tensile behavior of the samples. Fractography was used in understanding the tensile-tested fracture surfaces of the 316L samples in these different forms with the characterization of the both base metal and welded samples using electron microscopy. Irradiation of the tensile specimens made free of defects of cutting and mechanical polishing showed a reduction in their tensile ductility with increased radiation-induced hardening up to 1.40 × 10 19 n/cm 2 (E > 0.1 MeV) fluence that corresponds to 1.1x 10 -2 dpa, even at the low irradiation temperatures. These low-temperature neutron irradiated base metal and e-beam welded 316L specimens also consisted of closely similar fracture surfaces characteristic of ductile rupture.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Irradiation damage reduces alloy corrosion rate via oxide space charge compensation effects

Radiation effects in materials often compound and accelerate other detrimental phenomena such as embrittlement, oxidation and creep. However, irradiation can also decrease the oxidation rate, for instance with ZrNb alloys nuclear fuel cladding. In this study, we rationalize this observation on Zr-0.5Nb alloy by introducing a mechanism based on oxide space charge modification, resulting from irradiation enhanced Nb clustering. Here, this mechanism is investigated using a multiscale approach: from the macroscale, to determine post-irradiation oxidation kinetics, to the atomic scale, using in-situ atom probe tomography sample oxidation, to observe elemental solute redistribution across the oxide/metal interface. The mechanism is further supported by high resolution transmission electron microscopy characterization and density functional theory calculations. A point defect model is proposed to account for oxide space charge effects and their changes under irradiation. This integrated, multiscale experimental and modeling approach challenges the current paradigm on irradiation effects and how they can potentially improve materials performance in extreme environments.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Vertically Aligned Single-Crystalline CoFe 2 O 4 Nanobrush Architectures with High Magnetization and Tailored Magnetic Anisotropy

Micrometer-tall vertically aligned single-crystalline CoFe 2 O 4 nanobrush architectures with extraordinarily large aspect ratio have been achieved by the precise control of a kinetic and thermodynamic non-equilibrium pulsed laser epitaxy process. Direct observations by scanning transmission electron microscopy reveal that the nanobrush crystal is mostly defect-free by nature, and epitaxially connected to the substrate through a continuous 2D interface layer. In contrast, periodic dislocations and lattice defects such as anti-phase boundaries and twin boundaries are frequently observed in the 2D interface layer, suggesting that interface misfit strain relaxation under a non-equilibrium growth condition plays a critical role in the self-assembly of such artificial architectures. Further, magnetic property measurements have found that the nanobrushes exhibit a saturation magnetization value of 6.16 μB/f.u., which is much higher than the bulk value. The discovery not only enables insights into an effective route for fabricating unconventional high-quality nanostructures, but also demonstrates a novel magnetic architecture with potential applications in nanomagnetic devices.

36 MATERIALS SCIENCE↗
NASA NTRS1978

Scanning microscopy in microcircuit failure analysis

A three-phase microcircuit failure analysis procedure is presented. In the first phase, the device is nondestructively tested and the data obtained is correlated with the circumstances surrounding the failure event. The device is then subjected to a limited nondestructive analysis dominated by optical and scanning electron microscopy (SEM). Knowing that microcircuits usually fail from manufacturing defects or misuse, the analyst looks for one of the probable mechanisms. The SEM has two special operating modes that provide unique data for nondestructive analysis: voltage contrast and conductive current. These are used with other SEM modes and surface analysis techniques to analyze complicated microcircuits. The last phase includes the destructive procedures. The end product of these analyses is a corrective action that will yield a highly reliable system.

Nicolas, D. P.↗
NASA NTRS1986

Nondestructive Evaluation (NDE) of structural ceramics by photoacoustic microscopy

Photoacoustic microscopy (PAM) was utilized to detect surface and subsurface defects in structural ceramic materials. A computerized PAM data acquisition, color imaging and analysis system was developed and used. Subsurface simulated cylindrical holes can be detected to about 1 mm below the interrograting surface. Simulated tight surface cracks of 96 microns length and 48 microns depth can be detected in these materials under optimum conditions.

Khandelwal, P. K.↗
DOE OSTI2021

The dynamic evolution of swelling in nickel concentrated solid solution alloys through in situ property monitoring

Defects and microstructural features spanning the atomic level to the microscale play deterministic roles in the expressed properties of materials. Yet studies of material evolution in response to environmental stimuli most often correlate resulting performance with one dominant microstructural feature only. In this work, the dynamic evolution of swelling in a series of Ni-based concentrated solid solution alloys under high-temperature irradiation exposure is observed using continuous, in situ measurements of thermoelastic properties in bulk specimens. Unlike traditional evaluation techniques which account only for volumetric porosity identified using electron microscopy, direct property evaluation provides an integrated response across all defect length scales. In particular, the evolution in elastic properties during swelling is found to depend significantly on the entire size spectrum of defects, from the nano- to meso-scales, some of which are not resolvable in imaging. Observed changes in thermal transport properties depend sensitively on the partitioning of electronic and lattice thermal conductivity. This emerging class of in situ experiments, which directly measure integrated performance in relevant conditions, provides unique insight into material dynamics otherwise unavailable using traditional methods.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Enhanced Water Interaction at Dual Cu Sites Within the Defects on a Copper Sulfide Layer

Electrochemical transformations of stable molecules and water into fuels and value-added chemicals require efficient catalyst surfaces. Introducing controlled defects at atomic scales can offer promising routes to enhance catalyst performance. In this study, we found novel dual copper site (-Cu-Cu-) defects within a copper sulfide (Cu-S) layer supported on Cu(111). Using scanning tunneling microscopy (STM) and density functional theory (DFT), we found these dual copper sites enhance molecular adsorption strength, specifically for water molecules, compared to intact Cu-S layer or pristine copper surfaces. This discovery highlights the potential of engineered dual-site copper defects to advance electrochemical catalytic materials, particularly for reactions involving water activation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Optical activation and detection of charge transport between individual colour centres in diamond

Understanding the capture of charge carriers by colour centres in semiconductors is important for the development of novel forms of sensing and quantum information processing, but experiments typically involve ensemble measurements, often impacted by defect proximity. In this study, we show that confocal fluorescence microscopy and magnetic resonance can be used to induce and probe charge transport between individual nitrogen-vacancy centres in diamond at room temperature. In our experiments, a ‘source’ nitrogen vacancy undergoes optically driven cycles of ionization and recombination to produce a stream of photogenerated carriers, one of which is subsequently captured by a ‘target’ nitrogen vacancy several micrometres away. We use a spin-to-charge conversion scheme to encode the spin state of the source colour centre into the charge state of the target, which allows us to set an upper bound to carrier injection from other background defects. We attribute our observations to the action of unscreened Coulomb potentials producing giant carrier capture cross-sections, orders of magnitude greater than those measured in ensembles.

36 MATERIALS SCIENCE↗
DOE OSTI2021

An antisite defect mechanism for room temperature ferroelectricity in orthoferrites

Single-phase multiferroic materials that allow the coexistence of ferroelectric and magnetic ordering above room temperature are highly desirable, motivating an ongoing search for mechanisms for unconventional ferroelectricity in magnetic oxides. Here, we report an antisite defect mechanism for room temperature ferroelectricity in epitaxial thin films of yttrium orthoferrite, YFeO 3 , a perovskite-structured canted antiferromagnet. A combination of piezoresponse force microscopy, atomically resolved elemental mapping with aberration corrected scanning transmission electron microscopy and density functional theory calculations reveals that the presence of Y Fe antisite defects facilitates a non-centrosymmetric distortion promoting ferroelectricity. This mechanism is predicted to work analogously for other rare earth orthoferrites, with a dependence of the polarization on the radius of the rare earth cation. Our work uncovers the distinctive role of antisite defects in providing a mechanism for ferroelectricity in a range of magnetic orthoferrites and further augments the functionality of this family of complex oxides for multiferroic applications.

36 MATERIALS SCIENCE↗
NASA NTRS1981

EBIC/TEM investigations of process-induced defects in EFG silicon ribbon

Electron bombardment induced conductivity and scanning transmission electron microscopy observations on unprocessed and processed edge-defined film-fed growth ribbon show that the phosphorus diffused junction depth is not uniform, and that a variety of chemical impurities precipitate out during processing. Two kinds of precipitates are found (1) 10 nm or less in size, located at the dislocation nodes in sub-boundary like dislocation arrangements formed during processing and (2) large precipitates, the chemical composition of which has been partially identified. These large precipitates emit dense dislocations tangles into the adjacent crystal volume.

Cunningham, B.↗
DOE OSTI2024

Evolution of extended defects in UO 2 during high temperature annealing

The evolution of thermophysical characteristics of uranium oxide (UO 2 ) under irradiation is a critical aspect of nuclear fuel performance of light water reactors. This study examines the effect of high-temperature annealing at 1000 °C - 1600 °C on defect evolution in krypton irradiated UO 2 at room temperature. Transmission electron microscopy analysis reveals that the size of irradiation-induced bubbles and dislocation loops increases but their density decreases with annealing temperatures. Perfect dislocation loops with = <110> dominate, regardless of the annealing temperature. A rate theory model for extended defect evolution is applied to conclude that current understanding of dynamical loop and bubble evolution at high-temperature annealing is governed by defect coalescence.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

Influence of structural defects on charge density waves in 1T-TaS2

Abstract The influence of intrinsic defects of 1T-TaS 2 on charge density waves (CDWs) is studied using scanning tunneling microscopy and spectroscopy (STM, STS), angle-resolved photoelectron spectroscopy (ARPES), and density functional theory (DFT). We identify several types of structural defects and find that most have a local character limited to a single CDW site, with a single exception which effectively behaves as a dopant, leading to band-bending and affecting multiple neighboring sites. While only one type of defect can be observed by STM topographic imaging, all defects are easily resolved in STS mapping. Our results indicate modulation of the Mott band gap commensurate with the CDW and breaking of the three-fold symmetry of electronic states. DFT calculations (with included Coulomb interactions) are used to investigate the electronic structure, focusing on both sulfur vacancy and oxygen-sulfur substitution. The sulfur vacancy system, characterized with a metallic behavior, is identified as the origin of one of the experimentally observed defects. Additionally, the effect of oxidation of 1T-TaS 2 depends on the substitution site, leading to the heterogeneity of electronic properties.

Chemistry↗
DOE OSTI2020

Dynamic Manipulation in Piezoresponse Force Microscopy: Creating Nonequilibrium Phases with Large Electromechanical Response

We discuss how domain walls and topological defects in ferroelectric materials have emerged as a powerful tool for functional electronic devices including memory and logic. Similarly, wall interactions and dynamics underpin a broad range of mesoscale phenomena ranging from giant electromechanical responses to memory effects. Exploring the functionalities of individual domain walls, their interactions, and controlled modifications of the domain structures is crucial for applications and fundamental physical studies. However, the dynamic nature of these features severely limits studies of their local physics since application of local biases or pressures in piezoresponse force microscopy induce wall displacement as a primary response. Here, we introduce an approach for the control and modification of domain structures based on automated experimentation, whereby real-space image-based feedback is used to control the tip bias during ferroelectric switching, allowing for modification routes conditioned on domain states under the tip. This automated experiment approach is demonstrated for the exploration of domain wall dynamics and creation of metastable phases with large electromechanical response.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Embedding of Fiber Optic Sensors in Stainless Steel for Sensing in Harsh Environments

Structural health monitoring is critical for components working in harsh environments to assess their safety and integrity. This can be realized with advanced sensors, such as fiber optic sensors, embedded in these components. Recent studies have used ultrasonic consolidation (UC) and laser-based additive manufacturing (AM) techniques to embed fiber optic sensors in metals. However, sensor embedding using these techniques has been challenging, with gaps and voids around the embedded fiber. Successful embedding of fiber optic sensors requires good contact between the fiber and the matrix to eliminate potential gas/liquid leaks in critical systems such as in nuclear and aerospace services. Defect-free fiber/matrix bond is also essential for accurate measurement of parameters of interest, such as temperature and strain. This study developed a novel fiber embedding technique based on electric field-assisted sintering (EFAS). Sapphire optical fibers with diameters of 125 µm and 250 µm were embedded in stainless steel (SS) 316L using EFAS. The embedding was completed by sintering SS 316L powders at a pressure of 50MPa, hold time of 5 min, and temperatures of 1000°C, 1100°C, and 1200°C. Joule heating mechanism during EFAS enabled rapid sintering of the SS 316L powder with resulting sample densities over 99%. Microscopy analysis performed on the cross-sections revealed a defect-free bond between the embedded fiber and SS 316L. The good integrity of the embedded fiber was evidenced by optical transmittance measurement. Optical attenuation of the fiber before and after embedment was examined in the near-infrared region. Scanning electron microscopy was employed to investigate the grain morphology of SS 316L near the embedded fiber. Hardness distribution in the sintered part was also investigated to study the effect of the embedded fiber on the mechanical properties of the as-fabricated component. The results indicated that EFAS was able to embed fiber in SS with good fiber functionality and part quality.

36 - MATERIALS SCIENCE↗
DOE OSTI2021

Scanning ultrafast electron microscopy reveals photovoltage dynamics at a deeply buried $p^- \mathrm{Si/SiO_2}$ interface

The understanding and control of charge carrier interactions with defects at buried insulator/semiconductor interfaces is essential for achieving optimum performance in modern electronics. In this work, we report on the use of scanning ultrafast electron microscopy (SUEM) to remotely probe the dynamics of excited carriers at a Si surface buried below a thick thermal oxide. Our measurements illustrate a previously unidentified SUEM contrast mechanism, whereby optical modulation of the space-charge field in the semiconductor modulates the electric field in the thick oxide, thus affecting its secondary electron yield. By analyzing the SUEM contrast as a function of time and laser fluence we demonstrate the diffusion mediated capture of excited carriers by interfacial traps.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Metallic line defect in wide-bandgap transparent perovskite BaSnO 3

A line defect with metallic characteristics has been found in optically transparent BaSnO 3 perovskite thin films. The distinct atomic structure of the defect core, composed of Sn and O atoms, was visualized by atomic-resolution scanning transmission electron microscopy (STEM). When doped with La, dopants that replace Ba atoms preferentially segregate to specific crystallographic sites adjacent to the line defect. The electronic structure of the line defect probed in STEM with electron energy-loss spectroscopy was supported by ab initio theory, which indicates the presence of Fermi level–crossing electronic bands that originate from defect core atoms. These metallic line defects also act as electron sinks attracting additional negative charges in these wide-bandgap BaSnO 3 films.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Detection of defects in atomic-resolution images of materials using cycle analysis

The automated detection of defects in high-angle annular dark-field Z-contrast (HAADF) scanning-transmission-electron microscopy (STEM) images has been a major challenge. Here, we report an approach for the automated detection and categorization of structural defects based on changes in the material’s local atomic geometry. The approach applies geometric graph theory to the already-found positions of atomic-column centers and is capable of detecting and categorizing any defect in thin diperiodic structures (i.e., “2D materials”) and a large subset of defects in thick diperiodic structures (i.e., 3D or bulk-like materials). Despite the somewhat limited applicability of the approach in detecting and categorizing defects in thicker bulk-like materials, it provides potentially informative insights into the presence of defects. The categorization of defects can be used to screen large quantities of data and to provide statistical data about the distribution of defects within a material. This methodology is applicable to atomic column locations extracted from any type of high-resolution image, but here we demonstrate it for HAADF STEM images.

36 MATERIALS SCIENCE↗