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Results for “in situ TEM”

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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

In situ TEM observation of calcium silicate hydrate nanostructure at high temperatures

Fire poses a substantial threat to concrete structures because calcium silicate hydrate (C-S-H) is not thermally stable at high temperatures. Herein, in situ TEM at temperatures from 20 to 800 °C was conducted to study the thermal-induced structural changes in C-S-H. We captured C-S-H shrinks at an average rate of 0.02 μm{sup 2}/{sup o}C upon heating with three stages observed, including induction, constant, and rapid periods. Our observation revealed that an 800 nm pore could be healed during pore structure evolution owing to the reconstruction and deformation among C-S-H blocks. The Ca/Si ratio was dropped at higher temperatures because of the leakage of calcium ions from the C-S-H structure to form CaO precipitates. The temperature-driven phase transformation and degradation were also detected using electron diffraction that C-S-H was transformed into metastable calcium silicate minerals above 800 °C. This work provides insights into the nanoscale transformation of C-S-H at high temperatures.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography

In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample 6 exposed to molten KCl-MgCl 2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl 2 . Here, both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and 10 deeper understanding beyond conventional analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Shape-preserving amorphous-to-crystalline transformation of CaCO3 revealed by in situ TEM

Organisms use inorganic ions and macromolecules to regulate crystallization from amorphous- precursors, endowing natural biominerals with complex morphologies and enhanced properties. The mechanisms by which modifiers enable these shape preserving transformations are poorly understood. We used in situ liquid-phase transmission electron microscopy to follow the evolution from amorphous calcium carbonate to calcite in the presence of additives. A combination of contrast analysis and infrared spectroscopy shows that Mg ions, which are widely present in seawater and biological fluids, alter the transformation pathway in a concentration-dependent manner. The ions bring excess (structural) water into the amorphous bulk so that a direct transformation is triggered by dehydration in the absence of morphological changes. Molecular dynamics simulations suggest Mg-incorporated water induces structural fluctuations, allowing transformation without the need to nucleate a separate crystal. Thus, the obtained calcite retains the original morphology of the amorphous state, biomimetically achieving the morphological control of crystals seen in biominerals

crystallization, biomineralization, calcium carbon↗
DOE OSTI2023

In-situ TEM investigation of void swelling in nickel under irradiation with analysis aided by computer vision

Understanding the stability of irradiation-induced voids in materials is important for engineering material's swelling behavior under irradiation. In-situ TEM offers a spatial and temporal resolution that is suitable for investigating the evolution of voids under irradiation. However, the in-situ videos have often been too large to be analyzed manually, leaving the valuable data underutilized. For this work, we developed a deep learning-based semantic segmentation model to consistently study the growth and shrinkage of voids in nickel under 1 MeV krypton ion irradiation at various temperatures from 525 °C to 650 °C. With a foil thickness near 100 nm and ion flux of 6.3 × 10 11 ions∙ cm –2 ∙s –1 , the pre-existing voids, which were created beforehand by irradiation at 600 °C to 0.5 dpa, shrank at low temperatures and grew at high temperatures under irradiation, where the transition occurred at 575 °C (~0.5 T M ). The observed stability transition provided new insight for the shrinkage mechanism of voids under irradiation. In addition, an annealing experiment on nickel, previously irradiated at 600 °C to 3 dpa, was performed sequentially at 650 °C to 720 °C to reveal the shrinkage rate of void as a function of temperature and void size. The advantage of combining computer vision and in-situ TEM to obtain comprehensive void evolution was demonstrated.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Understanding and quantifying electron beam effects during in situ TEM nanomechanical tensile testing on metal thin films

Transmission electron microscopy (TEM) imaging relies on high energy electrons for atomic scale resolution, however, the electrons themselves interact with and may alter the material being imaged. Using an in situ TEM MEMS-based nanomechanical testing technique, the effect of the electron beam (e-beam) on the deformation behavior of nanocrystalline Al and ultrafine-grained Au is investigated and quantified. We show that the e-beam enhances plastic deformation, leading to an increase in plastic strain rate and a decrease in true activation volume V* in Al (28 to 21b 3 , with b being the Burgers vector length). The e-beam has a much weaker effect on Au. The e-beam effect is not caused by knock-on damage, but rather an effective temperature increase due to additional atomic fluctuations provided by the e-beam. The effective temperature increase is larger for Al than Au. This e-beam effect does not change the deformation mechanisms, but instead accelerates the stress-driven, thermally activated plastic deformation. These experiments provide insight into the effects of the e-beam on plastic deformation in different metals and underscore the importance of understanding and quantifying these effects for proper interpretation of measured mechanical properties during in situ TEM experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2022

DefectTrack: a deep learning-based multi-object tracking algorithm for quantitative defect analysis of in-situ TEM videos in real-time

Abstract In-situ irradiation transmission electron microscopy (TEM) offers unique insights into the millisecond-timescale post-cascade process, such as the lifetime and thermal stability of defect clusters, vital to the mechanistic understanding of irradiation damage in nuclear materials. Converting in-situ irradiation TEM video data into meaningful information on defect cluster dynamic properties (e.g., lifetime) has become the major technical bottleneck. Here, we present a solution called the DefectTrack , the first dedicated deep learning-based one-shot multi-object tracking (MOT) model capable of tracking cascade-induced defect clusters in in-situ TEM videos in real-time. DefectTrack has achieved a Multi-Object Tracking Accuracy (MOTA) of 66.43% and a Mostly Tracked (MT) of 67.81% on the test set, which are comparable to state-of-the-art MOT algorithms. We discuss the MOT framework, model selection, training, and evaluation strategies for in-situ TEM applications. Further, we compare the DefectTrack with four human experts in quantifying defect cluster lifetime distributions using statistical tests and discuss the relationship between the material science domain metrics and MOT metrics. Our statistical evaluations on the defect lifetime distribution suggest that the DefectTrack outperforms human experts in accuracy and speed.

42 ENGINEERING↗
NASA NTRS1984

Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

Source record↗
DOE OSTI2021

In-situ TEM observation of shear induced microstructure evolution in Cu-Nb alloy

Phase boundaries in multiphase alloys govern defect interaction and chemical intermixing across different phases during plastic deformation. Dynamic interaction of defects with phase boundaries in multiphase alloys, especially for immiscible alloys, has been topic of significant research interest in recent years. In this work, we describe a novel approach for carrying out in-situ TEM shear deformation to directly observe interfacial microstructural evolution of a Cu-Nb alloy. A unique double shear specimen geometry is microfabricated by a focused ion beam technique to apply shear deformation upon push loading inside the TEM. From the real-time observation, we discover that the phase boundary with a zigzag morphology effectively blocks stacking faults nucleated in a Cu grain from slipping into a Nb grain. Meanwhile, the Cu phase bears the most plastic deformation through slip or twinning mechanisms. This work sheds light on understanding the shear deformation and the behavior of phase boundaries in multiphase alloys during shear deformation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Evolution of dislocation loops and voids in post-irradiation annealed ThO 2 : A combined in-situ TEM and cluster dynamics investigation

The effect of isochronal annealing on the evolution of dislocation loop and void population in proton irradiated ThO 2 has been investigated. Post-irradiation annealing in other actinide oxides like UO 2 shows significant loop coarsening. ThO 2 samples were irradiated with 2 MeV protons up to a dose of 0.1 dpa at 600°C. Post-irradiation isochronal annealing was performed at 600, 800, 1000 and 1100°C for 1 h at each temperature using in-situ TEM. Only faulted 1/3<111> type dislocation loops were observed, and their sizes and distribution were characterized. Further, the population of self-interstitial atom (SIA) dislocation loops did not show any significant growth and coarsening. Additionally, nanometric voids were observed at annealing temperatures of 1000 and 1100°C. Using cluster dynamics (CD), we have studied the nucleation and growth of point defects and defect clusters, i.e., SIA prismatic dislocation loops and nanometric and sub-nanometric voids in proton irradiated ThO 2 . The CD model was further utilized to predict the growth and coarsening of loops and voids during isochronal annealing at the experimental and higher temperatures. The model did not predict significant SIA loop growth which closely corresponds to the TEM observations. CD predicted SIA loop coarsening is insignificant even at high annealing temperature of 1500°C because the model only considers the growth of defect clusters by absorption of like point defects, i.e., SIA loops absorb interstitials and voids absorb vacancies, and cannot account for their migration and coalescence due to elastic interaction. The CD model also predicts the evolution of nanometric voids having mean size within the error bounds of TEM observations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

In-situ TEM study of Kr ion irradiation tolerance of SiFeOC nanocomposite

Here, in this work, ion irradiation of polymer derived SiFeOC nanocomposite was carried out using 1.2 MeV Kr ions at room temperature and 600°C. The starting composite was composed of Fe 3 Si, SiC, SiOC, SiO 2 , and graphitic C. In-situ TEM investigations show uniform distribution of nano-crystalline Fe 3 Si and SiC phases in the amorphous SiOC matrix. During ion irradiation, the SiOC bulk microstructure and interfaces between Fe 3 Si or SiC crystallites and the SiOC matrix remain defect-free and demonstrate outstanding ion irradiation resistance. At room temperature, the crystalline domains are stable up to 2 dpa. At 600°C, Fe 3 Si crystallites are more stable than SiC; SiC crystallites are stable up to 4 dpa while the Fe 3 Si crystallites are stable up to 10 dpa. These crystallites also coalescence and amorphize simultaneously during ion irradiation. The exceptional tolerance to defect formation and irradiation of the SiFeOC nanocomposite provides important guidance to developing irradiation resistant fuels for advanced gas cooled reactors.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In Situ TEM Tensile Testing of Bicrystals with Tailored Misorientation Angles

Grain boundaries have complex structural features that influence strength, ductility and fracture in metals and alloys. Grain boundary misorientation angle has been identified as a key parameter that controls their mechanical behavior, but the effect of misorientation angle has been challenging to isolate in polycrystalline materials. Here, we describe the use of bicrystal Au thin films made using a rapid melt growth process to study deformation at a single grain boundary. Tensile testing is performed on bicrystals with different misorientation angles using in situ TEM, as well as on a single crystalline sample. Plastic deformation is initiated through dislocation nucleation from free surfaces. Grain boundary sliding is not observed, and failure occurs away from the grain boundary through plastic collapse in all cases. The failure behavior in these nanoscale bicrystals does not appear to depend on the misorientation angle or grain boundary energy but instead has a more complex dependence on sample surface structure and dislocation activity.

36 MATERIALS SCIENCE↗
DOE OSTI2024

In-situ TEM EELS analysis of memristive thin films for neuromorphic computing

Neuromorphic computing stands as a promising frontier for advancing AI algorithms and applications like ChatGBT, offering significant energy efficiency gains. This paper delves into the hardware design intricacies of memristive thin films and their elementary switching mechanisms, including anion migration, electron migration, and phase transitions. Through comprehensive analysis of electron energy loss spectroscopy (EELS) data via in-situ transmission electron microscopy (TEM), we will deduce the primary memristive switching mechanisms vital for optimizing thin film fabrication parameters and achieving desired film thickness, conductivity, and memory retention. A single crystal ptype Si substrate was used with TiN as the bottom metal electrode, TiO x as the insulating dielectric layer, and Pt as the top metal electrode. In-situ TEM was able to tell us the thin film didn’t behave like a filamentary or phase transition material. EELS data deduced that electron trapping/detrapping was one of the primary switching mechanisms. By shedding light on these elementary mechanisms, our study aims to catalyze the development of more 2 efficient and effective neuromorphic computing systems to be deployed into mainstream technologies.

97 MATHEMATICS AND COMPUTING↗
DOE OSTI2024

Real-Time Observation of Nanoscale Kink Band Mediated Plasticity in Ion-Irradiated Graphite: An In Situ TEM Study

Graphite IG-110 is a synthetic polycrystalline material used as a neutron moderator in reactors. Graphite is inherently brittle and is known to exhibit a further increase in brittleness due to radiation damage at room temperature. To understand the irradiation effects on pre-existing defects and their overall influence on external load, micropillar compression tests were performed using in situ nanoindentation in the Transmission Electron Microscopy (TEM) for both pristine and ion-irradiated samples. While pristine specimens showed brittle and subsequent catastrophic failure, the 2.8 MeV Au2+ ion (fluence of 4.378 × 1014 cm−2) irradiated specimens sustained extensive plasticity at room temperature without failure. In situ TEM characterization showed nucleation of nanoscale kink band structures at numerous sites, where the localized plasticity appeared to close the defects and cracks while allowing large average strain. We propose that compressive mechanical stress due to dimensional change during ion irradiation transforms buckled basal layers in graphite into kink bands. The externally applied load during the micropillar tests proliferates the nucleation and motion of kink bands to accommodate the large plastic strain. The inherent non-uniformity of graphite microstructure promotes such strain localization, making kink bands the predominant mechanism behind unprecedented toughness in an otherwise brittle material.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Cross-slip and easy-glide CRSS in titanium: Theoretical predictions and in-situ TEM measurements

This study investigates the mechanics of prismatic and first-order pyramidal $\langle$a$\rangle$ slip in titanium (Ti), elucidating the physics of easy-glide and cross-slip through a combination of theory and experiments. Screw-character prismatic (Pr) dislocations in Ti are of particular interest because their complex cores can be stable or unstable, leading to activation by either cross-slip or planar glide. To investigate these mechanisms, site-specific micro tensile samples were prepared using focused ion beam (FIB) milling and mounted on a push-to-pull (PTP) device for in-situ transmission electron microscopy (TEM) tensile testing. The in-situ experiments provide direct observations of the onset of dislocation motion and the precise determination of the critical resolved shear stress (CRSS) for the activated mechanisms, and its evolution with load cycling. A comprehensive theory has been developed to predict the CRSS values for easy glide, cross-slip, and multiplication of dislocations. Predicted critical stresses for pyramidal (π)-to-Pr and reverse cross-slip agree closely with the experimental measurements. The latter cross-slip stress is a factor of two higher than that of unobstructed planar slip. The model accounts for overlapping dislocation cores and employs a Wigner-Seitz based cell to evaluate misfit energies. By combining ab initio density functional theory (DFT) with anisotropic elasticity, the framework identifies minimum energy pathways for dislocation glide, which can be intermittent and zig-zag. A simplified expression utilizing (π) and Pr Schmid factor ratios is proposed for critical stress corresponding to (π)-to-Pr cross-slip transition. The results are strongly dependent on crystal orientation, underscoring non-Schmid behavior. Overall, this study explores key critical stress parameters essential for informing higher-scale simulations of plasticity in Ti.

Critical stress↗
DOE OSTI2021

In situ TEM measurement of electrical properties of individual BaTiO 3 nanocubes

We report on the measurement of the electrical properties of individual pristine and doped BaTiO 3 nanocubes by using in situ transmission electron microscopy with a two-electrode configuration. The dimensions of the nanocubes tested are between 10 and 20 nm, which rendered their in situ electrical characterization challenging. We characterized 4%Cr and 5%La (atomic percentage) doped BaTiO 3 nanocubes and compared them with the properties of pristine BaTiO3 nanocubes synthesized by the same solvothermal method. We found that the resistance of all three types of nanocubes when displayed in log-scale shows a nearly linear dependence on the applied electric field (R2 ≥ 0.95) over a wide range of electric fields (50–900 kV/cm). Compared with pristine BaTiO 3 nanocubes, the resistance of both 4%Cr and 5%La doped nanocubes showed reduced variation rates with respect to the electric field, with 5%La doping, demonstrating a better reduction in the variation rate. By developing techniques capable of evaluating the properties of individual BaTiO 3 nanocubes, we expect that our work to open the door to the use of BaTiO 3 nanomaterials in the design of future multilayer ceramic capacitors with improved volumetric efficiency and ferroelectrics-enabled nanodevices with advanced functionality.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Microstructure and phase evolution in the U-10Zr fuel investigated by in situ TEM heating experiments

The development of U-Zr metallic nuclear fuel for fast spectrum reactors is impacted by a lack of mechanistic understanding of the fuel behavior evolution under thermal irradiation conditions, despite previous works providing substantial fuel performance data. This work uses in-situ transmission electron microscopy heating experiments to study phase and microstructural evolution in several unirradiated U-10Zr specimens during rapid heating ramps (from room temperature to 1000 °C). The starting a-U + bcc-(Zr, U) eutectic microstructure began to decompose above 600 °C. The decomposition initiated from the bcc (U,Zr) phase. Similar results were observed for all specimens even when fabricated by different routes (e.g., cold rolled or annealed). As a result, the impact of observed microstructure and phase evolutions at high temperatures on fuel fabrication and in-pile fuel transient test was also discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗