Results for “In situ characterization” — Page 21

DOE OSTI2021

Multi-Resolution Characterization of the Coupling Effects of Molten Salts, High Temperature and Irradiation on Intergranular Fracture

This project focused on providing a fundamental physico-chemical understanding of the coupling mechanisms of corrosion- and radiation-induced degradation at material-salt interfaces in Ni-based alloys operating in emulated Molten Salt Reactor(MSR) environments through the use of a unique suite of aging experiments, in-situ nanoscale characterization experiments on these materials, and multi-physics computational models. The technical basis and capabilities described in this report bring us a step closer to accelerate the deployment of MSRs by closing knowledge gaps related to materials degradation in harsh environments.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2023

Discovering Reactant Supply Pathways at Electrode/PEM Reaction Interfaces Via a Tailored Interface-Visible Characterization Cell

In situ and micro-scale visualization of electrochemical reactions and multiphase transports on the interface of porous transport electrode (PTE) materials and solid polymer electrolyte (SPE) has been one of the greatest challenges for electrochemical energy conversion devices, such as proton exchange membrane electrolyzer cells (PEMECs), CO 2 reduction electrolyzers, PEM fuel cells, etc. Here, an interface-visible characterization cell (IV-CC) is developed to in situ visualize micro-scaled and rapid electrochemical reactions and transports in PTE/SPE interfaces. Taking the PEMEC of a green hydrogen generator as a study case, the unanticipated local gas blockage, micro water droplets, and their evolution processes are successfully visualized on PTE/PEM interfaces in a practical PEMEC device, indicating the existence of unconventional reactant supply pathways in PEMs. Further comprehensive results reveal that PEM water supplies to reaction interfaces are significantly impacted with current densities. Here these results provide critical insights about the reaction interface optimization and mass transport enhancement in various electrochemical energy conversion devices.

30 DIRECT ENERGY CONVERSION↗

NASA NTRS2017

Quantitative Characterization of Structural and Mechanical Properties of Boron Nitride Nanotubes in High Temperature Environments

The structural stability and mechanical integrity of boron nitride nanotubes (BNNTs) in high temperature environments are of importance in pursuit of their applications that are involved with extreme thermal processing and/or working conditions, but remain not well understood. In this paper, we perform an extensive study of the impacts of high temperature exposure on the structural and mechanical properties of BNNTs with a full structural size spectrum from nano- to micro- to macro-scale by using a variety of in situ and ex situ material characterization techniques. Atomic force microscopy (AFM) and high resolution transmission electron microscopy measurements reveal that the structures of individual BNNTs can survive at up to 850 °C in air and capture the signs of their structural degradation at 900 °C or above. In situ Raman spectroscopy measurements reveal that the BN bonds in BNNT micro-fibrils undergo substantial softening at elevated temperatures of up to 900 °C. The AFM-based nanomechanical compression measurements demonstrate that the mechanical integrity of individual BNNTs remain intact after being thermally baked at up to 850 °C in air. The studies reveal that BNNTs are structurally and mechanically stable materials in high temperature environments, which enables their usages in high temperature applications.

Chen, Xiaoming↗

DOE OSTI2022

Predicting melt pool depth and grain length using multiple signatures from in-situ single camera two-wavelength imaging pyrometry for laser powder bed fusion

In laser powder bed fusion (LPBF), the in-situ process signatures are known to have a direct correlation with the microstructural properties of the solidified melt pool (MP). It is known that the MP cooling and heating rates, and laser processing parameters can critically determine the grain structure and thereby affect the part properties. The objective of this work is to study the feasibility of using in-process, high-speed imaging pyrometry for evaluating the solidified MP properties “below” the surface, such as depth and microstructural properties. To accomplish this, we employ an in-house single camera-based two-wavelength imaging pyrometry (STWIP) system for monitoring the printing of single-scan tracks with Inconel 718 on a commercial LPBF printer (EOS M290). Further, the lab designed STWIP system is a coaxial high-speed (>10,000 fps) imaging system capable of monitoring MP temperature, morphology, and intensity profiles. The temperature measurements from STWIP are emissivity independent. The STWIP measured MP signatures of the printed tracks are correlated with the ex-situ microscopy characterized MP depth and the average grain lengths. From the data analysis, using support vector machine (SVM)-based regression models, we found that the MP temperature signatures are crucial for an accurate prediction of MP depth and the grain length, thus validating the novelty and necessity of the developed in-situ monitoring methods and analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Calibration-Free Quantitative Analysis of Lithium-Ion Battery (LiB) Electrode Materials Using Laser-Induced Breakdown Spectroscopy (LIBS)

Recent years have seen a surge in the demand for high-performance battery electrode materials for automotive and various electronic device applications. Improving battery performance requires precise knowledge of the structure–composition properties of active electrode materials. To this effect, quantitative and precise estimation of the composition of advanced electrode materials, containing trace amounts of dopants, provide immense value toward developing next-generation high-capacity battery materials. Herein, we demonstrate the application of calibration-free laser-induced breakdown spectroscopy (LIBS) as a powerful analytical tool for rapid and reliable quantitative spectrochemical characterizations of layered Li metal oxide cathodes containing Mo and Cr dopants (<5 atom %). Specifically, we employ the LIBS using an internal calibration methodology to establish the quantitative elemental ratios of major (Ni, Mn, Co) and trace dopant (Cr, Mo) transition metals to bulk Li contents in diverse cathode material samples such as LiNi 0.5 Mn 0.5 O 2 (NM-50/50), LiNi 0.33 Mn 0.33 Co 0.33 O 2 (NMC), LiNi 0.317 Mn 0.317 Co 0.317 Cr 0.05 O 2 (Cr-doped NMC), and LiNi 0.5– x /2 Mn 0.5– x /2 Mo x O 2 ( x = 0.03, 0.04, 0.05) (Mo-doped NM-50/50) that were synthesized via sol–gel routes. The LIBS-estimated elemental compositions are in good agreement with the nominal stoichiometric values. Furthermore, ex situ LIBS characterizations presented here pave the path for future high-efficacy application of calibration-free quantitative LIBS for rapid in situ analyses of elemental composition changes in battery electrode materials under operation that need not resort to off-site analytical techniques requiring cumbersome sample preparations and/or external standards.

25 ENERGY STORAGE↗

DOE OSTI2023

Microstructural characterization of the oxidation of nuclear graphite under chronic and accident conditions via XCT and synchrotron XCT

Graphite is a candidate material to moderate fast neutrons and for structural components in the US next-generation graphite-moderated reactors. A graphite core is conceived as a large formation of interconnected bricks that primarily serves as the moderator of fast neutrons, holds instrumentation, fuel elements, control rods, and is a receptacle for molten salts for Molten Salt Reactors (MSRs) designs. During the operation of a graphite-moderated power plant, graphite components might be subjected to chronic oxidation during normal operating conditions or aggressive oxidation as a result of accidental ingress of air that reacts vigorously with the graphite core. Using synchrotron, x-ray computed tomography (XCT), this research systematically characterized microstructural changes that accompanied these two oxidation scenarios. Chronic oxidation was studied by characterizing IG-110, PCEA, and NBG-18 specimens that were gradually oxidized in air at a low temperature (520°C). The accidental ingress of air into the graphite reactor was simulated by subjecting the grades mentioned above to high-temperature oxidation at approximately 750°C. This research is the first, in situ, systematic characterization of nuclear graphite microstructural evolution that can be associated with the two possible oxidation scenarios and provide insight into related repercussions. The results show that the microstructure and pore connectivity influence the rate of oxidation and evolution of the microstructure under the two oxidation regimes. These results are crucial to understanding which grades are more resilient to each type of oxidation and documenting the damage created in the graphite.

Arregui Mena, Jose'↗

DOE OSTI2022

Synthesis of La 2–x Sr x CuO 4 films via atomic layer-by-layer molecular beam epitaxy

Atomic layer-by-layer molecular beam epitaxy (ALL-MBE) is a sophisticated technique to synthesize high-temperature superconductor (HTS) materials. ALL-MBE produces single-crystal HTS films with atomically smooth surfaces and interfaces, as well as precise multilayer heterostructures engineered down to a single atomic layer level. This enables the fabrication of tunnel junctions, nanowires, nanorings, and other HTS devices of interest. Our group has focused on ALL-MBE synthesis and materials science of La 2–x Sr x CuO 4 (LSCO), a representative HTS cuprate. In the past two decades, we have synthesized over three thousand LSCO thin films and characterized them by a range of analytical techniques. Here, we present in full detail a systematic process for the synthesis and engineering of atomically perfect LSCO films. The procedure includes the preparation of substrates, calibration of the elemental sources, the recipe for ALL growth of LSCO films without any secondary-phase precipitates, post-growth annealing of the films, and ex situ film characterization. This report should aid replication and dissemination of this technique of synthesizing single-crystal LSCO films for basic research as well as for HTS electronic applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2020

Correlating dynamic microstructure to observed color in electrophoretic displays via in situ small-angle x-ray scattering

Electrophoretic deposition (EPD) is an industrially relevant and scalable technique used to form particle deposits from colloidal suspensions. Highly concentrated particle suspensions generally prevent real-time in situ microscopy observations which limit the characterization of EPD films to ex situ, or postprocessed, laboratory techniques. For dynamic systems, such as tunable amorphous photonic crystals (APCs), only reversible deposits are formed during the EPD process. Since reversible deposits cannot be characterized with standard ex situ methods, the particle-particle and particle-field interactions that govern the displayed color and crystallinity of these systems are not well understood. In this paper, we present in situ small-angle x-ray scattering and UV-Vis techniques for measuring both the structural and optical response of an APC under applied electric fields. Furthermore, we also develop a computational model based on colloidal interactions to explain the observed change in the interparticle spacing of APCs due to the applied electric field which correlates to displayed color. Ultimately, this work provides a new in situ characterization method that could be expanded for other dynamic, tunable colloidal systems.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Active-Site Determination and Mechanistic Insights in a MOF-Supported Polymerization Catalyst

The structural elucidation of catalyst active sites in heterogeneous catalysts when supported by traditional metal oxides remains a challenge despite the advanced characterization techniques that have been developed. The catalyst-deposition-site nonuniformity in metal oxides inhibits clear structural characterization through bulk spectroscopic methods and rules out the use of single-crystal X-ray diffraction. However, for metal-organic framework (MOF)-supported catalysts, the crystallinity and uniform structures of the underlying support enhance our ability to identify the precatalyst and catalytically active sites and open the door to using single-crystal X-ray diffraction coupled with spectroscopy under reaction conditions. Additionally, the use of in situ X-ray absorption spectroscopy identifies the catalytically active site in diethylaluminum chloride (DEAC)-pretreated Cr-SIM-NU-1000 to be a Cr-ethyl when used for ethylene polymerization. Further kinetic experiments elucidate the effects of ethylene pressure, temperature, catalyst loading, and cocatalyst loading, furthering mechanistic knowledge and helping to deconvolute the structure-function relationship.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogeneities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogeneities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogeneities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogenities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

ICME and In-Situ Process Monitoring for Rapid Qualification of Components Made by Laser-based Powder Bed Additive Manufacturing Processes for Nuclear Structural Applications

Additive manufacturing (AM) through selective powder bed melting of successive layers is being considered as disruptive technology for rapid production of low-cost nuclear reactor internal components with complex geometries. However, there is a potential for non-uniform distribution of physical features, such as porosity or microstructural differences, due to variations of temperature across a component build. These heterogenities make the deployment of traditional material qualification and non-destructive evaluation of AM components difficult. This research project explored the feasibility of using in-situ process monitoring methods and integrated computational materials engineering (ICME) principles as an alternate qualification methodology and approach. This project included six individual tasks: (i) design of artifacts relevant to the nuclear power industry, (ii) evaluation of laser processing and in-situ measurements, (iii) computational modeling, (iv) ex-situ microstructural characterization, (v) evaluation of scaling the methodology for large-scale structures, and (vi) development of a data package to codes and standards organizations. As a part of this research, laser powder bed fusion of metals (316L, Alloy 718, and Ti6Al4V) was explored. This document provides an overview of the research performed over three years and serves as the final U.S. Department of Energy report for this project. In the third year, the project focused on the following activities: (a) in-situ infrared and optical imaging of each layer during processing of representative stainless steel geometries; (b) development of methodologies to analyze the data; and (c) application of ICME methodologies and other experiments to estimate the relevance of defects and microstructure to tensile properties.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Characterizing Stress Roughness at Utah FORGE Through Simulation of Hydraulic Fracture Growth During 16A Stage 3 Stimulation

In most geologic formations, the vertical gradient of the minimum horizontal stress (𝜎 h ) exceeds the hydrostatic gradient, often driving hydraulic fractures to propagate upward. However, observations indicate that the upward growth of real hydraulic fractures is less pronounced than theoretical predictions based on smoothly varying 𝜎 h fields. In fact, the layered structure of sedimentary rocks hinders fracture propagation across layers, partially explaining the limited height growth observed in practice (Zoback et al., 2022). While crystalline rocks lack the pervasive layered fabric of sedimentary formations, they still possess structural fabric formed over their geologic history, resulting in inherently "rough" in situ stress fields. Recent studies have identified another key factor: the "roughness" of in situ stress, characterized by temporal, relatively short-wavelength fluctuations superimposed on the overall stress gradient. This stress roughness leads to apparent toughness anisotropy, where the vertical toughness appears significantly larger than the horizontal toughness (P. Fu et al., 2019; Dontsov & Suarez-Rivera, 2021). Neglecting the effects of rock fabric and stress roughness can yield inaccurate predictions of hydraulic fracture geometry and growth rates at larger length scales.

58 GEOSCIENCES↗

DOE OSTI2021

Reduction and Agglomeration of Supported Metal Clusters Induced by High-Flux X-ray Absorption Spectroscopy Measurements

Supported metal clusters are widely used in catalysis for many important reactions. To understand the catalytic properties, in situ/operando characterization techniques, such as X-ray absorption spectroscopy (XAS), provide essential details of the size, shape, and chemical composition of the cluster and the nature of the active sites. New-generation synchrotrons combined with focusing beamlines provide high-flux-density X-rays for improved detection sensitivity as well as higher time and spatial resolution. Understanding the effects of a high-flux-density X-ray beam on the catalyst during the actual measurement, whether XAS or another synchrotron-based technique, is crucial. This is especially important for in situ and operando studies where both the high flux density and reaction conditions can affect the catalyst structure. In this work, we investigated the effect of the flux density on rhodium clusters supported on Al 2 O 3 at two different beamlines: National Synchrotron Light Source II beamline 08-ID and Stanford Synchrotron Radiation Light Source (SSRL) beamline 4-1. We show that the higher flux density at beamline 08-ID causes the reduction of the highly dispersed RhO x /Al 2 O 3 catalyst, even at room temperature. Additionally, exposure to the higher flux density X-rays at beamline 08-ID during in situ reduction results in significant agglomeration of the Rh clusters. The final size of the Rh nanoparticles reduced at 310 °C is equivalent to that of particles formed after the reduction at 600–650 °C in the absence of the beam. Significant beam-induced reduction and agglomeration is also shown for Ni supported on beta zeolite during in situ reduction at an intermediate-flux-density beamline 9-3 at SSRL, indicating that beam-induced changes in heterogeneous catalysts could be common at intermediate- and high-flux-density beamlines. We provide precautions and recommendations for detecting and minimizing beam damage during in situ/operando XAS measurements.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Rapid multiplex ultrafast nonlinear microscopy for material characterization

We demonstrate rapid imaging based on four-wave mixing (FWM) by assessing the quality of advanced materials through measurement of their nonlinear response, exciton dephasing, and exciton lifetimes. We use a WSe 2 monolayer grown by chemical vapor deposition as a canonical example to demonstrate these capabilities. By comparison, we show that extracting material parameters such as FWM intensity, dephasing times, excited state lifetimes, and distribution of dark/localized states allows for a more accurate assessment of the quality of a sample than current prevalent techniques, including white light microscopy and linear micro-reflectance spectroscopy. We further discuss future improvements of the ultrafast FWM techniques by modeling the robustness of exponential decay fits to different spacing of the sampling points. Employing ultrafast nonlinear imaging in real-time at room temperature bears the potential for rapid in-situ sample characterization of advanced materials and beyond.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Synthesis and Advanced Characterization of Polymer–Protein Core–Shell Nanoparticles

Enzyme immobilization techniques are widely researched due to their wide range of applications. Polymer–protein core–shell nanoparticles (CSNPs) have emerged as a promising technique for enzyme/protein immobilization via a self-assembly process. Based on the desired application, different sizes and distribution of the polymer–protein CSNPs may be required. This work systematically studies the assembly process of poly(4-vinyl pyridine) and bovine serum albumin CSNPs. Average particle size was controlled by varying the concentrations of each reagent. Particle size and size distributions were monitored by dynamic light scattering, ultra-small-angle X-ray scattering, small-angle X-ray scattering and transmission electron microscopy. Results showed a wide range of CSNPs could be assembled ranging from an average radius as small as 52.3 nm, to particles above 1 µm by adjusting reagent concentrations. In situ X-ray scattering techniques monitored particle assembly as a function of time showing the initial particle growth followed by a decrease in particle size as they reach equilibrium. The results outline a general strategy that can be applied to other CSNP systems to better control particle size and distribution for various applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗