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At least 703 records · Page 39

Repeatability and sensitivity characterization of the far-field high-energy diffraction microscopy instrument at the Advanced Photon Source

In the last two decades, far-field high-energy diffraction microscopy (FF-HEDM) and similar non-destructive techniques have been actively developed at synchrotron light sources around the world. As these techniques (and associated analysis tools) are becoming more available for the general users of these light sources, it is important and timely to characterize their performance and capabilities. In this work, the FF-HEDM instrument implemented at the 1-ID-E endstation of the Advanced Photon Source (APS) is summarized. The set of measurements conducted to characterize the instrument's repeatability and sensitivity to changes in grain orientation and position are also described. When an appropriate grain matching method is used, the FF-HEDM instrument's repeatability is approximately 5 µm in translation, 0.02° in rotation, and 2 × 10 −4 in strain; the instrument sensitivity is approximately 5 µm in translation and 0.05° in rotation.

3DXRD↗

Sample Preparation for 3D Characterization of Irradiated Fuel

Thorough characterization of nuclear fuel is essential when striving to understand its microstructural evolution in response to varying irradiation conditions. A detailed understanding of the microstructural evolution of irradiated fuel can be useful when predicting the fuel’s response to off-normal conditions and related phenomena such as high burnup fuel fragmentation (HBFF) and fission gas release. This sort of characterization and the study of complex phenomena like HBFF that are related to fuel performance are an important part of the US Department of Energy Office of Nuclear Energy’s Advanced Fuels Campaign (AFC). Multiple characterization techniques are commonly used to perform post-irradiation examination (PIE) analysis on an irradiated fuel sample, but many of these techniques are limited to the 2D surface analysis of the fuel pellet. Although there is a lot of useful information to be gained by analyzing the fuel pellet surface, a 2D analysis provides only an approximation of the nature of the material’s features, such as porosity and grain structure. Therefore, it is critical to analyze the 3D structure of the material, as materials exist and respond to conditions in all three dimensions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Addressing Critical Problems in Materials Science Through Multiscale and Multimode Characterization (Project 1); Characterization and Optimization of Novel Triple-Conducting Oxide Materials for Energy Applications (Project 2) (CRADA Final Report)

PROJECT 1: Address critical problems in materials science and simultaneously advance the state-of-the-art in multiscale and multimode characterization using the combined advanced analytical capabilities and expertise of Colorado School of Mines (CSM) and the National Renewable Energy Laboratory (NREL). The primary effort of the Phase I of this CRADA is to establish the International Center for Multiscale Characterization using shared resources at both NREL and CSM. Phase II will focus on capability development and marketing, choosing candidate materials science issues in the areas of structure imaging, chemical composition mapping, and correlating properties and performance of materials for impact in energy-related, environmental and critical materials areas. The CRADA will be modified to include specific topics of concern in materials science to industry member partners. Advanced analytical capabilities and expertise at CSM and NREL will be used to advance materials understanding and performance through characterization of multiscale phenomena including structural imaging, chemical composition mapping, and other techniques correlating properties and performance of materials. PROJECT 2: As part of the International Center for Materials Characterization, work under Modification #1 will be led by Colorado School of Mines (CSM), working in collaboration with NREL staff to mentor and advise CSM postdoctoral researchers on set up of diffusion annealing experiments. The purpose of the modification is to provide for NREL staff to mentor and advise CSM postdoctoral researchers on set up of diffusion annealing experiments, including mentoring and advising the CSM-NREL team on proper Secondary Ion Mass Spectrometry (SIMS) data analysis as needed. SIMS measurements of 10-20 samples will be performed at NREL during the project duration.

08 HYDROGEN↗

Development of Spectroscopic Tools for Nuclear Forensics Signatures Development

Diversion of nuclear materialsfrom legitimate commercial processes for use by nefarious actors is a frightening and surreptitious problem. Smuggled nuclear material can be used to manufacture a simple radiological dispersion device (RDD) and potentially incorporated into the development of a nuclear weapon. With some frequency, smuggled nuclear material is interdicted in foreign countries as actors cross border checkpoints. Nuclear material interdicted in this way can be analyzed using a variety of tools. Plutonium-239 is commonly used as the fissile material in nuclear weapon production as an alternative to uranium-235. Plutonium in a production, refining, or finishing facility will exist in many forms including oxide precursors (PuF4, PuF3, Pu oxalate, etc.), oxide, and metal. The ability to identify plutonium in each of these forms and determine properties, characteristics, or history of these materials is crucial for determining if the processes occurring in a nuclear facility are legitimate or not. This presentation will focus on the development and application ofspectroscopic tools developed at SRNL using doubled-walled cells (DWC) to characterize Pu-bearing compounds. Advances in the use of vibrational spectroscopy techniques (Raman and IR), UV-VIS-SWIR diffuse reflectance spectroscopy, gamma emission spectroscopy, luminescence spectroscopy, laser-induced breakdown spectroscopy in conjunction with XRD and SEM in the characterization of Pu-bearing compounds will be presented with emphasis in material processing history.

Villa-Aleman, Eliel↗

Characterization of an Integral Thermal Protection and Cryogenic Insulation Material for Advanced Space Transportation Vehicles

NASA's planned advanced space transportation vehicles will benefit from the use of integral/conformal cryogenic propellant tanks which will reduce the launch weight and lower the earth-to-orbit costs considerably. To implement the novel concept of integral/conformal tanks requires developing an equally novel concept in thermal protection materials. Providing insulation against reentry heating and preserving propellant mass can no longer be considered separate problems to be handled by separate materials. A new family of materials, Superthermal Insulation (STI), has been conceiving and investigated by NASA's Ames Research Center to simultaneously provide both thermal protection and cryogenic insulation in a single, integral material.

Salerno, L. J.↗

Pyroelectric thin films—Past, present, and future

Pyroelectrics are a material class that undergoes a change in polarization as the temperature of the system is varied. This effect can be utilized for applications ranging from thermal imaging and sensing to waste-heat energy conversion to thermally driven electron emission. Here, we review recent advances in the study and utilization of thin-film pyroelectrics. Leveraging advances in modeling, synthesis, and characterization has provided a pathway forward in one of the more poorly developed subfields of ferroelectricity. We introduce the complex physical phenomena of pyroelectricity, briefly explore the history of work in this space, and highlight not only new advances in the direct measurement of such effects but also how our ability to control thin-film materials is changing our understanding of this response. Finally, we discuss recent advances in thin-film pyroelectric devices and introduce a number of potentially new directions the field may follow in the coming years.

36 MATERIALS SCIENCE↗

Species-Specific Duplication Event Associated with Elevated Levels of Nonstructural Carbohydrates in Sorghum bicolor

Simple sugars are the essential foundation to plant life, and thus, their production, utilization, and storage are highly regulated processes with many complex genetic controls. Despite their importance, many of the genetic and biochemical mechanisms remain unknown or uncharacterized. Sorghum, a highly productive, diverse C4 grass important for both industrial and subsistence agricultural systems, has considerable phenotypic diversity in the accumulation of nonstructural sugars in the stem. We use this crop species to examine the genetic controls of high levels of sugar accumulation, identify genetic mechanisms for the accumulation of nonstructural sugars, and link carbon allocation with iron transport. We identify a species-specific tandem duplication event controlling sugar accumulation using genome-wide association analysis, characterize multiple allelic variants causing increased sugar content, and provide further evidence of a putative neofunctionalization event conferring adaptability in Sorghum bicolor. Comparative genomics indicate that this event is unique to sorghum which may further elucidate evolutionary mechanisms for adaptation and divergence within the Poaceae. Furthermore, the identification and characterization of this event was only possible with the continued advancement and improvement of the reference genome. The characterization of this region and the process in which it was discovered serve as a reminder that any reference genome is imperfect and is in need of continual improvement.

59 BASIC BIOLOGICAL SCIENCES↗

Unraveling the multi-step crystallization mechanism of polytetrafluoroethylene, modified polytetrafluoroethylene, and their nanocomposites with boron nitride nanobarbs: Experimental insights and theoretical analysis

The non-isothermal crystallization behavior and kinetics of polytetrafluoroethylene (PTFE) composites with boron nitride nanobarb (BNNB), a new generation nanostructure with unique surface morphology and mechanical “barbs” have been analyzed, understanding these properties is essential for their high-end applications as thermal interface materials (TIM) for microwave, 5G and microelectronic devices. The analysis of the crystallization parameters includes crystallization onset, peak and end temperatures, crystallization half-life and overall crystallinity of PTFE, modified PTFE and their BNNB composites. The results were further analyzed using theoretical models such as the combined Avrami-Ozawa model. It was found that BNNB supports crystallization in the modified PTFE but shows minimal effect on the crystallization of PTFE. Due to the limitation of the classical theoretical models used above in fully characterizing the multi-step crystallization process of PTFE, an in-depth analysis using the model-free advanced isoconversional computation was used to characterize the PTFE crystallization based on the evolution of activation energy with fractional crystallinity and for the first time with temperature. Three kinetic regions were identified in the crystallization mechanism. Here, this study investigated the molecular organization and microstructural evolution of PTFE, modified PTFE and their composites during non-isothermal crystallization using advanced X-ray scattering measurements. An insight into the changes undergone by the material's microstructural units including crystallite size and morphology, lamellar thickness and lamellar interfacial layer thickness, and crystallographic phase dynamics during non-isothermal cooling from the melt, was provided here in this work. The effect of copolymer modification of PTFE and the inclusion of pristine and functionalized BNNB (a thermally conductive and electrically insulating ceramic) are both new investigations that provide valuable knowledge for the development of materials with strong matrix-nanofiller interaction and guidance for optimizing sintering and cooling cycles, two key steps in PTFE processing that largely affect the material microstructural features. Overall, the result of the three-part investigation demonstrates that BNNB supports crystallization in the modified PTFE up to 20 wt% concentration and at low and high cooling rates typically used in the industrial processing of PTFE.

36 MATERIALS SCIENCE↗

Measuring the Burgers vector of dislocations with dark-field X-ray microscopy

The subsurface dynamics of dislocations are essential to many properties of bulk crystalline materials. However, it is challenging to characterize a bulk crystal by conventional transmission electron microscopy (TEM) due to the limited penetration depth of electrons. A novel X-ray imaging technique – dark-field X-ray microscopy (DFXM) – was developed to image hierarchical dislocation structures in bulk crystals. While today's DFXM can effectively map the line structures of dislocations, it is still challenging to quantify the Burgers vectors, the key characterization governing the dislocation behaviors. Here, we extend the 'invisibility criterion' formalism from the TEM theory to the geometrical-optics model of DFXM and demonstrate the consistency between DFXM and dark-field TEM using multi-diffraction-peak imaging for a single edge dislocation. Due to the practical difficulty of multi-peak DFXM experiments, we further study how the Burgers vector effect is encoded for a single-peak DFXM experiment. Using the geometrical-optics DFXM simulation, we explore the asymmetry of rocking tilt scans at different rolling tilts and develop a new method to characterize the Burgers vector. The conclusions of this study advance our understanding of the use of DFXM in characterizing individual dislocations, enabling the connection from bulk DFXM imaging to dislocation mechanics.

36 MATERIALS SCIENCE↗

ATOMIC AND MICROSTRUCTURAL ORIGINS OF STORED ENERGY RELEASE IN NEUTRON-IRRADIATED SILICON CARBIDE

Here, we employ a combination of advanced synchrotron-based scattering characterization techniques to understand and unravel the atomic origins of the colossal stored energy release in neutron irradiated silicon carbide. The quantification of the neutron irradiation-induced defects, and their impact on the structureproperty relationship is important for the design and safe operation of advanced fission and fusion reactors. Our experimental results show that the atomic structure in the as irradiated samples is significantly perturbed due to a large fraction of vacancy and interstitial type defects that lead to complex microstructures and additional components in the x-ray diffraction and pair distribution function results. We directly correlate the stored energy release to the recovery of the sub-lattices, with pair distribution function analysis highlighting that the carbon interstitial and vacancy-type defects contribute to stored energy more than those of silicon. We find these results to be striking and believe our discoveries to be timely and noteworthy given the technological importance of silicon carbide to the nuclear fission and fusion communities.

Sprouster, D.J.↗

Ultrasonic Nondestructive Evaluation Techniques Applied to the Quantitative Characterization of Textile Composite Materials

In this Progress Report, we describe our recent developments of advanced ultrasonic nondestructive evaluation methods applied to the characterization of anisotropic materials. We present images obtained from experimental measurements of ultrasonic diffraction patterns for a thin woven composite in an immersion setup. In addition, we compare apparent signal loss measurements of the thin woven composite for phase-sensitive and phase-insensitive detection methods. All images of diffraction patterns have been included on the accompanying CD-ROM in the Adobe(Trademark) Portable Document Format (PDF). Due to the extensive amount of data, however, hardcopies of only a small representative selection of the images are included within the printed report. This Progress Report presents experimental results that support successful implementation of single element as well as one and two-dimensional ultrasonic array technologies for the inspection of textile composite structures. In our previous reports, we have addressed issues regarding beam profiles of ultrasonic pressure fields transmitted through a water reference path and transmitted through a thin woven composite sample path. Furthermore, we presented experimental results of the effect of a thin woven composite on the magnitude of an insonifying ultrasonic pressure field. In addition to the study of ultrasonic beam profiles, we consider issues relevant to the application of single-element, one-dimensional, and two-dimensional array technologies towards probing the mechanical properties of advanced engineering composites and structures. We provide comparisons between phase-sensitive and phase-insensitive detection methods for determination of textile composite structure parameters. We also compare phase-sensitive and phase-insensitive - - ---- ----- apparent signal loss measurements in an effort to study the phenomenon of phase cancellation at the face of a finite-aperture single-element receiver. Furthermore, in this Progress Report we extend our work on ultrasonic beam profile issues through investigation of the phase fronts of the pressure field. In Section H of this Progress Report we briefly describe the experimental arrangement and methods for data acquisition of the ultrasonic diffraction patterns upon transmission through a thin woven composite. Section III details the analysis of the experimental data followed by the experimental results in Section IV. Finally, a discussion of the observations and conclusions is found in Section V.

Miller, James G.↗

Development of advanced fuel cell system, phase 2

A multiple task research and development program was performed to improve the weight, life, and performance characteristics of hydrogen-oxygen alkaline fuel cells for advanced power systems. Development and characterization of a very stable gold alloy catalyst was continued from Phase I of the program. A polymer material for fabrication of cell structural components was identified and its long term compatibility with the fuel cell environment was demonstrated in cell tests. Full scale partial cell stacks, with advanced design closed cycle evaporative coolers, were tested. The characteristics demonstrated in these tests verified the feasibility of developing the engineering model system concept into an advanced lightweight long life powerplant.

Handley, L. M.↗

Ultrasonic Nondestructive Evaluation Techniques Applied to the Quantitative Characterization of Textile Composite Materials

In this Progress Report, we describe our further development of advanced ultrasonic nondestructive evaluation methods applied to the characterization of anisotropic materials. We present images obtained from experimental measurements of ultrasonic diffraction patterns transmitted through water only and transmitted through water and a thin woven composite. All images of diffraction patterns have been included on the accompanying CD-ROM in the JPEG format and Adobe TM Portable Document Format (PDF), in addition to the inclusion of hardcopies of the images contained in this report. In our previous semi-annual Progress Report (NAG 1-1848, December, 1996), we proposed a simple model to simulate the effect of a thin woven composite on an insonifying ultrasonic pressure field. This initial approach provided an avenue to begin development of a robust measurement method for nondestructive evaluation of anisotropic materials. In this Progress Report, we extend that work by performing experimental measurements on a single layer of a five-harness biaxial woven composite to investigate how a thin, yet architecturally complex, material interacts with the insonifying ultrasonic field. In Section 2 of this Progress Report we describe the experimental arrangement and methods for data acquisition of the ultrasonic diffraction patterns upon transmission through a thin woven composite. We also briefly describe the thin composite specimen investigated. Section 3 details the analysis of the experimental data followed by the experimental results in Section 4. Finally, a discussion of the observations and conclusions is found in Section 5.

Miller, James G.↗

Genome-Scale Transcription-Translation Mapping Reveals Features of Zymomonas mobilis Transcription Units and Promoters

Efforts to rationally engineer synthetic pathways in Zymomonas mobilis are impeded by a lack of knowledge and tools for predictable and quantitative programming of gene regulation at the transcriptional, posttranscriptional, and posttranslational levels. With the detailed functional characterization of the Z. mobilis genome presented in this work, we provide crucial knowledge for the development of synthetic genetic parts tailored to Z. mobilis . This information is vital as researchers continue to develop Z. mobilis for synthetic biology applications. Our methods and statistical analyses also provide ways to rapidly advance the understanding of poorly characterized bacteria via empirical data that enable the experimental validation of sequence-based prediction for genome characterization and annotation.

59 BASIC BIOLOGICAL SCIENCES↗

Characterization of Porous Transport Layers Towards the Development of Efficient Proton Exchange Membrane Water Electrolysis

The current goals for implementing the hydrogen economy have highlighted a need to further optimize water-splitting technologies for clean hydrogen production. Proton exchange membrane water electrolysis (PEMWE) is a leading technology, but further optimizations of anode materials including the porous transport layer (PTL) and the adjacent catalyst layer (CL) are required to increase overall cell performance and reduce cost. This literature review describes advances in PTL development and characterization, highlighting early PTL characterization work and most common methods including capillary flow porometry and mercury intrusion porometry, optical imaging, neutron and x-ray radiography, and x-ray computed tomography. The article also discusses PTL protective coatings and their characterizations, focusing on platinum group metal (PGM)-based coatings, alternative non-PGM-based coatings, post-treated PTLs, and investigations into thin PGM-based coatings. Furthermore, it highlights the integration of the PTL and the adjacent CL along with associated characterization challenges. Lastly, this review discusses future developments in the characterization needed to improve PEMWE's performance and long-term durability are discussed.

08 HYDROGEN↗