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DOE OSTI2021

Connection between the physicochemical characteristics of amorphous carbon thin films and their electrochemical properties

Connecting a material's surface chemistry with its electrocatalytic performance is one of the major questions in analytical electrochemistry. This is especially important in many sensor applications where analytes from complex media need to be measured. Unfortunately, today this connection is still largely missing except perhaps for the most simple ideal model systems. Here we present an approach that can be used to obtain insights about this missing connection and apply it to the case of carbon nanomaterials. In this paper we show that by combining advanced computational techniques augmented by machine learning methods with x-ray absorption spectroscopy (XAS) and electrochemical measurements, it is possible to obtain a deeper understanding of the correlation between local surface chemistry and electrochemical performance. As a test case we show how by computationally assessing the growth of amorphous carbon (a-C) thin films at the atomic level, we can create computational structural motifs that may in turn be used to deconvolute the XAS data from the real samples resulting in local chemical information. Then, by carrying out electrochemical measurements on the same samples from which x-ray spectra were measured and that were further characterized computationally, it is possible to gain insight into the interplay between the local surface chemistry and electrochemical performance. To demonstrate this methodology, we proceed as follows: after assessing the basic electrochemical properties of a-C films, we investigate the effect of short HNO 3 treatment on the sensitivity of these electrodes towards an inner sphere redox probe dopamine to gain knowledge about the influence of altered surface chemistry to observed electrochemical performance. Overall, these results pave the way towards a more general assessment of electrocatalysis in different systems and provide the first steps towards data driven tailoring of electrode surfaces to gain optimal performance in a given application.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2025

Measuring thermal curing induced shrinkage of material extrusion based additive manufacturing silicone elastomer lattices by X-ray computed tomography

Thermal curing induces shrinkage in material extrusion based additive manufacturing silicone elastomer samples, resulting in discrepancies between as printed and final geometries. Knowing the extent to which the samples change in shape and size allows us to make appropriate modifications to the printing design to better control the geometry of the samples. We present an X-ray computed tomography (CT) based approach to determine filament-level shrinkage due to thermal curing of silicone elastomer samples printed with direct ink writing (DIW). The approach relies on custom-designed build plates that are resistant to the elevated curing temperatures and that have sufficiently distinct X-ray absorption characteristics from the silicone elastomer to ensure adequate segmentation of the latter in X-ray imaging data. We implement the approach to evaluate shrinkage in DIW ‘log pile’ samples with three distinct strand arrangements and demonstrate of how filament-level information can be extracted from the X-ray CT data.

Additive manufacturing↗

DOE OSTI2022

Improved Understanding of Zircaloy Hydrogen Pickup Mechanisms in BWRs. NSUF Report (Final Report)

Using an instrumented autoclave operating at 288°C and 1100 psi, electrical impedance spectroscopy (EIS) measurements were taken from three neutron irradiated fuel channel samples (Zircaloy-2 and Zircaloy-4). The three high priority fuel channel samples were tested at 288°C using a simulated PWR water with the AC frequency range extending down through 10 -4 Hz, with corresponding DC measurements to validate the resistance measurements. EIS measurements were also taken at room temperature using a simulated PWR water from four neutron irradiated fuel channel samples (Zircaloy-2 and Zircaloy-4). and four water rod samples (Zircaloy-2). EIS measurements were also performed on unirradiated Zircaloy-2 tubes that were previously oxidized in autoclaves at various temperatures for different time durations to obtain oxide layers of different thicknesses. These experiments proved to be more challenging than anticipated because of the small size of the samples, which required development of fixtures to allow valid testing of the materials, some of which are radioactive, under pressure and temperature. Equivalent circuits were used to model the data. Some samples resulted in Nyquist plots where the arcs were too close to each other resulting in the inability to separate the different oxide morphological thicknesses. Microstructural characterization in the form of optical microscopy, scanning electron microscopy and (scanning) transmission electron microscopy was performed to document the microstructural features of the oxidized Zr-2 and Zr-4 samples (oxide and metal/oxide interface) and to interpret the EIS results. At the start of this work, it was assumed that despite the laminar cracks and porosity visible in both optical and SEM, the oxide scale is dense near the metal, effectively preventing the water from contacting the metal directly. While it is generally accepted that the large laminar cracks pores allow the water to percolate into the oxide film, it is unknown just how deep it can go, and how interconnected is the porosity, which will dictate how much the porosity is connected electrically to the water within the oxide scale. The EIS results demonstrated that there is in fact a distribution of oxide thicknesses over the various samples, and within each material condition, that are communicating to the liquid. This is derived from the fact that Nyquist plots have an arc radius whose center point is often below the Z’ axis, implying that instead of a single oxide thickness, these oxides have a distribution of thicknesses. This distribution of thicknesses produces arcs that are not clearly separable in most of the samples.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2026

Investigation of nonlinear mechanical behavior of two superfine-grained graphites with DIC assisted disc splitting test

Using standardized uniaxial tensile test specimens is not practical due to the limited volumes in irradiation capsules, molten salt degradation facilities, or oxidation apparatus. The ASTM International Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite (ASTM D8289) was developed to provide a convenient way for estimating tensile strength. Unlike the traditional uniaxial tensile test in ASTM C749 (International Standard Test Method for Tensile Stress–Strain of Carbon and Graphite), which uses dog-bone shaped specimens larger than 12.95 mm × 120.65 mm, the ASTM D8289 standard uses smaller discs with diameters of 6–12.7 mm. A digital image correlation (DIC) system, which uses a full-field noncontact surface displacement measurement technique, was applied along with the ASTM D8289 disc splitting test on IG-110 samples and compared with previous measurements from Mersen 2114 samples. Results confirmed that the DIC technique can measure the surface displacement/strain on these small (Ø6 mm × 3 mm) graphite specimens with good repeatability. However, Mersen 2114 and IG-110 samples exhibited strain discrepancies when DIC measurements were compared with analytical and finite element simulation values. The loading history and strain results also indicated different mechanical behaviors between Mersen 2114 and IG-110, particularly the nonlinear behavior of the IG-110 samples. Good agreement was observed by comparing the splitting tensile strengths of two superfine-grained grades with results from other work. The specimen size effect is discussed when comparing the splitting tensile strength with corresponding uniaxial tensile strength of these two graphite grades.

Lin, Lianshan [ORNL] (ORCID:0000000203399219)↗

DOE OSTI2021

Plasma catalytic ammonia synthesis on Ni nanoparticles: The size effect

Herein we demonstrate the synthesis of ammonia via atmospheric DBD plasma discharge over nickel nanoparticles supported on silica. We evaluated the performance of nickel nanoparticles with average sizes of 5.6nm and 13.5 nm. The smallest nanoparticle size sample resulted in an ammonia synthesis rate at least 2 times higher than that of the larger nanoparticle size sample and nickel bulk at equimolar composition. This allowed us to observe experimentally, for the first time, the size effect in the area of plasma catalysis. Moreover, the presented results allowed us to investigate a hydrogen sink metal such as nickel under atmospheric plasma conditions and determine the gas composition that resulted beneficial for this surface chemistry.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Big Data Processing for Power Grid Event Detection

In this paper we present the application of big data processing for the development of machine learning(ML) models to detect relevant events in power gridoperations. This is based on almost 20TB of phasormeasurement unit data corresponding to up to two years of operation of three grid interconnections which provide power to most of the United States. A significant aspect of the work consists in having all data processing performed on a single standard GPU server, from pre-processing to ML model training and testing. We describe the data and computational infrastructure, challenges faced and methods used in dataprocessing, main findings and results. The ML approach employed for best utilization of the big data is also discussed, including sample results.

Paes Leao, Bruno↗

DOE OSTI2020

Big Data Processing for Power Grid Event Detection

In this paper we present the application of big data processing for the development of machine learning (ML) models to detect relevant events in power grid operations. This is based on almost 20TB of phasor measurement unit data corresponding to up to two years of operation of three grid interconnections which provide power to most of the United States. A significant aspect of the work consists in having all data processing performed on a single standard GPU server, from pre-processing to ML model training and testing. We describe the data and computational infrastructure, challenges faced and methods used in data processing, main findings and results. The ML approach employed for best utilization of the big data is also discussed, including sample results.

Paes Leao, Bruno↗

DOE OSTI2024

Characteristics of graphene oxide-like materials prepared from different deashed-devolatilized coal chars and comparison with graphite-based graphene oxide, with or without the ultrasonication treatment

Deashed-devolatilized coal chars were prepared from anthracite, bituminous, subbituminous, and lignite coals, then oxidized to prepare graphene oxide (GO)-like materials that were extensively characterized and compared with a pristine graphite-based GO sample (CGO). Coal-based GO-like materials and CGO were then subjected to ultrasonication treatment for delamination, which also impacted their physicochemical properties. The surface oxygen contents of CGO and coal-based samples were ~32 % and ~26–35 %, respectively, that were reduced to ~27 % and ~21–24 %, respectively, after ultrasonication. The Fourier transform infrared and X-ray photoelectron spectroscopy spectra of all samples showed different profiles before and after the ultrasonication, suggesting a change in chemical functionalities. The Raman spectra of CGO and coal-based samples exhibited similar D and G bands with D/G intensity ratios (I D /I G ) of 0.93 and 0.88–0.92, respectively. The I D /I G ratio of CGO and most of the coal-based samples increased after the ultrasonication due to creation of more defects. The main X-ray diffraction (XRD) peak for CGO and coal-based samples were observed at ~11° and ~22–24°, respectively. Ultrasonication of the samples resulted in a reduction of crystallite size and number of layers for all CGO and coal-based samples, confirming both splitting and delamination of carbon layers. Additionally, different coal-based samples exhibited almost overlapping XRD profiles after the ultrasonication.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Sample Identifiers and Metadata Reporting Format for Environmental Systems Science

The ESS-DIVE sample identifiers and metadata reporting format primarily follows the System for Earth Sample Registration (SESAR) Global Sample Number (IGSN) guide and template, with modifications to address Environmental Systems Science (ESS) sample needs and practicalities (IGSN-ESS). IGSNs are associated with standardized metadata to characterize a variety of different sample types (e.g. object type, material) and describe sample collection details (e.g. latitude, longitude, environmental context, date, collection method). Globally unique sample identifiers, particularly IGSNs, facilitate sample discovery, tracking, and reuse; they are especially useful when sample data is shared with collaborators, sent to different laboratories or user facilities for analyses, or distributed in different data files, datasets, and/or publications. To develop recommendations for multidisciplinary ecosystem and environmental sciences, we first conducted research on related sample standards and templates. We provide a comparison of existing sample reporting conventions, which includes mapping metadata elements across existing standards and Environment Ontology (ENVO) terms for sample object types and environmental materials. We worked with eight U.S. Department of Energy (DOE) funded projects, including those from Terrestrial Ecosystem Science and Subsurface Biogeochemical Research Scientific Focus Areas. Project scientists tested the process of registering samples for IGSNs and associated metadata in workflows for multidisciplinary ecosystem sciences. We provide modified IGSN metadata guidelines to account for needs of a variety of related biological and environmental samples. While generally following the IGSN core descriptive metadata schema, we provide recommendations for extending sample type terms, and connecting to related templates geared towards biodiversity (Darwin Core) and genomic (Minimum Information about any Sequence, MIxS) samples and specimens. ESS-DIVE recommends registering samples for IGSNs through SESAR, and we include instructions for registration using the IGSN-ESS guidelines. Our resulting sample reporting guidelines, template (IGSN-ESS), and identifier approach can be used by any researcher with sample data for ecosystem sciences.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

The Impact of Sintering Atmosphere and Temperature on the Phase Evolution of High Surface Area LSCF Prepared by In Situ Carbon Templating

The thermochemical stability of lanthanum strontium cobalt ferrite (LSCF) processed between 1000 °C–1200 °C via the in situ carbon templating method was studied. This method generates high surface area ceramics at traditional solid oxide fuel cell (SOFC) sintering temperatures by generating a carbon template in situ and subsequently removing the template by oxidation at 700 °C. Argon processed samples produced an amorphous carbon template, whereas nitrogen tended to form graphitic carbon. Prior to the oxidation step, nitrogen samples comprised larger La 2 O 3 crystallites (22–40 nm) compared to argon (9–17 nm). Upon oxidation, argon samples resulted in a pure LSCF phase with surface areas in the 21–29 m 2 ·g −1 range, whereas nitrogen samples contained significant impurities. This demonstrates that the size of La 2 O 3 crystallites formed during inert processing limited the ability to produce a pure LSCF phase. Symmetrical cells comprising nano-LSCF electrodes generated by the templating method were compared to cells sintered directly in air. Impedance results suggest that nano-LSCF cells and cells processed in air were dominated by interfacial charge transfer resistance and gas diffusion, respectively. The results map out conditions for preparing and integrating high surface area, nanostructured LSCF into SOFC electrodes at traditional sintering temperatures. Strategies for improving the interfacial resistance of nano-LSCF electrodes are discussed.

Muhoza, Sixbert P. (ORCID:0000000299864241)↗

DOE OSTI2020

Use of the lignocellulose-degrading bacterium Caldicellulosiruptor bescii to assess recalcitrance and conversion of wild-type and transgenic poplar

Abstract Background Biological conversion of lignocellulosic biomass is significantly hindered by feedstock recalcitrance, which is typically assessed through an enzymatic digestion assay, often preceded by a thermal and/or chemical pretreatment. Here, we assay 17 lines of unpretreated transgenic black cottonwood ( Populus trichocarpa ) utilizing a lignocellulose-degrading, metabolically engineered bacterium, Caldicellulosiruptor bescii . The poplar lines were assessed by incubation with an engineered C. bescii strain that solubilized and converted the hexose and pentose carbohydrates to ethanol and acetate. The resulting fermentation titer and biomass solubilization were then utilized as a measure of biomass recalcitrance and compared to data previously reported on the transgenic poplar samples. Results Of the 17 transgenic poplar lines examined with C. bescii , a wide variation in solubilization and fermentation titer was observed. While the wild type poplar control demonstrated relatively high recalcitrance with a total solubilization of only 20% and a fermentation titer of 7.3 mM, the transgenic lines resulted in solubilization ranging from 15 to 79% and fermentation titers from 6.8 to 29.6 mM. Additionally, a strong inverse correlation ( R 2 = 0.8) between conversion efficiency and lignin content was observed with lower lignin samples more easily converted and solubilized by C. bescii . Conclusions Feedstock recalcitrance can be significantly reduced with transgenic plants, but finding the correct modification may require a large sample set to identify the most advantageous genetic modifications for the feedstock. Utilizing C. bescii as a screening assay for recalcitrance, poplar lines with down-regulation of coumarate 3-hydroxylase 3 (C3H3) resulted in the highest degrees of solubilization and conversion by C. bescii . One such line, with a growth phenotype similar to the wild-type, generated more than three times the fermentation products of the wild-type poplar control, suggesting that excellent digestibility can be achieved without compromising fitness of the tree.

09 BIOMASS FUELS↗

DOE OSTI2020

Crack Growth Rate and Fracture Toughness Tests on Irradiated Ex-Plant Materials

The performance of structural materials is critical for the safe and economic operation of light water reactors. Exposed to neutron irradiation during service, the reactor core internal materials can undergo significant microstructural and microchemical changes, leading to irradiation hardening and embrittlement. To ensure the structural integrity and functionality of nuclear reactor components during long-term operation, material degradation and damage mechanisms must be understood and managed adequately. In this work, irradiated materials harvested from the decommissioned Zorita reactor were studied for their cracking susceptibility and fracture resistance as a function of irradiation dose up to 47 displacement per atom (dpa). The material is a Type 304 stainless steel sectioned from the baffle plates of this pressurized water reactor with 38 years of service. Crack growth rate and fracture toughness J-resistance (J-R) curve tests were performed in low-corrosion-potential environments at ~315°C. All samples behaved similarly under cyclic loading, and no deteriorated corrosion-fatigue behavior was observed in the test environments. Under constant stress intensity factors, most samples did not show elevated crack growth rates, suggesting an adequate stress corrosion cracking resistance in the test environments. However, an unstable cracking behavior was observed in a 47-dpa sample, resulting in significantly higher crack growth rates than expected at high stress intensity factors. Crack instability was also observed in a 0.06-dpa sample but did not lead to a sustained high crack growth rate. The impact of neutron irradiation was more evident in the fracture toughness J-R curve tests. As the dose increased, the J-R curve declined considerably and became very shallow at high doses. A fully intergranular fracture morphology was also observed among the high-dose samples ruptured in an air atmosphere at room temperature. This brittle fracture mode in the absence of high temperature water environment confirmed a high degree of embrittlement of this material resulting from its service exposure to neutron irradiation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Use of Ionic Liquids for Hemp Fiber Degumming

Degumming or retting to remove pectin, lignin, and hemicellulose is a critical step in the production of high-quality hemp fibers. Current technologies, including traditional water or dew retting, as well as chemical, enzymatic, and physical degumming processes, have inherent environmental risks and produce fibers of varying qualities. Herein we explore the use of an ionic liquid (IL) capable of dissolving pectin, lignin, and hemicellulose, but not cellulose, in combination with different oxidating agents to degum hemp. In this study, we observed that treating raw hemp fibers with the IL choline acetate ([Cho][OAc]), alone or in combination with aqueous H 2 O 2 , led to a reduction in the gummy materials and lignin content of the resulting samples of up to 63 and 78%, respectively. More importantly, the high crystallinity and low reduction in tensile strength of the resulting fibers make these novel and relatively simple IL-based processes promising alternatives toward the sustainable preparation of hemp-based materials suitable for use in the textile industry.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Nevada National Security Site 2019 Data Report: Groundwater Monitoring Program Area 5 Radioactive Waste Management Site

This report presents groundwater and leachate sample results from the Area 5 Radioactive Waste Management Site (RWMS) at the Nevada National Security Site in Nye County, Nevada. Since 1993, groundwater samples have been collected and static water levels have been measured from the aquifer immediately below the Area 5 RWMS. The data are evaluated for evidence of effects on the aquifer related to the Area 5 RWMS. Leachate from the Cell 18 lined mixed waste cell has been sampled since 2011, and leachate from the Cell 25 lined mixed waste cell was first sampled in 2019 after it began receiving waste in August 2018. Leachate data are analyzed for hazardous contaminants to determine appropriate leachate handling and disposal. This report includes five years of data from 2015 through 2019.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

NEVADA NATIONAL SECURITY SITE 2020 DATA REPORT- GROUNDWATER MONITORING PROGRAM AREA 5 RADIOACTIVE WASTE MANAGEMENT SITE

This report presents groundwater and leachate sample results from the Area 5 Radioactive Waste Management Site (RWMS) at the Nevada National Security Site in Nye County, Nevada. Since 1993, groundwater samples have been collected and static groundwater depths have been measured from the aquifer immediately below the Area 5 RWMS. The data are evaluated for evidence of effects on the aquifer related to the Area 5 RWMS. Leachate from the Cell 18 lined mixed waste cell has been sampled since 2011, and leachate from the Cell 25 lined mixed waste cell was first sampled in 2019 after it began receiving waste in August 2018. Leachate data are analyzed for hazardous contaminants to determine appropriate leachate handling and disposal. This report includes five years of data from 2016 through 2020.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Texture analysis of AGR program matrix materials

We report the fuel form for high-temperature gas-cooled reactors consists of tristructural isotropic (TRISO) particles embedded in a matrix of graphite flake and carbonized resin. The process of overcoating particles prior to compacting yields a circumferential orientation of the graphite flake surrounding the TRISO particles, which is modified to varied extents when overcoated particles are pressed into the final fuel form. As graphite is highly anisotropic, the texture may impact the properties and performance of the fuel. Ellipsometry was used to measure the texture of the matrix for fueled compacts and unfueled “matrix-only” samples. Results indicated local texture related to the spherical particles in compacts associated with overcoating versus a more linear layered structure in “matrix-only” samples.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Data-driven electron-diffraction approach reveals local short-range ordering in CrCoNi with ordering effects

Abstract The exceptional mechanical strength of medium/high-entropy alloys has been attributed to hardening in random solid solutions. Here, we evidence non-random chemical mixing in a CrCoNi alloy, resulting from short-range ordering. A data-mining approach of electron nanodiffraction enabled the study, which is assisted by neutron scattering, atom probe tomography, and diffraction simulation using first-principles theory models. Two samples, one homogenized and one heat-treated, are observed. In both samples, results reveal two types of short-range-order inside nanoclusters that minimize the Cr–Cr nearest neighbors (L1 2 ) or segregate Cr on alternating close-packed planes (L1 1 ). The L1 1 is predominant in the homogenized sample, while the L1 2 formation is promoted by heat-treatment, with the latter being accompanied by a dramatic change in dislocation-slip behavior. These findings uncover short-range order and the resulted chemical heterogeneities behind the mechanical strength in CrCoNi, providing general opportunities for atomistic-structure study in concentrated alloys for the design of strong and ductile materials.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Effect of particle characteristics on the evolution of particle size, particle morphology, and fabric of sands loaded under uniaxial compression

This work presents the results and analyses of uniaxial compression experiments performed on three silica sands. The sands have comparable particle-size distributions, but their particles differ in morphology and strength. Cylindrical samples of the three sands were compressed in a loading device placed inside an X-ray microscope (XRM) and scanned at multiple stress levels during uniaxial compression. 3D tomography data of the samples obtained from the XRM at different stress levels were then analyzed to obtain the distributions of particle size, particle morphology, and interparticle contact normals within the sample. Results indicate that: (1) the compressibility of the sands loaded under uniaxial compression is closely tied to particle morphology and strength and (2) the anisotropy in the orientations of interparticle contact normals generally increases with axial stress; however, this increase is limited by the occurrence of particle crushing in the sample.

3D X-ray computed tomography↗