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DOE OSTI2016

Site-Specific Preparation of Intact Solid–Liquid Interfaces by Label-Free In Situ Localization and Cryo-Focused Ion Beam Lift-Out

Abstract Scanning transmission electron microscopy (STEM) allows atomic scale characterization of solid–solid interfaces, but has seen limited applications to solid–liquid interfaces due to the volatility of liquids in the microscope vacuum. Although cryo-electron microscopy is routinely used to characterize hydrated samples stabilized by rapid freezing, sample thinning is required to access the internal interfaces of thicker specimens. Here, we adapt cryo-focused ion beam (FIB) “lift-out,” a technique recently developed for biological specimens, to prepare intact internal solid–liquid interfaces for high-resolution structural and chemical analysis by cryo-STEM. To guide the milling process we introduce a label-free in situ method of localizing subsurface structures in suitable materials by energy dispersive X-ray spectroscopy (EDX). Monte Carlo simulations are performed to evaluate the depth-probing capability of the technique, and show good qualitative agreement with experiment. We also detail procedures to produce homogeneously thin lamellae, which enable nanoscale structural, elemental, and chemical analysis of intact solid–liquid interfaces by analytical cryo-STEM. This work demonstrates the potential of cryo-FIB lift-out and cryo-STEM for understanding physical and chemical processes at solid–liquid interfaces.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Neutron and Thermal Embrittlement of RPV Steels: An Overview

Because the reactor pressure vessel (RPV) represents the first structural line of defense against the release of radiation to the public, the design and fabrication of the RPV for any nuclear reactor facility is performed at very high standards in accordance with consensus codes that are based on mechanical and physical properties of the steels used to construct the vessel. Nuclear RPVs may weigh up to 800 tons with wall thicknesses up to approximately 330 mm and are clad on the inside with stainless-steel weld metal and given a final post-weld heat treatment. The RPV is a unique structural component in that it operates under high pressures and temperatures and is exposed to relatively high neutron radiation. Although typical RPV steels and welds have excellent fracture toughness at room temperature and above when put into service, the degrading effects of high-energy neutron irradiation can cause levels of irradiation-induced embrittlement in radiation-sensitive materials of concern for the structural integrity of the RPV. In recent decades, remarkable progress has been made in developing a mechanistic understanding of irradiation embrittlement. This progress includes developing physically based and statistically calibrated models of Charpy V-notch-indexed transition temperature shifts based on results from RPV surveillance programs complemented by significant results from comprehensive research experiments performed in test reactors. In addition, advances in elastic-plastic fracture mechanics allow for a relatively small number of relatively small specimens to characterize the fracture toughness of RPV steels with statistical confidence. This paper presents a review of the primary mechanical properties, test procedures, examples of applicable codes and standards, and specimen types used to characterize RPV steels and welds, the effects of neutron irradiation on those most relevant mechanical properties, and a brief review of the effects of thermal aging on RPV materials. The paper closes with a summary.

Nanstad, Randy K.↗

DOE OSTI2018

International Network for Nuclear Waste Characterization (IAEA-Labonet) - Facts and Future - 18566

LABONET was launched early 2011 by the International Atomic Energy Agency (IAEA) as an international network on nuclear waste characterization. Its objective is to improve the quality of, and harmonize, activities related to the radioactive waste characterization in IAEA Member States. It is widely accepted that proper characterization of radioactive waste through its entire flow-sheet is a key activity. In particular the needs and problems in radioactive waste characterization in the participating countries are a main concern within LABONET, as the programs are not elaborated to the same level in the various countries. LABONET wants to facilitate the exchange of international experience in the application of proven, quality assured practices for the characterization of waste and waste packages. This will be beneficial for the less developed countries. The objectives of LABONET are achieved via different actions: a) exchanging information and expertise via presentations and discussions at technical meetings; b) expert meetings on particular topics of interest, for instance e-learning and e-platforms; c) training sessions in less developed countries, for instance, on non-destructive assay of waste packages; d) facilitate the exchange of information amongst its members; and e) assist member states in establishing characterization plans that are cost effective and of good quality. LABONET is continuously encouraging institutions or professionals who need some assistance or can help in solving questions about characterization to be a member. Currently, LABONET is preparing for its future, including projects addressing common problems of its members. Aiming at the dissemination of this important network for the professionals involved in radioactive waste characterization, this paper will discuss the following issues: (1) the objectives of LABONET, (2) its structure, membership and organization of meetings, (3) some achievements, and (4) plans for the future. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2004

NASA Thermographic Inspection of Advanced Composite Materials

As the use of advanced composite materials continues to increase in the aerospace community, the need for a quantitative, rapid, in situ inspection technology has become a critical concern throughout the industry. In many applications it is necessary to monitor changes in these materials over an extended period of time to determine the effects of various load conditions. Additionally, the detection and characterization of defects such as delaminations, is of great concern. This paper will present the application of infrared thermography to characterize various composite materials and show the advantages of different heat source types. Finally, various analysis methodologies used for quantitative material property characterization will be discussed.

Cramer, K. Elliott↗

DOE OSTI2022

Characterization of modeling and experimental data inconsistencies from burst testing for high-burnup commercial fuel rod applications

Fuel fragmentation, relocation, and dispersal are some of the largest issues remaining in the nuclear industry before rod-average burnup can be increased beyond 62 GWd/tU. The issue is primarily related to the potential for fuel to be dispersed into the reactor primary system, which may increase public risk. One way to prevent dispersal is to avoid cladding burst. The objective of this work is to support the high burnup safety case by evaluating cladding burst under high-burnup, full-length fuel rods and to identify uncertainties that could improve model predictions. The results of this analysis will evaluate realistic, prototypic loss-of-coolant accident (LOCA) conditions; support future cladding burst test designs; and inform the development of mechanistic material models. Realistic high-burnup operating conditions were implemented in the BISON fuel performance code to simulate steady-state and LOCA transient fuel rod evolution to the point at which cladding burst occurred. Parametric studies are performed to assess code response to changes in rod internal pressures and heating rates. Results were compared with simulated LOCA experiments to identify inconsistencies between commercial fuel rod analysis and experimental validation. The representative full-length fuel rod LOCA simulation results did not agree with cladding burst tests. Cladding burst tests indicated burst occurring well below (100–150 °C) those calculated in the full-length fuel rod LOCA analysis. Further investigation indicated that the cladding burst tests do not appear to be representative for full-length fuel rods. The inconsistency investigated in this work showed that the differences between the BISON simulation and the experiment's cladding burst conditions arise from an incomplete characterization of the cladding surface temperature, detailed rodlet characterization, lack of cladding strain measurements, and uncertainty in the cladding creep and failure models.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS2019

Analysis of the DebriSat Fragments and Comparison to the NASA Standard Satellite Breakup Model

Existing DOD and NASA satellite breakup models are based on a key laboratory test, the 1992 Satellite Orbital debris Characterization Impact Test, which has supported many applications and matched on-orbit events involving older satellite designs reasonably well over the years. In 2014, the NASA Orbital Debris Program Office, in collaboration with the Air Force Space and Missile Systems Center, The Aerospace Corporation, and the University of Florida, conducted a hypervelocity impact test using a high-fidelity, mock-up satellite, DebriSat, in controlled and instrumented laboratory conditions to update and improve these models. DebriSat is representative of present-day, low Earth orbit satellites, having been constructed with modern spacecraft materials and techniques. The DebriSat fragment ensemble provided a variety of shapes, bulk densities, and dimensions. Fragments down to 2 mm in size are being characterized by their physical and derived properties. The data will inform updates to the current NASA Standard Satellite Breakup Model (SSBM), which was formulated using laboratory and ground-based measurements of on-orbit fragmentation events to describe an average breakup for spacecraft and upper-stage collisions and explosions. Although individual fragment collection and characterization is still ongoing, this paper will present the status of the DebriSat fragment data analysis including cumulative characteristic length and cumulative mass distributions, area-to-mass distributions, and characteristic length versus mass distributions. Additionally, comparisons to the NASA SSBM will be presented.

Murray, James↗

DOE OSTI2018

Infrastructure development for radioactive materials at the NSLS-II

The X-ray Powder Diffraction (XPD) Beamline at the National Synchrotron Light Source-II is a multipurpose instrument designed for high-resolution, high-energy X-ray scattering techniques. In this article, the capabilities, opportunities and recent developments in the characterization of radioactive materials at XPD are described. The overarching goal of this work is to provide researchers access to advanced synchrotron techniques suited to the structural characterization of materials for advanced nuclear energy systems. XPD is a new beamline providing high photon flux for X-ray Diffraction, Pair Distribution Function analysis and Small Angle X-ray Scattering. The infrastructure and software described here extend the existing capabilities at XPD to accommodate radioactive materials. Such techniques will contribute crucial information to the characterization and quantification of advanced materials for nuclear energy applications. We describe the automated radioactive sample collection capabilities and recent X-ray Diffraction and Small Angle X-ray Scattering results from neutron irradiated reactor pressure vessel steels and oxide dispersion strengthened steels.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2014

Characterization of scatter in digital mammography from use of Monte Carlo simulations and comparison to physical measurements

Purpose: Monte Carlo simulations were performed with the goal of verifying previously published physical measurements characterizing scatter as a function of apparent thickness. A secondary goal was to provide a way of determining what effect tissue glandularity might have on the scatter characteristics of breast tissue. The overall reason for characterizing mammography scatter in this research is the application of these data to an image processing-based scatter-correction program. Methods: MCNPX was used to simulate scatter from an infinitesimal pencil beam using typical mammography geometries and techniques. The spreading of the pencil beam was characterized by two parameters: mean radial extent (MRE) and scatter fraction (SF). The SF and MRE were found as functions of target, filter, tube potential, phantom thickness, and the presence or absence of a grid. The SF was determined by separating scatter and primary by the angle of incidence on the detector, then finding the ratio of the measured scatter to the total number of detected events. The accuracy of the MRE was determined by placing ring-shaped tallies around the impulse and fitting those data to the point-spread function (PSF) equation using the value for MRE derived from the physical measurements. The goodness-of-fit was determined for each data set as a means of assessing the accuracy of the physical MRE data. The effect of breast glandularity on the SF, MRE, and apparent tissue thickness was also considered for a limited number of techniques. Results: The agreement between the physical measurements and the results of the Monte Carlo simulations was assessed. With a grid, the SFs ranged from 0.065 to 0.089, with absolute differences between the measured and simulated SFs averaging 0.02. Without a grid, the range was 0.28–0.51, with absolute differences averaging −0.01. The goodness-of-fit values comparing the Monte Carlo data to the PSF from the physical measurements ranged from 0.96 to 1.00 with a grid and 0.65 to 0.86 without a grid. Analysis of the data suggested that the nongrid data could be better described by a biexponential function than the single exponential used here. The simulations assessing the effect of breast composition on SF and MRE showed only a slight impact on these quantities. When compared to a mix of 50% glandular/50% adipose tissue, the impact of substituting adipose or glandular breast compositions on the apparent thickness of the tissue was about 5%. Conclusions: The findings show agreement between the physical measurements published previously and the Monte Carlo simulations presented here; the resulting data can therefore be used more confidently for an application such as image processing-based scatter correction. The findings also suggest that breast composition does not have a major impact on the scatter characteristics of breast tissue. Application of the scatter data to the development of a scatter-correction software program can be simplified by ignoring the variations in density among breast tissues.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS1992

Development and characterization of Powder Metallurgy (PM) 2XXX series Al alloy products and Metal Matrix Composite (MMC) 2XXX Al/SiC materials for high temperature aircraft structural applications

The results of a series of material studies performed by the Lockheed Aeronautical Systems Company over the time period from 1980 to 1991 are discussed. The technical objective of these evaluations was to develop and characterize advanced aluminum alloy materials with temperature capabilities extending to 350 F. An overview is given of the first five alloy development efforts under this contract. Prior work conducted during the first five modifications of the alloy development program are listed. Recent developments based on the addition of high Zr levels to an optimum Al-Cu-Mg alloy composition by powder metallurgy processing are discussed. Both reinforced and SiC or B4C ceramic reinforced alloys were explored to achieve specific target goals for high temperature aluminum alloy applications.

Chellman, D. J.↗

DOE OSTI2016

Characterization of the photocurrents generated by the laser of atomic force microscopes

The conductive atomic force microscope (CAFM) has become an essential tool for the nanoscale electronic characterization of many materials and devices. When studying photoactive samples, the laser used by the CAFM to detect the deflection of the cantilever can generate photocurrents that perturb the current signals collected, leading to unreliable characterization. In metal-coated semiconductor samples, this problem is further aggravated, and large currents above the nanometer range can be observed even without the application of any bias. Here we present the first characterization of the photocurrents introduced by the laser of the CAFM, and we quantify the amount of light arriving to the surface of the sample. The mechanisms for current collection when placing the CAFM tip on metal-coated photoactive samples are also analyzed in-depth. Finally, we successfully avoided the laser-induced perturbations using a two pass technique: the first scan collects the topography (laser ON) and the second collects the current (laser OFF). We also demonstrate that CAFMs without a laser (using a tuning fork for detecting the deflection of the tip) do not have this problem.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2021

Electrochemistry of Thin Films with In Situ/Operando Grazing Incidence X-Ray Scattering: Bypassing Electrolyte Scattering for High Fidelity Time Resolved Studies

Electroactive polymer thin films undergo repeated reversible structural change during operation in electrochemical applications. While synchrotron X-ray scattering is powerful for the characterization of stand-alone and ex situ organic thin films, in situ/operando structural characterization has been underutilized-in large part due to complications arising from supporting electrolyte scattering. This has greatly hampered the development of application relevant structure property relationships. Therefore, a new methodology for in situ/operando X-ray characterization that separates the incident and scattered X-ray beam path from the electrolyte is developed. As a proof of concept, the operando structural characterization of weakly-scattering, organic mixed conducting thin films in an aqueous electrolyte environment is demonstrated, accessing previously unexplored changes in the $\pi-\pi$ peak and diffuse scatter, while capturing the solvent swollen thin film structure which is inaccessible in previous ex situ studies. These in situ/operando measurements improve the sensitivity to structural changes, capturing minute changes not possible ex situ, and have multimodal potential such as combined Raman measurements that also serve to validate the true in situ/operando conditions of the cell. Finally, new directions enabled by this in situ/operando cell design are examined and state of the art measurements are compared.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2018

Characterization of the Impact of Soft Errors on Iterative Methods

Soft errors caused by transient bit flips have the potential to significantly impact an application’s behavior. This has motivated the design of an array of techniques to detect, isolate, and correct soft errors using microarchitectural, architectural, compilation-based, or application-level techniques to minimize their impact on the executing application. The first step towards the design of good error detection/correction techniques involves an understanding of an application’s vulnerability to soft errors. In this paper, we present the first comprehensive characterization of the impact of soft errors on the convergence characteristics of six iterative methods using application-level fault injection. In particular, we consider the use of iterative methods to incrementally solve a linear systems of equations, which constitutes the core kernel in many scientific applications. We analyze the impact of soft errors in terms of the type of error (single- vs multi-bit), the distribution and location of bits affected, the data structure and the statement impacted, and variation with time. In addition to understanding the vulnerability of iterative solvers to soft errors, this characterization can aid the design of fault injection campaigns that ensure systematic coverage.

fault injection, iterative methods, Silent data co↗

DOE OSTI2020

Quantitative Performance Assessment of Proxy Apps and Parents (ECP Proxy App Project Milestone ADCD-504-9)

This report presents highlights of these efforts. Section 2 describes work that has been done to compare the performance of proxy applications on AMD MI60 vs. Nvidia V100 GPUs. So far only a small set of ECP proxies are running on AMD GPUs, but we will continue to expand this analysis as additional proxies become available. We find that although the MI60 and V100 have nearly the same measured memory bandwidth, memory bound proxy app kernels perform 20-30% worse on the MI60. Further work is needed to refine these comparisons to determine whether the root cause is due to differences in the hardware, software stack, platform specific optimization, or some combination of the three. Section 3 describes our continuing effort to find methods to accurately assess the similarity of proxies and parents. We have recently seen very encouraging results using a cosine similarity metric. This technique uses the angle between two vectors of hardware performance counters to characterize the similarity (or difference) between two applications or proxies. We show not only that several widely used proxies are highly similar to their parents, but also that they differ from non-related codes. We also show that cosine similarity can be used to identify gaps and redundancies in suites and even to gain insight into the effects of architectural differences between platforms. Our work on assessing the Exascale toolchain is ongoing. Our successes with performance measurement tools are evident from the data provided in this report. However, our assessments across the broader tool chain are still too incomplete to provide a meaningful report at this time. We will continue to assess tools and work with vendors and third party developers as issues are identified.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2016

Characterization of intermetallics in aluminum to zinc coated interstitial free steel joining by pulsed MIG brazing for automotive application

In order to meet the demand for lighter and more fuel efficient vehicles, a significant attempt is currently being focused toward the substitution of aluminum for steel in the car body structure. It generates vital challenge with respect to the methods of joining to be used for fabrication. However, the conventional fusion joining has its own difficulty owing to formation of the brittle intermetallic phases. In this present study AA6061-T6 of 2 mm and HIF-GA steel sheet of 1 mm thick are metal inert gas (MIG) brazed with 0.8 mm Al–5Si filler wire under three different heat inputs. The effect of the heat inputs on bead geometry, microstructure and joint properties of MIG brazed Al-steel joints were exclusively studied and characterized by X-ray diffraction, field emission scanning electron microscopy (FESEM), electron probe micro analyzer (EPMA) and high resolution transmission electron microscopy (HRTEM) assisted X-ray spectroscopy (EDS) and selective area diffraction pattern. Finally microstructures were correlated with the performance of the joint. Diffusion induced intermetallic thickness measured by FESEM image and concentration profile agreed well with the numerically calculated one. HRTEM assisted EDS study was used to identify the large size FeAl{sub 3} and small size Fe{sub 2}Al{sub 5} type intermetallic compounds at the interface. The growth of these two phases in A2 (heat input: 182 J mm{sup −1}) is attributed to the slower cooling rate with higher diffusion time (~ 61 s) along the interface in comparison to the same for A1 (heat input: 155 J mm{sup −1}) with faster cooling rate and shorter diffusion time (~ 24 s). The joint efficiency as high as 65% of steel base metal is achieved for A2 which is the optimized parameter in the present study. - Highlights: • AA 6061 and HIF-GA could be successfully joined by MIG brazing. • Intermetallics are exclusively studied and characterized by XRD, FESEM and EPMA. • Intermetallic formation by diffusion is worth considering or not. • HRTEM-EDS, SAD pattern identifies the morphologies and size of intermetallics. • A compromise concerning formation of IMC is necessary.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Illuminating the Material World: Autonomous Microscopy to Understand Order, Disorder, and Everything In Between

Artificial intelligence (AI) holds immense promise for revolutionizing microscopy, yet its widespread adoption has been hindered by challenges ranging from user inexperience to limited model transferability and difficulties in operationalizing machine learning. This presentation showcases our approach to developing practical autonomy for materials discovery, aiming to accelerate the integration of AI into everyday microscopy workflows. As shown in Fig. 1, I will focus on three key areas: understanding order-disorder transitions, quantifying point defects, and achieving truly device-scale microscopy. First, I will demonstrate the power of multi-modal knowledge graphs for integrating diverse microscopy data. By combining imaging, spectroscopy, and diffraction data, these graphs provide a holistic view of material behavior, capturing the intricate relationships between different modalities [1,2]. I will present a case study on how these models illuminate the structural and chemical changes associated with irradiation in oxide thin films, revealing critical insights for designing materials for extreme environments like spaceflight and nuclear energy. Specifically, I will show how multi-modal analysis clarifies the evolution of order-disorder transitions under irradiation, a key factor influencing material performance in these applications. Next, I will address the challenge of quantifying point defects in 2D materials. We demonstrate the application of computer vision and transfer learning to accurately identify and classify various defect types, such as vacancies and substitutional atoms, and to quantify their concentrations. This information is crucial for understanding and tailoring the properties of 2D materials for applications in electronics, optoelectronics, and catalysis. For example, I will show how our models can characterize the topological distribution of point defects in MXene transition metal carbides, providing valuable insights for optimizing their performance in energy storage and separation science. Finally, I will discuss our progress toward autonomous device-scale microscopy [3,4]. We are fundamentally redesigning electron microscopes around the principles of machine reasoning, enabling automation beyond basic tasks like sample navigation and data acquisition to include sophisticated experimental design. This approach paves the way for truly reproducible and massively scaled analysis campaigns. I will emphasize the importance of autonomous microscopy platforms for high-throughput materials discovery and characterization, facilitating the rapid screening of materials for a broad range of applications and accelerating the development of next-generation technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Empirically testing vaterite structural models using neutron diffraction and thermal analysis

Otoliths, calcium carbonate (CaCO 3 ) ear bones, are among the most commonly used age and growth structures of fishes. Most fish otoliths are comprised of the most dense CaCO 3 polymorph, aragonite. Sturgeon otoliths, in contrast, have been characterized as the rare and structurally enigmatic polymorph, vaterite a metastable polymorph of CaCO 3 . Vaterite is an important material ranging from biomedical to personal care applications although its crystal structure is highly debated. We characterized the structure of sturgeon otoliths using thermal analysis and neutron powder diffraction, which is used non-destructively. We confirmed that while sturgeon otoliths are primarily composed of vaterite, they also contain the denser CaCO 3 polymorph, calcite. For the vaterite fraction, neutron diffraction data provide enhanced discrimination of the carbonate group compared to x-ray diffraction data, owing to the different relative neutron scattering lengths, and thus offer the opportunity to uniquely test the more than one dozen crystal structural models that have been proposed for vaterite. Of those, space group P6 5 22 model, a = 7.1443(4)Å , c = 25.350(4)Å , V = 1121.5(2)Å 3 provides the best fit to the neutron powder diffraction data, and allows for a structure refinement using rigid carbonate groups.

60 APPLIED LIFE SCIENCES↗

NASA NTRS2006

2.4 Micron Cutoff AlGaAsSb/InGaAsSb Phototransistors for Shortwave IR Applications

Shortwave infrared detectors are critical for several applications including remote sensing and optical communications. Several detectors are commercially available for this wavelength range, but they lack sufficient gain, which limits their detectivity. The characterization results of an AlGaAsSb/InGaAsSb phototransistor for shortwave IR application are reported. The phototransistor is grown using molecular beam epitaxy technique. Spectral response measurements showed a uniform responsivity between 1.2 and 2.4 micron region with a mean value of 1000 A/W. A maximum detectivity of 3.4 X 10(exp 11) cmHz1/2/W was obtained at 2 micron at -20 C and 1.3 V.

Refaat, Tamer F.↗

DOE OSTI2014

RISMC Advanced Safety Analysis Project Plan – FY 2015 - FY 2019

In this report, a project plan is developed, focused on industry applications, using Risk-Informed Safety Margin Characterization (RISMC) tools and methods applied to realistic, relevant, and current interest issues to the operating nuclear fleet. RISMC focuses on modernization of nuclear power safety analysis (tools, methods and data); implementing state-of-the-art modeling techniques (which include, for example, enabling incorporation of more detailed physics as they become available); taking advantage of modern computing hardware; and combining probabilistic and mechanistic analyses to enable a risk informed safety analysis process. The modernized tools will maintain the current high level of safety in our nuclear power plant fleet, while providing an improved understanding of safety margins and the critical parameters that affect them. Thus, the set of tools will provide information to inform decisions on plant modifications, refurbishments, and surveillance programs, while improving economics. This set of tools will also benefit the design of new reactors, enhancing safety per unit cost of a nuclear plant. The proposed plan will focus on application of the RISMC toolkit, in particular, solving realistic problems of important current issues to the nuclear industry, in collaboration with plant owners and operators to demonstrate the usefulness of these tools in decision making.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗