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DOE OSTI2025

Characterization and Quantification of Radiation-Induced Clusters/Precipitates in RPV Steels Using STEM-EDS and Machine Learning

Over the operational lifespan of a nuclear reactor, reactor pressure vessel (RPV) steels are subjected to significant neutron irradiation, resulting in complex microstructural changes and the consequent degradation of mechanical properties. Various physically motivated correlation models have been developed to predict neutron irradiation-induced embrittlement of RPVs under different irradiation conditions. However, the efficient and accurate characterizations and quantification of radiation-induced clusters in RPVs are still challenging, which will affect the precision of the predictive models for embrittlement of RPV components. In the DOE Visiting Faculty Program (VFP) research work at Oak Ridge National Lab (ORNL), I integrate machine learning to aid Scanning Transmission Electron Microscopy – Energy Dispersive X-ray Spectroscopy (STEM-EDS) analyses, which improve the characterization and quantification of radiation-induced clusters in RPV steels, thereby enabling more accurate predictions of material behavior under irradiation. The surveillance base- and welded- RPV steels were annealed at various temperatures of 340 °C, 450 °C and 500 °C for up to 168 hours, respectively. Afterwards, I have characterized radiation-induced clusters using advanced STEM-EDS techniques and subsequently applying machine learning algorithms to analyze and refine STEM-EDS datasets, enhancing the quantification of clusters compositions and distributions. In the end, an efficient workflow for integrating STEM-EDS data analysis with machine learning to address challenges including noise reduction has been developed. The completion of this VFP work will support bridge critical gaps in the accurate quantification of radiation-induced clusters in RPV steels using STEM-EDS and support the development of more precise models for predicting RPV embrittlement in the Light Water Reactor Sustainability program supported by Department of Energy and enhancing the collaboration between ORNL and Alred University. The outcome of the VFP project will leverage a few research papers submission to peer-reviewed journals in the relevant scientific field and a few oral presentations at national and international conferences.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2025

Effects of dose rate on the microstructure and deuterium retention in γ-LiAlO 2 pellets

This report presents experimental findings obtained from November 2024 to September 2025. Defect accumulation and microstructural evolution during ion irradiation at elevated temperatures are governed by two competing processes: defect production, driven by dose rate, and defect recovery, controlled by defect diffusion, interaction, and annihilation. At a given dose, the resulting microstructural evolution depends on both the dose rate and irradiation temperature. As a continuation of our FY24 tritium science project, which investigated temperature effects at a fixed dose rate, this study focuses on dose-rate effects at a fixed temperature to provide deeper insights into the irradiated microstructure and compositional changes in γ-LiAlO 2 pellets. The study aims to elucidate the impact of dose rate on microstructure, precipitate morphology, deuterium retention, and lithium volatility in γ-LiAlO 2 pellets under sequential 120 keV He + and 80 keV D 2 + ion irradiation. Three dose rates of 7.3×10 4 , 2.9×10 4 and 6.8×10 5 dpa/s were applied to achieve the same total ion fluence of 2×10 17 (He + +D + )/cm 2 at 500 °C, corresponding to a maximum combined dose of 7.55 dpa at ~255 nm. The irradiated pellets were subsequently characterized using scanning transmission electron microscopy (STEM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The microstructural response of γ-LiAlO 2 to ion irradiation was found to be strongly dose-rate dependent. At medium and high dose rates, irradiation produced a surface amorphized layer and an underlying crystalline layer containing LiAl 5 O 8 precipitates, with implanted gases accumulating and forming blisters at the crystalline-amorphous interface. It remains to be investigated whether the amorphized layer was produced by He + ion irradiation prior to D 2 + ion irradiation. In contrast, at low dose rates, the material remained crystalline, with cavities, likely gas-filled, distributed around precipitates, within the γ-LiAlO 2 matrix, and along grain boundaries. While precipitate morphology exhibited anisotropy, their size showed little sensitivity to dose rate in the applied range of this study. This result, however, does not rule out the possibility that further reductions in dose rate could influence precipitate size. High dose-rate irradiation enhanced protonium–deuterium isotopic exchange and lithium depletion in the amorphized region. Collectively, the results show that dose rate governs amorphization, gas redistribution, isotopic exchange, and lithium depletion, providing important insights into the mechanisms underlying structural evolution in γ-LiAlO 2 pellets under reactor-relevant irradiation conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2024

Characterization of Mn 5 Ge 3 Contacts on a Shallow Ge/SiGe Heterostructure

Mn 5 Ge 3 is a ferromagnetic phase of the Mn-Ge system that is a potential contact material for efficient spin injection and detection. Here, we investigate the creation of Mn 5 Ge 3 -based contacts on a Ge/SiGe quantum well heterostructure via solid-state synthesis. X-ray diffraction spectra fitting indicates the formation of Mn 5 Ge 3 -based contacts on bulk Ge and Ge/SiGe. High-resolution scanning transmission electron microscopy imaging and energy dispersive X-ray spectroscopy verify the correct Mn 5 Ge 3 -based phase formation. Schottky diode measurements, transmission line measurements, and Hall measurements reveal that Mn 5 Ge 3 -based contacts serve as good p-type contacts for Ge/SiGe quantum well heterostructures due to having a low Schottky barrier height of 0.10 eV (extracted from a Mn 5 Ge 3 /n-Ge analogue) and a contact resistance in the order of 1 kΩ. Furthermore, we show that these electrical characteristics have a gate-voltage dependence, thereby providing tunability.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Heterogeneous Morphologies and Hardness of Co-Sputtered Thin Films of Concentrated Cu-Mo-W Alloys

Heterogeneous microstructures in Cu-Mo-W alloy thin films formed by magnetron co-sputtering immiscible elements with concentrated compositions are characterized using scanning transmission electron microscopy (STEM) and nanoindentation. In this work, we modified the phase separated structure of a Cu-Mo immiscible system by adding W, which impedes surface diffusion during film growth. The heterogeneous microstructures in the Cu-Mo-W ternary system exhibited bicontinuous matrices and agglomerates composed of Mo(W)-rich phase. This is unique, as these are the slower-diffusing species, contrasting past reports of binary Cu-Mo thin films that exhibited Cu-rich agglomerates. The bicontinuous matrices comprised of Cu-rich and Mo(W)-rich phases exhibited bilayer thicknesses of less than 5 nm. The hardness of these thin films measured using nanoindentation is reported and compared to similar multilayers and nanocomposites in binary systems.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Size dependent lattice pseudosymmetry for frustrated decahedral nanoparticles

Geometric frustration—where geometry prevents simultaneous satisfaction of local interactions—generates pseudosymmetry and emergent behaviors across physical and biological systems. At the nanoscale, pseudosymmetric features in crystalline materials manifest as local strain and distortion, but how they depend on particle size and control structural stability remains unclear. Here, we report the first study of a size-dependent crossover in pseudosymmetry in multi-twinned gold nanoparticles (NPs), combining four-dimensional scanning transmission electron microscopy with nanoscale strain mapping grounded in continuum solid mechanics. Analysis of more than 20 decahedral NPs (20–55 nm) reveals pronounced heterogeneity in multiple modes of in-plane strain and displacement field in small NPs as five tetrahedral grains close the geometric gap, without extended defects. With increasing particle size, strain fields homogenize across grains and local phases shift from predominantly low-symmetry body-centered tetragonal motifs at small sizes to face-centered cubic character approaching the bulk limit. We identify a crossover particle size of ~35 nm, well below bulk, correlating with a transition from modified-Wulff shapes to pentagonal bipyramids, consistent with finite element predictions. This quantitative framework for mapping size-dependent strain and pseudosymmetry enables precise design and control of functional crystalline solids and phase transformation for catalysis, photonics, electronics, and energy storage.

Lin, Oliver [University of Illinois at Urbana-Cham↗

DOE OSTI2026

Synthesis of epitaxial TaO$_2$ thin films on Al$_2$O$_3$ by suboxide molecular-beam epitaxy and thermal laser epitaxy

Tantalum dioxide (TaO2) is a metastable tantalum compound. Here, we report the epitaxial stabilization of TaO2 on Al2O3 (1-102) (r-plane sapphire) substrates using suboxide molecular-beam epitaxy (MBE) and thermal laser epitaxy (TLE), demonstrating single-oriented, monodomain growth of anisotropically strained thin films. Microstructural investigation is performed using synchrotron X-ray diffraction and scanning transmission electron microscopy. The tetravalent oxidation state of tantalum is confirmed using X-ray absorption and photoemission spectroscopy as well as electron energy-loss spectroscopy. Optical properties are investigated via spectroscopic ellipsometry and reveal a 0.3 eV Mott gap of the tantalum 5d electrons. Density-functional theory and group theoretical arguments are used to evaluate the limited stability of the rutile phase and reveal the potential to unlock a hidden metal-insulator transition concomitant with a structural phase transition to a distorted rutile phase, akin to NbO2. Our work expands the understanding of tantalum oxides and paves the way for their integration into next-generation electronic and photonic devices.

FOS: Physical sciences↗

NASA NTRS1971

Methods of analyzing microsize particulate aerosols and contaminants.

Methods for analyzing atmospheric aerosols and particulate contaminants from natural and industrial sources are briefly described. Their development was spurred by interest in cosmic dust investigations. These methods make it possible to analyze individual particles ranging in size from 0.01 to 1000 microns for elemental and mineralogical content. The described methods include transmission electron microscopy, scanning electron microscopy, electron probe microanalysis, X-ray diffraction, optical mineralogy, and density measurement.

Blanchard, M. B.↗

NASA NTRS1974

The response of single human cells to zero gravity

The SO15 experiment was designed to extend observations of the effects of zero-gravity to living human cells during and subsequent to a 59-day flight on Skylab 3. A strain of diploid human embryonic lung cells, WI-38, was chosen for this purpose. The studies were concerned with observations designed to detect the effects of zero-gravity on cell growth rates and on cell structure as observed by light microscopy, transmission and scanning electron microscopy and histochemistry. Studies of the effects of zero-gravity on the cell function and the cell cycle were performed by time lapse motion picture photography and microspectrophotometry. Subsequent study of the returned living cells included karotyping, G- and C-banding, and analyses of the culture media used. Some of the living cells returned were banked by deep freeze techniques for possible future experiments.

Montgomery, P. O., Jr.↗

NASA NTRS1981

EBIC/TEM investigations of process-induced defects in EFG silicon ribbon

Electron bombardment induced conductivity and scanning transmission electron microscopy observations on unprocessed and processed edge-defined film-fed growth ribbon show that the phosphorus diffused junction depth is not uniform, and that a variety of chemical impurities precipitate out during processing. Two kinds of precipitates are found (1) 10 nm or less in size, located at the dislocation nodes in sub-boundary like dislocation arrangements formed during processing and (2) large precipitates, the chemical composition of which has been partially identified. These large precipitates emit dense dislocations tangles into the adjacent crystal volume.

Cunningham, B.↗

NASA NTRS1982

Surface characterization and failure analysis of thermally aged, polyimide bonded titanium

This study of high temperature stable adhesive systems using 6Al-4V titanium adherends found that certain adhesive/adherends exhibit a change from cohesive to adhesive failure mode during long term 450 F thermal aging. Lap-shear specimens which exhibited adhesive failures were subjected to failure analysis using scanning transmission electron microscopy (STEM) and surface analysis techniques. Data is presented which supports the conclusion of interfacial failures for these samples.

Peters, P. D.↗

NASA NTRS1986

Lunar sample analysis

A wide variety of lunar sample and meteorite studies were performed. Abstracts of the most recent reports are also attached. Experimental techniques employed have included scanning electron microscopy, transmission electron microscopy, Mossbauer spectroscopy, atomic absorption analysis and a variety of simulation studies.

Housley, R. M.↗

NASA NTRS1987

Origin and evolution of osmoregulatory mechanisms in blue-green algae (cyanobacteria) as a function of metabolic and structural complexity: Reflections of Precambrian paleobiology

Major accomplishments underlying the basic understanding of cyanobacterial resistance to salt tolerance and osmotic stress were made. The methodology proposed included: the tracing of the pathways of formation of osmoregulatory solutes by traditional methods involving C-14 labelled substrates; gas chromatography; amino acid analysis; X-ray analysis using scanning transmission electron microscopy; and most importantly, C-13 labelled substrates, followed by Nuclear Magnetic Resonance (NMR) spectroscopy. It was found that the cyanobacteria employ a diversity of organic, osmoregulatory solutes. Osmoregulatory solutes were found to serve four functions: adjustment of water activity, noninhibition of enzymes; lowering of K sub m of enzymes to allow functioning at normal levels when the intracellular salt accumulates, and extending the pH optimum of enzymes as intracellular pH rises due to proton-potassium ion pump action during osmoregulation. Differences in osmoregulatory solutes may, but are not always, be attributed to differences in nutritional capabilities. The mechanism of osmoregulation and concomitant salt tolerance in halophilic cyanobacteria was elucidated. The activities of betaine and S-Adenosylhomocysteine hydrolase are discussed.

Yopp, John H.↗

NASA NTRS1987

Surface characterization in composite and titanium bonding: Carbon fiber surface treatments for improved adhesion to thermoplastic polymers

The effect of anodization in NaOH, H2SO4, and amine salts on the surface chemistry of carbon fibers was examined by X-ray photoelectron spectroscopy (XPS). The surfaces of carbon fibers after anodization in NaOH and H2SO4 were examined by scanning transmission electron microscopy (STEM), angular dependent XPS, UV absorption spectroscopy of the anodization bath, secondary ion mass spectrometry, and polar/dispersive surface energy analysis. Hercules AS-4, Dexter Hysol XAS, and Union Carbide T-300 fibers were examined by STEM, angular dependent XPS, and breaking strength measurement before and after commercial surface treatment. Oxygen and nitrogen were added to the fiber surfaces by anodization in amine salts. Analysis of the plasmon peak in the carbon 1s signal indicated that H2SO4 anodization affected the morphological structure of the carbon fiber surface. The work of adhesion of carbon fibers to thermoplastic resins was calculated using the geometric mean relationship. A correlation was observed between the dispersive component of the work of adhesion and the interfacial adhesion.

Devilbiss, T. A.↗

NASA NTRS1988

Investigation of a SiC/Ti-24Al-11Nb composite

A summary of ongoing research on the characterization of a continuous fiber reinforced SiC/Ti-24Al-11Nb (at percent) composite is presented. The powder metallurgy fabrication technique is described as are the nondestructive evaluation results of the as-fabricated composite plates. Tensile properties of the SiC fiber, the matrix material, and the 0-deg SiC/Ti-24Al-11Nb composite (fibers oriented unidirectionally, parallel to the loading axis) from room temperature to 1100 C are presented and discussed with regard to the resultant fractography. The as-fabricated fiber-matrix interface has been examined by scanning transmission electron microscopy and the compounds present in the reaction zone have been identified. Fiber-matrix interaction and stability of the matrix near the fiber is characterized at 815, 985, and 1200 C from 1 to 500 hr. Measurements of the fiber-matrix reaction, the loss of C-rich coating from the surface of the SiC fiber, and the growth of the Beta depleted zone in the matrix adjacent to the fiber are presented. These data and the difference in coefficient of thermal expansion between the fiber and the matrix are discussed in terms of their likely effects on mechanical properties.

Brindley, P. K.↗

NASA NTRS1999

Surface Diagnostics in Tribology Technology and Advanced Coatings Development

This paper discusses the methodologies used for surface property measurement of thin films and coatings, lubricants, and materials in the field of tribology. Surface diagnostic techniques include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and tribology examination. Each diagnostic technique provides specific measurement results in its own unique way. In due course it should be possible to coordinate the different pieces of information provided by these diagnostic techniques into a coherent self-consistent description of the surface properties. Examples are given on the nature and character of thin diamond films.

Miyoshi, Kazuhisa↗

NASA NTRS2000

Mechanical, Chemical and Microstructural Characterization of Monazite-Coated Silicon Carbide Fibers

Tensile strengths of as-received Hi-Nicalon and Sylramic fibers and those having monazite surface coatings, deposited by atmospheric pressure chemical vapor deposition, were measured at room temperature and the Weibull statistical parameters determined. The average tensile strengths of uncoated Hi-Nicalon and Sylramic fibers were 3.19 +/- 0.73 and 2.78 +/- 0.53 GPa with a Weibull modulus of 5.41 and 5.52, respectively. The monazite-coated Hi-Nicalon and Sylramic fibers showed strength loss of approx. 10 and 15 percent, respectively, compared with the as-received fibers. The elemental compositions of the fibers and the coatings were analyzed using scanning Auger microprobe and energy dispersive X-ray spectroscopy. The LaPO4 coating on Hi-Nicalon fibers was approximately stoichiometric and about 50 nm thick. The coating on the Sylramic fibers extended to a depth of about 100 to 150 nm. The coating may have been stoichiometric LaPO4 in the first 30 to 40 nm of the layer. However, the surface roughness of Sylramic fiber made this profile somewhat difficult to interpret. Microstructural analyses of the fibers and the coatings were done by scanning electron microscopy, transmission electron microscopy, and selected area electron diffraction. Hi-Nicalon fiber consists of fine beta-SiC nanocrystals ranging in size from 1 to 30 mn embedded in an amorphous matrix. Sylramic is a polycrystalline stoichiometric silicon carbide fiber consisting of submicron beta-SiC crystallites ranging from 100 to 300 nm. Small amount of TiB2 nanocrystallites (approx. 50 nm) are also present. The LaPO4 coating on Hi-Nicalon fibers consisted of a chain of peanut shape particles having monazite-(La) structure. The coating on Sylramic fibers consisted of two layers. The inner layer was a chain of peanut shape particles having monazite-(La) structure. The outer layer was comprised of much smaller particles with a microcrystalline structure.

Bansal, N. P.↗

NASA NTRS1999

Measurements and Diagnostics of Diamond Films and Coatings

The commercial potential of chemical-vapor-deposited (CVD) diamond films has been established and a number of applications have been identified through university, industry, and government research studies. This paper discusses the methodologies used for property measurement and diagnostic of CVD diamond films and coatings. Measurement and diagnostic techniques studied include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and friction examination. Each measurement and diagnostic technique provides unique information. A combination of techniques can provide the technical information required to understand the quality and properties of CVD diamond films, which are important to their application in specific component systems and environments. In this study the combination of measurement and diagnostic techniques was successfully applied to correlate deposition parameters and resultant diamond film composition, crystallinity, grain size, surface roughness, and coefficient of friction.

Miyoshi, Kazuhisa↗

NASA NTRS2004

Growth of Multi-Walled Carbon Nanotubes by Injection CVD Using Cyclopentadienyliron Dicarbonyl Dimer and Cyclooctatetraene Iron Tricarbonyl

Preferential oriented multiwalled carbon nanotubes were prepared by the injection chemical vapor deposition (CVD) method using either cyclopentadienyliron dicarbonyl dimer or cycloctatetraene iron tricarbonyl as the iron catalyst source. The catalyst precursors were dissolved in toluene as the carrier solvent for the injections. The concentration of the catalyst was found to influence both the growth of the nanotubes as well as the amount of iron in the deposited material. As deposited the multiwalled carbon nanotubes contained as little as 2.8% iron by weight. The material was deposited onto tantalum foil and fused silica substrates. The nanotubes were characterized by scanning electron microscopy, transmission electron microscopy, Raman spectroscopy and thermogravimetric analysis. This synthetic route provides a simple and scalable method to deposit MWNTs with a low defect density, low metal content and preferred orientation.

Harris, Jerry D.↗